Wear 297 (2013) 841–848

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Wear
journal homepage: www.elsevier.com/locate/wear

Surface observations of a powder layer during the damage process under

particulate lubrication
Wei Wang n, Xiaojun Liu, Kun Liu
Institute of Tribology, Hefei University of Technology, Tunxi Road 193, Hefei, Anhui 230009, China

a r t i c l e i n f o abstract

Article history: Loose powder is used to lubricate the tribopair with the replenishing mechanism. This work analyzes
Received 3 April 2012 the contact and the damage behavior of the powder layer during powder lubrication. The typical life
Received in revised form cycle of a powder layer includes the full powder layer, partial detachment, serious detachment, and
13 August 2012
complete destruction, which can be concluded from the powder layer images. The carbon and copper
Accepted 15 October 2012
Available online 2 November 2012
content remaining on the surface are analyzed using scanning electron microscopy and energy
dispersive X-ray spectroscopy. Layer blistering, partial detachment, delamination, and scuffing, which
Keywords: represent the different forms of damage and deterioration grades, are observed using an optical
Graphite microscope. Layer blistering, partial detachment, and delamination are the damage forms that occur at
Sliding friction
earlier stages. Meanwhile, most of the speed difference is accommodated via shearing and sliding of the
Scuffing
powder layer. Scuffing, which indicates direct contact and rubbing between the steel surface of the top
Solid lubricants
Optical microscopy sample and the copper surface of the bottom sample, is a serious form of damage and is often observed
before the full destruction of the powder layer.
& 2012 Elsevier B.V. All rights reserved.

1. Introduction for quasi-hydrodynamic lubrication using particulate matter, and

Solid lubricants can be applied to a tribological interface in
various forms, and used successfully in many engineering areas
[1–4]. In most modern applications, thin films of solid lubricants
are typically deposited on surfaces via advanced vacuum deposi-
tion processes to achieve strong bonding and obtain a dense
microstructure and uniform thickness [5–8]. Moreover, solid
lubricants can strongly bond with a surface using proper adhe-
sives to provide a longer wear life [9–11], and can also be
dispersed or impregnated into a composite structure [12–14].
However, the lifetime of most solid lubricants are still limited
because of the finite lubricant film thickness. To increase their
durability, a self-replenishing or resupply system is needed but is
difficult to achieve [15].
Loose powders were also successfully used to lubricate sliding
bearing surfaces. Certain powder lubricants have been blended in
an aerosol carrier and sprayed directly onto the surfaces [16–19].
The results showed that powder lubricant films provide a lift and
separate the bearing surfaces, resulting in a drastically reduced
friction coefficient and wear of the tribomaterials. Furthermore,
bearing side leakage carries away most of the heat generated by
shearing [20]. Heshmat et al. [21] proposed a theoretical model
n
Corresponding author. Tel./fax: þ 86 551 290 1359.
E-mail address: wangwe@gmail.com (W. Wang).
several solutions were obtained. The in situ deposition of boric
acid in dry powder form is investigated as a potential, environ-
mentally benign, solid lubricant for sliding metal contacts [22]. In
their study, boric acid powder is aerosolized and entrained in a
low velocity jet of nitrogen gas, which is directed at a sliding
contact in a rotating pin-on-disk tribometer. Friction coefficient
below 0.1 can be consistently reached and maintained as long as
the powder flow continues. Wear rate is reduced over two orders
of magnitude.
Many factors, such as the powder properties, the experimental
setup, and service conditions affect the characteristics of powder
lubrication. Higgs and his colleagues [23–25] conducted a series
of tests on a tribometer consisting of simultaneous pellet-on-disk
and pad-on-disk sliding contacts, and proposed an asperity-based
fractional coverage model for studying the process of lubricant
film transfer. Their work showed that the MoS2 pellet actually
acted as a self-repairing, self-replenishing, and oil-free lubricant,
and found that abrasive wear is the predominant wear mechan-
ism governing the transfer film process. Their analysis model can
predict both the friction coefficient at the pad/disk interface and
the wear factor of the lubricated pellet/disk sliding contact.
McKeague et al. [26,27] presented a theory for predicting the
behavior of a powder-lubricated slider bearing that considers the
slip of the flow velocity at the boundaries. The formulation
includes the boundary roughness and granular temperature.
Kimura et al. [28,29] investigated the effect of the components

