This article was downloaded by: [Moskow State Univ Bibliote]

On: 30 May 2013, At: 10:08

Publisher: Taylor & Francis
Informa Ltd Registered in England and Wales Registered Number: 1072954 Registered office: Mortimer
House, 37-41 Mortimer Street, London W1T 3JH, UK

A S L E Transactions
Publication details, including instructions for authors and subscription information:
http://www.tandfonline.com/loi/utrb19

Friction, Wear, and Evaporation Rates of Various

-7

Materials in Vacuum to 10 mm Hg
a

Donald H. Buckley , Max Swikert & Robert L. Johnson

a

NASALewis Research Center, Cleveland 35, Ohio

Lubrication Section, NASALewis Research Center, Cleveland 35, Ohio

Published online: 25 Mar 2008.

To cite this article: Donald H. Buckley , Max Swikert & Robert L. Johnson (1962): Friction, Wear, and Evaporation
-7

Rates of Various Materials in Vacuum to 10 mm Hg, A S L E Transactions, 5:1, 8-23

To link to this article: http://dx.doi.org/10.1080/05698196208972448

PLEASE SCROLL DOWN FOR ARTICLE

Full terms and conditions of use: http://www.tandfonline.com/page/terms-and-conditions
This article may be used for research, teaching, and private study purposes. Any substantial or
systematic reproduction, redistribution, reselling, loan, sub-licensing, systematic supply, or distribution
in any form to anyone is expressly forbidden.
The publisher does not give any warranty express or implied or make any representation that the
contents will be complete or accurate or up to date. The accuracy of any instructions, formulae, and
drug doses should be independently verified with primary sources. The publisher shall not be liable for
any loss, actions, claims, proceedings, demand, or costs or damages whatsoever or howsoever caused
arising directly or indirectly in connection with or arising out of the use of this material.

ASLE TRAN SACTI ON S

5, 8-23 (1 962)

Friction, Wear, and Evaporation Rates of Various

7
Materials in Vacuum to 10- mm Hg
By DONALD H . BUCKLEY,t MAX SWIKERT,2 and ROBERT L. JOHNSON3

Downloaded by [Moskow State Univ Bibliote] at 10:08 30 May 2013

Evaporat ion data on soft m etals, lubricatin g inor ganic com pounds, and varia li S reference ma terials
are repor ted for te m peratu res from 75 to 1000 Fin vacuum as low as 10 - 7 111m H g, Observa tion s
on 11I0d es of vacuu m degradation (e .g., eva poration or dissociation ) and m ethods of ex periment ation are relat ed . Fricti on and we ar data are present ed for several unl ubr icated m etal s (e .g., typ e
440-C steel ) and m etal s coated with inorganic (e .g., MoS 2 , CaF 2 ) as well as with soft m etal
film s in va cullm at ambient pressures between 10- 6 and 10- 7 111m H g,

in the vacuum systems. One of the problems associated

With such systems is that of back-mi gration of oil vapors
from the pump to the test chamber. This back -migration
even with cold traps and baffles can serve as a source
of specimen contamination and result in a pronounced
reduction in friction and wear.
There is a need for data on the evaporation rates of
lubricants and also on the friction and wear characteristics of potential bearing and seal materials; these data
must be obtained in a vacuum environment to facilitate
the proper selection of lubricants and slider materials
intended for use in space. The friction and wear data
should be obtained in systems which are free from
sourc es of specimen contamination like that associated
with the oil diffusion pumps.
The objectives of this investigation were to determine
in vacuum ( 10- 6 to 10- 7 mm H g) : (a) the evaporation
rates for various organic and inorganic lubricants, (b)
the evaporation rates of solid lubricant coatings, (c) the
friction and wear properties of unlubricated slider mao
terials for reference , and (d) the friction and wear properties of these slider materials coated with solid lubricant
films. Evaporation-rate experiments were used to select
the most promisin g solid lubricants for use as surface
films on slider materials in vacuum. Evaporation rates
were measured at temperatures from 55 to 1000 F . Friction and wear experiments were conducted with a 3/16in. radius rider slidin g on a 20 in. diameter disk specimen at a sur face speed of 390 ft / min. The rider was
loaded against the disk with a 1000 g load. The duration of the experiments was 1 hr .

Introduction

THE requirements for bearings and seals to operate in

the environment of space dictate a new area for lubrication research. The low ambient pressures encountered
in space can be expected to influence the behavior of oil,
grease , and solid-film lubricants. The property of these
materials most significantly affected by low ambient
pressures is the evaporation rate. Various investigators
have therefore measured the evaporation rates of oils
and greases in vacuum as one method of establishing
their relative merit for space applic ations (1-3). The
results of this work have given some indication as to
the oils and greases with the greatest stability at reduced ambient pressures. Only limited experimental
work, however , has been reported in the literature for
inorganic solids and soft metals which have potential
use as solid lubricant films or coatings for hard alloy
substrates [e.g. Reference (4)] . In general, the evaporation rates of these materials would be lower than those
of oils and greases. These films might therefore be very
attractive as lubricants for high vacuum service.
The lack of oxygen in outer space creates another
problem for lubrication systems , namely, the absence
of the protective metal surface oxides normally encountered in air. In the absence of these or other protective
surface films, mass metal transfer, welding, and high
coefficients of friction may be experienced for metals in
sliding contact (5-7) . Some data are presented in the
literature for the fricti on and wear of metals and soft
alloys in vacuum [e.g. Reference (8)] . In general , th ese
data were obtained with conventional oil diffusion pumps

Materials
Presented as an American Society of Lubrication Engineers
paper at th e Lubrication Conference held in Chicago, Illin ois,
October 1961.
1 Aeronautical
Research En gineer, NASA- Lewis Resear ch
Center, Cleveland 35, Ohio.
2 Aeronautical
Resear ch En gineer, NASA-Lewis Research
Center, Cleveland 35, Ohio.
3 Head, Lu brication Section , NASA-Lewis Research Center,
Cleveland 35, Ohio.

The specimens used in the evaporation experiments

of this investigation were oils, greases, inorganic solids.
metal s, and solid lubricant coatings. The oils included
MIL-L-7808 (di-2-ethyl hexyl sebacate), two mineral
oils (viscosities of 380 and 235 centistokes at 100 F )
designed for high-temperature use, and a polyphenyl
ether r1-(p-a -cumyl phenoxy) -4-phenoxy benzene 1. The
ether was a solid at room temperature. The greases
8

Friction of M a terials in Vac uum

T ABLE 1
Alloy C om position s
Co m po sit io n
Metal

Downloaded by [Moskow State Univ Bibliote] at 10:08 30 May 2013

52100

Fe

:'\i

Co

Cr

1.3

Hal.
of
co rnp,

to
1.6

0.95
to
1.10

440-C

Bal.
oi
cornp .

16.0
to
18.0

0.95
to
1.20

Ni-Cr

0.250

18.0
to
20.0

0.06
to
.12

Ni-Cr-Fe

5.0
to
9.0

70.0

15.0

0.08

Cobalt alloy

3.0

2.5

.\ 1.0

2.4

Ni-bonded T iC
and CbC"

Bal.
oi
co rnp .

11.0
to
12.0

43.0

25.0

13.2

Mo

Ti

0.75

9.0
to
10.5

3.2

Si

l\In

0.20
to
.35

0.25
to
.45

P , 0 .Q2 5
S. 0.025

1.0
M ax .

1.0

P. S

0.010

0.050

0.50

17.0
5.0

Ocher

52.0

Va cuu m appa ra t us for bulk eva pora tion studies

Hardn ess,
R ockwell
R~

60-43

R " 54

R c 43

1.50

S,C b
AI,Mn

R ~ 29

R~

1.0

a Ti and Cb a re p resent as mi xed carbide s.

F IG. I (a ) .

AI

Cb , 4 .5 ;
T a , 0.3

52-63

R .\ 89

Downloaded by [Moskow State Univ Bibliote] at 10:08 30 May 2013

10

DONALD

H.

BUCKLEY, ]\ I AX SWIKERT, AND ROBERT

included were a radiation-resistant grease and two

mineral-oil-base greases with phthalocyanine thickeners .
The inorganics included chemically pure materials obtained from commercial supply houses: cadmium iodide
(CdI 2 ) , cobalt chloride (C oCI2 ) , nickel fluoride (N iF 2) ,
lead oxide (PbO ) , calcium fluoride (Ca F 2 ) , barium
fluoride (BaF 2 ) , tungsten disulfide (WSJ , and molybdenum disulfide (MoS 2 ) . The nickel bromide (NiBr2)
could not be readily obtained commercially and was
therefore prepared in the laboratory. The metals included
were cadmium (Cd) , indium (In) , zinc (Zn) , magnesium
(Mg) , tin (Sn), gallium (Ga) , lead (Pb), and silver
(Ag). Two organics other than the oils and greases for
which evaporation rates were measured were poly tetrafluoroethylene (PTFE) and epoxy (diglycidyl ether of
bisphenol A with a diethylene triamine catalyst).
The alloys used in the friction and wear experiment
with their compositions are presented in Table 1.

L.

