COMPOSITES

SCIENCE AND
TECHNOLOGY
Composites Science and Technology 65 (2005) 741748
www.elsevier.com/locate/compscitech

Nanocomposite and nanostructured tribological

materials for space applications
A.A. Voevodin *, J.S. Zabinski
MLBT, Air Force Research Laboratory, Materials and Manufacturing Directorate, WrightPatterson Air Force Base, OH 45433-7750, USA
Received 31 August 2004; accepted 20 October 2004

Abstract
Satellites and space-born systems have a number of moveable mechanical parts, whose reliability is severely limited by degradation of lubricants and excessive wear. Many systems may remain in space for 1030 years and, therefore, exposed to atomic oxygen,
solar radiation, energetic particles, and temperature cycling from cryogenic to 400 C. Furthermore, these systems are frequently
tested on the ground and stored for many years under controlled environments before launching. Also, reusable launch vehicles
are so planned that they will operate with spaceterrestrial cycling and with temperature spikes in excess of 800 C during re-entry.
A chameleon tribological coating concept was developed to address this challenge. This approach relies on the coating to change
its surface (both chemistry and structure) to self-adjust to the environment and thus achieve long durability. The rst chameleon
coatings were made of WC, WS2, and diamond-like carbon (DLC); they provided superior mechanical toughness and performance
in space/terrestrial environmental cycling. In order to address the temperature variation, the second generation of chameleon
coatings were made of yttria stabilized zirconia (YSZ) in a gold matrix with encapsulated nanosized reservoirs of MoS2 and
DLC. Encapsulation of MoS2 nanoparticles into Al2O3 matrix and high temperature lubrication with low melting point glassy ceramic phases were also explored. Chameleon coatings with various chemistries are discussed along with their characterization by
various analytical, mechanical, and tribological methods. Coating toughness was remarkably enhanced by a grain boundary sliding
mechanism. Unique friction and wear performance was demonstrated by testing in controlled humidity air, dry nitrogen, vacuum,
500600 C air, and in environmental cycling.
Published by Elsevier Ltd.

1. Introduction
Space-born systems include various moveable devices
[1]: reaction wheels, gyroscopes, solar arrays, antenna
drives, sensor pointing mechanisms, gears, pumps, actuators, latches, releases, etc. Together they cover a broad
range of contact stresses from 107 to 1010 Pa and sliding
speeds from near zero in restraining mechanisms to
above 20 m/s in control-moment gyros. They experience
low frequency launch vibrations, and some of them
operate with dithering motion at frequencies up to 500

Corresponding author. Tel.: +1 9372559001; fax: +1 9372552176.

E-mail address: andrey.voevodin@afrl.af.mil (A.A. Voevodin).

0266-3538/$ - see front matter. Published by Elsevier Ltd.

doi:10.1016/j.compscitech.2004.10.008

Hz and high peak loads, e.g. gimbal bearings on space

platforms capable of rapid re-targeting.
Other challenges are extreme operation conditions
and a long service life. Satellites designed for the high
vacuum of space can be exposed to moisture during
assembly, ground tests, or launch, and contact atomic
oxygen in low Earth orbit. They operate in the broad
temperature ranges, where
100 to +100 C span is typical for satellites. Shuttle-type operations introduce both
terrestrial/space environmental cycling and temperatures in excess of 1000 C during atmosphere re-entry.
These extreme operating conditions are coupled with
an extended service life expectancy, which could be as
long as 30 years for an unattended satellite operation.
Estimates for 1530 years of service give about

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A.A. Voevodin, J.S. Zabinski / Composites Science and Technology 65 (2005) 741748

1091010 cycles in gimbal bearings of momentum control

devices or 106108 oscillations in solar array joints.
The mechanical, environmental, and endurance
requirements of space applications exceed the available
lubrication and wear reduction technologies, demanding
novel materials and advanced technologies. Presently,
low outgasing liquids (e.g. mineral oils, synthetic hydrocarbons, peruoropolyalkylethers) and solid lubricants
(e.g. PTFE polymers, soft metals, dichalcogenides) are
the predominant materials used for space lubrication
[25]. Liquids are used when tribo-assembly can be
sealed from the outside environment. In other cases, solid lubrication is preferred. Advanced concepts of solid
lubrication and wear reduction using recent progress
in nanocomposite tribological materials are discussed
in this paper.

