UDK 621.771:669.017.

Microstructural Behaviour of Tempering Steels

during Precision Forging and Quenching
from Hot-forming Temperatures
F. Nürnberger, O. Grydin, Z. Yu, M. Schaper
Faculty of Mechanical Engineering, Institute of Materials Science,
Leibniz University Hanover, An der Universität 2, 30823 Garbsen, Germany,
[email protected]

To design a precision forging or twin-roll casting process combined with heat treating from the hot-forming
temperature, flow curves for a selection of hardening and tempering steels were recorded using a deformation
dilatometer. In addition to this, continuous cooling transformation diagrams were generated for the 42CrMo4
hardening and tempering steel. These diagrams take into account the influence of deformation on the trans-
formation behaviour during quenching from a temperature of 850 °C. The results of the investigations show
an increase in the flow stresses with decreasing temperatures and the deformation's minor influence on the re-
sulting material's hardness and microstructural constituents.

Keywords: TEMPERING STEEL, QUENCHING FROM HOT-FORMING TEMPERATURE, FLOW

CURVES, CCT

1. Introduction steels, such as 10MnB6 or 5CrB4 alloys, enable

quenching to simultaneously produce a martensitic
The controlled heat treatment of hardening and microstructure and reduced susceptibility to cracking
tempering steels using the hot forming temperature of [5]. Also, air-hardening steels such as 21CrMnCu8-6
metal forming processes such as precision-forging, and 40SiMnCrMo7-6-6-4 or LH800 materials are
deep drawing or twin-roll casting enables significant suitable for obtaining a martensitic microstructure
savings of resources in comparison to conventional during cooling in still air. Additional steels are em-
methods. On the one hand, a smaller amount of mate- ployed in the automotive industry, particularly for
rial is required during flashless precision forging crash-relevant parts, such as 22MnB5 sheet mate-
since the usual proportion of flash of approx. 30% is rial alloyed with boron for manufacturing ex-
eliminated. On the other hand, the forgings already tremely high strength body elements by means of
have their final near-net shapes [1] so that the avail- press-hardening using heated, closed dies [6].
able hot-forming heat can be employed to heat treat Conventional hardening and tempering steels are
the material [2]. Twin-roll casting allows high energy not generally employed in these processes but they
and material savings due to the highly reduced manu- offer the possibility, particularly with controlled
facturing chain, since most of the conventionally cooling using locally variable cooling rates, of
necessary steps of hot rolling can economized. manufacturing high strength, bulk-formed compo-
Among the materials specially developed for heat nents possessing various requirements matched to
treating from the hot-forming heat comprise, for functional surfaces. This is possible by means of,
instance, the AFP-steels with which a controlled for example, spatially varied and temporally con-
transformation is carried out into the pearlite stage. trolled cooling based on water-air spraying [7].
Typical AFP-steels are the alloys 38MnVS6 and During the controlled cooling from the hot-
46MnVS3. The essential mechanism for increasing forming temperature with the aim of obtaining spa-
hardness values during the controlled cooling is the tially different microstructures, it is essential to take
selective solid-solution and precipitation hardening account of the microstructure's transformation behav-
for these steels [3]. The ultimate strengths of conven- iour which is influenced by the forming and the aus-
tional hardening and tempering steels, such as tenitising temperatures. Deformation time-
42CrMo4, are, however, currently not obtainable temperature-transformation diagrams (Deformation
using these materials [4]. Relatively soft martensitic TTT diagrams) and deformation continuous cooling

