Transient Processes in Tribology

G. Dalmaz et al. (Editors)

9 2004 Elsevier B.V. All fights reserved

377

Performance and Surface Analysis of Tapered Bearings Lubricated with a Manual

Transmission Fluid
Carl F. Kernizan a Susie Hurley b, Michael Gahagan b and Wayne D. Jennings c

aThe Lubrizol Corporation, 29400 Lakeland Blvd Wickliffe, OH 44092-2298, USA

bLubrizol International Laboratories, The Knowle Hazelwood Belper Derbyshire DE56 4AN, UK
CCase Western Reserve University, Cleveland OH 44106, USA

The comparative tribological performance of a series of tapered bearings lubricated with a fully
formulated manual transmission fluid (MTF) and its PAO base oil was obtained using a KRL thrust bearing
tester. Bearing performance was based on the successful completion of an eight hour test procedure created for
the KRL tester. Optical microscopy was used to conduct textural analyses on the body contact areas of tested
rollers while X-ray photoelectron spectroscopy (XPS) depth profiles were used to collect surface film
composition at the previously mentioned contact area. The KRL results indicated that the MTF operated at lower
temperatures and performed better than the PAO. This difference was ascribed to the enhanced thermal stability
of the additive packages used in the fluid. The optical analyses detected a series of dark bands at the body
contact area of all tested rollers indicative of the presence of an EP/AW surface film. XPS depth profiles of the
base oil indicated that it generated a mixture of organic carbon and iron oxide which proved ineffective under
more severe test conditions. In contrast, the profile of the MTF included a mixture of carbonate, borate, sulfide,
phosphates and oxide throughout the film. Finally, the combination of thermal stability and EP/AW film
composition was attributed to the better performance of the MTF.
1. INTRODUCTION
Over the past decade, dedicated manual
transmission fluids have been developed to meet the
ever increasing requirements demanded by
equipment manufacturers (OEM) and government
legislations [1-2]. This process has involved the
careful balance between meeting these requirements
and the cost of development.
The first sets of costs are associated with the
selection of the base oil. This step is predicated by
the need for fuel efficiency, reduced oil capacity,
shear stability, thermal and oxidative stability.
These requirements have eliminated most of the base
stocks except those with high viscosity indices
(HVI) [3-4.]. Even with these requirements, their
high prices have somewhat limited their usage. But,
cost balance has been improving with reports of 5 to
10~
reductions in operating temperatures of
transmissions lubricated with such base stocks [3].
Other requirements such as load carrying capacity,
wear, pitting, synchromesh compatibility and
corrosion resistance have been found to depend on

the careful selection of chemical additives [1, 5-6].

Significant cost reduction has been achieved by the
systematic use of experimental designs [6]. Graham
et al. have reported that certain sulfur-phosphorous
additives were found to impact synchromesh and
pitting while O'Connor et al. have reported the
careful balance of the dispersants, friction modifiers
and Cu passivators to be critical for effective wear
and friction reduction [ 1, 6].
The second sets of costs involved in MTF
development are associated with proof of
performance of the blends derived from these
experimental designs. Obviously, the time required
to obtain API GL-4 qualification greatly limits the
number of blends that can be selected for this
process [1, 5]. To minimize the testing time and
achieve the performance requirements, lubricant
manufacturers have used various types of bench tests
[6-7]. This approach has allowed greater control
and flexibility over the operating parameters,
specific topics from the OEM list of requirements
and types of components used in these tests. It has

378
also increased the ability to correlate tribological
responses with the additive effects in the fluid and
surfaces of the tested components [9-13].
The aim of this paper is to present the use of
this approach for the development of an MTF. First,
a KRL bearing shear stability tester was selected for
the performance testing. [8-9]. Field experience had
shown that this method showed good correlation
with actual transmission tests [1]. With additional
modification of the rig, thermal stability and
frictional torque were also monitored and recorded.
Finally, surface analysis was used to verify that
typical tribological films could be generated with
this approach.
2. E X P E R I M E N T A L
A PAO and its fully formulated MTF
analogue used for this study were selected from a
multi blend lubricant matrix. They were designated
A and B, respectively. A was selected because of its
viscosity, HVI and shear stability [3]. B was then
formulated with a series of additive packages
designed to reduce operating temperatures, promote
surface film formation, and passivate non steel based
components. The relevant information for the two
fluids was listed in Table 1.
All tribological tests were conducted with a
Shell four-ball tester modified in accordance to the
DIN 51350 Part 6 procedure referred to as a KRL
thrust-bearing rig (8-9). All tests were conducted
with a 40mm bore tapered bearing, a 35ml lubricant
volume and a four step two cycle 8H tribological
sequence. In Step 1 of the KRL test, the load was
set at the maximum value of 5.825KN to 350rpm for

