metals

Article
Determination of Critical Transformation Temperatures for the
Optimisation of Spring Steel Heat Treatment Processes
Velaphi Jeffrey Matjeke 1, * , Josias Willem van der Merwe 1 and Nontuthuzelo Lindokuhle Vithi 2

1 School of Chemical and Metallurgical Engineering, University of the Witwatersrand,

Johannesburg 2000, South Africa; [email protected]
2 Transnet Engineering, Research Development, Private Bag X528, Kilnerpark 01272, South Africa;
[email protected]
* Correspondence: [email protected]; Tel.: +27-(0)12-743-0515

Abstract: Bogie spring performance can be improved by using the exact heat treatment process
parameters. The purpose of the study is to determine the critical transformation temperatures and
investigate the effect of the cooling rates on microstructural and mechanical properties. The precise
determination of the required cooling rates for the particular grade of steel is important in order to
optimise the heat treatment process of heavy-duty compression helical spring manufacturing. A
traditional heat treatment system for the manufacture of hot coiled springs requires heating the steel
to homogenize austenite; then, it is decomposed to martensite by rapid cooling. By analyzing the tran-
sition properties by heating and differing cooling rates, this analysis examines the thermal behaviour
of high strength spring steel. Using the dilatometer and differential scanning calorimeter, scanning
electron microscope, optical microscope, and hardness checking, critical transition temperatures and





 cooling rates of three springs steels were measured. Although the thermal transformation of materials
Citation: Matjeke, V.J.; van der has been researched for decades using dilatometers, not all materials have been characterized. The
Merwe, J.W.; Vithi, N.L. research offers insights into the critical transformation temperatures for the defined grades of spring
Determination of Critical steel and the role of cooling rates in the material’s properties. Mechanical properties are influenced
Transformation Temperatures for the by the transition data obtained from the dilatometric analysis.
Optimisation of Spring Steel Heat
Treatment Processes. Metals 2021, 11, Keywords: dilatometer; spring steel; critical transformation temperature
1014. https://doi.org/10.3390/
met11071014

Academic Editor: Zhenjia Xie 1. Introduction

The recent global economic development has led to an increased demand for rail
Received: 3 May 2021
Accepted: 25 May 2021
freight, resulting in higher traffic, tonnage, and train speeds [1–3]. The durability of safety-
Published: 24 June 2021
critical suspension elements, such as bogie springs, must be strengthened in order to run
heavy haul trains safely [3]. To bear the load within a specified range without plastic
Publisher’s Note: MDPI stays neutral
deformation, these springs depend on elastic deformation [4]. In determining the mate-
with regard to jurisdictional claims in
rial applicability of the springs, the EN 10,089 norm relies on hardness and strength [5].
published maps and institutional affil- The chemical composition and cooling rate are usually a function of the microstructures,
iations. hardness, and strength of steel [6]. The steels chosen for this investigation were selected to
maximize the development of bogie springs and are graded as grades 55Cr3, 54SiCr6, and
52CrMoV4 by EN 10089. With respect to alloying elements, these steel grades differ con-
siderably. The 54SiCr6 grade has a significantly higher silicon content than the other two
Copyright: © 2021 by the authors.
grades which, in theory, delays carbon diffusion within steel, thus promoting martensite
Licensee MDPI, Basel, Switzerland.
formation at lower quenching rates, thereby improving hardenability [7]. Grades 55Cr3
This article is an open access article
and 52CrMoV4 have higher manganese contents and 52CrMoV4 has a higher chromium
distributed under the terms and content than the other two, and has a significant increase in hardenability. The manufac-
conditions of the Creative Commons turing process needs to be optimised in order to enhance the mechanical properties of
Attribution (CC BY) license (https:// hot coiled springs. A thorough understanding of the critical transformation temperatures
creativecommons.org/licenses/by/ and behavior of the spring steel grades selected is therefore required. Austenitisation
4.0/). and quenching processes are the key steps in the development of hot coiled springs [8].