© Metallurgical and Mining Industry, 2011, Vol. 3, No. 7 79

transformation diagrams (CCT diagrams) can map these tures. Within the scope of this work, the transforma-
circumstances [8]. Thus, it was possible for Weise to tion behaviour is characterised at additional austeni-
represent the transformation behaviour with respect to tising temperatures from 850 °C. The diagrams are
hot rolling a 42CrMo4 hardening and tempering steel generated by employing linear cooling rates so that it
and austenitising temperatures of 900 °C [9]. Moreover, is possible to subsequently compute the isothermal
investigations of the microstructure's transformation transformation kinetics or, as the case may be, the
kinetics were carried out at austenitising temperatures of isothermal deformation TTT diagrams based on an
1200 °C and true strains of up to 0.6 for isothermal [10] approach according to Rios [12, 13]. The context for
and continuous cooling [11]. Especially during isother- this is that isothermal diagrams, which require rela-
mally controlled temperatures, changes in the transfor- tively less effort to generate, can be employed for the
mation intervals can be established whereas the micro- numerical design procedures to predict microstruc-
structures mainly change their distinctive features dur- tures for arbitrary cooling profiles [14].
ing a continuous transformation.
3. Materials and methods
2. Objectives
3.1. Chemical composition of the investigated
To design metal forming processes in combina- materials
tion with the hardening and tempering using the hot- A selection of heat treatable steels, 34CrMo4,
forming temperature, flow curves are required for the 42CrMo4, 50CrMo4, 51CrV4 and 34CrNiMo6, were
process simulation. These curves are recorded by used for the experimental investigations of the con-
means of a deformation dilatometer for a selection of tinuous transformation behaviour and to record the
heat treatable steels by which cylindrical specimens flow curves. The chemical composition in weight %
are compressed to true strains of up to 0.6. Further- determined by means of Glow Discharge Optical
more, deformation continuous cooling transformation Spectroscopy GDOS is given in Table 1. The meas-
diagrams are required which take into account the urements were performed on polished specimens
influence of a deformation on the transformation using a GDA 550 device made by the company Spec-
behaviour during quenching. In addition to the de- truma. The alloys’ compositions differ, particularly
formation CCT diagrams for austenitising tempera- in their carbon contents, which is decisive for their
tures of 900 °C [9] and 1200 °C [11], which are al- strength. Moreover, the 34CrNiMo6 alloy is distin-
ready available in the literature, supplementary dia- guished by its high nickel and chromium content for
grams are required for the 42CrMo4 heat treatable its ability to be fully quenched and tempered as large
steel at other austenitising and deformation tempera- forgings or thick-walled parts.

Table 1. Chemical compositions of the used alloying elements in weight %

alloy C Si Mn P S Cr Cu Mo Ni Al Nb
34CrMo4 0.325 0.289 0.577 0.007 0.003 0.945 0.286 0.132 0.098 0.025 0.019
42CrMo4 0.410 0.336 0.701 0.011 0.025 0.998 0.380 0.171 0.191 0.029 0.019
50CrMo4 0.491 0.212 0.647 0.005 0.004 1.039 0.219 0.133 0.092 0.024 0.020
51CrV4 0.467 0.223 0.845 0.006 0.017 1.015 0.223 0.013 0.083 0.018 0.063
34CrNiMo6 0.326 0.263 0.588 0.001 0.004 1.433 0.260 0.126 1.469 0.023 0.020

3.2. Dilatometric measurements For reference purposes, a diagram was con-

The microstructural transformations produced structed without deformation. The measurements
during cooling from the hot-forming temperature are were carried out using a deformation dilatometer DIL
influenced by the austenitising temperatures and the 805A/D, made by the company BÄHR-
deformation strain. To simulate the metal forming Thermoanalyse GmbH, (see Table 2) in collabora-
processes, material samples of the investigated tion with the Częstochowa University of Technology,
42CrMo4 alloy (5 mm diameter, 10 mm long) were Poland. The investigations were carried out accord-
inductively heated to an austenitising temperature of ing to the Polish standard PN-68/H-04500, which
850 °C within 30 s. Following isothermal soaking for essentially corresponds to the German "Stahl-Eisen-
600 s, samples were deformed to true strains of 0.16 Prüfblättern" SEP 1680 or SEP 1681, as the case may
or 0.35, as the case may be, at a deformation rate of be. The start and finish of the respective microstruc-
1 s-1. Following this, the samples were linearly tural transformations were determined from the
cooled using cooling rates in the region of 50 K s-1 to measured length changes of the dilatometer's time-
0.02 K s-1 (see Figure 1). profile curves as well as from the metallographic

80 © Metallurgical and Mining Industry, 2011, Vol. 3, No. 7

 30 s 600 s
850 °C
temperature in °C

20 °C
cooling rate: 50 30 15 6.0 2.0 1.0 0.6 0.3 0.15 0.04 0.02 K s-1
time in s
Figure 1. Schematic of the time-temperature controlled linear cooling profiles for generating the deformation CCT diagrams

Table 2. Technical of the quench and deformation dilatometer device DIL 805 A/D, made by the company Thermoanalyse
Bähr GmbH