2. Composite coating approach for space tribology

Transition metal dichalcogenides of (MoS2, WS2,
NbSe2, etc.) are the most common space solid lubricants. They are applied as powders mixed with various
organic and inorganic binders, burnished to the surface
from powders, or deposited by spray and vacuum deposition methods [6]. These lubricants are soft, not abrasion resistant, and oxidize in air. To comply with
endurance requirements of space applications, more advanced approaches were explored. One of them was selflubricating composites, where solid lubricant was
pressed into a supporting matrix, such as in bronze/lead
composites, glass-ber- and polyimide-reinforced PTFE
composites coated with MoS2 [79]. The composite approach was also used in high-temperature tribological
coatings, such as the NASA PS-200 series coatings produced by plasma spray which consisted of BaF2/CaF2
lubricant, Ag lubricant and binder, and Cr3C2 support
[10]. In the NASA PS-300 series coatings [11], Cr3C2
was replaced with Cr2O3 to improve high temperature
stability and reduce processing cost.
Development of vacuum deposition methods added
new capabilities for controlling the chemistry, structure,
morphology, and thickness of solid lubricants. This improved their friction, endurance, environmental adaptation and allowed precision components to be coated.
Examples are textured MoS2 lms [1217], metal doped
MoS2 and WS2 lms [1822], CFx doped WS2 lms [23],
metalMoS2 multilayers [2426], temperature adaptive
PbO/MoS2, ZnO/MoS2, ZnO/WS2 and moisture resistant PTFE/MoS2, LaF3/MoS2 composites [2731], etc.
Vacuum deposition technologies can be also used to
produce nanocomposite and nanostructured coatings,
whose mechanical and tribological properties are not
subjected to volume mixture rules but depend on grain
boundary eects and synergetic interactions of the composite constituents. Nanostructured designs oered a

unique opportunity to produce adaptive or smart tribological coatings, which were termed chameleon for
their ability to resist friction and wear by changing surface chemistry and microstructure in response to environment and loading changes [32,33], much like a
chameleon changing its skin color to avoid predators.
Although quite challenging, practical realization of
smart coatings is extremely rewarding for tribological
pairs subjected to multiple environmental changes, as
for example in aerospace applications. The tribological
coating adaptive concept was rst explored with previously mentioned coatings of oxides and dichalcogenides
(PbO/MoS2, ZnO/MoS2, ZnO/WS2), which can operate
in a broad range of temperatures [2830]. Multilayer
structures were then designed to combine these composites with buried diusion barrier layers and achieve surface self-adaptation during repeated temperature
cycling. Recently, novel wear resistant materials were
developed, which combine nanocrystalline carbides
(TiC, WC), oxide based ceramics (YSZ and AlON),
dichalcogenides (MoS2, WS2), and amorphous diamond-like carbon (DLC) into nanocomposite structures
[3234].
DLC is often referenced as a potential space tribological material due to its high hardness, low friction, and
low wear [35,36]. However, in long duration, heavily
loaded, and/or high sliding speed applications, the use
of DLC leads to its graphitization and associated increase of friction coecient in the high vacuum environment [37]. A hydrogenated DLC phase increases life
through hydrogen termination of active carbon bonds,
but not for long durations due to hydrogen depletion
after about 104 cycles [38,39]. An alternative approach
is incorporation of dichalcogenide space lubricants, such
as MoS2 or WS2, into a carbide/DLC/dichalcogenide
composite.
For example, chameleon coatings made of an
amorphous DLC matrix with incorporation of nanocrystalline TiC [40,41], WC [42,43], WS2 [32,44] and laser processed MoS2 reservoirs [45] demonstrated an
order of magnitude improvement in toughness above
that of single phase carbides while maintaining the same
level of hardness, a low friction coecient in cycling
from dry to humid environments, and an extremely long
life in both terrestrial and space environments. The surface chemistry, structure, and mechanical behavior of
these nanocomposite materials were shown to reversibly
change in the tribological contact, depending on applied
loads and operational environment to maintain low friction and prevent wear.
While maintaining the low friction in any environment is important, wear resistance requires an additional blend of both hardness and fracture toughness.
This is especially true for space applications due to the
reliability and unattended durability requirements. The
following sections of this paper discuss the most recent

