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NASA Technical Memorandum 107342 /

Surface Chemistry, Friction, and Wear Properties


of Untreated and Laser-Annealed Surfaces of
Pulsed-Laser-Deposited WS 2 Coatings

Kazuhisa Miyoshi and Donald R. Wheeler


Lewis Research Center
Cleveland, Ohio

Jeffrey S. Zabinski
Wright Laboratory
Wright-Patterson Air Force Base, Ohio

December 1996

National Aeronautics and


Space Administration
SURFACE CHEMISTRY, FRICTION, AND WEAR PROPERTIES
OF UNTREATED AND LASER-ANNEALED SURFACES OF
PULSED-LASER-DEPOSITED WS2 COATINGS

Kazuhisa Miyoshi and Donald R. Wheeler


National Aeronautics and Space Administration
Lewis Research Center
Cleveland, Ohio 44135

Jeffrey S. Zabinski
Wright Laboratory
Wright-Patterson Air Force Base, Ohio 45433-7750

SUMMARY

An investigation was conducted to examine the surface chemistry, friction, and wear behavior of untreated
and annealed tungsten disulfide (WS2) coatings in sliding contact with a 6-mm-diameter 440C stainless-steel
bail. The WS2 coatings and annealing were performed using the pulsed-laser-deposition technique.
All sliding friction experiments were conducted with a load of 0.98 N (100 g), an average Hertzian contact
pressure of 0.44 GPa, and a constant rotating speed of 120 rpm. The sliding velocity ranged from 31 to
107 mm/s because of the range of wear track radii involved in the experiments. The experiment was performed
at room temperature in three environments: ultrahigh vacuum (vacuum pressure, 7x10 -7 Pa), dry nitrogen
(relative humidity, <1 percent), and humid air (relative humidity, 15 to 40 percent). Analytical techniques,
including scanning electron microscopy (SEM), energy-dispersive x-ray spectroscopy (EDX), x-ray photo-
electron spectroscopy (XPS), surface profilometry, and Vickers hardness testing, were used to characterize the
tribological surfaces of WS2 coatings.
The results of the investigation indicate that the laser annealing decreased the wear of a WS2 coating in
an ultrahigh vacuum. The wear rate was reduced by a factor of 30. Thus, the laser annealing increased the
wear life and resistance of the WS2 coating. The annealed WS2 coating had a low coefficient of friction
(<0.1) and a low wear rate (10 -7 mm3/N.m), both of which are favorable in an ultrahigh vacuum.

INTRODUCTION

While graphite and molybdenum disulfide continue to be the most commonly used inorganic solid lubri-
cants, a number of other inorganic compounds were suggested for special applications, particularly at high
temperatures (ref. 1).
Tungsten disulfide (WS2) is a transition metal disulfide and an effective inorganic lubricant in a vacuum.
It behaves very similarly to molybdenum disulfide (MoS2), although it provides significantly better oxidation
resistance during heating in air than MoS 2. WS 2 has an advantage of about 100 °C over MoS 2, with respect to
oxidation resistance and thermal stability (refs. 1 and 2).
This present investigation was conducted to examine the friction and wear behavior of untreated and laser-
annealed surfaces of the pulsed-laser-deposited WS2 coatings and to determine the effect of laser annealing on
their tribological properties. Unidirectional sliding experiments were conducted with the WS2 coatings
deposited on 440C stainless-steel disks in contact with 6-mm-diameter 440C stainless-steel balls in three
environments: ultrahigh vacuum, dry nitrogen, and humid air.

MATERIALS

The WS 2 coatings had a mean surface roughness of 359 nm rms and were deposited on 440C stainless-
steel disk substrates. The coatings were produced at room temperature using a pulsed laser beam with a 2- by
4-mm focused spot at 220 mJ/pulse and a 50-Hz pulse rate with KrF gas (248 nm) and a WS2 target. The
thickness of WS2 coatings was approximately 1 gtm. The annealing was performed by impacting a pulsed laser
beamat38mJ/cm2
for6 minandata 10-Hzpulserate, using KrF gas (248 nm). The annealed WS 2 coating
surface had a roughness of 285 nm rms.

