Materials Science and Engineering A 415 (2006) 7279

Development of a high-speed cryogenic tribometer:

Design concept and experimental results
B. Subramonian a , Bikramjit Basu b,
aJSPS Ronpaku fellow, Department of Space, Thiruvananthapuram, India
b Laboratory for Advanced Ceramics, Department of Materials and Metallurgical Engineering,
Indian Institute of Technology, IIT-Kanpur, India
Received in revised form 31 August 2005; accepted 20 September 2005

Abstract
In order to evaluate the tribological properties of ball bearings used in high-speed cryo-turbopumps of liquid rocket engines, a tribometer to
operate at high sliding speed in cryogenic environment is required. In order to meet the above requirements, a new high-speed cryo-tribometer has
been designed. With this new tribometer, the evaluation of friction and wear mechanisms of various self-mated materials and solid lubricant coatings
under high sliding speeds (>0.545 m/s) with high Hertzian contact stresses (up to 2.5 GPa) in cryogenic fluid is now possible. Two additional
features available with this new cryo-tribometer are: (a) a mono-ball rolling-on-disk tester under the above conditions for the analysis of rolling
friction and (b) the testing of unlubricated and lubricated ball bearing (10 mm diameter bore) submerged in liquid nitrogen or liquid helium under
very high-speed (36,000 rpm). An additional provision has been made for the continuous measurement of bearing frictional torque at a maximum
axial load of 50N. The design details of the new tribometer are the major focus of discussion in this paper. This paper also reports the results of a
very first set of experiments conducted on self-mated 440C steel and AISI 304 steel under liquid nitrogen (LN2 ) immersed condition with selected
testing parameters. Testing of ball bearings with Pb-IP coating at 36,000 rpm under liquid nitrogen also has been carried out. Additionally, the
wear mechanisms for self-mated steel in cryogenic liquid are also discussed.
2005 Elsevier B.V. All rights reserved.

Keywords: Cryo-tribometer; COF; Space tribology

1. Introduction coating composition. Chaudhuri et al. investigated the sliding

The research results related to the friction and wear of
potential materials in cryogenic environment are of rele-
vance to space tribological applications. The literature reports
on metallic materials are available and the reports on the
use of ceramics, as bulk material or coating are limited.
Boes et al. [1] investigated the performance of different
solid lubricated ball bearings in the temperature range of
142 to +537 C with rotational speed up to 20,000 rpm.
The investigated coatings include 70Ag20PTFE10MoSe2 ,
80Ag15PTFE5MoSe2 and 70AgHg20PTFE10MoSe2 (all
compositions in vol%). At temperature of 24 C, the coefficient
of friction (COF) of investigated materials varies from 0.11 to
0.21 with the lowest measured for 70AgHg20PTFE10MoSe2 .
At 315 C, even lower COF of 0.06 is measured with the same
Corresponding author. Tel.: +91 512 2597771; fax: +91 512 2597505.
E-mail address: bikram@iitk.ac.in (B. Basu).
wear of self-mated 440C steel in the temperature range of 185
to 675 C in an oxygen atmosphere [2]. It was observed that
the mean kinetic COF is independent of load under steady state
conditions, while it decreases with increase in sliding speed and
bulk temperature.
Among the metallic materials, AISI 440C martensitic stain-
less steel is the material of choice for the high-pressure oxygen
turbo pump (HPOTP) of the space shuttle main engine (SSME).
Chaudhuri et al. [3] examined the effects of load, speed and tem-
perature (185 to 675 C) on unlubricated sliding friction and
wear (average dynamic coefficient of friction and wear rate) of
440C steels. Very high flash temperature in excess of 1000 C is
generated during the severe wear. The temperature drops to about
200 C when a steady state is reached. The decrease in tempera-
ture follows similar decrease in the COF from a sliding value of
0.60 to a steady state value of about 0.25 [4]. Although the tribo-
logical properties of metallic, ceramic and polymer-based bulk
materials and coatings are relatively well investigated at room
temperature in varying humidity conditions [5], such a study

