395

On the tribo-cryogenic characteristics of titanium alloys

N S M El-Tayeb∗ , T C Yap, and P V Brevern
Faculty of Engineering and Technology, Multimedia University, Melaka, Malaysia

The manuscript was received on 7 August 2009 and was accepted after revision for publication on 25 November 2009.
DOI: 10.1243/13506501JET703

Abstract: Friction and wear behaviours of Ti-6Al-4V (Ti64) and Ti-5Al-4V-0.6Mo-0.4Fe (Ti54)
alloys sliding against a tungsten carbide wheel under dry and cryogenic sliding conditions were
investigated at different sliding speeds, loads, and distances. Mathematical models utilizing
response surface methodology were developed as a function of sliding conditions for predict-
ing the friction and wear characteristics of both titanium alloys. The controlling variables were
determined by utilizing design of experiments. The developed models are able to predict the mea-
sured friction coefficient and wear volume with reasonable degree of accuracy for both titanium
alloys within the ranges of studied parameters.
Results showed no substantial difference between tribo-characteristics of both titanium alloys.
Under cryogenic sliding condition, tribo-characteristics were lower than those obtained under
dry sliding, except at higher load, cryogenic sliding surprisingly gave higher friction coefficient.
Analyses of worn surfaces and wear debris by using scanning electron microscopy and energy-
dispersive spectroscopy revealed that the role of cryogenic conditions at the sliding interface was
partially attributed to changing material properties and possible hydrodynamic effect. Under dry
sliding, the main wear modes were adhesion and delamination, while under cryogenic sliding, in
addition to delamination, abrasion wear mode dominated.

Keywords: friction coefficient, wear volume, titanium alloys, cryogenic sliding, response surface
methodology

1 INTRODUCTION of titanium alloys, and positive results of tool wear

Titanium and its alloys are well known by their
lightweight, high strength, corrosion resistance, and
biocompatibility [1–3]. They are widely used in many
applications, such as aeronautical, military [1, 2], bio-
material for joint replacement and dental appliances
[3, 4], and many other applications [5]. However, in
sliding applications, titanium alloys have poor tribo-
logical properties. Low thermal conductivity of tita-
nium alloys is one of the main reasons that was
reported earlier [1, 2] for poor machinability of these
alloys. This causes the temperatures in the cutting tool
and work piece to rise dramatically during machining,
resulting in short life of the cutting tool (tool wear)
and poor quality of the machined surface. Therefore,
cryogenic fluid such as liquid nitrogen was used to
replace conventional cutting fluid in the machining
∗ Corresponding author: Faculty of Engineering and Technology,
Multimedia University, Jalan Ayer Keroh, Melaka 75450, Malaysia.
email: nabil.eltayeb@mmu.edu.my; nabil.eltayeb@gmail.com
JET703
and surface finishes were obtained [6–10]. The mech-
anism of cryogenic sliding can be understood better
through tribological tests. However, work on cryogenic
friction and wear of titanium alloys is very rare in
the literature. The nearest work available in the liter-
ature is the friction and wear of high-purity titanium
studied by Basu et al. [11]. They found that friction
and wear of high-purity titanium decreased when slid
against steel in liquid nitrogen. Other researchers from
German’s Federal Institute for Materials Research and
Testing (BAM) studied the tribological behaviours of
various material pairs using special designed cryo-
tribometers and investigated the wear and friction of
several pairs of material at room temperature and low
temperature [12]. They reported that the tribologi-
cal behaviour of steel–steel and TiN coating–steel are
unchanged at 77 K but the wear and friction behaviour
of polymers against steel changed completely at low
temperature; that is the wear decreased from room
temperature to 77 K. Similar results were reported by
Theiler et al. [13] for PTFE against steel at room tem-
perature, in liquid nitrogen (77 K) and in liquid helium
Proc. IMechE Vol. 224 Part J: J. Engineering Tribology
396 N S M El-Tayeb, T C Yap, and P V Brevern
(4.2 K). Beside this, Hübner et al. [14] and Pinto et al.
[15] reported that at extreme low temperature (4–
20 K), the austenite in stainless steel and steel were
transformed into martensitic resulting in both stain-
less steel and steel to be more brittle. As a result, the
harder steels became more wear resistant. Ukraine’s
researchers [16, 17] found that friction coefficient for
non-metal material–steel and steel–steel decreased
at low temperature. They also found that some hard
and superhard diamond-like carbon (DLC) coating
gave higher friction coefficient in low temperature. In
another work reported by Chevalier et al. [18], the fric-
tion of steel against steel at the supercool condition
was found to be less than the friction in the ambient
condition, but the results were not stable.
The above review indicated that there was a strong
potential of introducing cryogenic fluid at the inter-
face to control the tribological behaviour of sliding
surfaces. Thus further work is therefore needed to
understand the tribo-cryogenic behaviour of these
alloys in order to better rationalize the use of the cryo-
genic condition. Moreover, most of the literature has
conducted investigation using one-factor-at-a-time. If
these factors were varied in an orderly way, even over
a narrow range [19, 20], a more complete picture of
the friction and wear behaviour of the titanium alloys
could be obtained. Therefore, in the current research,
cryogenic tribotests based on design of experiment are
conducted using a cryogenic tribometer based on pin-
on-disc configuration. The titanium alloys (pins) are
tested against a tungsten carbide wheel (disc) under
dry and cryogenic conditions. The alloys studied are
conventional Ti-6Al-4V alloy (Ti64) and a new titanium
alloy Ti-5Al-4V-0.6Mo-0 4Fe (Ti54) that was developed
and provided by Titanium Metals Inc (TIMET), USA.
Response surface methodology (RSM) was utilized to
produce a set of empirical expressions for friction coef-
ficient as well as wear volume for both titanium alloys
as a function of applied load, sliding velocity, and
sliding distance (time) at cryogenic conditions. The
wear mechanisms of worn surface and wear debris
were analysed by using scanning electron microscopy
(SEM) and energy-dispersive spectroscopy (EDS).
2 EXPERIMENTAL WORK
2.1 Tested materials
Titanium alloys are classified into three main groups
based on the basic metallurgical characteristics: α
alloys and near α alloys, α–β alloys, and β alloys.
Table 1 Chemical composition of Ti64 and Ti54 alloys [19]
Alloy Al V Mo Fe
Ti-6Al-4V 5.5–6.75 3.5–4.5 – 0.40 maximum
Ti-5Al-4V-0.6Mo-0.4Fe 4.5–5.5 3.0–5.0 0.4–1.0 0.2–0.8
Proc. IMechE Vol. 224 Part J: J. Engineering Tribology
α alloys and near α alloys contain α stabilizers and have
excellent tensile properties and creep stability at room
and elevated temperatures up to 300 ◦ C. α–β alloys
contain α and β stabilizers and they have microstruc-
ture of α- and β-phase. They can be heat treated to high
strength levels. β alloys contain significant quantities
of β stabilizers and are characterized by high harden-
ability, improved forgeability, and cold formability, as
well as high density [2].
In this work, two types of titanium alloys (con-
ventional Ti-6Al-4V alloy and newly developed alloy)
are tested at room and cryogenic environments. The
first is the conventional Ti-6Al-4V alloy, which covers
about 45–60 per cent of the total world production of
titanium alloys [2]. The second is a newly developed
Ti-5Al-4V-0.6Mo-0 4Fe alloy, which was supplied by
Titanium Metals Inc (TIMET), USA. These alloys will
subsequently be referred to as Ti64 and Ti54. Details of
the chemical composition and material properties are
given in Tables 1 and 2 [19] and their microstructures
are shown in Figs 1(a) and (b), respectively. The typical
α- and β-phase grain structure can readily be iden-
tified on the etched cross-sections of titanium alloys
Ti54 and Ti64, respectively. As can be seen, Ti54 has
finer grain size and is dominated by the α-phase.
2.2 Tribotest and procedure
Dry and cryogenic tribological experiments were car-
ried out using a tribometer based on block-on-ring
arrangement [19]. Dry tests were carried out at ambi-
ent temperature (Fig. 2(a)), whereas cryogenic tests
were conducted in low temperature under cryogenic
jet condition using liquid nitrogen (LN2 ), as shown
in Fig. 2(b). Titanium alloys (Ti64 and Ti54) in the
form of blocks (5 mm × 5 mm × 20 mm were rubbed
against a tungsten carbide counterface (25 mm diam-
eter and 9 mm thickness) [19].
During cryogenic tribotests, LN2 was directed to the
interface between the titanium pin and the circumfer-
ence of the counterface ring using a nozzle, as shown
in Fig. 2(b). LN2 was selected as the cryogen in this
study because it is safer to use and it offers higher
cooling effect compared to carbon dioxide. The fric-
tion forces at the interface between the titanium pin
and the carbide counterface were measured by using
a load cell attached to the load lever; then friction
coefficient was determined and averaged over each
test interval. Before and after each test, the weight
differences were determined by using a digital scale
(Setra EL-410S) with 0.001 g resolution. In this study,
C O N Ti
0.08 maximum 0.20 maximum 0.05 maximum Balance
0.1 maximum 0.2 maximum 0.03 maximum Balance
JET703
 On the tribo-cryogenic characteristics of titanium alloys 397