Device's properties Characteristics of the deformation dilatometer

Temperature range 20 °C to 1500 °C
Heating method inductive
Specimen material electrically conducting solid
Atmosphere shielding gas, vacuum, air
Resolution Δl and °C 0.05 µm; 0.05 °C
Specimen geometry Solid specimens (5 mm diameter, 10 mm long)
Heating and cooling rate max. 100 K s-1
Applied deforming force max. 25 kN
Ram velocity 0.01 mm s-1 to 125 mm s-1
Strain rate 0.1 s-1 to 12.5 s-1
True strain 0.05 to 1.2

analyses and hardness measurements. For reasons of process by wet grinding with increasing paper
readability, no hardness values are given in the con- grades. The locations of the micrographic images and
structed deformation CCT diagrams. The curves in the subsequent hardness measurements were 1/3 of
the diagrams for the start and fnish of the transforma- the specimen's radius and 1/3 of its length [15]. The
tions were drawn by hand. Based on the selected specimens were polished to 1 µm and etched using
minimum cooling rate of 0.02 K s-1, only a few data 2 % nitric acid (HNO3) in order to contrast the indi-
points exist for the ferrite or, as the case may be, the vidual constituents. By means of an Axioplan reflect-
pearlite regions so that the depicted curves’ trajecto- ing light microscope made by the company Zeiss and
ries for longer periods of time represent an estimate. a digital camera, digital images were produced at
Lower cooling rates are not technically relevant for various magnifications. The various microstructures
above mentioned metal forming processes with inte- occurring in the different materials are generally
grated heat-treatment since this cooling rate already differentiated by means of their characteristic size,
corresponds to a cooling period of more than 11 h to form, alignment and colour. Moreover, a microstruc-
reach room temperature from the hot forming tem- ture can be identified by using a low-load or micro
perature. hardness tester since the various microstructures
differ due to their structural hardness values. For
3.3. Metallographic specimen analysis measuring the phase fractions of the individual mi-
To quantitatively measure the microstructural crostructural constituents, the frequency distribution,
constituents following the dilatometry tests, the for example, of the micrographic images' brightness
specimens were first embedded at room temperature (histogram) can be employed. The software analy-
and longitudinal segments, along the specimen's axis SIS doc 5.0 was employed for differentially deter-
of rotation, were subsequently ground and polished. mining the microstructural fractions in the HIS-space
The preparation was carried out using a heat avoiding using the colour tones, saturation and intensity. For

© Metallurgical and Mining Industry, 2011, Vol. 3, No. 7 81

this purpose, the digital image data was initially pre-  L1 
pared in which the pixel errors were removed by k f  F  2
 (Eq. 2)
using median filters. In addition to this, the contrast    r0  L0 
was boosted using a DCE (differential contrast en- k f  a0   a1  expa2     exp a3  T  (Eq. 3)
hancement) filter. With respect to the individual
microstructural fractions, it can be assumed that the Since only flow curves at the forming tempera-
measuring error is just a few percentage points. ture of 1200 °C were recorded for the 34CrMo4,
50CrMo4, 51CrV4 and 34CrNiMo6 hardening and
3.4. Hardness measurements tempering steels, a regression analysis was performed
To characterize the hardness of the dilatometer by assuming that a3 = 0 is valid in this case.
specimens' microstructure, tests were carried out
4. Results and discussion
according to DIN EN ISO 6507-1 using either an
Instron-Wolpert-Testor 930/250 or a Duramin 20, 4.1. Flow curves
fully automated micro hardness tester made by the The measured flow curves modelled according to
company Struers. The functionality of the employed equation 3 are depicted in Figure 2. The curves' trajec-
hardness testing device was controlled prior to starting tories for the five alloys exhibit very similar profiles at
the test by means of a calibrated hardness-reference a forming temperature of 1200 °C. Here, the flow
piece. The relative error was less than 0.2 %. Four stress initially rises almost linearly and, following a
hardness measurements HV10 were performed on flattening, reaches a maximum flow stress of approx.
each of the dilatometer specimens in their unetched 55 MPa to 65 MPa at true strains of about 0.2 to 0.3.
condition. The respective mean values were calcu- Subsequent to this, the flow stress falls until the
lated and, where appropriate, supplemented by low- maximum true strain of 0.6 is reached at about 5 MPa
load hardness tests HV0.1 in the etched condition to to 10 MPa, respectively. Table 3 contains the parame-
identify the structural phase. ters determined according to equation 3 of the ap-
proach by Hensel and Spittel by specifying the coeffi-
3.5. Flow curves cient of multiple determination R2 and the maximum
The flow curves required for numerically repre- error ME as well as the respective austenitising tem-
senting the process were determined from steel perature TA. For example, the 42CrMo4 hardening and
specimens (5 mm diameter, 10 mm long) of the 5 tempering steel shows that the maximum flow stresses
alloys investigated here for an austenitising and a significantly increase from 67 MPa and 99 MPa to
soaking temperature of 1200 °C. For this purpose, the 190 MPa for decreasing forming temperatures from
specimens were inductively heated within 30 s to 1200 °C and 1050 °C to 850 °C, respectively. This
1200 °C. Following isothermal soaking for 600 s, corresponds to almost a tripling of the maximum flow
samples were plastic deformed to true strains of 0.6 stress. In comparison to the models according to
using a strain rate of 1 s-1. In addition to this, flow Hensel and Spittel [16], very good agreement within
curves for the 42CrMo4 hardening and tempering the considered interval is reached for forming tempera-
steel were determined for austenitising and forming tures of 1200 °C and 1050 °C. However, the flow
temperatures of 1050 °C and 850 °C. The logarithmic curve's profile measured here for the forming tempera-
or true strain φ and the flow stress kf corresponding to ture of 850 °C lies approx. 30 MPa above the values
equation 1 and equation 2, respectively, were com- specified by the model. Moreover, the drop in stress
puted from the measured force-displacement curve. following its maximum value at true strains of approx.
Plotting kf against φ gives the corresponding flow 0.2 to 0.3 remains neglected using the considered
curve where L0 signifies the specimen's initial length, model. Coefficient of multiple determination R2 for the
investigated alloy 34CrMo4 is comparatively low
L1 the current length and r0 the specimen's initial
since scattering of the five as an input used flow
radius. F is the measured applied force. For each
curves, though the approximation itself can be as-
combination of material and forming temperature,
sumed highly accurate.
five flow curve profiles each were evaluated and
using a regression analysis, a mean flow curve was 4.2. Evaluation of the microstructure
computed by employing Software Datafit 8.0.32 The CCT diagram for the steel 42CrMo4 (see
developed by the company Oakdale Engineering. Figure 3, top) exhibits ferritic, pearlitic, bainitic and
equation 3 was applied as the modelling approach martensitic constituents. The measured upper critical
according to a flow curve model of Hensel and Spit- cooling rate is 15 K s-1. Bainite is formed at cooling
tel [16], which takes into account the true strain and rates of between 6 K s-1 and 0.3 K s-1. Ferrite and
the forming temperature. pearlite can be established at cooling rates from
1 K s-1 and less (see Table 4). Between the regions of
L  martensite and bainite formation as well as between
  ln  1  (Eq. 1) bainite and pearlite formation there is a temperature
 L0  interval which is free of transformations.

