황산전해조에서 양극산화에 의한 다공성 알루미나 막의 제조

장윤호; 이창우; 함영민

HWAHAK KONGHAK, Vol.36, No.5, 653-660, October, 1998

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황산전해조에서 양극산화에 의한 다공성 알루미나 막의 제조

Preparation of Porous Alumina Membrane by Anodic Oxidation in Sulfuric Acid

장윤호, 이창우, 함영민

초록

본 연구에서는 시판용 99.8%금속알루미늄을 황산전해액에서 정전류 방식에 의하여 양극산화하여 다공성 알루미나 막을 제조하는 실험을 행하였다. 전기화학 반응은 표면반응으로 양극산화에 앞서 알루미늄판을 열산화, 화학연마 및 전해연마 등의 전처리를 행하였으며, 반응온도(0, 10, 20℃), 전기량(1,000, 1,500, 2,500 C), 전해질 농도(5, 10, 15, 20wt%) 및 전류밀도(5, 10, 20, 30mA/cm²)의 변화에 따라 양극산화를 시행하여 형성된 다공성 알루미나 막의 세공크기와 분포, 세공밀도 및 막의 두께를 조사하였다. 양극산화에 의해 제조된 다공성 알루미나 막의 기하구조는 직선적인 원통형 세공을 가지며, 세공직경과 세공분포가 매우 균일하고 세공밀도가 높은 우수한 알루미나 막을 제조할 수 있었다. 이때 30-60μm 의 두께를 가지며, 세공직경은 20-40 nm이고, 세공밀도는 2.1-9.2 X 10¹⁰개/cm²를 갖는 막을 얻을 수 있었다

Porous alumina membranes were prepared by anodic oxidation using DC power supply of constant current mode in an aqueous solution of sulfuric acid. The aluminum metal plate was pretreated with thermal oxidation, chemical polishing and electropolishing before anodic oxidation. Membrane thickness, pore size and distribution were examined with several anodizing conditions ; reaction temperature, cumulative charge, electrolyte concentration and current density. Scanning electron microscopy was used to determine pore size, pore density and membrane thickness. The pore size and thickness of membrane were dependent on the cumulative charge, the reaction temperature, the current density and the concentration of sulfuric acid. The membrane pores obtained uniformly had almost straight cylindrical forms having average pore diameter of 20-40 nm and thickness of 30-60μm.

Keywords:Porous Alumina Membrane;Constant Current Mode;Anodic Oxidation;Straight Cylindrical Forms

[References]

Wernick S, Pinner R, "The Surface Treatment of Aluminum and Its Alloys," 4th ed. Robert Draper Ltd., Teddington (1972)
Franklin RW, Stirland DJ, J. Electrochem. Soc., 110, 262 (1963)
Zahavi J, Metzer M, J. Electrochem. Soc., 119, 1479 (1972)
Thomas AW, Whitechead TH, J. Phys. Chem., 35, 27 (1931)
Tayer CS, Tucker JD, Trans. J. Electrochem. Soc., 88, 325 (1945)
Dorsey GA, J. Electrochem. Soc., 116, 466 (1969)
Keller F, Hunter MS, Robinson DL, J. Electrochem. Soc., 100, 411 (1953)
O'Sullivan JP, Wood GC, Proc. Royal Soc. London A, 317, 511 (1970)
Smith AW, J. Electrochem. Soc., 120, 1068 (1973)
Jensen KF, Chem. Eng. Sci., 42, 923 (1987)
Itaya K, Sugawara S, Arai K, Saito S, J. Chem. Eng. Jpn., 17, 514 (1984)
Dalvie S, Baltus K, Ruth E, J. Membr. Sci., 71, 247 (1992)
Itoh N, Kato K, Tsuji T, Hongo M, J. Membr. Sci., 117(1-2), 189 (1996)
Nyquist RA, Kagel RO, "Infrared Spectra of Inorganic Compounds," Academic Press, Inc., p. 208 (1996)

[Referenced By]

[1] Wernick S, Pinner R, "The Surface Treatment of Aluminum and Its Alloys," 4th ed. Robert Draper Ltd., Teddington (1972)

[2] Franklin RW, Stirland DJ, J. Electrochem. Soc., 110, 262 (1963)

[3] Zahavi J, Metzer M, J. Electrochem. Soc., 119, 1479 (1972)

[4] Thomas AW, Whitechead TH, J. Phys. Chem., 35, 27 (1931)

[5] Tayer CS, Tucker JD, Trans. J. Electrochem. Soc., 88, 325 (1945)

[6] Dorsey GA, J. Electrochem. Soc., 116, 466 (1969)

[7] Keller F, Hunter MS, Robinson DL, J. Electrochem. Soc., 100, 411 (1953)

[8] O'Sullivan JP, Wood GC, Proc. Royal Soc. London A, 317, 511 (1970)

[9] Smith AW, J. Electrochem. Soc., 120, 1068 (1973)

[10] Jensen KF, Chem. Eng. Sci., 42, 923 (1987)

[11] Itaya K, Sugawara S, Arai K, Saito S, J. Chem. Eng. Jpn., 17, 514 (1984)

[12] Dalvie S, Baltus K, Ruth E, J. Membr. Sci., 71, 247 (1992)

[13] Itoh N, Kato K, Tsuji T, Hongo M, J. Membr. Sci., 117(1-2), 189 (1996)

[14] Nyquist RA, Kagel RO, "Infrared Spectra of Inorganic Compounds," Academic Press, Inc., p. 208 (1996)