Effect of Poly(vinylpyrrolidone) As a Stress-Relaxing Additive in Fabrication of PbZrxTi1-xO3 Thin Films Using Sol–Gel Route

We investigated how poly(vinylpyrrolidone) (PVP) suppresses crack generation during fabrication. It was confirmed that PVP plays the role of a stress-relaxing agent by in situ stress development measurement at temperatures from 200 to 300 °C. We found that PVP in the film was removed in two steps and that the residual PVP-decomposition product can be the cause of void generation. It was revealed that Young's modulus of the lead zirconate titanate (PZT) film prepared from PZT–PVP-sol was lower at temperatures from 300 °C to less than that from 400 °C than from PZT-sol during fabrication despite the fact that the each values at 450 °C are almost the same. It implies that PVP suppress crack formation by degrading Young's modulus of the film before crystallization. We obtained a 2-µm-thick PZT film with only 10 coatings and its electrical properties is equivalent to previously reported values obtained using the sol–gel route.

[1]  Takaaki Suzuki,et al.  Characterization of Pb(Zr,Ti)O3 thin films deposited on stainless steel substrates by RF-magnetron sputtering for MEMS applications , 2006 .

[2]  Y. Fukuda,et al.  Dielectric Properties of (111) and (100) Lead-Zirconate-Titanate Films Prepared by Sol-Gel Technique , 1994 .

[3]  Zhitang Song,et al.  Growth of highly (100)-oriented Zr-rich PZT thin films on Pt/Ti/SiO2/Si substrates by a simple sol-gel process , 2000 .

[4]  J. Akedo,et al.  Influence of Carrier Gas Conditions on Electrical and Optical Properties of Pb(Zr, Ti)O3 Thin Films Prepared by Aerosol Deposition Method , 2001 .

[5]  Low Temperature Crystallization and Thick Single Layer of PbTiO3 Thin Film by Metallo-Organic Compound Decomposition with an Additive of PVAC , 2006 .

[6]  R. Whatmore,et al.  SOL-GEL FABRICATION OF PZT THICK FILMS FOR MEMS , 2007 .

[7]  David A. Payne,et al.  Origins and evolution of stress development in sol-gel derived thin layers and multideposited coatings of lead titanate , 1998 .

[8]  K. Maki,et al.  Lowering of crystallization temperature of sol-gel derived Pb(Zr, Ti)O3 thin films , 2000 .

[9]  Qi Zhang,et al.  Development of residual stress in sol-gel derived Pb(Zr,Ti)O3 films: An experimental study , 2008 .

[10]  Nicolas Ledermann,et al.  {1 0 0}-Textured, piezoelectric Pb(Zrx, Ti1−x)O3 thin films for MEMS: integration, deposition and properties , 2003 .

[11]  H. Kozuka,et al.  Effects of the Heat‐Treatment Conditions on the Crystallographic Orientation of Pb(Zr,Ti)O3 Thin Films Prepared by Polyvinylpyrrolidone‐Assisted Sol–Gel Method , 2007 .

[12]  H. Kozuka,et al.  Single‐Step Deposition of Gel‐Derived Lead Zirconate Titanate Films: Critical Thickness and Gel Film to Ceramic Film Conversion , 2004 .

[13]  Masaru Shtmizu,et al.  Preparation of PZT thin films by MOCVD using a new Pb precursor , 1995 .

[14]  H. Kozuka,et al.  Sol–gel preparation of single-layer, 0.75 μm thick lead zirconate titanate films from lead nitrate-titanium and zirconium alkoxide solutions containing polyvinylpyrrolidone , 2001 .

[15]  K. Yao,et al.  Effects of poly(ethylene glycol) additive molecular weight on the microstructure and properties of sol-gel-derived lead zirconate titanate thin films , 2003 .

[16]  T. Doi,et al.  The Orientation and Grain Texture Effect on Life Time Reliability of Sol–Gel Derived PbZr0.52Ti0.48O3 Films , 2012 .

[17]  Takeshi Sawa,et al.  Simplified method for analyzing nanoindentation data and evaluating performance of nanoindentation instruments , 2001 .

[18]  Paul Muralt,et al.  Piezoelectric thin films for MEMS , 1997, Applied Physics Letters.

[19]  Paul Muralt,et al.  Fabrication and characterization of PZT thin-film vibrators for micromotors , 1995 .

[20]  Y. Hishinuma,et al.  Characterization of Nb-doped Pb(Zr,Ti)O3 films deposited on stainless steel and silicon substrates by RF-magnetron sputtering for MEMS applications , 2010 .

[21]  Susan Trolier-McKinstry,et al.  Temperature dependence of the piezoelectric response in lead zirconate titanate films , 2004 .

[22]  I. K. Naik,et al.  Processing and characterization of sol-gel derived very thin film ferroelectric capacitors , 1991 .

[23]  G. Pharr,et al.  An improved technique for determining hardness and elastic modulus using load and displacement sensing indentation experiments , 1992 .

[24]  Paul Muralt,et al.  Growth and properties of gradient free sol-gel lead zirconate titanate thin films , 2007 .

[25]  H. Kozuka,et al.  Single-step sol-gel deposition and dielectric properties of 0.4 μm thick, (001) oriented Pb(Zr,Ti)O3 thin films , 2008 .

[26]  Hidetoshi Kotera,et al.  Crystallographic characterization of epitaxial Pb(Zr,Ti)O3 films with different Zr/Ti ratio grown by radio-frequency-magnetron sputtering , 2003 .

[27]  H. Funakubo,et al.  Effect of Grain Size on Mechanical Properties of Full-Dense Pb(Zr,Ti)O3 Ceramics , 2010 .

[28]  Takashi Nakamura,et al.  Micro-Patterning of PbZrxTi1-xO3 Thin Films Prepared by Photo Sensitive Sol-Gel Solution , 1993 .