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Tribology International 117 (2018) 112–118

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Tribology International
journal homepage: www.elsevier.com/locate/triboint

Multi-pass micro-scratching and tribological behaviors of an austenitic steel


in media
Qilong Wei *, Jiangang Lü, Qiang Yang, Xiaoyuan Li
Institute of Machinery Manufacturing Technology, CAEP, Mianyang, China

A R T I C L E I N F O A B S T R A C T

Keywords: Micro-scratching and tribological behaviors of an austenitic steel in media including a nano-caria slurry, a carrier
Micro-scratch liquid and air are researched thoroughly, with the purpose to provide a technical method for simulation of
Nano-ceria slurry microscopic mechanisms in polishing. It is found that penetration depth increment and remnant depth increment
Coefficient of friction
are highest in the first pass and they decrease markedly in later passes, while coefficient of friction decreases with
Depth increment
pass. Both penetration depth increment and coefficient of friction are maximal in the nano-ceria slurry. Based on
the Hertzian theory, it can be deduced that multi-pass scratch transforms interaction form between indenter and
surface, while the particles are embedded into the softer surface under higher load, both of which influence latter
scratch.

1. Introduction method when scratch depth was very small [10]. Beake et al. conducted
nano-scratch on a single-crystal silicon with a spherical indenter of
Polishing is a key technology which endows material surfaces with 4.6 μm in radius, and obtained the critical fracture load and toughness-
optical properties and other functions, and it has played important roles brittleness transformation characters [11]. Zhang et al. onducted nano-
in various scientific and technological fields [1–3]. Development of new scratch on a KDP crystal, and found that it was the non-uniform defor-
technologies has brought forward more and more high requirements on mation of material before the indenter that produced marked fluctua-
polishing of surfaces. For example, extreme ultraviolet photo-mask blank tions of friction force and coefficient of friction [12]. But these researches
requires surface roughness less than 0.15 nm [4,5], and super-polish all reduce the three-body conditions in polishing process to two-body
aspheres require surface roughness less than 0.2 nm [6]. These conditions, which are different from actual polishing conditions and
rigorous requirements demand both advanced polishing methods and produce results with large deviations.
scientific understanding of polishing. Many researchers analyzed polishing process with micro-scratch
In polishing process there are complex three-body interactions among method, but they did not take abrasive particles into consideration. For
abrasive particles, polishing pad and material surfaces, where a large example, Demirci et al. simulated polishing of glasses by triple scratch
number of abrasive particles are constrained weakly by polishing pads. In test, and found that distance between scratches and scratching speed had
some extreme conditions, polishing pad constrains abrasive particles so marked influences on formation of chips and material removal [13]. Gu
strongly that the situation is simplified to a two-body interaction. Ac- et al. also studied influence of separation distance between parallel
cording to constraints from polishing pad, abrasive particles remove scratches on material removal of BK7 glass [14]. There lacks of research
material by plowing or rolling [7–9]. Thus concourse of large number of on scratch in suspensions of small particles and multi-pass scratch, which
abrasive particles removes material macroscopically and creates both are key characters in polishing processes.
smooth surface. In fact, micro-scratch technology is more suitable to simulate the
The basic material removal has been researched by simulation with three-body conditions in polishing process, as it has more suited radius
AFM and scratch methods, where a sphere glued to the tip scratches ratio of the indenter and abrasive particles. Size of abrasive particles
material surfaces, or the tip scratches material surfaces directly. usually is about 100 nm, while radius of spherical indenter is about 5 μm
Komanduri et al. scratched on single-crystal aluminum with a tip with for nano-scratch and 10–100 μm for micro scratch [15,16], which means
radius 25 nm in AFM, and found that material was removed by a plowing that indenter size of micro scratch is about 100–1000 times of size of

* Corresponding author.
E-mail address: weiqilong2004@126.com (Q. Wei).