A.A. Voevodin, J.S. Zabinski / Composites Science and Technology 65 (2005) 741748

743

developments in smart nanocomposite tribological coatings, starting with design criteria and examples of tough
tribological nanocomposites and progressing to chameleon coatings. All coatings were prepared by hybrid
physical vapor deposition processes, combining magnetron sputtering and pulsed laser deposition. Discussion
of the preparation processes can be found in
[32,33,41,46,47].

3. Tough nanocomposite coatings for high contact loads

Embedding grains of a hard, high yield strength
phase into a ductile matrix has been widely explored
in macrocomposites made of ceramics and metals, which
are known as cermets [34]. However, if grain sizes and
matrix separations are reduced to a nanometer level, dislocation activity as a source of ductility is eliminated
and new mechanisms are required to provide toughness
enhancement. Uniquely, these nanocomposites contain
a high volume of grain boundaries with a crystalline/
amorphous transition across grainmatrix interfaces,
limiting initial crack sizes and helping to deect and terminate growing cracks. These mechanisms helped to explain the fracture resistance of novel super-hard
composites, where both amorphous ceramic [4850]
and metal [5153] matrices were used to encapsulate
nanocrystalline ceramic grains. More on the super-hard
nanocomposite coating design and discussion of the active mechanisms can be found in available review articles [49,50,52,54,55].
Grain boundary diusion [56] and grain boundary
sliding [5660] were suggested as mechanisms for
improving ductility and providing super-plasticity of
single phase ceramic nanocrystalline systems. The recent
research indicates also that high ductility can be more
easily achieved in multiphase structures [61] and that
grain boundary sliding can be a primary mechanism of
super-plasticity [6265]. It was also found that equiaxial
grain shapes, high angle grain boundaries, low surface
energy, and the presence of an amorphous boundary
phase facilitate grain boundary sliding [56,57]. The
ongoing verication of possible deformation mechanisms also indicates the importance of nanovoid opening and nanocrack branching around nanocrystalline
grain inclusions for crack energy dissipation.
These ndings were used to develop tough tribological nanocomposite coatings, whose design is schematically shown in Fig. 1. The design includes the
following main concepts:
(1) a graded interface layer is applied between the substrate and crystalline/amorphous composite coating to enhance adhesion strength and relieve
interface stresses (combination of functional gradient and nanocomposite designs) [6668];

Fig. 1. Schematic of a tough nanocomposite coating design, combining a nanocrystalline/amorphous structure with a functionally gradient
interface.

(2) encapsulation of 310 nm sized hard crystalline

grains in an amorphous matrix restricts dislocation
activity, diverts and arrests macrocrack development, and maintains a high level of hardness similar
to super-hard coating designs [49,52];
(3) a large volume fraction of grain boundaries provides ductility through grain boundary sliding and
nanocracking along grain/matrix interfaces
[32,41,49,69,70].
These design concepts provide toughness enhancement through stress minimization, crack deection,
and ductility. They are close but still dier from the design concepts of super-hard nanocomposite coatings.
The primary dierences are viewed in the selection of
a matrix phase with a lower elastic modulus, relaxation
of the requirement for strong binding between the matrix and grains, and selection from a greater range of

Fig. 2. TEM image of an YSZ/Au nanocomposite coating with

improved toughness characteristics.

