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Tribology International
journal homepage: www.elsevier.com/locate/triboint
Department of Control Engineering, Faculty of Electrical Engineering, Czech Technical University in Prague, Technicka 2, Prague 6, Czech Republic
nCATS, Faculty of Engineering and Environment, University of Southampton, Higheld Campus, SO17 1BJ Southampton, UK
art ic l e i nf o
a b s t r a c t
Article history:
Received 9 August 2013
Received in revised form
3 February 2014
Accepted 13 February 2014
Available online 12 March 2014
Pin-on-disc is widely used to evaluate tribological properties of thin lms. However, the results are often
present without standard uncertainties; moreover, in many cases the standard uncertainty is replaced by
standard deviation, which is a strong underestimation of real uncertainty. In this study we have followed
ISO and NIST guidelines to investigate the possible sources of uncertainties related to friction and wear
rate measurement and to apply them on two selected coating systems TiN and DLC. We show that
inuence of operator is a signicant contribution to the uncertainty of the wear rate, particularly in the
case of very low wear of DLC coatings. We discuss why variance should be used instead statistic
deviation and suggest a method to calculate uncertainties in case of small number of measurements. The
paper could be used as a guide to evaluate friction and wear data of thin lms and coatings using the
pin-on-disc technique.
& 2014 Elsevier Ltd. All rights reserved.
Keywords:
Pin-on-disc
Coatings
Uncertainty
Friction and wear
1. Introduction
The experimental evaluation of friction coefcient and wear
rate using pin-on-disc is a common laboratory procedure. Despite
the simplicity of measurement and calculation, there are practical
challenges to quantify these basic tribological parameters accurately. Friction is a typical non-equilibrium process and sliding
often leads to wear, which is highly stochastic. The values of
friction coefcients and wear rates reported in the literature
typically show wide variation even for nominally identical tests;
the origin of these variations is often not known. To assess
uncertainty of tribological measurement is thus a complex problem. Due to the high spread of measured data, a high number of
identical measurements is required to estimate values of friction
and wear. The tribological measurement is a lengthy and expensive process; therefore, an optimum number of repetitive measurements must be found to satisfy both precision and economy of
the testing. Moreover, in some cases the number of samples and
thus number of available tests is limited.
Tribological analysis of thin protective lms is in many ways
different from that of bulk materials. The thickness of the lm is in
the range 0.110 mm with 13 mm being the typical value. The
n
Corresponding author at: Department of Control Engineering, Faculty of
Electrical Engineering, Czech Technical University in Prague, Technicka 2, Prague
6, Czech Republic. Tel.: 420 224 357598.
E-mail address: polcar@fel.cvut.cz (T. Polcar).
http://dx.doi.org/10.1016/j.triboint.2014.02.011
0301-679X & 2014 Elsevier Ltd. All rights reserved.
155
2. Measurement uncertainties
The standard uncertainty of measurements is determined using
Type A and Type B uncertainty evaluations [1,2]. To evaluate Type
A uncertainty the measurement is repeated under the same
conditions and the statistical methods are applied to the set of
measured values. However, the tribological tests are destructive
and the test cannot be repeated under the repeatability conditions
stated in Refs. [1,2]. It is clearly demonstrated by the wear rate
data dispersion for which orders-of-magnitude variations are
common [9]. Thus, the results of the set of measurements cannot
be (at least in general) treated with statistical methods; in other
words, uncertainties Type A cannot be evaluated. Nevertheless, the
testing procedure involves some steps, such as instrument calibration, which fulll the repeatability conditions and therefore
could be evaluated by means of a statistical methods and Type A
uncertainty could be determined. The standard uncertainty of
tribological measurement is dominated by Type B uncertainties.
The uncertainty Type B is evaluated by an engineering and/or
scientic judgment based on all available information. In our case
it is the estimation of instrument and method errors and operator
induced uncertainties.
