P. KUČERA, E.

MAZANCOVÁ ISSN 0543-5846

METABK 55(2) 165-168 (2016)
UDC – UDK 669.15.26.28:621.78:621.56/.59:620.18:620.17=111

MECHANICAL AND STRUCTURAL RESPONSE

OF AISI 4135 STEEL AFTER CONTROLLED
COOLING PROCESS
Received – Primljeno: 2015-03-06
Accepted – Prihvaćeno: 2015-09-20
Original Scientific Paper – Izvorni znanstveni rad

AISI 4135 steel is a commonly used material for high strength applications such as shafts, forgings and high pressure
steel cylinders. The mentioned steel is used in a variety of microalloying by Nb, Ti, V, N, respectively of those ele-
ments combinations. In this presented paper, three different microalloyed (by N and V) heats of mentioned steel
were studied. Three heat treatment modes were applied. The first mode was based on heating at 700 °C, subsequent
quenching and tempering at 470 °C. In the second and the third mode the material was heated at 890 °C and sub-
sequently different controlled cooling process followed in both modes. Microstructural and microfractographic
analyses compared with found mechanical properties were part of the solution.
Key words: AISI 4135, heat treatment, control rolling, microstructure, mechanical properties

INTRODUCTION EXPERIMENTAL PROCEDURE

The AISI 4135 steel type represents a good balance Samples of 3 heats (AISI 4135) manufactured under
among different properties as strength, toughness, fa- the same conditions (Table 1), after hot reserved extru-
tigue and corrosion resistance under extreme working sion from billet and reversed hot rolling (10,2 mm in
conditions and therefore it is used for a variety of indus- thickness) including ACC were used.
trial and constructional applications, such as, forgings,
rolled plates, cranes, wind turbines, mining equipment Table 1 Average chemical composition of used heats / wt. %
and also for the production of high pressure steel cylin- C Mn Si Cr Mo
ders (HPSC) and vessels, including compressed natural 0,36 0,84 0,27 1,13 0,21
gas (CNG) transportation and storages etc. 1-4. Varia- P S V N -
tions of microalloying by Nb, V, Ti, B and N are often 0,12 0,004 0,073 0,0113
used in the AISI 4135 [5, 6]. Steel purity, deformation
temperatures, strain rate, chosen heat treatment (HT) Three heat treatment modes were realized. The HT1
and cooling processes (CP) influence the final micro- was based on the heating at 700 C, fast cooling in
structure and mechanical properties. Nűrnberger [2, 3] quenching bath (QB) and tempering at 470 C. The
confirmed the important influence of the cooling rate HT2 consisted of a controlled cooling process (CCP)
and strain level on final microstructure, however with- based on the heating to the austenitic zone (-zone) with
out accelerated cooling process (ACC) consideration. subsequent fast air cooling to the intercritical zone (IZ).
In 7 authors showed the low cycle lifetime response of Afterwards, fast cooling in QB to the temperature T just
42CrMo4 steel after normalization and after tempering above the martensite start (MS) followed with air cool-
related to the change of modulus of elasticity. Chen [8] ing to 40 C under the MS, and cooling (QB) to the room
detected in steel AISI 4135 quenching cracks caused by temperature with tempering at 470 C / air. Further, the
uneven surface cooling. Moli-Sanches [9] ascribed heating to -zone followed-up air cooling to the IZ with
higher hydrogen mobility in the AISI 4135 treated at fast cooling (QB) to 200 C above the MS and air cool-
680 °C than at 540 °C to higher dislocation density and ing to 90 °C above the MS followed by QB cooling to
hydrogen trapping. the room T with tempering at 470 C / air represented
Nowadays, development of the similar steel the HT3 mode. Testing of mechanical properties was an
42CrMo4 to AISI 4135 is targeted on maximum strength integral part of the solution. The yield stress and tensile
simultaneously with high toughness and favorable cor- strength (Rp0,2, Rm), elongation (A), Brinell´s hardness
rosion resistance in a sour environment 4. This is also (HB) and notch toughness (KCV) parameters were es-
the aim of the presented paper. tablished. Testing of Rp0,2, Rm and A was realized by use
of the Zwick/Roell Z 250 machine (EN ISO 6892-1).
P. Kučera, Vitkovice Cylinders Inc., Czech Republic
E. Mazancová, VŠB - Technical University of Ostrava, Faculty of Met- The HB was measured using the M4U750 hardness test-
allurgy and Materials Engineering, Czech Republic ing machine (EN ISO 6506-1) and KCV was tested by

