The Production of a Silicon-Based Proton-Exchange Membrane with Different Porosity Layers

Yıl 2018, Cilt: 11 Sayı: 1, 58 - 65, 24.04.2018

Meltem Gör Bölen , Tevhit Karacalı

Öz

The aim of this study, which combines renewable energy and porous silicon – two prominent issues in recent years – was to make a porous proton exchange membrane for a proton exchange membrane fuel cell. To make a membrane of the desired thickness, wet etching was performed on the 4.41 cm2 rear side of a double-sided, polished, p-type silicon wafer with a thickness of 200 μm and a resistivity of 0.001 to 0.005 Ω-cm. Then the silicon wafer was cleaned using the RCA cleaning method and the grid shape on the mask was printed on the front side of the silicon using photolithography. The 3.61 cm2 front face of the silicon was placed in a double-tank electrochemical cell designed by us and was anodized at various current densities for certain periods of time to allow the formation of a porous layer throughout the sample. Finally, the pore formation was completed by passing a high current through the rear surface of the silicon to ensure that the pore tips were opened. The thickness of the porous layer formed was observed by scanning electron microscopy. Electrochemical impedance spectroscopy was performed, with the help of a fuel passage test and with formic acid, to measure the usability of the porous silicon as a membrane. Ion passage was observed as a result of the experiments performed.

---

---

---

Anahtar Kelimeler

Porous silicon, Proton exchange membrane, Silicon etching, Electrochemical impedance spectroscopy, Electrolytic polishing

The Production of a Silicon-Based Proton-Exchange Membrane with Different Porosity Layers

Öz

Son yıllarda dikkat çeken iki konu olan, yenilenebilir enerji ve gözenekli silikonu birleştiren bu çalışma, proton ileten membran yakıt hücresi için gözenekli silikon proton ileten membran yapmayı amaçlamaktadır. Bu amaçla, öncelikle istenilen kalınlıkta membran yapabilmek için 200μm kalınlık, 0.001-0.005 Ωcm özdirencine sahip çift yüzü parlak p tipi silikon dilimin 4.41 cm2’ lik arka yüzüne ıslak aşındırma yapılmıştır. Daha sonra RCA yöntemi ile silikon dilimin temizliği yapılıp silikonun ön yüze fotolitografi yardımı ile maske üzerindeki ızgara şekli basılmıştır. Bizim tarafımızdan tasarlanmış bir çift tanklı elektrokimyasal hücreye yerleştirilen silikonun 3.61 cm2’ lik ön yüzüne çeşitli akım yoğunluklarında belirli sürelerde anodizasyon yapılıp gözenekli tabakanın numune boyunca oluşumu sağlanmıştır. Son olarak gözenek uçlarının açıldığından emin olmak için silikonun arka yüzeyinden yüksek akım geçirilmek suretiyle gözenek oluşumu tamamlanmıştır. Oluşturulan gözenekli tabaka kalınlığı taramalı elektron mikroskobu ile gözlemlenmiştir. Gözenekli silikonun membran olarak kullanılabilirliğinin ölçüsü olarakta methanol yardımı ile yakıt geçiş testi ve formik asit yardımı ile elektrokimyasal empedans spektroskopi yapılmıştır. Yapılan deneyler sonucunda iyon geçişi gözlemlenmiştir.

Anahtar Kelimeler

Gözenekli silikon, Proton ileten membran, Silikon aşındırma, Elektrokimyasal empedans spektroskopi, Elektrolitik parlatma