0043-1648/$ - see front matter & 2012 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.wear.2012.10.020
842 W. Wang et al. / Wear 297 (2013) 841–848
and composition of powder lubricants on their insulating and
lubricating ability. Results showed that the insulating ability of
powder lubricants is higher than that of conventional oil- or
water-soluble lubricants and effectively prevents the formation of
a scattered chill structure. Drozdov et al. [30,31] applied magnetic
powder as a lubricant to the rubbing zone. Gears were placed in a
magnetic field so that the lubricant and the magnet formed a
single magnetic circuit. Using magnetic powder lubricants
enabled the toothed reduction gears to operate satisfactorily
under Hertzian contact loads of up to 1100 MPa. Reddy et al.
[32,33] conducted a series of experiments to study the effect of a
graphite lubricant on surface roughness, grinding force, and
specific energy during the grinding of silicon carbide (SiC)
materials. Results showed a considerable improvement in the
performance of grinding SiC using graphite as a lubricant com-
pared with dry grinding in terms of specific energy requirements,
surface roughness, and damage. Wang et al. [34,35] carried out
the ring-on-flat experiments that proved the powder properties
significantly affect the tribological characteristics of powder
lubrication and analyzed the effects of the sliding velocity and
normal load.
The presence of powder in the rubbing interface is the pre-
condition for powder lubrication. Previous experiments showed
that powder could be introduced into the frictional clearance
without any special treatment. In these studies, the powders were
compacted, and the powder layer was formed under pressure from
the tribopair. Several macroscopic phenomena related to the
powder layer were reported, while the microscopic process are
not well discussed. The process and mechanism of powder layer
micro-damage is yet to be elucidated because little research has so
far focused on this topic. However, the damage behavior of the
compacted powder layer is important to the lubrication character-
istics. The current study tries to reveal the state of the powder layer
during powder lubrication. It, especially, focuses on the typical
microscopic damage and its inherent mechanism, which helps to
understand better the process of powder lubrication.
2. Experimental setup
The tribotester used in the experiments is equipped with a
ring-on-flat contact rubbing pair (Fig. 1). The annular top sample,
with a 24 mm outside diameter and 16 mm inside diameter, is
made of carbon steel, with a hardness of HRC52 and a surface
roughness Ra of 0.75 mm. To facilitate powder entrance into the
frictional interface, four notches (3 mm) are made along the radial
direction, and the contact face corner (1 mm) is rounded. The
lower sample is manufactured via powder metallurgy, which
Fig. 1. Schematic diagram of the tribopair and images of the rubbing pairs.
consisted of several steps, namely, mixing the alloy powders
(LBC3/Cu10Sn10Pb), spreading the mixture on a carbon steel belt
(Thickness 1 mm), sintering (850 1C, 15 min, ammonia decom-
position N2 þH2), roller compaction (Diameter 260 mm, double
roller, rolling reduction 20%), resintering (820 1C, 15 min, ammo-
nia decomposition N2 þH2), and roller re-compaction. The sheet is
cut into 32  32  3 mm square pieces. The surface roughness Ra
of the lower sample is 5 mm. The residual porosity of the copper
alloy layer is approximately 5%. Before the top sample is brought
in contact with the bottom sample, ten grams of loose graphite
powder are covered on the bottom sample evenly. These loose
powders are then compacted by the normal load, which is applied
along the vertical axis of the upper specimen. During the experi-
ments, the upper sample keeps rotated, whereas the lower
sample is fixed. Some powder inside the interface may leaked
out from the friction interface. Meanwhile, some of the powder
remains outside of contact occasionally drawn in the interface
along with the movement of the top sample. The average
diameter of graphite powder particles is 30 mm. The duration
time of every test is 10 min. The environment temperature is
25 1C, and the relative humidity is 75%. The sliding velocity, which
is calculated based on the middle line of the annular face, is from
0.2 to 0.8 m/s and the normal load is from 2.94 to 17.64 MPa. The
friction torque and normal load are obtained using two force
sensors, and the friction coefficient is calculated via conversion
based on the structural relationship. The sample temperature is
measured in real time using a thermocouple placed at the center
of the bottom sample. After the tests, the powder layers on the
surface of the bottom sample are observed using a digital camera,
an Olympus BH-20 optical microscope and a scanning electron
microscope (SEM, JSM-6490LV). The surface elements are ana-
