Wear 238 Ž2000.

131–137
www.elsevier.comrlocaterwear

Enhanced wear resistance of titanium surfaces by a new thermal

oxidation treatment
H. Dong ) , T. Bell
School of Metallurgy and Materials, The UniÕersity of Birmingham, Birmingham, B15 2TT, UK
Received 29 July 1999; received in revised form 2 November 1999; accepted 2 November 1999

Abstract

The wear behaviour of thermal oxidation ŽTO.-treated as well as untreated Ti6Al4V alloy has been investigated using an Amsler
tribometer in rolling–sliding motion under boundary lubrication conditions. The results show that the TO treatment can significantly
enhance the wear resistance of Ti6Al4V alloy. Based on the experimental results, in conjunction with systematic analyses, the
wear-reduction mechanisms involved in the TO-treated material are discussed. It was found that the significantly reduced tendency to
adhesive wear and the improved wettability, which increases the effectiveness of lubrication, have contributed to the enhanced wear
resistance of the TO-treated material. q 2000 Elsevier Science S.A. All rights reserved.

Keywords: Ti6Al4V; Oxidation; Rolling–sliding; Wear

1. Introduction being understood. However, it appears that this may be

Titanium is the fourth most abundant structural metal in
the world, and titanium and titanium alloys have been
developed rapidly since the pure metal first became com-
mercially available about half a century ago. This is pri-
marily because of their combination of outstanding proper-
ties in terms of high strength to weight ratio, exceptional
resistance to corrosion, and excellent bio-compatibility.
These attractive properties of titanium alloys makes them
suitable for a wide range of applications, ranging from
aerospace through defence, chemical, petrochemical, ma-
rine and offshore. On the other hand, titanium alloys are
characterised by, especially in sliding situations, poor tri-
bological properties, including high and unstable friction
coefficients, severe adhesive wear, susceptibility to fretting
wear, and a strong tendency to seize w1–3x. Notwithstand-
ing the fact that the reputation of titanium and titanium
alloy for poor tribological characteristics has been well
documented, the mechanisms operating are still far from
)
Corresponding author. Tel.: q44-121-414-5197; fax: q44-121-414-
7373; e-mail: h.dong.20@bham.ac.uk
related to their electron configuration, crystal structure and
lubrication characteristics.
1.1. Electron configuration
Buckley and Miyoshi w4x correlated the chemical activ-
ity and the friction coefficient with the d-bond character
and found that the lesser the percentage of d-bond charac-
ter, the more active is the metal and the greater is the
friction. Since titanium possesses the lowest value of d-
bond character Ž27%., it is extremely active and ready to
alloy with other materials.
1.2. Crystal structure
Alpha titanium, although a hexagonal metal, has an
axial ratio cra of 1.588, which is less than the ideal for
closest packing Ž1.633., which tends to make the basal
plane less favourable for slip and allows prismatic  10 1 04
and the first-order pyramidal  10 1 14 slip to occur w5x, thus
increasing the number of possible slip systems. The in-
creased possible slip systems promotes continuous junction
growth, which requires slip on different slip planes w6x.