0921-5093/$ see front matter 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2005.09.086
 B. Subramonian, B. Basu / Materials Science and Engineering A 415 (2006) 7279
Table 1
Specifications of the high-speed ball-on-disk cryo-tribometer
Parameter Minimum
Ball diameter (mm) 4 10
Disk diameter (mm) 20
Axial load (N) 0 50
Wear track diameter (mm) 10
Test speed (rpm) 850
Frictional force (N) 0 5
Test environment Normal ambient, liquid nitrogen, liquid helium
in cryogenic/sub-zero temperature is limited [14,6], primarily
because of the availability of a few tribometer to be operated
under such severe conditions.
However, the ball bearings, typically used in space shuttle
main engine or liquid rocket engines, need to survive the high
friction and wear loss during its operation at high-speed (up
to a 35,000 rpm) for a few minutes (up to 10 min). Therefore,
a tribometer, to simulate high stress high-speed sliding condi-
tions is required. Firstly, such a tribometer, once designed and
fabricated can be used to assess the potential of various bulk
materials/coatings for application in rocket engines. Secondly,
the fundamental studies to probe into the influence of change
in mechanical properties (at sub-zero temperature) on wear of
materials can be conducted for a variety of materials. Thirdly,
one can also study whether cryogenic environment can poten-
tially provide any lubrication effect for different tribomaterials.
It is with the above motivation, the present work is taken up to
design and fabricate a high-speed ball-on-disk tribometer, which
can operate in cryogenic conditions. This paper also reports the
results of a very first set of experiments conducted on SS 304 and
440C grade stainless steels, widely used currently as space shut-
tle bearing materials. Additionally, the torque testing of angular
contact ball bearings with Pb-IP coating and without any coat-
ing also has been carried out at 36,000 rpm in liquid nitrogen
immersed condition. The overall technical details of the appara-
tus, the salient features and typical test results are discussed in
this paper.
2. Description of the new cryo-tribometer
A new high-speed ball-on-disk type cryo-tribometer is basi-
cally designed to study friction and wear characteristics in slid-
ing contacts under cryogenic fluid conditions at high sliding
speeds. Also, a provision has been made for the torque test-
ing of a ball bearing under cryo-fluid immersed condition at
a maximum speed of 36,000 rpm. Cryogenic media is either
liquid nitrogen or liquid helium. Sliding occurs between a sta-
tionary ball and a high-speed rotating disk. The normal load
and rotational speed can be varied. The tangential frictional
force along with normal load and speed can be simultane-
ously monitored during the test. The coefficient of friction
data can be acquired as functions of load, speed and environ-
mental condition for continuous monitoring. Table 1 gives the
overall technical specifications of the newly developed high-
speed cryo-tribometer. Fig. 1a shows the external view of the
73
Maximum Variables
4, 6, 8 and 10 mm
40 2040 mm
1, 2, 5, 10 and 20N
30 10, 15, 20, 25 and 30 mm
36000 7 steps
Any value in 0.1N accuracy
ball-on-disk cryo-tribometer and the details of the design draw-
ing are shown in Fig. 1b. The tribometer consists of the following
major modules; a brief description of which follows subse-
quently:
a. Spindle assembly unit.
b. Specimen housing with ball-pot assembly and bearing-
mounting unit.
c. Mounting arrangement of test specimen and loading arrange-
ment.
d. Drive motor and gear box.
e. Data acquisition system and electronic controller.
2.1. Spindle assembly unit
The spindle assembly consists of flexible drive shaft, which
is secured into a Stainless steel 440C shaft, which is held by lin-
ear motion bearing (LMB) bush and enclosed in an aluminum
body. One end of flexible shaft is connected to the test disk and
the other end is connected to the drive motor. Fig. 2 shows the
flexible drive-shaft assembly for mounting to the test disk. The
ball-disk assembly of this tribometer has been designed with
the stationary ball holder assembly at the bottom of the test
disk assembly, which is rigidly connected to the flexible drive
shaft. This feature ensures the instantaneous removal of wear
debris from the wear track and aids to get a near realistic test
data. It should be further noted here that if the debris consisting
of the mating solids were allowed to remix continuously, the
wear scenario would be different from the one with instanta-
neous removal. In fact, if the wear debris will stay on between
the mating solids, then it will cause three body-wear, instead of
two body-wear. The bearing unit of the spindle is maintained at
ambient temperature using radiant heater to protect against the
conductive cooling by the cryogenic fluid. During the experi-
ments, a constant level of liquid nitrogen is maintained inside
the cryocan, in which the test disk-ball assembly was completely
immersed.
2.2. Specimen housing with ball-pot assembly and
bearing-mounting unit
The ball-pot assembly unit has a unique feature of holding the
test ball at four different radial positions on the disk specimen.
With this feature, different ranges of linear sliding speeds can
be obtained. The linear sliding speed (v) can be computed as
74 B. Subramonian, B. Basu / Materials Science and Engineering A 415 (2006) 7279