Table 2 Properties of titanium alloys [19] of factors (k = 3, that is normal load, N; sliding veloc-
ity, m/s; and sliding distance, m) and p refers to the
Titanium alloys Ti64 Ti54
number of levels. From the literature [21–24, 26, 27],
Phase α+β α+β the second-order model can lead to a reasonable
Density (g/cm3 ) 4.42 4.44 approximation of the response. Besides, a second-
Ultimate tensile strength (MPa) 965 NA
Thermal conductivity (W/m K) 6.6 at 20 ◦ C 6.96 at 25 ◦ C order model was able to predict coefficient of friction
Specific heat (J/g K) 0.580 at 20 ◦ C 0.54 at 25 ◦ C (COF) and wear rate of PCTFE/A12024 under LN2 as
Young’s modulus (GPa) 107–122 NA a function of pressure and sliding speed [21]. Thus,
Shear modulus (GPa) 41–45 NA
for the present work, a second-order polynomial rela-
tionship between the responses (tribo-characteristics)
(a) (b) and the independent variables (load, speed, and dis-
β tance) was selected and expressed in a general form
α
[20] as

α 
k 
k 
k−1 
k

β y = β0 + βi x i + βii xi2 + βij xi xj+ε

i−1 i=1 i=1 j=1

for i < j (1)

Fig. 1 (a) Microstructure of Ti54 and (b) microstructure
of Ti64 where k is the number of input factors; x1 , x2 , . . . , xk
are the input variables that influence the response y.
(a) (b) βo , βi (i = 1, 2, . . . , k) and βij (i = 1, 2, . . . , k, j = 1, 2,
. . . , k) are the unknown regression coefficients or
parameters to be estimated by using the method of
least squares.
1. ε are experimentally random errors.
Dry test Cryogenic test
The performance of the model depends on a large
number of factors that can act and interact in a com-
Fig. 2 Tribometer set-up plex manner. The matrix approach was adopted to
solve equation (1) in which y is defined as (kx1) vector
Table 3 Levels of independent variables for experiment observation, x is a (kxp) matrix of independent vari-
ables, β is a (px1) vector of parameters to be estimated,
Level and ε is an (nx1) vector of errors. In compact vector–
Lowest Low Centre High Highest matrix notation, the equation for a polynomial least
Variable −1.682 −1 0 1 1.682 square fit equation (1) is given by
x1 , speed (m/s) 0.1295 0.3 0.55 0.8 0.9705
x2 , load (N) 6.464 9.81 14.715 19.62 22.956 y = βx + ε (2)
x3 , time (min) 2.636 4 6 8 9.364