0043-1648r00r$ - see front matter q 2000 Elsevier Science S.A. All rights reserved.
PII: S 0 0 4 3 - 1 6 4 8 Ž 9 9 . 0 0 3 5 9 - 2
132 H. Dong, T. Bell r Wear 238 (2000) 131–137
Fig. 1. Materials factors affecting the tribological performance of tita-
nium.
1.3. Lubrication
It has been reported that all conventional lubricants
Žmineral oils and greases., which are successfully and
widely used for most metals, have been shown to be
ineffective when applied to titanium alloys w7x. Addition-
ally, the low heat conductive nature of titanium adds to the
problem of the ineffectiveness of lubricants. This is be-
lieved to partially account for the high tendency to scuff-
ing of titanium alloys w8x.
It can be seen from the above discussion that there are
many factors that affect the tribological properties of tita-
nium and its alloys. Although it is still open for debate as
to the dominant factor and relative importance of individ-
ual factors, it is the synergy of all these factors that
determines the tribological characteristics of titanium and
its alloys ŽFig. 1.. As a result, the use of titanium alloys
has generally been restricted to non-tribological applica-
tions. Clearly, the poor tribological characteristics of tita-
nium and its alloys are related to their inherent materials
nature. Consequently, this problem may be overcome only
by changing the nature of the surface, i.e., through surface
engineering. Surface engineering has proven to be the most
promising way to enhance the tribological performance of
titanium alloys w3,9,10x.
Recently, a novel surface engineering process based on
thermal oxidation ŽTO. has been successfully developed
w11x. Essentially, the TO technique is a thermochemical
process, which is usually carried out in a controlled atmo-
sphere containing oxygen as well as nitrogen at 600–6508C
for 50–100 h. Unlike some previous processes w12,13x, the
newly developed TO process can effectively harden tita-
nium alloys without causing scaling or surface damage.
Actually, the benefits conferred by the TO process can be
attributed to both the formation of a thin rutile oxide layer
Ž; 2 mm. and an oxygen diffusion zone Ž; 20 mm.. The
TO process has been successfully used for the surface
treatment of titanium components for off-shore and racing
car engine industry. However, the potential of the novel
TO process in enhancing the tribological properties of
titanium and its alloys cannot be fully realised until a
systematic characterisation is conducted, which forms the
theme of the present paper.
2. Experimental
2.1. Materials and surface treatment
Ti6Al4V supplied by Timet in the form of hot rolled
and annealed bar of 50-mm diameter was chosen as the
main experimental material. The nominal composition cor-
responds to the designation, Ti–6Al–4V. This material
was selected based on the consideration that Ti6Al4V is a
versatile titanium alloy with a combination of good proper-
ties and ease of production, and that there is ever increas-
ing interest in improving its tribological properties to meet
varying requirements arising from diverse application con-
ditions. Discs cut from 50-mm rod were used for tribotests.
Oxidising treatments were carried out in atmosphere con-
taining about 80% oxygen and 20% nitrogen at 6008C for
65 h. The typical cross-sectional microstructure of the
TO-treated material is shown in Fig. 2. The surface layers
in TO-treated samples, as with most thermochemically
treated materials, comprise a thin rutile oxide layer Ž; 2
mm. and an oxygen diffusion zone Ž; 20 mm. beneath.
The detailed characterisation results have been reported
elsewhere w14x. It can be clearly seen that the problem with
severe scaling, which some early work w15,16x experi-
enced, has been successfully addressed.
2.2. Wear tests
The wear tests under a combined rolling–sliding contact
were conducted on an Amsler Wear Test Machine Type
A135 with wheel-on-wheel configuration. During the test,
the lower specimen wheel was rotated against the upper
counterpart wheel. Both wheels had the same size and
geometry with a 48-mm outer diameter, and a 16-mm
inner diameter, and they were 10 mm in thickness. The
rotation speed of the lower specimen wheel and upper
counterpart wheel was 400 and 360 rpm, respectively.
Thus, the corresponding sliding ratio Ž Vl y Vu .rVl was
Fig. 2. SEM micrograph showing general microstructural characteristics
of TO-treated Ti6A14V alloy.
 H. Dong, T. Bell r Wear 238 (2000) 131–137 133