Fig. 1. Overall external look at the cryo-tribometer (a) and the detailed design description of the ball-on-disk high-speed cryo-tribometer (b).

follows: Therefore, four experiments with four varying linear sliding

 speed can be conducted with one disc surface. Such factor is
2 r rotational speed (rpm)
v(m/s) = critical when the availability of bulk material or expensive sur-
60 face coatings is limited. In our tester, wear track radii of 7.5, 10,
where r the track radius in m. 12.5 and 15 mm are provided to facilitate different sliding speeds
from 0.6 to 45 m/s. Bearing-mounting unit facilitates the rigid
fixing of the inner ring of the test bearing to the flexible drive
shaft. The torque testing of a ball bearing (maximum speed of
36,000 rpm) can be conducted by using this bearing-mounting
unit.

2.3. Mounting arrangement of test specimen and loading

arrangement

A loading pan is over-hung on a pulley with balancing dead

weight, which maintains a constant normal load conditions
throughout the test. This kind of loading arrangement ensures a
constant load irrespective of any film transfer and wear of coat-
ing/substrate material during dynamic conditions of repeated
Fig. 2. Flexible drive shaft. sliding wear-tests. A maximum normal load up to 50N can be
 B. Subramonian, B. Basu / Materials Science and Engineering A 415 (2006) 7279 75

2.4. Drive motor and gear box

The drive motor, used in the fabrication of the cryo-

Fig. 3. Normal load and frictional force load cells.
applied. The ball comes in contact with the disk as soon as the
normal load is applied. Fig. 3 shows the provision of two load
cells for the in situ sensing of the normal load and frictional load
during dynamic testing conditions. Fig. 4 shows the mounting
details of a test bearing, whereas Fig. 5 shows that of a test disk
in this tribometer
tribometer, can operate at high speeds up to 36,000 rpm without
any vibration and sound. With built-in gearbox unit, the speed
of the test spindle can be changed in 14 speed-steps in the
range from 850 to 36,000 rpm. Due to the unique feature of
flexible shaft system of the drive spindle, the main motor
cum gear unit can be easily isolated from the tribometer.
This facilitates a smooth operation of the tester with high
sensitivity of frictional force measurement and related data
acquisition.
2.5. Data acquisition system and electronic controller
The data acquisition system is computerized and the frictional
force is measured based on the high-speed torque measurement
using piezoelectric force transducer having high enough band-
width and the data is continuously acquired using commercial
software, LABVIEW.

Fig. 4. Mounting of test-bearing.

Fig. 5. Disk and disk holder.