and the solution can be found from

the tribotests were conducted for three independent
variables at five levels (Table 3) [19], that is normal
loads (6.4–22.96 N), sliding speed (0.1295–0.971 m/s),
and sliding time (2.64–9.36 min).
3 RESPONSE SURFACE METHODOLOGY
3.1 Mathematical models for friction and wear
RSM is commonly applied in situations where several
input variables potentially influence the response of
interest and it has been used by many researchers for
modelling and predicting friction and wear proper-
ties of materials other than titanium alloys [21–24],
abrasive wear analysis [25, 26], tool life [27], surface
roughness [27, 28], and so on.
In the current work, a factorial design of experiment
of the type pk was used [19]. ‘k’ refers to the number
b = (xT x)−1 xT y (3)
where x T is the transpose of matrix x and (x T x)−1 is
the inverse of (x T x). The regression coefficients were
calculated by using MATLAB software, and the lack of
fit and the degree of significance of the models were
tested by using analysis of variance (ANOVA).
3.2 Experimental design and coding of variables
A central composite design (CCD) with nc = 3 centre
runs and α = 1.682 was used to describe the response
surface of the response (wear volume or friction coef-
ficient). The factorial portion is a complete 2k factorial
design with factor levels coded by −1 and +1. The axial
portion (the star points) is points located on the coor-
dinate axes of the factorial portion at a distance α from

JET703 Proc. IMechE Vol. 224 Part J: J. Engineering Tribology

398 N S M El-Tayeb, T C Yap, and P V Brevern

the design centre. The centre point is given for a num- 4 RESULTS AND DISCUSSION
ber, n0 , of repetition runs conducted for the condition
in (0, 0, 0). Table 4 shows the design matrix and the The experimental results of friction coefficient and
experimental results for both alloys in dry (D) and wear volume for both titanium alloys sliding under
cryogenics (C) conditions. The experiment included dry and cryogenic conditions are given in the design
three independent variables with five levels as pre- matrix shown in Table 4.
sented in Table 3. The five levels are coded according
to the transforming equation (4)
4.1 Models of friction coefficient and wear volume
speed − 0.55 load − 14.715
S = x1 = , L = x2 = , A total of 17 experiments were conducted according to
0.25 4.095
Table 4, and regression coefficients were calculated.
time − 6 By substituting these coefficients into equation (1),
T = x3 = (4)
2 four models for average friction coefficients and other

Table 4 Matrix of experiments with friction coefficients and wear volume for CCD

Independent variables Measured responses

Speed Load Time Average COF Wear volume (mm3 )
x1 x2 x3 Ti64D∗ Ti64C∗ Ti54D∗ Ti54C∗ Ti64D∗ Ti64C∗ Ti54D∗ Ti54C∗

1 1 1 1 0.6149 0.5814 0.4849 0.5898 3.7707 2.5641 3.3784 2.7027

2 1 −1 1 0.5432 0.4513 0.4847 0.5098 1.6591 1.5837 2.2523 2.0270
3 1 1 −1 0.5948 0.4367 0.5647 0.5797 2.2624 1.5083 1.6517 1.2763
4 1 −1 −1 0.5265 0.4062 0.5566 0.4663 0.9050 0.6033 0.8258 0.6006
5 −1 1 1 0.6023 0.4852 0.5270 0.4727 2.1870 1.3575 2.0270 1.1261
6 −1 −1 1 0.4764 0.2925 0.4764 0.2507 2.4887 1.1312 1.3514 1.5015
7 −1 1 −1 0.5948 0.3840 0.5421 0.3990 1.1312 0.6787 0.9760 0.4505
8 −1 −1 −1 0.4513 0.4513 0.4964 0.3159 0.6787 0.4525 0.7508 0.4505
9 1.682 0 0 0.5587 0.5945 0.5731 0.5229 2.3379 2.2624 2.4775 1.9520
10 −1.682 0 0 0.5516 0.4298 0.5158 0.4871 0.7542 0.4525 0.7508 0.8258
11 0 1.682 0 0.5556 0.5923 0.5464 0.6061 2.2624 1.8100 2.4775 2.1772
12 0 −1.682 0 0.4566 0.4566 0.4566 0.4566 0.8296 0.8296 1.1261 0.6757
13 0 0 1.682 0.5731 0.5444 0.6160 0.3486 2.4887 1.7345 2.4775 2.1772
14 0 0 −1.682 0.5014 0.5014 0.5892 0.4764 0.6787 0.8296 0.7508 0.6757
15 0 0 0 0.5659 0.5945 0.5802 0.4155 1.7345 1.3575 1.5015 1.2012
16 0 0 0 0.5945 0.4155 0.5731 0.4513 1.7345 1.5083 1.8018 1.5015
17 0 0 0 0.5516 0.4943 0.6017 0.5014 1.7345 1.5837 1.7267 1.3514
∗ D for dry and C for cryogenic. The response y denotes the coefficient of friction COF.
Referring to sliding speed x1 ⇒ S, normal load x2 ⇒ L, and sliding time x3 ⇒ T .

Table 5 Predicted friction coefficients equations (5) to (8) and wear volume equations (9) to (12)

Independent variables Predicted responses

Speed Load Time Average COF Wear volume (mm3 )
x1 x2 x3 Ti64D∗ Ti64C∗ Ti54D∗ Ti54C∗ Ti64D∗ Ti64C∗ Ti54D∗ Ti54C∗