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 P. KUČERA et al.: MECHANICAL AND STRUCTURAL RESPONSE OF AISI 4135 STEEL AFTER CONTROLLED COOLING...

use of the RKP 450 Charpy Impact Testing Machine

(ISO 148-1) at -50 C. Metallographic evaluation was
carried out using a light microscope Neophot 21 (purity
- ČSN ISO 4967), microstructure analysis, the grain
size (G) - ASTM E 112. For micro-fractography trans-
verse KCV samples were used (SEM JEOL JSM-6490).

Table 2 Resulting mechanical properties and grain size (G)

of three heats after three different modes of heat
treatment
HTM HT1 HT2 HT3
Rp0.2 / MPa 676 1 120 1 272
Rm / MPa 824 1 257 1 397
A/% 17,6 12,5 9,8
KCVtrans. / Jcm-2 22 34 23
KCVlong. / Jcm-2 19 35 22
HB (2,5 / 187,5) / - 248 402 424
G / grade 10 11 8

RESULTS AND DISCUSSION

The lowest levels of strength and KCV properties
were found the in case of HT1. In both testing direc- Figure 1 Micrographs (Nital) of a) HT1- general view,
tions, KCV values showed an insignificant difference of b) HT1- detail, c) HT2 - general view, d) HT2 – detail,
e) HT3 – general view, f ) HT3 – detail
3 Jcm-2. After HT2 application tensile properties were
lying between the HT1 and HT3 values, however bal-
anced KCV values in both testing directions were sig- of reverse rolling which allowed significant segregation
nificantly higher than those in cases of HT1 and HT3. of elements such as Cr, Mo, and C to the segregation
The resulting A and HB values fully correspond with the bands, which are moderately thick and of continuous
upward trend of tensile properties as can be seen in Ta- character as shown in Figures 1a – 1d.
ble 2 including the G. The non-metallic inclusions The heating at 700 C was approx. 25 C under the
evaluation of all three3 heats revealed a considerably Ac1 due to deficient heating temperature and the aus-
high purity level of all investigated heats. Fine sul- tenitization process was not achieved. Resulting coarse
phides were revealed once (HT3) of the 1,1 grade. Alu- microstructure (grade 10) contained numerous carbide
minates were not detected, silicates were in the range particles, which precipitated during the tempering pro-
from 0 - 0,5 and fine oxides from 0,1 - 0,8. The most cess. Significantly banded microstructure, which origi-
favorable and balanced values of tensile properties and nated during the process of forming and subsequent
KCV in both testing could be ascribed to the HT2 with cooling, was not reduced due to low heating tempera-
the finest G. ture. Resulting tensile properties fully correspond with
Microstructure was evaluated from the areas close to the microstructure and the differences of KCV values
the inner surface of the semi-product of HPSC. The rea- (Table 2), in which testing KCV values (Table 2), in
son for this choice of place is the most commonly used which testing directions are consistent with the segrega-
HT of cylinders in closed state. Namely, there is no ac- tion banding in the microstructure. Figures 1c and 1d
cess of the quenching medium to the inner surface of represent microstructure of finer morphology obtained
cylinders. This causes heating of the inner and slightly after the HT2 application with significantly reduced
under the inner surface area of the cylinder by trapped segregation bands (thinner and discontinuous).
gases for a longer time than the outer surface, where the This corresponds with the highly balanced KCV re-
cooling rate is much higher due to direct contact with sults in both testing directions as well as highly bal-
the quenching medium. This results in more noticeable anced strength and KCV parameters (Table 2). Micro-
segregation banding in the inner under surface area due structure consists of fine tempered martensite (´), AF
to longer times for possible segregation processes. Mi- and LB in small portion. The phase of AF was obtained
crostructure after the HT1 predominantly revealed low by cooling on the air from the fully -zone to the IZ,
bainite (LB) partially mixed with ferrite (F), low por- which is able to suppress harmful segregation banding.
tion of acicular ferrite (AF) and pearlite (P) - see Fig- Presented oxisulfitic inclusions supported AF nuclea-
ures 1a,1b. This was also the reason for the 34 % lower tion and Mo in steel modified its shape. Subsequent fast
Rm of the HT1 in comparison with the HT2. Microstruc- cooling in the QB to the T just above the MS ensured
ture after the TH1 is similar to the microstructure after restriction of the segregation processes to the minimum
the slow air cooling after the hot forming temperatures according to the resulting reduced banded microstruc-