76 B. Subramonian, B. Basu / Materials Science and Engineering A 415 (2006) 7279
Fig. 6. COF vs. time of self-mated 304 stainless steel with sliding speed of
22.4 m/s.
3. Preliminary experimental results of the high-speed
cryo-tribometer
To assess the performance of this new apparatus, some
preliminary cryogenic wear tests have been carried out with
smoothly polished SS 304 stainless steel and 440C grade marten-
sitic stainless steel flat samples against ball (10 mm diameter)
of the respective material. The tests have been carried out at
a spindle speed of 17,100 rpm for self-mated SS 304 stainless
steel and at 850 rpm for self-mated 440C martensitic stainless
steel. Dead weight has been used to load the ball against the
disc. All the test samples are smoothly polished to have same
surface roughness (Ra ) and also ultrasonically cleaned in ace-
tone to remove any surface film. With the special feature of this
cryo-tribometer, the high-speed torque testing of ball bearings
under liquid nitrogen immersed condition has also been carried
out successfully.
The experiments to measure the COF of self-mated SS 304
stainless steel and self-mated 440C martensitic stainless steel
samples were carried out in liquid nitrogen atmosphere with dif-
ferent testing parameters and the frictional behavior is studied.
From Figs. 68, it can be inferred that at very high sliding speeds
(13.4, 17.9 and 22.4 m/s), keeping all the other parameters iden-
tical, the COF of self-mated 304 stainless steel was found to be
0.1 at sliding speed of 22.4 m/s and is 0.2 at sliding speeds
of 17.9 and 13.4 m/s. Referring to Fig. 9, for self-mated 440C
Fig. 7. COF vs. time of self-mated 304 stainless steel with sliding speed of
17.94 m/s.
Fig. 8. COF vs. time of self-mated 304 stainless steel with sliding speed of
13.4 m/s.
martensitic stainless steel, COF increases from very low value
to around 0.15 in the run-in-period (first 10 s) and subsequently
the steady state COF of 0.15 is maintained for first 5 min of the
test run. A slight increase in COF from 0.15 to 0.27 is noted
during the last 5 min of test run. It may be noted that COF of
0.50.6 is commonly reported in literature for self-mated steel
at room temperature and normal humidity (3540% RH) [5].
From above observation, it is clear that the cryogenic environ-
ment has a significant influence on reduction (50%) in COF
of self-mated SS 304 steel.
The testing of typical angular contact ball bearings of rocket
engine cryo-turbo pump in liquid nitrogen immersed condition
at 36,000 rpm has been carried out for understanding the effect
of solid lubricant coating on the races of the bearing. The ball
bearings are having bore diameter of 10 mm, outer diameter of
26 mm and with cages made out of glass fiber reinforced PTFE
composite material, which is generally used in cryogenic con-
ditions. Figs. 10 and 11 plot the COF versus sliding time for the
bearings without any coating and with ion-plated Pb coating (the
inner and outer races of the bearing was pre-lubricated coating
of 0.70 m thickness of Pb by ion-plating deposition), respec-
tively. In both the cases, the initial value of COF is relatively
high due to the combined effect of start transient and run-in of
the cage material. With regard to the bearing without any coat-
ing, the initial value of rolling = 0.037, whereas it reaches the
steady state value of rolling = 0.009 from 120 s onwards up to
800 s. In the case of bearing with Pb-IP coating the initial value
Fig. 9. COF vs. time of self-mated SUS440C steel with sliding speed of 0.89 m/s.
 B. Subramonian, B. Basu / Materials Science and Engineering A 415 (2006) 7279 77

Fig. 10. Rolling COF vs. time of ball bearing without any coating at 36,000 rpm.

Fig. 11. Rolling COF vs. time of ball bearing with Pb-IP coating at 36,000 rpm.

of rolling = 0.017, whereas it reaches the steady state value of the counterbody (Fig. 12). Similar worn surface cracking is also
rolling = 0.008 from 150 s onwards up to 800 s. observed on disks tested with sliding speed of 17.4 m/s. The
localized delamination of third body/transfer layer on worn self-
4. Discussion on wear of materials in liquid nitrogen mated 304 stainless steel disk is also noted (Fig. 13). The wear