JOHNSON

The molybdenum disulfide coatings used were coatings

of the following types: silicon resin bonded, epoxyphenolic resin bonded, ceramic bonded, and a metal
matrix coating. The coatings were applied to 0.003 in.
thick metal tabs for evaporation experiments. The
thickness of the applied coating was 0.001 in. In the
friction and wear experiments, however , the coating
thickness on the disk specimens was 0.0002 to 0.0003 in.
Apparatus
The apparatus used in this investigation is presented
in Figs. 1(a) to 1(c). The evaporation apparatus consisted of a commercial bell-jar vacuum system with a
4 in. oil diffusion pump system. Pressures in the 18 in.
diameter chamber were measured with thermocouple
and hot cathode ionization gages . Inside the bell-jar
chamber just above the throat of the diffusion pump,

ELECTRONIC BALANCE

LIQUID-NITROGEN
COOLING COILS

CONDENSING
PLATE

FURNACE

FIG.

l(b) . Vacuum evaporation apparatus with balance for continuous rate measurements

11

Downloaded by [Moskow State Univ Bibliote] at 10:08 30 May 2013

Friction of Materials in Vacuum

a large pla te was used to s up p ort a heater and th e
test specimen. The heat er co ns isted o f a hou sing of
machinable cera mic a nd a wire-wound tungst en heating
element. T he spe cime n was p lac ed on th e heati ng element. A th ermocoupl e was p ositi on ed on the top edge
of the specimen for t em p er a t ur e measurem ent a nd co ntrol.
Approximatel y 4 in. a bove th e sp ecime n wa s a co ndensing shield . This shield was cooled with a liqui dnitrogen coil. a nd th e t emperature measured at th e ce nter
of the conden sin g shield wh en liquid passed throu gh th e
coil was - 20-l F . O n th e side o f th e shield fac ing th e
specimen \ \'a 5 a copper ta b for making X -ray analyses
of condensa te composition .
The bell-jar eva pora t ion apparatus was modifi ed for
use with a continuous recordin g balance. The apparat us
with associat ed modi ficati on s is present ed in Fi g. 1( b ) .
The \Hjghin!! mech ani sm o f a co m me rc ia lly availabl e
electronic ba lan ce wa s mount ed on a support in th e
upper par! of th e bell ja r. Suspe nded from th e bala nce
beam \\"a ~ a thin wir e th at exte nde d fr om th e ba la nce
beam through th e co nde ns ing shield to a s t ir rup that
suppo rted t he spe cimen . The spe cimen a nd st irr up wer e
suspended in th e mouth of a cylind rica l furnace . The
walls of till" fu rn a ce conta ine d th e heating elements of
wound tunuste n wire. A d ummy spec imen with ther mo couple placed beneat h th e t est specime n was used to

measure a nd co nt ro l spec ime n temper atures . The d um my

speci me n techni qu e ha s bee n employe d by o thers in
simila r experime n ts (9) . W eight cha nges in th e specimen
wer e co nt in uo usly recor ded on a s trip cha rt.
The vac uum frict ion a nd wea r ap paratus is shown
schema t ica lly in F ig . 1( c) . The ba sic elem en ts of t he
appa ra tus wer e a 2.0 in. dia meter d isk a nd a 3/ 16 in .
radi us rid er specimen. The disk wa s ro ta te d by means
of a n indu cti on mot or with a ca n ned ro tor a nd sta tor .
The enclosur e of ro to r a nd sta to r pe rm itted a va cuum
in th e mot or cha mb er. A va cuum valve co n necte d th e
mot or cha mbe r with a mech ani cal p ump sys tem . The
syst em included a liquid-nit rogen co ld trap to inhibit oil
migrat ion from th e pum p . The specim en cha m be r containin g th e disk and rider wa s a ttache d to th e mot or.
The motor drive shaft ex t ende d into th e specimen
cha mber with th e d isk specimen bolt ed direct ly to th e
end . Th e only sea l between cha mbers was that a fforded
by a ball bearing mount ed on th e drive sha ft. Since
th e presen ce of th e ba ll bea rin g did not provide a va cuum
sea l, th e ionization p ump pumpe d bot h cha mbers . When
th e pr essure in th e specimen cha mbe r was 10 - ; mm H g,
it was approx ima te ly 10 - 1 m m H g in t he mot o r cha mber.
The rider specimen was s uppo rted in th e spe cim en
cha mb er by a reta ining a rm that was gimba l a nd be llo ws
mount ed to th e cha mber. A lin ka ge a t th e end of th e

/ MOTOR
TO PUMP
~

LOAD
BAKEOUT HEATERS

MOTOR CHAMBER
:4

10 . mm Hg

SPECIMEN CHAMBER
I0

1' 1(; ,

1( c) ,

-7

Va cuu m i rict io n a nd wea r a p pa ra t us

mm Hg

Downloaded by [Moskow State Univ Bibliote] at 10:08 30 May 2013

12

D ONALD

H.

B U CKLEY, MAX SWIKERT, AND R OBERT

retairung arm away from the rider specimen was connected to a strain-gage assembly . The assembly was
used to measure frictional force . Load was appli ed
through a dead-weight loading system.
Attached to the lower end of the specimen chamber
was a vacuum valve. The side of th e valve away from
the chamber had aT-section. On the lower portion of
the T was connected a 400 liters/ second ionization pump.
The remaining portion of the T connected with a vacuum
valv e and a mechanical pump usin g liquid-nitrogen cold
tr ap s.
The first high-vacuum pump to be used with the
vacuum friction and wear app aratus was a conventional
oil diffusion pump. In initial experiments it was est ablished , however , that specimen contamination by oil
vapors had occurred (see Appendix A). Various liquidnitrogen cold-trap designs were employed to elimin ate
this problem. Subsequ ent specimen examinations, however , indicated surface contamination . Combinations of
cold traps, optical baffies, and heating grids for decomposition of oil vapors were then tried with little or no
suc cess. Since, even with the best trapping techniques,
the possibility of specimen contamination did exist , th e
diffu sion pump was replaced by an ionization pump. Thi s
pump employs no fluids or vapors in its opera tion.
Experimental procedure

The pro cedure used in th e evapora tion st udies consist ed of first preparing the experimental specimens. This
was accomplished for the solids by oven-drying and dehy drating the materials. When the powders were dry,
small charges were placed in a mold and compressed
into tablet form und er a 10,000 psi compression force .
When the specimens were removed, they measured % in .
in diameter and were approximately ;Is in. thick . The
tablets were then placed into a small preweighed glazed
ceramic dish that had side walls of ;Is in . and inside
diameter just lar ge enough to accommodate the tablet
sp ecimen . The specimens and hold ers were then stored
in a desiccator until ready for use. The oils and grea ses
were placed directly in the dishes with the specimen filling the dish .
Prior to an experiment the specimens were removed
from the desiccator and weighed . The specimen and
holder were then placed into the vacuum chamber, and
the chamber was evacuated. At a pressure between 10- 6
and 10- 7 mm H g the experiment was started. In those
experiments conducted above room temperature, the
specimens were heated by a tungsten heater on which
the specimen was placed.
The evaporation-rate experiments made with solid
lubricant coatings were run using the electronic balance
with a continuous measure of weight change with time.
During an experiment a tab was placed on the stirrup
that was suspended from the balance at the top end of
the furnace , and the chamber was then evacuated. At
a pressure between 10- 6 and 10- 7 mm Hg the evaporation experiments were started.

L.

J OH NSO N

The disk and rider specimens used in friction and wear

experiment s were finish-ground at 4 to 8 f! in. Before
each experiment the disk and rider were given the
same preparatory treatment. This treatment consisted
of (a ) a thorou gh rinsin g with acetone to remove oil
and grease, (b ) polishing with moist levigated alumina
on a soft cloth , and (c) a thorough rin sing with tap
wat er followed by distilled wat er. For each experimen t
(da ta point) a new set of specimens was used . In tho se
experiments in which disks with coatings were used , the
coatings were applied after the cleaning procedure
Plated specimens were solvent-cleaned, and bonded coatings were carefully handled following coating in order
to avoid contamination.
The specimens were then placed in the apparatus.
Mechanical pumps with liquid-nitrogen cold traps were
used to obtain a pre ssure of 10- 4 mm Hg in the specimen chamber. In the startup of the ionization pump .
ionization of chamber gases was produced by the pump .
This ionization generally persi sted for 20 to 30 min.
In the event that oil molecules had migrated through
the liquid-nitrogen cold traps of th e mechanical pumps
prior to bein g valved off from the specimen chamber.
the ionization would decompose them.
When the specimen chamber pre ssure was between
5.0 X 10- 7 and 2.0 X 10- 6 mm Hg as measured by
a hot cathode ionization gage and by the ionization
pump current , the friction experiment was sta rted . A
1000 g load was applied to the rid er loading it again st
the disk. Friction force was continuously measur ed and
recorded on a strip chart. The wear was measured as
volume loss of the rider specimen upon completion of
1 hr of running. The wear to the disk specimen sur face
was recorded with a surface profile measuring device .
Results and discussion
EVAPO RATIO N DATA

The evaporation rates for some low-vapor-pressure oils

and greases were determined in vacuum at various tem peratures. The results obtained in these evaporation
experiments are presented in Fig. 2. The sebaca te MILL-7808 bubbled cont inuously while evaporating. The
high-temperature mineral oils (viscosities of 380 and
235 centi stokes at 100 F) did not exhibit this characteristic , and the surfaces were rather quie scent during
evaporation at 55 and 200 F. The ether (l-a-cumyl
phenoxy-4-phenoxy-benzene was a solid at 55 F and exhibited no detectable weight change in 60.0 hr. At 200 F
the ether was in a liquid state, and the evaporation rate
was quite high (2 .5 X 10- 6 g/ cm-/sec ).
The greases appeared to lose the base oil with increase in temperature, leavin g the bulk of the thickener
behind. The evaporation experiments were terminated
before complete evaporation of the base oil had occurred. This was found desirable in order to avoid a
change in evaporation rates once the base stock had
completely evaporated and the thickener with its own
characteristic rate began to evaporate. The radia tion -