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A.A. Voevodin, J.S. Zabinski / Composites Science and Technology 65 (2005) 741748

Fig. 3. Knoop and Vickers indentation marks into the surface of 1 lm thick (a) TiC/DLC, (b) WC/DLC, and (c) YSZ/Au tough nanocomposite
coatings. Indents were performed with the maximum available load of 1000 gm, providing about 9 lm indentation depths due to the steel substrate
deformation. In all cases, there were no cracks at the indentation corners, which serve as stress risers.

acceptable grain sizes of the nanocrystalline phase that

is embedded in an amorphous matrix.
The conceptual design in Fig. 1 provides both high
cohesive toughness and high interface (adhesive) toughness in a single coating. Several examples of tough
wear resistant composite coatings are provided. Two
of them combined nanocrystalline carbides with an
amorphous DLC matrix designated as TiC/DLC and
WC/DLC composites. In another example, nanocrystalline YSZ grains were encapsulated in a mixed
YSZAu amorphous matrix as shown in Fig. 2. In
all cases, the large fraction of grain boundary phase
provided ductility by activating grain boundary slip
and crack termination by nanocrack splitting. This
provided a combination of high hardness and toughness in these coatings. Fig. 3, compares Vickers indentations made at the highest load of the machine (1 kg).
There are no observable cracks in these coatings, even
after signicant substrate compliance (indentation
marks are 9 lm deep into 1 lm thick coatings). The
coating hardness was quite high ranging from 18 to
30 GPa, and for most other typical hard coatings at
these loads, cracks in the corners of the indentations
are expected.
Thus, novel nanocomposite designs of tough tribological coatings are very promising. They explore fundamentally dierent concepts of toughness improvement,
when compared to macrocomposite materials such as
cermets. Furthermore, their design can be taken to the
next level by realizing that both matrix and nanograins
can serve as reservoirs of solid lubricants. These lubricants will be then released in a friction contact during
the course of sliding. The active tribological role of matrix and encapsulated grains is a basis for the tough and
low friction chameleon coatings, which are discussed
in the next section.

4. Chameleon tribological nanocomposite coatings

The objective of chameleon tribological coating designs is to provide a reversible self-adjustment of surface

chemistry, structure, and mechanical behavior in the

friction contact, depending on applied loads and operational environment to maintain low friction and prevent
wear.
In order to achieve reversible adaptation, two additional design concepts were developed and combined
with the tough nanocomposite coating concepts as it is
shown in Fig. 1 (design concept numbering is continued
here from Section 3):
(4) solid lubricant reservoirs are introduced as amorphous or poorly crystalline inclusions to minimize
reduction in composite hardness and elastic modulus, since crystalline solid lubricants are typically
very soft [32,71];
(5) friction forces and surface reactions with the environment are used to generate a lubricious transfer
lm or skin at the tribological contact, which
can self-adjust with each environmental change
[32,71]; i.e. coating components serve as reservoirs
to supply material for the tribo-skin, where formation of a lubricating lm with the required chemistry and structure reduces friction.
Fig. 4 presents a schematic of a nanocomposite coating design that exhibits chameleon behavior. This design was implemented in the fabrication of the YSZ/Au/
DLC/MoS2 and WC/DLC/WS2 chameleon coatings
(12 lm in thickness) where an amorphous matrix and
a hard nanocrystalline phase (e.g., YSZ or WC) were
used to produce optimum mechanical performance
and load support. Nanocrystalline and amorphous Au,
MoS2, and DLC were added to achieve chemical and
structural adjustment of transfer lms formed in friction
contacts during dry/humid environment and low/high
temperature cycling. Chameleon behavior is observed
during the following sequence. As deposited, all lubricant phases (WS2 or MoS2, DLC, soft metals, and oxides) are either amorphous or poorly crystalline and
are buried in the coating where they are sealed from
the environment. When sliding commences, wear processes expose the near surface components to the

A.A. Voevodin, J.S. Zabinski / Composites Science and Technology 65 (2005) 741748

Fig. 4. Schematic of a conceptual design of the YSZ/Au/MoS2/DLC

tribological coating with chameleon-like surface adaptive behavior.

