R.

Hemachandran1,
M. Pugazhvadivu2,
Development of Electroless Ni-P Coatings
S. Jayabal3 on Sisal Fiber
DOI: 10.5604/12303666.1227879
1
Department of Mechanical Engineering, Abstract
Pondicherry Engineering College, Improving the properties of natural fibers can be interesting from atechnological point of
Puducherry-605014, India, view. Modifications can result in ahigh specific strength, electromagnetic interference (EMI)
E-mail: [email protected] shielding, antistatic brush etc. Plant fiber composites would make them an option for use in
2
Department of Mechanical Engineering, components such as rifle stocks and knife handles etc. The greatest challenge would be to
Pondicherry Engineering College, ensure that the components are all weather capable, but today several materials exist that have
Puducherry-605014, India, ahigh moisture tolerance. Moreover with proper surface coating techniques, most natural
E-mail: [email protected] fibers materials can be toughened up to use as reinforcement. An attempt was made using
aproprietary experimental set-up to coat natural fiber with electroless nickel phosphorus
3
Department of Mechanical Engineering, (ENi-P), since sisal fiber is anon-conducting material. In this article the surface morphology,
A.C.College of Engineering and Technology, ingredients and cross-section images of the modified natural fibers were characterised by
Karaikudi-630003, India, ascanning electron microscope equipped with EDAX.
E-mail: [email protected]
Key words: composite, mechanical properties, electroless, nickel, sisal, SEM, EDAX.

tion, which is followed by activation, and composite applications. One researcher

then controlled electron deposition using reported the effect of silver coating and
achemical reduction reaction with suita- the size of fibre on the electrical proper-
ble additives for acceleration or retarda- ties of sisal fibre-reinforced epoxy com-
tion of the deposition rate [1, 2]. posites [9].

Sisal fiber is anatural fiber extracted To shield and limit against electromag-
from the leaves of the sisal plant. Sisal is netic interference (EMI) and electrostat-
the most commonly produced fiber glob- ic discharge (ESD), conductive polymer
ally and accounts for the worlds largest composites started replacing coated ma-
plant fiber production. The sisal plant terials for various shielding applications
produces 200-250 commercially usable in the electrical and electronics indus-
leaves during its life- cycle. The major tries, especially for electronic household
producers of sisal fiber are Brazil, Mex- appliances. This trend has been driven
ico, China, Tanzania, Kenya and Mada- mainly because of the better characteris-
gascar. The areas of application of sisal tics of these polymers in terms of elec-
fiber are the automotive industry, in elec- trostatic discharge (ESD), shielding from
trical applications, railways, geo-textiles, EMI, thermal expansion, density, corro-
defense and the packaging industry. sion and oxidation resistance properties
[10,11].
Most of the research on sisal-polymer
composites were carried out in the mid- In order to explore the possibility of using
1990s, and sisal fiber was proved suc- modified sisal fibers as reinforcements in
cessful in composite applications. With composites, an attempt was made to de-
this in mind, Kuruvilla et al (1999) made velop and characterise electroless nickel
areview of sisal fiber reinforced compos- phosphorus (ENi-P) coatings on sisal fib-
ites. Sisal-polymer composites were also er in the present investigation.
fabricated and their mechanical proper-
ties were studied by most of the research-
ers concerned [4,5]. The various coating
Materials & methods
procedures adopted for synthetic fibers The interface between the matrix and re-
created an interest in the coating of sisal inforcement is critical and can affect the
fibers in order to improve the mechanical properties of composites manufactured
properties of sisal-polymer composites significantly. If the interface is not mod-
Introduction
[6,7]. The oxidation of carbon and metal ified properly, it can lead to the degrada-
Electroless coating finds applications in coated carbon fibers was introduced in tion of the properties of composites. To
the chemical, nuclear, telecommunica- 1970 [8]. In this continuation, electro- develop better adhesion and interfacial
tions, consumer electronics and comput- phoretic deposition (EPD), followed by bond between sisal fiber and epoxy ma-
er industries. The first inventors of Ni-P pressureless sintering, to produce dense, trix, the electroless coating process was
electroless coating were Brenner and defect-minimised, carbon-fiber-rein- used to deposit Ni-P onto sisal fiber in
Riddel in the year 1946. Electroless plat- forced borosilicate-glass-matrix compos- the present investigation. The electroless
ing involves anumber of steps carried ites with a nickel interface were proposed coating of the fiber, which is asimple,
out in order. The first step is sensitisa- as aplatform for coating carbon fibers for low-cost and easy- to- use process has