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Fracture surface of specimens after the application of

HT2 revealed similar character of fracture surfaces like
in the of HT1, however cleavage and/or quasi-cleavage
facets were significantly finer and more even, corre-
sponding to the found grain size (Table 2), partially
decorated with thin ductile ridges and also thicker and
longer ductile ridges were observed (Figure 2c). This
was the cause of increased KCV values. Finer micro-
structure and partial elimination of unfavorable segre-
gation banding of the HT2 microstructure unlike the
HT1, contributed to balanced tensile properties and
KCV levels. Figure 2 demonstrates the fracture surface
of the KCV specimen after the application of HT3. In
this case, the fracture surface showed rather trans-crys-
Figure 2 Fracture surface of CVN specimen after a) HT1, b) talline cleavage character with creeks detected in some
HT2, c) HT3
facets. In given case, the facets were the coarsest. Duc-
ture. Cooling in air to the T = 40 C resulted in partial tile ridges were observed sporadically and were thin
LB and by subsequent quenching in QB, the ´ micro- and short. This morphology fully corresponds with the
structure was obtained. lowest grain size of used HT2 compared to the other
The microstructure after the HT3 application (Fig- two used treatments with finer grain size. Fracture sur-
ures 1e, 1f) is formed by tempered ´, AF and polygo- face character also corresponds with the highest tensile
nal F. Both after the HT2 and the HT3 application, the properties showing the lowest elongation value.
AF phase was obtained due to the cooling from fully -
zone to the IZ and segregation banding was considera- CONCLUSIONS
bly eliminated, however cooling in air from 200 °C to
90 C above the MS before cooling in QB, caused unde- The paper summarizes the results of mechanical
sirable extended polygonal F formation which disrupts properties, metallographic and fractographic observa-
the microstructure homogeneity and from the point of tions of three different heat treatment modes of the AISI
view of mechanical properties e.g. sulfide stress crack- 4135. The best achieved results of achieved mechanical
ing resistance. This phenomenon appeared due to the properties from the point of view of tensile properties
long-lasting cooling in air from 200 °C to 90 C with vs. balanced and high KCV in two testing directions
the contribution of hot trapped gases inside of the heat were seen in case of HT2, where the segregation band-
treated cylinder which were continuously heating the ing in microstructure was significantly restricted in
inner and under inner surface area of the material. Re- comparison with the HT1 and HT3 modes. Microstruc-
striction of noticeable segregation banding was directly ture obtained by the HT2 mode revealed slight discon-
reflected in balanced KCV values in both testing direc- tinuous banding and its elimination would be possible
tions (see Table 2). by increasing the cooling rate from the -zone to IZ.
The (´) transformation occurred as a result of fast The subsequent time and tempering temperature should
cooling in the QB from the temperature of 90 C above be increased in order to moderately increase the values
MS to the room temperature. By subsequent tempering, of A and KCV at the cost of a moderate Rm decrease to
primarily tempered (´) phase and the precipitation of approx. 1 200 MPa. This experimental procedure
carbide particles in (´) and LB was formed as was ob- proved that the most influencing factor of high tensile
served after the HT2 application. The achieved higher properties and as high values of KCV as possible is the
Rp0.2 and Rm levels resulted from higher quenching tem- grain size as it was reported in [6].
perature used to realize the quenching as compared with
the HT2 mode. Observed coarser G might probably Acknowledgements
cause decrease of the KCV and elongation values to-
gether with higher level of tensile properties. As Figure This paper was created in company Vítkovice Cylin-
2 shows, fractured KCV specimens showed coarser ders Inc. and at the FMMI in the Project No. LO1203
trans-crystalline cleavage character (HT1, HT3) and/or “Regional Materials Science and Technological Centre
quasi-cleavage facets with ductile ridges (HT2). Their – Feasibility Program” funded by Ministry of Educa-
occurrence was sporadic and found ridges were very tion, Youth and Sports of the Czech Republic.
thin. The reason for the disproportional values of KCV
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