13

Friction of M ater ials in Vacuum

A -

EVAPORATION RATE LESS THAN I.OX IO- IO

9/CM

2/SEC

GREASES

r......
:::] 55

~ 200 0 F

en

[-:,:-:-:,:1
...... 350 0 F

<,
N

<,
c>

0:::

RADIATIONRESISTANT
GREASE

#159

W
I-

<t

A
MINERAL -OIL
BASE WITH
PHTHALOCYANINE
THICKENER 0

10- 5

0:::

Downloaded by [Moskow State Univ Bibliote] at 10:08 30 May 2013

a,

\"0-"

<t

>

380CENTISTOKE
VISCOSITY
OILS

Evaporati on rat es for va rious oils a nd greases in vacuum. Ambient pr essur e,

8.0 X 10- 7 to 2.0 X 10- 6 mm H g.
FI G. 2.

resistant greas e exhibi ted a very low rate of evaporation

at 55 F. At 200 F , however, t he rate increased a nd the
specimen became rubbery. T he greas es using phthalocyanine as a thicke ner both showed evidence of the
thickener evap ora ting wit h th e base stock, as determined
by examination of the condensate on the liq uid-nit rogen
condensing shield. T he evaporation rates of th e greases
were tolerable at 200 F; however , a t 350 F t he ra te was
quite high. T he tot al per cen t of th e oil a nd grease
samples lost depended upon the evapora tio n rates of
the various ma te ria ls. For exa mp le a t 200 F only 3 pe r
cent of the greas e with H t hickener was lost in 20 hr
while 86 per cent o f the ~ II L-L-7 808 had evaporated
in 14.0 hr. T he oil a nd greas e evapora tion exp er imen ts
were genera lly of 20 h r d uration. In those cases where
the evaporation ra tes were very high (l\H L-L -7808) th e
experiments were te rminated in sho rter pe riod s. D uplicate experi ments indi cated a reproducib ility of data within 5 per cent.
The evaporation ra tes for compressed disks of various
lubricant coati ng con stit uents were determ ined , a nd the
results obtained in vac uum at va rious temperatur es are
presented in F ig. 3. T he nick el fluoride showed no evidence of evapora tio n a t 55 or 200 F. At 350 F , however ,
the nickel fluo ride dissociated to met all ic nick el and
fluorine. T he specimen surface changed from ye llowgreen to a black color. X-ray analysis of th e sur face
indicated th e bla ck film to be met alli c nickel. T he lea d
oxide also dissocia ted at 350 F to metalli c lea d and
oxygen. X-ray analys is indica ted the presenc e of lead

on th e specimen surface. T he cobal t chloride sample

exhibited a color chan ge from blu e to gree n at 500 F;
however, th e evapora tion rate was low. X -r ay ana lys is
of th e sample indi cated its composition to be cobalt
ch loride (CoCIJ . The cobalt chlor ide , cadmium iodide,
a nd nickel brom ide evaporated and condensed on th e
conde nsi ng shield as cobalt chl oride, cadmium iodide,
a nd nickel bromide, respecti vely. The epoxy compositi on (digly cidy l ether of bisphenol A with a catalyst of
diethy lene tr iam ine) showe d evide nce of deco mposit ion
a t 350 F .

A - EV APOR AT~N RAT E LESS THAN

I.OXI0-10 g/ CM2 / SEC

Cfl

<,

"'L 10'7
U
<,

o-

w I 0. 9 L -_

- - 'I..U..;.,:.J.="-"-_ _""""'-'=-L:C:""-_ _

Q:

10. 5

I-

Q:

~
>

~A--'"

liJ
%=

"'---

CADMIUM IODIDE

I-

55 0 F

20 0

G:7:1 35 0 0 F
Cd
F

500

10. 7

10 . 9

NICKEL FL UORIDE

8.5 XI0 - 5

COBALT
CHLORIDE

r ,""
JIlL

NICKEL BROMIDE

FIG. 3. Evaporation rat es for possible coat ing constituents in

vacuum. Ambi ent p ressure, 8.0 X 10- 7 to 2.0 X 10- 6 mm H g,

Downloaded by [Moskow State Univ Bibliote] at 10:08 30 May 2013

14

DONALD

H.

BUCKLEY, MAX SWIKERT, AND ROBERT

The evaporation rates for molybdenum disulfide , tun gsten disulfide , calcium fluoride , and barium fluoride at
temperatures to 1000 F are presented in Fig. 4. The
weight losses for these materials in vacuum at elevated
temperatures were very low, and in general these materials appeared to be the most stable of the inorganics
tested. The rates for molybdenum disulfide , calcium
fluoride , and barium fluoride were extremely close, and
a single curve was drawn to represent the evaporation
rate of these three materials. The molybdenum and
tun gsten disulfide had to be heated in vacuum prior to
an experiment to remove adsorbed gases.
The evaporation rates for polytetrafluorethylene (pure
polymer without plasticizer ) were determined at various
ambient temperatur es and pressures . The results obtained in these experi ments are prese nted in Fig . 5.
While the polytetrafluorethylene exhibited some weight
change at various ambient press ures , this weight change
was extremely small . The evaporation rate of poly tetrafluorethylene at various temperatures was determined at
a n ambient pressure of 8.0 X 10- 7 to 2.0 X 10- 6 mm
Hg. The evaporation rate of polytetrafluoroethylene was
low to 350 F ; at 650 F the rate was high . Poly tetrafluorethylene begins to decompo se at temperatures above

JOH NSON

500 F ; this may well account for the high evaporation

obtained at 650 F .
The evaporation rate s for various metals were determined in vacuum over a ran ge of temperatures, and
the results obtained in these experiments are presented
in Figs. 6 and 7. Cadmium and zinc exhibited relatively
high rates of evaporation. The rates were higher tha n
obtained with polytetrafluorethylene. Lead, tin , and
silver had the lowest rates of evapo ration of the soft
metals investigated.
When the evaporation rates determined experimentally in this investigation are compa red with data calculated
from vapor press ure pre sented in the literat ur e (10), the
results appear to be in good agreement (Fig. 6) . Any
differences observed could be due not only to experimental erro r but to error in the calculated val ues. The
calculated values are based on thermodynamic relation s
where an error of 10 per cent is not unlikely . Since the
evaporation rate can be determined from vapor pressure,
the reverse must also be possib le. The use of evaporation
- - -- CALCULA TED FROM
VAPOR PRESSURE
DATA (POINTS ARE
EXPERIMENTAL DATAl
A -

Do TUNGSTEN DISUL FIDE

o MOLYBDENUM DISULF IDE
o CAL CIUM FL UORIDE
o BARIUM FLU ORIDE
A -

L.

EVAPORATlON RAT E
LE SS THAN

LOX IO'

IO

9/CM /SEC

EVAPORATION RATE LE SS
2/S
EC

THAN LOXIO- IO 9 /CM

ti

10. 8

0..

>

lLJ

500
650
TEMP, OF

FIG. 4. Evaporation ra tes for variou s inor ganic compounds in

vacuum. Ambient pressure , 8.0 X 10- 7 to 2.0 X 10- 6 mm H g ,

UJ
U)

<,

'"u

:;:~
10.,2

'"

A -

EVAPORATION RA TE L ESS
2
IO
9/ CM / SEC

-o

ROOM TEMPERATURE

10. 2

10. 3

10 . 4

10. 5

10. 6

10. 7

0- -

GALLIUM
A

_-SILVER

J)- -

-<r

-'--

- - ' - -BOO

AMBIENT PRESSURE, mmHg

2.09xI04

....<l

0::

a
;:::

10 ' 6

THAN LOXIO'

10 . 11

<,

FIG. 6. E vaporation rates for various metals in vacuum. Ambient pr essure , 8.0 X 10 - 7 to 2.0 X 10 - 6 mm Hg,

10 . 6

<l

0::

-,L
-'" '"

0..

<l

>

10. 8

UJ

10" 0

IOIOL--'i?'--

50

--'i?'---

....1....-

350

....1....-

500

650

-'--

950

TEMP. OF

FIG. 5. Evaporation ra te of PTFE at various temperatures

a nd pressures .

F IG. 7. Evaporation rates for va rious metals in vacu um . Am bient pressure , 8.0 X 10 - 7 to 2.0 X 10- 6 mm Hg.

15

Fricti on of Materials in Vacuum

rates to det ermine vapor pressure ca n b e accom pli shed
for pure met al s by a simp le eq uatio n :

PIIlIll

17.14 G

where

Pmm
G
T
In

Downloaded by [Moskow State Univ Bibliote] at 10:08 30 May 2013

l1J
f/l
<,

:r
u

<,
0'

....l1J
<l

Cl:

t=

<l

Cl:

::1 ~
:1
"I
10 . 9

IJ1

det ermined fr om it s

IS

METAL MATRI X MoS 2 COATING

~

o I

6:>.3 8

Em

AIR
~ VACUUM

0:

~~
:;: ;;

0:

10

'

lJ.JZ

0-

52
.1

.6

::=:=:

SILICO NE RESIN BONDED MoS 2

0

PHENOLIC-EPOXY BONDED MoS 2

Q.

