Sains Malaysiana 52(8)(2023): 2209-2224
http://doi.org/10.17576/jsm-2023-5208-04
Copper Nanoparticles Coating on FTO with Improved
Adhesion using Direct and Pulse Electrodeposition Techniques from a Simple
Copper Sulphate Solution
(Salutan
Nanozarah Kuprum pada FTO dengan Lekatan yang Diperbaiki menggunakan Teknik
Elektrodeposisi Terus dan Nadi daripada Larutan Kuprum Sulfat Ringkas)
NUR AZLINA ADRIS1, LORNA JEFFERY MINGGU1,*,
KHUZAIMAH ARIFIN1,2, ROZAN MOHAMAD YUNUS1, MOHAMAD AZUWA
MOHAMED1,3, MASLIANA MUSLIMIN4 & MOHAMMAD B. KASSIM1,3
1Fuel Cell Institute, Universiti Kebangsaan Malaysia,
43600 UKM Bangi, Selangor, Malaysia
2Research Center for Advanced Materials, National Research and Innovation Agency (BRIN), Building 224, KST BJ Habibie, South Tangerang 15314, Banten, Indonesia
3Department of Chemical Sciences, Faculty of Science
and Technology, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor,
Malaysia
4Hydrogen Technology Unit, Materials Technology Group,
Industrial Technology Division, Malaysian Nuclear Agency, 43000 Kajang,
Selangor, Malaysia
Diserahkan:
10 April 2023/Diterima: 14 Julai 2023
Abstract
Copper (Cu) metal nanoparticles were deposited onto FTO
glass using the electrodeposition method. The precursor used was CuSO4×5H2O with Na2SO4 as
the inorganic additive. The formation of Cu was characterized using field
emission scanning electron microscopy (FESEM), energy-dispersive X-ray
spectroscopy (EDX), and X-ray diffraction (XRD). This
study investigated the impacts of the electrodeposition method (direct
electrodeposition vs. pulse electrodeposition), voltages (‑0.4 V and
‑0.8 V), electrodeposition time (60s to 900s) and pulse cycles (50 cycles
to 300 cycles), and FTO etching (fixed to 20s etching) towards the morphology
and adhesion of Cu deposited. The grain size and thickness of Cu deposited
vary with deposition time and pulse cycles. The voltage of -0.4 V successfully
deposits shiny, metallic brown Cu onto FTO glass. Meanwhile, the voltage of
-0.8 V gives powdery brown Cu on the surface. In addition, compared to direct
electrodeposition (DD), pulse electrodeposition (PD) provides a more compact
and homogeneous coverage of Cu onto FTO glass. The tape-test results also
indicate that FTO etching by electrolysis reduction can improve the adhesion
strength between deposited thin Cu film and the FTO glass. This work
demonstrates a facile electrodeposition technique with substrate etching as an
effective deposition of Cu metal with the potential for application in a wide
range of fields.
Keywords: Adhesion; copper;
electrodeposition; inorganic additive; FTO glass
Abstrak
Nanozarah logam kuprum (Cu) diendapkan di atas kaca FTO menggunakan
kaedah pengendapan elektrokimia. Prekursor yang digunakan ialah CuSO4×5H2O dan Na2SO4 sebagai bahan tambah tidak organik. Pembentukan Cu dicirikan menggunakan
mikroskop elektron pengimbasan pelepasan medan (FESEM), spektroskopi sinar-X
penyebaran tenaga (EDX) dan pembelauan sinar-X (XRD). Penyelidikan
ini mengkaji kesan kaedah elektroendapan (elektroendapan langsung lawan
elektroendapan denyutan), voltan (‑0.4 V dan ‑0.8 V),
masa elektroendapan (60s dan 900s) dan kitaran denyutan (50 hingga 300 kitaran)
dan punaran FTO (ditetapkan selama 20s) terhadap morfologi dan lekatan Cu yang
diendapkan. Saiz butiran dan ketebalan Cu yang diendapkan berbeza mengikut
masa endapan dan kitaran denyutan. Voltan -0.4 V berjaya mengendapkan Cu coklat
metalik berkilat pada kaca FTO. Sementara itu, voltan -0.8 V memberikan Cu
coklat serbuk pada permukaan. Di samping itu, berbanding dengan elektroendapan
langsung (DD), Elektroendapan denyutan (PD) memberikan liputan Cu yang lebih
padat dan homogen di atas kaca FTO. Keputusan ujian pita juga menunjukkan
bahawa FTO yang dipunarkan melalui penurunan elektrolisis boleh meningkatkan
kekuatan lekatan antara filem Cu nipis terendap dan kaca FTO. Kajian ini
menunjukkan teknik elektroendapan yang mudah dengan punaran substrat bagi
endapan logam Cu yang berkesan dengan potensi untuk digunakan dalam pelbagai
bidang.
Kata kunci: Bahan tambah tidak organik; elektroendapan; kaca FTO;
kuprum; lekatan
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*Pengarang untuk surat-menyurat; email:
lorna_jm@ukm.edu.my
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