Process for preparing fine powder of perovskite-type compound

• US 5,445,806 A
• Filed: 03/04/1992
• Issued: 08/29/1995
• Est. Priority Date: 08/21/1989
• Status: Expired due to Fees

• Current Assignee: Tayca Corporation
• Original Assignee: Tayca Corporation
• Inventors: Kinugasa, Masanori, Tsubomoto, Naoto, Kobayashi, Osamu
• Primary Examiner(s): BOS, STEVEN J
• Application Number:
  US07/845,670
• Time in Patent Office: 1,273 Days
• Field of Search: 423/593, 423/594, 423/598
• US Class Current: 423/598
• CPC Class Codes: C01B 13/363 Mixtures of oxides or hydroxides by precipitation
• CPC Class Codes: C01G 23/003 Titanates C01G23/001 takes precedence
• CPC Class Codes: C01G 23/006 Alkaline earth titanates
• CPC Class Codes: C01G 25/006 Compounds containing, besides zirconium, two or more other elements, with the exception of oxygen or hydrogen
• CPC Class Codes: C01G 30/00 Compounds of antimony
• CPC Class Codes: C01G 30/026 containing at least two metals
• CPC Class Codes: C01G 33/00 Compounds of niobium
• CPC Class Codes: C01G 49/009 Compounds containing, besides iron, two or more other elements, with the exception of oxygen or hydrogen
• CPC Class Codes: C01P 2002/34 perovskite-type (ABO3)
• CPC Class Codes: C01P 2002/72 by d-values or two theta-values, e.g. as X-ray diagram
• CPC Class Codes: C01P 2002/77 by unit-cell parameters, atom positions or structure diagrams
• CPC Class Codes: C01P 2004/03 obtained by SEM
• CPC Class Codes: C01P 2004/52 highly monodisperse size distribution
• CPC Class Codes: C01P 2004/62 Submicrometer sized, i.e. from 0.1-1 micrometer
• CPC Class Codes: C01P 2006/32 Thermal properties
• CPC Class Codes: C01P 2006/80 Compositional purity

Abstract

A process for preparing a fine powder of perovskite-type compounds having an average particle size of at most 0.3 μm and uniform particle sizes, which comprises subjecting to a reaction an aqueous solution of a mixture of at least one compound selected from group A element compounds comprising alkaline earth metal elements and/or bivalent metal elements with at least one compound selected from group B element compounds comprising tetravalent metal elements such as Ti, Zr, Hf and Sn and/or composite metal elements composed of a bivalent or trivalent metal element such as Zn, Ni, Co, Mg, Fe or Sb and a pentavalent metal element such as Nb or Sb in an A/B atomic ratio of more than 1, calcining the resulting powdery reaction product at a temperature which is lower than the temperature at which the growth of particles takes place and which is higher than the temperature at which the growth of particles takes place when A/B is 1, and cleaning the calcined product with an acid solution to remove the excess group A elements. The process provides fine powders of perovskite-type compounds having a good crystallinity, particularly tetragonal barium titanate, which are useful particularly as raw materials of ceramics for electronic devices.

Claims

1. A process for preparing a fine powder of tetragonal crystalline barium titanate having an average particle size of at most 0.3 μ

m, which comprises reacting an aqueous solution of a mixture of a compound containing Ba and a compound containing Ti in a Ba/Ti atomic ratio of 1.02-1.40, obtaining a powdery reaction product of barium titanate, calcining the powder reaction product having a Ba/Ti atomic ration of 1.02-1.40 at a temperature of 1,000°

to 1,100°

C., and removing excess Ba element from a resulting calcined product.

2. The process of claim 1, wherein the Ba compound is an hydroxide or oxide, and the Ti compound is an hydroxide or oxide.

3. The process of claim 1, wherein the Ba compound tis an hydroxide or oxide, and the Ti compound is an organometallic compound.

4. The process of claim 1, wherein the Ba compound is an organometallic compound, and the Ti compound is an hydroxide or oxide.

5. The process of claim 1, wherein the Ba compound is an organometallic compound, and the Ti compound is an organometallic compound.

6. The process of claim 1, wherein the Ba compound is barium hydroxide and the Ti compound is hydrated titanium oxide.

7. The process of claim 1, wherein the Ba compound is barium hydroxide, the Ti compound is hydrated titanium oxide, and the tetragonal barium titanate has an average particle size of 0.05 to 0.3 μ

m.

8. The process of claim 7, wherein the Ba/Ti atomic ratio of the powdery reaction product is from 1.02 to 1.04.

9. The process of claim 7, wherein a c/a ratio of said tetragonal barium titanate calculated from (002) and (200) peaks by X-ray diffraction pattern is not less than 1.009.

10. The process of claim 1, wherein the calcining converts the resulting powdery reaction product into a tetragonal system crystalline structure.

11. The process of claim 1, wherein the calcined product has an average particle size of at most 0.3 μ

m.

12. The process of claim 1, wherein tetragonal barium titanate has an average particle size of 0.05 to 0.3 μ

m.