lyzed using an energy dispersive X-ray spectrometer (EDS, JSM-
6490LV), which conducted the area measurement at the same
area observed under SEM. The roughness of the friction surface is
measured by a Talyor-Hobson-6.
3. Typical life cycle of the powder layer
3.1. Four distinct stages
Known from previous studies [34,35], the effects of the sliding
velocity and normal load on the lubrication characteristics and
powder layer formation are complicated and should be analyzed
according to the running conditions of a real application. In Fig. 2,
four regions have been divided to indicate the powder layer state
and friction characteristics according to variations of service
condition. It should be noted that no critical value indicated the
transition of each powder layer state. Instead, the transition from
one state to another was gradual and was related to real service
conditions. Region I is working under high velocity and light load.
The friction coefficient is 0.08–0.16 and the full powder layer
Fig. 2. State chart of powder lubrication corresponding to service conditions.
 W. Wang et al. / Wear 297 (2013) 841–848
(Fig. 3a) formed on the surface of the bottom sample. The top
sample slides on the powder layer rather than on the bare
substrate of the bottom sample, and shearing occurs in the
powder layer; hence, the direct contact of the tribopair is
prevented. The compact third body powder smoothed the original
surface whose roughness Ra reduced from 5 to 0.9 mm. The
friction coefficient in Region II is 0.15–0.21, and the temperature
is the lowest one due to its low velocity and light load. The
friction coefficient in Region III is 0.08–0.12, and the temperature
is the highest one due to its high velocity and heavy load. The
formation of the powder layer in Region II and Region III is
similar. The powder layer starts to deteriorate, and a small
portion of the powder layer may lose its adhesion to the bottom
sample. At first, the blistering or partial detachment of the
powder layer occasionally occurs (Fig. 3b). However, most of the
load is still carried by the powder layer and no direct surface
contact occurs. Then, serious damage to the powder layer may
occur, and a large portion of the powder layer begins to detach
from the bottom sample (Fig. 3c). Both the powder layer and the
contact surfaces carry the load at the same time. The speed
difference is accommodated not only via powder layer shearing
but also via sliding between the rubbing surfaces. The surface
roughness Ra in Regions II and III are varied from 0.2 to 0.6 mm,
which is rougher than that in Region I. It may attribute to the
smoothed asperity on the bottom surface. At the final stage
(Region IV), the friction coefficient is 0.08–0.21. Although the
powder layer is fully destructed, there are little residual powder
remaining in the valley of the surface at first (Fig. 3d). Meanwhile,
the surface roughness Ra is 0.8–0.9 mm. While the residual
powder exhausted, the metal-to-metal contact becomes the
Fig. 3. Typical life cycle of a powder layer: (a) full powder film; (b) partial detachment; (c) serious detachment; and (d) complete destruction.
843
primary behavior in the friction interface. The surface roughness
Ra increased to 5–6 mm while serious wear track was found.
Therefore, the heavier load tends to deteriorate the powder
layer, which is in accordance with common experience. However,
the effect of velocity is quite different, that higher velocity
prolongs the life of powder layer. It indicates that higher velocity
facilitates the powder to flow into the friction interface. Because
of the excellent lubricity of solid lubricant under extreme pres-
sure, the friction coefficient is low at high load while the powder
layer is badly broken. Therefore, the analysis of the powder layer
is difficult, and how to keep it in good state is a tough challenge.
The characteristics of the powder layer are the comprehensive
results under the effect of the running conditions, the physical
characteristics of the powder and sample surface design.
3.2. Element contents on the wear track
Fig. 4 shows the micro observation results on the frictional
surface by SEM. The element contents of the same zone as Fig. 4
are analyzed separately using EDS. Table 1 lists the weights and
atomic percentages of carbon, oxygen, copper, tin and lead.
Fig. 4(a) is the original surface of the bottom sample, which is
produced by powder metallurgy. The original surface has the
minimum carbon percentage and the maximum copper percen-
tage. During partial detachment, most of the frictional surface is
covered by graphite powder (Fig. 4b). Meanwhile, the weight
proportion of carbon on the surface is 60.71%, and that of copper
is 23.1%. Fig. 4(c) shows that the detachment of the powder layer
worsened during the serious detachment period, and the area
covered by the powder layer is smaller than that of the opposing
844 W. Wang et al. / Wear 297 (2013) 841–848