EXPERIMENT

Characterization

Analytical techniques were used to characterize the tribological surfaces of WS 2 coatings: SEM, to deter-
mine the morphology of the wear-surface and wear-debris particles; EDX, to analyze the composition of the
wear debris particles, scars, and tracks; XPS, to characterize surface chemistry; surface profilometry, to deter-
mine the surface morphology, roughness, and wear of the coatings; and Vickers hardness testing, to determine
microhardness of the disk and ball specimens.

Apparatus

Figure 1 shows a vacuum friction apparatus. The apparatus consists of a ball-on-disk assembly mounted in
an ultrahigh vacuum chamber, a drive system, and a friction-force measuring system. All components within
the vacuum chamber are compatible with oxidizing, inert, and reducing gases.
The specimens of the vacuum friction apparatus are a 19-mm-diameter (5-mm-thick) flat disk and a 6-mm-
diameter ball specimen, as shown in the insert (Detail) of figure 1. The disk specimen is mounted on a shaft
driven by a gear motor, which is connected to a rotary feedthrough with a ferrofluidic seal. The drive assembly
provides rotation at various speeds, which are regulated by a dc motor controller.
For this study, all experiments were performed at a constant rotating speed of 120 rpm. During disk rota-
tion, the ball slid on a constant-diameter wear track located on the disk. The friction force measuring system
assembly permitted rotation at various track diameters ranging from 5 to 17 mm, which produced sliding
velocities ranging from 31 to 107 mm/s, respectively.
The ball specimen was mounted in a holder attached to one end of a stainless-steel beam. The beam was
supported by the friction force measuring system assembly, which was bearing-mounted. The bearing mounting
permitted deadweight loading of the ball against the disk surface.
Horizontal movement of the ball, that is, with the disk as it rotated, was restrained by the beam acting as
a bending spring. The displacement of the ball was continuously monitored with a linear variable differential
transformer during the experiments. The friction force could continuously be recorded in a computerized data
acquisition system during friction experiments. A friction force as low as 1 mN (0.1 g) could be measured.
The vacuum system was evacuated in 12 to 15 hr without bakeout to a pressure in the 10-7-pa range using
a turbomolecular vacuum pump and an oil-sealed mechanical pump. Pressure was measured by a nude ioniz-
ation gage. Residual gas analyses were conducted before, during, and after the friction and wear experiment by
using a quadrupole gas analyzer.

Friction and Wear Experiments

Sliding friction experiments were conducted in the chamber shown in figure 1. Before each experiment,
the as-received ball specimen was ultrasonically rinsed in an ethanol bath. The ball specimen was then dried
in a vacuum desiccator at a pressure of 70 Pa for 20 min at room temperature. The cleaned, dry ball and the
as-received WS2 disk specimen were positioned in the vacuum chamber (fig. 1).
For experiments in an ultrahigh vacuum, the system was evacuated to 7x 10 .7 Pa or better and maintained
at this pressure. For experiments in dry nitrogen, the entire vacuum chamber was filled with dry nitrogen at a
relative humidity of less than 1 percent; nitrogen gas was admitted through an inlet valve into the system
(fig. 1) and maintained at that condition during the entire sliding friction experiment. For experiments in humid
air, the vacuum chamber was conditioned in laboratory air at a relative humidity of 40 percent or less during
the entire sliding friction experiment.
After the system was conditioned to the desired environment, the pin and disk specimen surfaces were
brought into contact and loaded. Afterward, unidirectional, rotating sliding friction experiments were performed
in humid air at a relative humidity of 15 to 40 percent; in dry nitrogen, at a relative humidity of less than
l percent; or in an ultrahigh vacuum at a vacuum pressure of 7x10-7 Pa or less. All sliding friction experiments
were conducted with a load of 0.98 N (100 g), an average Hertzian contact pressure of 0.44 GPa, and a con-
stant rotating speed of 120 rpm. The sliding velocity ranged from 31 to 107 mm/s because of the range of wear
trackradiiinvolvedin theexperiments.
Asthediskrotated,
theballscribed
a circular wear track on the flat
surface of the disk. In each experiment, a new surface of the ball specimen was used.
Wear volumes of the flat disk specimens were obtained from stylus tracing across the wear tracks of at
least four locations. The average cross-sectional area of the wear track was then multiplied by the wear track
length, which was computed from the diameter of the track at its center to determine the wear volume. Since
many of the ball-on-disk or pin-on-disk results were reported using the average specific wear rate or the dimen-
sional wear coefficient expressed in mm3/N-m, an attempt was made to estimate average specific wear rates
for WS2 coatings. The calculated specific wear rate value in this case, being an average, changed with the
number of passes completed. Simple compaction of the WS2 coating under load may primarily occur during
running in. Afterwards, a burnishing wear could dominate the overall wear rate. Therefore, the average specific
wear rate for a material such as the WS2 coating should be viewed with caution.