http://dx.doi.org/10.1016/j.triboint.2017.08.016
Received 7 January 2017; Received in revised form 24 April 2017; Accepted 16 August 2017
Available online 18 August 2017
0301-679X/© 2017 Published by Elsevier Ltd.
Q. Wei et al. Tribology International 117 (2018) 112–118

abrasive particles. Then it can ensure that there are enough particles was done in air. Then another group of scratch experiments were con-
participating in the three-body interactions under the indenter when ducted in air by the manner shown in Fig. 2, to obtain dimensions of
micro-scratch is conducted in abrasive slurries. impressions. Six parallel strips were scratched with load 2.0 N and pass
Some researchers studied the microscopic three-body conditions by from 1 to 6, distance between nearby strips about 300 μm. Then four
simulation with nano-scratch in slurries. For example, Fu et al. [17] glued parallel strips perpendicular to these six strips were scratched with dis-
a silica sphere with radius 400 nm on the AFM tip, and scratched copper tance 200 μm–300 μm (P-scan A), and additional two parallel strips were
films with it in various media including air, de-ionized water, and silica scratched in the same direction outside the six parallel strips with dis-
slurry with mean particle size 110 nm. He obtained variations laws of tance 200 μm–300 μm (P-scan B).
depth, friction force and wear rate with media, and determined contri- Six-pass scratch with constant load 2.0 N was done in the CL and the
butions from slurry chemistry and liquid buoyancy. But he did not nano-ceria slurry respectively. The slurry or CL was added onto selected
consider radius ratio of glued silica sphere and sphere in slurry, as there locations before scratch, and was cleaned with filter paper after scratch.
could not have enough abrasive particles which participated in friction Besides, the indenter was cleaned with de-ionized water in an ultrasonic
between glued sphere and copper films. bath after each group of scratches and dried with filter paper.
On the other hand, multi-pass scratch which is done on the same
location repeatedly can simulate repeated movements of abrasive parti- 3. Experimental results
cles in polishing by and large. But micro-scratch do not have high signal-
to-noise as nano-scratch, which may make it difficult to distinguish and Fig. 3(a) shows results of the first scratch on the austenitic steel with a
exhibit results with small differences in scratching on hard and brittle constant load 1.0 N in air, where Pd, Rd and μ are penetration depth,
materials such as K9 and fused silica. As single-phase austenitic steels remnant depth after elastic recovery, and coefficient of friction respec-
have low hardness and high plasticity, they are good candidates for tively. It is found that Pd, Rd and μ all fluctuate in different ranges, and Pd
scratching, which will provide better scientific and technological bases and Rd fluctuate synchronously. Average values of Pd, Rd and μ in the
for researching on hard and brittle materials. total length of 2.0 mm are 1.401 μm, 0.930 μm and 0.15 respectively,
Besides, as physical meanings are not clear for penetration depth and while their relative standard deviation (rsd) are 5.99%, 10.1% and 8.31%
remnant depth during multi-pass scratch, a group of six parallel scratches respectively. In the latter sections, Pd, Rd and μ are used to represent their
and a perpendicular scanning will be conducted. average values.
Fig. 3(b) shows statistical results of all first scratches on the austenitic
2. Experiments and materials steel with different constant loads in air. It is found that when the load
increases from 0.5 N to 2.0 N, Pd, Rd and μ all increase monotonously,
An austenitic steel (AS) specimen and a slurry of ceria particles were with the maximal increased percentage 244%, 227%, and 52.3%
used in micro-scratch experiments. Fig. 1(a) shows a microscopic image
the AS, and it is found that grains are near equi-axial with size between
10 μm and 100 μm. Fig. 1(b) shows a TEM image of ceria particles, and it
indicates that the particles are irregular polyhedrons with size between
100 nm and 200 nm.
An aqueous solution of sodium carboxymethyl cellulose and sodium
nitrite was used as the carrier liquid (CL). A ceria slurry with particles
weight concentration 1% was prepared by dispersing the nano-ceria
particles into the CL with an ultrasonic probe. Thus media used in ex-
periments included the nano-ceria slurry, the carrier liquid, and air.
A micro scratch tester of CMS Instruments was adopted in micro-
scratch experiments, and the diamond indenter was a spherical Rock-
well one with a tip of 100 μm in radius. An advanced scratch mode was
selected, with both pre-scan load and post-scan load 0.03 N, scratch
length 2.0 mm, scratch speed 2.0 mm/min, acquisition rate 30 Hz.
Before scratching, microscopic characters on the sample surface were
observed by optical microscopy of the tester, and locations without
obvious defects, polishing tracks and contamination were chosen to be
used in experiments.
Firstly, six-pass scratching with constant loads from 0.5 N to 2.0 N
Fig. 2. Schematic of the six parallel strips and perpendicular scanning.

