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art ic l e i nf o
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Article history:
Received 28 August 2014
Received in revised form
5 February 2015
Accepted 9 February 2015
Available online 17 February 2015
The effect of heat treatment on microstructure and abrasive wear resistance of AISI D2 steel has been
investigated in the present work. The structural characterization of hardened and multiple tempered
specimens was carried out using scanning electron microscopy (SEM), energy dispersive spectrometer
(EDS) and X-ray diffraction (XRD). Two body abrasive wear tests were carried out using silicon carbide
abrasive with systematic and simultaneous variation of test parameters. The abrasive wear volume loss
increased with increasing tempering temperature and increasing severity of test conditions, although
the increase was not proportionate. The worn out surface, wear debris and subsurface damage were
examined using SEM, EDS and XRD. The results of present work were rationalized with respect to
microstructure and operating wear mechanisms as inuenced by severity of wear test conditions.
& 2015 Elsevier B.V. All rights reserved.
Keywords:
Two body abrasion
Hardness
Steel
Wear testing
Electron microscopy
1. Introduction
High-carbon high-chromium (HCHCr) steels were rst developed as a substitute for high speed (HS) steels, but were found to
be of limited use due to insufcient hot hardness and brittleness.
However, these steels proved useful in applications where high
wear resistance and non-deforming properties were required e.g.
in dies and punches [14]. The high wear resistance in HCHCr
steels is attributed to high volume fraction of hard chromium
carbides [4]. D2 steel nds applications in drawing and forming
dies, cold drawing punches, blanking/stamping dies and extrusion
dies. Die steels are usually subjected to compressive-tensile
stresses, shear stresses and hence die steels require high strength
and toughness apart from good wear resistance [5].
In general, an increase in hardness of material results in an increase
in its wear resistance. This correlation is true only in case of pure
metals in the annealed condition and alloys of same family [6]. The
research investigations in the past have focused on improvement of
the wear resistance mainly by alteration of microstructure by using
conventional heat treatment techniques. The abrasive wear loss has
been reported to decrease with increase in the volume fraction of
martensite. It has also been reported that the hardness of martensite
has a greater inuence on the abrasive wear resistance of steels than
its volume fraction [79]. The martensitic microstructure with carbides
exhibited better wear resistance as compared to bainitic or pearlitic
microstructures [10]. The abrasive wear in steels with multiphase
n
207
2. Experimental method
2.1. Material and heat treatment
The material used in the present investigation (AISI D2 steel) was
obtained in form of a forged bar of 100 mm diameter. The chemical
Table 1
Chemical composition (weight%) of D2 steel.
Elements
Mn
Si
Cr
Mo
Fe
Wt%
1.5
0.45
0.3
12
0.9
0.03
0.03
1.0
Balance
Table 2
Summary of test parameters used for abrasive wear of D2 steel in the present work.
(Constant test parameters: linear velocity 0.8 ms 1 and specimen rotation
50 rpm).
Specimen designation
AN
AN
OQ
T523
T723
T923
10,20,30 and 40
20 N
10
20
30
40
10
20
30
40
10
20
30
40
10
20
30
40
52
52, 92, 122 and 320
52
92
122
320
52
92
122
320
52
92
122
320
52
92
122
320
Fig. 2. Secondary electron scanning electron microscopy (SEM) images of the abrasive papers used for the wear tests (a) 80 grit (320 m) (b) 150 grit (122 m) (c) 220 grit
(92 m) and (d) 320 grit (52 m).
208
Fig. 4. SEM micrographs of heat treated specimens showing size, distribution and morphology of carbides for different conditions (a) annealed at 1158 K (b) as-quenched
after austenitizing at 1303 K (c) quenched and tempered at 523 K (single stage) (d) quenched and tempered at 623 K (two stage) (e) quenched and tempered at 723 K (three
stage) (f) quenched and tempered at 823 K (four stage) (g) quenched and tempered at 923 K (ve stage). All the samples were etched with 2% Nital to reveal the matrix
(dark) followed by etching with Vilella's reagent to reveal the carbides (bright).
(Bruker XFlash) attached to SEM and XRD to study size, distribution and morphology of carbides, to obtain chemical composition
of the carbides and to determine retained austenite content. The
specimens for microstructural observations were prepared using
standard metallographic polishing techniques followed by etching
with 2% Nital and then with Villella's reagent for 10 s each [3132].
XRD patterns were measured using PANalytical Xpert Pro MPD
system with Cu-K radiations and diffracted beam monochromator. The XRD patterns were then analyzed using XPert Highscore
software to obtain type of carbides and retained austenite (RA)
[3334]. For the measurement of RA, {220} and {200} peaks of
austenite and {200} peak of ferrite were considered.