1 1 1 1 0.5969 0.6425 0.5218 0.5323 3.4798 2.6060 3.4467 2.7773

2 1 −1 1 0.5413 0.4683 0.5072 0.4241 1.7672 1.6452 2.2457 1.9267
3 1 1 −1 0.5645 0.4607 0.5726 0.5171 2.4338 1.6978 1.7549 1.5491
4 1 −1 −1 0.5161 0.4665 0.5564 0.4617 0.7212 0.7746 0.9291 0.5109
5 −1 1 1 0.6039 0.4929 0.5518 0.4327 2.1018 1.2460 1.9435 1.3361
6 −1 −1 1 0.4835 0.3363 0.4932 0.2685 2.0484 1.0016 1.2681 1.3487
7 −1 1 −1 0.5735 0.4347 0.5442 0.4399 0.7542 0.6770 1.0025 0.6711
8 −1 −1 −1 0.4603 0.4581 0.4840 0.3285 0.7008 0.4702 0.7023 0.4961
9 1.682 0 0 0.5868 0.5309 0.5449 0.5823 2.3241 2.0150 2.3274 1.9161
10 −1.682 0 0 0.5458 0.3980 0.5092 0.3865 1.1481 0.6153 0.8725 0.6916
11 0 1.682 0 0.5884 0.5400 0.5160 0.4984 2.4787 1.7685 2.4190 1.7727
12 0 −1.682 0 0.4463 0.4132 0.4528 0.3137 0.9935 0.7865 1.1565 0.9102
13 0 0 1.682 0.5718 0.5004 0.5678 0.3731 2.7805 1.8452 2.5493 2.2165
14 0 0 −1.682 0.5251 0.4500 0.6028 0.4108 0.7675 0.6345 0.6506 0.4665
15 0 0 0 0.5694 0.5069 0.5870 0.4581 1.7129 1.4880 1.6783 1.3610
16 0 0 0 0.5694 0.5069 0.5870 0.4581 1.7129 1.4880 1.6783 1.3610
17 0 0 0 0.5694 0.5069 0.5870 0.4581 1.7129 1.4880 1.6783 1.3610
∗ D for dry and C for cryogenic.

Proc. IMechE Vol. 224 Part J: J. Engineering Tribology JET703

 On the tribo-cryogenic characteristics of titanium alloys 399

four models for wear volumes of Ti64 and Ti54 for μC64 = 0.5069 + 0.0395S + 0.0377L + 0.015T
each sliding condition, that is for dry and cryogenic
− 0.015S 2 − 0.0107L 2 − 0.0122T 2
condition, were obtained as
+ 0.0044SL + 0.0309ST + 0.045LT (6)
(a) friction models for Ti64 alloy under dry and cryo-
genic sliding conditions are given as
(b) friction models for Ti54 alloy under dry and cryo-
genic sliding conditions are given as
μD64 = 0.5694 + 0.0122S + 0.0422L + 0.0139T
− 0.0011S 2 − 0.0184L 2 − 0.0074T 2 μD54 = 0.5870 + 0.0106S + 0.0187L − 0.0104T
− 0.0162SL + 0.0005ST + 0.0018LT (5) − 0.0212S 2 − 0.0363L 2 − 0.0006T 2
− 0.0110SL − 0.0146ST − 0.0004LT (7)

(a) Normal Probability Plot (a) Normal Probability Plot

(response is Fric 64Dry)
(response is wear 64D)
99 99

95 95
90 90
80 80
70 70
Percent

60
50 Pe r c e n t 60
40 50
30 40
30
20
20
10
5 10
5
1
-0.05 -0.04 -0.03 -0.02 -0.01 0.00 0.01 0.02 0.03 0.04 1
Residual -0.50 -0.25 0.00 0.25 0.50
Residual
Versus Order
(b)
Versus Order (b) (response is wear 64D)
(response is Fric 64Dry)
0.03 0.5

0.4
0.02
0.3
0.01
0.2
Residual

0.00
Re s id u a l

0.1

-0.01 0.0

-0.1
-0.02
-0.2
-0.03
-0.3
-0.04 -0.4
2 4 6 8 10 12 14 16
Observation Order 2 4 6 8 10 12 14 16
Observation Order

Versus Fits
Versus Fits (c) (response is wear 64D)
(c) (response is Fric 64Dry)
0.5
0.03
0.4
0.02 0.3

0.01 0.2
Re s id u a l

0.1
Re s id u a l

0.00
0.0
-0.01
-0.1
-0.02
-0.2
-0.03 -0.3

-0.04 -0.4
0.450 0.475 0.500 0.525 0.550 0.575 0.600 1.0 1.5 2.0 2.5 3.0 3.5
Fitted Value Fitted Value

Fig. 3 Residuals analysis of the friction model for Ti64D: Fig. 4 Residuals analysis of the wear model for Ti64D:
(a) normal probability plots of residuals (equation (a) normal probability plots of residuals (equation
(5)), (b) residuals against the observed order of (9)), (b) residuals against the observed order of
data, and (c) residuals against the fitted values data, and (c) residuals against the fitted values