~ ',J~~I'
50

fllIi
33-_

IOOOXIO 6

17.14 ( 2.0 X 10 - 6)

The vapor p ress ure of zinc at 500 F presented in th e

lit era t ur e (1 0 ) is 1.0 X 10- 4 mrn H g .
E vapora t ion-ra te experiments wer e conducted with
four molybdenum disulfide coatings in va cuum at various t emperatures . An elect ronic bal an ce wa s used to continuou sly measure weight ch an ges with t ime . The results
ob tai ned in these exp eriments a re presented in Fi g. 8.
I n gene ra l, th ere appears to be a break in evaporation

CERAMIC BONDED MoS2

0

PIIIIIl = 9 .8 1 X 10 - :;

vapor p ress ure in mrn H g

evaporat ion rate in g / cm- /sec
temperature in 0 K
molecular wei ght

The vap or pressure of zin c

evaporation rate at 500 F:

PIIIIII

200

350

500
TEMP. of

80 0

.4

~~

U::: ~

"-"-

1J.J

0"-

.2

950

FIG. 8. Evap ora tion ra te o f various M o S ~ coa ting s in va cuum .

Ambient pressure, 1.0- 2.0 X 10 - 6 m m H g ; O.OO I-in . M o S ~ coa t ing on Ni- Cr a lloy .

I AI DISK SPECIt:1E N. 5~1 0 0 TOOL,

STEEL IN AIR
O.OOOS"

z o

uu

u o

L=:
65 0

I-Z

~
~2100

'---.r--'
440 -C

Ni -Cr
COBAL TBASE ALLOY ALLOY
F IG. 9. Fricti on a nd w ea r of va ri ou s a lloy s in a ir a nd in
va cuu m . Va cu um , 5.0 X 10 - ' to 2.0 X 10 - 6 mm H g ; slid ing
veloci t y , 390 ft / min j load , 1000 g ; duration of ru n , I h r.

----~~-..,----(Cl DISK SPECIMEN. 440-C STAINLESS

STEEL IN_ AIR

0.02S"

. ..
t

l:

" 1

\.

,:;

. '',

:'... .1.

-~-(8) DISK 'SPECIMEN, 52 100 TOO L

-STEEL IN VACUUM

(D) DISK SPECIMEN, 440-C STA INLESS

STEEL iN VACUUM

F IG. IO(A ) - ( D ) . Ph ot omi cro gra ph s a nd sur fa ce p r ofile tra cin gs o i w ea r a reas o n di sk spe cime ns , loa d , 1000 g j slid ing
veloci t y , 390 ft /min ; duration o f r un , I h r j X 20 . (A ) Di sk spe ci me n, 52 100 tool ste el in a ir . ( B ) Di sk spe ci m en , 52 100
tool ste el in vacu um. ( C ) Disk s pe cime n, 440 -C sta inless st eel in air. ( D ) Di sk spe cim en , 440- C sta inless steel in vacuum.

16

DONALD

H.

BUCKLEY, MAX SWIKERT , AND ROBERT

L.

JOH NSON

.1

~~i

;At ' :

~ l~

p,

-----~
(EI DISK SPECIMEN.
CaBAL T-BASE l ~Lf;l O Y IN

.
/

l~Lp I S K S.~~CIMEN,

0.0005" L

Ni-Cr AllOY IN AIR

AIR

0.025"

I.

,1~ .'
i

Downloaded by [Moskow State Univ Bibliote] at 10:08 30 May 2013

Eb

----~---~---------

(HI DISK SPECIMEN,

Ni-Cr AllOY IN VACUUM '

(FI DISK SPECIMEN.

COBALT-BASE AL LOY IN' VACUUM

FIG. lO (E )- (H ) . Ph ot om icrograph s a nd sur face profile t ra cin gs of wear a rea s o n disk specimens, load, g; sliding veloci ty , 3 90
fpm ; duration o f run , 1 hr ; X 20 . ( E ) Di sk specime n , coba lt-base a lloy in ai r . ( F) Disk specimen , co ba lt-base alloy in va cuum .
( G ) Di sk spe cime n, Ni -Cr -AI a lloy in air. (H ) Disk specime n , Ni -C r -Al all oy in va cuum .

(I) DISK SPECIMEN. Ni-:BONDtD TiC AND CbC

CERMET IN AIR f

0.0005"L
0.025

...

(J) DISK SPECIMEN, Ni-BONDED TiC AND

'CERME T-IN

YAc uu".B
:~:.......--....

11

esc I___

F IG. 10 ( I ) , (J ) . Photomicro graphs a nd surface profile tr acings of wear areas on di sk specimens ,

load , g ; sliding velocity , 3 90 fpm ; duration of run , 1 hr; X 20 . (I ) Sp ecimen a nd rid er , Ni bonded Ti C a nd CbC cermet in air. (J ) Sp ecim en and rid er , Ni-bonded TiC and C bC cermet
in vacuum .

17

Friction of Xlaterial s in Vacuum

curves for all coatings ; thi s result indicates a change in
evaporation rate. This change ma y be du e to two different evaporation rates, one for th e binde r, a nd th e
other for moly bd enum disul fide itself.

Downloaded by [Moskow State Univ Bibliote] at 10:08 30 May 2013

F RI CTIO;-; Ar-;'O \VE AR D AT A

Unlubricat cd metals, Fri cti on and wea r experiments

were conducted in a ir and vacuum with five a llov combinations. The results obta ined in th ese experiments ar e
presented in Fi g. 9. The fri cti on a nd wear values for
521 00 steel sliding on itself were lower in vacu um
than in air. Ex amina tion of th e disk surfaces a fte r th e
experiments ind icated a chan ge in th e wear mechanism
[Figs. 10(a) and ( b) J. Free met a l wear particles a re
oxidized in air, a nd th e resulting metal oxides on the
particles pr event adherence to th e ba se met al. At an
ambient pre ssure of lO- u mm H g, however , where oxygen
availability was ap preciably reduced, the wear surface
of the disk showed evidence of consid erable metal transfer as nascent wear particles readily adhered to the
parent metal. The s urface pr ofile tracings of Fig. 10 (b )
indicate " build up" on th e disk sur face. This was apparently du e to th e transfer of met al from th e rid er to
the disk specimen.
The low fricti on coefficients experienced for 5210 0
steel in vac uum ( lO- U mm H g ) may be accounted for
in that , even a t lO- t; mm Hg, oxyge n is pr esent. Bowden
and Tabor ( 11) hav e indicated th at copper will oxidize
as rapidly a t 1O- :{ mm H g pressur e as it will a t a tmospheric pressure ; also , it has been established elsewhere
that, at 10- 6 mm H g, a clean metal surface will ad sor b
a monolay er of gas in a second . Since some oxygen is
available at 10- 6 mm H g, it is pr obabl e th at as pieces
of metal, which ar e quite hot , tr an sfer from one specimen surface to th e other , localized oxida tion of th e
transferred met al occurs . With th e limited oxygen avai lable the lower oxides of iron , FeO and F ea04 ' would
.50

z
Q .40

o
o

RUN STARTED AT 10- mmHg

DRY AIR

form on fer rous metal a nd result in a fricti on coefficient

lower than normally encounte red in air at atmospheric
pressur e ( 12 ) where F e:!O;j is one of th e oxides present.
Result s ob ta ined a t pr essures lower than lO- u mm H g
sho uld differ from th ose obta ined at lO- t; mrn H g.
The coefficient of frict ion for 52 100 tool steel sliding
on 52100 tool steel a t va rious a mb ient pressures is pr ese nted in F ig. 11 (a) . The frictio n decreased from 0.45
at 760 mm H g pr essure to 0.2 between 10- 1 and 1O- :!
mm Hg. The fricti on began to increase again at 10- .1
mm Hg, a nd a t 5.0 X 10- 7 mm H g it was 0.375.
In order to red uce th e oxygen concent ra tion availabl e
for surface reaction at pr essures of lO- u to 10- 7 mm H g
a liq uid helium condensin g coil was added to th e fricti on
and wear apparatus. L iqu id helium will cond ense all
gases except helium . A friction experiment was made a t
2.0 X 10- 7 mm Hg using th e liqu id helium cond enser.
The result s obtained are pr esented in Fig. 11 (b ) . T he
init ial coefficient of fricti on was 0.2. This low value
being associated with th e pr esence of the lower iron
oxides on th e specimen surfaces. As time pr ogressed ,
however , th e coefficient of fricti on bega n to increase and
af ter 30 min of ope ra tion when th e residual surf ace
oxides ha d worn away , a fricti on of 5.0 was observe d .
The specimen then welded together and th e experiment
was te rmina ted by thi s complete seizur e.
The fricti on and wear results ob tai ned with 440- C
stainless steel sliding on itself in vacuu m wer e about
the sa me as in air (F ig. 9) . Examina tion of sur face
ph ot omicrograph s and pr ofile tr acin gs of th e disk wear
a rea I Figs. 10 (c) a nd (d) 1 indi cat e that particles were
tran sf err ed to th e disk specimen .
The friction and wear of a coba lt- base all oy were
det ermined in vacuum and air , a nd th e resu lts obtained
ar e pr esent ed in Fi g. 9. The fricti on and wear were lower
in vacuum than in air, and exa mina tion of th e sur face
topography indica ted no evidence of mass metal transfer
in vac uum [Fig. IOU ) 1. Similar results have been observed for th is particular alloy in inert a nd reducin g

RUN STARTED AT 760mmHg

t-

5 .0

MAS S WELDING
SPECIM ENS

OF

~ 4 .0

IU

u, .30

u,

t-

!!:! .20

u,
u,

I-

w 2.0

u,

u,

~
u,

UJ

u,

S .10

ol...:--l---l...:::--l.....-...l....,,--l...---lL....l..-.......L----l-~-'----l
6
1
4
4
10

3.0

10 -

10-

10-

10 -B

PRESSURE , m m Hg
FIG. It (a ). Coe fficient of fr iction for 52100 sliding on 52 100
at var ious a m bient pressures. Slidin g velocit y , 39 0 fpm ; load ,
1000 g; temperature , is F .

