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Journal of Science and Arts Year 18, No. 3(44), pp.

785-794, 2018

ORIGINAL PAPER
METALLURGICAL STUDY OF MANGANESE STEEL
F. SABIR1, O. BEN LENDA1, S. SAISSI1, Y. TAMRAOUI2, F. MIRINIOUI2, B.
MANOUN2, A. IBENLFASSI3, K. OUZAOUIT4, R. BOULIF5, E. SAAD1,6
_________________________________________________
Manuscript received: 16.05.2018; Accepted paper: 22.07.2018;
Published online: 30.09.2018.

Abstract. This study shows the effects of heat treatment on the manganese steel which
microstructure consists essentially of 18.447% of manganese, 0.745% of chromium, and
1.169% of carbon. The techniques used are: X-ray diffraction, optical microscope, scanning
electron microscope.After heat treatment at 600 °C and 1050 °C for 30 minutes, metallurgical
analysis will connect the microstructural changes occurring during the temperature
maintenance to the mechanical behavior of the material. The characterization of the
microstructures and the surface morphology of the alloy before and after the heat treatment
determine that this treatment process favors the dispersion of carbides in the austenitic matrix
and the appearance of precipitates which causes structural hardening.
Keywords: X-ray diffraction, optical microscope, electronic scanning microscope,
microstructural changes, structural hardening.

1. INTRODUCTION

Many researchers have begun to focus on the replacement of conventional steels Fe-
Cr-Ni by Fe-Cr-Mn, because Mn substitutes for Ni with decreasing the Cr content. Indeed, Cr
was found to be most effective for improving high-temperature oxidation resistance and
embrittlement of the environment [1, 2]. Carbon promotes the hardening of the alloy by
precipitation and manganese improves the mechanical properties at elevated temperatures
[3-6]. Manganese steels have many advantages, including low cost, corrosion resistance [7-
18]. Thus, they are suited to use in shipbuilding, and the land of the automobile industry.
The mechanical properties of manganese steels at casting raw state are low, but these
can be considerably increased by the completion of heat treatment, and also have to study and
examine the effects of content C, Mn and Cr. The characterization of the microstructures and
the surface morphology of the alloy before and after heat treatment were studied by optical
microscopy, scanning electron microscope, X-ray diffraction (XRD) and thus the hardness
measurements indicate the evolution of the mechanical properties of our steel.

1
University Hassan 1st, Laboratory of Physicochemistry of Materials and Processes (MPCP), Settat, Morocco.
E-mail: [email protected].
2
University Hassan 1st, Laboratory of Materials Science, Media and Modeling, 25000 Khouribga, Morocco.
3
University Hassan 1st, Department of Environmental Sciences and Development, Settat, Morocco.
4
Managem Group, REMINEX Research Center, Marrakech, Morocco.
5
OCP Group, Laboratory of Research and Development, 24000 El Jadida, Morocco.
6
University Hassan 1st, Higher Institute of Health Sciences, Settat, Morocco.

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786 Metallurgical study of manganese steel F. Sabir et al.

2. MATERIALS AND METHODS

The alloy that will be the subject of the metallurgical study is manganese steel. Its
composition is shown in Table 1. It essentially consists of iron with a ratio of chromium and
manganese. Our alloy is prepared as follows: the elements are melted in an electric arc
furnace provided with carbon electrodes at a temperature almost equal to 1500 °C [19]. The
crude steel, before being poured into molds, it is refined to adjust the chemical composition
by adding elements (i.e. Manganese, Chromium, Silicon, Copper, Nickel, Phosphorus,
Vanadium, Molybdenum, sulfur, titanium) to form requested alloy.
Table 1. Chemical composition [%] of steel based on iron.
C Si Mn P S Cr Mo Ni Cu V Fe
1.169 0.668 18.447 0.001 0.0065 0.745 0.034 0.184 0.302 0.0017 78.368

Hardness
The treated sample was cut into smaller samples; sections are obtained by sawing and
mechanical abrasion. All sections are heat-treated at various temperatures for 30 minutes at
600 °C and 1050 °C in the furnace, and then quenched with water.
The objectif to place the hardness test at the center of this study comes from the fact
that it is a fast and reliable mean to follow the kinetics of aging. This Hardness tests is
performed by Rokwell method using a durometer testweel under a load of 60 kgf. This
protocol makes possible monitoring the overall behavior of the material.

Metallographic Examination
Manganese steels after heat treatment has undergone a mechanical polishing with a
series of abrasives (from 120 to 1200), then etching using nitric alcoholic solution, this
reagent is composed of 2 ml to 5 ml of acid nitric in 100 ml of pure ethanol. Observation of
the structure of the steel was observed by optical microscope and scanning electron
microscopy of type Philips XL30, the microscope is coupled to a type detector EDAX
(Energy Dispersive X-Rays Spectrometer) which permits quantitative analysis for local
composition.

