Tribol Lett (2010) 38:25–32
DOI 10.1007/s11249-009-9565-9
ORIGINAL PAPER
Influence of Steel Type on the Propensity for Tribochemical Wear
in Boundary Lubrication with a Wind Turbine Gear Oil
R. D. Evans • G. L. Doll • C. H. Hager •
J. Y. Howe
Received: 22 September 2009 / Accepted: 23 December 2009 / Published online: 23 January 2010
Ó Springer Science+Business Media, LLC 2010
Abstract Tribochemical wear may occur at the interface
between a surface and a lubricant as a result of chemical
and mechanical interactions in a tribological contact.
Understanding the onset of tribochemical wear damage on
component surfaces requires the use of high resolution
techniques such as transmission electron microscopy
(TEM). In this study, two steel types, case carburized AISI
3310 and through-hardened AISI 52100, were wear tested
using a ball-on-disk rolling/sliding contact tribometer in
fully formulated commercial wind turbine gearbox oil
under boundary lubrication conditions with 10% slip. With
the exception of steel type, all other test conditions were
held constant. Conventional tribofilm analysis in the wear
tracks was performed using X-ray photoelectron spectros-
copy, and no significant composition differences were
detected in the tribofilms for the different steel disk types.
However, TEM analysis revealed significant tribochemical
wear differences between the two steel types at multiple
length scales, from the near-surface material microstructure
(depth \ 500 nm) to the tribofilm nanostructure. Nano-
meter-scale interfacial cracking and surface particle
detachment was observed for the AISI 52100 case, whereas
the tribofilm/substrate interface was abrupt and undamaged
for the AISI 3310 case. Differences in tribofilm structure,
including the location and orientation of MoS2 single sheet
inclusions, were observed as a function of steel type as
well. It is suggested that the tribochemical wear modes
observed in these experiments may be origins of
R. D. Evans (&)
G. L. Doll
C. H. Hager
Timken Technology Center, North Canton, OH, USA
e-mail: ryan.evans@timken.com
J. Y. Howe
Oak Ridge National Laboratory, Oak Ridge, TN, USA
macroscopic surface-initiated damage such as micropitting
in bearings and gears.
Keywords Antiwear additives
Extreme pressure
additives
Additive interaction
Additive decomposition