82 © Metallurgical and Mining Industry, 2011, Vol. 3, No. 7

 70 250
1200 °C 42CrMo4
flow stress in MPa 60

flow stress in MPa

200 850 °C
50
40 150
34CrMo4 1050 °C
30 100
34CrNiMo6
20 42CrMo4
50CrMo4 50 1200 °C
10 51CrV4 [16]
0 0
0 0.1 0.2 0.3 0.4 0.5 0.6 0 0.1 0.2 0.3

logarithmic strain logarithmic strain

Figure 2. Flow curves according to equation 3 determined by means of a regression analysis for various materials and form-
ing temperatures; deformation rate 1 s-1. As a comparison, the computed flow curves according to the approaches of Hensel
and Spittel [16] are depicted in the right hand figure

Table 3. Regression parameters for the flow curves according to equation 3 each determined from the regression analysis of
5 measurements; R2: coefficient of multiple determination; ME: maximum error in %; TA: austenitising temperature

TA 1200 °C 850 °C to 1200 °C 1200 °C 1200 °C 1200 °C

alloy 34CrMo4 42CrMo4 50CrMo4 51CrV4 34CrNiMo6
a0 196 6000 175 180 233
a1 0.526 0.422 0.508 0.488 0.570
a2 -1.875 -1.335 -1.735 -1.613 -1.892
a3 0 0.003 0 0 0
R2 > 0.64 > 0.91 > 0.93 > 0.91 > 0.93
ME 12.5 9.1 5.8 6.1 4.8

Table 4. Metallographically determined microstructural constituents as well as hardness values of 42CrMo4 heat treatable
steel specimens for various linear cooling rates in K s-1 and true strains  at austenitising and forming temperatures of 850 °C

 K s-1 50 30 15 6 2 1 0.60 0.30 0.15 0.04 0.02

F - - - - - 2 4 6 15 12 15
P - - - - - *) 3 50 85 88 85
0 B - - - 4 18 42 58 27 - - -
M 100 100 100 96 82 56 35 17 - - -
HV 723 - 705 673 598 470 408 340 242 219 219
F - - - - - 3 3 4 5 12 15
P - - - - - *) 7 23 58 88 85
0.16 B - - - **) 12 45 59 40 37 - -
M 100 100 100 100 88 52 31 33 **) - -
HV 719 732 724 696 595 450 407 345 317 237 234
F - - - - **) **) 2 1 8 12 11
P - - - - - - 1 1 71 88 89
0.35 B - - - 3 17 44 68 90 20 - -
M 100 100 100 97 81 56 29 8 1 - -
HV 730 725 721 701 585 470 448 361 297 240 221