X-Ray Diffraction
The X-ray diffraction of the spectra of the samples during aging and over aging are
obtained at room temperature using a diffractometer D2 PHASER Bragg-Brentano geometry,
type of radiation Cu Ka = 1.5406 Å (40 kV, 40 mA) and the 2θ scanning range is 15° to 100 °
with a step of 0.02 (2θ).

X-Ray Fluorescence
Quantification and qualification of all elements of the alloy was given by mobile
Spectrometry XRF the mark of Bruker.

3. RESULTS AND DISCUSSION

Manganese steel based on iron in the initial state


The hardness measurements of austenitic steel with manganese at the receiving state
before heat treatment give an average of 47 HRF. The micrographic study of manganese steel

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Metallurgical study of manganese steel F. Sabir et al. 787

in the rough cast shows that the sample structure is austenitic with presence of carbides of
manganese and chromium which precipitated at the grain boundaries by altering the strength
and ductility (Figs. 1-2). From Table 2, we see that the matrix and the precipitates are
composed essentially of manganese and chromium carbides.

Figure 1. Scanning Electron Microscopy - the structure of manganese steel for the raw cast shows
heterogeneous precipitates of chromium and manganese dispersed in the austenitic matrix.

Figure 2. The SEM micrograph and EDAX of As‐cast manganese steel.

Table 2. Chemical Composition of the target points.


Fe Mn Cr
ZONE/ Element
Wt% At% Wt% At% Wt% At%
A 76.69 76.34 22.15 22.42 1.16 1.24
B 71.10 70.69 27.27 27.56 1.64 1.75

Study of heat treatment effect on the hardening of manganese steel

After heat treatment at 600 °C, we have followed the evolution hardness of manganese
steel treated on time. We see a linear increase in hardness with time in order to achieve a
hardness value of 49 HRF after 20 minutes of aging at room temperature. The hardness stays
constant before decreasing to a 47 HRF value after 3 hours. For maintain long time the
hardness remains constant [20].

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788 Metallurgical study of manganese steel F. Sabir et al.

Figure 3. Evolution hardness of the manganese steel treated at temperature 600 °C as a function of time.

The micrographic study of the heat treated alloy at 600 °C shows a non-uniform
dispersion of the second phase in the microstructure which can be observed in Fig. 4.The
figure shows also the heterogeneity of the distribution of second phase particles of the steel
treated at 600 °C.

Figure 4. Visualization of the manganese steel structure after 20 days of aging treated at 600 °C, quenched
with water, attacked by the nitric alcoholic solution.

Figs.5-6 show the result of SEM and EDAX. The structure of the steel after the
treatment at 600 ° C is composed by a matrix essentially rich in Fe and Mn (Fig. 5), and the
precipitates rich in Mn and Cr (Fig. 6). In fact the observation of the structure by scanning
electron microscope shows that the structure is heterogeneous, this observation is similar to
the optical microstructure obtained in Fig. 4.
Fig. 7 shows the evolution hardness of manganese steel as function of time. For
prolonged maintain the hardness remains constant and have a value of 47.5 HRF to 1050 °C.
The increase in the hardness may be due to a relatively uniform distribution of the carbide
phase in the austenite phase which explains the increase hardening structure increase treated
at 1050 °C compared to the As-cast state of manganese steel [21].

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Metallurgical study of manganese steel F. Sabir et al. 789

Zone A

Figure 5. Visualization manganese steel by a scanning electron microscope, treated at 600 °C.

Zone B

Figure 6. Identification of phases with different chemical compositions by EDAX on manganese Steel
treated at 600 °C.

Table 3. Chemical Composition of the target points.


Fe Mn Cr
ZONE/ Element
Wt% At% Wt% At% Wt% At%
A 78 78 21 21 1 1
B 55 55 41 41 4 4

Figure 7. Evolution of hardness of manganese steel treated at 600 °C and 1050 °C depending on time.

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790 Metallurgical study of manganese steel F. Sabir et al.

Table 4 shows the chemical composition of manganese steel obtained using mobile X-
ray fluorescence spectrometry; we see that there is no heat treatment influence on the
chemical composition of treated alloy.