Power generation
Boundary lubrication wear

Rolling element bearings: general
Ferrous alloys: steel

Tapered roller bearings
TEM
Wear mechanisms
1 Introduction
Tribochemical wear occurs at the interface between a
surface and a lubricant as a result of chemical and
mechanical interactions in a tribological contact. Evidence
of this type of wear is found by analyzing residual surface
tribofilms and the near-surface material exposed to the
tribological contact (depth \ 500 nm). Damage on this
length scale is not usually detectable in its early stages
using standard observation techniques, such as optical
microscopy or surface analytical techniques that do not
have nanometer-scale location resolution. Cross-sectional
transmission electron microscopy (TEM) is well-suited for
probing the microstructure of materials and surfaces on the
nanometer scale. For steel surfaces, the authors have
observed that tribochemical wear can be manifested as
residual material strain, nanometer scale shallow cracks,
and surface particle lift-off into the tribofilm. Although
other mechanisms must be considered, it is believed that
tribochemical wear damage on the nanometer scale
undoubtedly has the potential of initiating macroscopic
surface-related damage modes such as micropitting, peel-
ing, and point-surface origin fatigue spalling.
Enabled by advances in focused ion beam technology
(FIB) to produce TEM specimens during the last decade,
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26
tribochemical wear studies from real hardware surfaces
have become possible. Rainforth et al. [1] were able to
characterize friction-induced oxide layers generated in rig
sliding tests from a variety of material types using classical
TEM sample preparation techniques, but their ability to
perform site-specific analysis on their wear tracks was
admittedly limited. On the other hand, Evans et al. utilized
FIB sample preparation and were the first to evaluate
tribofilm formation and near-surface material damage
trends in tapered roller bearings as a function of lubricant
type and dimensionless film thickness k [2, 3]. In those
studies, shallow cracks were observed on case carburized
AISI 8119 steel raceways only for the most severe
boundary lubrication conditions in an oil without sulfur–
phosphorus extreme pressure/antiwear additives [2]. No
cracks were observed under comparable test conditions
when commercially available sulfur-phosphorus additives
were used [3]. In a separate but similar study, shallow
cracks were observed in a tested tapered roller bearing
raceway surface made of case carburized AISI 8119 steel
only when an intentionally aggressive experimental sulfur–
phosphorus additive package was used [4]. Reichelt et al.
used FIB/TEM to evaluate tribochemical wear of through-
hardened AISI 52100 bearing surfaces after testing with a
variety of lubricants, showing that differences in lubricant
additive formulation can be responsible for stark differ-
ences in tribofilm thickness and composition [5]. Other
recent studies have applied FIB/TEM to evaluate tribofilms
formed in a sliding contact using a lubricant containing
zinc dialkyl dithiophosphate (ZDDP) [6] and in a rolling/
sliding contact using ZDDP and molybdenum dialkyl
dithiocarbamate (MoDTC) [7]. The later study by Laine
et al. sought to characterize the additive effects on micro-
pitting, and shows an example of tribochemical wear
damage (detached steel particles suspended in the tribo-
film) on a case carburized AISI 5115 (equiv.) steel surface,
albeit for the sample tested in ZDDP ? MoDTC with the
best micropitting resistance. It is assumed that the intent of
that study was not to do a full tribochemical wear com-
parison because TEM data were not included for surfaces
tested in the lubricant most susceptible to micropitting
(ZDDP with no MoDTC).
In the previous studies, emphasis was placed on char-
acterizing the effects of lubricant additive formulation and/
or contact conditions on tribofilm formation and tribo-
chemical wear. To the hardware designer, material selec-
tion for tribological surfaces is of equal concern, especially
in applications such as wind turbine transmissions where
new components must work well in a pre-determined
lubrication environment. The objective of this work was to
characterize tribochemical wear with FIB/TEM for two
different types of steel surfaces, one case carburized (AISI
3310) and one through-hardened (AISI 52100), that were
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Tribol Lett (2010) 38:25–32
rig tested identically in a commercially available wind
turbine gearbox oil lubricant. Results indicated that the
manifestation of tribochemical wear was strongly influ-
enced by surface material composition and structure.
2 Experimental
Friction and wear tests were performed using the WAM6
ball-on-disk tribometer (Wedeven Associates, Inc., Edg-
mont, PA), which allows independent control of ball and
disk spindles under load while monitoring traction (fric-
tion) coefficient for the contact. Test balls were made of
AISI 52100 steel with an outer diameter of 20.64 mm and
finished to AFBMA grade 25. Surface finish was measured
for each ball using an interferometric surface-mapping
microscope. The root mean square roughness Sq was cal-
culated for each measurement using three-dimensional
datasets. Ten measurements were made per ball using 209
magnification and the median roughness for each ball fell
within the range Sq * 23–33 nm. Medians are reported
because they better represented the modes of the non-
Gaussian datasets than means. A different ball wear track
was used for each test on the tribometer. The disks were
either through-hardened AISI 52100 or case carburized
AISI 3310 steel with an outer diameter of 101.6 mm. The
nominal composition of AISI 52100 steel is 1.04 wt% C,
0.35 wt% Mn, 0.25 wt% Si, and 1.45 wt% Cr with the
balance Fe. The nominal composition of AISI 3310 steel is
0.11 wt% C, 0.53 wt% Mn, 1.58 wt% Cr, and 3.5 wt% Ni
with the balance Fe. Both disk types had a circumferen-
tially ground finish with median Sq * 471 nm for the AISI
52100 disk and median Sq * 435 nm for the AISI 3310
disk. The disks were measured with an interferometric
surface-mapping microscope in the same manner as the
balls, but with fifty measurements per disk at 109 mag-
nification. The hardness of the test balls and disks was
within the range 58-62 HRC. Post-test optical metallo-
graphic evaluation confirmed the expected microstructures
