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Abstract
Purpose – The objective of this paper is to study the effect of a commercial lubricant, which contains a 50-50 mixture of zinc diamyldithiocarbamate
and petroleum oil, on the fretting corrosion of tin-plated copper alloy contacts.
Design/methodology/approach – The change in contact resistance as a function of fretting cycles was used to assess the effectiveness of the
lubricant in preventing the fretting corrosion of tin-plated contacts. The surface profile, surface roughness, extent of fretting damage and extent of
oxidation of the contact zone were assessed by a laser scanning microscope and surface analytical techniques to correlate the change in contact
resistance with fretting cycles.
Findings – The lubricant film provides a surface coverage of 6.76 ^ 1 mg/cm2 and it easily establishes metallic asperity contact between the mated
tin-plated contacts. The contact resistance of lubricated contacts remains stable for several thousand fretting cycles. Lubricated contacts reach
a threshold value of 0.1 V around 100,000 cycles, whereas unlubricated contact reaches this value around 13,500 cycles itself. For lubricated contacts,
the extent of mechanical wear of the tin coating is significantly reduced. As a result, they experience a lesser damage at the contact zone and exhibit a
smoother profile. The formation of tin oxide is not appreciable and there is no oxide accumulation at the contact zone even at 380,000 cycles. The
lubricant is very effective in delaying the fretting wear during the initial stages and in preventing the oxidation and accumulation of oxidation products
at the contact zone in the later stages.
Originality/value – Metallic dialkyldithiocarbamates are useful anti-wear and extreme pressure additives for lubricating oils. Dithiocarbamates
improve the antioxidant properties of the lubricants and are effective in reducing the wear and increasing the friction-reducing and load-carrying ability
of the base stock. The use of molybdenum dithiocarbamate as a grease additive is found to be effective in reducing fretting corrosion of ball bearings
under random rotary vibrating conditions. The effect of dithiocarbamate containing lubricant oils or greases on the fretting corrosion of electrical
contacts has not far been studied. The paper explores the effect of a lubricant that contains a 50-50 mixture of petroleum oil and zinc
diamyldithiocarbamate on the fretting corrosion of tin-plated contact.
233
Fretting corrosion of lubricated tin-plated contacts Industrial Lubrication and Tribology
T.S.N. Sankara Narayanan et al. Volume 60 · Number 5 · 2008 · 233 –241
Najman et al., 2004). Dithiocarbamates improves the fretting and reciprocating sliding wear strongly depends on
antioxidant properties of the lubricants and they are test conditions and type of materials used. The observations
effective in reducing the wear and increasing the friction- made from our earlier studies, on the change in contact
reducing and load-carrying ability of the base stock (Huanga resistance as a function of fretting cycles, the surface profile,
et al., 2004). Dithiocarbamate is also a good corrosion morphological features, the wear mechanism, etc. suggest the
inhibitor (Aljinovic et al., 2000) and it is used as an additive in occurrence of fretting. A stroke length (peak-to-peak
phosphating formulations (Sankara Narayanan and amplitude) of 180 mm is chosen so as to increase the
Subbaiyan, 1990, 1992). The use of molybdenum
possibility of oxidation of the contact zone as this study
dithiocarbamate as a grease additive with anti-fretting
mainly focuses on the fretting corrosion of tin plated contacts
properties has been studied earlier (Duque et al., 2004).
for electrical connector contact applications. The contact area
According to Duque et al. (2004), greases containing
dithiocarbamates are effective in reducing fretting corrosion is defined to be a point contact by sphere plane’ geometry. An
of ball bearings under random rotary vibrating conditions. electric current of 100 mA was applied between the contacts
The effect of dithiocarbamate containing lubricant oil or by an electrical circuit (Figure 2) and the contact resistance
grease on the fretting corrosion of electrical contacts has not was continuously measured as a function of fretting cycle. All
been studied earlier. In this context, the present paper aims to tests were performed at 27 ^ 18C and at 60 ^ 1 per cent RH.