2.1. Standard uncertainty of the friction coefcient
In this study we consider traditional pin-on-disc tribometer with
a ball pressed against a rotating sample (Fig. 1(a)). The pin 1 is
mounted on a stiff lever 2, designed as a frictionless force transducer.
The dead weight 3 produces the normal force Fn. The friction force Ff
is evaluated from the deection of the elastic arm 4 measured by
inductive displacement transducers 5; the calibration referred to
above is used to calculate force from measured deection.
If umA and umB denote the Type A and Type B uncertainties, the
standard uncertainty um of the friction coefcient m is given
by [1,2]
u2 u2A u2B :
Since the friction measurement cannot be repeated under identical conditions due to progressive destruction of the surfaces in
the contact, Type A uncertainty is related only to the calibration
procedure. Calibration is provided by a dead weight (5 N) applied
to a ball holder (Fig. 1(b)) giving offset for frictional force gauge
(zero load is obviously used as the second point). However, it
should be pointed out that the calibration could be only considered as an uncertainty Type A provided it is carried out before any
individual measurement. In normal testing practice it is not the
case the equipment is calibrated after a certain number of tests
156
Ff
:
Fn
2 2
u2i
u2F f
uF n :
4
F f
F n
Zero covariance, i.e. no correlation between the separate input
variables, is assumed in our analysis. Combining of Eq. (4) and
Eq. (1) yields
u2 i
u2F
F 2n f
F 2f
F 4n
u2F n :
where
ui;r
u i
uF f ;r
uF f
Ff
uF n ;r
uF n
:
Fn
0
p ;
100 3
a2
2
2R
sin 2
a2
2R2
2 :
12
F//
n
13
R cos
R cos a== sin
14
R== GR cos
15
M == M
1 cos
M
16
2
2
17
0
p
100 3
2
a2
2R2
2
!2
:
18
The force Fn in Eqs. (3) and (5) is the normal component of force
acting on the pin and the uncertainty of this value is calculated
using Eq. (19)
F n 2 2
F n 2 2
u2Fn
um
u ;
19
m
21
gm
m
2 r sin cos t:
22
dt 2
R
R2
Considering low deviation
we can simplify
u sin
to obtain
F n gm
J
2
23
m 2 r cos t:
24
m
25
r
R2
157
p
ui;r
:
26
2
m 3
100 3
2R2
The uncertainty umi is, however, only a part of umB; its remaining
component umv is often predominant. To obtain umv it is necessary
to repeat the measurements with the same type of samples under
identical conditions. The best estimation of the friction coefcient
is the arithmetic mean of the registered values m1, m2,, mN. The
difference m between highest and lowest values of mi should be
used as a base for estimation of umv. Supposing the rectangular
distribution of the probability of values mi in the interval between
the highest and the lowest values, in agreement with [1,2]
we obtain
uv p:
2 3
27
2
:
12
28
V
;
Fnd
be calculated as
u2A u2Ai u2Ao u2Av ;
10
A
mm3 N m 1 :
FnN
where N is the number of sample revolutions (sometimes denominated as cycles or laps). Standard uncertainty uw is given as
u2w u2wA u2wB :
32
33
bz z
bh
h
35
600
400
200
0
-200
0.0
30
31
800
0.1
0.2
0.3
0.4
0.5
20
R1
R2
P1
P2
Height (nm)
A=
1000
where V is the worn volume during the wear test, Fn is the normal
force and d is the total sliding distance. Applying the method of
loss volume evaluation based on the wear track cross section area
A [mm2] and the wear track radius r [m], the wear rate is given as
3
34
Height (nm)
158
-20
-40
-60
-80
0.00
0.05
0.10
0.15
0.20
0.25
0.30
0.35
0.40
0.45
159
Ao
41
12 A
3 m
A
h
b
and the standard combined uncertainty uw using Eq. (42)
s
2
2
2 2
z
2 x
u
1 A
1 m 2
Ao
uw w
12 A
3 m
A
h
b
42
3. Experimental details
Fig. 5. Cross section of (a) shallow and (b) deep wear track.