JET703 Proc. IMechE Vol. 224 Part J: J. Engineering Tribology

400 N S M El-Tayeb, T C Yap, and P V Brevern
μC54 = 0.4581 + 0.0582S + 0.0549L − 0.0112T
+ 0.0092S 2 − 0.0185L 2 − 0.0235T 2
− 0.014SL + 0.0056ST + 0.0132LT (8)
(c) wear models for Ti64 alloy under dry and cryogenic
sliding conditions are given as
WV 64D = 1.7129 + 0.3496S + 0.4415L + 0.5984T
+ 0.0082S 2 + 0.0082L 2 + 0.0216T 2
+ 0.4148SL − 0.0754ST (9)
Fig. 5 Residuals analysis on the developed cryogenic
friction model of Ti64 (equation (6)): (a) normal
probability plots of residuals, (b) residuals against
the observed order of data, and (c) residuals
against the fitted values
Proc. IMechE Vol. 224 Part J: J. Engineering Tribology
WV 64C = 1.488 + 0.4161S + 0.2919L + 0.3599T
− 0.0611S 2 − 0.0744L 2 − 0.0877T 2
+ 0.1791SL + 0.0848ST + 0.0094LT
(10)
(d) wear models for Ti54 alloy under dry and cryogenic
sliding conditions are given as
WV 54D = 1.6783 + 0.4325S + 0.3753L + 0.5644T
− 0.0277S 2 + 0.0387L 2 − 0.0277T 2
+ 0.1314SL + 0.1877ST + 0.0938LT
(11)
Fig. 6 Residuals analysis on the developed dry friction
model of Ti54 (equation (7)): (a) normal proba-
bility plots of residuals, (b) residuals against the
observed order of data, and (c) residuals against
the fitted values
JET703
 On the tribo-cryogenic characteristics of titanium alloys
WV 54C = 1.361 + 0.364S + 0.2564L + 0.5202T
− 0.0202S 2 − 0.0069L 2 − 0.0069T 2
+ 0.2158SL + 0.1408ST − 0.0469LT
(12)
The regression coefficients indicate the significant
effects of the different variables on the test results [29].
The higher the regression coefficient, the higher the
effect of the variable. It can be noted from equations
(5) to (8) that the applied load plays an important
Fig. 7 Residuals analysis on the developed cryogenic
friction model of Ti54 (equation (8)): (a) normal
probability plots of residuals, (b) residuals against
the observed order of data, and (c) residuals
against the fitted values
JET703
401
role in controlling the friction coefficient under dry
condition while sliding speed dominates cryogenic
sliding behaviour. Meanwhile, sliding distance (sliding
time) is less effective in controlling friction coeffi-
cient compared to the other parameters. Regarding
the wear models (equations (9) to (12)), the regression
coefficients suggest that sliding time is strongly influ-
enced by wear volume for all cases except Ti64 cryo-
genic and the quadratic effect of all variables is not that
significant compared to the effect of a single variable.
(a)
(b)
(c)
Fig. 8 Residuals analysis on the developed cryogenic
wear model of Ti64 (equation (10)): (a) normal
probability plots of residuals, (b) residuals against
the observed order of data, and (c) residuals
against the fitted values
Proc. IMechE Vol. 224 Part J: J. Engineering Tribology
402 N S M El-Tayeb, T C Yap, and P V Brevern
Also, the combined effect of speed and load is highly
contributed to the wear volume. The predicted values
of friction coefficients (produced by equations (5) to
(8)) and wear volume (produced by equations (9) to
(12)) are given in Table 5.
4.2 Diagnostic analysis on the developed models
Residual defines the difference between the exper-
imental values and the predicted values. Residual
Fig. 9 Residuals analysis on the developed dry wear
model of Ti54 (equation (11)): (a) normal prob-
ability plots of residuals, (b) residuals against the
observed order of data, and (c) residuals against
the fitted values
Proc. IMechE Vol. 224 Part J: J. Engineering Tribology
analysis has been applied to the models (equations
(5) to (12)). The normal probabilities of residuals for
equation (5) are shown in Fig. 3(a). In this figure,
spreading the data along the straight line indicates that
the data are normally distributed. Moreover, Fig. 3(b)
shows that the residuals are distributed in both pos-
itive and negative sides for all tests, which indicates
that the residuals are independent of runs. Figure 3(c)
shows that the residuals range between 0.03 and
−0.035. This plot indicates that the fitted model is
adequate and other than this, no obvious pattern was
Fig. 10 Residuals analysis on the developed cryogenic
wear model of Ti54 (equation (12)): (a) nor-
mal probability plots of residuals, (b) residuals
against the observed order of data, and (c)
residuals against the fitted values
JET703
 On the tribo-cryogenic characteristics of titanium alloys 403

observed. Residual analysis for the wear model for Ti64 be relatively higher and this should reduce the shear
under dry sliding (equation (9)) is shown in Fig. 4 and strength, leading to lower friction [30–32], but this is
the same analyses were also repeated for equations (6) unlikely the case in the current results. In Fig. 11(a), dry
to (12) (see Figs 5 to 10). sliding of titanium alloys against tungsten carbide for
6 min increases the interface temperature and causes
softening effect. However, under cryogenic sliding, the
heat is neutralized by the liquid nitrogen jet and main-
4.3 Results of friction coefficient and wear volume
tained the hardness of titanium Ti64 even after sliding
Figures 11(a), (c), and (e) present the experimental for 360 s. Therefore, the skin friction (adhesion fric-
results of dry friction coefficients for both Ti64 and tion) under cryogenic cooling is less compared to dry
Ti54. From these figures, one might observe that sliding [33]. Besides this, cryogenic cooling seemed
in most of the cases, the dry friction coefficient of to delay the deformation of asperity, which in turn
Ti54 is comparable to the dry friction coefficient of reduced the actual contact area leading to a reduc-
Ti64 and sometimes is slightly higher. In addition, tion of friction force. However, when speed increased,
both dry and cryogenic friction coefficients exhibited the rate of heat generation increased and the cool-
increasing trends with increasing load and/or speed, ing effect of liquid nitrogen became less. This resulted
Figs 11(a) and (c). On the contrary, Ti54 showed a in an increase in the adhesion friction. Similar pro-
decreasing trend of cryogenic friction with increas- cesses occurred when normal load increased from
ing sliding distance (Fig. 11(e)). On the other hand, 6.45 to 22.96 N. At lower load (Fig. 11(c)), no differ-
at higher levels of load, surprisingly cryogenic fric- ence between dry and cryogenic friction coefficients
tion is higher than dry friction (Fig. 11(c)). At higher was detected for both alloys. This might be due to
load and/or speed, contact temperature is expected to insignificant rise in the frictional heating at lower load.

(a) Measured friction coefficient at 14.72 N and 6min (b) Predicted friction coefficient at 14.72 N and 6min
0.60 0.60
F ric t ion c oef f ic ient

0.55
Friction coefficient

0.55

0.50 0.50

0.45
0.45
Ti64D Ti64C 0.40 Ti64D Ti64C
0.40 Ti54D Ti54C Ti54D Ti54C
0.35
0.35
0.0 0.2 0.4 0.6 0.8 1.0 1.2
0.0 0.2 0.4 0.6 0.8 1.0 1.2
Speed (m/s) Speed (m/s)

(c) Measured friction coefficient at 0.55 m/s and 198 m (d) Predicted friction coefficient at 0.55 m/s and 198 m
0.60
0.60
Friction coefficient

Fric tion c oeffic ient

0.55
0.55
0.50
0.50
0.45
0.45 Ti64D Ti64C 0.40
0.40 Ti64D Ti64C
Ti54D Ti54C 0.35
Ti54D Ti54C
0.35
0.30
5 10 15 20 25
5 10 15 20 25
Load (N)
Load (N)

(e) Measured friction coefficient at 0.55 m/s and (f) Predicted friction coefficient at 0.55 m/s and
14.715 N 14.715 N
F r ictio n co e fficie n t

0.60
Friction coeffic ient

0.60
0.55 Ti64D Ti64D
0.50 Ti64C 0.50 Ti64C
0.45 Ti54D Ti54D
0.40 0.40
Ti54C
0.35 Ti54C
0.30 0.30
0 100 200 300 400 0 100 200 300 400
Sliding distance (m) Sliding distance (m)