10%, where Vu and Vl are the cylindrical speed of the

upper and low wheel, respectively. The counterpart mate-
rial for the wear tests was 709M40 ŽEn19. with the
following nominal composition Žwt.%.: 0.36–0.44 C, 0.9–
1.2 Cr, 0.25–0.35 Mo and balance Fe ŽBS 970.. The
709M40 steel wheels were hardened and tempered to a
hardness of 600HV10.
The rolling–sliding wear tests were carried out under
lubricated conditions, at room temperature and with ambi-
ent humidity. The lubricating oil was SHELL’s 20r20 W
Rimula= oil. The minimum oil film thickness Ž h min . was
calculated to be 0.006–0.008 mm, and, thus, the ratio of
minimum oil film thickness to composite roughness Ž s . of
the friction pairs, l s h minrs, was found to be - 1,
indicating that tests were conducted under boundary lubri-
cation condition w8x. Fig. 4. SEM micrograph showing typical adhesive wear morphology
After each test period, the specimens were first ultra- observed on the tested surface of the untreated Ti6A14V wheel. ŽThe
direction of movement is indicated by the grooves..
sonically cleaned for 20 min and rinsed in acetone, then
dried and weighed using a balance accurate to 0.1 mg.
Care was taken to ensure that the wheels were put back in
the original arrangement after weighing such that the ŽFig. 4.. This mechanism was further verified by the
contact situation of the wheels would not be changed to surface morphology and corresponding composition analy-
any significant extent during each test. For each treatment ses using X-ray mapping of the counterpart. The pull-out
andror material, at least three tests were carried out and
the average results reported.

3. Results

The variation of weight loss with time for the TO-treated

and untreated Ti6Al4V, together with the 709M40 counter-
part running against the TO-treated wheel, is shown in Fig.
3. The untreated material was characterised by a very high
wear rate Ž2.76 = 10y3 mg my1 ., which may be associ-
ated with the preferential transfer of Ti6Al4V onto the
steel counterpart and the strong abrasive action of the
transferred material. After wear testing, the worn surfaces
were examined using a SEM, and they were found to be
very rough, with typical adhesive wear features evidenced
by numerous adhesive craters and deep ploughing grooves

Fig. 3. Weight loss in lubricated rolling–sliding wear tests for untreated
and TO-treated Ti6A14V wheels, together with the hardened steel coun-
terpart for comparison.
Fig. 5. SEM micrographs of Ža. the worn surface, and Žb. the correspond-
ing Ti K a X-ray mapping of steel counterpart wheel against untreated
Ti6A14V wheel specimen, showing the material transfer from the
Ti6A14V specimen to the steel counterpart. ŽThe direction of movement
is from top to bottom..
134 H. Dong, T. Bell r Wear 238 (2000) 131–137
Fig. 6. Weight loss vs. revolutions for TO-treated Ti6A14V wheel in oil
lubricated rolling–sliding wear tests under different loads.
material was transferred and smeared onto the surface of
the counterpart, as is evidenced in Fig. 5. It can be seen
that there are two distinct areas on the steel counterface
ŽFig. 5a.: one is rough Žarea A. and the other is relatively
smooth Žarea B.. Ti K a X-ray mapping ŽFig. 5b. indicated
that the rough area Ž A. was covered by the material
transferred from the Ti6Al4V testing wheel. Clearly, un-
treated titanium cannot be used rubbing condition even
with oil lubrication and a low sliding to rolling ratio.
As has been demonstrated in Fig. 3, the wear rate
Ž1.57 = 10y5 mg my1 . of the TO-treated specimen was
Fig. 7. SEM micrographs showing surface morphology of Ža. the as-TO-
treated material, and Žb. short-time Ž10 4 revolutions. tested TO-treated
material. ŽThe direction of movement is from top to bottom..
dramatically reduced by more than two orders of magni-
tude over the untreated material, and it was even lower
than that of the hardened 709M40 steel counterpart Ž1.61
= 10y4 mg my1 . by a factor of more than 10. This can be
understood by the fact that intermetallic contact Žin the
case of Ti against steel. was replaced by a steelrceramic
tribological pair.
The effect of applied load on the wear of the TO-treated
material is shown in Fig. 6. It appears that the success of
the TO treatment in improving the wear resistance of the
titanium alloy also varied with the loading conditions.
Under low stress Ž300 MPa. and intermediate stress Ž500
MPa. conditions, wear rates for the testing wheel were
low. However, when a higher load of 650 MPa was
applied, a much higher wear rate for the testing wheel was
observed. Careful examination of the worn surface of the
TO-treated specimen against a 709M40 counterpart, re-
vealed essential information regarding the wear mecha-
nism involved. Fig. 7a represents the morphology of the
cylindrical surface of the as-TO-treated material, showing
original parallel ridges which are believed to be associated
with original turning marks. As expected, the real contact
Fig. 8. SEM micrographs of the worn surface of TO-treated T16A14V
specimen, showing Ža. general wear morphology, and Žb. typical wear
feature. ŽThe direction of movement is from top to bottom..
 H. Dong, T. Bell r Wear 238 (2000) 131–137 135