Kaynakça

• Aslan M., (2016), Membran Teknolojileri, T.C. Çevre ve Şehircilik Bakanlığı.
• Bisi, O., Ossicini, S., & Pavesi, L., (2000). Porous silicon: a quantum sponge structure for silicon based optoelectronics. Surface science reports, 38(1), 1-126.
• Burham N., hamzah A. A., majlis B. Y. (2014). Mechanical characteristics of porous silicon membrane for filtration in artificial kidney. IEEE-ICSE2014. Kuala Lumpur, Malaysia.
• Canham L. T., (1990), Silicon quantum wire array fabrication by electrochemical and chemical dissolution of wafers, Appl. Phys. Lett. 57, 1046.
• Canham L. T., (2014), Handbook of Porous Silicone.
• Ehteshami, S., M., M., & Chan, S., H., (2014). The role of hydrogen and fuel cells to store renewable energy in the future energy network–potentials and challenges. Energy Policy, 73, 103-109.
• Gold, S., Chu, K., Lu, C., Shannon, M.A., Masel, R., I., (2004). Acid loaded porous silicon as a proton exchange membrane for micro-fuel cells. Journal of Power Sources 135, 198–203. USA.
• Gör, M., ve Karacalı, T., Porous Silicon Based Membrane Fabrication for Proton Transportation. 13. Nanobilim & Nanoteknoloji konferansı, 2017.
• Hecini, M., Khelifa, A., Palahouane, B., Aoudj, S., & Hamitouche, H. (2015). A new advance in the study of p-type silicon/electrolyte interface by electrochemical impedance spectroscopy. Research on Chemical Intermediates, 41(1), 327-341.
• Karacali T., (2003), Darbeli anodizasyon tekniği ile gözenekli ve Si tabanlı fabry-perot yapılarının üretimi: Yapısal ve optik özelliklerinin incelenmesi. Doktora Tezi, Atatürk Üniversitesi. Fen Bilimleri Enstitüsü, Erzurum.
• Lai C., Xiang Z., Liu C., Zhu C., Wang H., Zhu H., (2015). Study on corrosion of macroporous silicon in sodium hydroxide solution by electrochemical methods and scanning electron microscopy, International Journal of Corrosion.
• Lim, B. H., Majlan, E. H., Daud, W. R. W., Husaini, T., & Rosli, M. I. (2016). Effects of flow field design on water management and reactant distribution in PEMFC: a review. Ionics, 22(3), 301-316.Nayak, A. P., Islam, M. S., & Logeeswaran, V. J. (2012). Wet Etching. Encyclopedia of Nanotechnology, 2829-2830.
• Park, J.; Yanagida, Y.; Hatsuzawa, T., (2016), Fabrication of p-type porous silicon using double tank electrochemical cell with halogen and LED light sources, Sens. Actuators B Chem., 233, 136–143.
• Pichonat, T., Gauthier-Manuel, B., (2006). Realization of porous silicon based miniature fuel cells. Journal of power sources 154, 198-201.
• Sharma, S., & Ghoshal, S. K. (2015). Hydrogen the future transportation fuel: from production to applications. Renewable and sustainable energy reviews, 43, 1151-1158.
• Torres, N., Duch, M., Santander, J., Sabaté, N., Esquivel, J. P., Tarancón, A., & Cané, C. (2009). Porous silicon membrane for micro fuel cell applications. Journal of New Materials for Electrochemical Systems, 12(2–3), 93-96.
• Uhlir A., (1956), Electrolytic shaping of germanium and silicon, Bell Syst. Tech. J. 35,333.
• Wang, M., Liu, L., & Wang, X. (2017). A novel proton exchange membrane based on sulfo functionalized porous silicon for monolithic integrated micro direct methanol fuel cells. Sensors and Actuators B: Chemical, 253, 621-629.
• Westra K., (2010). KOH and TMAH etching of bulk silicon recipes, tricks, what is possible and what is impossible.
• www.microchemicals.eu/technical_information, “Wet-Chemical Etching of Silicon” 2011-01-17.
• Xiang Z., Liu C., Lai C., (2014). Corrosion of Fresh Porous Silicon in Potassium Hydroxide Solution Int. J. Electrıchem Sci., 3935-3948.
• Zoltowski P., (1998). On the electrical capacitance of interfaces exhibiting constant phase element behaviour. Journal of Electroanalytical Chemistry, 443(1), 149-154.