==
A==
A
2hx 2x
:
bh
b
36
==2
2
2
2 x
b
37
A
uAv p:
2 3
38
And then
u2A;r u2Ai;r u2Ao;r u2Av;r
z
h
2
2x
b
2
uAo
A
2
2
1 A
:
12 A
39
m
p:
m 3
40
43
160
u2i;r
2
100 3
m 3
2R2
2
0:069
u2
0:57 10 8
7:9 u2
Fnu
12
Operator no.
A (mm2)
A (mm2)
Ao,r
115
121
122
119
119
12
0.03
18
0.043
22
0.041
17
0.036
15
0.036
Table 2
Friction and wear rate of TiN coating as a function of relative air humidity.
TiN coating: Fn 5 N, v 10 cm s 1, r 6.5 mm, t 237 1 1C
Rel. humidity (%)
w (10 6 mm3 N 1 m 1)
2530
3140
4145
1.088 7 0.035
1.056 7 0.029
1.0737 0.037
8.7 7 0.9
9.8 7 1.3
9.2 7 1.7
46
Ao
2:3 10 5 2 :
uw;r
12 A
A
h
b
47
where the wear track width b and depth h are in nanometers.
4. Results
4.1. Friction and wear of TiN coatings
The experiments carried out with 10 samples consisted in a set
of measurements focused on estimation of (i) operator induced
uncertainties of wear rate values, (ii) effect of air humidity and
(iii) impact of the wear track radius r on friction coefcient and
wear rate w values.
In order to nd the operator induced uncertainties, the following pin-on-disc experiment was arranged: the load Fn 5 N, the
linear speed v 10 cm s 1 and the number of laps N 3000. Then
the cross section areas were measured in eight positions evenly
distributed along the wear track. The measurements were performed by ve operators with different laboratory skills. The
comparison of their results, i.e. the arithmetic mean A and the
difference A of these eight values of cross section area measured
by particular operators, is given in Table 1.
If all A values measured by these ve operators are considered
as one set, the mean value of the cross-section area and its relative
uncertainty are
A 119:5 7 6:4 m2 ; uAo;r 0:053:
Table 1
Cross-section area measured by 5 different operators, TiN coating.
48
To evaluate the effect of the humidity on the tribological properties, 10 samples were tested with identical parameters (Fn, v, r, N)
except for air humidity, which was varied in the range 2545%.
Results of this experiment summarized in Table 2 clearly demonstrate that there are no noticeable dependences of measured
values on air humidity since all values are within the limits given
by their standard combined uncertainties.
The standard combined uncertainties u and uw presented in
Table 2 were calculated using Eqs. (50) and (52). By substituting
the values of Fn and measured difference m, we obtain
"
#
0:015 2
2
5
8
2
2
u 7:9 10
49
0:57 10
12
By neglecting negligible terms in Eq. (49) we can write
s
2
;
u 2:25 10 4
12
50
0:05
2:3 10 5 2
500
12 A
4:7 105
51
It is apparent that all instrument uncertainties could be neglected
in comparison with operator induced uncertainty and with variance of A values. Thus the uncertainty uw could be given as
s
2
1 A
:
52
uw w 2:5 10 3
12 A
The last experiment was aimed to the investigation of the wear
track radius effect on the friction coefcient and the wear rate. We
varied radius r in the range 318 mm using a set of ve samples.
The results of this experiment are presented in Table 3 and
summarized in Fig. 6. The friction coefcient slightly increases
with radius; the increase in the wear rate w is even more evident.
We can conclude here that the relative humidity in the range
2541% does not affect the tribological measurement. However,
161
Table 3
The effect of radius on friction and wear rate of TiN coatings.
TiN coating: Fn 5 N, t 2225 1C, RH 3840 %
r (mm)
12
15
18
w (10 6 mm3 N 1 m 1)
0.917 0.13
5.6 7 1.6
0.93 7 0.08
6.5 7 2.1
0.917 0.04
6.9 7 1.4
0.977 0.04
9.6 7 0.4
0.99 7 0.04
11.3 7 0.7
1.067 0.02
9.7 7 0.9
1.1
Table 4
Cross-section area measured by 5 different operators, DLC coating.