Disk Substrates and Ball Specimens

The average surface roughness of the 440C stainless-steel disk substrates, as measured with a surface pro-
filometer, was 12 nm rms. Each roughness value was the average of 20 measurements. The average Vickers
microhardness number measured for the uncoated 440C stainless-steel disks was 695 (i.e., 6.8 GPa) over the
load range from 0.49 to 4.9 N.
The 6-mm-diameter ball specimens were 440C stainless-steel balls. The average surface roughness of the
as-received 440C stainless-steel balls, measured with a surface profilometer, was 8 nm rms. Each roughness
value was the average of 20 measurements. The average Vickers microhardness for 440C stainless-steel balls
was approximately 25 percent greater than that for uncoated stainless-steel disks over the load range from 0.49
to 4.9 N.

RESULTS AND DISCUSSION

X-ray Photoelectron Spectroscopy Analysis

Figure 2 presents XPS survey spectra of the untreated and laser-annealed WS2 coatings taken with Mg Ka
radiation. The major elements present in both coatings were W, S, O, and C. A small amount of N was present
on the surface of the untreated specimen. XPS depth profiles showing the concentrations of the major elements
as a function of the depth from the surface were obtained from both films. The N on the untreated coating dis-
appeared immediately upon sputtering and so was not included in the profiles. The profiles were done by
recording high-resolution spectra of the W4f, S2p, Ols, and Cls regions, sputtering 50 s, and repeating the
procedure until the total sputter time reached 300 s. Under the conditions used, the sputter etch rate was
0.021 nm/s as calibrated on a Ta205 standard. Quantification of the profiles was done using sensitivity factors
supplied by the instrument manufacturer. No standards were run.
The major difference in the XPS analyses of the two films is evident from the depth profiles shown in
figure 3. In the unannealed coating, there was almost no C or O below the depth of 3 nm. On the other hand, in
the laser-annealed coating, C and especially O persisted throughout the profile. The S concentration in the
laser-annealed coating was correspondingly less than in the untreated coating, although the W concentrations
were about the same.
The high-resolution Ols spectra taken after 300-s sputtering confirmed the much greater O concentration in
the laser-annealed coating than in the unannealed film (fig. 4). High-resolution S2p spectra from the surface
(fig. 5) and from 6 nm deep (fig. 6) showed that the S was present as the sulfide at all levels in both coatings.
In particular, any sulfate would give a peak at a much higher binding energy, as indicated on these spectra.
The high-resolution W4f spectra were composed of a poorly resolved 7/2 and 5/2 doublet in the 31- to 35-eV
range and a 5p3/2 line around 37 eV (figs. 7 and 8). The published positions of the 7/2 line for several possible
W compounds are indicated in figure 7. Each of these would have a corresponding 5/2 and 5p3/2 component.
In summary of XPS analysis, the surface oxides, represented by the initial high O concentrations in the
depth profiles, were 1 to 2 nm deep. To a depth of 6 nm, the untreated coating was relatively uncontaminated
WS2, while the laser-annealed coating contained high levels of O and somewhat less C, which replaced S in
the coating. In all cases, the S was present as the sulfide.
Friction Behavior