study the effect of a commercial lubricant, which contains a The lubricant used in this study contains a 50-50 mixture of
50-50 mixture of zinc diamyldithiocarbamate and petroleum zinc diamyldithiocarbamate and petroleum oil. The important
oil, on the fretting corrosion of tin plated copper alloy properties of the lubricant are given in Table I. Only one drop
contacts. (, 0.01 ml) of the neat lubricant was applied with the help of
a syringe (5 ml) only on the flat contact which was held
Experimental details vertically and the lubricant was allowed to flow under
gravitational force to form a thin film. The surface coverage of
The fretting corrosion behaviour of unlubricated and
the lubricant on the flat contact was measured using the gain
lubricated tin plated copper alloy contacts was studied using
in weight and the surface area covered by the lubricant film.
a fretting apparatus in which the relative motion between the
The surface coverage was measured on ten different samples
contacts was provided by a variable speed motor/precision
stage assembly. The schematic of the fretting apparatus used and averaged out. After testing, the surface profile and surface
in this study is shown in Figure 1. roughness across the fretted zone was assessed using a Carl
The normal contact force was supplied by the weights Zeiss laser scanning microscope (LSM) (Model: LSM-5
placed on the balance arm. The contacts were flat verses PASCAL). Scanning electron microscopy (SEM) and energy
1.5 mm radius hemispherical rider, both of them were made dispersive X-ray analysis (EDX) were used to characterize the
of copper alloy (Ni-1.82 per cent, Si 0.75 per cent; Zn 0.01 extent of fretting damage, extent of oxidation and the nature
per cent; Sn 0.37 per cent and Cu-balance) and tin plated to a of the contact zone.
thickness of 3 m, supplied by the Korea Electric Terminal
Company Ltd, Korea. The rider and flat specimens were Figure 2 The geometry of the rider and flat samples and the circuit
degreased using acetone in an ultrasonic cleaner, dried and used to measure the contact resistance
carefully mounted in the fretting test assembly. The tests were
conducted under gross slip conditions. A periodic relative Flat
Specimen Ampere meter
displacement with amplitude of ^ 90 mm and a frequency of
10 Hz were applied between the rider and flat contacts loaded A
V
by a constant normal force of 0.5 N. The actual effective
stroke length (peak-to-peak amplitude) used in this study is Volt meter DC
180 mm. This leads to query that whether this condition Hemisphere Power supply
Specimen
represents fretting or sliding. Though a stroke length of
d100 mm is usually used in fretting tests, some researchers
have studied the fretting behaviour using a stroke length
. 100 mm while others have used a stroke length of even Table I Properties of the lubricant used
up to 800 mm (Okado et al., 1999; Liu and Zhou, 2000)
Chemical name/formulation Zinc diamyldithiocarbamate in oil
According to Chen and Zhou (2001) the transition between
Composition Zinc diamyldithiocarbamate – 50
Figure 1 Schematic of the fretting apparatus used in the present study per cent by weight petroleum oil – 50
per cent by weight
Weight Colour and appearance Amber liquid
Counter Weight Molecular weight 530.22 g/mol for dithiocarbamate
Plate Spring
Cam Density 970 kg/m3 at 258C
VS Motor
Viscosity 0.098 m2/s at 1008C; 0.336 m2/s at
Specimen
258C
Vapour pressure , 1.3 pa at 208C
Solubility Very soluble in acetone, toluene,
chloroform and petroleum
hydrocarbons
Spring Flexible Parts
234
Fretting corrosion of lubricated tin-plated contacts Industrial Lubrication and Tribology
T.S.N. Sankara Narayanan et al. Volume 60 · Number 5 · 2008 · 233 –241
Results and discussion 100,000 cycles. This observation suggests that the lubricant
consists of a 50-50 mixture of petroleum oil and zinc
Contact resistance of lubricated contacts diamyldithiocarbamate is effective in improving the
One of the important criteria when lubricants are applied to performance of the tin plated copper alloy contacts under
electrical contacts is to ensure that the lubricant must not act fretting conditions. Though lubrication has been shown to
as an insulator or interfere with the formation of electrically improve the fretting corrosion behaviour of connector
active spots (known as a’-spots). The contact resistance of tin contacts, the extent of improvement achieved with