Table 1
EDS analysis results
Positions in Fig. 11 Intensity Žcounts per 100 s.
O Fe Ti Al V
A 800 20 ) 3000 ) 3000 1950
B 320 640 ) 3000 2600 800
C 120 20 ) 3000 2800 2200

area was only a small portion of the nominal contact

surface area Žas shown in Fig. 7b.. The asperities in real
contact were plastically deformed and slightly worn due to
the rubbing of the counterpart, and darkened by the trans-
ferred steel from the counterpart.
A small amount of exfoliated surface oxide was ob-
served on the TO-treated wheel tested under 300 and 500
MPa, and the overall morphology is shown in Fig. 8a.
Detailed SEM examination ŽFig. 8b. assisted by EDS with
an ultra-thin window, demonstrated that these craters Ž‘C’
in Fig. 8b. were surrounded by a dark coloured area Ž‘B’.,
which yielded high Fe peaks in the EDS spectrum ŽTable
1.. It can also be deduced that exfoliation of the surface
oxide probably initiated at the interface between the sur-
face oxide and the diffusion zone.
The morphology of the worn surface of the high stressed
Ž650 MPa. TO-treated titanium wheel appears to differ
from those for the low and intermediate stressed TO-treated
wheels ŽFig. 9.. Firstly, it is obvious that in addition to
some small craters Žas observed in Fig. 8., large craters
were formed as a result of high stress loading. Secondly,
and perhaps more importantly, interfacial fatigue was Fig. 10. SEM micrographs showing Ža. interfacial fatigue origin and
clearly observed as is evidenced by the beach marks ŽFig. beach marks, and Žb. interfacial net cracking, as pointed.
10a., indicative of crack growth. Finally, embedded in the
bottom of a large crater, a net cracked region can also be
noted ŽFig. 10b., signalling that the subsurface cracks were
due presumably to the high contact stress. Thus, interfacial fatigue and subsurface cracking modes are proposed and
will be discussed in Section 4.