2.3. Abrasive wear tests
Two body abrasive wear tests were carried out on pin-on-plate
abrasive wear test apparatus [35] (DUCOM make, India) as shown in
Fig. 1. The commercially bonded silicon carbides paper with
different particle sizes was used as abrasive media. Fig. 2(ad)
shows secondary electron SEM micrographs of silicon carbide (SiC)
abrasive paper with average particle size of 320 m, 122 m, 92 m
and 52 m used in the present study. The shape of SiC abrasive
209
particles was predominantly angular, although ner particles exhibited relatively greater angularity. The specimens for abrasive wear
tests were in the form of pin (cylindrical shape) with the length
25 mm and diameter of 10 mm. The specimens were metallographically polished prior to each wear test. The objective of simultaneous variation of abrasive particle size and load was to examine
regime of wear i.e. mild, moderate or severe as reected in abrasive
wear loss. The data on the effect of simultaneous variation of test
parameters on abrasive wear of die and tool steel is scarce. The
objective was also to assess the change in mechanism of material
removal from the matrix and the carbides associated with change in
tempering temperature and tempering cycles (single stage to ve
stage) with respect to severity of abrasive wear test conditions. Two
body abrasive wear tests were conducted as per the experimental
conditions mentioned in Table 2. The mass loss was well distributed
over the surface due to rotation of specimen, which also avoids the
possibility of intense wear of the edges. The lateral displacement of
specimen ensures that the specimen always traverses new track.
The specimens were cleaned with ethanol and weighed using
digital micro-balance (to an accuracy of 0.1 mg) prior to and after
each wear test. The difference in the initial and nal weight of
the sample was recorded to calculate abrasive wear loss. Two
210
Table 3
Chemical composition of primary and secondary carbides (wt%) as determined by
energy dispersive spectrometer (EDS).
As-quenched
Weight %
Primary carbides
Secondary carbides
Fe
Cr
Si
88.25
51.19
11.06
44.67
0.69
0.22
o 0.05
o 0.05
90.54
93.88
8.82
6.21
0.49
0.37
o 0.05
o 0.05
51.83
48.03
0.07
o 0.05
92.58
51.05
8.03
46.84
0.57
0.29
o 0.05
0.11
91.39
8.15
0.46
o 0.05
Retained austenite
(%)
As-quenched at 1303 K
17.20
Quenched and tempered at 523 K (single tempered)
17.00
Quenched and tempered at 723 K (three stage
11.82
tempered)
Quenched and tempered at 923 K (ve stage tempered) 6.39
Fig. 6. High resolution indexed X-ray diffraction patterns of (a) as-quenched sample (b) quenched and 523 K tempered sample (single stage) (c) quenched and 723 K
tempered sample (three stage) and (d) quenched and 923 K tempered sample (ve stage).
211
sequence has been reported for a study on En31 steel [40]. The
XRD patterns of the as-quenched, quenched-tempered 523 K,
quenched-tempered 723 K and quenched-tempered 923 K D2 steel
samples are shown in Fig. 6. The XRD data supplements SEM
observations on microstructural changes associated with multiple
tempering treatment of D2 steel. The as-quenched D2 sample
showed the presence of martensite (indexed as ferrite, since the
resolution of the diffractomter was not sufcient to resolve the
tetragonality of the martensite), alloyed cementite (indexed as Fe3C),
Fig. 8. Abrasive wear volume loss (cm3) vs. simultaneous variation of load and
abrasive particle size at a velocity of 0.8 m/s and rpm of 50.
Fig. 9. Variation of abrasive wear volume loss (cm3) as a function of hardness (HRc)
at a load of 10 N and 40 N.
Fig. 7. (a) Abrasive wear volume loss (cm3) as a function of load for annealed specimen for abrasive particle size of 52 m. (b) Abrasive wear volume loss (cm3) as a function
of abrasive particle size for annealed samples at a load of 20 N and at a velocity of 0.8 cm/s and at 50 rpm.
212
Fig. 10. (a,b): SEM micrographs of worn out surface of quenched and tempered specimens of D2 steel at a load of 40 N. (a) tempered at 723 K (triple tempering) and (b) ve
stage tempered at 923 K.