plated copper alloy contacts in presence of lubricant with a lubrication varies a lot from one type of lubricant compared
surface coverage of 6.76 ^ 1 mg/cm2 remains stable and is to the other (Freitag, 1977; Antler, 1987a, b, 1996; Abbott,
very similar to that of the value obtained for unlubricated 1996). A variety of factors, which include, the properties of
contacts. This observation suggests that the lubricant film has the lubricant, the dose and method of application, the
sufficiently lower shear strength so that metallic asperity thickness, compactness and surface coverage of the lubricant
contact could be easily established between the mated tin film, ability of the lubricant to remain in place without
plated copper alloy contacts. creeping away and, ability to flow back over freshly exposed
The change in contact resistance of unlubricated and metal when the contact slip has pushed it aside, should be
lubricated tin plated contacts as a function of fretting considered when comparing the improvement in performance
cycles is shown in Figure 3(a) and (b), respectively. For achieved with lubrication. In order to get better insights on
unlubricated contacts, a hump is observed in the initial stages these aspects, the surface profile, fretting damage, extent of
(, 400 cycles) followed by a low contact resistance up to oxidation and, accumulation of wear debris and oxidation
8,000 cycles. Beyond 8,000 cycles, there is a gradual followed products, are assessed using LSM, SEM and EDX analysis.
by a rapid increase in contact resistance. The initial hump is The surface profiles of the contact zone of unlubricated and
due to the presence of a thin film of tin oxide on the surface of lubricated tin plated contacts after 20,000 cycles are shown in
the tin plated contact, which is removed in a very short span Figure 4(a) and (b), respectively. The surface roughness
of time. The low-contact resistance values observed up to parameters obtained under these conditions are given in
8,000 cycles after the initial hump is due to the conducting Table II. It is evident from Figure 4 and Table II that the
nature of the soft tin plating. The subsequent gradual increase lubricant is very effective in preventing the fretting wear and
in contact resistance could be attributed to the formation of oxidation of the contact zone. The smooth profile of the
tin oxide film as well as accumulation of debris and oxidation contact zone of lubricated contact suggests that the lubricant
products, further reducing the electrical conducting area. The is effective in dispersing the wear debris and oxidation
rapid increase in contact resistance suggests that with increase products.
in the number of fretting cycles, the current is conducted
through an increasingly smaller area of contact. These Surface characteristics of the contact zone of lubricated
observations correlate well with those of other researchers contacts
(Lee and Mamrick, 1987; Neijzen and Glashorster, 1987; The surface morphology of lubricated tin plated contacts after
Malucci, 2001; Flowers et al., 2004). 100,000 and 380,000 fretting cycles are shown in Figure 5(a)
For lubricated contacts, the contact resistance remains and (b), respectively.
stable for several thousand fretting cycles. Though there is a The fretting direction is vertical (indicated by the dotted
steady increase in contact resistance, the extent of increase is line in Figure 5). The area of the fretted region is oval or
not appreciable compared to that of unlubricated contacts. elliptical in shape. The absence of bright tin oxide debris in
For lubricated contacts, the contact resistance has reached a areas adjacent to the fretted zone indicates that the lubricant
value of 0.1 and 0.5 V around 100,000 and 380,000 cycles, is effective in preventing the oxidation of the contact zone and
respectively. In contrast, for unlubricated contacts, the the wear debris generated during fretting is effectively
contact resistance has reached 0.1 and 0.5 V around 13,500 dispersed by the lubricant. A closer look at the morphology
and 15,200 cycles, respectively. indicates the occurrence of cracks and severe surface damage
A threshold value of contact resistance has been used as the in the form of scoring marks. The formation of surface cracks
failure criterion to assess the performance of connector was also observed for un-lubricated and lubricated tin plated
contacts and the time to failure is represented by the number contacts (Shao and Zhang, 1998).
