Short Paper

Proc. of Int. Conf. on Advances in Mechanical Engineering 2012

Abrasive Wear Properties of Plasma Nitrided H11

Steel
S.G.Sapate1, Amit Kumar2, R.K.Khatirkar3, S.Chandel4,
1, 2,3
Department of Metallurgical and Materials Engineering, South Ambazari Road, VNIT Nagpur – 440011
Email: sgsapate@yahoo.com
4
HAL Bangalore

Abstract—In the present work, abrasive wear studies were In the present work, abrasive wear studies were carried out
carried out on hardened and tempered H11 steel and plasma on surface hardened and tempered H11 steel and plasma
nitrided H11 steel. Plasma nitrided coating was characterized nitrided H11 steel. Plasma nitrided coating was characterized
by metollography and image analysis. Micro hardness by metollography and image analysis. Micro hardness
measurement was made on surface of plasma nitrided steel.
measurement was made on surface of plasma nitrided steel.
Abrasive wear studies were carried on plasma nitrided H11
steel with sand abrasive Plasma nitrided and surface hardened Abrasive wear studies were carried on plasma nitrided H11
and tempered H11 steel showed considerable difference in steel. Plasma nitrided and surface hardened and tempered
abrasion rates, under different abrasion condition. Plasma H11 steel showed considerable difference in abrasion rates,
nitrided coated H11 steel exhibited lower wear rates as under different abrasion condition. Plasma nitride coated
compared to hardened and tempered H11 steel. SEM studies H11 steel exhibited lower wear rates as compared to hardened
were made on worn surface of coated steel to study morphology and tempered H11 steel. SEM studies were made on worn
of worn surfaces. surface of coated steel to study morphology of worn surfaces.
Index Terms— Steel, hardening, tempering, plasma nitridng,
II. EXPERIMENTAL
nitrides, abrasion
In the present work H11 steel samples were used. The
I. INTRODUCTION chemical composition was determined by using wet analysis
and is given in Table1. The chemical composition of H11
Surfaces of engineering components are often nitrided to
steel was ( wt %) ; C-0.38, cr-4,85, Mo-1.32, Si-).9, Mn-0.42, V-
improve their corrosion, fatigue and wear properties prior to
0.42, Ni- 0.23 %. The Heat Treatment was carried out an H11
use in different types of applications. During nitriding,
steel specimens prepared for abrasive wear testing. The
nitrogen diffuses into the steel surface, where it combines
carbon content of the steel suggests that the steel is a hypo-
with alloying elements such as chromium and aluminium to
eutectoid steel consisting of pearlite and ferrite in the as
form fine dispersion of alloy nitrides. These precipitates
received state. This steel was quenched from 960OC ± 5
strengthen the surface region and introduces beneficial
(soaking time – 60 minutes). leading to formation of martensite
compressive stresses at the surface. Therefore, the response
with some retained austenite. This quenched steel was
of steel to the nitriding treatment depends principally on its
tempered at 580OC.
composition and the process temperature[1-6].
The hardened and tempered specimens were polished to
The significant advantage of nitriding is that it causes
the surface roughness of before plasma nitriding. The
less distortion than hardening & carburising, because of
hardned and tempered specimens were then nitrided in a
relatively low processing temperature, usually below 570OC.
commercial sensor – controlled plasma nitriding furnace pulse
The minor probability of surface distortion and dimensional
plasma mode at Sumeet Surface Technologies, Pune.
variations also makes it possible to reduce or even to eliminate
Specimen were nitrided at 10KHZ of pulse frequency and on
the need for expensive finishing operations before the
time of 90%. Plasma nitriding was carried out at 500OC for 10
component is put into surface on the other hand, nitriding
hour in25H2–75%N2 atmosphere at pressure of 3 mbar. The
causes the formation of a compound or white layer of iron
specimens were subjected to metallography examination
nitride, e.g. Fe2—4 N, at the surface. Although this layer has
before and after plasma nitriding. The specimens were ground
high hardness of 900-1100 HV and good frictional
and polished with successive emery papers 1/0, 2/0, 3/0, 4/0
characteristic, high internal stresses makes it friable and brittle,
followed by polishing with diamond paste (0.5 µm). Polished
which can often lead to spalling during service. This fact
specimen were etched with 2% Nital for observation of
somewhat restrict the use of nitriding process. In addition to
microstructure.
hardness and wear resistance, fatigue strength is significantly
The bulk hardness of as received, heat-treated specimens
increased by plasma nitriding. Parts where nitriding is not
and plasma nitrided specimen was measured using Rockwell
required can be shielded by simple mechanical masking. With
hardness tester at load of 150 Kg. an average of three reading
the lower distortion to work piece, plasma nitriding has no
was reported in the result as shown in Table 1. The specimens
environmental hazards. The plasma nitriding of stainless steel
for micro hardness measurement were prepared for in a similar
and alloy steels is documented in the literature[7-18], however
way as that for metallography. The micro hardness was
abrasive wear properties of nitrided H11 steel is not reported.
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Proc. of Int. Conf. on Advances in Mechanical Engineering 2012

