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a r t i c l e i n f o
abstract
Article history:
Received 10 August 2012
Received in revised form
20 September 2012
Accepted 3 October 2012
Available online 9 October 2012
The process of tempering a martensitic medium carbon steel was investigated with the aim to study
resulting material properties. The experimental results were used to model residual stresses caused by
local heating, with the nite element method. Tempering was followed for times from 0.1 s up to 1 h by
using laser heating and conventional salt bath furnace treatments within the temperature interval
500700 1C. In addition, the thermal expansion was evaluated using dilatometry. Experiments showed
that the initial stages of martensite decomposition, associated with loss of crystal tetragonality, proceed
almost instantly. An initial large decrease of hardness within the rst tenth of a second of the tempering
process was measured, followed by only limited further softening with increased tempering time. Thus
for the current material the tempering time had limited inuence on hardness, governed primarily by
the peak temperature during the heating process. Finite element modelling of rapid local heating and
cooling showed that the tempering behaviour and associated dilatation effects yield a peak temperature dependent residual stress eld with a broad tensile stress distribution for the case of un-tempered
martensite. However, for tempered martensite the residual stress eld depends primarily on the
heating rate and peak temperature and shows large gradients with tensile stresses in the surface and
compressive below. Thereby, for both cases, residual stresses were obtained but with completely
different residual stress gradients.
& 2012 Elsevier B.V. All rights reserved.
Keywords:
Martensite tempering
FE
Flash heating
Dilatometry
Laser heat treatment
Residual Stresses
1. Introduction
Pearlitic steels are commonly used for a wide range of
applications due to their strengthwear properties and cost
efciency. In industrial processes like laser or electron beam
welding, laser ash hardening, adiabatic shearing and in operating environments such as wheelrail contact in railway trafc, the
material is sometimes subjected to rapid heating and cooling
within a localised volume [16]. Such local heating often has a
short duration and is normally followed by self-cooling with large
cooling rates. If the heating pulses cause peak temperatures above
some 400600 1C, softening of the pearlitic microstructure takes
place resulting in easier plastic deformation and distortion under
loading [7]. Even more important are heating cycles extending
over the austenitisation temperature (TA1) which may lead to
martensite formation during rapid cooling. The volumetric
322
Table 1
Chemical composition of material in wt%.
C
Mn
Si
Cr
Mo
Cu
0.50
0.75
0.37
0.12
o0.08
o0.06
o0.11
2. Experimental
Ferriticpearlitic steel with some 90 vol% ne pearlite and
10 vol% proeutectoid ferrite was used as a starting material. The
nominal chemical composition of the steel is presented in Table 1.
Martensitic material was obtained by austenitisation at 900 1C in
a tube furnace with protective argon atmosphere for 5 min and
thereafter quenched in brine. The Vickers hardness after this
treatment was 780710 HV30.
Samples for laser experiments were coin-like with a thickness
of 3.0 mm and diameter of 22.5 mm. To attain rapid heating and
cooling of the material, a 2.8 kW diode laser was used for heating
a spot on the sample surface. To have uniform laser radiation
absorption between samples, the radiated surface was ground
and then polished with 3 mm diamond suspension. The laser
beam was guided via an optical bre and defocused to a diameter
of 6 mm at the centre of the coin surface. The temperature within
the innermost 2 mm diameter of the laser exposed area was
measured with a pyrometer, using a sampling frequency of
60 kHz. The samples were mounted in a temperature controlled
copper sample holder within a vacuum chamber, evacuated down
to 10 8 bar during the experiments.
Tempering treatments for times longer than 10 s were made in
a salt bath furnace using sodium nitrate for tempering at 500 1C
and barium chloride salt for higher temperatures. Samples were
thin rectangular plates with 2 mm thickness. A type S thermocouple inserted within a reference sample was used to obtain the
actual sample temperature. Hardness indentation was made on a
cross-section to avoid inuence of thin decarburised layers on the
surface.
For laser tempered samples, hardness (HV5) was measured
along two orthogonal lines on the surface both crossing the centre
of the irradiated area. On a perpendicular section containing one
of the surface lines with surface hardness indents, hardness
mapping was made with a distance between indents of 0.5 mm.
Retained austenite in martensite was measured with X-ray
diffraction technique using an Xstress 3000 X-ray equipment
with vanadium Kb blocking lters.
Dilatometry was performed for martensite and pearlite by means
of a push-rod dilatometer, Netzsch Dil 402 C, with a tungsten
thermocouple in protective atmosphere. Thermal expansion and
solid state transformations of as-quenched and tempered material
were studied using single and multi-runs. Analyses were made for
different maximum temperatures up to 990 1C, all starting at 30 1C
(isotherm, 30 min before each run). Heating and cooling rates were
5 1C/min and 10 1C/min respectively. Alumina (Al2O3) was used as a
reference. Samples were cylindrical with diameter 6 mm and length
50 mm.