F: ferrite, P: pearlite, B: bainite, M: martensite, HV: Vickers hardness in HV10

*) Traces in the segregations, **) Traces in the microstructure

© Metallurgical and Mining Industry, 2011, Vol. 3, No. 7 83

 900

Ac3
800
ferrite
700 perlite
Ac1
temperature in °C
600
austenite

500

bainite
400

300 logarithmic
martensite
strain 0
200
1 2 3 4
10 10 10 10 time in s
900

Ac3
800
ferrite
700
Ac1 perlite
temperature in °C

600
austenite

500

bainite
400

300 logarithmic
martensite strain 0.16
200
1 2 3 4
10 10 10 10 time in s
900

Ac3
800
ferrite
700
Ac1 perlite
temperature in °C

600
austenite

500

bainite
400

300 logarithmic
martensite strain 0.35
200
1 2 3 4
10 10 10 10 time in s

Figure 3. Deformation CCT diagrams for the materials 42CrMo4 for logarithmic strains of 0 (top), 0.16 (centre) and 0.35
(bottom), austenitising temperature 850 °C

84 © Metallurgical and Mining Industry, 2011, Vol. 3, No. 7

 A deformation of 16 % (see Figure 3, centre) 300 °C. A comparison of the microstructural constitu-
produces a slowly accelerated ferrite transformation ents formed at different deformations exhibits reduced
together with bainite, which is also formed at lower fractions of pearlite at a cooling rate of 0.3 K s-1
cooling rates. The pearlite stage's temperature inter- (see Table 4 and Figure 4).
val is somewhat broadened. On increasing the de- The deformation tends to lead to a slight in-
formation further to 35 %, the ferrite's transformation crease in hardness values. As a consequence of the
temperature interval is also augmented (see Figure 3) broadening of the bainite field with increasing de-
and the start of the pearlite formation is shifted to formation, an additional increase in hardness results
slower cooling rates. The martensite's start tempera- at lower cooling rates due to the elevated bainite
ture drops with increasing deformation to below content.

50 µm
logarithmic strain 0 logarithmic strain 0.16 logarithmic strain 0.35
cooling rate 0.3 K s-1 cooling rate 0.3 K s-1 cooling rate 0.3 K s-1

Figure 4. 42CrMo4 hardening and tempering steel's microstructure cooled at 0.3 K s-1 for logarithmic strains varied from 0,
0.16 and 0.35 (2 % HNO3)

5. Conclusions consequence of the deformation and larger fractions

of bainite are formed. Furthermore, a drop in the
The work carried out here produced the follow- martensite start temperature is established.
ing results: Future work is planned to determine the trans-
The flow curves for the five hardening and tem- formation behaviour for austenitising and deforma-
pering steels considered here exhibit comparable tion temperatures from 1050 °C by using the
profiles possessing a maximum true strain at approx. 42CrMo4 hardening and tempering steel as an exam-
0.2 or 0.3 and maximum flow stresses from 55 MPa ple. In doing this, the investigations in [11] will be
to 65 MPa at deformation temperatures of 1200 °C. augmented and the complete deformation time-
In contrast to the data according to [16], a drop in the temperature-transformation behaviour for this mate-
flow stress can be discerned after attaining a maxi- rial would be recorded for the temperature interval
mum value. from 850 °C to 1200 °C.
i) Flow curves for the 42CrMo4 hardening and
tempering steel show a marked rise in the flow Acknowledgements
stresses by a factor of approx. 2.9 with falling defor-
mation temperatures within the temperature interval The authors would like to thank the German Re-
from 1200 °C to 850 °C. search Foundation (DFG) for their financial support
ii) For the hardening and tempering steel, a de- of the work carried out within the scope of the Col-
formation at the austenitising and deformation tem- laborative Research Centre 489, sub project A3 as
peratures of 850 °C exerts only a small influence on well as Ms. M. Reiter and Mr. K. Oelker for support-
the material's hardness value which exists following ing the materials’ and metallographic analyses. Spe-
cooling. In contrast to this, the hardness value is cial thanks go Dr. eng. B. Koczurkiewicz and Prof.
substantially influenced by the selected cooling rate. Dr. hab. inż. A. Milenin regarding the dilatometric
iii) The metallographic analyses show that the investigations at the Częstochowa University of
bainite field, in particular, broadens to later times as a Technology, Poland.

© Metallurgical and Mining Industry, 2011, Vol. 3, No. 7 85

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86 © Metallurgical and Mining Industry, 2011, Vol. 3, No. 7