Figure 9 shows friction traces for the untreated WS2 coating deposited on a 440C stainless-steel disk in
sliding contact with 440C stainless-steel balls obtained in the three different environments: ultrahigh vacuum,
dry nitrogen, and humid air. In these figures, the coefficients of friction for WS2 coatings are plotted as a func-
tion of the number of passes. The trends of the coefficient of friction with the number of passes varies with the
environment. In general, the coefficient of friction gradually increased with the increasing number of passes in
air, while in dry nitrogen, the coefficient of friction decreased with the increasing number of passes. In an
ultrahigh vacuum, the coefficients of friction showed considerable scatter, as shown in figure 9(c).
The traces in figure 9 show closely spaced irregularities. In general, the heights of the irregularities in the
friction traces that were investigated strongly depended on the environment, and, were, in ascending order: dry
nitrogen, humid air, and ultrahigh vacuum.
In air and dry nitrogen, friction traces of the laser-annealed WS2 coating were similar to those of the
untreated WS2 coating. In ultrahigh vacuum the coefficient of friction for the laser-annealed WS2 coating was
less scattered than that for the untreated one (fig. 10). The heights of irregularity in the friction trace of the
laser-annealed WS2 coating was much smaller than that of the untreated WS2 coating.

Wear Behavior

The SEM observations indicated that the wear surfaces of the untreated and annealed WS2 coatings took
on a burnished appearance (e.g., fig. 11), regardless of environment. Both coating surfaces exhibited adhesive
wear, (i.e., burnishing).
The wear track of the untreated and annealed WS2 coatings revealed that the sliding action generated a
smooth wear surface, fine wear-debris particles, and agglomerated, pasty wear debris (e.g., fig. 12). Thin,
layered WS2 was present on the smooth wear tracks. Most of the wear debris accumulated outside the wear
tracks.
The wear scar of 440C stainless-steel balls revealed that the wear scar was generally smooth (e.g.,
fig. 13), regardless of whether the coatings were untreated or annealed, and of the environment. Thin, smeared
wear patches of WS2 generally covered the smooth wear scars. Smeared tongues of thin, layered, agglomer-
ated wear debris were also present. Most of the loose and smeared wear debris accumulated outside the wear
scars.

Wear Life

Sliding wear (endurance) lives of the WS 2 coatings deposited on 440C stainless-steel disks were deter-
mined to be the number of passes at which the coefficient of friction rapidly rose to approximately 0.8 in
humid air, to 0.15 in dry nitrogen, and to 0.30 in an ultrahigh vacuum. The sliding wear lives are presented in
figure 14.
The sliding wear lives varied with the environment, similar to the coefficient of friction. With both
untreated and annealed WS2 coatings, the wear life and resistance of the films were, in ascending order:
humid air, ultrahigh vacuum, and dry nitrogen. The wear life of both coatings were around 9000 passes in
humid air, while the wear life was greater than 2 million passes in dry nitrogen. In an ultrahigh vacuum, the
wear life of the laser-anneaied WS2 coating was 10 times or more greater than that of the untreated one; the
wear life of the untreated WS2 coating was around 50,000 passes, while that of the laser-annealed WS2 coat-
ing was greater than 500,000 passes. Thus, laser annealing greatly increased the sliding wear life of WS2
coating, especially in an ultrahigh vacuum.

Coefficient of Friction and Wear Rate

Figure 15 presents the steady-state (equilibrium) coefficients of friction and wear rates (dimensional wear
coefficient) for the untreated and annealed WS2 coatings in an ultrahigh vacuum, dry nitrogen, or humid air.
Both the steady-state coefficients of friction and wear rates of the WS2 coatings depended on the environment
and, were, in ascending order: dry nitrogen, ultrahigh vacuum, and humid air.
The annealing had an influence on the wear rate of the WS2 coatings in an ultrahigh vacuum; the wear
rate of the untreated WS 2 coating was 30 times greater than that of the annealed one. The coefficient of fric-
tion for the annealed surface revealed slightly lower friction and much less erratic behavior than that for the
untreated
surface.
Ontheotherhand,theannealing
didnothavemuchinfluence
on the coefficients of friction
and wear rates of WS2 coatings in dry nitrogen and humid air.

