Ferritic Nitrocarburizing of Plain Carbon Steels: Scholarship at Uwindsor

University of Windsor
Scholarship at UWindsor
Electronic Theses and Dissertations
11-7-2015
Ferritic Nitrocarburizing of Plain Carbon Steels

Madhavan Manivannan
University of Windsor
Follow this and additional works at: http://scholar.uwindsor.ca/etd
Recommended Citation
Manivannan, Madhavan, "Ferritic Nitrocarburizing of Plain Carbon Steels" (2015). Electronic Theses and Dissertations. Paper 5486.
This online database contains the full-text of PhD dissertations and Masters’ theses of University of Windsor students from 1954 forward. These
documents are made available for personal study and research purposes only, in accordance with the Canadian Copyright Act and the Creative
Commons license—CC BY-NC-ND (Attribution, Non-Commercial, No Derivative Works). Under this license, works must always be attributed to the
copyright holder (original author), cannot be used for any commercial purposes, and may not be altered. Any other use would require the permission of
the copyright holder. Students may inquire about withdrawing their dissertation and/or thesis from this database. For additional inquiries, please
contact the repository administrator via email ([email protected]) or by telephone at 519-253-3000ext. 3208.
By
Madhavan Manivannan
A Dissertation
Submitted to the Faculty of Graduate Studies
through the Department of Mechanical, Automotive and Materials Engineering
in Partial Fulfillment of the Requirements for
the Degree of Doctor of Philosophy
at the University of Windsor
Windsor, Ontario, Canada
2015
© 2015 Madhavan Manivannan

by
Madhavan Manivannan
APPROVED BY:
__________________________________________________
K. Li, External Examiner
Oakland University
__________________________________________________
J. Johrendt
Department of Mechanical, Automotive and Materials Engineering
__________________________________________________
R.J. Bowers
__________________________________________________
W. Altenhof
__________________________________________________
D. O. Northwood, Co-Advisor
__________________________________________________
V. Stoilov, Co-Advisor
13th May 2015

DECLARATION OF CO-AUTHORSHIP / PREVIOUS PUBLICATION
This dissertation includes [4] original papers that have been previously
published/submitted for publication in peer reviewed journals, as follows:
Dissertation Publication title/full citation Publication status
Chapter
Finite Element Simulations of Geometric

Chapter 4,5 Distortions in Ferritic Nitrocarburized SAE 1010 “published”
Plain Carbon Steel/Manivannan, M., Stoilov, V.,
and Northwood, D.O., Proceedings of the 5th
International Conference on Thermal Process
Modeling and Computer Simulation, pp. 139-144,
June 16, 2014, Orlando, FL, USA
Chapter 4,5 The Use of Navy C-rings to Study, and Predict,
Distortion in Heat Treated Components:
Experimental Measurements and Computer “published”
Modeling/Manivannan, M., Northwood, D.O., and
Stoilov, V., 2014, International Heat Treatment
and Surface Engineering, 8(4), pp. 168-175
Chapter 6 Ferritic Nitrocarburizing of SAE 1010 Plain
Carbon Steel Parts/Manivannan, M., Stoilov, V., “published”
and Northwood, D.O., 2015, SAE International
Journal of Materials and Manufacturing, 8(2), pp.
482-486
Chapter 6 Numerical Model of the Ferritic Nitrocarburizing
of SAE 1010 Plain Carbon Steel/Manivannan, M., “published”
Stoilov, V., and Northwood, D.O., European
Conference on Heat Treatment 2015 & 22nd
IFHTSE Congress, May 20-22, 2015, Venice, Italy
iii
I hereby declare this dissertation incorporates the outcome of a joint research under
the supervision of Dr. Derek O. Northwood and Dr. Vesselin Stoilov. I am aware of the
University of Windsor Senate Policy on Authorship and I certify that I have properly
acknowledged the contribution of other researchers to my dissertation, and have obtained
written permission from each of the co-authors to include the above material in my
dissertation.
I certify that, with the above qualification, this dissertation, and the research to
which it refers, is the product of my own work.
I certify that I have obtained a written permission from the copyright owner(s) to
include the above published material(s) in my thesis. I certify that the above material
describes work completed during my registration as graduate student at the University of
Windsor.
I declare that, to the best of my knowledge, my dissertation does not infringe upon
anyone’s copyright nor violate any proprietary rights and that any ideas, techniques,
quotations, or any other material from the work of other people included in my
dissertation, published or otherwise, are fully acknowledged in accordance with the
standard referencing practices. Furthermore, to the extent that I have included copyrighted
material that surpasses the bounds of fair dealing within the meaning of the Canada
Copyright Act, I certify that I have obtained a written permission from the copyright
owner(s) to include such material(s) in my dissertation.
I declare that this is a true copy of my dissertation, including any final revisions, as
approved by my dissertation committee and the Graduate Studies office, and that this
iv
dissertation has not been submitted for a higher degree to any other University or
Institution.
v
ABSTRACT
Nitrocarburizing is a case hardening process which improves the hardness and
wear resistance of a component, but results in geometric distortions. Torque converter
pistons (automotive component) and Navy C-ring specimens (measuring tool) made from
SAE 1010 plain carbon steel were used for the distortion analysis. Navy C-rings are
generally used for studying the dimensional changes of a material before analyzing the
dimensional changes of the actual component. Navy C-rings of varying thicknesses were
used to analyze the effect of distortions with the change in thickness. Finite element
simulations of Navy C-rings and torque converter pistons were developed to study the
effect of nitrocarburizing process on distortions. For thinner specimens, the predicted
distortions compare favorably with the experimental values. However, the thicker C-ring
specimens showed high prediction error. To better understand the prediction difference of
the different C-rings and TC pistons, an empirical ratio (bulk volume to nitrocarburized
volume (V/VN)) was introduced. The V/VN ratio will not only help to separate the
nitrocarburized surface dominant and bulk dominant specimens, but also provide a better
comparison of the C-ring size with the actual component.
The reduction of bulk volume to nitrocarburized volume (V/VN) ratio led to a
decrease in both the C-ring’s inner diameter (ID) and gap width (GW) distortion, and a
small increase in outer diameter (OD) distortion.
A composition-depth profile simulation model was also developed to predict the
local distortion due to nitrocarburized phases. The local distortion results showed that the
γ′-phase (Fe4N) in the diffusion zone dominates the overall magnitude of distortion.
vi
The residual stress distribution for 1-step nitrocarburizing treatment was
successfully modeled and validated against the experimental stress. The surface stress for
one-step nitrocarburizing treatment was found to be tensile in nature. This tensile (surface)
residual stress was further reduced by introducing 2-step nitrocarburizing treatments.
Using the nitrogen profile model for 2-step nitrocarburizing, it was found that the
additional γ′-Fe4N phase at the surface resulted in a notable residual (tensile) stress
reduction. Also, the simulated 2-step nitrocarburizing treatments produced a same level of
distortion as 1-step nitrocarburizing treatments. Therefore, the proposed 2-step
nitrocarburizing treatments could potentially improve both the surface quality and fatigue
resistance.
vii
DEDICATION
This dissertation is dedicated to my family
viii
ACKNOWLEDGEMENTS
First, I would like to thank my academic supervisors, Dr. Derek O. Northwood and Dr.
Vesselin Stoilov for their time, technical support and guidance during my graduate studies.
I would like to extend my thanks to the committee members, Dr. William Altenhof, Dr.
Randy Bowers, and Dr. Jennifer Johrendt for their support and advice.
I would also like to acknowledge the support of Mr. Andy Jenner, and Dr. Gang Li.
Finally, the financial support of the Natural Sciences and Engineering Research Council of
Canada (NSERC), the Queen Elizabeth II Graduate Scholarship in Science and
Technology (QEII-GSST) program and the University of Windsor (A.R. & E.G. Ferriss
Graduate Endowment Award, Dr. Ross H. Paul Scholarship) are graciously acknowledged.
ix
TABLE OF CONTENTS
DECLARATION OF CO-AUTHORSHIP / PREVIOUS PUBLICATION .............. III
ABSTRACT ..................................................................................................................... VI
DEDICATION.............................................................................................................. VIII
ACKNOWLEDGEMENTS ........................................................................................... IX
LIST OF TABLES ....................................................................................................... XIV
LIST OF FIGURES ..................................................................................................... XVI
LIST OF APPENDICES .......................................................................................... XXIV
LIST OF ABBREVIATIONS/SYMBOLS................................................................ XXV
NOMENCLATURE .................................................................................................. XXVI
CHAPTER 1 INTRODUCTION ......................................................................................1
1.1 Research Objectives and Approach ............................................................................3
1.2 Dissertation Outline ....................................................................................................3
CHAPTER 2 LITERATURE REVIEW ..........................................................................5
2.1 Ferritic Nitrocarburizing (FNC).................................................................................5
2.1.1 Ion or plasma nitrocarburizing ...........................................................................9
2.1.2 Fluidized bed nitrocarburizing ..........................................................................10
2.1.3 Salt bath nitrocarburizing .................................................................................11
2.1.4 Gas nitrocarburizing .........................................................................................13
x
2.1.5 Vacuum nitrocarburizing...................................................................................14
2.2 Residual stress ..........................................................................................................15
2.3 Distortion ..................................................................................................................19
2.3.1 Distortion prevention methods ..........................................................................22
2.4 Types and use of Navy C-rings .................................................................................23
2.5 Modeling ...................................................................................................................27
2.5.1 Distortion modeling ...........................................................................................30
2.5.2 Composition-Depth profiles: experimental and modeling ................................37
2.5.3 Residual Stress Modeling ..................................................................................43
CHAPTER 3 ANALYTICAL APPROACH .................................................................47
3.1 Distortion reduction ..................................................................................................48
3.1.1 Navy C-ring geometry .......................................................................................49
3.1.2 Materials............................................................................................................49
3.1.4 Heat treatment conditions .................................................................................51
3.1.5 Sample preparation and optical microscopy .....................................................52
3.1.6 Nano-indentation measurements .......................................................................53
3.1.7 Experimental distortion measurements .............................................................54
3.1.8 Numerical (FEM) distortion prediction ............................................................55
3.1.9 Composition-depth profile numerical simulation ..............................................56
3.1.10 Composition-depth profile measurements (experimental) ..............................57
xi
3.2 Reduction in surface residual stress .........................................................................58
CHAPTER 4 NUMERICAL SIMULATIONS FOR NAVY C-RINGS AND
TORQUE CONVERTER PISTONS .............................................................................59
4.1 Material Properties ...................................................................................................59
4.2 Navy C-ring Probe ....................................................................................................60
4.3 Navy C-ring Finite Element Models .........................................................................61
4.3.1 Boundary Conditions .........................................................................................62
4.3.2 Discretization of the C-ring models...................................................................63
4.4 Simulation Procedure of C-ring models ...................................................................64
4.5 Axisymmetric Torque Converter Piston Model.........................................................65
4.6 Simulation procedure of axisymmetric TC piston model ..........................................66
CHAPTER 5 VALIDATION OF THE FINITE ELEMENT MODELS ....................68
5.1 Distortion results of Navy C-rings ............................................................................68
5.2 Bulk Volume/Nitrocarburized Volume Ratio ............................................................74
5.3 Distortion results of torque converter (TC) pistons ..................................................76
CHAPTER 6 COMPOSITION-DEPTH PROFILE SIMULATION MODEL .........80
6.1 Carbon and nitrogen composition-depth profile simulation ....................................80
6.2 Microstructure of torque converter (TC) piston samples .........................................83
6.3 Composition-depth profile results.............................................................................85
6.4 Residual stress determination – 1-step nitrocarburizing ..........................................87
xii
6.5 N composition-depth profile model for two-step nitrocarburizing treatments .........90
6.5.1 Composition-depth profile results – varying the 1st step temperature ..............93
6.5.2 Composition-depth profile results – varying the 2nd step temperature .............95
6.5.3 Composition-depth profile results – varying the 1st step N wt. % .....................97
6.5.4 Composition-depth profile results – increased process time ............................98
6.6 Residual stress determination – 2-step nitrocarburizing ........................................102
CHAPTER 7 CONCLUSIONS AND FUTURE WORK ...........................................105
7.1 Conclusions .............................................................................................................105
7.2 Major advances .......................................................................................................108
7.3 Suggestions for future work ....................................................................................108
REFERENCES ...............................................................................................................110
APPENDICES ................................................................................................................124
Appendix A ....................................................................................................................124
A.1 MATLAB program files for a single-step nitrocarburizing treatment ...............124
A.2 MATLAB program files for a two-step nitrocarburizing treatment ...................126
VITA AUCTORIS .........................................................................................................130
xiii
LIST OF TABLES
Table 2.1: Characteristics of carburizing methods for AISI 8620 steel [19] ...................... 10
Table 2.2: Surface residual stress values of TC pistons after FNC and CN [28] ............... 16
Table 2.3: Residual stresses due to salt bath nitrocarburizing (NC) and carbonitriding (CN)
[31] ...................................................................................................................................... 18
Table 2.4: Change in OD, ID, GW and flatness distortions of nitrocarburized and
carbonitrided 1010 Navy C-rings [44] ................................................................................ 25
Table 2.5: Hardness and distortion values of Navy C-ring specimens made from HSS 6-5-
2 after vacuum heat treatment [45] ..................................................................................... 26
Table 2.6: Summary of the distortion modeling ................................................................. 36
Table 2.7: Summary of the composition profile modeling ................................................. 42
Table 2.8: Summary of the residual stress-depth profile modeling .................................... 46
Table 3.1: Elemental compositions of SAE 1010 plain carbon steel [44] .......................... 50
Table 3.2: Heat treatment and specimen details ................................................................. 52
Table 4.1: Material properties used in the FEM models ..................................................... 60
Table 4.2: Mesh sensitivity study in a C-ring (C3) model .................................................. 63
Table 4.3: Details about the C-ring elements...................................................................... 64
Table 4.4: Finite element simulation set up for C-ring models .......................................... 65
Table 4.5: Finite element simulation set up for TC pistons ................................................ 67
Table 5.1: Measured ID, OD and GW distortions for nitrocarburized C-rings .................. 69
Table 5.2: C-ring’s Gap Width (GW) distortion results – Top location ............................. 69
Table 5.3: C-ring’s Gap Width (GW) distortion results – Middle location....................... 70
xiv
Table 5.4: C-ring’s Gap Width (GW) distortion results – Bottom location ....................... 70
Table 5.5 Comparison of the measured Outer Diameter (OD) distortion with the predicted
OD distortion ...................................................................................................................... 72
Table 5.6: Comparison of the measured Inner Diameter (ID) distortion with the simulated
results .................................................................................................................................. 73
Table 5.7: V/VN ratio of Navy C-rings and TC pistons ...................................................... 75
Table 5.8: Experimental ID and OD distortions for nitrocarburized TC pistons................ 78
Table 5.9: Comparison of measured and predicted OD distortion of TC pistons............... 79
Table 5.10: Comparison of measured and predicted ID distortion of TC pistons .............. 79
Table 6.1: Composition of nitrogen in ε, γ′ and α phases [94, 95] ..................................... 83
Table 6.2: Partial molar volume, predicted phase thickness and distortion........................ 86
Table 6.3: CMM measured distortion values of SAE 1010 torque converter piston .......... 87
Table 6.4: Comparison of measured and predicted surface residual stresses of
nitrocarburized SAE 1010 torque converter pistons. .......................................................... 90
Table 6.5: Simulated two step heat treatment conditions and N compositions .................. 92
Table 6.6: Predicted local distortions for two-step nitrocarburizing treatments ............... 102
xv
LIST OF FIGURES
Figure 2.1: Ferritic nitrocarburized gear and other components [6]. .................................... 5
Figure 2.2: Optical micrographs (a-g) showing different types of compound layers on α-
iron substrate by nitrocarburizing at 580oC [9]..................................................................... 6
Figure 2.3: Phase diagram of Fe-N-C system at 570oC (logarithmic concentration scales)
[13]. ....................................................................................................................................... 7
Figure 2.4: AISI 1020 isopleth predicted using Thermo-Calc [14] ...................................... 8
Figure 2.5: Optical micrographs of nitrided (823 K (549oC) / 5 hrs, 60/40 vol.% NH3/H2)
iron specimen ((a) before annealing & (b) after annealing) [15]. ......................................... 9
Figure 2.6: Schematic diagrams of ion nitrocarburizing system [17, 18] (x is carbon-carrier
gas) . ...................................................................................................................................... 9
Figure 2.7: Schematic diagram of Korund-300 installation for fluidized bed
nitrocarburizing treatment [21]. .......................................................................................... 11
Figure 2.8: (a) & (b) Salt bath nitriding/nitrocarburizing furnaces [20]. ............................ 12
Figure 2.9: Compound layer thickness vs. treatment time for mild steel, QT steel and hot
worked steel (12%Cr-steel cast iron) [23]. ......................................................................... 12
Figure 2.10: Schematic diagram of bell-type gas nitriding furnace, (a) heating bell and (b)
cooling bell [20]. ................................................................................................................. 13
Figure 2.11: Schematic diagram of gas nitriding / nitrocarburizing furnace (pit-
type) [24]. ............................................................................................................................ 14
Figure 2.12: Schematic of a horizontal vacuum nitriding/nitrocarburizing furnace
[25]. ..................................................................................................................................... 14
xvi
Figure 2.13: Microhardness and residual stress depth profiles of H11 tool steel, plasma
nitrocarburized at 580oC/8 hrs (C1), 580oC/16 hrs (C2), 580oC/24 hrs (C3), and 580oC/32
hrs (C4) [29]........................................................................................................................ 16
Figure 2.14: Residual stress-depth profiles of ε-phase iron nitride layer [30]. ................... 17
Figure 2.15: Residual stress-depth profile of a low carbon steel specimen that was vacuum
annealed at 900oC/1hr+ nitrocarburized at 570oC/3hrs and artificial aged at 170oC/45min
((a) before fatigue, (b) after fatigue) [32]. .......................................................................... 18
Figure 2.16: Flatness change of SAE 1010 torque converter (TC) pistons, gas ferritic
nitrocarburized at 510oC/15hrs, 540oC/10hrs, 565oC/5hrs and 595oC/4hrs [28]. ............... 19
Figure 2.17: Distortion comparison of FNC vs. SR + FNC front rotor, adapted from [35].
............................................................................................................................................. 21
Figure 2.18: (a) Finished bearing ring, (b) Inner radius change and surface residual stresses
of the ring due to turning [36]. ............................................................................................ 21
Figure 2.19: (a) Navy C-ring dimensions as used by French [37], and (b) Navy C-ring
specimen used by Webster and Laird [38] (dimensions in inches). ................................... 23
Figure 2.20: Dimensions of Navy C-rings used by (a) Bates et al. [40], and (b) Leskovsek
and Ule [41]. ....................................................................................................................... 24
Figure 2.21: (a) Size and (b) shape distortion changes of carburized SAE Navy C-rings:
carburizing treatments: 1) 927oC/6h (carbon potential 0.9), 2) 927oC/6h (carbon potential
1.0), 3) 927oC/6h (carbon potential 1.1), 4) 954oC/4h (carbon potential 0.9), 5) 954oC/4h
(carbon potential 1.0), 6) 954oC/4h (carbon potential 1.1) and 7) 954oC/4h (carbon
potential 1.2) [48]................................................................................................................ 27
xvii
Figure 2.22: (a) Carbon composition profile and (b) residual stress distributions for a
carburized + water quenched long cylinder steel containing molybdenum [57]. ............... 28
Figure 2.23: (a) Temperature history (experimental and computed) at centre of tool steel
block during gas quenching, (b) Distortion of gas quenched (3 bar N2) ORVAR
SUPREME tool steel block (experimental and computed). The distortion is magnified 50
times [58]. ........................................................................................................................... 29
Figure 2.24 : (a) Dimensional changes of a C-ring specimen before heat treatment (m and
n dimensions) and after heat treatment (m’ and n’ dimensions), (b) distortion simulation
(displacement magnification 20X) [60]. ............................................................................. 30
Figure 2.25: Computed Gap Width (GW) vs. time curve [61]. .......................................... 31
Figure 2.26: (a) Finite element model of one half of the C-ring, (b) Gap width (opening
displacement) distortion of AISI 8620 carburized C-ring [62]. .......................................... 31
Figure 2.27: Distortion engineering procedure by Zoch [34]. ............................................ 32
Figure 2.28: (a) 100 mm long C-ring, (b) comparison of experiment and simulation
distortion results, (c) banana effect, and (d) barrel or bobbin effect [63]. .......................... 33
Figure 2.29: Comparison of measured and predicted distortion (DANTE model) showing
the "bowing" of AMS 6308 coupon [64]. ........................................................................... 33
Figure 2.30: Radial displacement contour and distortion comparison of bore and tip
distortion of AISI 4320H gear component [65]. ................................................................. 34
Figure 2.31: (a) – Geometry of a simplified large gear, (b) – Distortion comparison at
seven points [66]. ................................................................................................................ 35
xviii
Figure 2.32: (a) Carbon steel ring specimen geometry (dimensions in mm), (b) Measured
and predicted distortion results at location 1 (outer diameter) and 2 (inner diameter) [67].
............................................................................................................................................. 35
Figure 2.33: Nitrogen and carbon concentration profiles measured using EPMA on
nitrocarburized Fe-0.8C (wt. %) and Fe alloys [68]. .......................................................... 37
Figure 2.34: Special ferritic nitrocarburizing (FNC) process for increased N2 and C
contents [69]........................................................................................................................ 37
Figure 2.35: Nitrogen concentration profile for nitrided 4140 steel (measured vs.
computed) [70]. ................................................................................................................... 38
Figure 2.36: Predicted nitrogen composition-depth profiles for pulse plasma nitride pure
iron. The experimental data (∆ symbol) were acquired from Yan et al. [72], (a) T=773K
(500oC) & (b) T= 793K (520oC) (1 represents ε phase, 2 is γ′ and 3 represents α phase)
[71]. ..................................................................................................................................... 38
Figure 2.37: Predicted and experimental nitrogen, carbon composition profiles of plasma
nitrocarburized austenitic stainless steel [73]. .................................................................... 39
Figure 2.38: Simulated and experimental nitrogen depth profiles of plasma nitrided AISI
316L (400oC/2hrs) with different N diffusion coefficients [76]. ........................................ 40
Figure 2.39: (a) schematic of housing, (b) plate-like component ....................................... 41
Figure 2.40: Nitrogen composition-depth profiles (measured and calculated) [77]. .......... 41
Figure 2.41: Predicted bore deformation for housing (case 1) and plate-like (case 2)
components due to 2 different FNC treatments [77]. ......................................................... 42
Figure 2.42: Predicted and measured axial residual stress of a carburized AMS 6308 steel
coupon [64]. ........................................................................................................................ 43
xix
Figure 2.43: (a) – Predicted hoop residual stress map (MPa), (b) - Residual stress-depth
profiles for a gas nitrided (550oC/120 hrs) tubular sample [78]. ........................................ 44
Figure 2.44: Residual stress-depth profiles at the center of the Almen strip, (a) 2.44 mm
thick and (b) 3.18 mm thick [79]. ....................................................................................... 44
Figure 2.45: Residual stress-depth profiles for the nitrided Fe-Al specimen (experimental
and predicted) [81]. ............................................................................................................. 45
Figure 3.1: Overview of the research plan. ......................................................................... 47
Figure 3.2: (a) Torque converter (TC), and (b) TC cross section [82]. .............................. 48
Figure 3.3: (a, b) Navy C-ring specimen geometry, (c) schematic for Navy C-rings C1, C2
and C3 (dimensions in mm). ............................................................................................... 49
Figure 3.4: Geometry of torque converter (TC) piston. ...................................................... 51
Figure 3.5: Schematic process diagram of the ferritic nitrocarburizing treatment. ............ 51
Figure 3.6: A light optical microscope (Leitz Laborlux 12 ME). ....................................... 53
Figure 3.7: (a) Hysitron (Ubi1) nanomechanical instrument, (b) loading-unloading
response for a SAE 1010 C-ring after FNC. ....................................................................... 54
Figure 3.8: PRISMO coordinate measuring machine (CMM) [83]. ................................... 55
Figure 3.9: Schematic of nitrogen composition-depth profile due to 1-step nitrocarburizing
treatment. ............................................................................................................................ 56
Figure 3.10: Schematic of the simulated nitrogen composition-depth profile due to 2-step
nitrocarburizing treatment. .................................................................................................. 57
Figure 3.11: Cameca SX50 Electron Probe Micro Analyzer (EPMA) at Earth Sciences,
University of Toronto [84]. ................................................................................................. 58
Figure 4.1: Navy C-ring geometry dimensions................................................................... 61
xx
Figure 4.2: Compound layer comparison of the Navy C-ring probe model and the optical
micrograph showing the compound layer of SAE 1010 steel............................................. 62
Figure 4.3: Half symmetric geometry of meshed Navy C-rings with varying thicknesses
19mm (C1), 10mm (C2), 3mm (C3). .................................................................................. 64
Figure 4.4: (a) Cross section of the torque Converter (TC) piston, (b) axisymmetric TC
piston model. ....................................................................................................................... 66
Figure 5.1: C-ring’s GW distortion measurement locations ............................................... 68
Figure 5.2: Measured and predicted gap width (GW) distortion profiles of Navy C-rings
((a) top, (b) middle & (c) bottom locations). ...................................................................... 71
Figure 5.3: Outer Diameter (OD) distortion profile of Navy C-rings (measured and
predicted). ........................................................................................................................... 73
Figure 5.4: Inner diameter (ID) distortion profile of Navy C-rings (measured and
predicted). ........................................................................................................................... 74
Figure 5.5: V/VN ratio vs. absolute errors for GW & ID distortions of Navy C-rings. ...... 76
Figure 5.6: V/VN ratio vs. absolute errors for OD distortions of Navy C-rings. ................ 76
Figure 6.1: Experimental nitrogen profiles for vacuum nitrocarburized (580oC/10hrs) and
gas nitrocarburized (580oC/10hrs) TC piston samples. ...................................................... 80
Figure 6.2: Simulated nitrogen composition-depth profiles ............................................... 82
Figure 6.3: (a), (b) and (c) Optical micrographs of SAE 1010 TC piston specimen
subjected to vacuum ferritic nitrocarburizing at 580oC/10hrs. ........................................... 84
subjected to gas ferritic nitrocarburizing at 565oC/5hrs. .................................................... 84
xxi
Figure 6.5: Carbon composition depth profile of SAE 1010 steel TC pistons measured
using EPMA. ....................................................................................................................... 85
Figure 6.6: Comparison of experimental and simulated nitrogen-profiling results of SAE
1010 nitrocarburized TC pistons ((a) – at the surface, (b) overall). ................................... 86
Figure 6.7: Predicted residual stress-depth profiles for FNC heat treatments (580oC/10hrs
and 565oC/5hrs). ................................................................................................................. 89
Figure 6.8: Simulated nitrogen composition-depth profile due to 2-step nitrocarburizing
process ‘A’ (595oC / 3.6 hrs / 8% + 427oC / 1.4 hrs / 3%). ................................................ 94
Figure 6.9: Predicted nitrogen composition-depth profile due to two-step nitrocarburizing
process ‘B’ (580oC/3.6 hrs/8% + 427oC/1.4 hrs/3%). ........................................................ 94
Figure 6.10: Predicted nitrogen composition-depth profile due to two-step
nitrocarburizing process ‘C’ (565oC / 3.6 hrs / 8% + 427oC / 1.4 hrs / 3%). ...................... 95
Figure 6.11: Predicted N composition-depth profiles for heat treatment ‘A’ and ‘D’
(595oC/3.6hrs/8wt.%+477oC/1.4hrs/3wt.%). ...................................................................... 95
Figure 6.12: Predicted N composition-depth profile for heat treatment ‘B’ and ‘E’
(580oC/3.6hrs/8wt.%+477oC/1.4hrs/3wt.%). ...................................................................... 96
Figure 6.13: Predicted N composition-depth profile for heat treatment ‘C’ and ‘F’
(565oC/3.6hrs/8wt.%+477oC/1.4hrs/3wt.%). ...................................................................... 96
Figure 6.14: Predicted N composition-depth profiles for heat treatment ‘G’
(595oC/3.6hrs/7wt.%+427oC/1.4hrs/3wt.%) and heat treatment ‘H’
(580oC/3.6hrs/7wt.%+427oC/1.4hrs/3wt.%). ...................................................................... 97
Figure 6.15: Predicted N composition-depth profile for heat treatment ‘I’
(565oC/3.6hrs/7wt.%+427oC/1.4hrs/3wt.%). ...................................................................... 98
xxii
Figure 6.16: Predicted N composition-depth profile for heat treatment ‘J’
(595oC/10hrs/8wt.%+427oC/2.7hrs/3wt.%). ....................................................................... 99
Figure 6.17: Simulated nitrogen composition-depth profile due to two-step
nitrocarburizing process (580oC/10hrs/8% + 427oC/2.7hrs/3%). ....................................... 99
nitrocarburizing process (565oC/10hrs/8% + 427oC/2.7hrs/3%). ..................................... 100
Figure 6.19: Residual stress distribution due to 2-step nitrocarburizing process. ............ 104
xxiii
LIST OF APPENDICES
Appendix A: MATLAB program files for 1-step & 2-step nitrocarburizing
treatment……………………………..…………………………………………...……...124
xxiv
LIST OF ABBREVIATIONS/SYMBOLS
OD Outer Diameter
ID Inner Diameter
GW Gap Width
LRO Lateral Run Out
TC Torque Converter
FNC Ferritic Nitrocarburizing
CL Compound Layer
CN Carbo-Nitriding
EPMA Electron Probe Micro Analyzer
CMM Coordinate Measuring Machine
GDOES Glow Discharge Optical Emission Spectroscopy
FEM Finite Element Method
FDM Finite Difference Method
XRD X-Ray Diffraction
xxv
NOMENCLATURE
E Young’s modulus
σ stress
ν Poisson’s ratio
ρ density
c elemental composition
D diffusion coefficient
t diffusion time
h heat transfer coefficient
T temperature
Vε partial molar volume of ε phase
Vγ’ partial molar volume of γ′ phase
lε thickness of ε phase
lγ’ thickness of γ′ phase
Δlε local distortion due to ε phase
Δlγ’ local distortion due to γ′ phase in the compound layer
Δlγ’in diff. zone local distortion due to γ′ phase in the diffusion zone
̂ Cauchy stress tensor
G shear modulus
K compressibility
εε strains due to ε phase
εγ’ strains due to γ′ phase
xxvi
M molar fraction
σε residual stress due to ε phase
σγ’ residual stress due to γ′ phase
xxvii
CHAPTER 1 INTRODUCTION
Surface engineering is used to improve properties like corrosion or wear
resistance that are not present in the bulk material. It also improves the quality,
performance and life-cycle cost of the products, which are widely used in industries like
automotive, aerospace, electronics and construction. The common surface engineering
treatments are mechanical, thermo-mechanical, thermal, thermo-chemical,
electrochemical & chemical, and physical techniques [1]. Heat treatments involving
carburizing, nitriding, carbonitriding, and nitrocarburizing are a class of thermo-chemical
surface engineering methods. The carburizing process produces a thick high-carbon
martensitic case by adding carbon in the steel surface at elevated temperatures (800-
1090oC) in the austenitic phase field. The main differences between carburizing and
carbonitriding are the ammonia addition and the lower temperature range (705-900oC) in
the carbonitriding process. The nitriding and nitrocarburizing processes, on the other
hand, produce a thin compound layer at relatively lower temperatures (495-650oC) in the
ferritic phase field.
Ferritic nitrocarburizing is a case hardening process in which gases, like
methane/propane, ammonia and nitrogen, react with the metallic surface at 500-650oC.
Ferritic nitrocarburizing offers excellent scuffing, wear and fatigue resistance by
producing a thin compound layer (containing ε-Fe2-3(C, N), γ′-Fe4 (N, C), cementite
(Fe3C) and various alloy carbides and nitrides) on the material surface. The thickness of
the compound layer is usually in the range of 5 to 30 µm. Ferritic nitrocarburizing is
widely used to case harden torque converter pistons, brake rotors, gears, pinion shafts and
1
other wear components. The highlights of nitrocarburizing are smaller distortion than
carbonitriding and no phase transformation in the bulk material [2]. However, this
smaller distortion, if left untreated, could lead to performance issues in the automotive
component. Machining or straightening the surface can eliminate the distortion but
requires additional work hours and cost. Moreover, machining will reduce the thickness
of nitrocarburized layer thereby reducing service performance of the component.
Residual stresses, which are developed during the manufacturing process
conditions, often lead to distortion. Although residual stress results in dimensional
changes of a material, it can provide resistance to crack initiation [3]. Any heat treatment
process is a major source for distortion [4].
Navy C-rings are generally used as a test specimen to observe the dimensional
distortion before analyzing an actual component (torque converter piston) for distortion.
To better understand the distortion mechanisms, SAE 1010 Navy C-rings with three
different thicknesses (2.8, 10, 19 mm) were used. These 3 different thicknesses were
chosen to report the distortion due to change in geometry of C-rings. Torque converter
(TC) piston is an automotive component that is used to measure and calculate distortion
for the application of the process in practice.
The numerical simulation of heat treatment conditions were started initially in the
mid-1970s [5]. The heat treatment simulations were mainly developed to predict the
residual stresses and distortion. In this study, numerical techniques including finite
element method (FEM) and finite difference method (FDM) are used to understand the
2
distortion mechanisms in Navy C-ring probe and Torque Converter (TC) piston
specimens.
1.1 Research Objectives and Approach
The main focus of this research is to methodically examine the distortion in
nitrocarburized SAE 1010 Navy C-ring and torque converter piston specimens. Finite
element models of Navy C-rings and torque converter pistons were developed to predict
the distortion trend. The predicted distortion results were compared with the experimental
distortion.
An electron probe micro analyzer (EPMA) was used to measure the composition-
depth profiles of nitrocarburized torque converter piston specimens. Using the
composition profiles, a numerical model was developed using finite difference method to
predict the compound layer thickness and distortion due to nitrocarburizing treatment.
The predicted composition-depth profiles were compared with the experimental profiles.
Also, the surface residual stress was predicted and compared against the experimental
surface residual stress.
Based on the distortion analyses and residual stress distribution after
nitrocarburizing treatments, a two-step nitrocarburizing technique is suggested, which
should produce smaller distortion than single stage nitrocarburizing, while improving the
surface characteristics in the automotive component.
1.2 Dissertation Outline
Chapter 2 presents a literature review of ferritic nitrocarburizing process, residual
stresses, distortion, and modeling of distortion and residual stress.
3
Chapter 3 shows the analytical approach taken to solve the distortion problem.
Experimental and numerical investigations are discussed in detail about the distortion
calculation, N profiles and residual stresses.
Chapter 4 presents the finite element simulations of Navy C-rings and torque
converter (TC) pistons.
Chapter 5 shows the validation of the finite element simulations of Navy C-rings
and TC pistons.
Chapter 6 discusses the composition-depth profile simulation models, which are
used to predict the distortion due to the nitrocarburized phases.
Chapter 7 highlights the summary and conclusions arising from this study and
provides suggestions for future work.
4
CHAPTER 2 LITERATURE REVIEW
The objective of the literature survey is to understand the ferritic nitrocarburizing
process, distortion mechanisms, distortion prediction methods, composition-depth
profiling and residual stress modeling.
2.1 Ferritic Nitrocarburizing (FNC)
Ferritic nitrocarburizing (FNC) was first introduced in 1947 in a cyanide, salt-
based batch process. The FNC process was later refined as a gaseous ferritic
nitrocarburizing process by Lucas Industries in 1961 [6]. Many engineering components
like rocker-arm spacers, textile machinery gears, pump cylinder blocks, jet nozzles,
crank-shafts and drive shafts are case-hardened using nitrocarburizing treatments [7].
Gear steels made of SAE 4140, 5160, 8620 and certain tool steels are also surface
engineered using the ferritic nitrocarburizing (FNC) process [8]. There are different
types of ferritic nitrocarburizing processes in the automotive industry: gas, ion or plasma,
fluidized bed, vacuum and salt bath. Figure 2.1 shows the automotive components that
have been ferritic nitrocarburized.
Figure 2.1: Ferritic nitrocarburized gear and other components [6].
5
The nitrocarburizing process is carried out in the ferritic region of the Fe-C phase
diagram. After nitrocarburizing, the surface of the part exhibits two distinct regions,
namely a compound layer and diffusion zone. These two regions are the main reason for
providing high resistance to wear and corrosion in nitrocarburized materials. The
compound layer can be a single-phase layer containing ε - Fe2-3(N, C) or a dual-phase
layer containing both ε and γ′. Leineweber et al. [9] reported the types of the compound
layer microstructures that can be formed on the α-iron substrate upon nitrocarburizing
(see Fig. 2.2):
(1) γ′ layers,
(2) ε/γ′ layers,
(3) ε/ε+γ′ layers,
(4) ε layers + cementite, and
(5) cementite (θ) layers
Figure 2.2: Optical micrographs (a-g) showing different types of compound layers
on α-iron substrate by nitrocarburizing at 580oC [9].
6
The phase transformation sequence in the nitrocarburizing surface of carbon steels
was found contradictory. Bell et al. [10] reported the nitrocarburized phase
transformation of carbon steels in the following form:   N  C     '. Mittemeijer
[11] presented the phase sequence of the compound layer due to gas nitrocarburizing as:
  N  C       ' . They both reported ε-phase formation before γ’. However,
Chen et al. [12] reported γ’ to ε phase transformation. They demonstrated the formation
mechanism of nitrocarburized phases as follows:   N  C    N  C   ' N  C   .
Microstructural examination in the transition layer (between the compound layer and the
diffusion zone) suggested that an intermediate phase state γ (austenite) was first produced
before the pearlite colonies, and the γ phase was transformed into γ’ during the ferritic
nitrocarburizing process.
Figure 2.3 shows the Fe-N-C phase diagram, where α gets transformed to α+ γ’
(point b, assuming negligible C wt. %). With the increase in N wt. %, ε phase will occur
from the α+ γ’ region (producing γ’ to ε phase transformation).
Figure 2.3: Phase diagram of Fe-N-C system at 570oC (logarithmic concentration
scales) [13].
7
Yang and Sisson Jr. [14] simulated the phase evolution of carbon steels to predict
the first forming phase. The first nitride phase was reported to be ε-phase during the
nitriding process. They have concluded that a single γ′-phase is not possible in carbon
steels: see isopleth in Figure 2.4 which shows no single γ′ phase region at typical
nitriding/nitrocarburizing temperatures.
Figure 2.4: AISI 1020 isopleth predicted using Thermo-Calc [14]
An interesting regrowth of γ′ sublayer was reported by Liapina et al. [15]. In their
study, an iron cast rod specimen was subjected to gas nitriding at 823 K (550oC) for 5hrs
followed by water quenching. The specimen was then annealed at 630 K (356oC) for 120
hrs and cold water quenched. Figure 2.5 shows the increase in γ′ sublayer at the cost of ε
phase due to the annealing process. Therefore, an individual γ′-phase is possible for iron
specimen.
8
Figure 2.5: Optical micrographs of nitrided (823 K (549oC) / 5 hrs, 60/40 vol.%
NH3/H2) iron specimen ((a) before annealing & (b) after annealing) [15].
The compound layer thickness depends on the type of ferritic nitrocarburizing
(FNC) process. The maximum thickness of the compound layer due to FNC was
observed to be approximately 40µm [16]. The different types of nitrocarburizing
processes are briefly discussed in sections 2.1.1 to 2.1.5.
2.1.1 Ion or plasma nitrocarburizing
Ion or plasma nitrocarburizing is a low pressure thermochemical treatment in
which nitrogen, hydrogen and carbon producing gases were utilized to produce a
compound layer (ε) and diffusion zone on the steel surface. A glow discharge with a high
ionization level is generated around the parts. The schematic of ion nitrocarburizing
systems are shown in Figure 2.6.
Figure 2.6: Schematic diagrams of ion nitrocarburizing system [17, 18] (x is
carbon-carrier gas) .
9
Cherian [19] has reported a microwave atmospheric plasma technology called
AtmoPlasTM to carburize the steel parts. The technology reduced the heating cycle times
and energy by reaching high temperature in seconds. By using microwave carburizing
technology, surface carbon concentration, case depth uniformity, and retained austenite
were found to be better than the conventional processes (see Table 2.1).
Table 2.1: Characteristics of carburizing methods for AISI 8620 steel [19]
Characteristic/ Conventional gas Vacuum AtmoPlas carburized