an operating time of one hour. This break-in step

was necessary to prevent bearing damage and
premature thermal runaway In Step 2 and Step 3, the
speed was changed to 1500rpm and 3000rpm for a
1H duration at each respective step. In Step 4, the
speed was first decreased to 350rpm and increased
to 450rpm for two hours. This step was designed to
allow the lubricant to recover thermally before the
process was repeated for the second cycle. A pass
or fail performance rating was then assigned to the
samples based on reaching the eight hour operating
time limit or premature motor shutdown. The cutoff limits for motor shutdown were set at 200~ and
5Nm for temperature and torque, respectively. This
tribological sequence is graphically shown in Figure
1.
Optical microscopy and XPS were then
used to analyze the surfaces of the tested bearings at
the end of test. Optical photographs of the roller
body (RB) were collected with a digital camera to
visualize the pre and post surface texture of the
various rolling element components. XPS survey
scans using a PHI 5600 XPS system were first used
to obtain surface elemental compositions at the large
end (LE) areas of the rollers [10]. To further probe
the composition and thickness of the tribological
films, depth profiles were then collected at the
previously surveyed locations. Depth profiling was
conducted by the removal of successive film layers
with an Ar ion sputtering gun attached to the XPS
system at a rate of 40A/min. An indication of film
removal was obtained once the Fe concentration
reached a maximum value and no longer increased.
The detectability limit for this technique is about 0.1
atomic percent for everything except H and He
which are not detectable.

Table 1. Listing o f the properties of the test matrix.

Samples
Type
A
B

PAO
Amine Phosphate AW; Sulfur EP-AW
Borated Dispersant; RI-Demulsifier
Amine Anti Oxidant, Foam Inhibitor; Cu Inhibitor

VI

Viscosity (cSt)
40~
44
48.0

100~
8.0
7.87

136 .......
137

379
Figure 1. Tribological test procedure.
Sequence

KRLTest
3500

"r

e
"I~

_~

Cycle 1

I~~

T
t Step3

-!

Cycle 2 .................... ~

~I

0~--~-Speed._
Load

Step3

.........................................

2000 I
~oo

. . . . . . . . . . . . . . . . . . . . .

3000 ...............
Ii
"-'t= 2 5 0 0

. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

~!

..........................

I000

l l l I. I~-I~III-I

I11 ~"ii

--~'~i "~III

..

500

t~

~I llllll Ill
Step

r~

r~

..................................................................

r~

v~

c~

Operating Time (H)

3. RESULTS & DISCUSSIONS
This section was divided into two
segments. In the first, explanations relating the
recorded thermal signals and their physical meaning
were presented. In the second, optical and XPS
analyses of the tested components were then used to
complement the tribological data.
3.1 Tribological Results
The temperature and torque results, T and
M, for A and B are shown in Figures 2 and 3,
respectively. The data indicated that B successfully
passed the test while the failures for A were thermal
rather than torque related. The traces suggested the
presence of at least four tribological regimes which
were directly coupled to the speed changes of the
testing sequence. These regimes depicted different
tribological interactions whether temperature and
torque were in or out phase with each other.
The first regime was observed during Step
1 or the break-in process of testing.
The
temperatures doubled in value from their room
temperature starting points while the torque values
steadily decreased. This out of phase behavior
signified the transition point from boundary to
mixed/EHD lubrication regime. It is usually the
point where the rib of the cone and the large end of
the roller are at their maximum contact [8-9]. It