CONCLUDING REMARKS

The surface oxides covered over a pulsed-laser-deposited WS 2 coating surface were 1 to 2 nm deep. To a
depth of 6 nm, the untreated coating was relatively uncontaminated WS2, while the laser-annealed coating
contained high levels of oxygen and somewhat less carbon, which replaced sulfur in the coating. In all cases,
the sulfur was present as the sulfide.
The laser annealing decreased wear of the WS2 coating. In the ultrahigh vacuum, the reduction of wear
rate by a factor of 30, was accompanied by an increase in the wear life and resistance of the WS2 coating.
The annealed WS2 coating had a low coefficient of friction (<0.1) and a low wear rate (10 -7 mm3/N.m), which
are a favorable friction and wear behavior in an ultrahigh vacuum.

ACKNOWLEDGMENTS

The authors would like to thank Dr. Kent Eisentraut of Wright Laboratory, Wright Patterson Air Force
Base, Ohio for supporting this study and producing the untreated and annealed WS2 coatings, Ronald E. Miller
and Mark Jansen for specimens preparation and experimental setups, and Duane J. Dixon for SEM.

REFERENCES

1. Campbell, M.E.: Solid Lubricants - A Survey. NASA SP-5059(01), 1972.


2. Clauss, F.J.: Solid Lubricants and Self-Lubricating Solids. Academic Press, New York, 1972.
Vacuum chamber -_._

Turbomolecular
vacuum pump -_,
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gas analyzer

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Speed // \

pickup -/ \
Drive motor
/
/
./
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_-- Pneumatic isolation table
Speed control--/

Figure 1 .---Vacuum chamber friction and wear apparatus.


7O • 01s

65 m

6O
55 m

5O_ OKL1

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45
U3 CKL1 , _ W4s C1.,
W4d
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Binding energy, eV

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o 25 I
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o S2s I

2O

15

10

5 -- (b) I I I ] J J I I I
1000 900 800 700 600 500 400 300 200 100 0
Binding energy, eV

Figure 2.reX-ray photoelectron spectroscopy (XPS) survey spectra of pulsed-laser-deposited WS 2


coatings. (a) Untreated. (b) Laser-annealed.
F
7O .- 01s
......... Cls
S2p
....... W4f

G)
o

i • .
i
o
,m
40

c
Q
o 3O
c
o
o
._o
E 2O
o

10

I t I .,--i .... [
2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0
Depth, nm

!
70 _- 01s
! ......... Cls

S2p
....... W4f

50-
W
Q.
/

/
/

Q
0
t- 3O
O
0
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E 0
o 2O

10 . ..
- C

• .. ..

(b) E I 'r ........ i l i _ , |

0 .5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0
Depth, nm

Figure 3.BX-my photoelectron spectroscopy (XPS) depth profiles of pulsed-laser-deposited WS 2


coatings. (a) Untreated. (b) Laser-annealed.
5200 t

5000'-- i

4800 _

=_4600
0 /
0 J

4400

4200 .--'. _'"'. . Unannealed


J

4000

I I [ I
540 538 536 534 532 530 528 526
Binding energy, eV

Figure 4.---0 ls spectra (at 300 s sputtering) of pulsed-laser-deposited WS 2 coatings.


WS2
2650
/

2550 ,/

/
/

2450 -- /

._ 235O
¢-

o
0 2250

2150 Sulfates \
',\
\
_J

2050
\

1950
(a) I [ I I I I I I _ l
174 172 170 168 166 164 162 160 158 156
Binding energy, eV

WS 2

3000

2800 - /_

=.-
-, 2600
8 - j

2400 _/ \

2200 - , ____

(b)_ I L _ ' I J ' i


174 172 170 165 166 1 64 162 160 158 156
Binding energy, eV

Figure 5._2p spectra of surfaces of pulsed-laser-deposited WS2 coatings. (a) Untreated. (b) Laser-
annealed.

I0
=WS 2
4000
I

38OO

360O

340O
i

¢- m
3200
0
L)
3000

2800

2600

2400
(a) I L L I L I L I

174 172 170 168 166 164 162 160 158 156
Binding energy, eV

3800

F
3600

3400

3200
0
0

30OO

2800

_J

2600

(b) I I L I _ I I I I I
174 172 170 168 166 164 162 160 158 156
Binding energy, eV

Figure 6._$2p spectra (at 300-s sputtering) of pulsed-laser-deposited WS 2 coatings. (a) Untreated.
(b) Laser-annealed.