property carburized carburized
Total 142min boost + Carburizing zone 112min boost + 80min
carburizing 110min diffuse + time =205 min diffuse + 20min
time 20min temp.drop = temp.drop = 212min
272min
Case depth ~0.035 in. (~0.9mm) ~0.035 in. ~0.045 in. (~1.14mm)
(~0.9mm)
Depth of retained austenite (%)
Corner ~15-30% to ~15-30% to ~5-20% to ~0.0067in
microstructure ~0.0125in ~0.0067 in (~0.172mm)
(~0.319mm) (~0.319mm)
Surface ~10-20% to ~5-15% to ~5-20% to ~0.0058in
microstructure ~0.0046in ~0.0095 in (~0.148mm)
(~0.119mm) (~0.243mm)
2.1.2 Fluidized bed nitrocarburizing
In fluidized bed nitrocarburizing treatment, ammonia, compressed air and
methane are blown to fluidize the catalyst (Al-Ni-Mg or aluminum oxide). The finely
divided aluminum oxide will then transfer the heat from the heating medium to the
workpiece. The heating medium can be electric or gas [20]. Figure 2.7 shows the
schematic diagram of Korund-300 fluidized bed furnace.
10
Figure 2.7: Schematic diagram of Korund-300 installation for fluidized bed
nitrocarburizing treatment [21].
[1) body of the shaft furnace, 2) retort, 3) header 4) container, 5) catalyst, 6) heater, 7) heat insulation, 8) thermocouple,
9) current feedthrough, 10) cover, 11, 12) body and chamber of the device for gas cleaning, 13) catalyst, 14) heater, 15)
heat insulation, 16) thermocouple, 17) gas inlet, 18) current feedthrough, 19) plug cock, 20) body of gas distribution
panel, 21) air rotameter, 22) ammonia rotameter, 23) natural gas rotameter, 24) mixer, 25) pipe for feeding gas-air
mixture to retort, 26) flange coupling, 27) pressure regulator in the natural gas feed line, 28) ammonia manifold, 29)
ammonia cylinders, 30) pressure regulator in the ammonia feed line, 31, 32) millivoltmeter, 33) power supply cabinet,
34) body of quenching tank, 35) quenching tank, 36) safety grate, 37) oil, 38) water jacket, 39) water feed, 40) header,
41) water discharge, 42) flume for sucking off oil vapors, 43) air duct, 44) washing tank, 45) steam inlet, 46) cold water
feed, 47) oil arresting compartment, 48) compressed air feed, 49) oil discharge, 50) water discharge, 51) oil vapor
arrester, 52) funnel, 53) hinged funnel, 54) combined extract and input ventilation, 55) monorail, 56) monorail hoist,
57) choke, 58), valve] [21].
2.1.3 Salt bath nitrocarburizing
In salt bath nitrocarburizing treatment, the automotive part is immersed in a
molten salt (NaCN, Na2CO3) containing nitrogen and carbon. The nitrogen and carbon
from the salt will then react with the part’s surface forming a compound layer and
diffusion zone. The externally heated salt bath furnaces are shown in Figure 2.8. Recent
development in the salt bath nitriding/nitrocarburizing treatment resulted in using a
regenerable non-cyanide salt bath that produces no waste salt [22].
11
(a) (b)
Figure 2.8: (a) & (b) Salt bath nitriding/nitrocarburizing furnaces [20].
TUFFTRIDE® is a salt bath nitrocarburizing process that takes place in a TF1
bath (containing alkali cyanate and alkali carbonate) at 480-630oC [23]. Figure 2.9 shows
the compound layer thickness after TUFFTRIDE® treatment (580oC/1-2hrs) for mild
steel, QT steel and hot worked steel (12%Cr-steel cast iron). It was found that the
thickness of the compound layer changes with the treatment time and material type. Mild
steel produced thicker compound layer than QT steel and 12%Cr-steel cast iron.
Figure 2.9: Compound layer thickness vs. treatment time for mild steel, QT steel
and hot worked steel (12%Cr-steel cast iron) [23].
12
2.1.4 Gas nitrocarburizing
Gas nitrocarburizing employs ammonia and hydrocarbon or carbon bearing gases
(like CO2, CO) into the steel surface to produce a compound layer and diffusion zone.
The ammonia and CO2 + CO gases dissociate according to the Equations 2.1 to 2.6 [24].
The atomic nitrogen and carbon are needed for the diffusion to take place at the steel
surface.
Gas nitriding/nitrocarburizing process can be carried out using bell-type and pit-
type furnaces, which are schematically shown in Figure 2.10 and 2.11. Using a bell-type
furnace, a uniform compound layer can be attained at the steel surface due to the
temperature uniformity caused by the internal fan.
2NH 3  2N  3H 2 (nitriding reaction) (2.1)
H 2 +CO 2  CO+H 2 O (2.2)
NH 3  CO  HCN  H 2 O (2.3)
2CO  CO 2 +C (carburizing reaction) (2.4)
2NH 3  CO 2  H 2O  (NH 4 ) 2 HCO3 (2.5)
NH 3 +CO 2 +H 2 O  NH 4 HCO3 (2.6)
(a) (b)
Figure 2.10: Schematic diagram of bell-type gas nitriding furnace, (a) heating bell
and (b) cooling bell [20].
13
Figure 2.11: Schematic diagram of gas nitriding / nitrocarburizing furnace
(pit-type) [24].
2.1.5 Vacuum nitrocarburizing
In vacuum nitrocarburizing treatment, the air is completely evacuated from the
furnace. Then the ammonia and carbon producing gases are passed into the hot chamber
to case harden the workload. Figure 2.12 shows the schematic diagram of a single-
chamber, front loading vacuum furnace. The cooling gas inlet and outlet will be used to
furnace cool the workload after nitrocarburizing.
Figure 2.12: Schematic of a horizontal vacuum nitriding/nitrocarburizing
furnace [25].
14
2.2 Residual stress
Residual stress prediction should be part of any heat treatment modeling because
residual stress affects the distortion, fatigue performance and corrosion resistance of a
component. A large amount of residual stress may cause the component to fail
prematurely. Ericsson [26] stated that the evolution of large residual stresses due to
thermal and thermochemical heat treatments was caused by the following reasons:
a) thermal stresses due to thermal expansion or contraction of a homogeneous
material in a temperature gradient field,
b) different thermal expansion coefficients of the various phases in a multiphase
material
c) density changes due to phase transformations in the metal
d) growth stresses of reaction products formed on the surface or as precipitates,
e) chemical composition gradients below the surface
In thermochemical heat treatments like nitriding and nitrocarburizing, residual
stresses are also the result of cohesion of the misfitting compound layer to the ferritic
substrate and cohesion within the compound layer [27]. Compressive residual stress
obtained in the surface of an automotive component is considered beneficial, since it can
prevent crack propagation and improve fatigue endurance. However, tensile residual
stresses exist in the ε-nitride surface layer due to nitrocarburization. Nan et al. [28]
reported tensile residual stresses for SAE 1010 torque converter (TC) pistons after ferritic
nitrocarburizing (FNC) process but compressive stresses for a carbonitriding (CN)
process (see Table 2.2). The tensile stress values for the ε-phase compound layer varied
from 76.5 to 268.2 MPa for all processing scenarios studied.
15
Table 2.2: Surface residual stress values of TC pistons after FNC and CN [28]
Heat treatment Surface residual stress (MPa)