Metals 2021, 11, 1014. https://doi.org/10.3390/met11071014 https://www.mdpi.com/journal/metals

Metals 2021, 11, 1014 2 of 14

The acceptable hardened microstructure for these types of springs is martensite, which is
dependent on the lower critical temperature (Ac1 ), upper critical temperature (Ac3 ), and
martensite start (Ms) temperature [9,10].
Ac1 and Ac3 are regarded as the beginning of austenite phase transformation and
the end of austenite formation during heating. The empirical data generated from the
JMatpro software show the critical transformation temperatures of steel grade 54SiCr6 to
be significantly lower than the one predicted using Andrew’s equation [11]. An earlier
study also showed that there is no agreement between the JMatPro simulation software
and Andrew’s equation in determining the Ms temperature of 54SiCr6 steel grade [12].
Andrew’s equation is commonly used to estimate the temperature of Ac1 , Ac3 , and the Ms
temperature [13,14]. The equations are listed as Equations (1)–(3).
Thermal dilatometry can be used during heating and cooling procedures to precisely
determine the critical transformation temperature [15,16]. This contributes to the existing
knowledge gap. The critical transformation temperature can be accurately determined
using dilatometry. The dilatometric phase change is accompanied by a significant change
in length, along with a temperature increase [17]. The transformation of the martensite
depends on the stabilization of the austenite process, which depends to a large extent on
heating above Ac1 and Ac3 [18]. The unreliability in the Ms temperature has warranted for
the heating and cooling characteristics of the three grades to be investigated.
The transformation kinetics of the steel phases are known and understood, but for the
unique steel grades, this study aims to predict the optimum transformation characteris-
tics. For instance, martensite is a diffusionless transformation that occurs by habit plane
shear when the steel is rapidly cooled from the austenitic range [19]. The transformation
encompasses the compression of the BCT lattice parameter c-axis and the extension of the
a-axis. Carbon atoms are trapped within the BCT structure. Generally, a martensite mi-
crostructure is attained when high-strength spring steel is supercooled from the austenitic
region [20,21]. It is often difficult to achieve 100 percent martensite on spring steel without
causing quench cracks [22–24]. The material’s ability to harden is largely influenced by the
chemical composition and quenching capacity of the quenching media. As a result, the
hardened microstructure usually has small percentages of either retained austenite, pearlite,
or bainite. The purpose of this study was to determine the exact critical temperature of the
transition and the effect of the cooling rate on the microstructure and mechanical proper-
ties of the spring steel. The selected spring steels are typically susceptible to quenching
cracks and microstructural defects when the quenching process is not controlled; thus, it
is necessary to determine the material’s critical transformation temperature and behavior
during cooling [22].

Ac1 (◦ C) = 723 − 20.7(%Mn) − 16.9(%Ni) + 16.9(%Cr) + 290(%As) + 6.38(%W); (1)

◦

√ 
A3 C = 910 − 203 %C − 15.2(%Ni ) + 44.7(%Si ) + 104(%V ) + 31.5(%Mo ) + 13.1(W ); (2)
◦

Ms C = 539 − 432(%C ) − 30.4(%Mn) − 17.7(%Ni ) − 12.1(%Cr ) − 7.5(%Mo ) + 13.1(W ) (3)

2. Materials and Methods

To perform the thermal analysis and determine the effect of cooling speeds on mi-
crostructures and mechanical properties, the three selected spring steel grades were pre-
pared for differential calorimeter scanning and dilatometry.
Dilatometer samples were machined to a length of 10 mm and a diameter of 5 mm,
while the differential scanning calorimeter (DSC) samples were prepared toward smaller
particles by grounding the solid-state metal. For each grade of spring steel, the dilatometric
test samples were heated to 860 ◦ C, followed by soaking them at the same temperature,
before cooling them at different speeds. Helium gas was used as the cooling media. In
order to produce dilatometric data for the steels, constant cooling speeds were used. Using
thermal expansion against temperature, the critical transition temperatures were calculated
by calculating the dilation, while the DSC used heat flow. The criteria for heat treatment are
Metals 2021, 11, 1014 3 of 14

outlined in Table 1. The chosen steel grades used in this experiment were 55Cr3, 54SiCr6,
and 52CrMoV4. The chemical compositions were validated using a spectrometer (Bruker
Q4 Tasman, Carteret, NJ, USA), as seen in Table 2.