1!
2400
I W03
iwo2
I
jl_ i WS2
2200

\ /

2000 ....
\j
t-

O
0
1800

/ L

1600
\

J -J
1400

i(a) j I i _ I i L

44 42 40 38 36 34 32 30 28 26
Binding energy, eV

38OO
W03 W02
1 !
iws2 .w
340O

30OO
\
I /

i /r
i-
2600
8 ;
/
/

I /

/ '!t
2200
-- // ',

1800 -- '\

(b)
1400 -- i i E L I I 1 I I
44 42 40 38 36 34 32 30 28 26
Binding energy, eV

Figure7.mW4fspectra ofsu_aces of pulsed-laser-depositedWS2 coatings.(_ Untreated.(b)Laser-


annealed.

12
6500

6000 - Iws2
wo2 iw

5500 -

5000--
/
/'

4500 -- j'

/
¢-
4000 -- J
0
,/
0
3500 -- /

• JJ

3O0O m t j"

2500

2000 \

1500_- L _ J i l I /. J

44 42 40 38 36 34 32 30 28 26
Binding energy, eV

rws2 iw
7000
iwo2
6500

6000

5500

5000
It

4500
¢.-
/
0
0 4000 /
/
J
3500 m _J

j_
j-
/-
3O00 7

2500 \

2000

1500 (b) i I ] t i I I _ J
44 42 40 38 36 34 32 30 28 26
Binding energy, eV

Figure 8._W4f spectra (at 300-s sputtering) of pulsed-laser-deposited WS 2 coatings. (a) Untreated.
(b) Laser-annealed.

]3
I I I I
2 4 6 8 10xl 03
Number of passes
.5--
1.0
(b)
t-
.4
O
•8 --
0
o .3
U
_E "6
•6 --
`6
o .2
"E U
._e •4 --
O
0
.1
•2 --

J I I I I
lW
0 1 2 3 4 5xl 05
.5 1.0 1.5 2.0x106 Number of passes
Number of passes Figure 10.-- Friction traces for laser-annealed WS2
coating in sliding contact with 440C stainless-steel
1.0 m
balls in ultrahigh vacuum environment.
(c)

•8 --
c-
o

T= •6 --
"6
'E
e •4 --
O

O .2

0 9 18 27 36 45x103
Number of passes
Figure 9.mFdction traces for untreated WS 2 coating
in sliding contact with 440C stainless-steel bells in
vadous environments. (a) Humid air. (b) Dry
nitrogen. (c) Ultrahigh vacuum.

14
Figure 11 .--Wear tracks produced on laser-annealed WS2 coating after
sliding contact. (a) Scanning electron microscopy (SEM) image of wear track
and its surroundings at 25 500 passes in air. (b) SEM image of wear track
and its surroundings at 2 million passes in dry nitrogen. (c) SEM image of a
wear track and its surroundings at 607 990 passes in ultrahigh vacuum.

15
Figure 11.---Concluded.

16
Figure 12.--Wear track produced on laser-annealed WS2 coating after sliding
contact at 607 990 passes in ultrahigh vacuum. (a) Secondary electron image
of wear track and its surroundings. (b) Backscatter electron image of wear
track and its surroundings.

17
Figure 13.-- Wear scar produced on 440C stainless-steel ball after sliding
contact with the laser-annealed WS 2 coating at 607 990 passes in ultrahigh
vacuum. (a) SEM image at low magnification. (b) SEM image at high
magnification.

18
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December 1996 Technical Memorandum

4. TITLE AND SUBTITLE 5. FUNDING NUMBERS

Surface Chemistry, Friction, and Wear Properties of Untreated and


Laser-Annealed Surfaces of Pulsed-Laser-Deposited WS 2 Coatings

WU-505-63-5A
6. AUTHOR(S)