measured by using a Shimadzu make micro hardness tester.

An average of five reading was reported in the Table I
TABLE I. HARDNESS AND MICRO H ARDNESS OF H11 STEEL

Fig. 3 Photograph of Pin on Disc Apparatus

Fig. 1. Micro structure of Heat Treated H-11 Steel (500X)
After the test was over the specimen was cleaned with
alcohol and final weight was measured using digital electronic
balance. The loss in mass(g) was calculated as the difference
of initial and final weight of the specimen. The abrasive wear
tests were carried on heat treated specimen and plasma
nitrided specimens.
The effect of load on wear loss was studied at a load of
0.5, 1, 1.5 and 2 kg. at 300 rpm. In other set of experiment, load
and sliding velocity was simultaneously changed, i.e., 0.5kg.
1.32m/sec, 1Kg., 1.98m/sec, 1.5Kg, 2.64m/sec, and 2 Kg. 3.3m/
sec. The abrasive medium used was 150 µm sand paper. To
assess the effect of operating parameters on morphology of
worn surface, abraded surfaces were examined under Scanning
Electron Microscope.

III. RESULTS AND DISCUSSION

The change in surface roughness caused by plasma
nitriding was measured by Tallysurf (Series-II, Taylorhobson
Fig. 2. Micro structure of plasma nitride H-11 Steel (500X) profilometer. After nitriding the average roughness value Ra
of the original grounded surface had increased. The average
The microstructure of Heat treated and plasma nitrided
roughness of the original grounded surface has increased
specimen of H-11 steels are shown in figure. The
from 0.1095µm to 0.4147µm. The roughness profile of nitrided
microstructure of heat Treated specimen shows very fine
and unnitrided (heat treated) surface is shown in the Fig. 4
tempered martensite with very fine carbide particles.The
(a&b). Surface roughness was measured to know the change
surface roughness was measured using profilometer before
in surface roughness caused by plasma nitriding. After nitriding
and after plasma nitriding. In order to determine the coating
the average roughness value Ra of the original grounded
thickness, cross section of plasma nitrided specimen of H-11
surface increased. The average roughness of the original
steel was analysed with Image Analyzer [Leco, USA]. The
grounded surface increased from 0.1095µm to 0.4147µm.
specimen for Image Analysis was prepared in same way that
Crystal growth of iron nitride layer at the surface of the work
for metallography. Specimen was etched by 4% Nital. The
piece may cause an increase in the surface roughness. Similar
thickness of Plasma nitrided coating zone was measured by
results have been reported by B.Podgornik and co workers
Image Analysis. Measurement was taken at different points
[15] in plasma nitrided AISI 4140 steel. In plasma atmosphere
at cross section and average of four reading was reported in
of 99.4%H2 – 0.6%N2 roughness increases from 0.3µm to .65
the results which was 75 micro meter.
µm where as in 75%H2 – 25%N2 atmosphere surface roughness
The abrasive wear resistance of surface treated flat ended
increases by 1.27µm Increases in surface roughness depends
pins was determined by using pin on disc machine (Ducom
upon nitriding conditions it has been proved in previous
make, Bangalore) as shown in Fig 3. The specimens for
studies. The micro hardness measurement results are shown
abrasive wear test were cylindrical pins having diameter of
in Table I. The plasma-nitriding treatment resulted in to
10mm & length of 25mm. The specimen were cleaned with
increase the surface hardness of material in comparison with
alcohol before measuring initial weight with digital electronic
the as received material, which has the hardness of 538H.V0.1.
balance to accuracy of 0.1 mg. Abrasive paper (sand paper)
The plasma nitrided specimen has hardness of 1088 H.V0.1.
was fitted on moving disc. The required track radius is
Nitrogen diffuses in the steel from the surface to the core.