environment, and stress and frictional heat cause

changes in chemistry and structure.
In low temperature humid environments, a graphiticlike transfer layer is formed by an sp3 ! sp2 phase transition of the DLC component, which eventually leads to
the formation of some crystalline graphite. This layer
provides a low friction coecient (i.e., 0.10.15) and signicantly reduces further wear. In humid environments,
formation of MoS2 or WS2 transfer layers is not favorable, due to their relatively high friction coecient.
Those phases also have a high wear rate and become
concentrated in the wear debris as the graphite-like
transfer lm forms.
When the environment changes to vacuum or dry N2
and the temperature remains low, a WS2 or MoS2 transfer layer is formed by an amorphous ! crystalline transformation of dichalcogenide inclusions. Rubbing orients
the crystalline material such that the low friction basal
plane is parallel to the surface. This provides friction

745

coecients as low as 0.01, reducing further wear of the

composite coating. Graphite from a previous cycle in
humid air is removed or covered over in the rst several
hundred cycles in dry conditions due to its high friction/
wear in the absence of intercalation by water molecules.
As an example of performance in cycling humidity,
Fig. 5 shows that the process repeats itself for YSZ/
Au/DLC/MoS2, providing a corresponding switch in
tribolm chemistry and friction response between
DLC in humid and MoS2 in dry conditions. The same
reversible process was also found for WC/WS2/DLC
nanocomposites, where surface chemistry was repeatedly switched between DLC in humid and WS2 in dry
or vacuum environments [71].
The long endurance of these composites in a high
vacuum environment is another very attractive property.
Fig. 6 shows an example of friction coecient tests for a
WC/DLC/WS2 coating over two million sliding cycles.
The friction coecient stayed in the range of 0.03
0.06. It was interesting to observe a reduction in friction
coecient with the number of cycles, which indicated

0.20

Friction Coefficient
0.16

in vacuum,
WC/DLC/WS2 coating

0.12
0.08
0.04
0.00
0

0.5

X10

1.0 X10

1.5X10

2.0X10

Cycles
Fig. 6. Friction coecient variation in a long duration sliding test of a
WC/DLC/WS2 coating in vacuum against a steel ball (Hertzian
contact pressure about 0.8 GPa).

Fig. 5. Friction coecient variation of a chameleon YSZ/Au/MoS2/DLC coating in a test with a cycled relative humidity. Friction response is
repeatedly switching from a lubrication provided by MoS2 in dry environments to lubrication provided by DLC in moist conditions.

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A.A. Voevodin, J.S. Zabinski / Composites Science and Technology 65 (2005) 741748

the ongoing process of WS2 phase re-orientation and

accumulation in the friction contact. The wear rate estimate after this long duration run was about 10
7
mm3 N
1 m
1. The most of the wear occurred within
rst 103104 sliding cycles, after which a steady state
friction with a negligible wear rate was achieved. The
low wear and friction coecients fulll the criteria of
self-lubricated wear resistant coatings for space applications, which was proposed to be 610
6 mm3 N
1 m
1
for wear rates and <0.1 for friction coecients [72].
In high temperature environments (above 500 C),
diusion of soft metal from the coating to the surface
and subsequent crystallization was explored as a selfadaptation mechanism. For YSZ/Au/DLC/MoS2 nanocomposites, Au grains of 2080 nm were nucleated on
the surface at 500 C (Fig. 7). This resulted in the formation of an easy-to-shear transfer lm for high temperature lubrication with a friction coecient of about 0.2
[33]. When temperature was cycled back to 25 C, the
friction coecient stayed at about the same level.
Using these mechanisms to provide adaptive lubrication, advanced tribological coatings can be produced
that survive multiple dry/humid cycling, temperature cycling, and provide long duration operation in many test
environments. Various carbides, nitrides, borides, and
oxides may be used as the hard nanocrystalline phase
in combination with carbon for lubrication in terrestrial
conditions, MoS2 and WS2 for lubrication in dry and
vacuum environments, and soft metals (Au, Ag, Ni) or
low viscosity glasses (network modied SiO2) for high
temperature lubrication. For example, similar success
was achieved with Al2O3/MoS2/CFx composites and
SiC/Cs2MoOS2/MoS2/DLC. In the last of these two
examples, a CsSiO2 glass transfer lm was formed in
the friction contact. This transfer lm material had a
low melting point and provided lubrication above
600 C [73].
For solid lubricant preservation at elevated temperatures, the encapsulation of nanosized grains of dichalc-