Gas FNC + Nitrogen cooling (510oC / 15 hrs) 122.0 ± 10.3
o
Gas FNC + Nitrogen cooling (595 C / 4 hrs) 76.5 ± 22.8
Ion FNC (560oC / 15 hrs) 186.2 ± 21.4
Ion FNC (525oC / 24 hrs) 224.1 ± 18.6
Gas FNC (N potential) + Nitrogen cooling (525oC / 52 hrs) 172.4 ± 9.7
Gas FNC (N potential) + Nitrogen cooling (570oC / 4 hrs) 241.3 ± 23.4
Vacuum FNC (580oC / 10 hrs) 262.7 ± 20.0
Gas FNC + quenching (580oC / 2 hrs + water quench) 252.3 ± 19.3
Gas carbonitriding (850oC / 4 hrs + 100oC oil quench) -188.9 ± 26.2
Leskovsek et al. [29] reported the microhardness and residual stress distribution
of plasma nitrocarburized H11 steel (see Fig. 2.13). The surface hardness increases with
longer plasma nitrocarburizing time while the surface residual stress (tensile) decreases
with increase in heat treatment time. Higher tensile residual stresses are not considered to
be good enough to protect the steel from wear and fatigue.
Figure 2.13: Microhardness and residual stress depth profiles of H11 tool steel,
plasma nitrocarburized at 580oC/8 hrs (C1), 580oC/16 hrs (C2), 580oC/24 hrs (C3),
and 580oC/32 hrs (C4) [29].
16
The residual stresses in the ε-phase iron nitride (within 2µm depth) have been
measured using ψ-tilt and grazing incidence x-ray diffraction methods [30]. The ε-phase
was produced on the part’s surface using a two-stage gas nitriding treatment. Figure 2.14
shows tensile residual stress at the ε-phase varied in the range of 200-1200MPa. The
residual stress values measured using the X-ray penetration is plotted as Tau profile
(open circles) and the predicted residual stress is plotted as Z-profile (solid line). The
dotted line represents the reconstructed tau profile calculated from the Z-profile.
Figure 2.14: Residual stress-depth profiles of ε-phase iron nitride layer [30].
In contrast to the tensile stresses of ε-phase iron nitride mentioned above,
compressive residual stresses were observed in the ε-phase of salt bath nitrocarburized
AISI O2 tool steel (see Table 2.3). Before salt bath nitrocarburizing, the samples were
annealed at 760oC for 1hr and tempered at 600oC for 1hr [31]. The surface residual
stresses of ε-Fe3N changed from -251±51 MPa to -276±30 MPa. Thomas and Bell [32]
have also reported compressive residual stress on the compound layer of annealed + gas
nitrocarburized low carbon steel specimen. Figure 2.15 (a) & (b) presents the
compressive surface residual stress profiles measured before and after fatigue testing. An
17
almost complete fading of the residual stress occurred on the early stages of fatigue (see
Fig. 2.15(b)).
Table 2.3: Residual stresses due to salt bath nitrocarburizing (NC) and
carbonitriding (CN) [31]
Heat treatment Nitride layers NC (MPa) CN (MPa)

Fe3N (113) Feα (211) Fe4N (200) γ (311)
o
NC (570 C/1hr) very thin - -239±38 - -
NC (570oC/3hrs) Fe3N>Fe4N<Feα -251±51 -259±67 -266±60 -
NC (570oC/4hrs) Fe3N=Fe4N>Feα -252±51 -411±82 -254±83 -
NC 570oC/5hrs Fe3N>Fe4N<Feα -268±55 -353±97 -281±75 -
NC 570oC/6hrs Fe3N>Feα -276±30 -340±35 - -
CN No - -122±38 - -52±15
(870oC/1hr+oil
quench to
180oC)
(a) (b)
Figure 2.15: Residual stress-depth profile of a low carbon steel specimen that was
vacuum annealed at 900oC/1hr+ nitrocarburized at 570oC/3hrs and artificial aged at
170oC/45min ((a) before fatigue, (b) after fatigue) [32].
18
Therefore, the surface stress for ε-phase in nitrocarburized tool steel (AISI O2)
can be compressive but the ε-phase for nitrocarburized carbon steels (SAE 1010) are
tensile in nature.
2.3 Distortion
Distortion can be defined as an inconsistent size or shape change of a material
caused by the manufacturing process conditions. Two types of distortions are produced
by the surface engineering treatments. They are size distortion and shape distortion. Size
distortion is caused by the change in volume between the base material and the surface
layer. Diameter changes and gap width changes are reported as size distortion. Materials
that undergo twisting, bending and curving without any change in volume produce shape
distortion. The changes in roundness, flatness and cylindricity are termed as shape
distortion. Figure 2.16 shows the change in flatness (shape distortion) of nitrocarburized
torque converter pistons. The mean of flatness change values ranged from 15.64% to
25.11%.
Figure 2.16: Flatness change of SAE 1010 torque converter (TC) pistons, gas ferritic
nitrocarburized at 510oC/15hrs, 540oC/10hrs, 565oC/5hrs and 595oC/4hrs [28].
19
In the automotive and other industries, distortion can occur due to various reasons.
Zoch [33] points out that minimizing distortion is not only a quality concern but is also an
economic concern since between 20 and 40% of the production cost for components such
as bearing races are due to machining costs to eliminate distortion. The carriers of
“distortion potential” include [34]:
a) Geometry
b) Chemical composition / segregation
c) Microstructure/ grain size
d) Residual stress
e) Temperature
f) Mechanical history
The geometry and chemical composition are the two factors that are related to
distortion even before subjecting the component to heat treatment. The microstructural
changes, residual stresses and temperature resulting from the heat treatment will also
produce distortion.
Holly et al. [35] from General Motors Company found that the stress relieved (SR)
FNC rotors showed lower distortion (lateral run out (LRO)) than as-machined FNC
rotors. The stress relief was performed at 607±15oC for 3hrs followed by furnace cooling
prior to FNC treatment. The FNC cast iron brake rotor exhibited better wear and
corrosion protection than the standard non FNC brake rotor after extended parking. By
providing excellent scaling resistance and static corrosion performance, FNC rotors can
also help to decrease the brake pulsation [35]. Figure 2.17 compares the distortion (LRO)
of FNC and stress relieved FNC front rotors.
20
0.08
0.07
0.06
LRO, mm
0.05
0.04
0.03
0.02
0.01 AVE
0 AVE+3σ
Sample
Figure 2.17: Distortion comparison of FNC vs. SR + FNC front rotor, adapted from
[35].
Although distortion is significantly influenced by heat treatment, machining
before heat treatment can give rise to distortion as well. Brinksmeier et al. [36] reported
the dimensional deviations of SAE 52100 steel bearing rings (see Fig. 2.18(a)) due to a
turning (soft machining) process. After machining, polygonal type deviations occurred
due to the elastic deformation caused by fixing the workpiece in the chuck. The inner
radius change was attributed to the locally varying residual stresses that enlarged the
bearing ring (Fig. 2.18(b)).
(a) (b)
Figure 2.18: (a) Finished bearing ring, (b) Inner radius change and surface residual
stresses of the ring due to turning [36].
21
2.3.1 Distortion prevention methods
Distortion is difficult to eliminate, but can be prevented by taking necessary steps
before and during heat treatment. The following methods were used to obviate distortion
in heat treated parts [3]:
(a) Straightening - It helps to relieve the residual stresses in plain carbon and
low-alloy steels. The major disadvantage of straightening is the loss of
fatigue properties and crack initiation.
(b) Support and restraint fixtures - Restraint fixtures are used during rapid
cooling operation to control the dimensional changes of the parts. Support
fixtures are used for parts that deliver sufficient self-restraint.
(c) Quenching fixtures - Quenching fixture helps to prevent distortion during
water or oil quenching. However, it requires accurate positioning,
unobstructed quenchant flow, and an arrangement for draining the hot
quenchant.
(d) Pressure quenching - Using high pressure (5 MPa) and a turbulent gas flow,
the heat treated parts are uniformly cooled to produce lower distortion.
(e) Press quenching - It is applied to a specific geometry like flat circular
diaphragms of spring steel where direct quenching is difficult.
(f) Rolling die quenching - In rolling die quench machine, the heat treated
parts are placed on the rollers and the rolls turn to minimize distortion.
(g) Stress relieving - To reduce distortion, residual stresses are released by
subcritical annealing or normalizing treatment prior to the final machining
22
operation. Plain carbon and low-alloy steels are stress relieved at
temperatures of 550-650oC.
2.4 Types and use of Navy C-rings
The Navy C-ring is the common type of specimen used for observing dimensional
changes due to heat treatment. Before analyzing an automotive component for distortion,
Navy C-ring specimens machined from the material of interest are heat treated to observe
any distortion. It is generally presumed that the dimensional change of a Navy C-ring
specimen is comparable with the change in dimensions of the actual component.
Navy C-rings have been widely used in different dimensions according to their
application. In the late 1920s, French [37] started using C-shaped gauges to study
distortion and cracking, primarily in quenched steels. He reported that the thin and heavy
sections of C-ring specimens, Figure 2.19(a), prevent uniform cooling thereby offering a
means to promote distortion. Another type of Navy C-ring that was used to check the size
and shape change distortion was the ‘modified Navy C-ring’. The dimensions of the
modified Navy C-ring test specimens are shown in Fig. 2.20. It is evident that the outer
diameter (OD) of the Bates C-ring (refer to Fig.2.20(a)) was reduced by half compared to
the OD dimension reported by Webster and Laird [38] (see Fig.2.19(b)).
(a) (b)
Figure 2.19: (a) Navy C-ring dimensions as used by French [37], and (b) Navy C-
ring specimen used by Webster and Laird [38] (dimensions in inches).
23
Leskovsek et al. [39] found that the hardness values of modified Navy C-ring
specimens and the metallographic specimens were comparable under identical heat
treatment conditions. Based on this hardness comparison, they also assumed that the
microstructure of modified Navy C-ring specimens will be similar to the metallographic
specimens under the same heat treatment conditions.
(a) (b)
Figure 2.20: Dimensions of Navy C-rings used by (a) Bates et al. [40], and (b)
Leskovsek and Ule [41].
Bates et al. [40] reported that the notched C-ring has greater crack sensitivity over
and above distortion. Also the dimensions of the notched C-ring (Fig. 2.20 (a)) and the C-
ring in Fig. 2.20 (b) are similar to the one used by French (see Fig.2.19 (a)).
Nan et al. [28, 42-44] used Navy C-ring specimens to study the distortion in
ferritic nitrocarburized SAE 1010 plain carbon steel. Ion, vacuum and gas ferritic
nitrocarburizing processes were applied to the Navy C-rings with varying thicknesses to
analyze distortion. Table 2.4 shows the inner diameter (ID), outer diameter (OD), gap
width (GW) and flatness distortions of nitrocarburized and carbonitrided SAE 1010 C-
ring specimens [44]. Nitrocarburized C-rings have lower ID, OD, GW and flatness
distortions than the carbonitrided C-rings.
24
Table 2.4: Change in OD, ID, GW and flatness distortions of nitrocarburized and
carbonitrided 1010 Navy C-rings [44]
Change in Change in Change in Change in
Heat Treatment ID, % OD, % GW, % flatness, mm
Gas ferritic nitrocarburizing
565oC/5hrs+N2 cooling 0.0201 0.0438 0.0311 0.0001
Gas carbonitriding
850oC/4hrs+oil quench (100oC) 0.1565 0.1146 2.4424 -0.0038
Distortion in high-speed steel was studied by Leskovsek and Ule [41] using the
Navy C-ring specimens shown in Figure 2.20 (b). Table 2.5 shows the distortion values
of high-speed steel Navy C-ring specimens used by Leskovsek [45]. The parameter ‘A’
denotes the outer diameter (OD), ‘B’ is the inner diameter (ID) and ‘D’ is the gap width
(GW) of C-rings (refer Fig. 2.20 (b)). The deep cryogenic treatment at -196oC in liquid
nitrogen caused greater dimensional stability (outer and inner diameters A and B) after
subsequent tempering, but increased the gap width distortion (ΔD). He attributed the
increase in gap width distortion to the transformational and thermal stresses.
25
Table 2.5: Hardness and distortion values of Navy C-ring specimens made from
HSS 6-5-2 after vacuum heat treatment [45]
Dimensions of NC specimens, (mm) Difference dimensions, (%)

Group Before vacuum After vacuum   
Vacuum heat of Hardness heat treatment heat treatment   
treatment and Navy HRC   
DCT C-ring A B D A B D A B D
sample
NC1 60.0 63.993 37.011 6.674 63.783 36.891 6.670 - 0.328 - 0.324 - 0.060
1050/80/830/4h/ NC2 59.9 63.991 37.012 6.618 63.783 36.895 6.615 - 0.325 - 0.316 - 0.045
20°C/h/600/25°C NC3 60.2 63.995 37.014 6.650 63.780 36.887 6.645 - 0.336 - 0.343 -
1230/80/2x500°C 0.075
NC4 63.9 63.999 37.034 6.676 63.882 36.926 6.547 - 0.183 - 0.292 - 1.932
1050/80/830/4h/ NC5 64.3 63.996 37.035 6.656 63.882 36.933 6.527 - 0.178 - 0.275 - 1.938
20°C/h/600/25°C NC9 64.7 63.993 37.024 6.674 63.890 36.934 6.586 - 0.161 - 0.243 - 1.318
1230/80/1x500/
-196/1x500°C
NC6 65.4 63.997 37.024 6.676 63.959 36.999 6.674 - 0.059 - 0.067 - 0.030
1050/80/830/4h/ NC7 65.4 63.998 37.018 6.673 63.957 36.994 6.669 - 0.064 - 0.065 - 0.060
20°C/h/600/25°C NC8 65.6 63.993 37.010 6.675 63.956 36.983 6.664 - 0.044 - 0.073 - 0.165
1230/80/2x540°C
NC10 66.0 63.998 37.017 6.636 64.008 37.017 6.631 + 0.016 0.000 - 0.090
1050/80/830/4h/ NC11 66.0 63.997 37.017 6.636 64.011 37.016 6.627 + 0.022 - 0.003 - 0.136
20°C/h/600/25°C NC12 66.0 63.996 37.025 6.637 64.011 37.030 6.624 + 0.023 + 0.013 - 0.196
1230/80/
-196/1x540°C
NC13 59.0 63.989 37.025 6.656 63.982 37.033 6.700 - 0.011 + 0.022 + 0.661
1050/80/830/4h/ NC14 59.0 63.994 37.017 6.635 63.988 37.025 6.678 - 0.009 + 0.022 + 0.648
20°C/h/600/25°C NC15 59.0 63.998 37.015 6.634 63.988 37.020 6.673 - 0.016 + 0.013 + 0.588
1150/80/2x500°C
Northwood et al. [28, 42-44, 46-51] have worked extensively on Navy C-rings to
determine distortion (size and shape) and residual stress in PS-18, SAE 8620, 4320 and
1010 steels. Their studies were mainly focused on minimizing distortion due to heat
treatment processes such as carburizing, carbonitriding and nitrocarburizing. Figure 2.21
(a, b) shows the size and shape distortion changes of carburized SAE 8620 C-rings. After
carburizing at 927/954oC, the C-rings were oil quenched (70oC) and tempered (149oC) to
improve dimensional stability. The results showed that the distortions are increased by
the increase in retained austenite and residual stress.
26
Figure 2.21: (a) Size and (b) shape distortion changes of carburized SAE Navy C-
rings: carburizing treatments: 1) 927oC/6h (carbon potential 0.9), 2) 927oC/6h
(carbon potential 1.0), 3) 927oC/6h (carbon potential 1.1), 4) 954oC/4h (carbon
potential 0.9), 5) 954oC/4h (carbon potential 1.0), 6) 954oC/4h (carbon potential 1.1)
and 7) 954oC/4h (carbon potential 1.2) [48].
2.5 Modeling
The use of high speed computations provided a new method to calculate internal
stresses and associated distortions. Computer modeling helps in preventing multiple
experimental attempts to develop a heat treatment practice that minimizes the distortion,
time and cost. It also became a useful tool to improve our understanding of the
mechanisms causing distortion.
Convergence analysis/mesh sensitivity is an important step in the finite element
simulation process. It is performed to reduce the discretization error in the mesh. The
element size is gradually decreased with every model and the final result (for example:
stress, displacement) is estimated repeatedly. By further decreasing the element size, the
final result of the current and previous model will eventually become the same. The
convergence error is then calculated by the percentage difference between the final result
of the current model and the previous model. This type of approach is called the h-
27
convergence [52] and with several runs, the discretization error can be significantly
reduced.
To determine distortion and residual stresses numerically, the temperature field
and the distribution of phases must be known. Inoue and Tanaka [53] published a model
estimating the temperature history including transformation heat and a finite element
model to calculate the residual stresses including transformation strains. Their model has
been refined over several years [54-57]. A finite element code called ‘HEARTS’ was
developed in which all six of the couplings (thermal stress, heat generation due to
deformation, temperature-dependent phase transformation, latent heat due to phase
transformation, transformation stress and transformation plasticity, and stress-induced
transformation) are included. The predicted carbon content after carburization agrees well
with the measured (XRD) carbon composition (see Fig. 2.22(a)). The residual stress
distributions of the carburized steel cylinder specimen showed compressive residual
stress at the surface and later became tensile until 3.5 mm from center (see Fig. 2.22(b)).
(a) (b)
Figure 2.22: (a) Carbon composition profile and (b) residual stress distributions for
a carburized + water quenched long cylinder steel containing molybdenum [57].
28
Thuvander et al. [58, 59] presented a numerical model to predict distortion during
heat treatment of tool steels using coupled temperature calculation and phase
transformation and subsequent analysis of mechanical response. The simulations have
been carried out with finite element model code ABAQUS with additional routines for
phase transformations. Both diffusion controlled and martensite transformations were
included in the model. Heat treatment simulations for quenching and tempering as well as
case hardening have been performed.
The temperature history of tool steel blocks (ORVAR SUPREME and DIEVAR)
were validated against the measured temperature (see Fig. 2.23(a)). The predicted
distortion of gas quenched tool steel blocks were found be in a good agreement with the
experimental distortion (Fig. 2.23(b)).
(a) (b)
Figure 2.23: (a) Temperature history (experimental and computed) at centre of tool
steel block during gas quenching, (b) Distortion of gas quenched (3 bar N2) ORVAR
SUPREME tool steel block (experimental and computed). The distortion is
magnified 50 times [58].
29
2.5.1 Distortion modeling
Silva et al [60] reported the distortions of AISI 4140 steel C-rings quenched in oil.
They predicted a 7% error between the experimental and numerical values of the C-ring
Gap Width (GW) and Outer Diameter (OD) distortions. These geometric distortions of
the C-rings were attributed to austenite-martensite transformation at the thicker regions of
the C-ring. Figure 2.24(a, b) shows the gap width distortion and distortion simulation of a
C-ring specimen due to heat treatment.
(a) (b)
Figure 2.24 : (a) Dimensional changes of a C-ring specimen before heat treatment
(m and n dimensions) and after heat treatment (m’ and n’ dimensions), (b)
distortion simulation (displacement magnification 20X) [60].
Hernández-Morales et al. [61] studied the evolution of thermal and stress fields in
a AISI 304 stainless steel modified Navy C-ring probe cooled to 40oC in still water. They
applied an uncoupled thermo-elasto-plastic model to predict the internal stress field and
distortion using DEFORM-HT (commercial software). The model was successfully
validated by comparing the computed and measured thermal response. The measured and
predicted gap length of C-ring also showed a good agreement. They concluded that the
C-ring gap widens at the early stages of quenching due to the thermal contraction of the
30
tip of the probe and then closes as the thermal contraction of the medium portion of the
probe arm pushes the tip inwards (see Fig. 2.25).
Figure 2.25: Computed Gap Width (GW) vs. time curve [61].
Li et al. [62] developed a finite element model of an AISI 8620 steel C-ring (Fig.
2.26(a)) using DANTE (commercial software) to simulate the furnace heating,
carburization, quenching and tempering processes. Adding carbon lowered the gap width
distortion from 0.05 to 0.02mm (see Fig. 2.26(b)). However quenching increased the
distortion to 0.22mm. The results showed that the gap width distortion of the C-ring was
very sensitive to the heat treatment conditions. The gap width distortion was caused by
the thermal gradient and phase transformation sequence.
(a) (b)
Figure 2.26: (a) Finite element model of one half of the C-ring, (b) Gap width
(opening displacement) distortion of AISI 8620 carburized C-ring [62].
31
Zoch [34] presented a methodology called “distortion engineering” (see Fig. 2.27)
to understand the dimensional changes of SAE 52100, 4140 and 5120 rings, shafts and
discs/gears. The simulated processes include rolling, forging, milling, heating,
carburizing and quenching. The distortion compensation was found to be difficult for
shafts and discs/gears but the distortion could be compensated successfully for rings.
Hence the material geometry is an important aspect that should be considered to reduce
distortion.
Figure 2.27: Distortion engineering procedure by Zoch [34].
Nicolas et al. [63] presented the experimental and simulation results of 3-D
distortion identification from quenched ASCOMETAL steel grade C-ring. The C-ring
test part was 100mm long with a 16mm wide opening. The dimensions of outer and inner
diameters were 70 and 45 mm with 11 mm off-centered. The 3-D distortion of C-rings
were reported as ovalization, barrel effect and banana effect (see Fig. 2.28).
32
(a) (b) (c) (d)
Figure 2.28: (a) 100 mm long C-ring, (b) comparison of experiment and simulation
distortion results, (c) banana effect, and (d) barrel or bobbin effect [63].
Freborg et al [64] developed a heat treatment simulation model to predict the
residual stress and distortion response in a carburized AMS 6308 steel coupon.
Convective heat transfer coefficients (htc) were calculated from the thermal response of a
304 stainless steel test block and a DANTE (commercial software) thermal model. A
constant heat transfer coefficient (htc) was assumed during gas quenching as the
temperature dependent properties like thermal conductivity and kinematic viscosity have
less effect on htc. Figure 2.29 shows the distortion comparison of an AMS 6308 coupon
that was vacuum carburized + subcritical annealed + austenitized + gas quenched +deep
frozen + double tempered.
Figure 2.29: Comparison of measured and predicted distortion (DANTE model)
showing the "bowing" of AMS 6308 coupon [64].
33
They have also modeled a heat treatment simulation involving carburization and
oil quenching for AISI 4320H gear component [65]. The radial distortion was predicted
and validated by the experimental measurements (see Fig. 2.30).
Figure 2.30: Radial displacement contour and distortion comparison of bore and tip
distortion of AISI 4320H gear component [65].
Depouhon et al. [66] presented a numerical model to anticipate the distortion in a
simplified large gear due to nitriding (see Fig. 2.31 (a)). The distortion was measured
experimentally using a 3D coordinate measuring machine (CMM) and the predicted
distortion results were validated against the measured distortion. The predicted and
measured distortion were calculated at seven different locations in the gear. The predicted
distortion values reported in Figure 2.31 (b) seem to be in good agreement with the
experimental values. The simulation method assumed that the volumetric eigen strains
were the only source of distortion.
34
(a) (b)
Figure 2.31: (a) – Geometry of a simplified large gear, (b) – Distortion comparison
at seven points [66].
A mathematical model was developed to predict the distortion, carbon and
nitrogen contents in a carbo-nitrided ASTM 4118 carbon steel specimen (see Fig. 2.32
(a)). The heat treatment starts with heating at 930oC/120 min followed by passing C/N
gas with carbon and nitrogen potentials of 1.1% and 0.3%. The carbo-nitriding process
was carried out for 240 min followed by cooling at 850oC for 40 min. In the end, the
specimen was oil quenched to 60oC. The predicted distortion shows partial agreement
with the experimental results (refer Fig. 2.32 (b)).
(a) (b)
Figure 2.32: (a) Carbon steel ring specimen geometry (dimensions in mm), (b)
Measured and predicted distortion results at location 1 (outer diameter) and 2
(inner diameter) [67].
35
Table 2.6 is a summary of the distortion modeling discussed in section 2.5.1. The
distortion was predicted mostly for carburizing treatments that involve austenite to
martensite phase transformation. Extensive literature is not available for the distortion
modeling of nitrocarburizing processes.
Table 2.6: Summary of the distortion modeling
Study Material/Heat treatment Compone Core material Agreement

