Thick self-organized porous zirconium oxide formed in H2SO4/NH4F electrolytes

Abstract We report the formation of self-organized porous layer of ZrO 2 by anodization of zirconium in H 2 SO 4 electrolytes containing low concentrations of NH 4 F. Under optimized electrolyte conditions and polarization in range of several 10 V, ordered sponge-like porous ZrO 2 is obtained. The pores typically have a diameter ranged from 10 to 100 nm. Most remarkably the porous ZO 2 layers can reach thickness in the order of several 10 μm. The pore size is almost independent of the applied potential, whereas the amount of well-structured area on the sample surface increases with a higher applied potential.

[1]  M. Lohrengel,et al.  Nucleation and growth of anodic oxide films , 1983 .

[2]  G. Thompson,et al.  Porous anodic alumina: fabrication, characterization and applications , 1997 .

[3]  P. Schmuki,et al.  Electrochemical formation of porous superlattices on n-type (1 0 0) InP , 2003 .

[4]  H. Föll,et al.  Formation Mechanism and Properties of Electrochemically Etched Trenches in n‐Type Silicon , 1990 .

[5]  Hideki Hasegawa,et al.  Formation of 〈001〉-aligned nano-scale pores on (001) n-InP surfaces by photoelectrochemical anodization in HCl , 1999 .

[6]  Heon-Cheol Shin,et al.  Porous Tin Oxides Prepared Using an Anodic Oxidation Process , 2004 .

[7]  Kenji Fukuda,et al.  Ordered Metal Nanohole Arrays Made by a Two-Step Replication of Honeycomb Structures of Anodic Alumina , 1995, Science.

[8]  Craig A. Grimes,et al.  Titanium oxide nanotube arrays prepared by anodic oxidation , 2001 .

[9]  T. Oishi,et al.  Formation of Porous TiO 2 by Anodic Oxidation and Chemical Etching of Titanium , 2000 .

[10]  G. Stucky,et al.  Highly Ordered Porous Zirconias from Surfactant-Controlled Syntheses: Zirconium Oxide−Sulfate and Zirconium Oxo Phosphate , 1999 .

[11]  Jian Yu,et al.  Synthesis of titanium-doped ordered porous zirconium oxide with high-surface-area , 2000 .

[12]  Andreas Stein,et al.  Synthesis of highly ordered, three-dimensional, macroporous structures of amorphous or crystalline inorganic oxides, phosphates, and hybrid composites , 1999 .

[13]  D. Stoychev,et al.  XPS and SEM characterization of zirconia thin films prepared by electrochemical deposition , 2000 .

[14]  S. Fujimoto,et al.  Morphological characterization of porous InP superlattices , 2004 .

[15]  M. A. Miller,et al.  Transmission and scanning electron microscopy of oxides anodically formed on zircaloy-2 , 1977 .

[16]  B. Cox Factors Affecting the Growth of Porous Anodic Oxide Films on Zirconium , 1970 .

[17]  Marc Aucouturier,et al.  Structure and physicochemistry of anodic oxide films on titanium and TA6V alloy , 1999 .

[18]  Frank Müller,et al.  Self-Organized Formation of Hexagonal Pore Structures in Anodic Alumina , 1998 .