4. Analysis
4.1. Temperature control and thermal properties
The initial sample temperature was set to 20 1C. On mounting
into the sample holder the sample was assumed to be heated to the
temperature of the holder, which in accordance with the experimental setup was set to 100 1C. The laser heating of the most central
part of the surface was done with different powers for different
cases, and adjusted to achieve a top-hat temperaturetime curve in
conformity with the experiments. It was found in the experiments
that the peak temperatures dominate the following material behaviour by controlling the degree of tempering. Initial cooling was
modelled by lm cooling to the sample holder; however, the hottest
parts of the specimen were mainly self-cooled. As the material
models are formulated as rate-independent, the exact cooling curve
is not required when temperature gradients are low. Mechanical
interaction between the sample and the sample holder was
neglected. Final cooling to 20 1C was accomplished by setting a
temperature boundary condition to the nodes. A nal temperature
of 20 1C was required to allow comparisons with experimental
hardness data.
The power from the laser was applied on the top surface at
0rr r3.0 mm with scaling of absorption coefcient to achieve a
narrow temperature range during the time of exposure within the
pyrometer sampling area, 0 rr r1.0 mm. Temperature dependent specic heat and thermal conductivity were implemented
for the actual chemical composition of the coin sample based on
data from Thermo-Calc (Thermo-Calc software), reported in earlier publications [15].
4.2. Mechanical properties and dilatation
The elastic response of the material was implemented with
slight temperature dependence of the Youngs modulus E,
decreasing from 210 GPa at 20 1C down to 150 GPa at 700 1C
according to data from JMatPro6.0 (Sentesoftware) calculated for
the actual chemical composition. The plastic behaviour was
described using a material model with isotropic hardening predened in Abaqus. This model has the capability to account for
both temperature and solution dependent variables, in this case a
tempering parameter explained below. Underlying data were
compiled from own experiments (compression tests at temperatures from 25 to 275 1C), extrapolated to higher temperatures
323
5. Results
5.1. Hardness and microstructural evaluation after tempering
Fig. 2. Flow stress curves for as-quenched martensite (QM) and tempered
martensite (TM) at different degrees of tempering, and at different temperatures.
Points connected with lines represent experimentally performed compression
tests. Room temperature (RT) ow stresses are assumed to be proportional to the
decrease in room temperature hardness. High temperature behaviour above
275 1C extrapolated with JMatPro6.0.
Table 2
Subdivision of the computation into different computational steps (NBnot time steps, each step contains several time steps).
Computational
step
What is simulated?
Step 1
Nodes along symmetry y axis xed in radial direction, bottom node also in y
direction. Retained for all following steps. Temperature of all nodes
increased to 100 1C
Heat absorption on central part of top surface; otherwise insulated surfaces
Heat conduction to sample holder on bottom surface
Temperature of all nodes decreased to 20 1C
Step 2
Step 3
Step 4
324
5.2. Dilatometry
Two main tempering stages were observed for the martensite
(see Fig. 6), visible as dilatation effects on the linear thermal
expansion curve (DL/L0). The linear thermal expansion differentiated with respect to temperature (al al(T)) is also included. The
negative dilatation effect (starting with a negative slope of al)
with a peak value around 160 1C is associated with carbon
segregation and precipitation of transition carbides, presumably
e carbide. A second tempering stage ranging from 220 to 400 1C
was observed in the form of second negative dilatation effect,
indicating further decomposition into ferrite and cementite
[16,1921]. The small positive dilatation effect around 230 1C
may be related to transformation of retained austenite [20,22].
Yet, this effect is minor since present XRD measurements indicated a retained austenite content of less than 1.5%.
The behaviour for re-tempering of martensite was also studied
to obtain an understanding of how tempering and associated
volumetric shrinkage proceed as a function of the peak temperature for multiple heat cycles. One such double run is presented in
Fig. 6b, where the total thermal cycle consisted of a rst heat run
to 200 1C with subsequent cooling to 30 1C, and a second run to
570 1C with subsequent cooling. After the initial heat run no
dilatation effects were apparent in the subsequent run-up to the
peak temperature of the initial run, while above the peak
temperature of the initial run, tempering advanced accordingly.
For a multi-run with tempering to 570 1C in both cycles, the
length decrease was 0.22% after the rst run and practically none
for the consecutive.
Table 3
Different cases simulated. Approximate peak temperature (Tpeak) and time spent
within some 30 1C from Tpeak are given.