Kazuhisa Miyoshi, Donald R. Wheeler, and Jeffrey S. Zabinski

7'. PERFORMING ORGANIZATION NAME(S) AND ADDRESS(ES) 8. PERFORMING ORGANIZATION

REPORT NUMBER

National Aeronautics and Space Administration


Lewis Research Center E-10351
Cleveland, Ohio 44135 -3191

9. SPONSORING/MONITORING AGENCY NAME(S) AND ADDRESS(ES) 10. SPONSORING/MONITORING

AGENCY REPORT NUMBER

National Aeronautics and Space Administration


Washington, D.C. 20546-0001 NASA TM- 107342

11. SUPPLEMENTARY NOTES

Kazuhisa Miyoshi and Donald R. Wheeler, NASA Lewis Research Center; Jeffrey S. Zabinski, Wright Laboratory,
Wright-Patterson Air Force Base, Ohio 45433-7750. Responsible person, Kazuhisa Miyoshi, organization code 5140,
(216) 433--6078.
12a. DISTRIBUTION/AVAILABILITY STATEMENT 12b. DISTRIBUTION CODE

Unclassified - Unlimited

Subject Category 27

This publication is available from the NASA Center for AeroSpace Information, (301 ) 62 I--0390.
13. ABSTRACT (Maximum 200 words)

An investigation was conducted to examine the surface chemistry, friction, and wear behavior of untreated and annealed
tungsten disulfide (WS2) coatings in sliding contact with a 6-mm-diameter 440C stainless-steel ball. The WS 2 coatings
and annealing were performed using the pulsed-laser-deposition technique. All sliding friction experiments were
conducted with a load of 0.98 N (100 g), an average Hertzian contact pressure of 0.44 GPa, and a constant rotating speed
of 120 rpm. The sliding velocity ranged from 31 to 107 mrn/s because of the range of wear track radii involved in the
experiments. The experiment was performed at room temperature in three environments: ultrahigh vacuum (vacuum
pressure, 7× 10 -7 Pa), dry nitrogen (relative humidity, <1 percent), and humid air (relative humidity, 15 to 40 percent).
Analytical techniques, including scanning electron microscopy (SEM), energy-dispersive x-ray spectroscopy (EDX),
x-ray photo electron spectroscopy (XPS), surface profilometry, and Vickers hardness testing, were used to characterize
the tribological surfaces of WS 2 coatings. The results of the investigation indicate that the laser annealing decreased the
wear of a WS 2 coating in an ultrahigh vacuum. The wear rate was reduced by a factor of 30. Thus, the laser annealing
increased the wear life and resistance of the WS 2 coating. The annealed WS 2 coating had a low coefficient of friction
(<0.1) and a low wear rate (10 -7 mm3/N.m), both of which are favorable in an ultrahigh vacuum.

14. SUBJECT TERMS 15. NUMBER OF PAGES


21
WS 2 coatings; Friction, Wear, Pulsed-laser-deposition 16. PRICE CODE
A03
17. SECURITY CLASSIFICATION 18. SECURITY CLASSIFICATION 19. SECURITY CLASSIFICATION 20. LIMITATION OF ABSTRACT

OF REPORT OF THIS PAGE OF ABSTRACT

Unclassified Unclassified Unclassified

NSN 7540-01-280-5500 Standard Form 298 (Rev. 2-89)

Prescribed by ANSI Std. Z39*1B


298-102
Untreated
i Laser-annealed

10 7

¢R
G)
10 6
W

¢z

105

o_
¢-
_ 10 4

103 Air Nitrogen Vacuum


Environment

Figure 14._Sliding wear (endurance) life of untreated


and laser-annealed surfaces of pulsed-laser-deposited
WS 2 coatings in sliding contact with 440C stainless-
steel balls in humid air, dry nitrogen, and ultrahigh
vacuum environments.

[] Untreated
A Laser-annealed

Open symbols indicate humid air environment


Half-open symbols indicate dry nitrogen environment
Solid symbols indicate ultrahigh vacuum environment

10-4
-- A

-- []

10-5
E

E
E
d 10-6---

10 -7 -z-
ztl

I L t IIIllL I I t J LLIJ
10-8
0.01 0.1 1
Coefficient of friction

Figure 15.--,Steady-state (equilibrium) coefficients of friction


and wear rates (dimensional wear coefficient) for untreated
and laser-annealed surfaces of pulsed-laser-deposited
WS 2 coatings in sliding contact with 440C stainless-steel
balls in humid air, dry nitrogen, and ultrahigh vacuum
environments.

]9

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