32 Hemachandran R, Pugazhvadivu M, Jayabal S. Development of Electroless Ni-P Coatings on Sisal Fiber.

FIBRES & TEXTILES in Eastern Europe 2017; 25, 1(121): 32-35. DOI: 10.5604/12303666.1227879
 Figures

been successfully applied to prevent un- the fibers absorbs the Tin II chloride ions,
desirable interfacial reactions and pro- which acts as catalyst for Ni deposition.
mote wettability through the increased Also activation is carried out for activat-
overall surface energy of the reinforce- ing the fiber surface for electroless nickel
ment [12]. Due to the lighter weight of Ni deposition. In activation, the nucleation
and relatively stable coating quality, plat- effect is performed on the sensitized sur-
ing Ni on the surface of sisal fibers has face in acidic palladium chloride solution
been widely used [1]. Sisal fiber (Sri Ba- (0.01 g/l).
laji Coir Industries, Dharmapuri, Tamil-
nadu, India) in the chopped form was The pH of the bath was adjusted to
used in this study. The electroless Ni-P 8.01.0 by the addition of the required
deposition process was undertaken to de- amount of ammonia solution as and Figure Fig.1 Cross1. Cross
section section of the sisal
of the uncoated uncoated
fiber
posit Ni-P onto the sisal fiber. The pro- when required. The bath temperature was sisal fiber.
cess constitutes the following sequence maintained at 801C. The electrolytic
of steps: cleaning, rinsing, drying, sensi- bath was heated by an electrically heat-
Table 1. Bath composition.
tising, activation and metallisation. ed water bath whose temperature was
maintained by aproportional integral de- Composition,
Element
Pre-cleaning is done for the fibers before rivative (PID) controller. The bath com- g/l
electroless nickel deposition so that the position is given in the Table 1. Based Nickel sulfate 30
properties required are obtained on the on the literature, the composition of the Sodium hypophosphate 32
Figures Tri-sodium citrate 40
surface of the fiber. The fibers are pre- bath is selected. The other compositions
Ammonium chloride 50
cleaned in acetone followed by ameth- are also tried and the coating obtained by
anol wash to remove the contaminants these compositions only. The activated
present in it. The alkali treatment process sisal fibers are immersed in the bath and
in hot sodium hydroxide (NaOH) solu- electroless coating is performed for var- 400 X Sisal
Fig.2 magnification
fiber coatedandwiththe
Ni-Player of si-
(5 mins)
tion removed lignin, hemi cellulose and ious coating durations, such as 5, 20, 25 sal fiber was observed. The main content
other soluble compounds on the surface and 60 minutes. As the coating duration of natural fiber is cellulose micro-fibrils
of the fiber. The alkali treatment imparts increased, the Ni-P coating on the fib- which are bonded by amorphous mate-
improved mechanical properties by the ers increased in thickness. The samples rials called hemicelluloses. Lignin acts
removal of impurities on the fibers. Gen- prepared were then characterised by an as acoupling agent, which helps to im-
erally the level of interfacial adhesion in-
Figures SEM, JSM 6390A, JEOL, Japan, fitted prove
Fig.1 Cross sectionthe stiffness
of the of the
uncoated sisal fibercellulose/hemi-
creases by use of treated fibers in the pro- with an EDS analyser. cellulose composite. SEM images of
cessing of fiber reinforced composites. cross-sectional and surface views of sisal
Results and discussion fibers coated with ENi-P for 5, 20, 25 and
Sensitization is aprocess of catalysing 60 minutes under the same plating condi-
the nonconductive substrate, which ena- SEM images of coated and uncoated tions are shown in Figures 2-5. With an
bles the fiber surface to act as acatalyst sisal fibers increase in the coating duration, the thick-
for the deposition of nickel. In the case Fig.3 Sisal fiber coated with Ni-P (20 mins)
The cross section of the uncoated single ness of the coating was found to increase
of sensitization, the fibers are subjected sisal fiber is shown in Figure 1. The esti- marginally from 1.42-8.23m. There
to asurface sensitizer (Tin II chloride mated diameter of the fiber from the SEM is no appreciable change in the coating
0.1g/l) for 15 min. During the process is ~100 m. An SEM image was taken at thickness beyond 60 minutes duration.
Fig.1 Cross section of the uncoated sisal fiber Fig.2 Sisal fiber coated with Ni-P (5 mins)