for the two steel types. Disk surface finish and hardness
levels were representative of those expected for large
rolling element bearings typically found in heavy industrial
and power generation machinery.
Commercially available wind turbine gear oil with ISO
320 viscosity grade and an extreme pressure and anti-wear
(EP/AW) additive package was used as the test lubricant.
The base stock for the oil was polyalphaolefin with specific
gravity *0.87 at 15.6 °C as reported by the manufacturer.
Measured kinematic viscosities were 332 cSt and 33 cSt at
40 and 100 °C, respectively, giving a viscosity index of
140. X-ray fluorescence and optical emission spectroscopy
measurements indicated significant quantities of S, Mg, P,
Zn, and Mo in the oil, which are constituents of the
Tribol Lett (2010) 38:25–32
otherwise unknown fully formulated additive package in
the lubricant.
Both Stribeck-type tests and 24-h wear tests were per-
formed in this study. Stribeck tests were performed to
evaluate traction coefficients in the lubricated contacts as a
function of dimensionless lubricant film thickness k, which
is the calculated minimum film thickness divided by the
composite root mean square surface roughness for the
contact ((S2q,1 ? S2q,2)1/2). Elastohydrodynamic minimum
film thicknesses were calculated using the Hamrock–
Dowson equation for fully flooded elliptical contacts [8]
using pressure-viscosity coefficient information that was
provided by the lubricant manufacturer. The applied nor-
mal load for Stribeck tests was 100 N giving a calculated
Hertzian contact stress of *1.32 GPa. Entrainment
velocity was ramped from 11 to 0 m/s over 150 s, slide-to-
roll ratio or slip was set at 10%, and the disk temperature
was held at 100 °C throughout the tests. Neglecting the
impact of slip on lubricant film thickness and assuming
initial ball and disk roughness levels for k calculations, the
Stribeck tests were estimated to scan from k * 1.2 ? 0.
As a result of these assumptions, the Stribeck plot k scaling
is approximate.
The test conditions for the 24-h wear tests were different
than those for the Stribeck tests. Their purpose was to
generate conditions amenable to tribofilm formation in a
short period of time. To do this, the contact stress was
increased and the entrainment velocity was decreased to
produce boundary lubrication conditions. Applied normal
load was 800 N resulting in a calculated Hertzian contact
stress of *2.65 GPa. Entrainment velocity was 0.6 m/s
with slip held at 10%. The test duration was 24 h, and the
disk temperature was held at 100 °C throughout the entire
test. These conditions provided for k * 0.1, based on the
initial surface roughness. Lubricant was continuously
administered to the center of the rotating disk where it was
spun out across the disk surface in all tests providing fully
flooded conditions. In addition, the ball spindle angle was
set according to the disk track diameter to minimize/
eliminate spin in the contact prior to each Stribeck and
24-h test.
In addition to the above tests, a combined protocol of
24-h tests followed immediately by Stribeck tests were
performed on the same wear track without dismounting the
specimens using the test conditions described above for
each test type.
Two Stribeck tests, two 24-h wear tests, and two com-
bined 24-h wear tests plus subsequent Stribeck tests were
performed on each of the AISI 52100 and AISI 3310 disks.
Examinations of the tribofilms were performed on the
second 24-h wear test track for each disk. To confirm the
presence of a tribofilm and characterize its chemical
composition, X-ray photoelectron spectroscopy (XPS) was
27
performed on the wear track surface. A PHI-VersaProbe
XPS Scanning Microprobe was used with an Ar? gun for
depth profiling. Cross-sectional wear track surface samples
were prepared using focused ion beam (FIB) milling for
evaluation with TEM. Prior to FIB milling, the samples
were ultrasonically cleaned in isopropyl alcohol for 5 min,
tungsten metal was sputtered onto the wear tracks, and the
samples were sectioned to a workable size using a diamond
saw. A Hitachi FB-2000 FIB system with 30 kV Ga? ions
and a micro-sampling apparatus was used for preparing the
lift-out TEM specimens, which were then examined with a
Hitachi HF-3300 FEG TEM/STEM at 300 kV. The lift-out
sample orientation was such that the ball rolled across the
horizon of all images, that is, the major axis of the lift out
sample was parallel with the wear track circumference.
Energy dispersive spectroscopy (EDS) for chemical anal-
ysis was performed in the HF-3300 TEM using a Noran
Six X-ray Special Acquisition system, which uses a
Nano Trace EDS detector with NORVAR light elements
window.
3 Results and Discussion
Traction performance was compared for experiments per-
formed on case carburized AISI 3310 and through-hard-
ened AISI 52100 disks using Stribeck and 24-h wear tests
as shown in Fig. 1. Initial Stribeck tests on the disks with
the wind turbine gear oil did not show a significant traction
difference between the two steel types as seen in Fig. 1a.
This was expected since the disks had comparable rough-
ness and the test duration was presumably too short to
permit full run-in and tribofilm formation. Traction coef-
ficient trends during the 24-h tests (two tests per disk type)
in Fig. 1b indicate lower traction for the AISI 3310 disk
than for the AISI 52100 disk. The wear tracks experienced
run-in and tribofilms formed in these longer duration tests,
so the traction coefficient trends reflect the results of those
dynamics. It is noteworthy that no significant wear loss or
plastic deformation was observed in either of the disk wear
tracks using an interferometric surface-mapping micro-
scope after the 24-h tests. The wear tracks were distin-
guishable from the original disk surface by a slight
reduction in roughness, on the order of Sq * 50–100 nm
lower depending on measurement location. When a Stri-
beck test was performed immediately after a 24-h wear test
on the same track, the traction coefficients across k were
decreased for both disk types as shown in Fig. 1a. This
trend is in agreement with the traction coefficients in the
24-h wear tests, and indicates the presence of run-in
roughness reduction and/or the presence of low friction
tribofilms. AISI 52100 appeared to run at a slightly higher
traction coefficient in the boundary lubrication regime than
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28 Tribol Lett (2010) 38:25–32