(Ref.) nt of phase with
modeling transformation experiment*
AISI 4140 steel/ austenite to
[60] carburizing C-ring martensite good
(900oC/1hr)+oil
quench(25oC/300s)
[61] AISI 304 stainless steel / modified no phase good
heating(900oC)+Water C-ring transformation
quench(40oC)
[62] AISI 8620 steel / good
carburizing(925oC/ C-ring austenite to
6hrs)+oil lower bainite &
quench(65oC/10min)+ martensite
tempering(150oC/2hrs)
[63] ASCOMETAL steel modified not mentioned partial
grade/heating(930oC)+ C-ring
quench(20oC)
[64] AMS 6308 steel/ notched austenite to
carburizing+anneal+ coupon martensite
austenitize+gas moderate
quench(10 bar N2) +deep
freeze+double temper
[65] AISI 4320H steel/ gear austenite to
Carburizing(927oC/ martensite & partial
15hrs+857oC/1hr)+oil bainite
quench(70oC)
[66] 32CrMoV13 steel/ gear no phase good
Gas nitriding(120hrs) transformation
[67] ASTM 4118 carbon
steel/carbonitriding ring austenite to partial
(930oC/360min)+cooled martensite &
(850oC/10min)+oil bainite
quench(60oC)
* ‘good’ denotes <10% difference between experimental and simulated values,
‘moderate’ indicate <25% difference between experimental and simulated values, and
‘partial’ denotes >40% prediction difference.
36
2.5.2 Composition-Depth profiles: experimental and modeling
Figure 2.33 shows the nitrogen and carbon composition-depth profiles of gas
nitrocarburized Fe-0.8C (wt. %) and Fe alloys. In the compound layer, the concentration
of nitrogen is higher than the carbon concentration during the nitrocarburizing treatment.
This situation can arise when the carbon and nitrogen content in the compound layer
cannot be altered independently of each other.
Figure 2.33: Nitrogen and carbon concentration profiles measured using EPMA on
nitrocarburized Fe-0.8C (wt. %) and Fe alloys [68].
Grafen and Edenhofer [69] have reported a method to overcome this problem by dividing
the nitrocarburizing process in two parts: the first part will have NH3 + CO2 + N2 gases to
increase the nitrogen content while the second part consists of NH3 + C3H8 + N2 gases to
increase the carbon content in the compound layer (see Fig. 2.34).
Figure 2.34: Special ferritic nitrocarburizing (FNC) process for increased N2 and C
contents [69].
37
Many researchers have investigated the composition-depth profiles during
nitriding/nitrocarburizing treatments to predict the compound layer growth. Yang and
Sisson Jr. [70] simulated the compound layer growth kinetics of nitrided AISI 4140 steel.
In their work, the N concentration was measured at four different locations (labelled as 1,
2, 3 and 4 in Fig. 2.35) within the surface layer and the solid (red) line indicates the
simulated nitrogen concentration profile. The simulated profile showed good agreement
with the measured results.
Figure 2.35: Nitrogen concentration profile for nitrided 4140 steel (measured
vs. computed) [70].
Keddam [71] presented a kinetic model to simulate the pulse plasma nitriding
process using Fick’s laws of diffusion. He developed a computer simulation program
using Turbo-Pascal language to predict the nitrogen composition profiles at two
temperatures (see Fig. 2.36).
Figure 2.36: Predicted nitrogen composition-depth profiles for pulse plasma nitride
pure iron. The experimental data (∆ symbol) were acquired from Yan et al. [72], (a)
T=773K (500oC) & (b) T= 793K (520oC) (1 represents ε phase, 2 is γ′ and 3
represents α phase) [71].
38
The model was limited to the compound layer only and the diffusion layer was not
included in the model. The regions 1, 2 and 3 in Fig. 2.36 helps to identify the ε/γ′
interface and γ’/α interface in the nitrogen profiles. The thickness of the nitrided phases
was found to decrease with the increase in process temperature (500 to 520oC).
Finite difference approximation is the most widely known technique used for simulating
the composition profiles of nitriding/nitrocarburizing steels. Gu et al. [73] performed a
numerical simulation of nitrogen and carbon composition-depth profiles using the finite
difference method with the Crank-Nicolson algorithm. The Crank-Nicolson algorithm is
an advanced implicit integration scheme proposed by Crank and Nicolson in 1947 [74]. It
is unconditionally stable and produces better truncation error than the basic implicit
method [75]. Figure 2.37 shows the simulated and experimental composition profiles for
low-temperature plasma nitrocarburized (430oC/30hrs) austenitic stainless steel. The blue
line indicates the nitrogen composition and the red line indicates the carbon composition.
The blue and red dots represent the experimental data measured using glow discharge
optical emission spectroscopy (GDOES). The general trend of the carbon and nitrogen
composition profiles agree well.
Figure 2.37: Predicted and experimental nitrogen, carbon composition profiles of
plasma nitrocarburized austenitic stainless steel [73].
39
Another example of nitrogen-depth profile simulation using a finite difference method
(Crank-Nicolson) is shown in Figure 2.38. The nitrogen profile in plasma nitrided
(400oC/2hrs) AISI 316L steel was experimentally obtained by GDOES. The diffusion
coefficient values (Do) of nitrogen were changed to predict the best profile
approximation. By comparing the experimental and simulated profiles, Moskalioviene et
al. [76] calculated the best fit (black line) at Do = 0.837 x 10-3cm2/s. It was found that the
nitrogen penetration depth and nitrogen diffusivity depends on the crystalline orientation
of AISI 316L steel (see Fig. 2.38 (b)).
(a) (b)
Figure 2.38: Simulated and experimental nitrogen depth profiles of plasma nitrided
AISI 316L (400oC/2hrs) with different N diffusion coefficients [76].
Torres et al. [77] also developed a numerical model using implicit finite difference
approximation to predict the nitrogen profile and distortion during FNC treatments. The
model was applied to housing (case 1) and plate-like (case 2) components made of sand-
cast ductile iron (Fig. 2.39 (a & b)). They have divided the model into two parts. The first
part of the model calculates the nitrogen profile. A second order kinetic reaction was
included in the model to account for the formation of nitrides.
40
(a) (b)
Figure 2.39: (a) schematic of housing, (b) plate-like component
The predicted N composition profile (solid line in Fig. 2.40) was in good
agreement with the experimental N profile (measured using GDOES). The second part
takes the nitrogen composition profiles as input and executes structural analysis to predict
the final distortion (see Fig. 2.41). The bore distortion initially decreases with the
distance along the bore, then increases back to the same level.
Figure 2.40: Nitrogen composition-depth profiles (measured and calculated) [77].
41
Figure 2.41: Predicted bore deformation for housing (case 1) and plate-like
(case 2) components due to 2 different FNC treatments [77].
Table 2.7 summarizes the composition profile modeling procedures reported in section
2.5.2.
Table 2.7: Summary of the composition profile modeling
Component of Agreement
Study Materials / Heat treatment modeling with
(Ref.) experimental
results*
[70] AISI 4140
steel/heating(843oC/
1.5hr)+oil quench disk good
(54 C)+tempered(579oC/
o
3hrs)+nitriding
(527oC/10hrs+548oC/
50hrs)
[71] Pure iron / plasma 15 x 15 x 10mm partial
nitriding(500oC) specimen
[73] AISI 316L steel / plasma -- good
nitrocarburizing
(430oC/30 hrs)
[76] AISI 316L / plasma -- good
nitriding (400oC/2hrs)
[77] Sand cast ductile iron / housing & plate- good
ferritic nitrocarburizing like
* ‘good’ denotes <10% difference between experimental and simulated results, and
‘partial’ denotes incomplete experimental data.
42
2.5.3 Residual Stress Modeling
Freborg et al. [64] applied an internal state variable (ISV) material model into the
DANTE simulation software to predict the residual stress of a notched AMS 6308 steel
coupon. The results showed compressive residual stress at the surface, which then tended
to become tensile with an increase in depth (see Fig.2.42). There is not much change in
the predicted residual stress values up to 0.6mm depth. At 0.6mm, the X-ray measured
residual (compressive) stress is almost half of the predicted stress.
Figure 2.42: Predicted and measured axial residual stress of a carburized AMS 6308
steel coupon [64].
Depouhon et al. [78] developed a nitriding model to predict the residual stresses
of 32CrMoV13 low alloy steel. The model has two sections: the chemical calculation was
solved by diffusion-reaction-convection model and the mechanical calculation by elasto-
visco-plasticity model. Figure 2.43 shows the predicted hoop residual stress and residual
stress profiles after gas nitriding. The model predicts a compressive stress of
approximately 500 MPa at the nitrided surface, and tensile stresses in the bulk material.
43
(a) (b)
Figure 2.43: (a) – Predicted hoop residual stress map (MPa), (b) - Residual stress-
depth profiles for a gas nitrided (550oC/120 hrs) tubular sample [78].
A multiphase material model was developed using ABAQUS (finite element
code) with DANTE user subroutines to simulate the residual stresses of a carburized
Almen strip [79]. Almen strip (100 mm long and 20 mm wide) is a calibration test
specimen used to quantify the residual stresses. The experimental residual stress points in
Figure 2.44 were measured using X-ray diffraction [80]. Although the residual stress data
(experimental) was not completely measured, a partial agreement exists between
experimental and simulated residual stresses.
(a) (b)
Figure 2.44: Residual stress-depth profiles at the center of the Almen strip, (a) 2.44
mm thick and (b) 3.18 mm thick [79].
44
The residual stress gradients of a nitrided Fe-Al specimen was studied using a
cross-sectional transmission X-ray micro-diffraction technique [81]. It was reported that
the Fe-Al specimen cutting can relax the residual stress in the near-surface region. FEM
simulations were developed to estimate the residual stress relaxation using ABAQUS
software. In the FEM model, the stress profile was varied until the predicted stress was
equal to the experimentally measured residual stress. The solid line in Figure 2.45
represents the predicted residual stress of the cross-sectional specimen using FEM. The
residual stress profiles were divided into five regions (I, II, III, IV and V) to understand
the stress gradients. The un-nitrided core (region V) with zero nitrogen has low tensile
stress. With the increase in nitrogen composition, compressive residual stress is
developed in region IV, III and II, but region I ended up with tensile residual stress at the
surface. The results showed that the misfit accommodation of incoherent AlN
precipitation was realized plastically. The AlN phase in Fe-Al specimen is similar to the
γ’ (Fe4N) phase in nitrided/nitrocarburized carbon steels.
Figure 2.45: Residual stress-depth profiles for the nitrided Fe-Al specimen
(experimental and predicted) [81].
45
Table 2.8 summarizes the residual stress-depth profile modeling discussed in section
2.5.3.
Table 2.8: Summary of the residual stress-depth profile modeling
Component Agreement
Study Material / Heat treatment of modeling with
(Ref.) experimental
results
[64] AMS 6308 steel /
carburizing + anneal + notched partial
austenitize + gas quench (10 coupon
bar N2) + deep freeze +
double temper
[78] 32CrMoV13 steel / gas tubular plate good
nitriding (550oC/120hrs)
[79] SAE 4023 & SAE 4620 steel
/ carburizing Almen strips partial
(927oC/7.5hrs+899oC/
2hrs+871oC/1.3hr) + oil
quench (177oC) + air cool
(25oC)
[81] Fe-4.7 at.% Al / rectangular
recrystallized (800oC/ specimen good
20min)+gas nitriding
(550oC/30hrs)+water quench
* ‘good’ denotes <10% difference between experimental and simulated results, and
‘partial’ denotes >40% prediction difference.
46
CHAPTER 3 ANALYTICAL APPROACH
The main goal of this research is to minimize the distortion and residual stress associated
with the ferritic nitrocarburizing treatment for SAE 1010 plain carbon steel specimens.
To calculate the distortion behaviour, two different specimen types were used, namely:
Navy C-ring (probe) and a torque converter (TC) piston (automotive component). Navy
C-rings were simply used as a measuring tool to observe the geometrical variations due to
the ferritic nitrocarburizing process. Figure 3.1 is an overview of the research plan for
evaluating the distortion of Navy C-rings and torque converter (TC) pistons and
subsequent validation of the simulation results.

To study distortion in ferritic
nitrocarburized SAE 1010 steel
Test specimen – Navy C-ring

Actual component – TC piston
Experimental method Numerical method
TC pistons Navy C-ring test Navy C-ring FEMs TC piston FEMs
CMM measured ID, OD & GW distortions Predicted ID, OD & GW distortions
Measured N Validation of measured & predicted Simulated N

composition distortions composition
profiles V/VN ratio profiles
Validation of measured & predicted

composition profiles
Local distortion due to ε & γ’ phases
Measured surface Predicted surface
Validation of measured & predicted
residual stresses residual stresses
residual stresses
Residual stress distributions for 1-step
& 2-step nitrocarburizing treatments
Figure 3.1: Overview of the research plan.
47
Torque converter (TC) is used to transmit power from an engine/motor to a
rotating drive load. The components of torque converter include: a pump impeller, a
turbine runner, a stator, and a piston [16]. TC piston (lockup clutch) is used to eliminate
the energy loss due to difference in rotational speeds of turbine and the impeller. TC
piston is ferritic nitrocarburized to improve the fatigue strength and wear resistance.
Figure 3.2(a, b) shows a typical torque converter (TC) and cross section of a torque
converter and piston.
TC in a transmission Piston (spring damper)

(a) (b)
Figure 3.2: (a) Torque converter (TC), and (b) TC cross section [82].
3.1 Distortion reduction
The first part of the research deals with the distortion reduction of nitrocarburized
SAE 1010 steel specimens. To solve the distortion problem, three different Navy C-ring
specimens (thickness: 19, 10, 2.8mm) and torque converter (TC) piston specimens were
used in the experimental and numerical methods. Navy C-ring probes were mainly
chosen to analyze the effect of its thickness on distortion.
48
3.1.1 Navy C-ring geometry
The Navy C-rings were cut from a bar stock of hot rolled SAE 1010 steel using
electrical discharge machining. Figure 3.3 (a, b & c) shows the geometry of three C-rings
(C1, C2 and C3) that were used to calculate the distortion.
6.35±0.127 GW 6.35±0.127 GW 6.35±0.127 GW
31.75±0.127 31.75±0.127 31.75±0.127

ID ID ID
50.8±0.127 OD 50.8±0.127 OD 50.8±0.127 OD Thickness: 19.05±0.127 10.05±0.127 2.8±0.127
(a) C1 C2 C3 (b) C1 C2 C3
19.05 10.05 2.8

6.35 ± 0.127 ±0.127 ±0.127 ±0.127
6.35±0.127
31.75 ± 0.127
15.875±0.127
50.8 ± 0.127 C1 C2 C3
(c)
Figure 3.3: (a, b) Navy C-ring specimen geometry, (c) schematic for Navy C-
rings C1, C2 and C3 (dimensions in mm).
3.1.2 Materials
The chemical composition of SAE 1010 plain carbon steel specimens used in the
present work is listed in Table 3.1:
49
Table 3.1: Elemental compositions of SAE 1010 plain carbon steel [44]
Element Wt.%
Carbon (C) 0.12
Manganese (Mn) 0.43
Phosphorus (P) 0.008
Sulfur (S) 0.008
Silicon (Si) 0.03
Chromium (Cr) 0.03
Nickel (Ni) 0.01
Molybdenum (Mo) 0.01
Copper (Cu) 0.02
Plumbum (Pb) Not detected
Aluminum (Al) 0.052
Vanadium (V) 0.001
Columbium (Cb) Not detected
Titanium (Ti) 0.002
Cobalt (Co) Not detected
Tin (Sn) Not detected
Boron (B) 0.0003
Calcium (Ca) 0.0001
Zirconium (Zr) Not detected
Tungsten (W) Not detected
3.1.3 Torque converter piston fabrication
Cold-worked SAE 1010 steel sheets (2.8 mm thick) were used to produce torque
converter (TC) pistons. The SAE 1010 sheets underwent a progressive five-stage
stamping operation to fabricate them into TC pistons [16]. Torque converter pistons were
then subjected to various ferritic nitrocarburizing processes. They have an outer diameter
50
(OD) of 260 mm and an inner diameter (ID) of 60 mm. Figure 3.4 shows the SAE 1010
steel torque converter (TC) piston geometry.
ID 60 mm
OD 260 mm
Figure 3.4: Geometry of torque converter (TC) piston.
3.1.4 Heat treatment conditions
The basic process scheme of a ferritic nitrocarburizing process is given below
(Fig. 3.5).
Nitrocarburization (525-650oC) Cooling