Fig. 4. SEM surface images: (a) original surface; (b) partial detachment; (c) serious detachment; and (d) complete destruction.

Table 1 compacted powder reduces the friction between the rubbing

Surface element analysis via EDS. surfaces. A powder layer starts to form between the two surfaces
as more powder enters the frictional interface. The full powder
Element Original Partial Serious Complete
surface detachment detachment destruction
layer is a fine, compacted, and shell-like layer, which separates
the bottom and top samples and prevents direct contact between
Wt% At% Wt% At% Wt% At% Wt% At% them. Meanwhile, the internal shearing of the powder layer and
the sliding between the powder layer and the top sample
C 1.18 5.16 60.71 84.90 37.31 69.74 14.36 42.92
accommodate the speed difference of the two surfaces. In
O 11.18 36.70 7.42 7.80 9.61 13.48 7.88 17.68
Cu 59.61 49.27 23.10 6.11 41.71 14.74 63.25 35.75 Fig. 5(a), the powder layer formed on the surface of bottom
Sn 9.33 4.13 2.66 0.38 4.81 0.91 7.89 2.39 sample is integrative and fully covers the substrate surface,
Pb 18.69 4.74 4.94 0.40 5.12 0.55 6.26 1.09 although obvious scratches and grooves are observed. Fig. 5(b)
shows the microscopic image of an edge of the powder layer. On
the left is the powder layer, and the right shows the original
copper substrate. EDS results show that the weight ratio of carbon surface of the bottom sample. The shell-like powder layer, which
is decreased to 37.31%, whereas that of copper is increased to prevents the direct contact between the rubbing surfaces, is
41.71%. When the powder layer is completely destroyed, the clearly observed from the edge. The thin, compacted powder
deformed copper covers most of the frictional area (Fig. 4d). The layer adheres well with the base material and can last a long time
weight ratio of carbon is decreased to 14.36%, whereas that of because of replenishment from the loose powder surrounding the
copper is increased to 63.25%. Therefore, SEM and EDS results tribopair.
confirmed that the tribological characteristics are closely related
to the state of the powder layer during powder lubrication. 4.2. Layer blistering
Meanwhile, the lubrication deterioration and the wear increase
are usually accompanied by the lack of powder in the friction As previously mentioned, the loose powder in the interface
interface. between the rotating top sample and the fixed bottom sample is
compacted to a thin shell-like layer. No adhesive treatment was
applied between the powder layer and the bottom sample in the
4. Typical micro phenomena experiments. Thus, the bond between the powder layer and the
bottom sample is weak. Meanwhile, the sliding between the top
4.1. Full powder layer sample and the powder layer mainly accommodates the speed
difference. However, the increase in shearing of the inner powder
As loose powder is introduced into the rubbing interface, the layer weakens the adhesion between the powder layer and the
powder fills the valleys of the rough surface during the early bottom sample when the running conditions are not optimal. A
stage. The powder in the valleys is then compacted under the portion of the shell-like layer detaches from the bottom sample,
pressure of the counterpart. Together with the asperities, these and a blister layer appears when the top sample is removed
powders begin to carry the load. More importantly, the (Fig. 6). In the current experiments, layer blistering occurred
 W. Wang et al. / Wear 297 (2013) 841–848 845

Fig. 5. Images of the full powder layer: (a) scratch traces on the full powder layer, and (b) an edge of the full powder layer.

Fig. 6. Layer blistering of the powder layer: (a) small blister at the edge; (b) large blister; and (c) cluster of blisters.