usually is very severe and requires EP/AW additives

to generate a tribological film with the proper wear
and friction reducing characteristics to help it
survive this transition. Since no failures occurred,
both fluids must have generated this type of
tribological film. This behavior was expected for B
but was somewhat surprising for A. However, the
literature suggests that this process could be
promoted by the oxidation induced polymerization
of the hydrocarbons in the base oil [11]. This
explanation is plausible since no anti oxidant was
present in A.
Two different behaviors were observed
during Step 2. They were called regime 3 and
regime 2 for A and B, respectively. After the speed
increase, the thermal traces for both tests with A
increased linearly until they reached the 200~ shutdown limit. The torques also increased but levelled
off before reaching the 5Nm values. Failure was
temperature related and was assumed to be caused
by two reasons. The first was due to the inability of
A to dissipate the heat induced by the speed
increase. This increase must have reduced the
effective fluid film in the contact zone due to higher
shear forces and caused a transition from EHD to
mixed or boundary lubrication mode [12]. This

380
Figure 2. Temperature traces.

behavior however is not completely understood

since discrepancies with experimental data such as
heat capacity, viscosity improvement, and
coefficient of traction still exist [13]. The second
was due to the inability of the existing tribological
film to effectively reduce the torque when the
contact transitioned from EHD to boundary
lubrication mode.
In this regime, torque and
temperature responses were in phase with each

other.
The observed behavior for B during Step 2
was very different and was called regime 2. In this
regime, the thermal responses nearly doubled but
equilibrated during the duration of the speed
increase. The ability of the fluid to dissipate this
thermal input was obviously related to its shear
stability and effectiveness of the additive
components in the formulation. The maximum

381
recorded temperature for both tests during that
operating time was 95~
Small spikes followed by
sharp decrease were also observed for the torque
responses. These spikes coincided with the speed
increase and were related to temporary reductions in
the fluid films due to the induced high shear forces.
However, unlike in A, the values decreased very
quickly. These sharp decreases were explained by
the formation of an effective surface AW film that
further helped with the reduction of the heat input
[14-15]. The observed stabilization was therefore a
combination of fluid thermal stability and AW film
formation. This combination must have promoted
the transition from temporary operation in the
mixed to true operation in the EHD lubrication
regime. In this regime, torque and temperature
were out of phase with each other. Interestingly,
regime 2 like behavior was also observed for Step 3
of the test cycle. The temperature similarly doubled
and gradually equilibrated to a maximum value
around 130~ for both tests. Similar to Step 2, the
torque spikes were related to the speed increase and
their reduction to the formation of the AW film.
Thus, shear stability, additive composition and AW
film formation were again responsible for this
excellent tribological behavior. However, it was
not clear whether the same type of AW surface
films were generated since time dependent studies
were not undertaken.
Table 2. Summary of tribological behaviors.
Regimes
Test Sequence
T&M

2&3

'4

Regime 4 was finally observed during the

speed decrease of Step 4.
The temperatures
decreased to about 50~ while the torques quickly
doubled followed by a gradual decay to their final
values. This process covered the entire half of the
1H time duration and was mostly a response to the
speed decrease. The speed change probably forced
a temporary transition from EHD to mixed
lubrication regime which would account for the
observed torque increase. However, the lowered
applied speed and load caused a decrease in the
temperatures and must have reversed the contact
back to the EHD regime. Torque and temperature
were out of phase. This was also the first case
where temperature decreased before torque.
Very similar behaviors were observed
during the steps of the second test cycle. However,
they did not seem to have the same performance
effects as in the first cycle since no failures were
recorded for B. The obvious differences were the
absence of a torque break-in spike and regime 3.
Besides these two, all remaining behaviors were
identical to those previously observed and described
by regimes 1, 2 and 4. The explanations and
correlations advanced for the four observed regimes
are summarized in Table 2.

Lubrication Regime

Out of phase

Boundary to EHD

Out of phase

EHD

In Phase

EHD to Boundary- Failure

Out of PhaSe

EHD to Mixed back to EHD

3.2 Optical and Surface Analysis

The optical and XPS analysis were then
used to confirm and differentiate the surface films
residing on the tested components.
Optical
photographs of a new roller and two used rollers
from tests AI and BI were shown in Figure 4.
When compared to the new roller, the tested rollers

showed a series of bands intertwined with

circumferential score marks along their RB areas [89]. They also showed a single band and a number
of tangential scratches along their rib roller contact
areas.
The orientation of these scratches was
suggestive of slip or misalignment in that area
during testing. These bands were clearly remnants