Fig. 11 Effects of speed, load, and sliding distance on the friction coefficient of Ti64 and Ti54
alloys under dry and cryogenic conditions: (a, c, and e) experimental results and (b, d,
and f) predicted results

JET703 Proc. IMechE Vol. 224 Part J: J. Engineering Tribology

404 N S M El-Tayeb, T C Yap, and P V Brevern

However, when the load increased to 14.72 N, frictional At longer distance (longer time) (Fig. 11(c)), cryogenic
heating became significant and softened the titanium cooling becomes more effective in terms of reducing
alloys resulting in an increase in the dry skin fric- friction coefficient. The predicted results are in good
tion (adhesion friction). Meanwhile, liquid nitrogen, agreement with the experimental results. However, the
in cryogenic sliding, prevented the softening effect model of cryogenic friction coefficient (equation (8))
and subsequently reduced the skin adhesion friction for Ti54C overestimated the friction at higher values
at lower load. However, when the load increased to of speed (compare Figs 11(a) and (b)) and underesti-
22.96 N, the cooling effect was less as liquid nitrogen mated the friction coefficient at higher load (compare
was notable to flow into the sliding interface and thus Figs 11(c) and (d)).
the friction coefficients remained high. Regarding the wear results, Figs 12(a), (c), and (e)
Apparently, liquid nitrogen was not effective at show increasing trends with increasing speed, load,
higher load level (19.62 N) and cryogenic friction coef- and distance. Besides, cryogenic wear results were
ficients for both titanium alloys were higher than consistently less than those under dry condition.
dry friction coefficients (Fig. 11(c)). In general, for Similar results of wear for dry sliding of Ti-6Al-4V
other test conditions, the cryogenic condition exhib- were reported earlier in reference [32]. According
ited lower friction coefficient as compared to those to reference [31], at low sliding velocity (0.3 m/s),
obtained under dry condition for both titanium alloys, wear was controlled by an oxidative mechanism,
especially at lower ranges of speed and load (Figs 11(a) while at higher velocity (0.8 m/s), the wear mech-
to (d)) and at longer sliding distance Figs 11(e) and (f ). anism was changed and a contribution of metallic

(a) Measured wear volume of Titanium alloys under (b) Predicted wear volume of Titanium alloys under
14.715 N and 6 min sliding 14.715 N and 6 min sliding
3.0 3.0
W ear v olum e (m m 3)

W e a r v o l u m e (m m 3 )

2.5 2.5
2.0 2.0
1.5 1.5
1.0 1.0 Ti64D Ti64C
Ti64D Ti64C
0.5 0.5 Ti54D Ti54C
Ti54D Ti54C
0.0 0.0
0.0 0.2 0.4 0.6 0.8 1.0 0.0 0.2 0.4 0.6 0.8 1.0
Sliding speed (m/s) Sliding speed (m/s)

(c) Measured wear volume of Titanium alloys after (d) Predicted wear volume of Titanium alloys after
slides 198 m at 0.55 m/s slides 198 m at 0.55 m/s
3.0 3.0
W e a r v o l u m e (m m 3 )
Wear v olum e (m m 3)

2.5 2.5

2.0 2.0
1.5
1.5
1.0 Ti64D Ti64C
1.0 Ti64D Ti64C
0.5 Ti54D Ti54C
0.5 Ti54D Ti54C
0.0
0.0
5 7.5 10 12.5 15 17.5 20 22.5 25
5 7.5 10 12.5 15 17.5 20 22.5 25
Load (N) Load (N)

(e) Measured wear volume of Titanium alloys slides (f) Predicted wear volume of Titanium alloys slides
under 14.7 N and 0.55 m/s under 14.7 N and 0.55 m/s
3.0 3.0
W e a r v o l u m e (m m 3 )
Wear v olum e (m m 3)

2.5 2.5
2.0 2.0
1.5
1.5
1.0 Ti64D Ti64C
1.0 Ti64D Ti64C
0.5 Ti54D Ti54C
0.5 Ti54D Ti54C
0.0
0.0
50 100 150 200 250 300 350
50 100 150 200 250 300 350
Sliding distance (m)
Sliding distance (m)

Fig. 12 Effects of speed, load, and sliding distance on wear volume of Ti64 and Ti54 alloys under
dry and cryogenic conditions: (a, c, and e) experimental results and (b, d, and f ) predicted
results

Proc. IMechE Vol. 224 Part J: J. Engineering Tribology JET703

 On the tribo-cryogenic characteristics of titanium alloys 405

delamination continuously increased and essentially (a) (b)