Fig. 8. TEM image of an Al2O3/MoS2 nanocomposite coating

consisted of an amorphous Al2O3 ceramic matrix encapsulating 510
nm inclusions of nanocrystalline MoS2 grains.

ogenides into an oxide ceramic matrix is especially

attractive. Such combination seals temperature sensitive
dichalcogenides (MoS2 and WS2 are easily oxidized at
above 400 C) inside a hard, thermo, and oxidation
resistant matrix. At normal operation temperatures,
the fresh non-oxidized lubricant is released to the surface by the wear process, providing long endurance in
vacuum. Fig. 8, shows an example of Al2O3/MoS2 nanocomposite coating, where 24 nm inclusions of nanocrystalline MoS2 grains were sealed inside an Al2O3
ceramic matrix. It was found that 1525 vol% inclusion
of MoS2 was sucient to provide friction coecients of
0.02 for over 600,000 sliding cycles in vacuum. One potential application of this material is space shuttle operations, where high vacuum low temperature operations
are interrupted by a short-term exposure to high temperature oxidizing environments during atmosphere
re-entry.
The coating design shown in Figs. 1 and 4 and the
examples provided previously were primarily tailored
to aerospace applications, but similar designs can be
developed to produce chameleon tribological coatings
for other environments. The concepts for producing
tough, hard, low friction nanocomposite coatings discussed here are universal such that they can be realized
using a variety of material systems and are easily tailored to specic applications.

5. Conclusions
Fig. 7. Gold grains nucleated on the surface of the YSZ/Au/DLC/
MoS2 nanocomposites after heating to 500 C in air.

The extreme mechanical, environmental, and endurance requirements of space systems require advanced

A.A. Voevodin, J.S. Zabinski / Composites Science and Technology 65 (2005) 741748

friction and wear protective coatings with unique tribological performance. Single-phase materials fail to deliver such performance, and multiphase materials are
currently explored to satisfy the growing demands of
space tribology. Modern vacuum deposition technologies provide the desirable performance by combining
hard and solid lubricant phases in thin nanocomposite
coatings.
Nanocomposite tribological coatings were designed
to respond to changing environmental conditions by
self-adjustment of their surface properties to maintain
good tribological performance in any environment.
These smart coatings have been dubbed chameleon
because, analogous to a chameleon changing its skin
color to avoid predators, the coating changes its skin
chemistry and structure to avoid wear. Their design concepts combine toughness improvement by nanocrystalline/amorphous structures, functionally gradient
interfaces, and incorporation of solid lubricant nano reservoirs to provide tribological self-adaptation in response to environment variations. Chameleon
tribological behavior is realized by activation of a number of surface-adaptation mechanisms: (i) formation of
hexagonal MoS2 or WS2 transfer lms in dry nitrogen
and vacuum tests; (ii) formation of graphite-like carbon
transfer lms from a DLC matrix in humid air; (iii) formation of transfer lms made of soft metal or low melting ceramic glassy phases in 500600 C sliding in air;
(iv) sealing solid lubricant nanograins in a ceramic matrix to protect them from a high temperature oxidation
and providing on demand lubricant release in the
wear process. The mechanisms controlling friction could
be repeatedly and reversibly switched, permitting good
performance during environmental cycling, e.g. terrestrial M space. The concept of chameleon composite
coatings can be realized in dierent material systems,
where nanoreservoirs of solid lubricants are encapsulated inside hard, tough and thermally stable nanocrystalline/amorphous matrices.
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