-1
0.9
10
0.8
0.7
FC
WR
0.6
2
10
12
14
16
18
Operator no.
A (mm2)
A (mm2)
Ao,r
1.90
1.85
2.08
1.38
2.04
0.41
0.06
0.4
0.06
0.29
0.04
0.31
0.06
0.78
0.11
-1
12
-6
Friction coefficient
1.0
14
4
20
Radius (mm)
Fig. 6. TiN the effect of the wear track radius on friction coefcient m and wear
rate w.
53
54
(ii) The effect of air relative humidity in the laboratory environment was evaluated by means of measurements at seven different
values RH whereas the tests conditions were held xed. The
results are presented in Table 5.
162
Table 5
Friction and wear rate of DLC coatings vs. relative air humidity.
DLC coating: Fn 5 N, v 10 cm s 1, r 7 mm
RH
29
30
35
36
39
42
47
Average
w (10 7 mm3/Nm)
0.076
1.23
0.08
0.96
0.085
1.18
0.095
1.28
0.092
1.04
0.084
1.24
0.096
1.43
0.087 70.016
1.19 70.17
Table 6
The friction and wear rate for two loads, DLC coating.
DLC coating: v 10 cm s 1, r 8 mm, t 237 1 1C, N 3000
Fn (N)
w (10 7 mm3 N 1 m 1)
A/A
5
10
0.087 7 0.015
0.0917 0.016
0.020
0.028
1.19 70.20
1.13 70.19
0.40
0.41
Table 7
The friction and wear rate for two sliding speeds, DLC coating.
DLC coating: Fn 5 N, r 7 mm, t 237 1 1C, N 3000
v (cm s 1)
w (10 7 mm3 N 1 m 1)
5
10
0.0737 0.015
0.0787 0.019
0.041
0.046
1.137 0.17
1.117 0.16
max
p :
2 3
55
U Aw kuAw
friction values (here the mean means average from actual friction
coefcient measured during one sliding test). However, sliding is a
very complex process and sometimes the steady state wear with
stabilized friction is not obtained. In such case the uncertainty of
friction will be higher and must be further analyzed. Another
possibility is regular oscillation of the friction value during one
revolution of the disc. Local imperfection, such as pores, microcracks, or sudden wear debris release, could lead to local changes
in the wear track and consequently local change in friction. The
average value of friction could be still treated in the same way as
above, but the uncertainty will again increase. We will deal with
these phenomena in our future study.
Our analysis helps to calculate uncertainty of the most used
tribological parameters, friction and wear rate. Although demonstrated on pin-on-disc system, the method could be easily adopted
for similar techniques. The tribological analysis of thin lm is
typically comparative different coatings tested at identical
conditions are compared, or the effect of test conditions on one
coating is studied. The knowledge of uncertainty helps to distinguish real difference (e.g. increase in friction) from random
uctuations and thus improve reliability of tribological measurements. We should stress here that uncertainty evaluation is a part
of tribological measurement; therefore, brief description of uncertainty evaluation should be always.
Based on our analysis of the equipment, measurement practice
and friction and wear results obtained for two fundamentally
different coatings, we can suggest following simplication to the
process of friction and wear rate uncertainty evaluation described
above:
56
:
58
U w kw
3 m
A
h
b
It is essential to note that the above described procedures of
uncertainties calculations do not involve other phenomena affecting the results of friction coefcient and wear rate measurements.
In our calculations we assumed constant friction coefcient during
the test, or, more precisely, during steady-state wear regime. This
condition is fullled for many material combinations and sliding
conditions; the friction value only oscillates regularly around mean
6. Conclusion
We evaluated standard uncertainty of the friction and the wear
rate of thin lms measured by pin-on-disc measurement. We
strictly followed uncertainty guidelines (ISO and NIST) and analyzed different parts of standard uncertainties, such as the effect of
163
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