Table 4. Chemical composition of manganese steel before and after heat treatment.
Steel with 18% Mn before heat treatment Steel with 18% Mn after heat treatment at 1050 ° C

Element % Element %

Cr 0.7 ± 0.02 Cr 0.69 ± 0.02

Mn 17.46 ± 0.08 Mn 17.28 ± 0.08

Fe 81.45 ± 0.15 Fe 81.58 ± 0.16

Ni 0.13 ± 0.02 Ni 0.16 ± 0.02

Cu 0.22 ± 0.01 Cu 0.27 ± 0.01

Mo 0.03 Mo 0.03

Visualization of manganese steel structure treated at 1050 °C after one month of aging
showed a significant effect of the heat treatment on the structural behavior of the sample. For
maintain prolonged in time, the grain boundaries are characterized by strong segregation of
chromium carbides (Fig. 8).

Figure 8. Optical micrograph manganese steel treated at 1050 °C.

The SEM micrograph of manganese steel heat treated at 1050 ° C is shown in Fig. 9,
the second phase particles, is uniformly dispersed with the austenitic matrix; this treatment
helps to dissolve the carbides in the matrix [19].

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Metallurgical study of manganese steel F. Sabir et al. 791

Figure 9. Identification of phases with different chemical compositions by EDAX for manganese Steel
treated at 1050 °C.

Table 5. Chemical Compositions of target points of manganese steel after treatment at 1050 °C.
Fe Mn Cr O
ZONE/ Element
Wt% At% Wt% At% Wt% At% Wt% At%

A 82.10 81.82 16.94 17.16 0.95 1.02 0.00 0.00

B 89.00 89.00 10.00 10.00 1.00 1.00 0.00 0.00

Fig. 10 shows the X-ray diffraction analysis of manganese steel before heat treatment
and also treated at 600 °C and 1050 °C. We observe the displacement of the peak position to
the right, this change of position is due to changes of the phases that characterize each
treatment (Table 5). In the result of X-ray diffraction, the carbides are uniformly dispersed
with the austenitic matrix; the operation of the heterogeneity of second phase carbide
segregation was dissolved at 1050 °C with the appearance of new precipitated phases.

Figure 10: Evolution of the X-ray diffraction patterns for manganese steel as a function of temperature
600 °C, 1050 °C and cast state.

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792 Metallurgical study of manganese steel F. Sabir et al.

Table 6. Characteristics of diffraction pattern at 1050 °C, and at 600 °C before heat treatment.
Steel before heat
Steel after heat treatment
treatment

hkl 2Ө Ihkl 2Ө Ihkl at 1050°C Ihkl at 600°C

002 - - 40.573 11.952 -

111 42 57.63 43.228 100 100

420 - - 46.548 46.181 -

200 48.80 30.19 49.867 29.208 62

551 - - 61.152 9.689 -

220 72.57 23.07 73.765 25.813 40

211 - - 82.129 20.156 -

311 88 29.17 90.228 26.096 37

222 93.68 10.78 94.742 9.406 12

Table 7 shows the crystal parameters a, b, c, and the angles α, β, ɤ of the crystal
structures. Stitch parameters have been refined from the experimental positions of diffraction
lines using the program PARAM [22, 23], we find that the crystal system changes from cubic
to orthorhombic after heat treatment (Table 7). Thus, as and as the treating temperature
increases, the cell volume decreases, passes from 46.9 A°3 to 45A°3.

Table 7. Parameter values and volume determined and refined using the software "PARAM".
Refinement By PARAM

Steel before heat Heat treatment at Heat treatment


treatment 600°C at 1050°C

crystal system cubic orthorhombic orthorhombic

a= 3.649±0.011 a= 3.586±0.039
Lattice
a=3.606±0.01923 b= 3.588±0.016 b= 3.589±0.064
parameter(A°)
c= 3.656±0.019 c= 3.458±0.0689

Volume of the
V= 46.856±0.750 V= 47.808±0.356 V= 44.5±1.318
stitch (A°3)

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Metallurgical study of manganese steel F. Sabir et al. 793

4. CONCLUSIONS

A metallurgical study connects the microstructural changes during the heat treatment
with the mechanical behavior of the material. The temperature and time are parameters
influencing the kinetics of microstructural transformations. For this reason, two aging
temperatures were selected; 600 °C and 1050 °C for industrial and scientific interests.
Characterization manganese steel at raw casting states showed that they have a
structure consisting of austenite, manganese and chromium carbides which precipitate, in
great quantities, in the austenitic grain boundaries. For that, the steel has followed an
annealing treatment at a temperature of 1050 °C; this treatment favors the dispersion of
carbides in the austenite matrix.
The scanning electron microscope is coupled to sensor type EDAX allowing for local
quantitative analysis of the composition. The EDAX analyzes carried out on the steel show
that for lower temperatures, the precipitates are very rich in carbon and the matrix consists of
Iron, Manganese and Chromium.
X-ray diffraction spectra obtained after the treatment revealed that the structure is
orthorhombic. These spectra also show the presence of several phases that characterize the
structure of the steel.

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