(a) 0.20 Fe and O. Chemical shift information indicated the pres-

0.18 52100 - initial ence of mixed phosphates, sulfides, zinc oxides/sulfides,
3310 - initial
0.16 52100 - after 24-hr test and molybdenum disulfide (MoS2) in both tribofilms.
Traction Coefficient
3310 - after 24-hr test
0.14 Excluding film coverage appearance in SXI imaging, the
0.12 XPS chemical data suggested indistinguishable tribofilms
0.10 on the AISI 52100 and AISI 3310 wear tracks.
0.08 To further characterize the differences in tribochemical
0.06 wear damage as a function of steel type, TEM evaluations
0.04 were performed on FIB samples taken from both inside and
0.02 outside of the disk wear tracks. A low magnification cross-
0.00 sectional view of the AISI 52100 sample ground surface
0.01 0.1 1 outside of the wear track is shown in Fig. 2. Selected area
λ (approx.) micro-diffraction (micro-SAD) patterns are inset for the
near-surface material (depth \ 500 nm) and the larger
0.12
(b) subsurface grains. The diffraction patterns were consistent
52100-1
0.10 52100-2 with mixed Fe phases (e.g., ferrite/martensite). Clear spot
3310-1
Traction Coefficient

3310-2
patterns such as the one shown for the deeper grains
0.08 indicated large grains with respect to the diffracting vol-
ume. On the other hand, large quantities of small grains
0.06 within the same diffracting volume produced many over-
lapping diffraction patterns, giving the appearance of rings.
0.04
Qualitatively by these trends, the patterns inset in Fig. 2
0.02 indicated smaller grains near the surface of the sample and
larger grains in the subsurface. The formation of small
0.00 near-surface grains observed in this specimen taken from
4 4 4 4
0 2x10 4x10 6x10 8x10 outside the wear track was attributed to the grinding pro-
Time (s) cess during disk fabrication. Large spheroidal carbides
(size * 1 lm) also were observed in the AISI 52100
Fig. 1 a Stribeck plots before and after 24-h wear tests. Two tests
were performed per disk type to confirm repeatability, but one curve sample shown in Fig. 2. Diffraction and the presence of
from each condition is shown for clarity. Initial disk roughness was bend contours in the image indicated that the carbides were
used to calculate k in the plots. b Traction coefficient as a function of crystalline. EDS revealed that the carbides contained Fe,
test time for the 24-h wear tests. Two tests were performed per disk Cr, and C, whereas minimal Cr was detected outside of the
type
carbides in the Fe matrix. Dark shadows/streaks visible in