From the above results it is observed that, the friction coeffi-

cient and wear rate data of the self-mated SUS304 and SUS440C
steel in liquid nitrogen are having a slight decreasing trend with
increase in sliding speed. Whereas the respective wear rate of
the counter body (ball) is predominant. The following are the
visual observations of the worn surfaces and related discussion
for understanding the wear mechanism. The characterization of
wear surfaces is performed using optical microscope.
The topographical observation of the worn surface of self-
mated SS 304 stainless steel and self-mated 440C martensitic
stainless steel samples were studied using optical microscope.
The wear track on self-mated 304 stainless steel disk was exam-
ined at sliding speed of 13.4 m/s and it was found that the material
suffers abrasive wear with plastic deformation. The width of
this wear track is 0.9 mm. The cracking of the worn surface is Fig. 12. Optical micrograph showing the topographical features of the wear track
clearly visible with oxidized steel wear debris transferred from on 304 steel disk worn against 304 steel ball with sliding speed of 13.4 m/s.
78 B. Subramonian, B. Basu / Materials Science and Engineering A 415 (2006) 7279

Fig. 13. Optical micrograph showing the topographical features of the wear track
on 304 steel disk worn against 304 steel ball with sliding speed of 17.9 m/s.
Fig. 14. Optical micrograph showing the topographical features of the wear track
on 304 steel disk worn against 304 steel ball with sliding speed of 22.4 m/s.
track on self-mated SS 304 stainless steel disk, tested with a
sliding speed of 22.4 m/s was found to have undergone severe
plastic deformation The width of wear track was found to be
2.11 mm. Due to the severe plastic deformation, a highly uneven
worn surface was observed on this wear track (Fig. 14). Micro-
structural study using optical microscope revealed the presence
of localized crack concentration. It is observed that the cracks
originate from the central region of the wear track and propagate
perpendicular to the sliding direction. The occurrence of severe
cracking induced tribomechanical wear of disk may be due to
Fig. 15. Optical micrograph showing topographical features of the wear track on
stainless steel 440C disk worn against 440C ball with sliding speed of 0.89 m/s.
high sliding speed (22.4 m/s). The wear of self-mated 440C
martensitic stainless steel, tested at sliding speed of 0.89 m/s
was carried out and the width of wear track was reported to be
1.1 mm. No observable cracking or the sign of severe wear is
noted on the wear track (Fig. 15).
The sliding test conditions as well as tribological data of a
very first set of experiments conducted on SS 304 steel and
440C grade steel are presented in Table 2. The wear of the ball
is calculated by measuring the mass loss using a high precision
electronic balance having an accuracy of five digits. The mass
loss is further converted to wear volume, based on the mass loss
and density data. The wear loss is presented as wear rate, which
is the wear volume normalized with respect to normal load and
total sliding distance.
Looking at the wear rate data for self-mated SS 304 steel,
it can be noticed that under the condition of same peak Hertz
stress (0.6 GPa), the wear rate of SS 304 steel ball increases
with increase in sliding speed, when all tests were conducted
at identical load (2N). With higher sliding speed, the contact-
ing asperities experience more repeated abrasion. For metallic
materials, like steels, the abrasive wear is dominated by plastic
deformation. However, at cryogenic temperature, the contribu-
tion of deformation would be much lower as dislocation acti-
vated slip processes would be limited at sub-zero temperature.
Therefore, during high-speed abrasion, the fracture process, as
evident from the presence of cracks running at perpendicular
to sliding direction (see Figs. 1214) contributes largely to the
high wear loss of material. Another observation is the presence
of adhered iron oxide transfer layer on the abrasive grooves
formed on steel disc. This indicates oxidative wear, involving

Table 2
Test data of experiments with high-speed ball-on-disk cryo-tribometer in liquid nitrogen
Tribosystem Hertz stress Sliding speed Sliding length Coefficient of Wear rate of ball in
(GPa) (peak) (m/s) (m) (for ball) friction () mm3 /Nm 104

Self-mated SS 304 steel 0.6 22.4 6160 0.10.12 4.4

Self-mated SS 304 steel 0.6 17.9 5370 0.190.20 1.8
Self-mated SS 304 steel 0.6 13.4 3819 0.190.21 1.25
Self-mated 440 steel 1.0 0.89 498 0.150.28 0.2