Fig. 1. Microscopic images of (a) the austenitic steel and (b) the ceria particles.

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Fig. 3. Results of the first scratch in air, (a) with a constant load 1.0 N, (b) statistical results with various constant loads.

respectively. At the same time, difference between Pd and Rd increases Fig. 5(b) shows results of these six parallel impressions by the
monotonously too, with the maximal increased percentage 275%. Be- perpendicular pre-scanning, where Wa is the actual scratched width, Wp
sides, rsd of Pd, Rd and μ all decrease markedly when the load increases is the nominal scratched width with pile-up effect, and Rs is the maximal
from 0.5 N to 2.0 N, which means that signal-to-noise of measurements remnant depth of the impressions. Besides, Rd in Fig. 4(a), the remnant
increases with load. depth averaged on the length 2.0 mm, is also depicted for comparison. It
Then a constant load 2.0 N is chosen to research influences of various is found that Wa and Wp increase with pass in whole, while increased
media on multi-pass scratching behaviors of the austenitic steel. value of Wp is much higher than that of Wa at pass six. Then it can be
Fig. 4(a) shows statistical results of six-pass scratches on the austenitic deduced that Wp increasing with pass may be mainly due to pile-up
steel with a constant load 2.0 N in air. It is found that Pd and Rd increase [18–20]. Besides, Wp after six-pass scratch is 60.8 μm, which is close to
monotonously with pass, while μ decreases monotonously with pass. that in Fig. 4(b), and the ratio of Wa to Rs in each pass is in the range from
Then Pd and Rd in the final pass increase by 41.3% and 57.9% compared 10 to 15.
with those in the first pass respectively, while μ in the final pass decreases More importantly, both Rs and Rd increase with pass, and they are
by 51.7% compared with that in the first pass. Besides, difference be- equivalent basically, which means that remnant depth obtained by
tween Pd and Rd fluctuates between 0.85 μm and 0.95 μm. An impression scratching directly and perpendicular pre-scanning are coincided well. It
after the six-pass scratch with load 2.0 N is shown in Fig. 4(b), where a reveals that measured Rd in each pass is accumulated depth increments
clear-cut groove is about 60 μm in width, and grains boundaries across from the first pass during multi-pass scratches, which is shown in Fig. 6,
the groove keep continuous basically. where symbol Δ represents increment. Similarly, measured Pd in each
The average values of the four groups of pre-scanned profile data in P- pass is the sum of penetration depth increment in the pass and accu-
scan A are used to draw impression shapes of the six parallel strips, while mulated remnant depth increments of front passes, which is shown in
the average values of the two groups of pre-scanned profile data in P-scan Fig. 6 too. Besides, Pd and Rd are increments of themselves in the
B are used to correct the surface gradient of the sample. Thus dimensions first pass.
of these six strips are obtained, and they are shown in Fig. 5(a), where Ro Then depth increments of each pass can be obtained according to the
is the original remnant depth curve without correction by surface principle in Fig. 6, and they will be used together with measured depths
gradient, and Rc is the corrected curve. The impressions from left to right to investigate influences of various media on micro-scratching behaviors.
are scratched from one pass to six passes respectively with load 2.0 N. Fig. 7 shows statistical results of six-pass scratches on the austenitic
From these curves, it is found that both remnant depth and the pile-up steel with load 2.0 N in various media, where cer, air and CL in icons
extent increase obviously with pass, and remnant depths have their denotes results measured in the ceria slurry, air and CL respectively. It is
maximal values of in the centers of impressions. found that Pd and Rd in the slurry and CL increase monotonously with

Fig. 4. Results of scratching with load 2.0 N in air, (a) statistical results of six-pass scratches, (b) an impression after six-pass scratch.

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Fig. 5. Results of the six parallel multi-pass scratches with constant load 2.0 N in air, (a) impression dimensions and (b) measured results.

second pass decrease to about half and one-tenth of those in the first pass
respectively and they basically keep constant in latter passes. At the same
time, ΔPd in the ceria slurry is highest and it is lowest in CL in the same
pass, while ΔRd does not show clear difference in these media.