Figure 2. Sisal fiber

Fig.2coated with
Sisal fiber Ni-P
coated with(5 mins).
Ni-P (5 mins) Fig.3 coated
Figure 3. Sisal fiber Sisal fiberwith
coated with (20
Ni-P Ni-P mins).
(20 mins)
Fig.4 Sisal fiber coated with Ni-P (25 mins)

Fig.3 Sisal
Sisal fiber coated with Ni-P (20
(25 mins)
Figure 4. Sisal fiber
Fig.4 coatedfiberwith Ni-P
coated with (25
Ni-P mins).
mins) Figure 5. Sisal fiber
Fig.5 coated
Sisal fiberwith Ni-P
coated with (60
Ni-Pmins).
(60 mins)

FIBRES & TEXTILES in Eastern Europe 2017, Vol. 25, 1(121) 33

 Fig.5 Sisal fiber coated with Ni-P (60 mins)
Full scale counts: 740 Base(10) Full scale counts: 488 Base(7)
Ni
500 Ni
700

600 400

500
300
400

300 200

Ni Ni
200 P
P
100
100
0
Ni Ni
0 0
1 2 345 67 8910 12 3 4 5 6 7 8 910
keV keV
Fig. 6 EDAX spectrum of Ni-P coating on Sisal fiber for 5 mins Fig. 7 EDAX spectrum of Ni-P coating on Sisal fiber for 20 mins

Figure 6. EDAX spectrum of Ni-P coating on sisal fiber for 5 mins. Figure 7. EDAX spectrum of Ni-P coating on sisal fiber for 20 mins.
Fig. 7 EDAX spectrum of Ni-P coating on Sisal fiber for 20 mins

Full scale counts: 535 Base(5) Ni Full scale counts: 482 Base(6)
Ni
500 400

400
300

300

200 Ni
200
Ni

100 P
P
100
Fig. 8 EDAX spectrum of Ni-P coating on Sisal fiber forNi25 mins
Ni
0 0
1 23 4 5 67 8 9 10 12345 67 89 10
keV keV
Fig. 8 EDAX spectrum of Ni-P coating on Sisal fiber for 25 mins Fig. 9 EDAX spectrum of Ni-P coating on Sisal fiber for 60 mins

Figure 8. EDAX spectrum of Ni-P coating on sisal fiber for 25 mins. Figure 9. EDAX spectrum of Ni-P coating on sisal fiber for 60 mins.