AISI 3310, consistent with the 24-h test results in Fig. 1b,
but additional tests would be required to confirm that
observation.
The 24-h wear tests and subsequent Stribeck tests sug-
gested the presence of tribofilms on the surface because
traction coefficients decreased from their initial levels with
increasing contact cycles and test duration. However,
detailed wear track analysis on the disks was required to
explore tribochemical interaction and wear differences.
The first step was to determine whether films were present
on the 24-h wear test tracks using X-ray photoelectron
spectroscopy (XPS). Scanning X-ray imaging (SXI) indi-
cated that tribofilms were present, but their appearance
differed depending on steel type. The tribofilm on the AISI
52100 appeared to be thin and covered the track in thin
streaks. On the other hand, the tribofilm on the AISI 3310
Fig. 2 Cross-sectional TEM image of the AISI 52100 surface outside
appeared thick in blotchy patterns within the wear track
the wear track. Shadows/streaks observed below the spheroidal
area. Depth profiling of these films indicated the presence carbides are attribued to FIB milling. Micro-SAD patterns were
of Mg, P, S, Zn, and Mo in both tribofilms, in addition to collected at the approximate depths indicated by arrows

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Tribol Lett (2010) 38:25–32
Fig. 3 Cross-sectional TEM image of the AISI 52100 wear track
surface. The ball rolled across the horizon of the image in the tribo-
test. Two images were spliced together in this figure, and white
arrows indicate the location of the overlap
Fig. 2 below the carbide particles were attributed to the
different etch rate of the carbide as compared to the matrix
during ion milling from a direction normal to the original
surface.
Tribochemical wear damage was apparent in the wear
track of the AISI 52100 sample as shown in Fig. 3. The
tribofilm appears bright in the TEM image because it has a
smaller interaction cross-section than the steel substrate.
The surface experienced shallow cracking and penetration
of the tribofilm into the surface. This damage was limited to
the near-surface material and did not penetrate deeper than
200 nm into the surface. In the center of the spliced image
in Fig. 3, the tribofilm completely surrounds a portion of the
original surface which presumably would have become a
debris particle by mechanical detachment with continued
tribological contact. The tribofilm was discontinuous across
the wear track sample, with thick (*100 nm) and thin
(*10 nm) regions, and there were areas with no tribofilm
present.
At conventional TEM magnification, the AISI 52100
wear track tribofilm appeared to be mostly homogeneous in
structure and composition. EDS data for the tribofilm
shown in Fig. 4 indicated the presence of Mg, P, S, Zn, and
Mo, as well as C, O, and Fe, consistent with the XPS
observations. Cu and W in Fig. 4 are attributable to the
TEM grid and FIB protective cap layer, respectively.
However, closer inspection of the AISI 52100 tribofilm in
high-resolution TEM mode (HRTEM) as shown in Fig. 5
revealed atomic-scale crystalline features. Figure 5a shows
a thick region of the tribofilm (*100 nm) in which long
lattice fringe sheets are visible (assuming three-dimen-
sional structure). The large sheets were found predomi-
nantly near the bottom of the tribofilm at the interface with
the steel and near the top surface of the tribofilm. As shown
in a thinner region of tribofilm (*30 nm) in Fig. 5b, the
sheets could consist of 2–10 lattice fringes and generally
were oriented parallel to the surface in these cross-sectional
29
C
1500
Counts
75 Zn W
Mg
P
Mo, S
50 Zn
W
Cu
25 Fe Zn Mo
Si
0
0 2 4 6 8 10 16 18 20
Energy (keV)
Fig. 4 EDS data indicating the overall composition of the tribofilm
on the AISI 52100 wear track sample. The Cu signal is from the TEM
grid
views. Measured fringe spacing was *0.6 nm, consistent
with the c-axis basal plane spacing of MoS2. In addition to
large MoS2 sheets, suspended Fe particles were detected in
the tribofilm with EDS that presumably detached from the
original substrate as the tribofilm was forming during tri-
bological contact.
Significant differences were observed in the near-sur-
face material and tribofilm structures found for the AISI
3310 disk as compared to the AISI 52100 disk. Figure 6
shows a cross section of the AISI 3310 disk at a location
outside of the wear track. Similar to the AISI 52100 case,
fine-grained material was found at the near-surface region
(depth\500 nm) and larger grains were observed deeper in
the material. The inset micro-SAD pattern of the near-
surface material in Fig. 6 shows distinct rings consistent
with Fe phases that indicate a finer grain structure than that
observed for the AISI 52100 sample at the same depth. In
addition, significantly smaller spheroidal carbide inclusions
(size * 100 nm, an order of magnitude smaller than car-
bides in AISI 52100) were uniformly distributed through-
out the sample. EDS indicated that Cr was segregated to
the carbide phase, and that Ni was present in the Fe matrix
as expected.
Tribochemical wear damage was not observed within
the AISI 3310 wear track. In fact, the AISI 3310 tribofilm
differed from the AISI 52100 tribofilm in thickness and
structure considerably. As shown in Fig. 7, the tribofilm on
AISI 3310 was mostly smooth, uniform, and continuous
across the sample. Its thickness was *200 nm, and a sharp
interface was observed between the tribofilm and the steel
surface. No cracks, tribofilm penetration, or suspended
debris particles were observed. Closer inspection of
the tribofilm structure in Fig. 8 revealed a mostly
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30 Tribol Lett (2010) 38:25–32