only the delamination wear mechanism was active.
The present experimental wear results are consis-
tent with the work of Molinari et al. [32] who studied
the dry sliding wear mechanism of Ti64 and reported
that at low speed (0.3 m/s), mainly oxidative wear took
place in Ti64. However, with an increase in sliding
speed, the extent of oxidative wear decreased and
delamination wear increased. They also added that (c) (d)
at 0.8 m/s, the wear mechanism in Ti64 was only
delamination. The current results may be explained by
making reference to the results obtained by Molinari
et al. [32] and later confirmed by the analysis of wear
debris in section 4.4. It should be noted that the slid-
ing speed employed in the present study was ranging
between (0.13 and 0.97 m/s) and therefore, oxida-
tive wear at lower speed (0.13 m/s) and delamination Fig. 14 SEM micrographs of worn Ti64 alloys (×250)
wear at higher speed (0.97 m/s) were the current wear tested against a tungsten carbide wheel at
mechanisms. 14.72 N and 6 min: (a) Ti64D at 0.13 m/s, (b)
Figure 13 summarizes the results produced under Ti64D at 0.97 m/s, (c) Ti64C at 0.13 m/s, and (d)
dry and cryogenic sliding for both titanium alloys. Ti64C at 0.97 m/s
It is clear that under dry sliding (Fig. 13(a)), the
friction coefficient has narrow range towards higher
friction 0.44–0.63. It depends on the other test condi- Continuous sliding marks with deep grooves and
tions. Under cryogenic sliding, these ranges extended ridges are seen on the worn surfaces of both alloys.
towards lower values of friction and wear volume. Thus The morphologies of the worn surfaces of Ti64 alloy,
under cryogenic condition, wider range of friction under dry sliding (Figs 14(a) and (b)), show adhe-
coefficient might help in utilizing such conditions in sion marks, signs of plastic deformation, and relatively
many applications. It is also clear that under certain wide scars parallel to sliding direction. Moreover, at
test conditions of cryogenic sliding, LN2 was not able higher sliding speed, this alloy shows gross plastic
to reduce the friction coefficients (Fig. 13(b), marked deformation, ploughing, and smearing characteristic
with a circle.) features (Fig. 14(b)). Similar features were observed
previously [31] when Ti-6Al-4V was tested against
a hardened steel counter-disc. At relatively higher
4.4 Analysis of worn surfaces and wear debris speed, the sliding scars are accompanied by gross
The worn surfaces of both titanium alloys and wear deformation in the Ti surface along with ploughing
debris were examined by SEM (ZEISS SUPRA 35VP) marks and smearing.
equipped with EDS. The chemical status of the ele- Meanwhile, under cryogenic sliding (Fig. 14(c) and
ments of the wear debris were analysed using EDS. (d)), it can be seen clearly that abrasion marks with
Typical worn surfaces of Ti64 and Ti54 alloys tested relatively narrow scars analogy to microcutting. In
against a tungsten carbide wheel under dry and addition, plastic deformation is hardly seen and the
cryogenic conditions are shown in Figs 14 to 17. wear scars become finer and uniformly parallel to

(a) Wear-volum e versus COF, for 17 different dry sliding (b) Wear-volume versus COF, for 17 different cryogenic
conditions sliding conditions
4.0
4.0
3.5 Ti64C Ti54C
3.5 Ti64D Ti54D
w ear v o l u m e, m m 3

3.0
w ear v o l u m e, m m 3

3.0
2.5
2.5
2.0
2.0
1.5
1.5
1.0
1.0
0.5 0.5

0.0 0.0
0.2 0.25 0.3 0.35 0.4 0.45 0.5 0.55 0.6 0.65 0.2 0.25 0.3 0.35 0.4 0.45 0.5 0.55 0.6 0.65

Coefficient of friction Coefficient of friction

Fig. 13 Correlation of wear volume and friction coefficient: (a) dry sliding and (b) cryogenic sliding