of fretting cycles needed for the contact resistance to reach The EDX line scanning performed across the fretted region
this threshold value. However, the choice of the failure criteria confirms the presence of tin and copper as the major elements
should be based on the application rather that the product (Figure 6).
specification (Mroczkowski, 1998). Whitley and Malucci Within the fretted zone (marked between the dotted lines in
(1978) have proposed a failure criterion for electronic Figure 6) the intensity of tin is decreased whereas the intensity
contacts to be 10Rc when neglecting film resistance, where of copper is increased suggesting that during fretting motion
Rc is the contact resistance for clean surface contact. Since tin the tin coating is removed and the base metal is exposed. It is
and tin alloy plated contacts contains an oxide layer at the interesting to note that the EDS profiles exhibit some steps
metal surface, the rule of 10Rc as the failure criterion does (cross over point of Sn and Cu lines) within the fretted zone
not apply for such contacts. In the present study, to compare (Figure 6). During fretting, the tin coating is continuously
the effectiveness of the lubricant, 0.1 V is considered as a removed due to wear and the fretting motion enables the wear
threshold value of contact resistance and the number of cycles debris to be thrown out of the contact zone. Hence, the EDS
at which this threshold value is reached is taken as a measure profile should clearly exhibit distinct Sn and Cu lines without
of performance. Accordingly, for unlubricated contacts, the any step (crossover point(s)) within the fretted zone. The
threshold value of 0.1 V is reached around 13,500 cycles EDS profile of unlubricated tin plated contacts subjected to
whereas lubricated contacts reach this threshold value around fretting at amplitudes of ^ 25 and ^90 mm does not exhibit
235
Fretting corrosion of lubricated tin-plated contacts Industrial Lubrication and Tribology
T.S.N. Sankara Narayanan et al. Volume 60 · Number 5 · 2008 · 233 –241
Figure 3 Change in contact resistance of (a) unlubricated; (b) lubricated tin plated contacts measured across the contact zone as a function of fretting
cycles
100
10
Contact resistance (ohm)
0.1
0.01
0 4,000 8,000 12,000 16,000 20,000
Cycles
(a)
100
10
Contact resistance (ohm)
0.1
0.01
10,000 1,00,000 10,00,000
Cycles
(b)
any such steps and this has already been reported in our ^ 90 mm. At such relatively high amplitude the EDS profile is
earlier papers (Park et al., 2006a, b, 2007; Sankara Narayanan expected to exhibit distinct Sn and Cu lines without any step.
et al., 2006). The crossover of the intensities of Sn and Cu However, the EDS profile of the lubricated tin plated contact
lines is observed only when the fretting amplitude is ^5 mm subjected to fretting for 100,000 and 380,000 cycles exhibit
(Park et al., 2006a). It is obvious to expect that at such low the presence of steps. The enhancement of the intensity of the
amplitudes (^ 5 mm) the possibility of accumulation of the Cu line within the fretted zone confirms the removal of the tin
wear debris in the contact zone is very high and this issue is coating and exposure of the base metal. Hence, the
already addressed in our earlier paper (Park et al., 2006a). occurrence of step in the EDS profile of lubricated tin
The present study evaluates the performance of lubricated tin plated contact could be due to the presence of wear debris in
plated contacts under fretting conditions at an amplitude of the contact zone. It is well known that lubricants have the
236
Fretting corrosion of lubricated tin-plated contacts Industrial Lubrication and Tribology
T.S.N. Sankara Narayanan et al. Volume 60 · Number 5 · 2008 · 233 –241
Figure 4 Surface profile across the fretted zone of (a) unlubricated; (b) lubricated the tin plated copper alloy contact after 20,000 fretting cycles
80
40 z (µm)
0
700
600
0
50 500
100
200 400
250 300
y (µm)
350
x(µm) 400 200
450
100
500
550 0
(a)
120
80 z (µm)
40
0
300
250
200
0
20 150
40 y (µm)
60
100
80
100
120 50
x (µm) 140
160
0
(b)
Table II Roughness of the fretted zone of unlubricated and lubricated tin plated contacts after 20,000 fretting cycles
Roughness parameter Unlubricated contact Lubricated contact
Arithmetic mean deviation, Ra (mm) 1.71 1.14
Highest peak, Rp (mm) 28.69 16.25
Lowest valley, Rv (mm) 23.68 4.84
Absolute peak to valley, Rt (mm) 52.37 21.10
Average peak to valley, Rz (mm) 24.56 5.79
Maximum peak to valley, Rmax (mm) 52.37 18.21
ability to disperse the wear debris and this is quite evident 380,000 cycles (Figure 6(b)) only very small amounts of
from the morphological features of the lubricated tin plated oxygen is detected at the fretted zone. This indicates that the
contacts (Figure 5). The intensity of oxygen is not appreciable lubricant effectively prevents oxidation of the contact zone.
