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Materials Today: Proceedings XX (2017) XXX–XXX www.materialstoday.com/proceedings
ICMMM - 2017
Abstract
Electroless process is employed to get uniform coating of copper on graphite particles. Electroless coating process was performed
based on Taguchi L16 orthogonal array. Optimal coating parameters were determined by Taguchi method using Grey Relational
Analysis. ANOVA technique was further employed to know the optimal parameters from grey relational grade. The present study
is to maximize thermal conductivity and coating thickness characteristics of electroless copper coated graphite, by optimizing the
four coating parameters viz. composition of zinc, copper sulphate, graphite and sensitization time. Microstructural aspects were
studied through SEM analysis.
1. Introduction
Sliding bearings should be able to withstand high temperature during running condition. PTFE is widely used in
sliding applications because of their low coefficient of friction [1-2]. PTFE bearing widely used in petrochemical
plants, pipelines, buildings and bridge girders where they can accommodate expansion, contraction and other
reciprocating motions of the structure[3]. The thermal properties of PTFE can be enhanced by adding conductive
fillers like graphite, ceramic or metal particles [4]. With outstanding thermal stability, coefficient of thermal
expansion (CTE), good chemical resistance and low friction coefficient, graphite has been used widely as
reinforcement for polymer metal matrix [5-8]. Graphite has some deficiencies like brittleness, low strength and
relatively poor conduction [9].
To overcome the problems many researchers developed metal coating techniques to coat graphite with metals such
as copper[10], silver[11] and nickel[12] which helps in preventing interfacial reaction and improves wettability of
the particles[13-14]. Rajkumar et al.[15] reported in his study that copper and its alloy are extensively used in the
applications that requires thermal conductivity, corrosion resistance and wear resistance properties. Moustafa et al.
[16] concluded in their studies that copper coated graphite composites showed high thermal conductivity and
excellent lubrication properties for sliding contacts. W Lu et al.[17] reported in his work that Copper coating acts as
a protective layer to minimize the exfoliation of the graphite in polymers.
The density difference between graphite and copper is high, because of that uniform powder mixture cannot be
obtained. So sintering cannot be done. Instead of mixing copper with graphite, when graphite particle coated with
copper better particle distribution expected to achieve and develops continuous copper network [18].
There are many coating methods available. Some of the methods are Electroless chemical and Electrochemical
method, physical vapour deposition, chemical vapour deposition, spraying, roll to roll coating process. For coating
on micro or nano particles only electroless process is preferable. Ashtiani et al.[19] reported in his work that uniform
coating thickness can be obtained by electroless process, which leads to reduction in corrosion due to absent of
galloan effect. Deposition of metals on the nonconductive and conductive materials without the source of electricity
is electroless process. Ashassi-Sorkhabi et al.[20] reported in his work that increased in coating time helps in
decreasing corrosion rate. Electroless coating technique is appealing because of its low cost, high quality thin films
[21]. Jaroslav[22] observed that electroless coating is the best method for coating graphite with copper to obtain
uniform coating. Caturla[23] reported that most of Graphite pores covered after electroless coating and amount of
coverage depends on thickness of copper coatings on graphite particles.
The objective of this work is to optimize the conditions to coat 2-10m size graphite particles with adherent uniform
and continuous coatings of copper for use in preparing polymer composite as reinforcement which increases
Thermal Conductivity. However not much work done to find optimum conditions for coating copper on graphite
particles based on coating Thickness and Thermal Conductivity. Taguchi orthogonal method is used to design the
optimum number of experiments to be conducted for Electroless copper coatings on Graphite. The amount of copper
coated on graphite depends on composition of bath, which is comprised of Copper sulphate, Graphite, Zinc.
Sensitization time is the amount of time graphite particles soaked in acetone. As all these parameter have effect, so
they were choosen as process parameters. Grey Taguchi method used for solving multiple response problems [24].
ANOVA further employed to find optimum level of factors based on maximum Grey relational Grade values.
Moreover the copper coating on graphite particles are characterized by SEM to understand the microstructural
characteristics.
2. Experimental Details
In full factorial design, all the factors with its various levels are studied. As there are four factors and each factor
has got four levels, so 44 i.e. 256 experiments has to be performed, to know the effect of these factors on the
responses. There is a chance of experimental error creeping because of variation in material and background
conditions [25]. Dr. G Taguchi developed Taguchi techniques, from which effect of input parameters on output can
be known with minimal number of experiments. Optimum number of experiments can be obtained through Taguchi
technique [26-30].In present study Taguchi OA (L16) is obtained using Minitab software. The four factors with their
four levels shown in the Table 1.