Sisal fibers are used to fabricate polymer used as reinforcements in polymer matrix as the coating duration increases, prefer-
composites using epoxy, polyester, vinyl composites, that would develop strong ential deposition of Ni takes place with
ester and other types of resins. Alow val- interfacial bonding between the matrix respect to P. The presence of nickel with
ue of mechanical properties is obtained as and reinforcement. maximum weight percentages of 91.90,
compared with synthetic fiber reinforced 93.13, 93.76 and 93.78 were observed for
polymer composites due to the poor in- EDAX spectrum of coated sisal fibers 5, 10, 25 and 60 minutes of coating, re-
terfacial bonding between the fiber and Energy dispersive X-ray analysis identi- spectively. The presence of phosphorous
matrix. In order to improve the adhesion fies the presence of various materials in with maximum weight percentages of
and interlaminar bond between the sisal the fiber coating. Table 2 lists the various 8.10, 6.87, 6.24 and 6.22 were observed
fiber and matrix, fiber coating was sug- materials and their oxides present in the for 5, 10, 25 and 60 minutes of coating,
gested in the present investigation. coating. The spectrum processing option respectively.
of oxygen by stoichiometry was used for
From Figures 2-5, it was observed that EDAX analysis. Fabrication and testing of sisal-epoxy
the surface seems to be rough and shows composites
strong adherence of the coating onto the EDAX analysis (Figures 6-9) of the Liquid epoxy resin and hardener
fiber. The surface roughness of the coat- coated fiber reveals the presence of Ni (HY951) at a10:1 ratio was placed in
ed fibers indicates that if these fibers are and P in the coatings. It is observed that aplastic container and mixed thorough-
ly for 20 min. Uncoated or coated sisal
fiber was added, mixed thoroughly, and
Table 2. Composition of coating as per EDAX. poured into aplastic mould. Astainless
steel mould of asize of 300 300 3 mm
PK Ni K
Coating time, was used for composite plate fabrication
min Weight, % Atom, % Weight, % Atom, %
using the compression molding process.
5 8.10 14.31 91.90 85.69
The samples were cut from the compos-
10 6.87 12.26 93.13 87.74
ite plate according to ASTM D 638-10.
25 6.24 11.21 93.76 88.79
The tensile behavior of the sisal-epoxy
60 6.22 11.17 93.78 88.83
composites was measured using aDual

34 FIBRES & TEXTILES in Eastern Europe 2017, Vol. 25, 1(121)

Table 3. Properties of uncoated and coated sisal fiber reinforced epoxy composites.

Uncoated sisal-epoxy composites Coated sisal-epoxy composites

Fiber length, Fiber loading, Tensile Flexural Impact Tensile Flexural Impact
Si. No
mm % strength, strength, strength, strength, strength, strength,
MPa MPa kJ/m2 MPa MPa kJ/m2
1 10 30 20.4 30.2 28.5 28.2 39.0 38.8
2 25 30 24.4 33.5 33.2 34.6 44.2 44.8
3 40 30 31 45.2 41.3 43.3 59.2 55.8
4 55 30 30.9 51.5 43.1 43.9 68.9 58.5
5 70 30 24.2 40.3 34.7 33.4 53.7 46.2