1.0

15

35

TI ME , M I N

FI G. II (b ) . Coefficient of fr iction for 52100 sliding on 5 2100

in vac uum with liquid helium cryogenic pumping; pr essure 2.0
X 10 - 7 mm H g., sliding velocity 390 fp m, load 1000 g.

Downloaded by [Moskow State Univ Bibliote] at 10:08 30 May 2013

18

DONALD

H.

B UCKLEY, MAX SWIKERT , AND ROBERT

atmospheres (data in process of publication) . T his particu lar alloy IS an air cast matenal and has about 1.0
per cent siLcon in its composition. Th e influence of
silicon on the friction and wear properties of materials
is discussed in Reference ( 11) . It was established in (11)
tha t sma ll quan tities of silicon rather markedly reduced
the friction and wear normally enco untered for alloys
in inert and reducing atmospheres. T his same mechan ism
could be expec ted to app ly in vacuum.
T he friction and wear properties of a vacuum-melted
nickel-base alloy (Ni-Cr ) were next dete rmined. The
results obtained in air and vac uum are presented in
Fig. 9. The coefficient of friction in vac uum was greater
than in air. The rider wear , however, was about the
same in both environments. Examination of this wear
area on the disk specimen indicated metal transfer in
vacu um [F ig. 10( h)] . From the photomicrograph it
appears that pieces of metal were transferred from rider
to disk and then smeared in the direction of sliding.
Though the ride r wear was nearly the same in air and
in vac uum, the wear mechanism on the disk surfaces
was q uite different, as indicated by comparison of the
photomicrograph and surface profi le traces of F igs. 10 (g)
and 10( h) .
T he friction and wear values for a nickel-bonded
titanium and columbium carbide cerme t sliding on itself
is presented in Fig . 9. For this particular material bot h
frict ion and wea r were higher in vac uum than in a ir.
T he photomicrograph and surface profile tracing of Fig .
10 (j) indicate evidence of metal transfer to the disk
surface in vac uum.
Lubricated metals. The mechanism of wear for metals in vacuum indicates that stable films should be
emp loyed to lubricate these materials. Since molybdenum
disulfide has been show n to be a good dry film lubricant
in air and has very low evaporation rates in vacuum ,
1.0 XIO 6

COATINGS, 0 .0002 TO 0 .0003 IN. IN THICKNESS

L.

J OH N SON

molybdenum disulfide coatings using various binders

were used as solid-film lubr icants for 440-C stainless
stee l in vacu um. The friction and wear resu lts obtained
with 440- C slidi ng on 440-C coa ted wit h vario us molybden um disulfide films in vac uum are presented in Fig .
12. From the results obtained, it appears the lubricant
binder plays an important role in the friction and wear
results obtained wit h molybdenum disulfide coatings.
The best friction and wear were obtained wit h an
epoxy-phenolic and a silicone resin-bonded molybdenum
disulfide coating. The metal matrix was less satisfactory,
and th e ceramic bonded gave the poorest results wit h a
continuous frictio n coefficient of about 0.3 over an en tire
1 hr of operating. These results, however, were obtained
at room temperature, and the epoxy-phenolic coa ting
may not appear as promising at elevated temperatures.
Friction and wear experiments were made wit h ot her
solid film, and the resul ts obtained are presented in
Fig. 13. A lead oxide-silicon dioxide coati ng developed
for high-temperature use in air was applied to 440-C
stainless stee l and was run in vacu um. A fric tion coefficient of about 0.17 was obt ained at 10- 6 to 10- 7 mm
H g amb ient press ure. In air at room temperature, with
a sliding velocity of 430 ft / min, th is particular coa ting
had a friction coefficient of 0.3 (14) . In vacu um th e surface became sufficiently hea ted witho ut an external hea t
addi tion to give a friction coefficient similar to tha t
obtained in air at 250 F in (14) .
A calcium fluoride solid lubricant coati ng developed
for high-temperature app lications was applied to a
N i-Cr disk . A Ni -Cr-Fe rider was used again st the disk
in vacu um . The friction and wear obtai ned a re presented
in Fig. 13. The coating gave a friction coefficient of 0.18
over a 1 hr period, and the wear to the rider specimen
was low. T he frictio n coefficient obtained wit h th is coating in vacuum was lower th an obtained in air at the
same temperature.
In the literature, instances are cited where thin, soft
metal films were used as pro tect ive coatings for bearings
run in vac uum (4, 15). Vario us soft metals were there-

.0 1

COATINGS, 0 .0004 IN.

IN THICKNESS

1.0X10-6
;-"

Q::

:g

.0 0 0 1L--==

0::

"'--_ _~=L-_--"="""-_

__""=""____

.30 6
u,

3=

0::

.0 8

l:j E.0 6
.0 4

.0 2

.01

WZ

0-

Z o

~~

Q:: ~ .

. 10

o
I- Z

Q::
~
wQ::

CERAMIC
BONDED

.000 I

;Z
W

.3

TIS:

I II

I
:i\IIIIIf

g lJ...Q . 2

'---...,.-1

'---...,.-1

'-... - '

METAL
MATRIX

SILICON
RESIN
BONDED

PHENOLlCEPOXY
BONDED

FIG. 12. Friction and wea r of 440-C on 440-C with vario us

MoS 2 films. Ambi ent pressure , 8.0 X 10- 7 to 2.0 X 10- 6 mm
Hg j slidin g velocit y, 390 fpm j load , 1000 g; duration of run ,
1 hr .

II

'-

'"'

~ o tJ
W
0:: . 1
o lJ...
RID~R _ _
0':'-;"
4 ~':"
""~::'
''''~''~'c~~~::---f7"~;:;--;'7'';~:---!''f'~';;----f':'~'='
ON
440-C Ni-Cr- AI 440-C
DISK
L UBRICANT-PbO Si0 2 CoF 2
TIN
COATING

FIG. 13. F riction and wear of alloys with various coatings in

vacuum . Ambient pressure, 8.0 X 10- 7 to 2.0 X 10- 6 mm Hg ;
sliding velocity , 390 fpm; load , 1000 g ; duration of run , 1 hr.

19

Friction of Materials in Va cuum

fore appli ed to 44 0- C s ta inless stee l s ubs t ra tes to det er mine th eir inl1uen ce on th e fricti on and wear of th ese
substrates in vac uum . The results ob tai ne d with a 440-C
stainless stee l rider slid ing on th e thin metal film (0 .000 4
in. thickn ess ) coa te d 44 0- C disk s are p resented in Fi g.
13. The fric t ion coeffi cient for lead , gold, a nd si lve r was
less than 0. 1 wh ile tin was a bo ut 0.14. The wear for
440-C sta inless stee l wa s low with all four coa tings . The
thin metal fi lms appear to have p roperti es wh en appli ed
to hard subs t ra tes that make th em pot enti al ca nd ida tes
as solid-film lubri cants for use in va cuum .
Summary of results

Downloaded by [Moskow State Univ Bibliote] at 10:08 30 May 2013

Evapora tion ra tes , and fric tion and wear wer e obtained at a pressure o f 10 - 6 to 10-; mrn H g. Since
the pressures enco un te re d in sp ace may be man y orde rs
of magnitude lower (a p p rox ima te ly IO -I~ mm H g ), th e
results obta ined in simila r expe rime nts a t low er p res sures may di ffer som ewha t from th ose ob ta ine d herein .
The results presented here, how ev er , do give some indication o f the effects of reduced a mbient pr essures on
lubricant s, frict ion, a nd wear. The results ob tai ned in
this study a re s umma rized as follo ws :
1. The use of l\I o S ~ coatings (e poxy-p he nolic resin
and silicone resin bonded 0.000 2 to 0 .0003 in . thi ck ness) p rovided effec t ive solid lub ricant films for 440-C
stainless stee l a t pressures of 10 - 6 to 10 - ; mm H g.
Both fricti on a nd wear wer e ex t re me ly low with th ese
coatings.
2. Some met al s (Ag, Sn, Au, and Pb ) wh en a pplied to s ubs t ra tes suc h as 440 -C sta inless stee l (0 .0004
in. thi ckn ess ) ap p rec ia bly redu ce th e fr ict ion a nd wear
normall y enco un te re d wit h thi s a lloy in vac u um ( 10 - 1'
to 10-; mm H g ).
3. The frict ion a nd wear results ob ta ine d with
various met al s in vac uu m ( 10 -(; to 10 - ; mm H g )
indicat e a wear mech ani sm unlik e th at enco un te re d
in air. I n ge ne ra l th e wea r in va cuum was cha rac te rized by mass m et al t ra ns fer . The fricti on coe fficien ts
were lower than ob ta ine d in a ir for so me a lloys (e.g .,
52100) a nd co ns ide ra bly hi gh er for othe rs (e .g., NiCr alloy a nd Ni-bon d ed Ti C a nd CbC). Opera tio n at
lower p ress ur es might be expec ted to furth er alter
the wear mech anism based on oxygen a va ilability.
4. Th e ev apo ra tion data for some in or ganics
(CaF~ a nd ::\l o S ~ ) and met al s (Ag a nd Sn) indica te
they have po te n t ia l for use as lubri can ts in vac u um
(10- 6 mm H g ) to temperatures as hi gh a t 1000 F .
5. T he evapora tio n data indi cate that so me oils
and greases ma y be used as lubri cants at pressures
of 10- 6 mm H g for sho r t pe riods of t im e p rovid ed
the a mb ie n t t emper ature is low (55 F ).
RE F E R EX C S
I. RIEHL. \V . A.. L OOXEY. W . C .. a nd CARUSO, S. D ., "Com -

patib ilit y of Engi neering Materials wit h Space Enviro nme nt,"
Army Ordnance Missile Co m ma nd . It em 1. P a rt II of ARP A
Order 92-5 9 (Oct ober , 1960 ) .