Fig. 11. (a,b): SEM micrographs of heat treated D2 steel after short duration abrasive wear test for quenched and tempered sample at 723 K (a) 10 N (b) 40 N. (c,d ): Subsurface SEM micrographs of worn out samples at 40 N load (a) as-quenched, (b) quenched and tempered at 523 K (single stage).
increased linearly and the volume loss at highest load (40 N) was
approximately two times as compared to that observed at the
lowest load (10 N).The abrasive wear volume loss increased with
the increase in the particle size as shown in Fig. 7b. With the
increase in particle size from 52 m to 122m, the increase in
the volume loss was approximately 1.6 times, whereas for increase
in particle size from 122 m to 320 m, the increase was only
marginal. These results can be understood in terms of particle size
effect, which can be attributed to clogging, adhesion of wear
debris to the tip of abrasive particle thus reducing its cutting
efciency, fracture of abrasive particles and increase in local ow
stress with decreasing scale of deformation for ner abrasive
particles leading to reduced wear loss [6,42,43]. In the annealed
condition, the matrix is very soft and the increase in load is
expected to result in higher depth of cut resulting in material
removal proportional to the applied normal load. SiC particles
have higher hardness as compared to the Cr7C3 carbides and hence
are expected to cause indentation and fracture of the carbides
since ratio of Ha/Hs ( ratio of hardness of abrasive to that of
carbide) was greater than 1.2 [6]. Fig. 8 shows the effect of
simultaneous variation of load and particle size of abrasive on
abrasive wear volume of heat treated D2 steel. The data points
were tted by best t line and regression coefcients were in the
range of 0.930.95. It can be observed that with the increase in
severity of wear condition from (10 N, 52 mm) to (40 N, 320 mm)
abrasive wear volume loss increased for D2 steel irrespective of
the heat treatment condition. The abrasive wear volume loss
213
V KHm
Fig. 12. SEM micrographs of wear debris of (a) and (b) as-quenched samples, (c) and (d) quenched and 523 K tempered samples (single stage), (e) and (f) quenched and
923 K tempered samples (ve stage). For (a), (c) and (e) the load used was 10 N, while for (b), (d) and (f), the load used was 40 N.
214
Fig. 13. High resolution X-ray diffraction (XRD) pattern of wear debris of D2 steel for (a) as-quenched (b) quenched and 523 K tempered (single stage) (c) quenched and
723 K tempered (three stage) and (d) quenched and 923 K tempered (ve stage) samples at a load of 40 N.
intensity for all the heat treated conditions which implied that the
wear mechanism was oxidative. The iron oxide lm provides a
lubricating lm with low shear strength reducing the friction between
surface and abrasive particles subsequently subsiding the effects of
capping and clogging [6]. At higher load and coarser particle size, iron
oxide lm is penetrated by abrasive particles with exposure to fresh
metal surface with increased wear loss. There was no formation of
white layer for very high loads for D2 steel as reported in a previous
study [25]. The above observations also indicate that D2 steel is
relatively more abrasive wear resistant under mild to moderate
abrasive wear conditions. From the above it can be concluded that a
combination of wear mechanisms was responsible for material
removal and the relative contribution of each (e.g. Plowing, microcutting, edge fracture, chipping, gross fracture of carbides, carbide pull
out) was decided by structural transformations associated with
tempering treatment and morphology of carbides. This can explain
the abrasive wear loss trends obtained in the present investigation
with increase in tempering temperature and with change in abrasive
wear test conditions from benign to relatively severe one. From the
results of the present investigation, it can be also pointed out that it is
difcult to pin point the effect of retained austenite (617%) in heat
treated D2 steel on the improvement of abrasive wear resistance. This
is further supported by the observation that abrasive wear volume
loss of heat treated D2 steel showed nearly similar dependence on
surface hardness at both lower and higher loads as indicated by the
hardness exponents. In fact, the contribution of change in mechanism
of material removal to abrasive wear resistance of D2 steel with
increasing severity of abrasive wear test conditions was more
signicant as compared to the effect of retained austenite. It is
difcult to compare the results of the present work with those of
previous studies due to different processing conditions, mode of wear,
conguration of the test apparatus and the test conditions, as far as
the effect of retained austenite on abrasive wear resistance is
concerned [28,47].
4. Conclusions
1. The morphology of carbides became coarser with increasing tempering temperature during multiple tempering treatment of D2 steel.
2. D2 steel in the as-quenched condition exhibited highest abrasive wear resistance which was attributed to martensitic
microstructure with ner morphology of carbides.
3. The simultaneous variation of load and abrasive particle size
increased abrasive wear volume loss with increasing temperature.
4. The dependence of abrasive wear resistance of heat treated D2
steel on hardness was almost similar irrespective of the load.
5. The relatively higher abrasives wear rate exhibited by multiple
tempered D2 steel at higher tempering temperature was due to
softer matrix and coarser morphology of carbides.
6. The abrasive wear resistance of tempered D2 steels was
predominantly inuenced by morphology of the carbides,
nature of the matrix and the change in mechanism of material
removal from benign to relatively severe test conditions. The
retained austenite had relatively minor effect on abrasive wear
behavior of heat treated D2 steel.
Acknowledgment
The authors are grateful to Director, VNIT Nagpur for providing
necessary facilities in carrying out this investigation. The authors
are also thankful to Mr. S. L. Gadge and Mr. Avishkar Rathod for
their help during heat treatment and SEM work.
215
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