Column Table Top Universal Testing Ma- n House hold applications (knife hold- 3. Kuruvilla Joseph, Romildo Dias Toldo
chine (Tinius Olsen H10K). The length, ers, trays) Filho, Beena James, Sabu Thomas and
width and thickness of each sample in Laura Hecker de Carvalho. A review on
n Electrical applications (switch boards)
sisal fiber reinforced polymer compos-
tensile testing were 165, 25 and 3 mm,
ites. Revista Brasileira de Engenharia
respectively. Athree point flexural test
was conducted for specimen dimensions Conclusions Agrcola e Ambiental 1999; 3: 367-379.
4. Kalaprasad G, Joseph K, Thomas S and
of 125 mm 12.5 mm 3 mm accord- Acontinuous thick Ni-P alloy layer was Pavithran C. Theoretical modelling of
ing to ASTM D 790-10. The izod impact coated on the surface of sisal fibers by tensile properties of short sisal fibre-re-
test was carried out using aTinius Olsen electroless plating. The coating thick- inforced lowdensity polyethylene com-
(Model: 104) Impact Tester as per Stand- posites. Journal of Materials Science
ness ranged between 1.42-8.23 m, and
1997; 32: 4261-4267.
ard ASTM D 256-10 and asample size of amaximum coating thickness of 8.23m 5. Mishra S, Misra M, Tripathy S S, Nay-
62.5 12.5 3 mm was used. was observed for acoating duration ak S K and Mohanty A K. The influence
of 60minutes. There is no appreciable of chemical surface modification on the
The values of tensile, flexural and impact change in the coating thickness beyond performance of sisal polyester biocom-
behaviors of uncoated and coated si- 60 minutes of the coating duration. posites. Polymer Composites 2002;
sal-epoxy composites observed are given TheSEM images reveal dense, uniformly 23(2): 164-170.
in Table 3. Fabrication conditions such as 6. Matkovi Potoi V M and Skenderi Z.
distributed nickel deposition on the sisal
Mechanical Properties of Polyurethane
fiber length and fiber loading were select- fiber. The EDAX spectrum revealed that Coated Knitted Fabrics. Fibres and Tex-
ed as per aliterature survey for short sisal an increase in nickel % with respect to tiles in Eastern Europe2013; 21, 4(100):
fibers. The uncoated sisal-epoxy com- the coating duration clearly indicates the 86-91.
posites exhibited better values of tensile, preferential deposition of nickel on sisal 7. Exequiel R and Francucci G. PHB
flexural and impact strength of 31MPa, fiber. Sisal epoxy composites were fab- coating on jute fibers and its effect on
51.5 MPa and 43.1 kJ/m2, respective- ricated using uncoated and coated sisal natural fiber composites performance.
ly, for an uncoated sisal fiber length of Journal of Composite Materials2015;
fibers. A40%, 32% and 35% improve-
0021998315601203.
55mm and fiber loading of 30% by ment in tensile, flexural and impact be- 8. Galasso F S and Pinto J., Oxidation
weight. The coated sisal-epoxy compos- haviors, respectively, were observed for of carbon and metal coated carbon
ites exhibited better values of tensile, coated sisal fibers in epoxy composites. fibers,Fibre Science and Technolo-
flexural and impact strength of 43.9 MPa, gy1970; 2(4): 303-315.
68.9 MPa and 58.5 kJ/m2, respectively, 9. Kaya C, Boccaccini A R and Chawla K
for the coated sisal fiber length of 55 mm K. Electrophoretic Deposition Forming of
and fiber loading of 30% by weight. Acknowledgement Nickel-Coated-Carbon-Fiber-Reinforced
Borosilicate-Glass-Matrix Composites.
The Author would like to thank the Late. N. Journal of the American Ceramic Soci-
Applications of coated sisal fiber Pushpanathan, Headmaster, Government ety2000; 83(8): 1885-1888.
reinforced epoxy composites Primary School, Kottucherrymedu, Karaikal, 10. Trihotri M, DeepakJain, Fozia Haque
The use of sisal fiber reinforced epoxy India for the support provided towards the Khan, Malik M M and Qureshi M S. Ef-
successful conduct of research in the field of fect of silver coating on electrical prop-
composites in engineering applications electroless coating.
such as the automobiles, construction erties of sisal fibre-epoxy composites.
Polymer Bulletin 2013; 70: 3501-3517.
and other industries are proposed because 11. Perumal R R. Electroless nickel plated
of its low cost, acceptable strength, low References composite textile materials for electro-
weight and ease of degradation. Thecoat- magnet compatibility. Indian Journal of
1. Xian Feng Xu, Peng Xiao and Jia Sun.
ing of sisal fiber for improvement in the The process of electroless plating Ni on Fiber and Textile Research 2011; 36:
mechanical behaviors of sisal-epoxy the surface of carbon fibers, Advanced 35-41.
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2. Karthigeyan R, Ezhil vannan S, Ran- ing Parameters on Coating Morphology
ganath G, Paul vizhian S and Annama- of Short Basalt Fiber. Jordan Journal of
n Sports goods applications (child toys, Mechanical and Industrial Engineering
lai K. Effect of Coating Parameters on
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Coating Morphology of Basalt Short
n Automobile applications (rear flaps, Fiber for Reinforcement Preparation of
mud guards, engine guards) Al/Basalt Metal Matrix Composites In-
n Structural applications (door panels, ternational Journal of Electrochemical
name plates) Science 2013; 8: 10138-10148. Received28.12.2015 Reviewed19.06.2016

FIBRES & TEXTILES in Eastern Europe 2017, Vol. 25, 1(121) 35