Temperature, oC
Time, hrs
Figure 3.5: Schematic process diagram of the ferritic nitrocarburizing treatment.
Table 3.2 lists the heat treatment processes that were used in the experimental and
numerical methods. For each of the gas ferritic nitrocarburizing (FNC) treatments, six
Navy C-rings with three different thicknesses were used for measuring the distortion. The
total number of torque converter (TC) pistons used for each FNC treatment is ten.
51
Table 3.2: Heat treatment and specimen details
Heat treatment No. of specimens used
Navy C-rings: 6
595oC/ 4hrs + air cooled to
Gas ferritic TC pistons: 10
room temperature
nitrocarburizing
Navy C-rings: 6
565oC/ 5hrs + air cooled to
TC pistons: 10
room temperature
TC pistons: 10
Vacuum ferritic 580oC/ 10hrs + air cooled to
nitrocarburizing room temperature
3.1.5 Sample preparation and optical microscopy
An optical microscope (Leitz Laborlux 12 ME) was used to analyze the
microstructure of the SAE 1010 TC piston samples after ferritic nitrocarburizing (FNC)
treatments (see Fig. 3.6). Small sections were cut from the heat treated TC pistons and
mounted in blue diallyl phthalate powder using a Buehler Simplimet mounting press. The
mounted samples were then ground using 240, 320, 400, 600 and 1200 grit silicon carbon
papers. After grinding, samples were polished using 1.0 µm and 0.5 µm alumina powder
suspended in distilled water. The TC piston samples were then etched using 3.5% Nital
solution for 10-15 seconds, followed by a water rinse and ethanol. The following
magnifications were used to finally examine the specimens: 200X, 500X and 1000X.
52
Figure 3.6: A light optical microscope (Leitz Laborlux 12 ME).
Nitrocarburized microstructures showed a compound layer containing ε-phase
(Fe2-3(C, N)), diffusion zone containing γ′-phase (Fe4N), and ferrite in the core. The
thickness of the compound layer was then measured for different heat treated samples.
3.1.6 Nano-indentation measurements
Nanoindentation testing was used to calculate the Young’s modulus values of the
compound layer and core material (SAE 1010). Figure 3.7(a) shows the instrument used
for nanoindentation (Hysitron Ubi1) in SAE 1010 steel samples. The indentation load is
applied from 0 to 500µN and then from 500µN back to 0µN. When the load is removed
from the indenter (500µN back to 0µN), the specimen will try to recover back to its
original shape due to the elastic strain relaxation. However, the specimen is unable to
fully recover due to plastic deformation. The Young’s modulus of the specimen is
calculated from the slope of the unloading curve of the load-displacement response (see
Fig. 3.7(b)). The depth of indenter penetration was ~ 40nm.
53
(a) (b)
Figure 3.7: (a) Hysitron (Ubi1) nanomechanical instrument, (b) loading-unloading
response for a SAE 1010 C-ring after FNC.
3.1.7 Experimental distortion measurements
The distortion of C-ring and TC piston specimens were measured using a
PRISMO coordinate measuring machine (CMM) (refer Fig. 3.8). The inner diameter
(ID), outer diameter (OD) and gap width (GW) dimensions were measured by conducting
contact scans on the specimen surface using a mechanical set-up probe. The specimen
features were scanned using Imageware Surface scanning software. The dimensional
accuracy was 0.1 microns.
The ID and OD dimensions were recorded at multiple locations along each
specimen before and after ferritic nitrocarburizing (FNC) treatment. The ID dimension of
the TC piston specimen was measured at 15mm below the lockup surface and the OD
dimension was measured at 21.5mm below the lockup surface of the TC piston.
54
The C-ring’s GW dimension was measured at top, middle and bottom positions of
the gap width. The difference in ID, OD and GW dimensions (after FNC – before FNC)
were then calculated for each specimen, and their average values were finally obtained as
geometric distortions.
Figure 3.8: PRISMO coordinate measuring machine (CMM) [83].
3.1.8 Numerical (FEM) distortion prediction
The predicted distortions were calculated from the finite element simulations of
Navy C-rings and torque converter (TC) pistons. The ID and OD distortions were
calculated throughout the inner and outer circumferences of the C-ring model and their
average values were compared with the experimental ID and OD (averaged) distortions.
The GW distortion was predicted at three locations (top, middle and bottom through the
thickness) similar to the experimental GW distortion of the C-rings. The details about the
Navy C-ring FEM models, TC piston FEM models and the distortion results are
discussed in detail in Chapter 4 and 5.
55
In addition to the predicted ID (inner diameter), OD (outer diameter) and GW
(gap width) distortions, a composition-depth profile simulation model was developed to
predict the local distortion due to ε & γ′ phases (see Chapter 6). The local distortion due
to the nitrocarburized phases will help to better understand and control the distortion
behavior.
3.1.9 Composition-depth profile numerical simulation
The nitrogen composition-depth profiles were calculated numerically using finite
difference method (FDM). The numerical models are addressed in Chapter 6. Figures 3.9
and 3.10 show the schematic diagrams for the simulated nitrogen composition-depth
profiles due to 1-step and 2-step nitrocarburizing treatments. The simulated composition-
depth profiles of 1-step and 2-step nitrocarburizing treatments were used to calculate the
compound layer (CL) thickness and local distortion due to ε and γ′ phases.
Nitrogen composition,wt.%
ε γ′
from diff.zone
α
Distance from surface,µm
Figure 3.9: Schematic of nitrogen composition-depth profile due to 1-step
nitrocarburizing treatment.
56
Nitrogen composition,wt.%
γ'+ε γ'from diff.zone α
Figure 3.10: Schematic of the simulated nitrogen composition-depth profile due to 2-
step nitrocarburizing treatment.
3.1.10 Composition-depth profile measurements (experimental)
Using electron probe micro analysis (EPMA), quantitative elemental analysis can
be performed at a very small spot size. It is commonly used to analyze geological
materials. Nitrogen and carbon composition profiles of ferritic nitrocarburized TC piston
samples were measured experimentally using a CAMECA SX50 electron probe micro
analyzer (EPMA) at the Earth Sciences Department, University of Toronto (see Fig.
3.11).
Point analysis along a linear direction was performed on nitrocarburized TC
piston samples perpendicular to the surface. A total of 15 point locations were selected in
the compound layer (on both the sample ends) and core material to measure the
57
intensities. The measured intensities were then compared with a standard of known
nitrogen and carbon compositions to conduct the quantitative chemical analysis.
Figure 3.11: Cameca SX50 Electron Probe Micro Analyzer (EPMA) at Earth
Sciences, University of Toronto [84].
3.2 Reduction in surface residual stress
The second part of research deals with the reduction of surface residual stresses in
TC piston specimens after ferritic nitrocarburizing. The surface residual stresses due to 1-
step ferritic nitrocarburizing were predicted and validated against the experimentally
measured stresses. The results showed tensile residual stresses at the TC piston surface.
In order to further reduce the surface (tensile) stress, the residual stress distributions for
the nitrocarburized phases were simulated for a set of 2-step nitrocarburizing treatments
(refer to Chapter 6).
58
CHAPTER 4 NUMERICAL SIMULATIONS FOR NAVY C-RINGS AND TORQUE
CONVERTER PISTONS
Experimental methods require several repetitions to obtain improvements in heat
treatment processes [85]. Repeated experiments are time consuming and expensive. To
overcome this problem, simulation tools are developed. Numerical simulations using the
finite element method (FEM) are widely used in the automotive industry to save time and
reduce cost in manufacturing processes. The accuracy of the simulation results depend on
providing the correct material data.
Distortion resulting from heat treatment can be calculated using numerical
methods. Two dimensional and three dimensional finite element models were developed
to simulate the heat treatment conditions and to investigate the effect of Navy C-ring and
torque converter (TC) piston geometries on distortion.
4.1 Material Properties
An isotropic fully elastic material model was selected for the Navy C-rings and
torque converter (TC) pistons. Table 4.1 lists the material properties (Young’s modulus,
Poisson’s ratio, thermal expansion coefficient) of the compound layer and bulk material
(SAE 1010 steel) used in the FEM models. The Young’s modulus values were measured
using nano-indentation test. The mean thermal expansion coefficient values were taken
from the literature [86, 87]. The density of SAE 1010 steel is 7.872x103 kg/m3 [86, 88].
The material model has been selected as elastic only, because the maximum yield
strength (from the simulated models) of the C-ring and TC piston are calculated as 78.55
59
MPa and 54.96 MPa respectively. At 600oC and room temperature, the yield strength of
the SAE 1010 steel are 110 MPa and 305 MPa respectively [89, 90] . Therefore, the
maximum calculated stress do not exceed the yield strength of 1010 steel.
Table 4.1: Material properties used in the FEM models
Young’s Poisson Mean thermal expansion
Material Modulus (E), ratio (ν) coefficient (x10-6), oC-1
GPa
Compound layer 205 0.29 7.62 (25oC)
Bulk material 192 0.29 14.6 (0-600oC)
(SAE 1010)
For a low carbon steel (C < 0.3%), the variation of Young’s modulus values with
temperature was found to be less than 20% [91]. Therefore, in the FEM models, the
Young’s modulus values were assumed constant and do not vary with temperature.
4.2 Navy C-ring Probe
Three different Navy C-rings were modeled with dimensions similar to the C-ring
geometries (C1, C2 and C3) shown in section 3.1.1. The Inner Diameter (ID), Outer
Diameter (OD) and Gap Width (GW) of the C-rings were calculated before and after heat
treatment simulations. Figure 4.1 shows the Navy C-ring dimensions used in the FEM
models.
60
6.35 mm Thickness
31.75mm ID
50.8 mm OD 19 mm 10 mm 2.8 mm
C1 C2 C3
Figure 4.1: Navy C-ring geometry dimensions
4.3 Navy C-ring Finite Element Models
Finite element simulations of Navy C-rings were developed to predict the
distortion of nitrocarburized SAE 1010 steel. Two different heat treatment conditions
(565oC/5hrs + air cooling, and 595oC/4hrs + air cooling) were simulated in this study.
The C-ring part was partitioned into sections: compound layer and bulk. The compound
layer of C-rings were modeled with a thickness of 13.73 µm for 565oC/5hrs+air cooling
and 19.12 µm for 595oC/4hrs+air cooling. These thickness values were obtained from
the previous work [16]. The material properties of the compound layer and bulk material
(SAE 1010) were applied to the modeled sections of the C-ring (refer to Table 4.1).
Figure 4.2 compares the modeled C-ring sections with the optical micrograph showing
the compound layer.
61
Compound
layer
Figure 4.2: Compound layer comparison of the Navy C-ring probe model and the
optical micrograph showing the compound layer of SAE 1010 steel.
The heat treatment process involving ferritic nitrocarburizing and air cooling does
not involve a phase transformation (in the bulk), so the FEM model will not take into
account any phase transformation phenomenon, e.g. austenite to martensite.
4.3.1 Boundary Conditions
Heat transfer that takes place between the material surface and the surrounding
environment by convection is related to the heat transfer coefficient as follows:
q = h · A · ΔT (4.1)
where h represents the convective heat transfer coefficient (W/m2 oC), A denotes the heat
transfer area of the surface (m2), q is the heat transferred per unit time (W), and ΔT
denotes the temperature difference (Ts-T∞) between the surface (Ts) and the fluid (T∞)
(oC). This convective heat transfer coefficient (h) was applied as a thermal boundary
condition at all Navy C-ring surfaces in contact with the gas. The heat transfer coefficient
used in the model was 200 W/m2C. In the model, one end of the Navy C-ring half was
fixed at the bottom to avoid rigid body motion.
62
4.3.2 Discretization of the C-ring models
All parts were assigned with a solid section property in ABAQUS (a commercial
software). Taking advantage of the C-ring symmetry, only half of the C-ring was
modeled. The discretized finite element model of the three different C-rings are
illustrated in Figure 4.3. Linear tetrahedral elements of type C3D4T were selected to
discretize the C-ring parts. The mesh density of the nitrocarburized layer was kept higher
than the bulk material; computer runs with different mesh densities were performed to
make sure that numerical solution for the predicted distortion was mesh independent.
After several computer runs, it was also found that a variable time step of 10-9 to 2000 sec
was appropriate for convergence. Table 4.2 shows the mesh sensitivity study for C3
sample. The total number of elements in each of the C-ring model are listed in Table 4.3.
Table 4.2: Mesh sensitivity study in a C-ring (C3) model
Model No. of GW distortion (top) Relative difference
number elements (mm) between consecutive
iterations (%)
1 114795 -0.0067 --
2 121218 -0.0071 5.6
3 121586 -0.0074 4.1
4 122359 -0.0076 2.6
63
C1 C2 C3
Figure 4.3: Half symmetric geometry of meshed Navy C-rings with varying
thicknesses 19mm (C1), 10mm (C2), 3mm (C3).
Table 4.3: Details about the C-ring elements
Specimens Total number of Total number of tetrahedral
nodes elements
C1 62860 348199
C2 36416 197330
C3 22999 122359
4.4 Simulation Procedure of C-ring models
A total of six FEM C-ring models were developed (two heat treatments per C-ring
type). The distortion problem was solved using an explicit time integration scheme. Each
FEM model has two operations: heating and cooling (see Table 4.4). The FEM
simulation of the C-ring’s heating operation involved the prediction of the ring expansion
due to the increase in temperature from 27oC to 565oC/595oC. Once expanded at 565 or
595oC for 4-5hrs, the C-ring was considered as completely nitrocarburized by
64
incorporating the material properties of the ε & γ′ phases. The expanded C-rings were
then passed into the cooling operation (27oC/1.1hr).
Table 4.4: Finite element simulation set up for C-ring models
Simulated
Operation Parameter Value compound layer
thickness, µm
565oC/ 595oC/
5hrs 4hrs
Specimens C-rings (C1, C2, C3)
1 - Heating Material SAE 1010 steel
Initial temperature 27oC
Heating temperature/time 565oC/5hrs & 595oC/4hrs 13.73 19.12
Specimens Expanded C-rings from operation 1
2 - Cooling Initial temperature 565oC & 595oC
Cooling temperature/time 27oC/1.1 hr
4.5 Axisymmetric Torque Converter Piston Model
Finite element simulations (2D axisymmetric model) of torque converter pistons
were developed. The torque Converter (TC) piston used in this study has a thickness
(2.8mm) which is same as the C3 C-ring type. The same heat treatment conditions that
were used for Navy C-rings were used for TC pistons. The piston part was partitioned
into two sections: compound layer and bulk. The compound layer section was meshed
finer than the bulk material.
The compound layer section was modeled to a thickness of 12.28 µm for
565oC/5hrs+air cooling and 14.22 µm for 595oC/4hrs+air cooling conditions. These
thickness values were obtained from the previous work [16]. Similar to the C-ring model,
65
the material properties of the compound layer and bulk material (SAE 1010) were applied
separately. The applied thermal and mechanical boundary conditions were similar to the
Navy C-ring probe models. Figure 4.4 (a) & (b) shows the torque converter piston cross
section and axisymmetric FEM model. Triangular elements of type CAX6MT were
selected to discretize the axisymmetric TC piston.
Lockup
surface
(a) (b)
Figure 4.4: (a) Cross section of the torque Converter (TC) piston, (b)
axisymmetric TC piston model.
4.6 Simulation procedure of axisymmetric TC piston model
Axisymmetric models were developed using an explicit time integration scheme
to simulate the nitrocarburizing processes (565oC/5hrs + air cooling & 595oC/4hrs + air
cooling). The heating and cooling job files were set to run with double precision. The
expanded piston after the heating operation was predefined as the initial state of the
cooling operation. Table 4.5 lists the simulation set-up of the axisymmetric model similar
to the C-ring model.
66
In order to validate the predicted distortion values, the ID distortion was estimated at
11mm below the lockup surface. Similarly, the OD distortion was estimated at 21.5mm
below the lockup surface (refer to section 3.1.7).
Table 4.5: Finite element simulation set up for TC pistons
Simulated
Operation Parameter Value compound layer
thickness, µm
565oC/ 595oC/
5hrs 4hrs
Specimens TC piston
1 - Heating Material SAE 1010 steel
Initial temperature 27oC
Heating temperature/time 565oC/5hrs & 595oC/4hrs
Specimens Expanded piston from operation 1 12.28 14.22
2 - Cooling Initial temperature 565oC & 595oC
Cooling temperature/time 27oC/1.1 hr
67
CHAPTER 5 VALIDATION OF THE FINITE ELEMENT MODELS
5.1 Distortion results of Navy C-rings
The distortion occurs either by expansion or contraction of the C-rings due to heat
treatment. Distortion with a negative value indicates the contraction of C-rings after heat
treatment. The predicted C-ring distortions were validated against the measured
distortions (ID, OD and GW).
Top
Middle
Bottom
Figure 5.1: C-ring’s GW distortion measurement locations
The GW distortion was measured at three different locations using a CMM (see
section 3.1.7), which are denoted top, middle and bottom in Fig. 5.1. The C-ring’s gap
width (GW), OD and ID distortions were calculated from the Navy C-ring FEM models
and experimental measurements. The experimentally measured distortion of C-rings were
calculated by subtracting the dimensions (ID, OD and GW) after heat treatment from the
dimensions (ID, OD and GW) recorded before heat treatment. The C-ring’s ID, OD and
GW distortion values were then averaged (6 C-rings per heat treatment = 2C1, 2C2 and
2C3, total=12 C-rings) and are reported in Table 5.1. The absolute errors were estimated
as the difference between measured and predicted distortion.
ID, OD, GW distortion = ID, OD, GW dimensions (after heat treatment) - ID, OD, GW
dimensions (before heat treatment) (5.1)
68
Absolute error = Measured distortion - Predicted distortion (5.2)
Table 5.1: Measured ID, OD and GW distortions for nitrocarburized C-rings

Heat Gas ferritic nitrocarburizing, Gas ferritic nitrocarburizing,
treatment 595oC/4hrs + air cooling 565oC/5hrs + air cooling
Specimen ID C1 C2 C3 C1 C2 C3
(thickness) (19mm) (10mm) (2.8mm) (19mm) (10mm) (2.8mm)
OD distortion, 0.0250 0.0235 0.0278 0.0223 0.0224 0.0193
mm
ID distortion, 0.0067 0.0006 -0.0049 0.0064 0.0004 -0.0025
mm
GW distortion 0.0067 -0.0148 -0.0085 0.0043 -0.0144 -0.0117
(top), mm
GW distortion 0.0033 -0.0146 -- -0.0002 -0.0174 --
(middle), mm
GW distortion 0.0055 -0.0155 -0.0125 -0.0003 -0.0173 -0.0124
(bottom), mm
Tables 5.2, 5.3, and 5.4 compares the measured and predicted GW distortion results of
the Navy C-rings.
Table 5.2: C-ring’s Gap Width (GW) distortion results – Top location
Heat C-ring V/VN GW distortion (mm), Location: Top
Treatment specimens ratio* Measured Predicted Absolute
error
595oC/4h + C1 (19 mm thick) 381 0.0067 -0.0035 0.0102
air cooling C2 (10 mm thick) 200 -0.0148 -0.0109 0.0039
C3 (2.8 mm thick) 56 -0.0085 -0.0076 0.0009
565oC/5h + C1 (19 mm thick) 381 0.0043 -0.0019 0.0062
C3 (2.8 mm thick) 56 -0.0117 -0.0043 0.0074
* defined as bulk volume (V) to nitrocarburized volume (VN) ratio.
69
Table 5.3: C-ring’s Gap Width (GW) distortion results – Middle location
Heat C-ring V/VN GW distortion (mm), Location: Middle
error
595oC/4h + C1 (19 mm thick) 381 0.0033 -0.0076 0.0109
C3 (2.8 mm thick) 56 -- -0.0062 --
565oC/5h + C1 (19 mm thick) 381 -0.0002 -0.0073 0.0071
C3 (2.8 mm thick) 56 -- -0.0046 --
Table 5.4: C-ring’s Gap Width (GW) distortion results – Bottom location
Heat C-ring V/VN GW distortion (mm), Location: Bottom
error
595oC/4h + C1 (19 mm thick) 381 0.0055 -0.0089 0.0144
C3 (2.8 mm thick) 56 -0.0125 -0.0053 0.0072
565oC/5h + C1 (19 mm thick) 381 -0.0003 -0.0059 0.0056
C3 (2.8 mm thick) 56 -0.0124 -0.0038 0.0086
Figure 5.2 shows the measured and predicted gap width (GW) profiles for the
nitrocarburized Navy C-rings. In all three locations (top, middle and bottom), sample C2
70
exhibited highest GW distortion than C1 and C2 samples. The predicted GW distortion
was in better agreement with the measured GW distortion for sample C2 and C3.
0.015
565°C/5h Measured
GW distortion, mm 0.01 565°C/5h Predicted
595°C/4h Measured
0.005 595°C/4h Predicted
0
-0.005
-0.01
-0.015
-0.02
-0.025
C1 (19mm thick) C2 (10mm thick) C3 (2.8mm thick)
C-rings
(a)
0.015
565°C/5h Measured
GW distortion, mm
595°C/4h Measured
0
-0.005
-0.01
-0.015
-0.02
C-rings
(b)
0.015
565°C/5h Measured
GW distortion, mm
595°C/4h Measured
0
-0.005
-0.01
-0.015
-0.02
-0.025
C-rings
(c)
Figure 5.2: Measured and predicted gap width (GW) distortion profiles of Navy C-
rings ((a) top, (b) middle & (c) bottom locations).
71
The predicted GW distortion (top location) of sample C1 showed C-ring gap
contraction while the measured distortion showed gap expansion, leading to high error.
This could be due to the thickness (19mm) of sample C1. For thicker samples, the
distortion contribution due to bulk material (SAE 1010) will be higher than the distortion
contribution due to nitrocarburized layer.
The measured OD distortion slightly increased with an increase in process
temperature from 565oC to 595oC (see Fig. 5.3). A similar trend profile is observed for
the predicted OD distortion. Tables 5.5 and 5.6 lists the OD and ID distortion results
(measured & predicted) with the change in heat treatment and C-ring thicknesses. The
OD distortion for thicker samples (C1 and C2) resulted in high error, which is similar to
the GW distortion results. Figure 5.3 shows the OD distortion profile with the change in
C-ring thicknesses.
Table 5.5 Comparison of the measured Outer Diameter (OD) distortion with the
predicted OD distortion
Heat C-ring V/VN OD distortion (mm)
Treatment specimens ratio* Measured Predicted Absolute error
595oC/4h + C1 (19 mm thick) 381 0.0250 0.0088 0.0162
air cooling C2 (10 mm thick) 200 0.0235 0.0064 0.0171
C3 (2.8 mm thick) 56 0.0278 0.0184 0.0094
565oC/5h + C1 (19 mm thick) 381 0.0223 0.0042 0.0181
air cooling C2 (10 mm thick) 200 0.0224 0.0032 0.0192
C3 (2.8 mm thick) 56 0.0193 0.0016 0.0177
72
0.03
565C Measured 565C Predicted
OD distortion, mm
0.025
0.02
0.015
0.01
0.005
0
C1 (19mm) C2 (10mm) C3 (2.8mm)
C-rings
Figure 5.3: Outer Diameter (OD) distortion profile of Navy C-rings (measured and
predicted).
There seems to be some sort of uncertainty in the ID distortion of C3 (2.8 mm
thick). The error bar of C3 (see Fig. 5.4) is larger than its measured value. Nevertheless,
the ID distortion prediction follows similar trend of the measured distortion. The
experimental measurements for Navy C-rings have shown that the ID distortion decreases
with the decreasing C-ring thickness (from 19 to 2.8 mm). This trend is confirmed by the
numerically calculated distortions.
Table 5.6: Comparison of the measured Inner Diameter (ID) distortion with the
simulated results
Inner Diameter (ID) (mm)
FNC C-ring V/VN Measured Predicted Absolute
specimens ratio* Distortion Distortion error
595oC/4h + C1 (19 mm thick) 381 0.0067 0.0014 0.0053

air cooling C2 (10 mm thick) 200 0.0006 -0.0024 0.0030
C3 (2.8 mm thick) 56 -0.0049 -0.0002 0.0047
565oC/5h + C1 (19 mm thick) 381 0.0064 0.0010 0.0054
air cooling C2 (10 mm thick) 200 0.0004 -0.0016 0.002
C3 (2.8 mm thick) 56 -0.0025 -0.0002 0.0023
73
0.015
0.01 595C Measured 595C Predicted
ID distortion, mm
0.005
-0.005
-0.01
-0.015
C1 C2 C3
C-rings
Figure 5.4: Inner diameter (ID) distortion profile of Navy C-rings (measured and
predicted).
The Navy C-ring model results show that the distortion is affected by the
nitrocarburized surface (compound layer) and bulk (core material) modifications due to
heat treatment. The distortion in thinner samples (smaller V/VN ratio) are controlled by
the nitrocarburized layers whereas the distortion in thicker samples are controlled by the
bulk. As the FEM simulations of C-rings didn’t take into account of the bulk volume
modifications and diffusion zone, the simulated distortion for the thicker samples have
higher error values than the thinner sample.
5.2 Bulk Volume/Nitrocarburized Volume Ratio
The GW, ID and OD errors decrease with decrease in C-ring thickness (19 to 2.8
mm). Hence, the thickness of the Navy C-ring becomes an important factor when
comparing the C-ring distortion with the actual component (TC piston). Based on the
74
nitrocarburized volume (VN) and bulk volume (V) (SAE 1010 steel), an empirical ratio
(V/VN) was introduced to identify the effect of distortion on C-ring thickness. According
to the V/VN ratio, the samples were divided into two categories: nitrocarburized volume
dominant (C3 & TC) and bulk volume dominant (C1 & C2). Table 5.7 lists the V/VN
ratio of three Navy C-rings (C1, C2 and C3) and torque converter (TC) pistons.
The V/VN ratio comparisons of the C-ring helps to recognize the magnitude of
distortion contribution due to nitrocarburized layer and bulk material of thicker and
thinner samples. From the error values (see Figs. 5.5 & 5.6), it is clear that the V/VN ratio
of the C-ring should be lower than 100 to obtain precise distortion prediction. The bulk
volume dominant samples (C1 & C2) exhibited higher error than the nitrocarburized
surface dominant sample (C3). The decrease in V/VN ratio caused lower OD, ID and GW
distortions. The GW distortion values becomes more negative with the decrease in C-ring
thickness. Therefore, the reduction of V/VN ratio led to an overall gap width (GW)
shrinkage.
Table 5.7: V/VN ratio of Navy C-rings and TC pistons
Sample Name V/VN ratio

C1 381
C2 200
C3 56
TC 56
75
0.016 0.006
595C/4h 565C/5h 595C/4h 565C/5h
ID Absolute error, mm
GW (bottom) Absolute
0.014
0.005
0.012
0.004
error, mm
0.01
0.008 0.003
0.006 0.002
0.004
0.001
0.002
0 0
381 200 56 381 200 56
V/VN ratio V/VN ratio
Figure 5.5: V/VN ratio vs. absolute errors for GW & ID distortions of Navy C-rings.
0.025
595C/4h 565C/5h
OD Absolute error, mm
0.02
0.015
0.01
0.005
0
381 200 56
V/VN ratio
Figure 5.6: V/VN ratio vs. absolute errors for OD distortions of Navy C-rings.
5.3 Distortion results of torque converter (TC) pistons
The OD and ID distortions for the TC piston specimens (10 specimens/FNC) due
to nitrocarburizing treatments are listed in Table 5.8. The distortion values of the ten
specimens were averaged and reported as measured distortions.
The OD distortion results showed that the outer diameter of the torque converter
piston shrank by reducing the nitrocarburizing temperature from 595oC to 565oC.
However, the ID distortion results for both nitrocarburizing treatments showed ID
76
expansion, and the distortion was found to decrease with the decrease in nitrocarburizing
temperature (595oC to 565oC).
The ID distortion of TC pistons were an order of magnitude higher than the ID
distortion of C-rings (see Tables 5.6 and 5.7). The OD distortion of C-rings varied from
0.0193mm to 0.0278mm and the OD distortion for TC pistons are in the range of
-0.0202mm to 0.0301mm. The ID distortion results showed inner diameter expansion in
C-rings (except C3) and pistons. But the OD distortion results showed outer diameter
contraction in the TC pistons and expansion in C-rings. This clearly proves that the OD
distortion of C-rings behave differently than the TC pistons.
Table 5.8 compares the measured and predicted OD distortions for two FNC
treatments (595oC/4h + air cooling and 565oC/5h + air cooling). Although the predicted
OD and ID distortions underestimate their measured distortion values (Tables 5.9 &
5.10), a similar decreasing distortion trend (decline in measured distortion) was observed
for the predicted values with decrease in nitrocarburizing temperature.
77
Table 5.8: Experimental ID and OD distortions for nitrocarburized TC pistons
Gas ferritic nitrocarburizing, Gas ferritic nitrocarburizing,

595oC/4hrs + air cooling 565oC/5hrs + air cooling
Specimen OD ID OD ID
No. distortion, distortion, distortion, distortion,
mm mm mm mm
1 0.0382 0.0427 -0.0175 0.0318
2 0.0344 0.0417 -0.0281 0.0317
3 0.0317 0.0405 -0.0280 0.0341
4 0.0226 0.0412 -0.0270 0.0301
5 0.0314 0.0438 -0.0301 0.0335
6 0.0409 0.0403 -0.0236 0.0345
7 0.0251 0.0453 -0.0176 0.0336
8 0.0311 0.0414 -0.0095 0.0360
9 0.0264 0.0433 -0.0087 0.0349
10 0.0192 0.0440 -0.0119 0.0341
average 0.0301 0.0424 -0.0202 0.0334
The ID distortion error of TC pistons seems to drop with the decrease in
nitrocarburizing temperature (595 to 565oC) but contrasting results were obtained for the
OD distortion error. Similar error results were obtained for the C-ring sample C3 which
has the same thickness (2.8mm) as TC piston. Therefore, the dimensions of the
measuring tool (C-ring) play a significant role in relating the distortion results with an
actual component of interest (TC piston).
78
Table 5.9: Comparison of measured and predicted OD distortion of TC pistons
Sample FNC V/VN OD distortion, mm
ratio Measured Predicted Absolute
error
595oC/4h + air 56 0.0301 0.0120 0.0181
TC pistons cooling
565oC/5h + air 56 -0.0202 0.0100 0.0302
cooling
Table 5.10: Comparison of measured and predicted ID distortion of TC pistons