JET703 Proc. IMechE Vol. 224 Part J: J. Engineering Tribology

406 N S M El-Tayeb, T C Yap, and P V Brevern
the sliding direction. This is clearly due to the effect
of interposing liquid nitrogen onto the sliding inter-
face during sliding process. In comparing the effect
of dry and cryogenic sliding contacts at higher speed
(Figs 14(b) and (d)), one can see that dry sliding pro-
duces more deleterious features on the worn surface
while cryogenic sliding produces well defined and
more fine uniform abrasion marks. Figures 14(a) and
(c) are magnified in Fig. 15, in which (under dry slid-
ing), ploughing marks (marked with p, Fig. 15(a)) with
different widths and depths, micro debris (marked
with D, Fig. 15(a)), and signs of plastic deformation
can be seen. Furthermore, it can also be observed
that surface cracks appeared only under cryogenic
sliding conditions (Fig. 15(b)) as a result of increasing
the brittleness of the titanium alloy under cryogenic
conditions.
On the other hand, the worn surfaces of Ti54 gen-
erated under dry and cryogenic conditions at two
different sliding speeds are shown in Figs 16(a) to
(d). Figures 16(a) and (b) show some worn parti-
cles adhered to the worn surface of Ti54D after dry
sliding (marked with wp, Figs 16(a) and (b)). Under
cryogenic sliding, fewer amounts of worn particles
with smaller size compared to dry condition were also
observed (marked with wp, Figs 16(c) and (d)). This
is expected to be partially due to flashing away the
particles by the liquid nitrogen jet and partially due
to changing the ductility and elasticity properties of
the worn surfaces under cryogenic condition. Accord-
ing to Singh [34], such remained particles increase the
friction coefficient of both moving surfaces under dry
sliding conditions. Wear particles on the worn surface
can change the mechanism of friction at the sliding
interface, two-body abrasion or three-body abrasion.
The role of wear particles at the interface depends on
whether wear particles slide or roll. It is well known
that rolling wear particles at the interface reduce
the friction coefficient whereas sliding wear particles
increase friction coefficient. In the current work, there
were some evidences of entrapped wear particles at
the sliding interface (two-body abrasion).
Wear debris from Ti64 and Ti54 with different mor-
phologies including irregular plates and fine frag-
ments (produced from dry sliding) and long cylindri-
P (a)
D
D
(a) (b)
Fig. 15 Magnified SEM micrographs of worn Ti64
(×500) at 14.72 N and 6 min at 0.13 m/s: (a) dry
sliding and (b) cryogenic sliding
Proc. IMechE Vol. 224 Part J: J. Engineering Tribology
(a) (b)
wp
wp
(c) (d)
wp
wp
Fig. 16 SEM micrographs of worn Ti54 alloys (×250)
tested against a tungsten carbide wheel at
14.72 N and 6 min: (a) Ti54D at 0.13 m/s, (b)
Ti54D at 0.97 m/s, (c) Ti54C at 0.13 m/s, and
(d) Ti54C at 0.97 m/s
cal shapes (produced from cryogenic sliding) were
observed in this work (Figs 17 to 19). In Fig. 17, similar
flaky wear debris was generated under dry sliding for
both Ti64D and Ti54D (marked with F, Fig. 17(a) and
(b)). However, in the case of Ti54D (Fig. 17(b)), the size
of the debris was relatively larger compared to those
produced from Ti64D. This may explain why the wear
volume of Ti54D is higher compared to Ti64D at higher
ranges of speed and load (0.97 m/s, 19.6 N, Figs 12(a),
(c), and (e)).
In general, flake-like metallic wear debris is the char-
acteristic feature of most debris, which indicates that
delamination occurs during wear [35]. Unidirectional
sliding of the metal surface nucleates surface or sub-
surface cracks. As the sliding continues, these cracks
extend and link resulting in crack beneath and paral-
lel to the surface. When the crack is large enough, it
breaks out to yield flaky debris. In the present study,
the dimensions of these plate-like debris were mea-
sured and found to be about 250–350 μm long and
50–70 μm wide. Cutting chip-like debris can also be
observed for Ti64D and Ti54D. It should be recognized
(b)
F
F
Fig. 17 SEM of wear debris collected under sliding con-
ditions of speed 0.55 m/s, load 14.72 N, and
sliding time 9.364 min: (a) Ti64D and (b) Ti54D
JET703
 On the tribo-cryogenic characteristics of titanium alloys
(a)
(b)
Fig. 18 SEM and EDX analysis of the wear debris col-
lected sliding Ti54D: (a) SEM micrograph show-
ing different types of wear debris and (b) EDX
spectrum from region 1
that the presence of large metallic flakes indicates
that wear debris is generated by severe delamination
mechanism as reported in reference [31].
The EDS analysis of the wear debris collected from
dry sliding (Fig. 18) confirmed that apart from small
portion of tungsten debris from the carbide wheel, the
main elements of the debris are Ti and Al. The plate-
like wear debris is from titanium alloys. This suggests
that delamination is the main wear mode. Besides
plate-like debris, cutting chip-like debris from micro-
cutting is also detected. Interposing liquid nitrogen
during sliding produced wear debris in the form of
long cylindrical chips with 500 μ m length and 40 μm
width (Fig. 19(a)). The EDS analysis of this wear debris
produced from cryogenic sliding of Ti64C confirmed
that the cutting chip-like wear debris was from the
titanium alloys, suggesting that in addition to delam-
ination, there was also microcutting (abrasion wear)
acting during cryogenic sliding.
Finally, three main aspects regarding the cryogenic
sliding should be emphasized. These are changing
the properties of materials at the sliding interface,
possible hydrodynamic effect, and suppressing the
adiabatic shear band. First, the liquid nitrogen con-
trols the temperature rise and reduces adhesion (less
sticky). As a result, the skin friction (adhesion friction)
under cryogenic cooling is less compared to dry
sliding (Fig. 11) [33]. Instead, the tungsten carbide
JET703
407
(a)
(b)
Fig. 19 SEM–EDX analysis of the wear debris collected
from sliding Ti64C: (a) SEM micrograph show-
ing different types of wear debris and (b) EDX
spectrum
particles produce microcutting on the titanium sur-
face resulting in abrasion wear under cryogenic slid-
ing. This is confirmed from the cutting chips of the
collected debris from the cryogenic sliding besides the
observed uniformly parallel abrasion marks analogous
to microcutting on the worn surfaces. Second, intro-
ducing the liquid nitrogen into the interface reduces
the true contact area followed by reduction in the
friction coefficient at lower load [33] and this effect
becomes less at higher load [36]. Less contact area also
reduces the chances of adhesion wear. Third, adiabatic
shear bands (localized deformation) take place when
high plastic shear strain rates occur [37]. Localization
of plastic flow in shear bands is usually attributed
to the plastic instability resulting from thermal soft-
ening. This instability can occur when the local rate
of heat generation due to plastic flow exceeds the
rate of heat dissipation to the surrounding materi-
als. In the present work, the titanium alloys have low
thermal conductivity and it was expected to fail by
adiabatic shear band. However, unsuccessful attempt
was made to detect the formation of adiabatic shear
band (ASB) under subsurface by taking cross-section
optical microscopy of the specimen and hence fail by
adiabatic shear band could not be confirmed in the
present study.
Proc. IMechE Vol. 224 Part J: J. Engineering Tribology
408 N S M El-Tayeb, T C Yap, and P V Brevern
5 CONCLUSIONS
1. Models for friction coefficients and wear volumes
of Ti64 and Ti54 were successfully developed for
dry and cryogenic sliding conditions. The pre-
dicted results are in good agreement with the
experimental results. However, the model of cryo-
genic friction coefficient for Ti54C slightly overes-
timated the friction at higher values of speed and
underestimated the friction coefficient at higher
load.
2. Dry friction coefficients of both Ti54 and Ti64 were
comparable. Both dry and cryogenic friction coef-
ficients exhibited increasing trends with increasing
load and speed. However, Ti54 showed a decreasing
trend of cryogenic friction with increasing sliding
distance. Surprisingly, liquid nitrogen at higher load
was not effective and thus cryogenic friction coef-
ficients of both titanium alloys were higher than
those of dry friction.
3. Wear results under both dry and cryogenic slid-
ing showed increasing trends with increasing
speed, load, and distance. Cryogenic wear results
were consistently less than those under dry
condition.
4. Analysis of worn surfaces showed adhesion marks
together with plastic deformation signs under dry
sliding and at higher sliding speed, Ti64 showed
gross plastic deformation, microcutting, ploughing,
and smearing characteristic features. Delamination
and abrasion wear modes were the characteris-
tic features of cryogenic sliding. Under this sliding
condition, abrasion marks with relatively narrow,
fine, and uniformly scars analogous to microcut-
ting were observed and plastic deformation signs
were hardly seen. Besides, surface cracks were only
observed under cryogenic sliding condition as a
result of increasing the brittleness of the titanium
alloy under cryogenic conditions.
5. Flake-like metallic wear debris is the characteris-
tic feature of most debris, which indicated that
delamination occurs during wear. Wear debris from
both titanium alloys contained irregular plates, fine
fragments, and cutting chip-like debris (from dry
sliding) and long cylindrical shapes (from cryogenic
sliding) were observed.
Finally, contribution of cryogenic condition to slid-
ing of titanium alloys was concluded to be due to a
change in the properties of materials at the sliding
interface, minimizing the true contact area as a result
of hydrodynamic pressure and a possibility of sup-
pressing the adiabatic shear band, but this could not
be confirmed in the current work and further work is
required.
© Authors 2010
Proc. IMechE Vol. 224 Part J: J. Engineering Tribology
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