382

of the EP/AW surface films formed by the two

lubricants during these tests. It was not surprising
to see heat or other failure related damage on A
since the test time was very short.
The profile of the LE area for the new
roller is shown in Figure 5. The elemental analysis
indicated the presence of Fe, C and O and a total
film thickness of the order of 900A. To further
probe the profile both Cls and Fe2p binding

energies are shown in Figure 6. The figure showed

binding energy, intensity and sputtering cycles as
the X, Y and Z axes, respectively. For the Cls
binding energy, a peak at 285.2eV was observed
until the 15 th cycle and a new peak at 282.3eV for
the remainder of the profile. The first assignment
suggested that the C was amorphous while the
second from a carbidic source [10].

Figure 4. Roller optical images.

Likewise, the Fe2p3/2 binding energy showed a

broad peak around 709eV from the surface to about
the 15 th sputter cycle. It then shifted to 707.3eV
from that point until the end of the profile. The first
transition was assigned to an iron oxide while the
second to Fe metal.
These analyses suggested that the film was

composed of a mixture of amorphous C and iron

oxide from its surface to a depth of about 150A.
Beyond this depth, it was most likely iron carbide
and Fe metal expected for an austenitic type bearing
steel.

Figure 5. XPS depth profile of a new roller.

11:1:1

..........................

x ............

x .....

. . . . . . . . . . . . . . . . . . . . . .

'%.

\\
\"\ ~\.
N
L-

..,.=-:

,4.

r:l

1 o

121

loo

21~

~ r'Jl~

r-j

L:5~:~u-H~_r

O~_p-tl

4-

-- Clt'J

383

Figure 6. C ls and Fe2p3 binding energies of the new roller.

2p312

,:/"

CIg

Fe2p 2p~2/ ~.

,t
t

!i

1--

'

03 m

'11!5
L

Beyond the 55 th sputter cycle, only the Fe metal

peak was visible. These results suggested that the
film was a mixture of a C-O rich phase and iron
oxide to a depth of 500A. It then became mostly
iron oxide and amorphous C around 1500A. At
greater depths, it was mostly mixture of iron
carbide and Fe metal.
These analyses partially supported the
behavior described during tribological regimes 1
and 3.
The organic carbon like phase in
combination with the iron oxide was most likely
the EP/AW surface film created during regime 1.
It was effective during the break-in step but failed
to mitigate the high heat input experienced during
regime 3.

The depth profile for AI is shown in

Figure 7. It indicated that the tribological film
was of the order of 2500A and composed of Fe, C
O and Si. Its Cls and Fe2p binding energies,
shown in Figure 8, indicated that this film was
more complex than that of the new roller. A peak
at 286.4eV was observed until the 6 th sputter
cycle of the C ls binding energy. The peak
position indicated that it belonged to organic C
bound to O. This peak then gradually shifted to
the C ls 285eV and to the carbidic 282eV binding
energies at higher sputtering cycles [10]. The
Fe2p3/2 binding energy showed a broad oxide
peak around 710eV from the surface to about the
30 th sputter cycle. From that position to the 55 th
cycle, both the oxide at 710eV and the Fe metal
peak around 707.3eV were present in the film.
Figure 7. Depth profile of the LE of a roller tested with A.
I~Zm~

~'-'-'~-----~,

I D o

--

.--o

~..,

'%,~

"\,.
,-..
",.,,.
. . . .

'----...

s--

..

"-% .......

=;oo

1 iOR:lO

15z:x3
"~:,u~k=r

13~plh

~ll:X3

384
Figure 8. C1 s and Fe2p3 binding energies for A.

Fe2p

9 I~

Cls

2p3/2

Z ~I~

2pl/Z

. . . .

~",,

The profile for the LE of B1 is shown in

Figure 9. It indicated that the film was of the
order of 2000A and composed of Fe, C O, B, N,
Ca, S, P and Na. The profile indicated that C, B,
P, S and O were very active at or very near the
surface of the film.
Due to this increased
complexity, the B ls, S2p and P2p binding
energies were shown in addition to the C ls, and
Fe2p. This information is presented in Figures 10
and 11, respectively. The data from Figure 10
indicated the B, S and P concentrations
disappeared by 24 th cycle or about 500A. One
peak at 192.03eV corresponding to a borate was
assigned for the B ls binding energy. It was
interesting to see that the dispersant behaved as
an AW agent in agreement with published data
[14-15].
A second peak at 162.61eV was
assigned to the S2p also in very good agreement
with published data [15-17]. The third peak at
133.2eV was assigned to the P2p and

-I

-n

.-2o

-I~

'le"

--- ~ L

corresponded to a polyphosphate type phase.