Table 1. Dilatometry parameters used on the three materials.

Temperature (◦ C) Cooling Rate (◦ C/s) Heating Rate (◦ C/s) Soaking Time (h)
860 0.01 2 45
860 0.1 2 45
860 1 2 45
860 10 2 45
860 20 2 45
860 30 2 45
860 100 2 45

Table 2. Chemical composition of the steels in wt%.

Element %C % Si % Mn %P %S % Cr % Ni % Cu % Mo %V
55Cr3 0.58 0.32 0.92 0.013 0.004 0.79 0.06 0.10 0.01 0.01
54SiCr6 0.56 1.33 0.71 0.014 0.002 0.75 0.01 0.01 0.00 0.06
52CrMoV4 0.55 0.28 0.92 0.012 0.007 1.05 0.01 0.01 0.19 0.11

The heat-treated dilatometer test samples were mounted and prepared for microscopic
inspection by grinding and polishing them to a 1-µm finish. Before the metallographic anal-
ysis using both the optical microscope (Olympus, Tokyo, Japan) and SEM, the samples were
etched with 2 percent nital etchant. The general microstructure of the as-received steel rods
from the mill was a pearlitic structure. To assess the hardness of the components compared
to the microstructure, the samples were further subjected to micro-Vickers hardness testing.
A micro-Vickers hardness test, with 0.5 kg.f, was used for microhardness; five indentations
were taken per sample with 400-µm radius spacing between the indentations to avoid the
deformation zones. The continuous cooling curves for the three steels were generated
from the dilation curves. The fastest cooling rate of 100 ◦ C/s was used to determine the
Ms temperature of the three steels. The Ac1 , Ac3 , and Ms temperature were compared
to the data produced by JMatPro software and DSC. The JMatPro simulation data and
phase distribution were determined using the calculation of phase diagrams (CALPHAD)
method as a function of the chemical composition of each steel [25]. The samples for the
DSC tests were heated to 860 ◦ C at 10 ◦ C/s for the purpose of validating the Ac1 .

3. Results and Discussion

3.1. Critical Transformation Temperature
For the purpose of process optimisation, dilatometric and DSC experiments were
performed to assess the precise phase transition temperatures. The dilation characteristics
of the three steels are seen in Figure 1 and Table 3. A tangent line is drawn along the
graph, and the temperature at which thermal expansion changes is called the critical
transformation temperature.
The DSC measurements verified the dilatometer results. The actual thermal test
measurements were compared to the JMatPro estimations and Andrew’s equation results. It
was found that there was no unanimity of the test results, between JMatpro, and Andrew’s
equation outputs. The optimisation of the heat treatment parameters is largely dependent
on the Ac1 , Ac3 , and Ms temperature. A higher Ac1 means a longer cooling period. It is
evident from the results that a general approach would be ineffective to optimise the heat
treatment parameters for the three steel grades. According to the dilation findings, it would
take the least time for 55Cr3 to initiate martensite formation, followed by 52CrMoV4. It is,
however, noteworthy that due to a higher Ms temperature, 54SiCr6 is the most hardenable.
Metals 2021, 11, 1014 4 of 14

(a) (b)

(c)

Figure 1. Critical transformation temperatures for the three steels: (a) Ac1 and Ac3 using dilatometer, (b) Ms temperature
using dilatometer, and (c) DSC phase transition.

Table 3. Critical transformation temperatures.

Identity Andrew’s Equation Dilatometer DSC JMatPro

Transition
Ac1 Ac3 Ms Ac1 Ac3 Ms Ac1 Ms Ac1 Ac3 Ms
Temperature (◦ C)
55Cr3 726 740 255 753 818 218 751 225 738 741 253
54SiCr6 759 945 271 793 846 235 777 235 767 775 260
52CrMoV4 727 909 264 772 823 216 762 227 749 750 266