Fig. 6 Cross-sectional TEM image of the AISI 3310 surface outside

the wear track. Gray spheroidal inclusions in the matrix are carbides.
Micro-SAD patterns were collected at the approximate depths
indicated by arrows

Fig. 5 Cross-sectional HRTEM image of the AISI 52100 wear track

tribofilm at a thick and b thin locations. Arrows indicate example
locations of lattice fringes with a measured spacing of *0.6 nm

homogeneous structure through the thickness of the film.

However, many *10 nm long curved sheets (again
assuming three-dimensional structure) filled the volume of
the film as indicated by lattice fringes in Fig. 8b. The
predominant orientation of these sheets was parallel to the
surface, but many examples of sheets that curl in random
directions were found. Although most of the sheets did not
appear to have long-range order in the c-axis direction, Fig. 7 Cross-sectional TEM image of the AISI 3310 surface inside
short stacks of sheets (2–5 sheets thick) were found with the wear track. The ball rolled across the horizon of the image in the
tribo-test
spacing of *0.6 nm, again consistent with MoS2 as was
observed for the larger sheets in the AISI 52100 tribofilm.
Micro-SAD was performed on the thick AISI 3310 tribo- A tribofilm structure containing dispersed small MoS2
film and rings indexable to MoS2 (molybdenite-2H) as sheets was reported previously by Grossiord et al. [9]. The
shown in Fig. 9a were observed. EDS as shown in Fig. 9b sheets were generated in reciprocating sliding tests in an
confirmed the expected presence of P, S, Zn, and Mo, as AISI 52100 steel contact with base oil containing the
well as C, O, and Fe in the tribofilm. MoDTC additive only. Wear debris were collected on a

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Tribol Lett (2010) 38:25–32 31

(a)

2500
(b) C

2000
Mo, S
1500
Counts

1000

O
Cu
500 Cu P Zn Mo
W Fe
Cu Mo
0
0 2 4 6 8 16 18 2
20
Energy (keV)

Fig. 8 Higher magnification cross-sectional TEM images of the AISI
3310 tribofilm structure. a A view of the tribofilm attached to the
substrate and b a higher magnification view of the film structure
revealing curved lattice fringes with a spacing of *0.6 nm in
locations where they are stacked
holey carbon grid after testing and examined in TEM.
Their tribofilm particles contained almost identical small
dispersed MoS2 sheets as were observed in the intact AISI
3310 tribofilm in the present study (Fig. 8). Consistent with
the present observations, Grossiord et al. did not detect
MoS2 crystals with long-range order or stacked sheets (i.e.,
no (002) rings in diffraction patterns collected from the
tribofilm particles). Because commercial wind turbine gear
oil was tested in the present experiments, it is not possible
to conclude whether MoDTC was present in this formu-
lation, but the agreement between the present and the
Grossiord et al. results are striking. It is also interesting that
the Grossiord et al. tribofilms were produced in an AISI
52100 reciprocating sliding contact whereas a similar
Fig. 9 a Micro-SAD pattern from the bulk tribofilm on the AISI 3310
wear track surface indexed to MoS2 (molybdenite-2H) and b EDS
spectrum also collected from the AISI 3310 tribofilm
tribofilm nano-structure was observed in the AISI 3310
case only in the present rolling/sliding contact study. This
observation suggests that base material alone likely does
not solely determine tribofilm structure, but that many
other tribological factors must influence tribofilm structure
formation on a nanometer scale.
4 Conclusions
Tribochemical wear differences between the AISI 52100
and 3310 steel types were apparent in the TEM on multiple
length scales. Whereas the traction coefficient results
during rig tests were similar and the tribofilm compositions
as measured by XPS were approximately the same, the
near-surface material structures and tribofilms were dif-
ferent at the micro- and nanometer levels in the samples
studied. The AISI 52100 near-surface material structure