4. Discussions

According to above results, penetration depth, remnant depth and


coefficient of friction all increase monotonously with load, during micro-
scratching on the austenitic steel. On the other hand, penetration depth
and remnant depth increase monotonously with pass, while coefficient of
friction decreases monotonously with pass, during multi-pass scratching
on the austenitic steel. Penetration depth increment and coefficient of
friction are highest in the slurry of nano-ceria particles. These results
reflect elastic and plastic deformations of the material, and roles of small
Fig. 6. Increments of penetration depth and remnant depth in the first two passes.
particles, which will be analyzed in detail as follows.
According to the Hertzian theory, the radius of elastic contact circle a
pass, while μ in these two media decreases with pass, which are similar
between a rigid indenter with tip radius R and a plane under indent load
with those manners in air. But media have their influences too, as Pd, Rd
P can be calculated by the following equation:
and μ of the same pass are all maximal in the ceria slurry, while they are
all minimal in CL. The difference of Pd of the same pass in the slurry and 3 PR
in CL varies from 0.286 μm to 0.535 μm, with average value 0.417 μm. a3 ¼ (1)
4 E*
These values are about two times of the size of ceria particles. On the
other hand, μ in the slurry is about two times of its corresponding values And the maximal elastic indented depth he is determined by the
in CL and air. following equation:
Based on scratch data in Fig. 7(a), depth increments, ΔPd and ΔRd, of  2=3  1=3
each scratch pass are calculated analytically according to the principle in 3P 1
he ¼ (2)
Fig. 6, and they are shown in Fig. 8. It is found that both ΔPd and ΔRd in 4E* R
the first pass are highest in different media, while ΔPd and ΔRd in the

Fig. 7. Statistical results of six-pass scratches with constant load 2.0 N in various media, (a) Pd and Rd, (b) coefficient of friction.

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Fig. 8. Depth increments of each pass during scratches with constant load 2.0 N in various media, (a) ΔPd and (b) ΔRd.

Table 1 austenitic steel is indented by the diamond indenter with load 2.0 N.
Materials' properties used in calculations with models. Thus the total indented depth is 2.193 μm, which is close to 2.499 μm of
Materials E(GPa) ν H(GPa) E* with AS (GPa) Pd in the first pass scratch with load 2.0 N. And the diameter of elastic
Diamond 1141 0.07 / 156.56 contact circle is 19.634 μm, which holds the main part of the actual
Ceria [26] 175 0.33 / 94.27 scratched width 23.4 μm in the first pass scratch with the same load.
AS [27] 174.06 0.20 2.59 / Besides, pressure in the center of the contact circle is 6.975 GPa, calcu-
lated with the actual scratched width.
During multi-pass scratch, interacting form between the indenter and
the surface changes. It is a sphere-plane one in the first pass while it is a
E* is the reduced modulus of the indenter and the plane and it is given by: sphere-concave one in the latter passes. Then tip radius of the indenter
and radius of the concave are close in values but they have opposite signs.
1 1  v2i 1  v2s Thus the relative radius increases obviously, and both he and hp decrease
¼ þ (3)
E* Ei Es in the second pass. But indented depth does not change continuously, as
the interacting form does not change after the second pass. Besides, the
where Ei and νi are elastic modulus and Poisson's ratio of the indenter, Es frontal scratches produce plastic deformation and deformation hardening
and νs are elastic modulus and Poisson's ratio of the plane [21–23]. [27,28], which decrease penetration depth of latter scratches to
On the other hand, pressure distribution under the indenter takes some extent.
the form: The reasons for coefficient of friction changing with pass are similar.
 1=2 Although Pd in the second pass increases, its increment decreases because
3 P r2 of the frontal groove, which is confirmed by Fig. 8. Thus the material
σZ ¼ 1  (4)
2 πa2 a2 which blocks movement of the indenter is reduced, and then coefficient
of friction reduces too from the second pass. But coefficient of friction
where r is the distance to the center of the contact circle [23]. Thus σz is decreases slowly from the third pass, as actual depth changes little. Be-
maximal in the center while it is zero in the boundary. sides, the frontal scratches remove surface asperities, which can reduce
At the same time, when the maximal plastic indented depth hp is coefficient of friction of latter passes to some extent.
much smaller than indenter tip radius, it can be calculated by Influencing mechanisms of media on friction are clear. The coefficient
the equation: of friction decreases to some extent due to lubricating action of water
[24] when the medium changes from air to the aqueous carrier liquid.
P
hp ¼ (5) More importantly, nano-ceria particles in the slurry are embedded into
2πHR the softer austenitic steel under action of higher normal load, which in-
fluences scratch and friction behaviors of the material.
where H is hardness of the plane [24].
It is commonly thought that nano-particles in slurries are advanta-
According to equations (2) and (5), both the maximal elastic indented
geous to friction and anti-wear of materials, as they reduce friction in
depth and the maximal plastic indented depth increase with load, and
various systems by transforming wearing modes, reducing friction area,
decrease with indenter radius.
and increasing thermal conductivity [29–32]. But the situation is
If both contacting bodies have curvatures, their relative radius [25] is
different in this research, where the nano-ceria particles are irregular
given by:
polyhedrons, and may be indented into the softer austenitic steel under
1 1 1 higher load.
¼ þ (6)
R R1 R2 A rough evaluation of normal force acted on a single particle is done
by assuming that particles have a same diameter and there has no cavity
where R1 is tip radius of the indenter and R2 is radius of its counter body. among particles. Then normal force applied on a single particle is the
For a concave surface with a negative R2, R is higher than R1. product of the pressure and the projected area of the particle. Thus the
Calculation on elastic and plastic deformations of the austenitic steel normal force applied on a single nano-ceria particle with diameter
(AS) under the diamond indenter is conducted according to these above 150 nm in the center of the contact circle is 1.569  104 N according to
models. And materials' properties used in calculation are listed in Table 1, this simple model, based on the pressure in the center of the contact circle
where data of the diamond are from the instrument manual. as mentioned in front. Then a spherical nano-ceria particle with diameter
Based on calculations, he is 0.964 μm, and hp is 1.229 μm when the 150 nm is indented into the austenitic steel with elastic depth 27.48 nm

