Iwantono, Yanuar, Taer E, Awitdrus, Jaya

Prosiding Simposium Fisika Nasional XX

ISSN 1411-4771
Menyonsong 100 Tahun Karya Besar Einstein
Pekanbaru, 25-26 Agustus 2004

PREPARATION OF NICKEL NANOPARTICLES ONTO ALUMINIUM

SUBSTRATE WITH THICKNESS VARIATION BY
ELECTRODEPOSITION

Dahyunir Dahlan, A. R. Daud, S. Radiman

School of Applied Physics, Faculty of Science and Technology, Universiti
Kebangsaan Malaysia (UKM) 43600 Bangi, Selangor - Malaysia.

ABSTRAK
Penumbuhan nikel secara elektrodeposisi diatas substrat aluminium telah dilakukan.
Substrat aluminium yang digunakan berbentuk plat dan lapisan tipis. Substrat plat
aluminium berdiameter 1,4 mm dan mempunyai ketebalan 1mm dan 2 mm. Substrat
lapisan tipis aluminium mempunyai ketebalan sekitar 150 nm diatas slide kaca.
Elektrodeposisi dari nikel dihasilkan dengan cara menggunakan larutan cair nikel
dengan pH 3,5 pada suhu kamar (25°C) menggunakan peralatan elektroplating.
Percobaan dilakukan pada tegangan konstan 4V selama 15 detik. Morfologi dan
komposisi partikel diuji menggunakan mikroskop elektron (SEM) dan analisa dispersi
energi sinar-X (EDX) berturut-turut. Hasilnya menunjukkan bahwa diameter partikel
nikel lebih kecil jika ketebalan substrat lebih kecil. Bagaimanapun hampir semua ukuran
partikel nikel adalah kurang dari 100 nm jika elektrodeposisi dilakukan pada substat
lapisan tipis.

ABSTRACT
Nickel growth by electrodeposition on aluminium substrate is reported. Aluminium
substrates used consist of plate and thin film. Aluminium plate substrates were 1.4 mm in
radius with 1 mm and 2 mm in thickness. Aluminium thin film substrate is about 150 nm
in thickness was prepared on a glass slide. Electrodeposition of nickel was produced by
using aqueous nickel solution of PH 3.5 at room temperature (25°C) using electroplating
sets. It is carried out under a constant voltage of 4V for 15 seconds. The morphology and
composition of selected particles was determined by Scanning Electron Microscope
(SEM) and Energy Dispersive X-ray (EDX) analysis, respectively. The results revealed
that diameters of the nickel particles were smaller when the thickness of substrates was
thinner. However, almost all of nickel particles sizes were less than 100 nanometers
when electrodeposition of substrate was made on thin film substrate.

1. INTRODUCTION
Metal nanoparticles have attracted attention recently because of their unusual
properties and potential technological application (i.e., electronic, optic, magnetic,
catalytic materials etc.). Several methods can be used to synthesize metal
nanoparticles, such as microemulsion technique, hydrazine and alcoholic
reduction, electroplating and wet chemical in micelle [1-5].
Nickel nanoparticles have important application in catalysis and in
conducting and magnetic materials. For examples, superparamagnetic properties
have been studied extensively using assembly of carbon encapsulated nickel
nanoparticles, Ni (C) nanoparticles [6]. The properties of nanocrystalline nickel in
multilayers may enhance significantly the recording and data applications [7].
Recently, electroplating has been focused for preparing nanoparticles,
since this technique is usually much cheaper and simpler than other methods. The
purpose of this work is to synthesize nickel nanoparticles from nickel salt solution

82
Iwantono, Yanuar, Taer E, Awitdrus, Jaya
Prosiding Simposium Fisika Nasional XX
ISSN 1411-4771
Menyonsong 100 Tahun Karya Besar Einstein
Pekanbaru, 25-26 Agustus 2004

electrodeposited on aluminium substrate. The size and structure of the

nanoparticles produced were characterized and the distribution of particle size was
also determined.

2. MATERIAL AND METHODS

2.1. Material.
Nickel plating solution was obtained from Okuno (Tokyo), Aluminium
bulk was a product from Aldrich (USA) and ethanol was supplied by Scarlau
(European Union). The reagents used were used as received.

2.2. Preparation and characterization.

The pure bulk aluminium was melted to produce a cylindrical shape as
cast alloy, and then cut to form sample substrates of 1 and 2 mm in thickness with
14 mm in diameter. The substrate was polished using emery sand and an oil-
based diamond suspension with polished roughness about 1µm. Washing the
substrate was done using pure water, vibrated in an ultrasonic bath (filled with
ethanol) for 15 minutes, rinsed with distilled water, and finally dried air.
Meanwhile thin film aluminium substrates were produced from aluminium bulk
using electron gun PLS 570 Balzers-German. The thickness of film onto glass
slides was about 150 nm. All electrochemical deposition was carried out in a one-
compartment with three electrodes cell. A piece of graphite was employed as the
counter electrode, saturated calomel electrode (SCE) used as a reference electrode
and aluminium substrates as a working electrode. The electrodes were immersed
into electroplating bath filled with nickel plating solution at room temperature
(25°C). The distance of counter electrode and working electrode was set at 3 cm;
reference electrode was placed close to the working electrode surface to measure
the potential used in electroplating process. A potential of 4 volt for 15 seconds
was applied using a direct current power supply (GPR 1830/GW4721409).
Results of potentials on reference electrode are as shown in table 1. Reference
potential was measured using SCE before electrodeposition process while plating
potential was measured at the time of process.