to be detected in the EDS profile of the sample run for The effectiveness of the lubricant is also evident from the
100,000 cycles (Figure 6(a)) and even for the sample run for low and stable contact resistance for several thousand
237
Fretting corrosion of lubricated tin-plated contacts Industrial Lubrication and Tribology
T.S.N. Sankara Narayanan et al. Volume 60 · Number 5 · 2008 · 233 –241
Figure 5 Surface morphology of the contact zone of lubricated tin plated copper alloy contact after (a) 100,000 fretting cycles; (b) after 380,000
fretting cycles
fretting cycles. Hence, the occurrence of step in the EDS contact with increase in fretting cycle is reported in our earlier
profile of the fretted zone is due to the ability of the lubricant paper (Park et al., 2006b).
having a dispersion of metallic Sn and Cu wear debris to flow The EDX pattern of the fretted region of the sample run for
back over the contact zone after being pushed aside from the 100,000 cycles reveals the presence of tin as the predominant
contact zone due to fretting motion. The observed difference element with some amount of copper and a very small amount of
in the occurrence of step (200 mm in Figure 6(a) and 300 mm carbon that might have originated from the lubricant
in Figure 6(b)) is due to increase in area of the contact zone (Figure 7(a)). The oxygen content is not appreciable. The
with increase in fretting cycle (from 100,000 to 380,000 EDX pattern taken on the center of the fretted zone (Figure 7(b))
cycles). The increase in the area of fretted zone of tin plated indicates the presence of some amount of zinc and sulphur other
238
Fretting corrosion of lubricated tin-plated contacts Industrial Lubrication and Tribology
T.S.N. Sankara Narayanan et al. Volume 60 · Number 5 · 2008 · 233 –241
Figure 6 EDX line scan performed across the fretted zone (indicated by of the fretted zone (Figure 7(d)) indicates the presence of tin,
the dotted line in Figure 4) after (a) 100,000 fretting cycles; (b) after copper, oxygen, zinc and sulphur.
380,000 fretting cycles The EDX spot analysis performed at the center of the
fretted zone indicates that it is predominantly copper
(59.17 at.%) and tin (28.99 at.%) with some amounts of
200 zinc (4.12 at.%), sulphur (4.36 at.%) and oxygen (3.36 at.%).
Fretted zone
Sn These observations suggest that even after the tin coating has
150
worn out in some areas the lubricant is effective in decreasing
Intensity (counts)
Cu
enables the contact resistance to remain stable for several
thousand fretting cycles. The ability of the lubricant to
100 decrease the rate of oxidation and, to effectively disperse the
wear debris and oxidation products, results in a slow and
steady increase in contact resistance.