obtained by adjusting the traverse of sliding assembly. The
During the the diffusion process, nitrogen partly replaces
desired load was placed on loading pan which is connected
carbon in the martensite, and forms steel nitrides such as iron
with pulley arrangement to loading arm.
© 2012 AMAE 114
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Proc. of Int. Conf. on Advances in Mechanical Engineering 2012
Fig. 4. (a) Surface Roughness Profile of Plasma Nitrided H11 Steel
(b) Surface Roughness Profile of hardened and tempered H11 steel
nitrides and chromium nitrides in the matrix and also at grain
boundaries.
Redistribution of carbon occurs in the diffusion zone,
and carbon is pushed back towards the core region. Near the
surface concentration decreases and towards the core region
higher concentration of carbon is observed in comparison to
overall carbon concentration [4]. Diffusion of nitrogen and
redistribution of carbon in the diffusion zone are function of
nitriding temperature and time. Increasing the time beyond
10 hours decreases the surface hardness of materials. A similar
decrease in hardness with increase in plasma-nitriding time
has been observed with plasma nitrided stainless steel
material [7,19,20]. A typical diffusion zone is shown in Fig. 5.
         Diffusion layer core
Fig. 5. Micrograph of Plasma Nitrided Coating (500X)
Thick diffusion zone can be observed from optical
micrograph shown in Fig. 5. In diffusion layer a dispersion of
nitride precipitate in metal matrix enriched in nitrogen is
observed. Similar structure of diffusion layer was observed
by F. Borgioli & co workers [2], while studying H11 steel,
plasma nitrided at 500OC for 5 hour, under gas atmosphere of
80 volume %N2-20 volume % H2.
© 2012 AMAE
DOI: 02.AETAME.2012.3.507
The results of abrasive wear studies under different test
conditions are shown In Fig. 7(a-d). The effect of load and
sliding velocity on volume loss for heat treated ( A) and plasma
nitride specimen (B). The data points were fitted by straight
line and slope of the line each case indicated volume wear
rates under different tets conditions.
TABLE II. VOLUME WEAR RATE AND R2 VALUE AT VELOCITY OF 1.32 M/S OF
SPECIMEN ‘A’ WHEN ABRADED WITH SAND PAPER.
It can be observed from Table II that volume wear rate at
0.5kg. load was 0.0004mm3/m which increased to 0.0007mm3/
m at 1kg. load, that is volume wear rate increased 1.75 times.
At 1.5 kg. load volume wear rate was 4.5 times and at 2kg.
load volume wear rate was six times more than that observed
at 0.5kg. load.
At sliding velocity of 1.32m/sec and 0.5kg. load, total volume
loss was 2.0358mm3 which increased to 6.3508mm3 at 1kg.
load and at velocity 1.98m/sec. thus more than three times
increase in volume loss was observed. The total volume loss
increases to 9.8335mm3 at 1.5kg. at velocity 3.3m/sec, total
volume loss was 53.5595mm3 which was twenty six times to
that at 0.5kg. load and 1.32m/sec. The volume wear rates
were calculated from slope of straight lines as given in Table
III.
TABLE III. VOLUME WEAR RATE AND R2 VALUE O F SPECIMEN ‘A’ WHEN
ABRADED WITH 150 µM SAND PAPER AT D IFFERENT VELOCITIES.
The volume wear rate increased 3.75 times at 1kg., 1.98m/
sec, where as volume wear rate increased to more than five
times at 1.5kg., at velocity of 2.64m/sec, than that observed
at 0.5kg., 1.32m/sec velocity. Under severe conditions (load
of 2kg. and velocity of 3.3m/sec), wear rate increases to 28
times than that observed under mild condition (1kg., 1.32m/
sec).
TABLE IV. VOLUME WEAR RATE AND R2 VALUE O F SPECIMEN ‘B’, WHEN
ABRADED WITH 150 µM SAND PAPER AT 300 R PM
.
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It can be observed from Table IV that volume wear rate at
2kg. load was more than 3 times than observed at 0.5kg. load
at same velocity. At 1.5kg. load increase in volume wear rate
was only 1.6 times more than that at 0.5kg. load, where as
only marginal increase in volume wear rate was observed at