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Fig. 9. Groove scratched by six-pass with load 2.0 N in the nano-ceria slurry.

and plastic depth 128.55 nm under such a normal force according to as follows.
models, which means that the maximal indented depth exceeds its
diameter. But the actual total indented depth must increase to some 1) Penetration depth, remnant depth and coefficient of friction all in-
extent for particles with cavities among them, irregular particles with crease markedly during single scratching on the austenitic steel in air
sharp angles, and bigger particles bearing higher load. when the constant load increases from 0.5 N to 2.0 N.
Thus the nano-ceria particles are indented into the steel with depths 2) During six-pass scratching on the austenitic steel in air with load
more than their sizes in the center of the contact circle with load 2.0 N, 2.0 N, both penetration depth and remnant depth increase monoto-
which means that they are embedded into the steel wholly. While those nously with pass, while coefficient of friction decreases monotonously
depart from the center are indented into the steel more shallowly due to with pass, and both penetration depth increment and remnant depth
lower pressure. Then the total penetration depth increases due to the increment decrease obviously in pass two to pass six.
particles embedment, as shown in Figs. 7 and 8. On the other hand, co- 3) Six-pass scratching results on the austenitic steel are similar in various
efficient of friction also increases as scratched material changes from the media with load 2.0 N, while penetration depth increment and co-
softer steel to its composite material strengthened by the particles, and efficient of friction are maximal in the nano-ceria slurry, and they are
micro-abrasion may appear too. Besides, the embedded particles below minimal in the carrier liquid at the same passes.
the indenter in the scratching direction are scratched with the austenitic 4) It is deduced that multi-pass scratching transforms interaction form
steel surrounding them by and large. between the indenter and the surface, while the nano-ceria particles
This analysis is supported by microscopic images in Fig. 9, which are embedded into the softer austenitic steel under higher load, both
shows the scratched groove in the nano-ceria slurry with load 2.0 N and of which influence latter scratching.
pass six. As slurry continues to flow into the scratched groove in multi-
pass scratch, the groove is filled with particles after scratch experi- Acknowledgements
ment. But the particles distribute in the groove unevenly, and there is no
particle at all in several small center locations where the pressure is Financial support of this work is provided in part by the Major Na-
maximal in scratching. Then it can be deduced that the embedded par- tional Science and Technology Special Projects of China
ticles may have been scratched out while most particles remain in the (2013ZX04006011), Challenge Program of Basic Science, Foundation of
tiny groove due to adhesive effect [33,34]. CAEP Key Laboratory of Ultra-precise Machining Technologies.
The change of depths and coefficient of friction in the ceria slurry
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