4. Discusssion

4.1. Wear characterisation of untreated material

As shown in Fig. 3, untreated Ti6Al4V is characterised

Fig. 9. SEM micrographs showing worn surface tested under a high
contact stress Ž650 MPa.. ŽThe direction of movement is from left to
right..
by a very high wear rate, which is in good agreement with
the morphology of the worn surfaces ŽFig. 4.. Adhesive
wear has obviously occurred with the untreated Ti6Al4V,
and the worn surface is very rough with deep ploughing
grooves and many craters. The observed high wear rate is
thought to be the result of the preferential transfer of
Ti6Al4V to the steel counterpart. This is confirmed by the
SEM observation ŽFig. 5., that more than half the steel
surface was covered with transferred titanium from the test
wheel. This can be understood by the fact that, as has been
discussed in Section 1, titanium and its alloys are chemi-
136 H. Dong, T. Bell r Wear 238 (2000) 131–137
cally active and have a high ductility, which gives rise to
the strong tendency to adhesion ŽFig. 1.. Therefore, the
adhesive strength of the junctions formed is usually much
higher than the strength of Ti6Al4V, and such junctions
will rupture within the weaker titanium asperities, which
accounts for the many craters on the worn surface of
untreated material. Moreover, the transferred titanium be-
comes work-hardened after the multiple contacts in the
wear couple, which in turn results in severe abrasive wear
damage to the titanium surface, as is demonstrated by the
deep abrasive grooves ŽFig. 4..
It is generally held that a thin oxide film always exists
on a titanium surface. However, under the test conditions
employed in the present investigation, no appreciable ben-
eficial contribution of such an oxide film could be identi-
fied. This is understandable in view of the thin and weak
nature of the air-formed oxide film w3x. When in contact
with another metal surface, under moderate or heavy loads,
such an oxide film is easily removed from the asperities,
leading to direct inter-metallic contact and, hence, severe
adhesive wear and scuffing. It can thus be concluded that
untreated Ti6Al4V cannot be used under rubbing condi-
tions, even with oil lubrication, and that to be effective for
protection against wear, an oxide film must have appropri-
ate cohesive strength, good adherence to the substrate, and
strong support from the substrate.
4.2. Wear mechanism of TO-treated material
The TO-treated material showed superior wear resis-
tance to the untreated material, which implies that the wear
mechanism of the TO-treated material should be different
from that of untreated material. Inspection of the worn
surfaces of the TO-treated material tested under 300 and
500 MPa has revealed some spots that are usually sur-
rounded by flat relatively dark areas. It is thus constructive
to systematically examine the worn surface further in order
to understand the formation of these morphological fea-
tures and, hence, the wear mechanisms operating. A typi-
cal spot morphology, as shown in Fig. 8b, consists of three
different areas Ž‘A’, ‘B’, and ‘C’.. Area ‘A’ represents the
as-TO-treated surface morphology, as is evidenced by the
original machine marks and the fine spherical oxide. The
corresponding EDS analysis has revealed a relatively high
oxygen peak ŽTable 1.. Area ‘B’ seems smoother and
darker than area ‘A’, and the corresponding EDS analysis,
in addition to Ti, Al, V, O peaks, showed high Fe peaks
ŽTable 1.. This implies that ‘B’ is the real contact area,
which was plastically deformed andror slightly worn by
the steel counterpart, and that steel was transferred onto it.
EDS analysis in area ‘ C’ revealed a much lower oxygen
peak than in either of areas ‘ A’ or ‘ B’ ŽTable 1.,
suggesting that flaking of the oxide has occurred in this
area.
Thus, for the low Ž300 MPa. and intermediate Ž500
MPa. stressed TO-treated Ti6Al4V wheel, the correspond-
ing wear mechanism can be proposed as follows. When the
TO-treated Ti6Al4V and hardened 709M40 wheels are in
contact under load, only a very small portion of the
nominal contacting area is really in contact. The asperities
in contact are plastically deformed or partially removed
due to the action of the counterpart. Preferential material
transfer from the steel counterpart to the TO-treated wheel
occurs at these real contact areas. With further preferential
material transfer, the true contact changes gradually from
steel against oxide to steel against steel, and the tangential
force acting on these junctions equivalently increases due
to the higher friction coefficient for steel against steel
compared with steel against oxide. At the same time, the
elastic energy in the transferred layer also builds up gradu-
ally. Eventually, these transferred agglomerates will be
detached under the combined action of the larger tangen-
tial force and high elastic energy w17x, thus forming wear
debris. While most detachment of the agglomerates took
place at the interface between the oxide and the transferred
layer, some occurred at the oxidersubstrate interface,
which eventually forms small craters observed on the
surface of the TO-treated Ti6Ai4V wheel.
From the transition in both the wear rate ŽFig. 6. and
the morphology of the worn surface of TO-treated titanium
wheels ŽFig. 8a vs. Fig. 9., it can be deduced that the wear
mechanism for the highly stressed TO-treated TI6Al4V