This type of structure has also been reported in
the literature [15-19]. The C1 s binding energy
indicated that the very top of the film was
composed of a carbonate at 288.8eV and
amorphous C at 285eV. The peak then shifted to
the carbidic region at 282.4eV after the 6 ~
sputtering cycle. The Fe 2p3/2 binding energy
indicted the simultaneous presence of an oxide at
709.90eV and Fe metal 706.28eV until the 10th
cycle. Beyond that point, it was mostly Fe metal.
These results were in very good
agreement with the tribological behaviors
observed for this lubricant. They indicated that a
very effective EP/AW film composed of a borate,
iron oxide, iron carbonate, iron sulfide and iron
phosphate was present at a depth of at least 500A
on the surface of the roller. Beyond that depth,
the surface film was mostly iron oxide. This was

Figure 9. Depth profile of the LE of a roller tested with B.

.~

WO-

,,,.,....

L aa-i--

/,

r,~

'-'Sputter Dept'h'*~)

385
Figure 10. B l s, S2p and P2p binding energies for B.

/
'~~

,'. ,,' ,

< v

2eo

~'""

,.

"

i'

'I"

"~(~',.

".-.

r.. g v V'" '-' "> I

!'90

;"

"," ..

'~

to/

1r

8imin 9 ~r~y

" '

. '

,,

tao--

1r

130 1

levl

Figure 11. C ls and Fe2p3 binding energies for B.

Cls

"'<

t"~. ~

z-

t1

"-

1--

--..~-..._~_.-~..._~ . ~ >
/

,/

....

'I 711:! tt

/-

-,,
o

Binding Energy (el/)

the typical tribological film expected and reported

in many tribological studies [ 14-19]. It featured a
series of phases usually associated with EP and
AW activities in filed tested components. Low
film thickness, 2000A for B, was obviously an
area of concern for this type of simulation. But, it
was clear that it was dependent on operating time.
The XPS analysis was summarized in Table 3.
4. CONCLUSIONS
These results indicated that a combination of
base oil properties and effective additive selection
is necessary to formulate a high performing MTF.
The data indicated that at low severity, the
viscometrics of the base oil and its ability to form
a surface film composed mostly of iron oxide and
amorphous C were sufficient to allow it to move

.--.111

-~o

.-

-z~

-~o

/-

-I s

.t-

-to

.i

-.on

Binding Energy (eV)

from the boundary to the mixed/EHD lubrication

mode. However, as test severity increased, the
previous combination became ineffective and the
base oil failed the tests. The analysis for B
indicated that it generated a fully functioning
EP/AW film matching the borate, sulfide,
polyphosphate type chemistries required to
transition form the boundary to a full EHD
lubrication mode in any MTF application.
Finally, this work has shown that the combination
of lubricant design, bench testing and surface
analysis can be used for the successful
development of manual transmission fluids.

386
Table 3. SummarT of the XPS analysis.
Samples
Elements
Binding Energies
(eV)
New
Cls
285.2
282.3
Fe2p3/2
709
707.3
A
Cls
286.4
285-282
Fe2p3/2
710
710-707
707
B
Cls
288.8
285.0
Bls
192.03
$2p3/2
162.61
P2p3/2
133.2
Fe2P3/2
709.9-706.8
706.8

Sputter Cycle

Thickness

Compound Type

0-15
15-30
0-15
15-70

0-120
120-900
0-40
40-900
0-40
40-2500
0-40
40-1200
1200-2500

C & Iron Oxide

Carbide
Iron Oxide
Fe Metal
C-O&C
C & Carbide
Iron Oxide
Oxide & Fe Metal
Fe Metal
Carbonate
C
Borate
Sulfide
Phosphate
Oxide & Fe Metal
Fe Metal

,,,

...