50
Sn
O
0 Conclusions
0 100 200 300 400 500
The effect of a commercial lubricant that consists of a 50-50
mixture of petroleum oil and zinc diamyldithiocarbamate on
Distance (micrometer)
the fretting corrosion of behaviour of tin plated copper alloy
(b)
contacts is studied. For the addition of only one drop
(, 0.01 ml) of the neat lubricant, the lubricant film provides a
than tin and copper. The copper content is significantly higher – surface coverage of 6.76 ^ 1 mg/cm2. The lubricant film has
indicates dispersion of the wear debris by the lubricant. The zinc sufficiently lower shear strength and it easily establishes
and sulphur might have originated from the lubricant that metallic asperity contact between the mated tin plated
contains about 50 per cent of zinc diamyldithiocarbamate. contacts. The contact resistance of lubricated contacts
The EDX spot analysis performed at the center of the remains stable for several thousand fretting cycles.
contact zone indicates that it is predominantly tin (49.19 at.%) Lubricated contacts reach a threshold value of 0.1 V around
and copper (38.53 at.%) with some amount of zinc 100,000 cycles whereas unlubricated contact reaches this
(5.80 at.%) and sulphur (6.48 at.%). The oxygen content is value around 13,500 cycles itself. Surface profile and surface
not appreciable. These observations suggest that though the roughness of lubricated contact exhibit a smoother profile as
tin coating has worn out in some areas of the contact zone,
it experiences a lesser damage at the contact zone. The
the lubricant is effective in preventing the oxidation of tin and
surface morphology of the contact zone of lubricated contact
the base metal.
confirms that the extent of mechanical wear of the tin coating
The EDX pattern of the fretted region of the sample run for
380,000 cycles reveals the presence of copper and tin as the is significantly reduced. EDX analysis performed on the
predominant elements with some amounts of oxygen, zinc contact zone suggests that the formation of tin oxide is not
and sulphur (Figure 7(c)). The intensity of copper is relatively appreciable and there is no oxide accumulation at the contact
high compared to that of the EDX pattern of samples run for zone even at 380,000 cycles. The study concludes that the
100,000 cycles, indicating that the tin coating has mostly lubricant used in the present study is very effective in delaying
worn out. The zinc and sulphur might have originated from the fretting wear during the initial stages and in preventing the
the lubricant that contains about 50 per cent of zinc oxidation and, accumulation of oxidation products at the
diamyldithiocarbamate. The EDX pattern taken on center contact zone in the later stages.
239
Fretting corrosion of lubricated tin-plated contacts Industrial Lubrication and Tribology
T.S.N. Sankara Narayanan et al. Volume 60 · Number 5 · 2008 · 233 –241
Figure 7 EDX pattern of the entire fretted zone (a and c) and the center of the fretted zone (b and d): (a and b) after 100,000 fretting cycles; (c and d)
after 380,000 fretting cycles
Full scale = 108 cps Cursor: 5.0475 kev Full scale = 44 cps Cursor: 1.2075 kev
Sn Cu
Sn Cu
Sn
Cu
o S Zn
C Si Cu o
0 2 4 6 8 10 12 14 16 18 20 0 2 4 6 8 10 12 14 16 18 20
kev kev
(a) (b)
Full scale = 48 cps Cursor: 12.0075 kev Full scale = 34 cps Cursor: 10.7675 kev
Sn Sn
Cu
Sn
Cu
Zn
Cu Cu
C S o S
C Si Zn Zn
0 2 4 6 8 10 12 14 16 18 20 0 2 4 6 8 10 12 14 16 18 20
kev kev
(c) (d)
240
Fretting corrosion of lubricated tin-plated contacts Industrial Lubrication and Tribology
T.S.N. Sankara Narayanan et al. Volume 60 · Number 5 · 2008 · 233 –241
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Corresponding author
“Fretting-corrosion mapping of tin-plated copper alloy
contacts”, Wear, Vol. 262 Nos 1-2, p. 228. Kang Yong Lee can be contacted at: kyl2813@yonsei.ac.kr
241