3.2. The Effect of Soaking Time on Phase Transformation

The austenite critical transformation temperature for 54SiCr6 steel is higher compared
to 55Cr3 and 52CrMoV4; however, it takes less time for austenite to stabilise. The rule
of thumb is that for complete austenitisation, the length of time required for steel to be
homogeneous is 1 h for a 25-mm diameter [26]. Carbon and other alloying elements require
time to be completely in solution [27]. It can be observed from Figure 2 that there is a
change in the length of the different steels during isothermal treatment at 860 ◦ C.
The change in length can be described as phase transformation from a BCC phase
to a smaller FCC phase. This change in length stabilises over time; however, the rate of
stabilisation varies from one steel to another. Figure 2 shows that the thermal expansion
of 54SiCr6 was stabilised approximately 30 min after soaking, while 52CrMoV4 was not
stabilised after fourty five (45) min of soaking. This proves that complete austenitisation
does not only depend on time but also on composition. Therefore, the Ac1 and Ac3
Metals 2021, 11, 1014 5 of 14

temperatures and the austenite stabilisation time are to be carefully considered during the
heat treatment optimisation process.

Figure 2. Thermal expansion rates for the three steels.

3.3. The Effect of Cooling Rates on Phase Transformation

The thermal dilatometric treatment results are presented in Figure 3. These graphs
present the critical transformation temperature achieved by varying the constant cool-
ing rates.

(a) (b)

Figure 3. Cont.
Metals 2021, 11, 1014 6 of 14

(c)

Figure 3. Dilatometric graphs of (a) 55Cr3, (b) 54SiCr6, and (c) 52CrMoV4 at various cooling rates.

There was a general increase in the Ms temperature for the three steels with a decrease
in the cooling rates, which varied as shown in Figure 4.
The variation in the Ms temperature is attributed to chemical compositional change
during cooling. Slower cooling rates allow for the diffusion process, whereby carbides may
form, changing the overall composition of the steel. 54SiCr6 exhibits higher Ms temperature
within the cooling rates of 20 ◦ C to 100 ◦ C/s. At 1 ◦ C/s and lower, for 54SiCr6, the cooling
rates were not significant to form martensite. This means that it was more hardenable
than 55Cr3 and 52CrMoV4. Although 55Cr3 exhibited the lowest Ms temperature at
100 ◦ C/s, it showed the highest Ms temperature at 1 ◦ C/s. The Ms temperature of 55Cr3,
at 100 ◦ C/s, was comparable to that of 52CrMoV4. However, the significant increase
in the Ms temperature of 52CrMoV4 was only observed with a cooling rate of 10 ◦ C/s,
before gradually decreasing at 1 ◦ C/s cooling rate. 55Cr3 was stable between 100 ◦ C/s
and 10 ◦ C/s before showing an increase in Ms temperature at 1 ◦ C/s. At 0.1 ◦ C/s, none
of the materials formed martensite. All the permutations stated above must be taken into
consideration when optimising the heat treatment parameters. The microstructures of each
steel grade are presented in Figures 5–7.

Figure 4. The effect of cooling rates on Ms temperature.

Metals 2021, 11, 1014 7 of 14

(a) (b)

(c) (d)

(e) (f)

Figure 5. Optical micrographs of 55Cr3 cooled at (a) 100 ◦ C/s, (b) 30 ◦ C/s, (c) 20 ◦ C/s, (d) 10 ◦ C/s, (e) 1 ◦ C/s, and (f)
0.1 ◦ C/s.

3.4. Effect of Cooling Rates on the Microstructure and Hardness Properties

The overall microstructure for the cooling rate, 20 ◦ C/s to 100 ◦ C/s, for the three steels
was martensite. The micrographs of 55Cr3 and 52CrMoV4, with a 10 ◦ C/s cooling rate,
presented mainly martensite and bainite microstructure. The bainite structure shown in
Figure 5d was coarser compared to that observed in Figure 7d, showing the negligible
presence of the bainite structure. Figures 5e and 7e indicated a significant percentage of
bainite and martensite present, while Figure 6e had a pearlitic structure with the presence
of pro-eutectoid ferrite. The percentage of bainite in Figure 5e was approximately equal to
that of martensite, while martensite constituted a larger fraction in Figure 6e. Figures 5f
and 7f showed pearlitic structures, while Figure 7f was pearlitic with proeutectoid ferrite.
The details of the microstructure were confirmed with an SEM. The images of the SEM
are presented in Figures 8–10. The microstructural characteristics were corroborated by
determining the hardness measurements.
Metals 2021, 11, 1014 8 of 14

(a) (b)

(c) (d)

(e) (f)

Figure 6. Optical micrographs of 54SiCr6 cooled at (a) 100 ◦ C/s, (b) 30 ◦ C/s, (c) 20 ◦ C/s, (d) 10 ◦ C/s, (e) 1 ◦ C/s, and (f)
0.1 ◦ C/s.