2. F REUXllL!CH . M . M ., an d H xx x o x , C . H .. " P rob lems of

L ubri ca ti on in Space," L ub ricat ion En g, 17 ( 2) , i2-77 (1961) .
3. J .\(;ODOWSKI, S. S.. and FREUIWLICH, M . M. , "I nve st iga tio n
of P rop ert ies of Lub ricants in H igh Vac u um," Thi rd P rogress
Repor t-WA D D Repo rt :\0 . i556- 1-3 Contract AF-3 3 (6 16)6S-I5 ( Octobe r, 1960 ) .
.i , ATI.EE. Z. J .. WII.SOX, J . T .. a nd FIDlER. J. C., " L ub ricat io n
in Va cu um by Vaporized T hi n M et alli c Fi lms," J . II pp l.
Phy s. 2 (9) . 611-6 15 (19 40) .
5. Bowm.x , F . P .. an d H UGHES, T . P. , "The Fric tio n of Clea n
M et al s a nd th e Infl uen ce of Adsorb ed Ga ses. Th e T emper at u re Coefficient o f F ricti o n," Pr oc. R oy . So c. ( L ond oni,
A172 , 263 ( 19.\9).
6. BOWDEX, F . P ., a nd Y OUXG , J. E ., " Frictio n o f Clea n M et al s
a nd th e In fluence of Ad sorb ed F ilm s," Pr oc. R oy . So c. ( L ondoni , A208. 3 11-3 25 (195 1) .
7. BOWDE X, F. P ., a nd ROWE, G. \V., "The Ad hesion of Clea n
M et al s." Proc, R oy . So c. ( L ondon v; A233 , 429-44 2 (1956) .
8. HAXSI:X. Sn:(;FR IED , "Research P rogram on H igh Va cuum
F ric tio n." Litt on Indu st ries of Ca lifornia. Beve rly Hill s, AF
Co ntract :\0 . 49 (6.\8)-343, ( M a rch , 1959) .
9. MO:--;K , G. W ., "A pparat us for Weigh in g in Vac uum ," J.
Ap pl. Phys . 19 ( 5) . 485-486 ( 19-18 ) .
10. D US Il ~ I.\X. S., " Scientific Foun da tions o f Vac uum T echnique,"
pp. 246-2-19, Wiley , Ne w York, 19-1 9.
11 . BOWD!:,', F . P ., and TABOR. D., "Frictio n a nd Lu b ricat ion ,"
p. 140 , Wil ey , Ne w Y ork , 195i .
12. J OIlXSOX, R . L., GODFREY, D ., an d BISSOX, E . E., "Friction
of So lid Films on Stee l at Hi gh Slid ing Veloci ties ," NACA
T :\ 1578 (19 48) .

L., "The I nflu en ce of

Silico n Ad d itio ns on Fricti on a nd Wear of Nickel Alloys
at T emp era t u res to 1000 F ," Tr an s. liS L E 3 (1 ) , 93- 100
(1960) .
1-/. J OHXSOX, R . L., a nd SLIXEY, H . E ., " H igh T em pera ture
F ricti on a nd Wear Pro pert ies of Bo nded Solid Lub rican t
Fi lms Co n tai ning Lead M on oxide," Lubrira tion Eng , 15 (1 2) ,
-I8i--I9 1:-196 ( 1959) .
15. e. B.S. Lab ora t ories T echni cal Bullet in 463-6, " Vac u um Bearin gs a nd Dry Fi lm L ub rica nts."

13 . B UCKLEY, D . H ., a nd J OH I'o"SOI'o" , R .

BIBLIOGR APHY
1. BOWIH:X. F . P. , a nd H UGHES, T . P ., " T he F rictio n of C lea n
M etal s an d th e Influ ence of Adsorbed Gases. Th e Te mperatu re Coe fficient of Fricti on ." Proc. R oy . So c. ( L on don v;
A172 , 263-2i9 (19 39) .
2. HOWDEX. F . P ., a nd Yo uxc , J. E ., "Frict ion of Diam on d ,
G rap hite . and Ca rbo n a nd th e Infl uen ce o f Su rface F ilms,"
Pr oc. R oy . Soc. ( L ond on'[ , A208 , 444-455 (195 1) .
3. BOWIJ EX, F . P ., an d YOUX(;. J . E., " Frictio n of Clea n M et al s
and th e Influence of Ad sor bed Films." Proc , R oy . Soc . ( Lon don i , A208 , 3 11-325 (195 1) .
.t , BOWlJ EX, F. P ., a nd R OWE, G . W . " T he Ad hesio n of Clea n
M etal s," Pro c. R oy . Soc. ( L ond onv . A233 , 429 -4-12 (19 56) .
5. SI~lOl'I , 1., M cMAHox, H . 0 ., an d Bow cx , R. J ., "Dry M et allic F rict ion as a fu nct io n of T em perature bet wee n 4.2 a nd
600 K," J . II ppl. Ph y s. 22 ( 2) , 177-1 84 (19 51) .
6. S.\\'A(;E, R. L., "Gra phite Lu b rica ti on ," J. A pp l. P hy s. 19 (1 ) ,
1-10 ( 1948) .
7. SA\"AGE, R . H ., a nd SCHA EFER, D . L. , "Vapo r Lu bri cati on of
G ra ph ite Slid ing Co ntac ts," J . Appl . Ph y s. 27 ( 2) , 136-138
(1956) .

20

D ONALD

H. BUCKLEY ,

MAX SWIKERT , AND ROBERT

8. ] OHNSOX, V. R ., a nd VAUGHX, G . W ., " Invest iga tio n of th e

M echanism of MoS 2 Lubrication of Vacuum ," J . Appl.
Ph ys. 27 (10 ) , 1173-11 79 ( 1956) .
9. BELL, M . E. , and F INDLAY, ]. H. , " Moly bde nite a s a Ne w
Lubricant ," J . A m . Ph ysic. So c. 59, 922 ( 1941) .
10. U.S. Patent No , 2,280,886- Ap plicat ion

filed M arch , 1941

by P ort er H. Bru ce, Assignor t o Westingh ouse El ectric a nd
M anu fa cturing Co .
11. L AVIK, M . T ., GROSS, G . E ., an d VAUGHX, G . W ., " Investigati on of th e M echani sm of Tungst en Disulfide Lu brication in
Vacuum ," Lubrication Eng . 15 (6) , 246- 249 :264 (1 959) .
12. H ANSEN, SIEGFRIED, " Res earch Program on H igh Vac uum
Friction ," Litton In du stries of Ca lifo rn ia, Beverly Hills, AF
Co nt rac t No . 49 ( 638)-343 (M a rch , 1959) .

Downloaded by [Moskow State Univ Bibliote] at 10:08 30 May 2013

13. BELLER, W ILLIAM, "Friction R esea rch Grinds to a H alt ,"

M issiles and R ock ets 7 (9) , 23-2 4 ( 1960) .

L. JOHN SON

chamber s. N umerous cold-trap and baffle designs have

been reported in th e literature and users of oil diffusion
pump s have employed these and other modificat ions in
vacuum system s. There appears, in general, to be very
littl e if any stan dardizati on on cold-trap and baffle designs. Various cold traps and baffles were therefore tried
in th e vacuum friction and wear apparatus in an attempt
to eliminate back-migrati on of oil vapors.
The first step tak en was to place a liquid-nitrogen
spiral cold trap in the apparatus between the experimental chambe r and th e oil diffusion pump . A schematic
of th is cold trap is shown in Fig. 14(a) . The gas being

SPECIMENS

14. RI EHL, W . A., LOONEY, \V. C. , a nd CARUSO, S. U ., " Co m patibility of Engin eering M at eri al s with Space En vironment ,"
Army Ordnan ce M issile Command , It em 1, P art II of ARPA
Or der 92-59 (October, 1960 ) .
15. ATKINS,] . H. , BISPLINGHOFF, R . L ., H AMON, ]. L ., ] ACKSON,
E . G ., a nd SIMOXS, ] . C ., ] R., "Effect of Spa ce En vironmen t
on M at erials," N RC R es. Report 40- 1-04, Ohi o St ate Univ .
R esear ch F oundat ion Proj ect No . 920 (A ug ust, 1960 ) .
16 . F REUNDLICH, M . M. , a nd H ANNOX, C. H ., "P rob lems of
Lu br ication in Spa ce," L ubrication Eng . 17 ( 2) , 72-77 (196 1) .
t r, F REUNDLICH, M . M ., a nd ] AGODOWSKI, S. S., "Lu br icants for
Hi gh -Vacuum En vironments," WAD D T echn ical Report 60728, Part I , Co nt rac t No . AF3 3 (6 16) -6845 Project No. 3044
(November , 1960).
18. ] AGODOWSKI, S. S., a nd F REUNDLICH, M. M ., "Investi gat ion
of P rop erties of Lubrican t s in Hi gh Vac uum ," Third Progr ess
R eport-WADD R ep ort N o. 7556- 1-3 Co ntract AF33(616)6845 (Oct ober, 1960) .
19. W ILLIAMSON, ] . G ., "Po la rity Ancho rs N ew Space Lu be
Theory ," Chem , Eng . New s 39 ( 5) , 48-4 9 ( 1961) .