Author name / Materials Today: Proceedings XX (2017) XXX–XXX 3
According to C B Lin [31], Graphite is coated with copper by cementation process, in which the copper ions are
replaced by zinc via heterogenous secondary nucleation process .Graphite particles of size 2-5 micron is taken and
dipped in Acetone solution. The contents are oscillated with the help of Ultrasonic Oscillator. Impurities on the
graphite particles are removed in this process. Copper sulphate solution is prepared by mixing 90 gm of CuSo 4 in
distilled water. Glacial acetic acid which acts as wetting agent is added to the bath. This serves as electrolyte. Dried
Graphite particles are added into the electrolyte. Zinc of particle size 12-14 m is immersed in the electrolyte bath
and agitated with the help of ultrasonic oscillator. During this period copper gets coated on the graphite particle. The
experimental setup is shown in fig.1.Coated particles are separated from electrolyte bath through filter papers of
diameter 125 mm and then dried in furnace.
Pallets are made out of the dried copper coated samples by compacting with hydraulic press at a pressure of
30KPa. The compacted pellets are sintered at a temperature of 300C for 10 min. Gaurav Awasthi et al.[32] in his
studies concluded that the rise in sintering temperature helps in obtaining uniform microstructures at the interface.
He contributed this because of formation of many meshes of grain boundary and their interactions with the
interwoven pores. He added that sintering temperature is directly proportional to coefficient of the atomic diffusion
within the particle.
The output parameters that will be analyzed are Thermal conductivity and coating Thickness. Particle Thickness is
measured by Particle Analyser. Thermal Conductivity is calculated from Electrical conductivity from Franz law
shown in Eq. 1, where K and L are thermal conductivity and proportionality constant(Lorenz number) respectively.
4 Author name / Materials Today: Proceedings XX (2017) XXX–XXX
Lorenz number at room temperature equals to 2.44e-8 WΩK-2. The results of coating thickness and thermal
conductivity for the 16 experiments are shown in Table 2.
K (1)
LT
Table 2. Values of coating thickness and thermal conductivity for different samples.
Grey Taguchi analysis is employed to convert multiple responses into single response, shown in Table 3. The
standard formulas are used for calculating grey relational coefficient [25].Further ANOVA is employed to find the
optimal levels from Grey Relational Grade, shown in Table 4. The parameters where highest coating thickness and
thermal conductivity registered are at 25.5 gm of Zinc, 90 gm of Copper sulphate, 19.5 gm of Graphite and 15
minutes of sensitization time.
Table 3. Calculations of Grey Relational Grade for coating thickness and thermal conductivity.
L1 L2 L3 L4
Zn 0.66625 0.725 0.7925 0.805
CuSo4 0.65875 0.74375 0.79125 0.795
Gr 0.7775 0.7125 0.7375 0.76125
Time 0.71875 0.74875 0.80875 0.7125
Graphite which is flake like structure can be observed in Fig. 2a. After electroless coating copper gets deposited on
graphite, which covers the graphite flakes shown in Fig. 2b. Uniform microstructure was formed at interface after
sintering copper coated graphite shown in Fig. 2c.
a b c
Fig. 2. SEM images of a) pure graphite b) copper coated graphite c) copper coated and sintered graphite.
3. Conclusion
Taguchi Orthogonal array (L16) designed using Minitab software. Copper gets coated on Graphite using
electroless coating process. The coating thickness is measured by Particle Analyzer. The maximum coating
thickness obtained at the 25.5 gm of zinc, 75 gm of copper sulphate and 23.5 gm of graphite and sensitization time
being 5 minutes. It was observed there is an increase in Thermal Conductivity of coated Graphite compared to
noncoated Graphite. The maximum Thermal conductivity registered at 23.5 gm of zinc, 82.5 gm of copper sulphate
and 19.5 gm of graphite and sensitization time being 10 minutes. Grey Relational Analysis Technique is employed
to know the optimum parameters for multiple responses. The optimal parameters for multiple responses are 25.5 gm
of Zinc, 90 gm of Copper sulphate, 19.5 gm of Graphite and 15 minutes of sensitization time. Through SEM
photographs difference between coated and noncoated graphite particles was observed.
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