when the load exceeded 8.82 MPa or the velocity was lower than
0.4 m/s. The powder layer began to detach from the bottom
sample as the blisters multiplied (Fig. 6(b) and (c)). In general,
layer blistering is the first sign prior to powder layer detachment.
When layer blistering occurs, the direct contact between the
frictional surfaces is yet to occur. However, necessary actions
need to be taken to prevent the detachment of the powder layer.
4.3. Partial detachment
Partial detachment means that a portion of the powder layer
detaches from the bottom sample. When the state of the powder
layer transformed into the partial detachment, the surface of the
bottom sample opposes the region where the powder layer has
detached. Meanwhile, direct contact and friction between the
tribopair is ignorable, and the surface of the bottom sample
preserves its original state. Fig. 7 illustrates several typical forms
of partial detachment. Fig. 7(a) is the microscopic image of the
pitting detachment, showing that a few pits are scattered in a
small area. The obvious feature of the plough detachment
(Fig. 7b), which is another form of partial detachment, is the
direction of the groove, which coincides with the sliding direction
of the friction track. The mechanism for this phenomenon is that
some hard particles, either introduced from the outside or
resulting from the aggregation of loose powder under the effect
of the rotating top sample, plowed the powder layer. Fig. 7(c)
shows a large partial detachment of the powder layer at the
margin of the friction ring. This indicates that the powder layer
detached from the bottom surface, and blistering may have
formed prior to detachment.
4.4. Delamination
Delamination is another major form of powder layer detach-
ment, in which shearing occurs and delaminates the powder layer
into several sub-layers, which can be carried by the rotating top
sample or remain on the bottom sample separately. In Fig. 8(a),
although a large piece of the powder layer has detached from
846 W. Wang et al. / Wear 297 (2013) 841–848

Fig. 7. Partial detachment of the powder layer: (a) pitting detachment; (b) plowing detachment; and (c) partial detachment at the edge.

Fig. 8. Delamination of the powder layer: (a) integrative delamination; and (b) irregular delamination.

bottom sample, the powder layer remaining on the surface is
preserved as homogenous and integrative. Different from that
observed in Fig. 8(a), the remaining powder as shown in Fig. 8(b)
is irregularly distributed in the detachment area.
4.5. Scuffing
The steel and copper surfaces meet and rub against each other
when the powder layer is detached, eventually resulting in
scuffing. Scuffing is another typical form of powder layer damage
and is much worse than partial detachment or delamination.
Little powder exists in the friction interface, and it is difficult to
introduce more powder into the friction interface. At the early
stage of scuffing (Fig. 9a), the load carrying and shearing of the
powder layer in the frictional interface are the dominant beha-
vior. The frictional track on the copper surface is observed at the
area where the powder layer has detached, indicating that the
powder supply has become scarce. Moreover, the powder layer
remaining on the bottom sample consists of many pieces of the
smaller region scattered throughout the friction area. Obvious
cracks at the boundary of these scattered regions are observed. As
scuffing proceeds (Fig. 9b) direct contact between the friction
surfaces increases, resulting in a long scuffing trace or a large
scuffing area. At this stage, the contact surface area is close to the
area where powder remains. Moreover, they exert similar effects
on the friction characteristics and load carrying capacity. Serious
scuffing eventually occurs under severe service conditions
(Fig. 9c). Meanwhile, the dominant behavior in the friction inter-
face is the direct contact between the rubbing surfaces, and
powder is barely detected in the friction area. Therefore, severe
scuffing seriously damages the surface of the tribopair via scratching
and wearing.
5. Conclusions
This work conducted a series of experiments on loose powder
lubrication using a ring-on-flat tester. Utilizing optical micro-
scopy, SEM, and EDS, the state and micro phenomena of powder
layer are discovered. The typical life cycle of the powder layer
 W. Wang et al. / Wear 297 (2013) 841–848
Fig. 9. Scuffing of the friction surface: (a) light scuffing; (b) medium scuffing; and (c) serious scuffing.
consists of the full powder layer, partial detachment, serious
detachment, and complete destruction. No critical values are
available to indicate the state of the powder layer because the
transition is gradual. During the transition process, the changing
of the powder layer form, the surface element content, and the
friction surface roughness closely related to the typical transition
state. Due to higher velocity facilitated the powder to flow into
the friction interface, powder layer is better at high velocity while
load keep constant. Because of the excellent lubricity of solid
lubricant under extreme pressure, the friction coefficient is lower
at high load while the powder layer exhibits worse.
When bonding between the powder layer and the bottom
sample weakens, layer blistering and partial detachment occurs at
an earlier stage. Meanwhile, the powder layer stays in a good
state and lubricates the friction surface well. As the powder layer
further detaches, scuffing and serious detachment occur, indicat-
ing the onset of serious wearing. Scuffing during powder lubrica-
tion should be avoided. Micro damages, such as blistering,
delamination, and detachment, appear in every state, but the
quantity and degree of deterioration is different at every stage.
Acknowledgment
National Natural Science Foundation of China under Grant no.
51005067 and no. 51175136 financially supports the present
research.
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