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 MINGGU^1,*, KHUZAIMAH ARIFIN^1,2, ROZAN MOHAMAD YUNUS¹, MOHAMAD AZUWA MOHAMED^1,3, MASLIANA MUSLIMIN⁴ & MOHAMMAD B. KASSIM^1,3

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

Received: 10 April 2023/Accepted: 14 July 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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*Corresponding author; email: lorna_jm@ukm.edu.my