(a) (b)

Figure 7. Cont.
Metals 2021, 11, 1014 9 of 14

(c) (d)

(e) (f)

Figure 7. Optical micrographs of 52CrMoV4 cooled at (a) 100 ◦ C/s, (b) 30 ◦ C/s, (c) 20 ◦ C/s, (d) 10 ◦ C/s, (e) 1 ◦ C/s, and (f)
0.1 ◦ C/s.

(a) (b)

(c) (d)

Figure 8. Cont.
Metals 2021, 11, 1014 10 of 14

(e) (f)

Figure 8. 55Cr3 SEM images of the microstructure cooled at (a) 100 ◦ C/s, (b) 30 ◦ C/s, (c).20 ◦ C/s, (d) 10 ◦ C/s, (e) 1 ◦ C/s,
and (f) 0.1 ◦ C/s.

(a) (b)

(c) (d)

Figure 9. Cont.
Metals 2021, 11, 1014 11 of 14

(e) (f)

Figure 9. 54SiCr6 SEM images of the microstructure cooled at (a) 100 ◦ C/s, (b) 30 ◦ C/s, (c) 20 ◦ C/s, (d) 10 ◦ C/s, (e) 1 ◦ C/s,
and (f) 0.1 ◦ C/s.

(a) (b)

(c) (d)

Figure 10. Cont.

Metals 2021, 11, 1014 12 of 14

(e) (f)

Figure 10. 52CrMoV4 SEM images of the microstructure cooled at (a) 100 ◦ C/s, (b) 30 ◦ C/s, (c) 20 ◦ C/s, (d) 10 ◦ C/s, (e)
1 ◦ C/s, and (f) 0.1 ◦ C/s.

To achieve adequate mechanical properties and microstructures, it is necessary to

choose the required quenching media. The microstructural properties are further corrobo-
rated by the hardness measurements summarized in Table 4. Generally, with decreasing
cooling rates, the hardness decreases.

Table 4. Hardness measurements determined at various cooling rates.

Micro-Vickers Hardness Tester

Cooling Rate (◦ C/s) 55Cr3 54SiCr6 52CrMoV4
100 810 ± 36 802 ± 16 770 ± 11
30 827 ± 7 791 ± 9 770 ± 13
20 821 ± 10 791 ± 17 761 ± 41
10 820 ± 6 762 ± 17 739 ± 36
1 547 ± 126 336 ± 11 629 ± 137
0.1 299 ± 6 285 ± 11 296 ± 17

4. Conclusions
For the three spring steels, this analysis provided detailed critical temperatures for
transformation. It is important to draw the following conclusions:
The results showed that to successfully optimise the heat treatment process parameters,
detailed knowledge of the material is paramount. Generally, empirical heat treatment data
are helpful for guidance; however, for optimisation purposes, the exact parameters are a
requirement. Emanating from the dilatometric results, the optimum heating and quenching
media can be predicted for each specific grade of spring steel.
54SiCr6 was the most hardenable, with the cooling rates ranging from 20 ◦ C to
100 ◦ C/s; however, it was the least hardenable, with slower cooling rates from 1 ◦ C/s. In
material hardenability, chemical composition plays an important role, but the cooling rate
and critical transformation of austenite are equally crucial.
The data obtained from this study are adequate to optimize the heat treatment process,
but to plot CCT for the three steels, additional dilatometer data are needed. The effect of
tempering heat treatment on the microstucture that has been cooled at various temperatures
will be measured as part of future work.
Metals 2021, 11, 1014 13 of 14

Author Contributions: Conceptualization, V.J.M. and J.W.v.d.M.; validation, N.L.V. All authors have
read and agreed to the published version of the manuscript.
Funding: This research received no external funding.
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Conflicts of Interest: The authors declare that they have no conflict of interest.

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