0-6

6-70
0-30
30-55
55-70
0-4
4-40
0-24
0-24
0-24
0-24
24-40

0-30

30-2000
0-500
0-500
0-500
0-500
500-2000

REFERENCES

1.

2.

3.

4.

5.

6.

7.

Graham, R., Cain, R.W., and Peal, S.N.,

"Fluid
Development
for
Manual
Transmission Applications," SAE Paper
961911 (1996).
Graham, R., Gahagan, M.P., Bigelow, S.S.,
and Cain, R.W., "Lubricants for Optimised
Manual Gearbox Performance," CEC97-TL3
(1997).
Sasaki, T., Ohmori, I., Furumoto, M.,
Tanaka, H., Komiya, K., Ohsumi, T. and
Henmi, M., "Development of automotive
Lubricants Based on High-viscosity Index
Base Stock," SAE Paper 951028 (1995).
Sztenderowick, M., and Lok, B., "Base Oils
to Meet Future Requirements: ILSAC GF-3
and Beyond," NPRA 1997 Annual Meeting,
(1997).
Demyen, G.Y., and Mullins, W.W.,
"Extended-Drain Field Testing of BoratedBased Group II Lubricants in Heavy-Duty
Axles and Manual Transmissions", SAE
Paper 982717 (1996).
O'Connor B.M., van Mullekom, J.H.,
Gahagan, M.P., Rank, R. and Jahn, W.,
"Influence of Additive Chemistry on Manual
Transmission Synchronizer Performance",
SAE Paper 2002-01-1697 (2002).
Barzaghi, C., Berti, F. and Gommelini, C.,

(A)

8.

9.

10.

11.
12.

13.

"Development of a Bench Test Procedure for

assessing the effect of Lubricant on Car
Manual Transmission efficiency", SAE Paper
951027 (1995).
Kernizan, C.F., "Comparative Tribological
Performance and Chemical Results of a
Commercial Grease Targeted for High
Performance Tapered Bearing Application,
NLGI Spokesman, 60, 5, 36 (1996).
IBID, Torque and temperature signatures of
grease lubricated tapered bearings", NLGI
Spokesman, 61, 2, 8 (1997).
Moulder, J., Stickle, W.F., Sobol, P.E., and
Bomben, K.D., "Handbook of X-ray
Photoelectron Spectroscopy", ed. Chastain,
J., Perkin-Elmer, MN (1992).
Fischer, T.E., "Tribochemistry," Ann. Rev.
Mater. Sci., 18, 303 (1988).
Glonea, R.P., Spikes, H.A., Jones, W.R. Jr.,
"Behaviour of Several Lubricants for Space
Applications
under
Transient
Speed
Conditions", J, Syn. Lubr., 19-3, 191 (2002).
Kernizan, C.F., Bartlett, M., Wetsel W.R.,
and Jennings, W.D., "Performance and
Surface Analysis of Tapered Bearings
Lubricated with a Poly-c~-Olefin and a Group
III Base Oil", Presented and submitted for
publication at the 58th STLE Meeting
(2003).

387
14. Liu, W., Yu, L., and Xue, Q., "An
Investigation of the film formed in the Borate
Oil Immersion Test", Thin Solid Films, 245,
1-2, 833 (1994).
15. Papay, A. G., "Antiwear and ExtremePressure Additives in Lubricants", Lubri. Sci.
10, 209 (1998).
16. Baldwin, B.A., "Relationship between
Surface Composition and Wear: an X-ray
Photoelectron Spectroscopic Study of
Surfaces
Tested
with
Organosulfur
Compounds", ASLE Trans. 19, 335, (1976).
17. Lara, J., Blunt, T., Kotvis, P.V., Riga, A and
Tysoe, W.T., "The surface and Tribological
Chemistry of Carbon Disulfide as an
Extreme-pressure Additive", Wear 239, 77
(2000).
18. Gauthier, A., Montes, H. and Georges, J.M.,
"Boundary
Lubrication
with
Tricresylphosphate (TCP). Importance in
Corrosive Wear", ASLE Trans. 25, 445
(1982).
19. Najman, M.N., Kasrai, M., Bancroft, G.M.
and Miller, A., "Study of the Chemistry of
films Generated from Phosphate Ester
Additives on 52100 steel Using X-ray
Absorption Spectroscopy", Trib. Lett. 13, 3
(2002).