1kg. load.
When the load and sliding velocity was simultaneously
changed, the plasma nitrided specimen ‘B’ exhibited different
trends in volume loss. The total volume loss at load 0.5 kg. at
velocity of 1.32m/sec was 1.2548mm3 which increases to more
than 2 times at 1kg. load and at velocity 1.98m/sec. The total
volume loss at load 1.5kg. at velocity 2.64m/sec was nearly 4
times that observed at 1.5kg. load and at velocity 1.32m/sec.A
increase in total volume loss at load of 2 kg. and velocity
3.3m/sec was observed which was nearly 8 times than that
observed at load of 0.5kg. and at velocity 1.32 m/sec.The
volume wear rates are shown in Table V.
TABLE V. VOLUME WEAR RATE AND R2 VALUE O F PLASMA NITRIDED SPECIMEN
WHEN ABRADED WITH 150 µM SAND PAPER AT DIFFERENT VELOCITIES.
Fig. 6. (a) Effect of load on volume loss of heat treated specimen
of H11 steel at 300 rpm when abraded with 150µm sandpaper
Fig. 6. (b) Effect of load and velocity on volume loss of
heat treated specimen of H11 steel(C=0.5kg., 300RPM,
D=1 kg., 450RPM, E=1.5kg., 600RPM, F=2kg, 750RPM.)
© 2012 AMAE
DOI: 02.AETAME.2012.3.507
Fig. 6. (c) Effect of load on volume loss of plasma
nitrided Specimen of H11 steel when abraded with 150µm sand
paper
Fig. 6. (d) Effect of load and velocity on volume loss of plasma
nitrided specimen of H11 steel when abraded with 150µm sand
paper (C=0.5kg., 300RPM, D=1kg., 450RPM, E=1.5kg., 600RPM,
F=2kg., 750RPM)
Fig. 7 (a-c) show SEM photograph of worn surface of
specimen A when abraded with sand paper at load of 1.5kg at
600 rpm, severe scratches with scratches lying parallel to
each other can be seen. As seen from 8(a) that width of
grooves ranges between 5-10 mm. The material is removed
by process of micro-ploughing and cutting. In Fig 8(a)
abrasive particle embedded in grooves can also be observed.
With increase in load from 0.5 kg to1.5kg, the depth of cut by
abrasive particles increases resulting in more wear loss as
shown in 8(b). The worn coated surface of H11 steel when
abraded with sandpaper at load of 2kg is show in Fig 8(c).
The spalling of coating is observed at few places. The rupture
of coating can also be observed at center of photograph. In
comparison at lower load of 1kg no gross spalling of plasma
nitrided coating was observed as shown in Fig. 8(c) resulting
in lower wear rates as compared to hardened and tempered
H11 steel.
CONCLUSIONS
Plasma nitrided coating on H11 steel exhibited increase in
surface roughness. The volume wear rate of heat treated H11
steel increased six times when the load was increased from
0.5kg to 2kg at velocity 1.32m/sec. At 2kg load and 3.3m/sec
velocity, heat treated H11 steel exhibited more than twenty
five times increase in volume wear rate as compared to load
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at 0.5kg, at velocity 1.32m/sec. The volume wear rate of
plasma nitrided specimen increased linearly with sliding
distance. The increase in volume wear rate was only three
times when the load increased from 0.5kg to 2kg. At a load of
2kg and 3.3 m/sec velocity, the increase in volume wear rate
of plasma nitrided coating was only eight times, which was
three times less as compared to heat treated H11 steel. SEM
observation of worn surfaces of heat treated and plasma
nitrided steel exhibited considerable difference in morphology.
ACKNOWLEDGMENT
The authors are thankful to Director VNIT for providing
facilities for the present investigation. The authors also
acknowledge the assistance of Ms Gauri in SEM work.
Fig. 7. (a) SEM photograph of worn surface of specimen A after
wear test at 1.5kg, 600RPM
Fig. 7. (b) SEM photograph of worn surface of specimen
B after wear test at 2kg, 300 RPM
Fig. 7. (c) SEM photograph of worn surface of specimen B after
wear test at 1kg,450RPM.
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© 2012 AMAE
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