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consisted of a Fe matrix with a relatively coarse grain
structure containing large (Fe, Cr) spheroidal carbides. In
contrast, the AISI 3310 near-surface material structure was
Fe containing Ni as expected and a relatively finer grain
structure with smaller (Fe, Cr) spheroidal carbide inclu-
sions. Tribochemical wear was detected for the AISI 52100
wear track only. It had a tribofilm with non-uniform
thickness, shallow cracks, and penetration of the tribofilm
into the surface. On the other hand, the AISI 3310 wear
track had a uniformly thick tribofilm with no cracks or
penetration into the surface and a sharp, smooth interface
with the original substrate. The tribofilm nanostructure for
the AISI 52100 case contained large MoS2 sheets that
generally ran parallel to the substrate and were segregated
to the surface and interface, as well as suspended Fe par-
ticles in the film. Smaller MoS2 sheets were dispersed
uniformly and oriented somewhat randomly throughout the
AISI 3310 tribofilm in sufficient quantity for identification
by micro-SAD.
This study introduced many new technical questions.
What characteristics of the AISI 52100 surface made it
more susceptible to tribochemical wear (e.g., cracking,
tribofilm penetration, surface particle detachment) under
the present test conditions than the AISI 3310 surface?
Why was MoS2 incorporated in the AISI 52100 tribofilm as
large sheets rather than smaller uniformly dispersed sheets
as in the AISI 3310 tribofilm? What roles did alloy com-
position (e.g., the presence of Ni in AISI 3310) play in
tribofilm formation and damage susceptibility? Future
work is required to address these open issues, and the
challenge remains to develop generalized scientific mech-
anisms that describe more than just one specific situation at
a time.
In addition, nanometer-scale tribochemical wear dam-
age has not yet been directly linked to macroscopic surface
damage modes like micropitting or point-surface origin
spalling. However, high-load, high slip in rolling/sliding
contact, and boundary lubricated contact conditions such as
those used to generate tribochemical wear damage in this
study have been associated with micropitting [10, 11] in
bearings and gears. Although the present results alone do
not definitively preclude the use of AISI 52100 in wind
turbine bearings, the intention of this work is to show the
extent to which lubricant-material interactions and result-
ing microscopic damage can differ based on the material
selection alone with all else constant. Admittedly, the ball-
on-disk test settings in this study were aggressive in contact
stress and slip compared to typical wind turbine gearbox
bearing conditions to accelerate the rate of tribofilm for-
mation within the 24-h test duration. However, this work
makes it clear that material selection and surface charac-
teristics can affect the propensity for tribochemical wear
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Tribol Lett (2010) 38:25–32
damage, so it is recommended that tribochemical wear and
lubricant compatibility be evaluated during the material
selection phase of new product development programs
whenever possible.
Acknowledgments The Timken Company is acknowledged for
support of this work and permission to publish. D. W. Coffey from
Oak Ridge National Laboratory is acknowledged for FIB sample
preparation. G. A. Richter from The Timken Company is thanked for
tribology test lab assistance and for performing the rig tests. P. J.
Shiller and R. L. Aubrey from Timken are also acknowledged for
lubricant characterization. W. Jennings from Case Western Reserve
University is thanked for X-ray photoelectron spectroscopy assis-
tance. Microscopy research at Oak Ridge National Laboratory’s
SHaRE User Facility was supported by the Scientific User Facilities
Division, Office of Basic Energy Sciences, U.S. Department of
Energy.
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