EXPANSION
BELLOWS

L1QUID- NITROGEN
COLD TRAP

20. ] OHXSOX, ] . R. , VAUGH X, G . W ., a nd L AVIK, M . T ., "Appar atus for F ricti on St udies at Hi gh Va cuum ," R ev . Sci.
In str. 27 (8) , 611-613 (1956) .
21. M ox x , G . W ., " Apparatus fo r Weighin g in Va cuum ," J.
A pp'; Phys. 19 (5) , 485-486 (1948) .
22. C.B.s. La bor at ories T echnical Bull etin 463-6, " Vac uum Bear in gs a nd Dry F ilm Lubrica nt s."
23. ATLEE , Z. j ., WILSON, ]. T. , and F ILMER, ]. C ., " L ubrication in Vac uum by Vaporized Thin M et alli c Films," J . Appl.
Ph ys , 11 (9) , 611-6 15 (19 40) .

Appendix
A

PUMP
FI G. 14 (a ) . Va rio us baffle designs used in vac uum fric tio n
and wear a ppa ra t us .

S TU DY OF THE EFFE CTIV EN ESS OF VA RIOU S TRAPPING

D EVI CES I N S TOP P IN G BA CK-MIGRATION OF DIFFU SIO N

P UMP OILS

The vacuum friction and wear apparatus used in this

investi gation originally employed an oil diffusion pump
to obtain high vacuum . The oil diffusion pump has associated with it the undesirable cha racteristic of permitting oil vapors to migrate from the pump. In the
vacuum literature it has been suggested that this problem can be eliminated by the use of baffles and /or cold
traps between the oil diffusion pump and experimental

pumped had to travel a spiral path along liquid-nitrogencooled walls. A friction experiment was conducted with
a disk and rider specimen in the experimental chamber.
The friction coefficient obtained with clean 440-C stainless steel was in a region (0.1) associated with effective
boundary lubric ation . The disk surface was checked with
distilled water after the experiment ; observations of high
contact an gle and lack of wettability gave evidence of
an oil film.
An optical baffle plate was then added between the
cold trap and specimens in an attempt to eliminate the
contamination. The baffle design used is shown in Fig.

Friction of Ma terials in Vacuum

21
I

\ C_OPPER !
BAFFLE

L '

I
I

LHEATER
Downloaded by [Moskow State Univ Bibliote] at 10:08 30 May 2013

F IG. 14 ( b ) , ( c) , (d).

Various baffl e designs used in vac uum fr ict ion a nd wear apparatus

.~~

.~

-.

4UNGSTEN
,GRID HEATER
FIG. 14 (e) , ( f) , (g) .

E l ---IE3

'4 PTICAL
BAFFLE

TWNGSTEN
HEATER GRID

Various baffle design s used in vacuum frict io n a nd wear a ppa ra t us

~-

JL

\ ...Ii---'- =c:

lJllr'

--

--.

f.-,

TUNGSTEN
HEA_TER
GRID

FIG. 14 (h), (i), ( j) .

COOLING
COILS"

t~

Va rio us baffle designs used in vac uum frict ion a nd wea r a pparat us

Downloaded by [Moskow State Univ Bibliote] at 10:08 30 May 2013

22

DONALD

H. BUCKLEY,

MAX SWIKERT , AND ROBERT

14(b) . Friction experiments with 440-C stainless steel

again gave a friction coefficient indicative of effective
boundary lubrication. Examination of the disk surface
with distilled water showed evidence of a contaminated
surface.
Th e use of a honeycomb copper structure as a baffle has been reported in the literature as a means of
trapping oil molecules. A baffle of this design was fitted
to the optical baffle, and th e unit was placed in the
specimen chamber above the liquid-nitrogen cold trap
[Fi g. 14(c )] . This arrangement was not effective in
preven ting specimen contamination by oil vapors.
Another approach to eliminating the back-mi gration
problem considered was that of using heat to decompose
oil vapors migrating to the specimen chamber. To achieve
this , a heater was attached to the optical baffle pr eviously used. The optical baffle with heater placed between
it and the liquid -nitrogen cold trap is shown in Fig. 14
(d). This arrangement was also inadequate in eliminating specimen contamination, as ascert ained by friction
experiments with clean 440-C stainless steel and wettabili ty checks . The heater plate was then replaced by a
heater grid of tun gsten coils. These coils were heated
to an orange-yellow heat in an attempt to decompose oil
vapors entering the specimen chamber. The heater grid
and optical baffle used are shown in Fig . 14(e). This arran gement was also unsatisfactory.
A tun gsten-wound heater coil was then placed in the
specimen chamber directl y beneath the disk and rider
in an attempt to keep vapors from the specimen surfaces
[Fi g. 14(f)]. This arrangement was insufficient, and the
specimens again exhibited evidence of surface contaminati on.
The design of the optical baffle previously used was
altered, and the new optical baffle is shown in Fig. 14( g) ,
where it was used in conjunction with the liquid-nitrogen
cold trap. In Fig. 14(h ) a tun gsten heater grid was
added below the baffle. N either of th ese systems accomplished the elimination of oil contamination as deter-

1.

JOHNSON

mined by friction coefficients and specimen surface examination.

T he next app roach to th e back-mi gration problem
considered was to remove the expansion bellows of the
appa ratus located between the specimen chamber and
the liquid-nitrogen cold trap and to replace it with a
heater-baffle assembly. Thi s assembly can be seen in
Fig. 14(i ). It consisted of two water-cooled optical baffle plates with a tun gsten-wound heater grid between the
plates. The temper ature of the space between the tun gsten grids maintained during diffusion pump operation
was 1000 F. The outside walls of the chamber were
water-cooled. Thi s assembly in conjunction with the
liquid-nitro gen cold trap minimized the specimen contamination. Examination of the disk surface with distilled water indicated a contact angle less than previou sly obtained ; however , the water still would not wet the
metal surface, and the coefficient of friction for 440-C
sta inless steel was about 0.2. An addition was then
made to the system, namely, the optical baffle used in
earlier trapping designs. Th e complete trapping syste m
can be seen in Fig. 14(j). The results obtained were
about the same as with the arrangement of Fi g. 14(i ).
A liquid-nitrogen-cooled plate type chevron baffle was
also considered for these experiments. This configuration was not , however, used because experimental evidence by colleagues showed that it also allowed testchamber contamination.
The experiences related here were obtained with a
common diffusion pump oil composed of petroleum
hydrocarbons. Separate experiments were conducted
with additional diffusion pump oils includin g a silicone
and a sebacate. In no case was back-mi gration of diffusion pump oil completely eliminated.
The inability to completely eliminate the back-migra tion of oil vapors from th e oil diffusion pump resulte d
in the replacement of the oil diffusion pump with an
ionizati on pump . Thi s pump employs no fluid or vapors
in its operation.

DISCUSSION
M.

H . H ABLANI AN AND E. G. J AC K SON (Na tional R esearch Corporation, Cambridge 42 , Massachusett s) :

th erefore difficult to determine exactly all possible cond itio n;

con trib uting to excessive backs trea ming.

We wish to comment particularl y on t he appe ndix of thi s pap er.

It is apparent fro m th e difficult ies th e a uthors had wit h diffusion
pumps th at th ere is a possibility of oil contamina tio n in diffusion
pum p syste ms. H owever, th ere is much evidence ava ilable indicating t hat t he difficult y is not an inh erent one, an d can be
a voided by suita ble ba ffle design and pump dow n techni qu es.
Th e authors' success with a n ion -m echan ical pump comb inatio n
shows that backst reaming can be tr a pped even at pr essures above
th e ultrah igh vacuum ra nge.
Th e au t ho rs do not give man y deta ils of th e diffusion pum p
system and pu mpin g proced ure, such as th e size and t ype of th e
diffusion pum p, th e pump -dow n sequence and associa ted pressu res, the presence or abse nce of sepa ra te roughing line, etc. It is

T he obv ious di fficulty appears to be insufficient trapping. The

majo r difficulties wit h t he tr appin g arrangements used by th e
a uthors are : (1) T he main liqu id nit rogen cold trap do es not
ensure at least one contact on a cryoge nic surface by molecule;
coming fro m any direct ion; (2) All ot her baffle ar ra ngeme nt;
used above th e main liqu id nit ro gen trap a re insufficient beca use
th ey a re eit her not cooled at all, or cooled only by wa ter.
The spiral liqui d nit rogen cold t rap permits molecules to pas,
th rough betwee n t he spira l a nd th e uncooled walls. In addition
molecules which happen to travel along pa ths parallel to th e
spiral surface, bo uncing off warm outer wa lls, will pass t hro ugh
th e t raps witho ut contacting th e cooled parts of t he t rap . After
some of th e oil molecules appear in th e space abov e t he cold t ra p.