Table1.
Potential used for electrodepositing process
Substrate Reference potential, V Plating potential, V
Potential and time
Aluminium (SCE) (V vs. SCE)
1. plate 2mm 2.7 Volt ≈ 2.4 to 2.7 Volt
2. plate 1mm 4 Volt, 15 seconds -377 mV ≈ -443 mV
3. thin film 150 -362 mV ≈ -375 mV
nm

The morphology of nickel deposits was analyzed by scanning electron

microscope (SEM) 1450 VP, manufactured by LEO Electron Microscopy. The
average composition of all deposition was measured by energy-dispersive
particles size X-ray (EDX) spectroscope INCA M. 7353 Oxford Instrument
incorporated in the same system using the same SEM. Distribution of particles
size was estimated using an image analyzer model.

83
Iwantono, Yanuar, Taer E, Awitdrus, Jaya
Prosiding Simposium Fisika Nasional XX
ISSN 1411-4771
Menyonsong 100 Tahun Karya Besar Einstein
Pekanbaru, 25-26 Agustus 2004

3. RESULTS AND DISCUSSION

Nickel particles onto aluminium plate substrates were shown in figures 1(a)
and 1(b). Distributions in the deposited size indicated progressive nucleation.
Although the surface of substrate was still rough when polished by 1 µm diamond
spray, the sizes of particles deposited were fairly uniform. The morphology of the
particles was mainly spherical. On Figure 1(a) electrodeposition used 2mm of
thickness substrate, shows that the particles which have been grown onto substrate
varied in size namely from approximately 300 nm to 1 µm with an average
particle size of 616nm. Distribution of particle sizes is shown in figure 2(a), where
the particles of 300 – 400 nm and 500-600 nm contribute about 45 % at the total
particle deposited onto the surface of substrate.

a b

Fig.1. SEM image of nickel particles deposited using 4V for 15 second onto (a) Al plate
substrate of 2mm in thickness, (b) Al plate substrate of 1mm in thickness and (c) Al thin
film substrate 150nm in thickness.

On the thin plate substrate that is 1 mm in thickness, electrodeposition

produced the particles with size was smaller than that onto the 2 mm plate in
thickness. The distributions of particles size were 50 to 300 nm (figure 2(b)). The
smaller of particles size came from the smaller potential caused by the thickness
of substrate. Table1 showed the effect of thickness of substrate aluminium related
to reference and plating potential. The lower potential for electrodeposition

84
Iwantono, Yanuar, Taer E, Awitdrus, Jaya
Prosiding Simposium Fisika Nasional XX
ISSN 1411-4771
Menyonsong 100 Tahun Karya Besar Einstein
Pekanbaru, 25-26 Agustus 2004

process caused a slower growth of particles. However, slow growth was

preferable since this gave uniform metal particles [8]. According to Ohm law
ρ=l/A, where l is the thickness of substrate and A is area that passed by current,
the smaller of thickness caused higher resistivity that made lower potential on
surface of substrate.
Aluminium thin film substrate (figure 1(c)), the particle size was very
small if compared to plate substrate. The surface of substrate was smooth and
particle dispersed almost to all of the substrate. There are no particles stacking
fault that could be seen. With the thickness of film substrate about 150 nm, the
particle size electrodeposited onto substrate between 20 to 100 nm. Most of
particles size was 20 to 40 nm (figure 2(c)).

Precentage of nickel particle onto Al plate Percentage of nickel particle onto Al plate
a (2mm) 4V 15 sec. b (1mm ) 4V 15 sec.
25 100
20
p ercen tag e (% )

80

p ercen tag e (% )
15
60
10
40
5
20
0
300- 401- 501- 601- 701- 801- 901- 0
400 500 600 700 800 900 1000 50-100 101-200 201-300
diameter (nm) diam eter (nm)

Percentage of nickel particles onto Al Thin

c film 4V 15 sec.
60
50
percentage (%)

40
30
20
10
0
20-40 41-60 61-80 81-100 101-110
diam eter (nm)

Fig.2. Histograms of particle size distribution estimated from SEM image in fig.1.

EDX analysis (Fig. 3) confirms that nickel atoms were deposited onto
aluminium substrate during electrodeposition process. Gold (Au) was present on
each substrate as coating layer to prevent sample from oxidizing before
characterization. Meanwhile, other elements came from glass slides that are used
as base of aluminium thin film substrate.

85
Iwantono, Yanuar, Taer E, Awitdrus, Jaya
Prosiding Simposium Fisika Nasional XX
ISSN 1411-4771
Menyonsong 100 Tahun Karya Besar Einstein
Pekanbaru, 25-26 Agustus 2004

a b

Fig.3. EDX analysis of aluminum substrate after electrodeposition: (a) aluminium

plate and (b) aluminium thin film.

4. CONCLUSION
The thinner the aluminium plate substrate, the smaller the nickel particle
size formed using electrodeposition methods. Aluminium thin film substrate
produced by electron-gun gave a smooth surface substrate and the nanoparticles
deposited onto the surface were much smaller than those formed onto thick
aluminium substrates.

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G.Q. Xu, Langmuir, 12 (1996) 909
[4] Allen Bai, Chi Chang Hu, Electrochemistry Comm. 5 (2003) 79
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[6] Madhuri Mandal, Subrata Kundu, Sujid Kumar Ghosh, Tapan K. Sau, S.M.
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[7] Xiang-Che Sun, J. Antonio Toledo, Current Applied Phys, 2 (2002) 114
[8] H. Liu, F. Favier, K. Ng, M.P. Zach, R.M. Penner, Electrochimica Acta 47
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[9] A. K. Pradhan, Applied Surface Science, xxx (2003) xxx
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ACKNOWLEGEMENTS
The authors would like to acknowledge the Government of Malaysia for funding
this work through research grant IRPA 09-02-02-0032-SR0004/04/04.

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