Sample FNC V/VN ID distortion, mm
ratio Measured Predicted Absolute
error
595oC/4h + air 56 0.0424 0.0025 0.0399
TC pistons cooling
565oC/5h + air 56 0.0334 0.0020 0.0314
cooling
79
CHAPTER 6 COMPOSITION-DEPTH PROFILE SIMULATION MODEL
The nitrogen composition-depth profiles of two heat treatment conditions (gas
FNC at 565oC/5hrs and vacuum FNC at 580oC/10hrs) were measured using electron
probe micro analyzer (Fig. 6.1).
9
580°C/10hrs experimental
8 565°C/5h experimental
Nitrogen composition, wt.%
7
6
5
4
3
2
1
0
0 200 400 600 800 1000 1200 1400
Figure 6.1: Experimental nitrogen profiles for vacuum nitrocarburized
(580oC/10hrs) and gas nitrocarburized (580oC/10hrs) TC piston samples.
6.1 Carbon and nitrogen composition-depth profile simulation
Fick’s second law of diffusion is the governing law of the evolution of the
nitrogen concentration during the ferritic nitrocarburizing process:
c   2c  2c  2c  D  c c c 
 D 2  2  2  +     (6.1)
t  x y z  c  x y z 
where c denotes the element composition, t is the diffusion time, D is the diffusion
coefficient, x, y and z are the spatial coordinates. In the considered system, the diffusion
coefficient is assumed constant (independent of element composition) within the same
80
𝜕𝐷
phase region (ε, γ’ and α) such that = 0. In addition, the thickness of the system (along
𝜕𝑐
𝜕2 𝑐 𝜕2 𝑐 𝜕2 𝑐
the x axis) is much smaller than any of the other two dimensions 𝜕𝑥 2 ≫ 𝜕𝑦 2 , 𝜕𝑧 2 .
Therefore, the final diffusion equation that was used to calculate the composition profile
is reduced to:
c  2c
D 2 (6.2)
t x
The composition-depth profile simulations are developed using MATLAB, in
which the governing partial differential equations are converted into a set of finite
difference equations. An explicit time integration scheme along with finite centered
difference discretization is used for solving the Equation (6.2) to calculate the nitrogen
composition-depth profile. The following boundary and initial conditions were applied to
the model:
c (x = 0, t) = 8 wt.% (6.3)
c (x = xn, t) = 8 wt.% (6.4)
c (x, 0) = 0 (6.5)
In the present work, xn = 0.0028 m (thickness of torque converter piston). The
simulation procedure takes part in the following manner. First, the initial composition of
nitrogen is stated explicitly. By utilizing the assigned diffusion coefficients and boundary
conditions, new concentration terms are then calculated based on the known ones.
Finally, growth of the phases and their contribution to distortion are predicted. N
composition-depth profiles for the nitrocarburized treatments were generated by
considering ε, γ′ and α as separate layers. Diffusion coefficients for nitrogen in ε, γ′ and
α, phases are given in Equations 6.6, 6.7 and 6.8 [71, 92, 93]:
81
 147600 
 
D N  0.227x104 e RT 
m2/s (6.6)
  73274  
  18.775 
'
D N e   RT  
m2/s (6.7)
 75150 
 8  RT 
D N  4.67x10 e m2/s (6.8)
where R = 8.32 J/mol K and T is the heat treatment temperature in Kelvin. The above
three equations ((6.6), (6.7) and (6.8)) were used in the numerical model to calculate the
nitrogen diffusivities. The developed model simulates the nitrogen composition-depth
profiles for samples subjected to ferritic nitrocarburizing (FNC) processes at 580oC/10hrs
and 565oC/5hrs (see Fig.6.2).
9
580C/10hrs computed
8
565C/5hrs computed
N2 composition, wt.%
7
6
5
4
3
2
1
0
0 300 600 900 1200 1500 1800 2100 2400 2700 3000
Distance from surface, µm
Figure 6.2: Simulated nitrogen composition-depth profiles
Distortion is predicted locally using the following relations:
Distortion due to γ′+N+C  ε phase transformation,
V '
Δlε  l (6.9)
V
Distortion due to α+N+C  γ′ phase transformation,
82
V '
Δlγ’  l ' (6.10)
V '
where Vε, and Vγ’ are the partial molar volumes of ε & γ′ phases; lε and lγ’ are the thickness
of ε and γ′ phases. ΔVε-γ’ and ΔVγ’-α are the change in partial molar volumes due to the
γ′ ε and α  γ′ phase transformations. From equations (6.9) and (6.10), it is clear that
the thickness of the nitrocarburized layer should be predicted first in order to find the
overall local distortion. The thickness of ε and γ′ phases can be predicted if the
composition of nitrogen in ε, γ′ and α phase regions are known. The threshold nitrogen
compositions required to induce the γ′  ε and α  γ′ phase transformations were taken
from the literature (see Table 6.1).
Table 6.1: Composition of nitrogen in ε, γ′ and α phases [94, 95]

Phases Nitrogen composition, wt.%
ε > 5.56
γ′ > 0.0876 and ≤ 5.56
α ≤ 0.0876
6.2 Microstructure of torque converter (TC) piston samples
Figures 6.3 and 6.4 shows the microstructure of SAE 1010 torque converter piston
sample after vacuum and gas ferritic nitrocarburizing (FNC) treatments. The ε compound
layer and ferrite grains containing γ′ precipitates in the diffusion zone were evident in the
micrographs. The micrographs were taken at a magnification of 200X, 500X and 1000X.
The compound layer has porous regions at the surface followed by a clean non-porous
region (near the compound layer/diffusion zone interface) (see Fig. 6.3(c)).
83
(a) (b)
(c)
subjected to vacuum ferritic nitrocarburizing at 580oC/10hrs.
(a) (b)
(c)
subjected to gas ferritic nitrocarburizing at 565oC/5hrs.
84
The compound layer of gas FNC TC piston sample revealed larger pores than the
vacuum FNC piston sample. These pores could affect the surface residual stresses. The
compound layer of the vacuum treated specimen was intact on the bulk material after
polishing. However, the compound layer of gas FNC piston specimen was irregular and
some regions were eaten away (probably due to nital etching).
6.3 Composition-depth profile results
Figure 6.5 presents the carbon composition profiles of SAE 1010 TC piston
specimens subjected to gas FNC and vacuum FNC treatments. At the surface, the gas
ferritic nitrocarburizing (FNC) treatment (565oC/5hrs) has a higher carbon wt. % than the
vacuum ferritic nitrocarburizing (FNC) treatment (580oC/10hrs).
2
Carbon composition, wt.%
1.5
0.5
0
0 200 400 600 800 1000 1200
Figure 6.5: Carbon composition depth profile of SAE 1010 steel TC pistons
measured using EPMA.
However, the vacuum FNC piston sample has a higher nitrogen wt. % than the
gas FNC treated piston (see Fig. 6.6). This observation shows that the nitrogen
penetration hinders the carbon penetration during FNC treatment. The predicted nitrogen
85
composition profiles were validated by the experimental nitrogen profiles in SAE 1010
torque converter (TC) pistons.
8 8
580C/10hrs simulation
580C/10hrs simulation

7 580C/10hrs experimental 7
580C/10hrs experimental
6 565C/5hrs simulation 6 565C/5hrs simulation
5 565C/5hrs experimental
5 565C/5hrs experimental
4 4
3 3
2 2
1 1
0 0
0 10 20 30 40 50 60 70 80 90 100 0 250 500 750 1000 1250 1500 1750 2000
Distance from surface, µm Distance from surface, µm
(a) (b)
Figure 6.6: Comparison of experimental and simulated nitrogen-profiling results of
SAE 1010 nitrocarburized TC pistons ((a) – at the surface, (b) overall).
Table 6.2 lists the predicted phase thicknesses and local distortions due to
nitrocarburized phases for the FNC treatments (565oC/5hrs and 580oC/10hrs). The phase
thicknesses were first calculated from the simulated N composition profiles using Table
6.1. Using the phase thickness values, the local distortion is then calculated using
Equations 6.9 & 6.10.
Table 6.2: Partial molar volume, predicted phase thickness and distortion
Partial Predicted phase Predicted local
molar ΔVε-γ’, ΔVγ’-α, thickness, µm distortion, µm
Phases volume, x10-6 x10-6 580oC/ 565oC/ 580oC/ 565oC/
x10-6 m3/mol m3/mol 10 hrs 5 hrs 10 hrs 5 hrs
3
m /mol
ε 8.37 16 10 0.29 0.18
γ’from diffusion zone 8.22 0.15 1.08 84 53 11.04 6.96
α 7.14
Total 11.33 7.14
86
The predicted distortion is found to be higher for 580oC/10hrs than 565oC/5hrs.
Similarly, the measured distortion for heat treatment (580oC/10hrs) is higher than
565oC/5hrs. Table 6.3 presents the measured ID and OD distortions of nitrocarburized
torque converter pistons.
Table 6.3: CMM measured distortion values of SAE 1010 torque converter piston
Heat Treatment CMM measured distortion
Inner diameter (ID), µm Outer diameter (OD), µm
Gas FNC 565oC/5 hrs 24.64 10.52
Vacuum FNC 580oC/10hrs 35.28 78.38
Although the predicted local distortion cannot really be compared to the inner
diameter and outer diameter distortions of TC piston, the local distortion due to ε and γ′
phases can be applied to any geometry (shape) whereas the global (experimental)
distortion (shown in Table 6.3) is applicable only to a specific geometry such as TC
piston.
6.4 Residual stress determination – 1-step nitrocarburizing
The conservation of linear momentum equation, neglecting body forces and
inertia forces, can be expressed as:
div 
ˆ 0 (6.11)
where ̂ is the Cauchy stress tensor.
  xx  yx zx 
 
div   xy  yy zy   0 (6.12)
 
  xz  yz zz 
87
For 1-dimensional stress state, equation (6.12) is reduced as:
 xx
0 (6.13)
x
Integrating the above equation yields:
xx  constant (6.14)
Equation (6.14) indicates that the residual stress is constant within a phase. The
residual stresses are predicted using the stress jump at the interface between the two
phases: see Equations 6.15 and 6.16 [96]:
4G
  '    '  M (6.15)
4
1  G  K
3
4G
 '     M (6.16)
4
1  G  K
3
where G is shear modulus, K is the compressibility, εε, εγ’ are the strains due to ε and γ′
phases and M is the molar fraction of the precipitates. The molar fraction (M) values are
taken from the literature [94]. The compressibility (K) and shear modulus (G) of γ′ are
0.00572 GPa-1 and 62.2 GPa [97, 98] respectively. The compressibility (K) and shear
modulus (G) of ε are 0.0065 GPa-1 (B=154 GPa; K=1/B) and 78 GPa [99, 100]
respectively.
The strain due to change in volume of the phases can be expressed as:
V '
 '  1 (6.17)
3 V '
 = 1 V '
(6.18)
3 V
Since for the bulk (α phase) σα = 0, equation (6.15) yields
88
Surface residual (tensile) stress for γ′-phase,  '  25.9 MPa (6.19)
Similarly for the ε phase,
4G
    '     M (6.20)
4
1  G  K
3
Surface residual (tensile) stress for ε-phase,   297.9 MPa (6.21)
Figure 6.7 shows the predicted residual stress distribution within the
nitrocarburized torque converter pistons. Nan et al. [16] have reported the residual stress
values of nitrocarburized pistons measured using X-ray diffraction (XRD) technique. The
residual stresses were measured at the lockup surface of the piston specimen. The
predicted stress value (σε) slightly overestimates the measured residual stress values (see
Table 6.4).
350
580C/10hrs
300 565C/5hrs
Residual stress, MPa
250
200
150
100
50
0
0 10 20 30 40 50 60 70 80 90 100 110 120
Figure 6.7: Predicted residual stress-depth profiles for FNC heat treatments
(580oC/10hrs and 565oC/5hrs).
The presence of porosity in the compound layer affects the residual stress
distribution. A heat treatment that produces more pores in the compound layer will have
89
less tensile stresses. The surface residual stress (tensile) could also be lowered by the
presence of γ′ phase in the compound layer (see section 6.5).
Table 6.4: Comparison of measured and predicted surface residual stresses of
nitrocarburized SAE 1010 torque converter pistons.
Surface residual stress

Heat treatment
Measured Predicted (MPa)
(MPa) ε γ’ sub-layer
Gas ferritic nitrocarburizing
268 ± 26 297.9 25.9
565oC/5hrs
Vacuum ferritic
263 ± 20 297.9 25.9
nitrocarburizing 580oC/10hrs
From Equations 6.15 and 6.16, it is clear that the residual stresses do not have
temperature dependence due to FNC treatments. Therefore, the predicted surface residual
stresses associated with the Gas FNC and vacuum FNC treatments remains the same.
6.5 N composition-depth profile model for two-step nitrocarburizing treatments
The microstructure of 1-step nitrocarburizing treatment produces a single phase
(ε-Fe2-3 (C, N)) compound layer and diffusion zone containing γ′ phase. The surface
residual stresses (tensile) for vacuum ferritic nitrocarburizing (580oC/10hrs) and gas
ferritic nitrocarburizing (565oC/5hrs) treatments were 263±20 MPa and 268±26 MPa
respectively [16]. In order to further reduce the tensile residual stresses and also to
improve the nitrocarburized surface quality, 2-step nitrocarburizing treatments are
introduced in this work. This 2-step treatment can potentially reduce the tensile stress at
the steel surface due to the additional γ′ phase (Fe4N). The phase sequence of the 2-step
nitrocarburizing treatment will be γ′ / ε / γ′diff.zone / α whereas the phase sequence of 1-step
90
nitrocarburizing is ε / γ′ / α. Based on the N profile model for the 1-step nitrocarburizing
process (refer to section 6.1), the nitrogen composition profiles of 12 different 2-step heat
treatment conditions are simulated in this study.
Table 6.5 lists the heat treatment conditions and nitrogen compositions modeled
to produce a two-phase (γ′ and ε) compound layer. The heat treatment conditions were
designed in four batches (ABC;DEF;GHI;JKL). In the first batch, the 1st step process
temperature was varied from 595oC to 565oC. Then the 2nd step process temperature was
raised by 50oC for heat treatments D, E and F. The 1st step nitrogen compositions of heat
treatments G, H and I was decreased from 8 to 7 wt. %. Finally, the process times were
increased from 3.6hrs to 10hrs and 1.4hrs to 2.7hrs for heat treatments J, K and L. The
parameters involved in heat treatments ‘A’ to ‘L’ were chosen to produce the same level
of distortion as 1-step nitrocarburizing but lowers the surface residual stresses.
The N compostion-depth profile simulation procedure for 2-step nitrocarburizing
treatment was performed in two stages. The first stage simulates the step 1 with a
nitrogen intake composition of 7 or 8 wt. % and the second stage reproduced the step 2
(Table 6.5) with a nitrogen composition of 3 wt. %. Fick’s second law of diffusion (Eqn.
(6.2)) was again used to calculate the composition-depth profiles using the explicit time
integration scheme with finite centered difference discretization.
91
Table 6.5: Simulated two step heat treatment conditions and N compositions
Heat Step Process Nitrogen composition

treatment number temperature/time (wt. %)
1 595oC/3.6hrs + 8%
A 2 427oC/1.4hrs 3%
1 580oC/3.6hrs + 8%
B 2 427oC/1.4hrs 3%
1 565oC/3.6hrs + 8%
C 2 427oC/1.4hrs 3%
1 595oC/3.6hrs + 8%
D 2 477oC/1.4hrs 3%
1 580oC/3.6hrs + 8%
E 2 477oC/1.4hrs 3%
1 565oC/3.6hrs + 8%
F 2 477oC/1.4hrs 3%
1 595oC/3.6hrs + 7%
G 2 427oC/1.4hrs 3%
1 580oC/3.6hrs + 7%
H 2 427oC/1.4hrs 3%
1 565oC/3.6hrs + 7%
I 2 427oC/1.4hrs 3%
1 595oC/10hrs + 8%
J 2 427oC/2.7hrs 3%
1 580oC/10hrs + 8%
K 2 427oC/2.7hrs 3%
1 565oC/10hrs + 8%
L 2 427oC/2.7hrs 3%
The following boundary and initial conditions were applied to the model: during
the first step nitrocarburizing treatment time (t1), the composition of nitrogen was applied
92
as c (x=0, t1) = 8 (wt. %). At the start of t2 (2nd step time) the N composition was
dropped to 3 (wt. %), so the N composition was given as c (x=0, t2) = 3 (wt. %).
Similarly, the other end of the specimen’s N compositions were expressed as: c (x=xn, t1)
= 8 wt. % (step 1), c (x=xn, t2) = 3 wt. % (step 2). The model was applied to SAE 1010
steel torque converter (TC) piston. The thickness of the SAE 1010 TC piston specimen
used was 0.0028m (xn). The initial composition of nitrogen in the bulk material is
considered to be zero such that c (x, 0) = 0.
In order to calculate the distortion due to γ′ and ε phases, the N composition-depth
profiles after 2-step treatments were divided into three separate regions (γ′+ε, γ′diff.zone and α
phases) using the threshold nitrogen compositions (see Table 6.1). The thickness of the γ′,
ε and γ′diff.zone phases were initially calculated from the N profiles and the distortion due to
γ′, ε and γ′diff.zone phases were then predicted (refer to Eqns. 6.22, 6.23 and 6.24) assuming
the following surface phase transformation sequence: α  γ′diff.zone ε  γ′.
6.5.1 Composition-depth profile results – varying the 1st step temperature
The simulated nitrogen composition profiles of the first heat treatment batch (A,
B and C) are shown in Figures 6.8, 6.9 and 6.10. A general decreasing nitrogen
penetration was observed with the decrease in 1st step temperature.
93
7.5
7 Heat treatment A: 595°C/3.6hrs+427°C/1.4hrs
6.5

6
5.5
5
4.5
4
3.5
3
2.5
2
1.5
1
0.5
0
0 4 8 12 16 20 24 28 32 36 40 44 48 52 56 60 64 68 72 76 80 84 88 92 96 100
Figure 6.8: Simulated nitrogen composition-depth profile due to 2-step
nitrocarburizing process ‘A’ (595oC / 3.6 hrs / 8% + 427oC / 1.4 hrs / 3%).
7.5
7 Heat treatment B: 580°C/3.6hrs+427°C/1.4hrs
6.5
6
5.5
5
4.5
4
3.5
3
2.5
2
1.5
1
0.5
0
0 4 8 12 16 20 24 28 32 36 40 44 48 52 56 60 64 68 72 76 80 84 88 92 96 100
nitrocarburizing process ‘B’ (580oC/3.6 hrs/8% + 427oC/1.4 hrs/3%).
94
7.5
7 Heat treatment C: 565°C/3.6hrs+427°C/1.4hrs

6.5
6
5.5
5
4.5
4
3.5
3
2.5
2
1.5
1
0.5
0
0 4 8 12 16 20 24 28 32 36 40 44 48 52 56 60 64 68 72 76 80 84 88 92 96 100
nitrocarburizing process ‘C’ (565oC / 3.6 hrs / 8% + 427oC / 1.4 hrs / 3%).
6.5.2 Composition-depth profile results – varying the 2nd step temperature
The heat treatment A and D have same 1st step process temperature but different
2nd step temperature. The nitrogen profile for heat treatment D (with higher 2nd step
temperature than B&E) predicted a thicker γ′-phase (purple dotted line) than the heat
treatment A (green dotted line) (see Fig. 6.11). However, the heat treatment A produced a
thicker ε-phase than heat treatment D.
7.5
7 Heat treatment A: 595°C/3.6hrs+427°C/1.4hrs
6.5
6 Heat treatment D: 595°C/3.6hrs+477°C/1.4hrs
5.5
5
4.5
4
3.5
3
2.5
2
1.5
1
0.5
0
0 4 8 12 16 20 24 28 32 36 40 44 48 52 56 60 64 68 72 76 80 84 88 92 96100
Figure 6.11: Predicted N composition-depth profiles for heat treatment ‘A’ and ‘D’
(595oC/3.6hrs/8wt.%+477oC/1.4hrs/3wt.%).
95
7.5
7 Heat treatment B: 580°C/3.6hrs+427°C/1.4hrs
6.5

Heat treatment E: 580°C/3.6hrs+477°C/1.4hrs
6
5.5
5
4.5
4
3.5
3
2.5
2
1.5
1
0.5
0
0 4 8 12 16 20 24 28 32 36 40 44 48 52 56 60 64 68 72 76 80 84 88 92 96 100
Figure 6.12: Predicted N composition-depth profile for heat treatment ‘B’ and ‘E’
(580oC/3.6hrs/8wt.%+477oC/1.4hrs/3wt.%).
Similar results were obtained for heat treatments B, E and C, F (Figs. 6.12 and
6.13). The higher 2nd step temperature in heat treatments E and F resulted in a thicker γ′-
phase and a thinner ε-phase than heat treatments B and C. The decrease in nitrogen wt. %
are similar for both the set of heat treatments.
7.5
7 Heat treatment C: 565°C/3.6hrs+427°C/1.4hrs
6.5 Heat treatment F: 565°C/3.6hrs+477°C/1.4hrs
6
5.5
5
4.5
4
3.5
3
2.5
2
1.5
1
0.5
0
0 4 8 12 16 20 24 28 32 36 40 44 48 52 56 60 64 68 72 76 80 84 88 92 96100
Figure 6.13: Predicted N composition-depth profile for heat treatment ‘C’ and ‘F’
(565oC/3.6hrs/8wt.%+477oC/1.4hrs/3wt.%).
96
6.5.3 Composition-depth profile results – varying the 1st step N wt. %
The third batch of heat treatments G, H and I involves changing the nitrogen
composition (from 8 to 7 wt. %) of the 1st step nitrocarburizing treatment. Decreasing the
N composition (from 8 to 7 wt. %) resulted in the smallest compound layer thickness
compared to the other heat treatments. The heat treatment I has the lowest γ′diff.zone
thickness in the diffusion zone; therefore it results in lower distortion than for heat
treatments G and H. Figures 6.14 (a & b) and 6.15 compare the simulated composition-
depth profiles for heat treatments G, H and I with A&D, B&E and C&F.
7.5
7 Heat treatment A:595°C/3.6hrs/8wt.%+427°C/1.4hrs/3wt.%
6.5 Heat treatment D:595°C/3.6hrs/8wt.%+477°C/1.4hrs/3wt.%

6 Heat treatment G:595°C/3.6hrs/7wt.%+427°C/1.4hrs/3wt.%
5.5
5
4.5
4
3.5
3
2.5
2
1.5
1
0.5
0
0 4 8 12 16 20 24 28 32 36 40 44 48 52 56 60 64 68 72 76 80 84 88 92 96100
(a)
7.5
7 Heat treatment B:580°C/3.6hrs/8wt.%+427°C/1.4hrs/3wt.%
6.5 Heat treatment E:580°C/3.6hrs/8wt.%+477°C/1.4hrs/3wt.%

6 Heat treatment H:580°C/3.6hrs/7wt.%+427°C/1.4hrs/3wt.%
5.5
5
4.5
4
3.5
3
2.5
2
1.5
1
0.5
0
0 4 8 12 16 20 24 28 32 36 40 44 48 52 56 60 64 68 72 76 80 84 88 92 96100
(b)
Figure 6.14: Predicted N composition-depth profiles for heat treatment ‘G’
(595oC/3.6hrs/7wt.%+427oC/1.4hrs/3wt.%) and heat treatment ‘H’
(580oC/3.6hrs/7wt.%+427oC/1.4hrs/3wt.%).
97
7.5
7 Heat treatment C:565°C/3.6hrs/8wt.%+427°C/1.4hrs/3wt.%
6.5 Heat treatment F:565°C/3.6hrs/8wt.%+477°C/1.4hrs/3wt.%
6 Heat treatment I:565°C/3.6hrs/7wt.%+427°C/1.4hrs/3wt.%