Downloaded by [Moskow State Univ Bibliote] at 10:08 30 May 2013

F riction of Materials in Vacuum

it is useless t o tr y to sto p th em fro m en te ring th e working chamber by optical baffles if those baffle s a re not ref rige ra ted .
It is import ant t o distingu ish between prima ry ba ckstreamin g
which occurs in a well-defin ed pattern from th e t op je t of th e
pump, and th e molecul es re- evaporating fro m t he wall s which
come from random directi on s and ca n no t be sto p ped by u ncooled baffles . A well-d esign ed liquid nitrogen baffle mu st ass ure
at least one conta ct on a refriger ated surf a ce for molecules comi ng
from any dir ecti on. In sensit ive expe rime n ts it ma y be desirab le
to have a minimum o f two or mor e such con tac ts. N . M iller on
at a recent Am eri can Vacuu m So ciet y meeting reported th at a
system designed t o ens u re a t least one con tact results in fou r or
five actual contacts fo r th e a ve rage m olecu le, a nd th er eby reduces the prob abilit y of a molecule passin g throu gh to truly
negligible prop ortions.
Although heat ed grids for oil decompositi on hav e been discussed in liter ature some tim e ag o, th eir effect has not been ev aluated. To be efficient. th ey should be ti ght . in whi ch case th ey
will occupy a lar ge a rea of th e inlet d uct a nd conse q uent ly d ecrease the pum pin g speed. Th er e is a possibility th at such heaters
may drive th e p rodu ct s o f oil d ecomposit ion into th e cha m ber.
It would be perh a ps better t o place such ba ffles below th e liquid
nitrogen tr ap rath er th an above as used by th e a ut hors. In addi tion, the heat ers in Fi g. 14d , c, a nd h a p pear t o heat th e op t ica l
baffles above th em by radiation a nd th eref or e mak e th ose baffles
even less effect ive . The cop pe r foil t rap s show n in Fi g. 14c a re
only effective afte r a th orou gh bak eout a nd th ey ha ve been
proven only in sma ll glass sys tems. It is not sur p rising th eref or e
that they were not helpfu l as used by th e a ut hors.
In addition. it would be d esi rable fo r fri ct ion experime nt s und er
space condi tions to hav e a h igh er vac uu m th an p rodu ced in th e
system descr ibed in th e pa per. Eve n with a liq uid helium condensing coil. th e a ut hc rs ac hieved only 2 X 10- 7 mm Hz, whi ch
is about th ree o rde rs o f ma gnitud e high er th an th e ca pa bilit ies of
presently ava ila ble ultrahi gh va cuum syste ms with oil diffusion
pumps.
Following a re some refer en ces which ind ica te th at vac uum
essentially free of hea vier hyd rocarb on s ca n be obta ined wit h oil
diffusion pumps.
I. "The M easu rem ent o f Low P arti al Ga s Pressu re with th e
Mass Spectr omet er " b y H . \V . D ra win a nd C. Brunee ( AtlasWerke AG. Germa ny) fr om Vn k u u m-Fechnik, f\o . 3 (1 960 ) . Th e
fo llowing pa rti al pr essures were ob ta ined wit h mercur y diffu sion
pumps:
Hydrogen . 1 X 1O - !f m m H z : Wat er. 1 X 10- 111 mm H <; ; Carbon monoxid e. 5 X 1O- 1nmI)1 H g ; N it rogen , 5 X 1O- 10mm H g ;
Carbon dioxid e. less th an 1.5 X 1O-!f m rn H u : H ydroca rb ons,
less than 1 X 10 - 111 mm H z ; M ercu ry , less tba n 1 X 10 - 1 (1 mm
Hg; Total p ressur e. less tha n 3.3 X 1O-!f m rn Hz . Using oil
diffu sion p ump s, very simila r results we re obta ined a t t otal pr essure of 3 X lO -! ' mrn Hg. Th e a ut hors sa y: " . . . With both
pump typ es. a bo ut th e sa me ulti ma te pa rti al p ressures ca n be obtained wit h th e excep tion of h ydrogen . Th e pa rti a l pr essure of
hydrogen wa s a t least t en times high er with th e oil diffu sion
pumps com pared to th e mer cu ry pumps." It may be not ed also
that redu cti on of for elin e pr essure of a diffu sion p um p red uces
the amou nt of hyd rogen on th e high vac u um side.
2. X . Mi llcr on ( La wre nce R adi ati on Lab or atcry, Unive rsity
of California, Li vermo re. Ca !if.) a t th e First Svmpo sium on Surface E it ects on Spa cecraf t Ma t erial s, Palo A lt o, Calijorn ia ( M ay,
1959). " Diffusio n Pumps ha ve been dem on strat ed to be inh er ently clean . . .. Fir st , diffu sion pumps, both mercury a nd oil,
can be com plete ly tr apped . N o oil o r crac ke d hyd rocar bon spec-

23

trum , and no mer cury, d own to par t ial pr essures o f 10 - 11 mm

H g for oil and 1O- 1fl mm H g for mer cury is de t ect ed ."
3. "Mass Sp ectrom et er Investi gations in th e Ult ra h igh Va cuum " b y P . J a hn a nd J . Zah rin ger ( M ax-P la nck In st itute for
Nuclear Physics, H eid elb er g) , Vuk uum -Technik , N o. 10, 5, p . 138
(June, 1961 ) .
"A ve ry sensitive mass spec t ro me te r-a llow ing th e measur ement o f partia l pr essures below 1O- 1:! t orr-was used to investi gate th e com po sitio n of th e resid ua l gas in a va cuum system,
as ob ta ined wit h oil diffu sion pumps plu s nonrefriger ated baffl es.
a nd with an io n-ge tte r pump. Th e spe ct rum of th e residual ga s
was chec ke d dail y durin g seve ra l week s wh er eby d iffer en t types
o f pumps, ba ffl es a nd pumpin g fluid s have been used ."
" T he inv esti gat ion s have shown that th e com bin a tion t wo-stage
pump plus silico ne -ult ra fluid plus a lu min um oxide tr ap has
been pr ov en suita ble for pr oduction of ultrahigh va cuum . T he
pr essure rema ins consta n t for man y weeks a t its in itia l va lue
and th e residu al ga ses fr om th e pump a re only methan e an d
hydrogen ."
In genera l, expe rime nts wh ich great ly d epend on su r fa ce con d ition s mu st be cond ucted wi th ve ry caref ul vacuu m design and
t echniques, or cont a minatio n is possib le with both diffusion
p u mp s a nd ion-getterin g p umps wh en used t ogether with mecha nica l pumps.
A U T H ORS '

CLOSU RE :

The com ments by M essrs. M. H . H ab lanian a nd E . G . J a ck so n

on va cuum techn ology with diff usion pum ps ar e m ost welc om e
even th ou gh th ey do not pertain t o th e bod y of th e pa per . Th e
ap pe ndix to t his paper t o whi ch th ey refe r was included prima rily
so that other investigators would not have to duplicate this
effort . It is reason able t o expec t th at t he p ro blem of back mi gr a ti on ca ll be solved . Th e effo rts described in th e a ppe ndix , how ev er .
did n ot solve the pr ob lem . R ath er t ha n to spe nd m or e effort,
th e pr ob lem was avoid ed by usin g an ion pump. The ion pumped
sys tem is not fr ee fr om p rob lem s but for tunately th ey a re differ ent th an t he one of p rim ary conce rn her e.
Th e refer en ces cit ed b y th e d iscusser s a re indi cated to sugge st
th at sys tems " essen tially" free of ba ck mi gr ation ca n be obta ined.
Th e p rob lem in frictio n, wea r, and lub rica ti on st ud ies is th at
sys t ems mu st be ab sol utely free of orga nic conta mina t io n. In
visits to a number of la bora t ories no diffu sion pumped sys t ems
wer e observed th a t could be considered a bsolute ly clean . f\ 0 d oubt
t hose sys te ms includ ed man y of t he design considera tio ns ad van ced by th e discussers. On e la bora to ry indicated th at a diffu sio n pumped sys tem wit h a zeolite tr ap was com pletely free of
ba ck m igr ation . The effect iveness o f such a tr ap has not been
veri fied by th e a u thors, howev er , it mer it s considera t io n wh er e
only di ffusion pum ped sys tems a re ava ila ble.
On e specific po int raised by th e discussers concerne d t he high
pr essure ac hieved with liquid helium cr yopumping. Th at pr essure
(2 X 10- 7 mm Hg ) was ob ta ined by d esign rath er th an as a
minimum pr essure. Th e point mad e was th at pr essure measu rements a lone ar e not a n a de q ua te mean s of definin g sp ace sim ulati on . It is im portant to d efine molecul a r a nd at om ic species present in th e cha m be r a nd to measur e pa rtial p ressures. Using liqu id
helium t o t he limit of it s cry op urnping ca pa bilit ies in th e a p para t us, we ac hieve d pr essures in th e 10 - (1 mm H g ran ge. Th e p ressu res were measured with a nude hot ca t hode ioni zation gage
ad jacen t to th e expe rime nta l specime ns. Using ot he r gage s o f
types more com mo nly em ploye d by ot hers includin g th e discu ssers, lower va lues would be obta ine d .