wheel is different from the low or intermediately stressed
TO-treated TI6Al4V wheels. Large craters were observed
on the surface of the highly stressed TO-treated TI6Al4V
wheel. Beach marks Žas shown in Fig. 10a., which are
indicative of fatigue crack growth, were observed in most
craters. Thus, from a contact mechanics and fatigue theory
viewpoint, such debonding is thought to be an interfacial
fatigue controlled failure process. This is because the shear
stress at the interface is essentially an alternating stress and
every cycle of the test wheel will impose this stress along
the interface since the contact region moves with time as
the test wheel rotates. Therefore, as in conventional fa-
tigue, cyclical stressing may lead to interfacial fatigue in
layered surface systems. Based on this interfacial fatigue
approach, a wear mechanism can be proposed as follows.
Voids or micro-cracks form in the oxiderdiffusion zone
interface due to the alternating shear stress at the interface.
Further cyclical stressing leads to the propagation of mi-
crocracks along the interface. Finally, debonded regions
will detach under the action of large tangential forces.
Alternatively, fatigue cracks may initiate at the existing
defects such as voids or subsurface cracking ŽFig. 10b.. A
similar failure model has been observed by He et al. w18x in
studies of the rolling wear of TiN coated steel.
4.3. Tribological enhancing mechanism
The TO-treated material has shown significant improve-
ment in wear resistance, representing two orders of magni-
tude in reduction in wear rate compared with untreated
 H. Dong, T. Bell r Wear 238 (2000) 131–137
material. Although there may be many factors that have
contributed to the significantly enhanced wear resistance, it
is believed that this is closely related to the tough, adherent
rutile oxide film formed on the TO-treated surface. Ac-
cordingly, the main enhancing mechanisms are likely to be
two-fold.
Firstly, as discussed in Section 4.1, titanium has a
strong tendency to severe adhesive wear when it is in
contact with a steel surface. According to the adhesive
theory of wear w8x, the adhesion of contact surfaces is
related to their metallurgical compatibility and deformation
behaviour. Therefore, adhesive wear should be effectively
eliminated for the TO-treated surface as a consequence of
the nature of the ceramicrmetal contact. The adhesion is
expected to be fairly low in view of the fact that the
metallurgical compatibility between the oxide and steel
surfaces is much lower than that between the untreated
titanium and steel surfaces. Thus, the TO-treated material
might be expected to exhibit quite a low adhesive tendency
owing to the significantly reduced metallurgical compati-
bility. Meanwhile, it has been reported that w14x the rutile
oxide layer formed during the TO treatment has a much
lower modulus Ž E . to hardness Ž H . ratio than that for the
untreated material Ž ErH: 13.8 vs. 26.9.. This significantly
reduced ErH ratio can promote elastic deformation and a
reduction in adhesion wear rate can be anticipated w19x.
Secondly, it is known that for a given tribosystem under
boundary lubrication conditions, the boundary lubricating
effect is to a large extent, associated with the wettability of
the surfaces in contact to the lubricant. Researches have
shown that the wettability of a surface to a given lubricant
is closely related to the degree of ionic character of the
surface w20x, with wettability increasing with increasing
ionic character. As expected, the TiO 2 rutile oxide formed
during the TO treatment possessed much higher wettability
than titanium surface since it has higher ionic character
w21x. In the case of titanium alloys, the oxide film formed
at room temperature in air is thin and weak. Thus, the
oxide film is easily removed from the asperities when in
contact with another metal surface under moderate or
heavy loads owing to severe plastic deformation in the
substrate and thus fracture of the oxide. The removal of the
passive oxide surface layer exposes the underlying bare
titanium, which has very low wettability.
5. Conclusions
Ž1. Untreated Ti6Al4V cannot be used under rubbing
conditions, even with oil lubrication because of its strong
tendency to severe adhesive wear and ineffectiveness of
conventional mineral oils for protection against roll–slid-
ing wear.
Ž2. The TO-treated material has shown a significant
improvement in wear resistance in sliding–rolling contact
137
with a steel surface under boundary lubrication conditions,
representing two orders of magnitude in reduction in wear
rate compared with untreated material.
Ž3. Th improved roll–sliding wear resistance of the
TO-treated material can be attributed to the tough, adher-
ent rutile oxide film formed on the treated surface during
the TO treatment. This rutile oxide layer can effectively
eliminate adhesive action and enhance boundary lubrica-
tion, thus giving rise to low wear rate.
Acknowledgements
The authors wish to acknowledge DTIrEPSRC for its
support of the LINK project ‘Advanced surface engineer-
ing of titanium alloy components ŽAdSurfEngTi.’. We
would also like to extend many thanks to all the partners
involved in the LINK project, specifically to our former
colleague, Dr. A. Bloyce Žnow with Balzers, Tilbrook,
UK. for his help and valuable discussion.
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