Case
Heating rate
Tpeak (1C)
Starting microstructure
M1
M2
M3
M4
M5
TM3
TM4
TM5
High
High
High
Low
Very high
High
Low
Very high
225
400
575
575
575
575
575
575
2
2
2
4
0.1
2
4
0.1
Un-tempered M, 780 HV
Un-tempered M, 780 HV
Un-tempered M, 780 HV
Un-tempered M, 780 HV
Un-tempered M, 780 HV
Tempered (600 1C), 408 HV
Tempered (600 1C), 408 HV
Tempered (600 1C), 408 HV
5.3. FE simulations
The inuence of peak temperature on the residual stresses
of un-tempered martensite was studied via cases M1M3
(cf. Table 3), and the inuence of heating rate and time at peak
temperature was examined in M4M5. For tempered martensite,
only the inuence of heating rate and time at peak temperature
(combined) was studied in TM3TM5, as heating at lower
temperatures did not generate residual stresses, as will be
discussed later. Temperature curves for the centre node on the
top surface for all cases are shown in Fig. 7.
The radial stress for case M5, the case with the highest
temperature gradients is shown in Fig. 8. The stress distribution
just before cooling (Tpeak E575 1C) is shown in Fig. 8a; the peak
stress is approximately 550 MPa. The von Mises stress has
approximately the same magnitude and is not sufcient to
plastically deform the material; this is valid in every location
and every time step for all of the cases M1M5. The radial stress
distribution for M3 after nal cooling to room temperature is
shown in Fig. 8b.
The radial stresses for case TM3 are shown in Fig. 9a. The
stress at the centre reaches 240 MPa, and rapidly declines;
predominantly the volume which was plastically deformed during heating shows large tensile stresses (Fig. 9b).
Depth proles of radial stresses for all cases along the centre
line after nal cooling are shown in Fig. 10. For case M1 stresses
are small, below 25 MPa. Case M2 shows a maximum radial stress
of around 100 MPa, decreasing towards the bottom surface, while
case M3 has a more even distribution of residual stresses, as most
of the dilatation differences have been exploited through the
entire sample thickness (the peak temperature at the centre line
towards the bottom of the sample is around 370 1C). Case M4 is
more extreme in this respect and stress levels are lower as a
larger part of the coin has decreased its volume (heating the
entire coin to the same temperature would give only shrinkage,
no residual stresses). M5, on the other hand, shows that the larger
temperature gradients achieved with rapid heating give correspondingly larger gradients in residual stresses. The fact that all
cases M1M5 show somewhat lower stresses at the surface is
believed to be due to the increasing degree of plane stress
condition naturally prevailing on a free surface. As seen from
the stress elds, the stresses were below the yield stress for all
locations in M1M5 (see Fig. 2); thus the strains are caused by
volume decrease upon tempering of martensite and to some
degree of warping of the sample. The most obvious difference
for the tempered materials (TM3TM5) is the much shallower
Fig. 4. Hardness maps for cross sections of tempered samples. Downward facing triangles represent surface hardness as measured before sectioning, while each diamondshaped mark represents an indent on the cross-section. Hardness scale bar applicable to all graphs. (a) 600 1C; 0.1 s, (b) 600 1C; 0.4 s, (c) 600 1C; 4.9 s, (d) 700 1C; 0.4 s and
(e) 500 1C; 0.4 s.
325
Fig. 5. Scanning electron micrographs (in-lens secondary electron detector). (a) Comparison of initial martensitic microstructure and (b) tempered at 700 1C for 0.1 s.
Carbide precipitates are brightly imaged in the tempered martensite.
Fig. 7. Temperaturetime curves for nodes on the heated surface. Time for heating
from room temperature to 100 1C (temperature of sample holder) and the nal
abrupt cooling to room temperature is arbitrary (needed for computational
reasons).
6. Discussion
6.1. Martensite tempering
326
Fig. 8. Radial stresses overlaid on the deformed mesh; deformations magnied 50 . (a) Case M5 before cooling. The peak stress is not sufcient to plastically deform the
material. (b) Case M3 after cooling to room temperature. Shrinkage due to local martensite tempering is clearly seen.
Fig. 9. (a) Radial stresses (MPa), and (b) accumulated plastic strain ( ) of case TM3 after cooling to room temperature. Deformations magnied 50 .
Fig. 10. Radial stresses after cooling to 20 1C for all cases in Table 3.
Fig. 11. Comparison of thermal expansion for tempered martensite and pearlite;
the behaviour is similar.
327
7. Conclusions
Tempering characteristics of a medium carbon steel in martensitic condition were examined for tempering times ranging
from 0.1 s to 1 h. Resulting material properties were studied
primarily by the indentation technique, and characterisation of
thermal expansion and solid state transformation were made by
dilatometry. Using the experimental results, residual stresses
arising on rapid local heating with subsequent cooling to room
temperature have been evaluated using the nite element analysis for as-quenched and tempered martensite. The following
conclusions were drawn:
Acknowledgement
This investigation has been performed within the National
Centre of Excellence CHARMEC (Chalmers Railway Mechanics).
Authors are grateful for cooperation with Materials Center Leoben
regarding laser tempering experiments. Peter Krahl and Alexandre Gorski are acknowledged for help with experimental work.
328
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