5.5
5
4.5
4
3.5
3
2.5
2
1.5
1
0.5
0
0 4 8 12 16 20 24 28 32 36 40 44 48 52 56 60 64 68 72 76 80 84 88 92 96100
Figure 6.15: Predicted N composition-depth profile for heat treatment ‘I’
(565oC/3.6hrs/7wt.%+427oC/1.4hrs/3wt.%).
6.5.4 Composition-depth profile results – increased process time
Due to longer process times, the nitrogen penetration from the atmosphere to the
steel surface was higher for last heat treatment batch J, K and L (see Figs. 6.16, 6.17 and
6.18). After reaching a peak composition in the compound layer region, the heat
treatments G, H and I (purple lines) have the highest nitrogen wt. % drop while the heat
treatments J, K and L exhibited lowest nitrogen wt. % drop. The decrease in nitrogen
intake (8 to 7wt. %) caused the lowest nitrogen penetration in the compound layer and
diffusion zone of G, H and I. The nitrogen rate of drop is therefore influenced by the
nitrogen intake (from 8 to 7 wt. %) and process times.
98
8
7.5 Heat treatment A: 595°C/3.6hrs/8wt.%+427°C/1.4hrs/3wt.%
7 Heat treatment D: 595°C/3.6hrs/8wt.%+477°C/1.4hrs/3wt.%
6.5 Heat treatment G: 595°C/3.6hrs/7wt.%+427°C/1.4hrs/3wt.%
Nitrogen composition, wt.% 6 Heat treatment J: 595°C/10hrs/7wt.%+427°C/2.7hrs/3wt.%
5.5
5
4.5
4
3.5
3
2.5
2
1.5
1
0.5
0
0 4 8 12 16 20 24 28 32 36 40 44 48 52 56 60 64 68 72 76 80 84 88 92 96100104108112116120
Figure 6.16: Predicted N composition-depth profile for heat treatment ‘J’
(595oC/10hrs/8wt.%+427oC/2.7hrs/3wt.%).
7.5
7 Heat treatment B: 580°C/3.6hrs/8wt.%+427°/1.4hrs/3wt.%
6.5 Heat treatment E: 580°C/3.6hrs/8wt.%+477°/1.4hrs/3wt.%
6 Heat treatment H: 580°C/3.6hrs/7wt.%+427°/1.4hrs/3wt.%
5.5 Heat treatment K: 580°C/10hrs/8wt.%+427°/2.7hrs/3wt.%

5
4.5
4
3.5
3
2.5
2
1.5
1
0.5
0
0 4 8 12 16 20 24 28 32 36 40 44 48 52 56 60 64 68 72 76 80 84 88 92 96 100
nitrocarburizing process (580oC/10hrs/8% + 427oC/2.7hrs/3%).
99
7.5
Heat treatment C: 565°C/3.6hrs/8wt.%+427°C/1.4hrs/3wt.%
7
Heat treatment F: 565°C/3.6hrs/8wt.%+477°C/1.4hrs/3wt.%
6.5 Heat treatment I: 565°C/3.6hrs/7wt.%+427°C/1.4hrs/3wt.%
6

Heat treatment L: 565°C/10hrs/8wt.%+427°C/2.7hrs/3wt.%
5.5
5
4.5
4
3.5
3
2.5
2
1.5
1
0.5
0
0 4 8 12 16 20 24 28 32 36 40 44 48 52 56 60 64 68 72 76 80 84 88 92 96100
nitrocarburizing process (565oC/10hrs/8% + 427oC/2.7hrs/3%).
The distortion due to the two-step nitrocarburizing treatments were predicted as follows:
Distortion due to α+N+Cγ’diff.zone phase transformation,
V '
Δlγ’ (in diff. zone)  l  'diff .zone (6.22)
V '
Distortion due to γ’ diff.zone+N+Cε phase transformation,
V '
Δlε  l (6.23)
V
Distortion due to ε+N+Cγ’ phase transformation,
V '
Δlγ’  l ' (6.24)
V '
100
where Vε, and Vγ’ are the partial molar volumes of ε & γ′ phases; lε and lγ’ are the thickness
of ε and γ′ phases. ΔVγ’-α, ΔVε-γ’, and ΔVγ’-ε are the change in partial molar volumes due
to α  γ′diff.zone, γ′diff.zone  ε and ε  γ′ phase transformations. The total distortion was
calculated by adding together all three distortions (Δlγ′, Δlε, and Δlγ′ (in diff. zone)).
Table 6.6 lists the predicted compound layer (CL) thicknesses and distortion due
to the CL (γ′+ε) & diffusion zone (γ′diff.zone). The results showed that the heat treatment J
(595oC/10hrs/8wt.%N+427oC/2.7hrs/3wt.%N) has the thickest compound layer whereas
the heat treatment I (565oC/3.6hrs/7wt.%N+427oC/1.4hrs/3wt.%N) has the thinnest
compound layer. The heat treatments C, F and I with low 1st step process temperature
resulted in minimum distortion. Heat treatments J, K and L, with longer nitrocarburizing
times, have the highest size distortion.
The local distortion due to γ′ in the 2-phase compound layer is almost constant for
all series of heat treatments except batch DEF. In the compound layer, the distortion due
to ε-phase was higher than the γ′ phase. The total distortion was mostly dominated by the
Δlγ′diff.zone, this could be due to a significant volumetric mismatch between the γ′diff.zone and α
phases in the diffusion zone.
101
Table 6.6: Predicted local distortions for two-step nitrocarburizing treatments
Heat Predicted phase thickness, µm Predicted local distortion, µm
treatment 2-phase CL (γ’+ε) 2-phase CL (γ’+ε)
lγ’ lε Total lγ’diff.zone Δlγ’ Δlε Δlγ’diff.zone Total
A 2 10 12 60 0.036 0.179 7.883 8.098
B 2 8 10 50 0.036 0.143 6.569 6.748
C 2 6 8 42 0.036 0.108 5.518 5.662
D 4 8 12 60 0.073 0.143 7.883 8.099
E 4 6 10 50 0.073 0.108 6.569 6.750
F 4 4 8 43 0.073 0.072 5.649 5.794
G 2 6 8 63 0.036 0.108 8.277 8.421
H 2 5 7 52 0.036 0.089 6.832 6.957
I 2 3 5 44 0.036 0.054 5.781 5.871
J 2 17 19 100 0.036 0.304 13.138 13.478
K 2 14 16 83 0.036 0.251 10.905 11.192
L 2 11 13 70 0.036 0.197 9.197 9.430
6.6 Residual stress determination – 2-step nitrocarburizing
The residual stress distribution for two-step nitrocarburizing treatment was
predicted in the same way as the residual stress distribution of 1-step nitrocarburizing
treatment (refer section 6.4), except an additional stress jump at the γ′/ε interface was
included in the calculation. The residual stress distribution was calculated according to
the model developed by Kolozsvary et al. [96]:
102
4G
  'diff .zone     '  M (6.25)
4
1  G  K
3
4G
 '     M (6.26)
4
1  G  K
3
4G
  '    '  M (6.27)
4
1  G  K
3
The residual stress within the compound layer is constant (Eqn. 6.14), similarly
the residual stress values do not vary for diffusion zone and bulk material. Since the
stress is zero for bulk phase (α), the residual stress for γ′diff.zone is initially calculated from
Equation 6.25. Using the γ′diff.zone stress, the residual stress due to ε-phase is then
calculated from Equation 6.26. The residual stress for γ′ is finally calculated from the
stress due to ε phase (Eqn. 6.27).
Two-step nitrocarburizing model results in lower surface (tensile) residual stress
when compared to the surface residual stress in single-step nitrocarburizing process. The
surface residual stress (γ′) was found to be 25.9 MPa and the residual stress of ε was
297.9 MPa. The residual stress for γ’diff.zone (in the diffusion zone) was 25.9 MPa. Figure
6.19 presents the residual stress distribution for 2-step nitrocarburizing treatments C, D
and J. The residual stress distribution changes with the change in compound layer
thicknesses but the pattern remains the same for all heat treatments.
103
350
Heat treatment J
300 Heat treatment D
Residual stress, MPa