The sliding tests on self-mated SS 304 were carried out at 2N load, while that on self-mated 440C steel at 7N load.
 B. Subramonian, B. Basu / Materials Science and Engineering A 415 (2006) 7279
the formation of iron oxide during sliding also took place. How-
ever, for self-mated SS 440C steel, the occurrence of fracture is
not noted and also the wear rate of SS 440C balls is less com-
pared to that of SS 304 ball. This should be attributed to the
higher hardness of SS 440C (Rc = 58).
Figs. 10 and 11, presenting the COF data for the bearing tests
at 36,000 rpm under liquid nitrogen immersed condition show
that compared to the bearing without any coating, the bearing
with solid lubricant coatings like Pb-IP ensures >50% reduction
of rolling COF (0.0370.017) during the start transient and 10%
reduction of rolling COF (0.0090.008) during the steady state
operation.
5. Conclusions
The major conclusions of the present work are as follows:
(a) With this newly developed high-speed ball-on-disk cryo-
tribometer, the challenging characterization of friction and
wear behavior of different materials and coatings in cryo-
genic fluid immersed environment (LN2/LHe) at higher
sliding speed conditions is now possible under more real-
istic conditions. It could be well realized from description
of the machine that unique feature of the new tribometer
is its capability to work at very high rotational speeds (up
to 36,000 rpm) and the special motor drive arrangement for
achieving such high speeds. It can be noted here that much
lower speed up to 1500 rpm is commonly used in the pin-on-
disk tribometer around the world. With the special additional
feature for testing ball bearing, the tribo-characterization of
ball bearings under cryogenic fluid immersed conditions and
at high sliding speeds with different kinds of solid lubricated
coatings and with different cage design has now become
very simple and cost-effective.
(b) In regard to the ball-on-disk test data of self-mated SS 304
steel, the obtained frictional behavior clearly reflects that the
high sliding speeds and cryogenic conditions have a strong
influence on the steady state value of . For self-mated SS
304 steel in liquid nitrogen immersed condition at very high
sliding speed of 22.4 m/s, = 0.1, whereas at sliding speed
of 13.4 m/s, = 0.190.21. This shows that the friction coef-
ficient () gradually decreases with higher sliding speeds in
cryogenic conditions.
(c) On the basis of the preliminary experimental results, it can
be stated that the ball wear rate is gradually increasing with
increase in sliding speeds in the range of 13.422.4 m/s.
A very high wear rate of ball of 4.4 104 mm3 /Nm was
observed at sliding speed of 22.4 m/s in liquid nitrogen
79
immersed condition. This is expected as high sliding speed
causes repeated abrasion and fracture of the asperitites lead-
ing to severe wear of SS 304 steel.
(d) The topographical investigation of the worn surface and
the wear rate of ball indicate the evidence of severe plas-
tic deformation and material transfer from counterbody and
extensive cracking for 304 stainless steel, tested under high
sliding speeds of 13.422.4 m/s. For 440C stainless steel,
the worn surface does not reveal severe wear. The wear rate
of ball was found to be 2.0 105 mm3 /Nm. This can be
attributed to the higher material hardness (58 HRc) and
lower sliding speed (0.89 m/s) conditions.
(e) In the case of high-speed testing of angular contact ball bear-
ings under liquid nitrogen conditions, it is well understood
that bearings with solid lubricant coatings like Pb-IP are hav-
ing more endurance life and high reliability in comparison
with bearings without any coating.
Acknowledgements
The financial assistance of IITK-ISRO project in fabricating
the experimental set-up is gratefully acknowledged. The authors
would like to thank Department of Space for their kind spon-
sorship, Prof. Koji Kato of Tohoku University, Japan, Late Prof.
V.S.R Murthy of Materials and Metallurgical department of IIT
Kanpur, India for their constant encouragement. Authors also
would like to thank Mr. Rajneesh Verma of IIT Kanpur and Mr.
V.P. Joseph of Department of space for their sincere technical
support for the experiments.
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