250 Heat treatment C
200
150
100
50
0
0 20 40 60 80 100 120
Figure 6.19: Residual stress distribution due to 2-step nitrocarburizing
process.
104
CHAPTER 7 CONCLUSIONS AND FUTURE WORK
This dissertation presents the FEM simulation results for nitrocarburized Navy C-
rings and torque converter piston specimens. The study examined the effect of geometry,
heat treatment and nitrogen composition on the distortion of nitrocarburized SAE 1010
plain carbon steel. The developed FEM models can predict the small distortions
associated with the nitrocarburizing treatment.
Using finite difference method, N profile simulation models were then developed
for 1-step and 2-step nitrocarburizing treatments to calculate the local distortion due to
the ε and γ′ phases.
7.1 Conclusions
The following conclusions were drawn from this study:
• The microstructure for 1-step nitrocarburizing revealed a single phase compound
layer (ε) followed by diffusion zone containing γ′ and core material (phase
sequence: ε / γ′ / α). The microstructure of the nitrocarburized surface revealed
porosity in the compound layer. The residual stress of the ε-phase was reported to
be tensile for SAE 1010 Navy C-rings and torque converter piston specimens. The
FNC process should properly balance the surface residual stress and distortion so
that the surface characteristics remains unaltered with the heat treatment that
produces minimum distortion.
• The microstructure for 1-step nitrocarburizing also revealed porosity in the
compound layer. The porosity in the compound layer will also affect the surface
residual stresses.
105
• Coupled thermo-elastic FEM models were developed to predict the distortion in
C-rings and torque converter pistons. The computed values of ID, OD and GW
distortions underestimates the measured ID,OD and GW distortions of SAE 1010
C-rings and torque converter pistons.
• Based on the obtained distortions, the thickness of the C-ring probe becomes an
important factor in comparing the distortions in the C-rings with those in an actual
component (TC piston). For specimen C1 (19mm thick), the nitrocarburized layer
in the FEM model has no significant effect on distortion leading to high error.
One possible reason for this effect is the heat treatment induced bulk modification
along with the intended surface modification. For thinner samples like torque
converter (TC) piston and C3 (Navy C-ring) specimens, the model seems to
compare favorably with the measured values because the nitrocarburized volume
(smaller V/VN ratio) is dominant over the bulk material volume. The reduction of
the bulk volume to nitrocarburized volume (V/VN) ratio led to a decrease in ID &
GW distortion and an increase in OD distortion.
• The predicted error is high, because the diffusion zone and quantification of bulk
phases are not included in the FEM models of C-rings and TC pistons.
• The gap width (GW) distortion profiles of the C-rings were similar in both
experimental and numerical methods as the C-ring gap tends to contract after heat
treatment. The gap width of C2 specimen shrank more than C1 and C3 specimens.
By comparing the measured and predicted GW distortions (at three different
locations: top, middle, & bottom), it was found that the GW relative error varied
from 10% to 330%.
106
• The measured OD distortion of C-rings (OD expanded after FNC) behaved
differently than the TC pistons (OD contracted after FNC).
• Although the C-ring acts as a probe to examine the heat treatment stability, the
geometry of C-rings should be carefully selected to match the actual component
of interest for better distortion comparison.
• A composition-depth profile model was developed for predicting the local
distortion due to the ε, γ′ phases. The measured and predicted nitrogen
composition-depth profiles of torque converter pistons were successfully
validated. The measured distortions are calculated from the change in specimen
dimensions and are therefore restricted to a specific geometry. But the local
distortion, estimated from the composition profile model, is not restricted to any
particular material geometries such as C-rings or TC pistons. The local distortion
model also helped to better understand the distortion behavior caused by the
nitrocarburizing treatment.
• The residual stress distributions due to 1-step nitrocarburizing treatments were
successfully developed. Although the stress distributions slightly change with the
phase thickness values, the trend profile is similar for 580oC/10hrs and
565oC/5hrs FNC treatments. The predicted surface (tensile) residual stress
(σε =297.9 MPa) was found to be in close agreement with the experimentally
determined values (242-294 MPa).
• Using the composition-depth profile model, the nitrogen composition-depth
profiles for 2-step nitrocarburizing treatments were optimized to further reduce
the tensile stresses and distortion. The nitrogen composition range for 2-step
107
nitrocarburizing revealed a two-phase (γ′ and ε) region in the compound layer.
The predicted distortion results showed that the diffusion zone in nitrocarburized
plain carbon steels play a major role in minimizing distortion. This could be due
to a significant volumetric mismatch between the γ’diff.zone and α phases in the
diffusion zone. The predicted residual stress (tensile) distribution showed a
notable stress reduction at the surface due to an additional γ′ phase in the
compound layer, which in fact can result in better fatigue life.
7.2 Major advances
 Use of Navy C-rings: consideration of V/VN ratio with respect to the size of C-
ring and actual component.
 Two-step nitrocarburizing process to obtain γ′-Fe4N phase at the surface and
reduce tensile residual stress.
Potential routes for obtaining desired microstructure
 γ’ / ε / γ’diff.zone / α (2-step nitrocarburizing - present work).
 γ’ / ε / α (1-step nitriding) [101].
7.3 Suggestions for future work
1. In the present work, the heat transfer coefficient was assumed to not vary with
temperature. The change in heat transfer coefficient with temperature can be
estimated in future to improve the model predictions.
2. Experimental nitrogen composition-depth profiles for 2-step nitrocarburizing
treatments can be measured using EPMA to validate the N profile model for 2-
step treatments.
108
3. The effect of porosity on material properties (such as Young’s modulus) and
residual stress of the compound layer could be studied for different heat treatment
conditions.
4. The temperature effects on the material properties (such as E(T), σ(T)) could be
estimated to further refine the input data of the FEM models.
109
REFERENCES
[1] Burakowski, T., and Wierzchon, T., 1999, "Formation of technological surface
layers," in 'Surface engineering of metals: principles, equipment, technologies', CRC
Press LLC, Boca Raton, FL, pp. 235-251.
[2] Campagna, V., Bowers, R., Northwood, D. O., Sun, X., and Bauerle, P., 2011,
"Comparison of carbonitriding and nitrocarburising on size and shape distortion of plain
carbon SAE 1010 steel," Surface Engineering, 27(2), pp. 86-91.
[3] Sinha, A. K., 1991, "Defects and Distortion in Heat-Treated Parts," in 'ASM
Handbook', Vol.4, Heat Treating, ASM International, Materials Park, OH, pp. 601-619.
[4] Wolff, M., Böhm, M., Bökenheide, S., and Dalgiç, M., 2012, "Some recent
developments in modelling of heat-treatment phenomena in steel within the collaborative
research centre SFB 570 "distortion Engineering"," Materialwissenschaft und
Werkstofftechnik, 43(1-2), pp. 136-142.
[5] Simsir, C., 2014, "Modeling and simulation of steel heat treatment: prediction of
microstructure, distortion, residual stresses, and cracking," in 'ASM Handbook', Vol. 4B,
Steel Heat Treating Technologies, ASM International, Materials Park, OH, pp. 409-466.
[6] Epler, L. J., 2000, "Ferritic nitrocarburizing gears to increase wear resistance and
reduce distortion," Gear Technology, 17(2), pp. 24-25.
[7] Bell, T., 1976, "Ferritic nitrocarburizing," Metals Engineering Quarterly, 16(2), pp. 1-
13.
[8] Herring, D. H., Otto, F. J., and Specht, F. R., 2012, "Gear Materials and their Heat
Treatment," Industrial Heating, pp. 77-84.
110
[9] Leineweber, A., Gressmann, T., and Mittemeijer, E. J., 2012, "Simultaneous control
of the nitrogen and carbon activities during nitrocarburising of iron," Surface and
Coatings Technology, 206(11–12), pp. 2780-2791.
[10] Bell, T., Sun, Y., and Suhadi, A., "Environmental and technical aspects of plasma
nitrocarburising," Proc. Second International Symposium on Applied Plasma Science
(ISAPS'99), 20-24 Sept. 1999, Elsevier, pp. 14-23.
[11] Mittemeijer, E. J., 2013, "Fundamentals of nitriding and nitrocarburizing," ASM
Handbook, Volume 4A, Steel Heat Treating Fundamentals and Processes, J. Dossett, and
G. E. Totten, eds., ASM International, Materials Park, OH, pp. 619-646.
[12] Chen, W. L., Wu, C. L., Liu, Z. R., Ni, S., Hong, Y., Zhang, Y., and Chen, J. H.,
2013, "Phase transformations in the nitrocarburizing surface of carbon steels revisited by
microstructure and property characterizations," Acta Materialia, 61(11), pp. 3963-3972.
[13] Slycke, J., Sproge, L., and Agren, J., 1988, "Nitrocarburizing and the ternary Fe-N-C
phase diagram," Scandinavian Journal of Metallurgy, 17(3), pp. 122-126.
[14] Yang, M., and Sisson, R. D., 2013, "Gaseous nitriding process control: Application
of customised lehrer diagrams," International Heat Treatment and Surface Engineering,
7(4), pp. 164-171.
[15] Liapina, T., Leineweber, A., and Mittemeijer, E. J., 2003, "Nitrogen redistribution in
ε/γ′-iron nitride compound layers upon annealing," Scripta Materialia, 48(12), pp. 1643-
1648.
[16] Nan, C., 2009, "Ferritic nitrocarburizing process development for minimization of
distortion," M.A.Sc Thesis, Mechanical, Materials and Automotive Engineering
Department, University of Windsor, Windsor ON.
111
[17] Alsaran, A., and Çelik, A., 2001, "Structural characterization of ion-nitrided AISI
5140 low-alloy steel," Materials Characterization, 47(3-4), pp. 207-213.
[18] Fernandes, F. A. P., Neto, A. L., Oliveira, A. M., and Totten, G. E., 2008, "Stainless
steel property improvement by ion nitriding and nitrocarburizing," Heat Treating
Progress, ASM International, Materials Park, OH, p. 41.
[19] Cherian, K., 2006, "Microwave carburizing shows promise," Heat Treating Progress,
ASM International, Materials Park, OH, pp. 46-47.
[20] Pye, D., 2003, Practical nitriding and ferritic nitrocarburizing, ASM International,
Materials Park, OH, pp. 111-118.
[21] Aliev, A. A., 2004, "Updating of equipment for thermochemical treatment of steel
parts in a fluidized bed," Met Sci Heat Treat, 46(11-12), pp. 559-562.
[22] Schwartz, M., 2011, "New innovative heat treating processes," Manufacturing,
fabrication and environmental safety, Taylor & Francis Group, LLC, Boca Raton, FL, pp.
483-502.
[23] Boblet, J., Retrieved from http://www.durferrit.de/media/pdf/Tenifer_QPQ_eng.pdf
on April 10, 2015.
[24] Korwin, M. J., Morawski, C. D., Tymowski, G. J., and Liliental, W. K., 2004,
"Design of nitrided and nitrocarburized materials," Handbook of metallurgical process
design, G. E. Totten, K. Funatani, and L. Xie, eds., Marcel Dekker, Inc., NY, USA, pp.
545-590.
[25] Jordan, D., 2009, "Vacuum gas-nitriding furnace produces precision nitrided parts,"
Heat Treating Progress, ASM International, Materials Park, OH, pp. 45-48.
112
[26] Ericsson, T., 1987, "Residual stresses caused by thermal and thermochemical surface
treatments," Advances in Surface Treatments, A. Niku-Lari, ed., Pergamon Press,
Oxford, England, pp. 87-113.
[27] Somers, M. A. J., and Mittemeijer, E. J., 1990, "Development and relaxation of
stress in surface layers; composition and residual stress profiles in γ'-Fe4N1-x layers on
α-Fe substrates," Metallurgical Transactions A (Physical Metallurgy and Materials
Science), 21A(1), pp. 189-204.
[28] Nan, C., Northwood, D. O., Bowers, R. J., Sun, X., and Bauerle, P., 2009, "Residual
stresses and dimensional changes in ferritic nitrocarburized navy C-rings and prototype
stamped parts made from SAE 1010 steel," SAE International Journal of Materials and
Manufacturing, 2(1), pp. 219-233.
[29] Leskovšek, V., Podgornik, B., and Nolan, D., 2008, "Modelling of residual stress
profiles in plasma nitrided tool steel," Materials Characterization, 59(4), pp. 454-461.
[30] Watkins, T. R., England, R. D., Klepser, C., and Jayaraman, N., 2000,
"Measurement and analysis of residual stress in ε-phase iron nitride layers as a function
of depth," Advances in X-ray Analysis - 49th Denver X-ray Conference, JCPDS-
International Centre for Diffraction Data 2000, Denver, CO, pp. 31-38.
[31] Fares, M. L., Touhami, M. Z., Belaid, M., and Bruyas, H., 2009, "Surface
characteristics analysis of nitrocarburized (Tenifer) and carbonitrided industrial steel
AISIO2 types," Surface and Interface Analysis, 41(3), pp. 179-186.
[32] Thomas, D. H., and Bell, T., 1980, "Fatigue behaviour of aged gas-nitrocarburized
low-carbon steel," Metal Science, 14(2), pp. 73-78.
113
[33] Zoch, H. W., 2009, "Distortion engineering: vision or ready to application?,"
Materialwissenschaft und Werkstofftechnik, 40(5-6), pp. 342-348.
[34] Zoch, H. W., 2012, "Distortion engineering - Interim results after one decade
research within the Collaborative Research Center," Materialwissenschaft und
Werkstofftechnik, 43(1-2), pp. 9-15.
[35] Holly, M. L., Devoe, L., and Webster, J., 2011, "Ferritic nitrocarburized brake
rotors," SAE 2011 World Congress & Exhibition ,New York.
[36] Brinksmeier, E., Sölter, J., and Grate, C., 2007, "Distortion engineering -
identification of causes for dimensional and form deviations of bearing rings," CIRP
Annals - Manufacturing Technology, 56(1), pp. 109-112.
[37] French, H. J., 1930, "A study of the quenching of the steels," Transactions of the
American Society for Steel Treating, 17(6), pp. 798-888.
[38] Webster, H., and Laird, W. J., 1991, "Martempering of steel," in 'ASM Handbook',
Vol. 4, Heat Treating, ASM International, Materials Park, OH, pp. 137-151.
[39] Leskovsek, V., Licic, B., and Ule, B., "Some aspects of sub-zero tempering at
vacuum heat-treatment of hss," Proc. Heat Treating: Proceedings of the 21st Conference,
November 5, 2001 - November 8, 2001, ASM International, pp. 25-31.
[40] Bates, C. E., Totten, G. E., and Brennan, R. L., 1991, "Quenching of steel," in 'ASM
Handbook', Vol. 4, Heat Treating, ASM International, Materials Park, OH, pp. 67-120.
[41] Leskovsek, V., and Ule, B., 2002, "Influence of deep cryogenic treatment on
microstructure, mechanical properties and dimensional changes of vacuum heat-treated
high-speed steel," Heat Treatment of Metals, 29(3), pp. 72-76.
114
[42] Nan, C., Northwood, D. O., Bowers, R. J., and Sun, X., 2010, "Study on the
dimensional changes and residual stresses in carbonitrided and ferritic nitrocarburized
SAE 1010 plain carbon steel," Materials Science Forum, pp. 829-834.
[43] Nan, C., Northwood, D. O., Bowers, R. J., and Sun, X., "Distortion in ferritic
nitrocarburized SAE 1010 plain carbon steel," Proc. SEM Annual Conference and
Exposition on Experimental and Applied Mechanics 2009, pp. 1630-1638.
[44] Nan, C., Northwood, D. O., Bowers, R. J., Sun, X., and Bauerle, P., "The use of
navy C-ring specimens to study distortion in ferritic nitrocarburized 1010 steel," Proc. 9th
International Conference on Surface Effects and Contact Mechanics - Computational
Methods and Experiments, Contact/Surface 2009, Algarve, 62, pp. 13-25.
[45] Leskovsek, V., 1999, "Optimisation of the vacuum heat treatment of high-speed
steels," PhD dissertation, University of Zagreb, Zagreb, Croatia.
[46] Campagna, V., Bowers, R., Northwood, D. O., Sun, X., and Bauerle, P., "The
nitrocarburizing of plain carbon steel automotive components," Proc. 24th ASM
International Heat Treating Conference and Exposition, pp. 239-244.
[47] Northwood, D. O., He, L., Boyle, E., and Bowers, R., 2007, "Retained austenite -
Residual stress - Distortion relationships in carburized SAE 8620 steel," Materials
Science Forum, 539-543, pp. 4464-4469.
[48] Boyle, E., Bowers, R., and Northwood, D. O., "The use of navy C-ring specimens to
investigate the effects of initial microstructure and heat treatment on the residual stress,
retained austenite, and distortion of carburized automotive steels," Proc. 2007 World
Congress, April 16, 2007 - April 19, 2007, SAE International, pp. 31-39.
115
[49] Clark, A., Bowers, R. J., and Northwood, D. O., 2014, "Heat treatment effects on
distortion, residual stress, and retained austenite in carburized 4320 steel," Materials
Science Forum, 783-786, pp. 692-697.
[50] Campagna, V., Northwood, D. O., Bowers, R., Sun, X., and Bauerle, P., 2009, "The
analysis and control of distortion in carbonitrided and nitrocarburized thin-shelled plain
carbon steel automotive powert rain components," Journal of ASTM International, 6(3),
pp. 1-17.
[51] Boyle, E., Northwood, D. O., Bowers, R., Sun, X., and Bauerle, P., 2009,
"Microstructural effects on residual stress, retained austenite, and case depth of
carburized automotive steels," SAE International Journal of Materials and
Manufacturing, 1(1), pp. 697-708.
[52] Kurowski, P., 1994, "Avoiding pitfalls in FEA," Machine Design, pp. 78-86.
[53] Inoue, T., and Tanaka, K., 1975, "An elastic-plastic stress analysis of quenching
when considering a transformation," International Journal of Mechanical Sciences, 17(5),
pp. 361-367.
[54] Inoue, T., Arimoto, K., and Ju, D. Y., 1991, 3rd International Conference on
'Residual Stresses', Society of Materials Science, Tokushima, Japan, pp. 226-231.
[55] Inoue, T., 1996, "Metallo-thermo-mechanics: application to phase transformation
incorporated processes," Transactions of Joining and Welding Research Institute, 25, pp.
69-87.
[56] Inoue, T., and Arimoto, K., 1995, "Implementation of program for simulating heat
treatment processes and some results," Industrial Heating, 62(4), pp. 41-45.
116
[57] Inoue, T., and Arimoto, K., 1997, "Development and implementation of CAE system
`HEARTS' for heat treatment simulation based on metallo-thermo-mechanics," Journal of
Materials Engineering and Performance, 6(1), pp. 51-60.
[58] Thuvander, A., 2002, "Numerical simulation of gas quenching of tool steels and the
influence of hardenability on distortion," 6th International Tooling Conference,Karlstad,
Sweden, pp. 625-642.
[59] Thuvander, A., 1996, "Calculation of distortion of tool steel dies during hardening,"
Proceedings of the 2nd International Conference on Quenching and Control of Distortion,
ASM International,Cleveland, Ohio, USA, pp. 297-303.
[60] da Silva, A. D., Pedrosa, T. A., Gonzalez-Mendez, J. L., Jiang, X., Cetlin, P. R., and
Altan, T., 2012, "Distortion in quenching an AISI 4140 C-ring – Predictions and
experiments," Materials & Design, 42(0), pp. 55-61.
[61] Hernández-Morales, B., Barba-Méndez, O., Ingalls-Cruz, A., and Barrera-Godínez,
J. A., 2005, "Mathematical modelling of temperature and stress evolution during cooling
of a stainless steel Navy C-ring probe," International Journal of Materials and Product
Technology, 24(1-4), pp. 306-318.
[62] Li, Z., Lynn Ferguson, B., Sun, X., and Bauerle, P., "Experiment and simulation of
heat treatment results of C-Ring test specimen," Proc. ASM Proceedings: Heat Treating,
2006, pp. 245-252.
[63] Nicolas, C., Baudouin, C., Leleu, S., Teodorescu, M., and Bigot, R., 2008,
"Dimensional control strategy and products distortions identification," International
Journal of Material Forming, 1(1), pp. 1039-1042.
117
[64] Freborg, A., Ferguson, B., and Li, Z., "Predicting distortion and residual stress in a
vacuum carburized and gas quenched steel coupon," Proc. Quenching Control and
Distortion - Proceedings of the 6th International Quenching and Control of Distortion
Conference, Including the 4th International Distortion Engineering Conference, 2012, pp.
22-33.
[65] Li, Z., Ferguson, B. L., and Freborg, A., "Modeling application to reduce distortion
of a carburized and quenched steel gear," Proc. Quenching Control and Distortion -
Proceedings of the 6th International Quenching and Control of Distortion Conference,
Including the 4th International Distortion Engineering Conference, 2012, pp. 200-211.
[66] Depouhon, P., Sprauel, J. M., Mailh, M., and Mermoz, E., 2015, "Modeling of
distortions induced by the nitriding process," Mechanics and Industry, 16(1).
[67] Mukai, R., Matsumoto, T., Ju, D. Y., Suzuki, T., Saito, H., and Ito, Y., 2006,
"Modeling of numerical simulation and experimental verification for carburizing-
nitriding quenching process," Transactions of Nonferrous Metals Society of China
(English Edition), 16(SUPPL.), pp. s566-s571.
[68] Du, H., Somers, M. A. J., and Ågren, J., 2000, "Microstructural and compositional
evolution of compound layers during gaseous nitrocarburizing," Metallurgical and
Materials Transactions A: Physical Metallurgy and Materials Science, 31(1), pp. 195-
211.
[69] Gräfen, W., and Edenhofer, B., 2005, "New developments in thermo-chemical
diffusion processes," Surface and Coatings Technology, 200(5–6), pp. 1830-1836.
[70] Yang, M., and Sisson Jr, R. D., 2012, "Modeling the nitriding process of steels,"
Advanced Materials and Processes, 170(7), pp. 33-36.
118
[71] Keddam, M., 2007, "Surface modification of the pure iron by the pulse plasma
nitriding: Application of a kinetic model," Materials Science and Engineering: A, 462(1–
2), pp. 169-173.
[72] Yan, M., Yan, J., and Bell, T., 2000, "Numerical simulation of nitrided layer growth
and nitrogen distribution in ε-Fe 2-3 N, γ'-Fe 4 N and α-Fe during pulse plasma nitriding
of pure iron," Modelling and Simulation in Materials Science and Engineering, 8(4), pp.
491-496.
[73] Gu, X., Michal, G. M., Ernst, F., Kahn, H., and Heuer, A. H., 2014, "Numerical
simulations of carbon and nitrogen composition-depth profiles in nitrocarburized
austenitic stainless steels," Metallurgical and Materials Transactions A: Physical
Metallurgy and Materials Science, 45(10), pp. 4268-4279.
[74] Ozisik, M. N., 1994, Finite difference methods in heat transfer, CRC Press LLC,
Boca Raton, FL, pp. 118-120.
[75] Fausett, L. V., 2008, Applied numerical analysis using MATLAB, Pearson
Education, Inc., Upper Saddle River, NJ, pp. 608-610.
[76] Moskalioviene, T., Galdikas, A., Riviere, J. P., and Pichon, L., 2011, "Modeling of
nitrogen penetration in polycrystalline AISI 316L austenitic stainless steel during plasma
nitriding," Surface and Coatings Technology, 205(10), pp. 3301-3306.
[77] Torres, J. L., Chuzhoy, L., Burns, K. W., Meng, C., Krzyaniak, B., Horrocks, S., and
El-Darazi, D., "Ferritic nitro-carburizing of ductile iron parts," Proc. International Surface
Engineering Congress - Proceedings of the 1st Congress, pp. 75-79.
119
[78] Depouhon, P., Sprauel, J. M., Mailhé, M., and Mermoz, E., 2014, "Mathematical
modeling of residual stresses and distortions induced by gas nitriding of 32CrMoV13
steel," Computational Materials Science, 82(0), pp. 178-190.
[79] Prantil, V. C., Callabresi, M. L., Lathrop, J. F., Ramaswamy, G. S., and Lusk, M. T.,
2003, "Simulating distortion and residual stresses in carburized thin strips," Journal of
Engineering Materials and Technology, Transactions of the ASME, 125(2), pp. 116-124.
[80] Larson, D., 1990, "Finite element analysis of residual stress and distortion in forged
and carburized gear steel," M.S Thesis T-3932, Colorado School of Mines, Golden, CO.
[81] Kurz, S. J. B., Meka, S. R., Schell, N., Ecker, W., Keckes, J., and Mittemeijer, E. J.,
2015, "Residual stress and microstructure depth gradients in nitrided iron-based alloys
revealed by dynamical cross-sectional transmission X-ray microdiffraction," Acta
Materialia, 87, pp. 100-110.
[82] Nan, C., Northwood, D. O., Sun, X., and Bauerle, P., 2008, "TMP Current 254 mm
45 RFE T/C Piston Production Report," University of Windsor, Windsor, ON, pp. 1-12.
[83] Boyle, E., 2007, "Microstructural effects on the mechanical properties of carburized
low-alloy steels," M.A.Sc Thesis, Mechanical, Automotive and Materials Engineering
Department, University of Windsor, Windsor ON.
[84] Retrieved from http://www.es.utoronto.ca/microprobe on March 27, 2015.
[85] Stringfellow, R., 1995, "Prediction and control of heat treat distortion of helicopter
gears (final report)," Aviation Applied Technology Directorate, Fort Eustis, VA, p. 192.
[86] Rothman, M. F., 1988, "High-Temperature Property Data: Ferrous Alloys," ASM
International, Materials Park, OH, pp. 2.7-2.8.
120
[87] Somers, M. A. J., van der Pers, N. M., Schalkoord, D., and Mittemeijer, E. J., 1989,
"Dependence of the lattice parameter of γ' iron nitride, Fe4N1-x, on nitrogen content;
accuracy of the nitrogen absorption data," Metallurgical Transactions A (Physical
Metallurgy and Materials Science), 20A(8), pp. 1533-1539.
[88] Lyman, T., Boyer, H. E., Unterweiser, P. M., Hontas, J. P., Mehlman, L. R., Carnes,
W. J., and Lawton, H., 1964, Metals Handbook, American Society for Metals, Metals
Park, OH, 2, pp. 52-55.
[89] Franssen, J. M., and Real, P. V., 2010, "Fire design of steel structures," Wiley-VCH
GmbH & Co. KGaA, Weinheim, Germany, p.452.
[90] Bauccio, M., Harvey, P. D., Boyer, H. E., and Giancoli, D. C., 1993, "AISI 1010
steel, cold drawn bar, 19-32mm round or thickness," Retrieved from
http://www.matweb.com/search/datasheet.aspx?MatGUID=4b64586941754ec2a4a8ef0fd
e2299db on May 20, 2015.
[91] "Young's modulus of elasticity for metals and alloys," Retrieved from
http://www.engineeringtoolbox.com/young-modulus-d_773.html on May 20, 2015.
[92] Lakhtin, Y. M., and Kogan, Y. D., 1976, Nitriding of Steel, Mashinostroenie,
Moscow.
[93] Campos, I., Torres, R., Bautista, O., Ramírez, G., and Zuñiga, L., 2005, "Evaluation
of the diffusion coefficient of nitrogen in Fe4N1−x nitride layers during microwave post-
discharge nitriding," Applied Surface Science, 249(1–4), pp. 54-59.
[94] Du, H., and ågren, J., 1996, "Theoretical treatment of nitriding and nitrocarburizing
of iron," Metall and Mat Trans A, 27(4), pp. 1073-1080.
121
[95] Jordan, D., 2010, "Controlling compound (white) layer formation during vacuum gas
nitriding," Retrieved from http://solaratm.com/white-layer-formation-paper.pdf on April
09, 2015.
[96] Kolozsvary, Z., Plasmaterm, S. C., and Mures-Tg, 2002, "Residual stresses in
nitriding," Handbook of residual stress and deformation of steel, G. E. Totten, M. Howes,
and T. Inoue, eds., ASM International, Materials Park, Ohio, USA, pp. 209-219.
[97] Kong, Y., Diao, X., Yang, J., and Li, F., 1997, "Evaluation of the compressibility of
iron-nickel nitrides," Journal of Magnetism and Magnetic Materials, 172(1–2), pp. L15-
L18.
[98] Gressmann, T., 2007, "Fe-C and Fe-N compound layer: growth kinetics and
microstructure," PhD dissertation, Max Planck Institute for Metals Research, Institute for
Materials Science, University of Stuttgart, Germany.
[99] Yin, W., Lei, L., Jiang, X., Liu, P., Liu, F., Li, Y., Peng, F., and He, D., 2014, "High
pressure synthesis and properties studies on spherical bulk ε-Fe3N," High Pressure
Research, 34(3), pp. 317-326.
[100] Niewa, R., Rau, D., Wosylus, A., Meier, K., Hanfland, M., Wessel, M.,
Dronskowski, R., Dzivenko, D. A., Riedel, R., and Schwarz, U., 2009, "High-pressure,
high-temperature single-crystal growth, ab initio electronic structure calculations, and
equation of state of ε-Fe3N1+x," Chemistry of Materials, 21(2), pp. 392-398.
[101] Maeda, S., Kobayashi, A., Shimizu, Y., Kanayama, M., Yuya, M., and Imataka, H.,
2015, "Development of γ′-Fe4N Phase Control Technology and Low-Carbon Alloy Steel
for High-Strength Nitrided Gear," SAE International Journal of Materials and
Manufacturing, 8(3), pp. doi:10.4271/2015-4201-0519.
122
PUBLICATIONS
1. Manivannan, M., Stoilov, V., and Northwood, D.O., 2015, “Ferritic
nitrocarburizing of SAE 1010 plain carbon steel parts,” SAE International Journal
of Materials and Manufacturing, 8(2), 482-486.
2. Manivannan, M., Stoilov, V., and Northwood, D.O., 2015, “Numerical model of
the ferritic nitrocarburizing of SAE 1010 plain carbon steel,” European
Conference on Heat Treatment 2015 & 22nd IFHTSE Congress, May 20-22, 2015,
Venice, Italy (accepted for presentation).
3. Manivannan, M., Northwood, D.O., and Stoilov, V., 2014, “Use of Navy C-rings
to study and predict distortion in heat treated components: experimental
measurements and computer modelling,” International Heat Treatment and
Surface Engineering, 8(4), 168-175.
4. Manivannan, M., Stoilov, V., and Northwood, D.O., 2014, “Finite element
simulations of geometric distortions in ferritic nitrocarburized SAE 1010 plain
carbon steel,” Proceedings of the 5th International Conference on Thermal Process
Modeling and Computer Simulation,” 139-144, June 16, 2014, Orlando, FL,
USA.
123
APPENDICES
Appendix A
An explicit time integration scheme was used to solve the finite difference simulations
involving the one-dimensional diffusion equation for 1-step and 2-step ferritic
nitrocarburizing treatments in TC pistons.
A.1 MATLAB program files for a single-step nitrocarburizing treatment
function [x,z]=heat(T,n,m,L)
h=L/n;
k=T/m;
x=0:h:L;
t=0:k:T;
u(1:n+1,1)=fx(x)'; % initial condition
u(1,1:m+1)=g0(t);
u(n+1,1:m+1)=g1(t); % boundary conditions
for j=1:m
c=Dcoef(u,j);
r=c*k/h^2;
s=1-2*r;
r1=r(1:n-1);
r2=r(3:n+1);
s1=s(2:n);
u(2:n,j+1)=r1.*u(1:n-1,j)+s1.*u(2:n,j)+r2.*u(3:n+1,j);
end
z=u;
% boundary conditions
function g=g1(t)
124
g=8;
end
function g=g0(t)
g=8;
end
% initial condition (N composition)

function f=fx(x)
f=0;
end
% calculation of N diffusivities
function c=Dcoef(u_conc,n)
[m,k]=size(u_conc);
c=zeros(m,1);
T=838.15;
for(i=1:m)
if(u_conc(i,n)>=0)
if(u_conc(i,n)<=8)
c(i)=0.227e-4*exp(-147600/(8.32*T));
elseif(u_conc(i,n)<=5.56)
c(i)=exp((-73274/(8.32*T))-18.775);
c(i)=4.67e-8*exp(-75150/(8.32*T));
end % if
end % if
end %for loop
end %function Dcoef
end
125
% Running the heat function file
clc;
n=300;m=8000;T=18000;L=0.0028;
[x1,z1]=heat(T,n,m,L)
where n and m represents the total number of spatial and time subdivisions, L
represents the thickness of the torque converter piston and T (in the ‘heat’ file)
denotes the total heat treatment time.
A.2 MATLAB program files for a two-step nitrocarburizing treatment
The MATLAB program files of 1-step nitrocarburizing treatment were modified
to solve the nitrogen composition-depth profile in 2-step nitrocarburizing
treatments:
function [distr]=heat_new(t1,T1,T2)
n=2500;
m=8000;
L=0.0028;
Ttime=45720;
h=L/n;
k=Ttime/m;
x=0:h:L;
t=0:k:Ttime;
u(1:n+1,1)=fx(x)'; % initial condition
u(1,1:m+1)=g0(t,t1);
u(n+1,1:m+1)=g1(t,t1); % boundary conditions
for j=1:m
c=Dcoef_new(u,j,k,t1,T1,T2);
126
r=c*k/h^2;
s=1-2*r;
r1=r(1:n-1);
r2=r(3:n+1);
s1=s(2:n);
u(2:n,j+1)=r1.*u(1:n-1,j)+s1.*u(2:n,j)+r2.*u(3:n+1,j);
end
z=u;
% Nitrogen composition (wt. %) input at one end of the TC specimen

function g=g1(t,t1)
m=length(t);
for(i=1:m)
if(t(i)<=t1)
g(i)=8;
else
g(i)=3;
end
end
% Nitrogen composition (wt. %) input at the other end of the TC specimen

function g=g0(t,t1)
m=length(t);
for(i=1:m)
if(t(i)<=t1)
g(i)=8;
else
g(i)=3;
end
127
end
% Initial composition (wt. %) of nitrogen in the bulk

function f=fx(x)
f=0;
% Nitrogen diffusion coefficients

function c=Dcoef_new(u_conc,n,k,t1,T1,T2)
[m,kk]=size(u_conc);
c=zeros(m,1);
if(n*k<t1)
T=T1;
else
T=T2;
end
for(i=1:m)
if(u_conc(i,n)>=0)
if(u_conc(i,n)<=8)
c(i)=0.227e-4*exp(-147600/(8.32*T));
c(i)=exp((-73274/(8.32*T))-18.775);
c(i)=4.67e-8*exp(-75150/(8.32*T));
end
end
end
% Running the heat_new function file

clc;
128
t1=36000;T1=868.15;T2=700.15;
[distortion]=heat_new(t1,T1,T2)
The heat treatment temperature was reported in Kelvin, where T1 represents the
1-step heat treatment temperature & T2 represents the second step temperature
and the heat treatment time was used in seconds (Ttime). The nitrogen
composition was used in wt. %.
129
VITA AUCTORIS
NAME: Madhavan Manivannan
PLACE OF BIRTH: Chennai, India
YEAR OF BIRTH: 1985
EDUCATION: Anna University, B. Tech., (Chemical &
Electrochemical Engineering) Chennai, India,
2002-2006
University of Windsor, M.A.Sc., (Engineering
Materials) Windsor, ON, 2007-2009
University of Windsor, PhD., (Engineering
Materials) Windsor, ON, 2010-2015
130

Ferritic Nitrocarburizing of Plain Carbon Steels: Scholarship at Uwindsor

Uploaded by

Copyright:

Available Formats

Ferritic Nitrocarburizing of Plain Carbon Steels: Scholarship at Uwindsor

Uploaded by

Document Information

Original Description:

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Ferritic Nitrocarburizing of Plain Carbon Steels: Scholarship at Uwindsor

Uploaded by

Copyright:

Available Formats

University of Windsor

Ferritic Nitrocarburizing of Plain Carbon Steels

Follow this and additional works at: http://scholar.uwindsor.ca/etd

Windsor, Ontario, Canada

© 2015 Madhavan Manivannan

13th May 2015

published/submitted for publication in peer reviewed journals, as follows:

Dissertation Publication title/full citation Publication status

Finite Element Simulations of Geometric

acknowledged the contribution of other researchers to my dissertation, and have obtained

which it refers, is the product of my own work.

describes work completed during my registration as graduate student at the University of

dissertation, published or otherwise, are fully acknowledged in accordance with the

owner(s) to include such material(s) in my dissertation.

Nitrocarburizing is a case hardening process which improves the hardness and

wear resistance of a component, but results in geometric distortions. Torque converter

effect of nitrocarburizing process on distortions. For thinner specimens, the predicted

comparison of the C-ring size with the actual component.

The reduction of bulk volume to nitrocarburized volume (V/VN) ratio led to a

small increase in outer diameter (OD) distortion.

A composition-depth profile simulation model was also developed to predict the

residual stress was further reduced by introducing 2-step nitrocarburizing treatments.

distortion as 1-step nitrocarburizing treatments. Therefore, the proposed 2-step

This dissertation is dedicated to my family

Canada (NSERC), the Queen Elizabeth II Graduate Scholarship in Science and

DECLARATION OF CO-AUTHORSHIP / PREVIOUS PUBLICATION .............. III

LIST OF TABLES ....................................................................................................... XIV

LIST OF FIGURES ..................................................................................................... XVI

LIST OF APPENDICES .......................................................................................... XXIV

LIST OF ABBREVIATIONS/SYMBOLS................................................................ XXV

NOMENCLATURE .................................................................................................. XXVI

CHAPTER 1 INTRODUCTION ......................................................................................1

1.1 Research Objectives and Approach ............................................................................3

1.2 Dissertation Outline ....................................................................................................3

CHAPTER 2 LITERATURE REVIEW ..........................................................................5

2.1 Ferritic Nitrocarburizing (FNC).................................................................................5

2.1.1 Ion or plasma nitrocarburizing ...........................................................................9

2.1.2 Fluidized bed nitrocarburizing ..........................................................................10

2.1.3 Salt bath nitrocarburizing .................................................................................11

2.1.4 Gas nitrocarburizing .........................................................................................13

2.2 Residual stress ..........................................................................................................15

2.3 Distortion ..................................................................................................................19

2.3.1 Distortion prevention methods ..........................................................................22

2.4 Types and use of Navy C-rings .................................................................................23

2.5 Modeling ...................................................................................................................27

2.5.1 Distortion modeling ...........................................................................................30

2.5.2 Composition-Depth profiles: experimental and modeling ................................37

2.5.3 Residual Stress Modeling ..................................................................................43

CHAPTER 3 ANALYTICAL APPROACH .................................................................47

3.1 Distortion reduction ..................................................................................................48

3.1.1 Navy C-ring geometry .......................................................................................49

3.1.4 Heat treatment conditions .................................................................................51

3.1.5 Sample preparation and optical microscopy .....................................................52

3.1.6 Nano-indentation measurements .......................................................................53

3.1.7 Experimental distortion measurements .............................................................54

3.1.8 Numerical (FEM) distortion prediction ............................................................55

3.1.9 Composition-depth profile numerical simulation ..............................................56

3.1.10 Composition-depth profile measurements (experimental) ..............................57