Methods of fabricating barium titanate powders

• US 7,182,930 B2
• Filed: 06/18/2004
• Issued: 02/27/2007
• Est. Priority Date: 06/18/2004
• Status: Active Grant

• Current Assignee: National Chung-Shan Institute of Science and Technology
• Original Assignee: Chung-Shan Institute of Science & Technology Armaments Bureau MND (Government of The Republic of China)
• Inventors: Tsay, Ming-Tseh, Lin, Pao-Yen, Shih, Zong-Whie
• Primary Examiner(s): Vanoy; Timothy C.
• Application Number:
  US10/870,463
• Publication Number:
  US 20050281733A1
• Time in Patent Office: 984 Days
• Field of Search: 423/598, 423/594.16, 423/69, 423/70, 423/71, 423/155, 423/157, 501/137
• US Class Current: 423/598
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C01G 23/006 Alkaline earth titanates
• CPC Class Codes: C01P 2002/72 by d-values or two theta-values, e.g. as X-ray diagram
• CPC Class Codes: C01P 2004/03 obtained by SEM
• CPC Class Codes: C01P 2004/64 Nanometer sized, i.e. from 1-100 nanometer
• CPC Class Codes: C01P 2006/12 Surface area
• CPC Class Codes: C01P 2006/13 thermal stability thereof at high temperatures
• CPC Class Codes: C04B 35/4682 based on BaTiO3 perovskite phase
• CPC Class Codes: C04B 35/62655 Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying

Abstract

A method of fabricating barium titanate powders uses titanium tetrachloride and barium hydroxide as reactants in a reaction solution. The pH value of the reaction solution is adjusted to strongly alkaline range by adding potassium hydroxide. Nitrogen is charged into a reaction tank at normal pressure, and the reaction solution is heated at 80–102°. The solution is intensively stirred at constant temperature, and then subjected to a hydro-thermal reflux. Then, the solution is treated through an ion exchange resin and dried to obtain a cubic BaTiO₃ powders.

Claims

1. A method of fabricating barium titanate powders made from titanium tetrachloride and barium hydroxide as raw materials, comprising:

(a) providing a titanium tetrachloride solution;

(b) adding excess ammonium aqueous solution into the titanium tetrachloride solution;

(c) adding a barium hydroxide aqueous solution into the titanium tetrachloride solution;

(d) adding a potassium hydroxide into the titanium tetrachloride solution to adjust the pH value of the titanium tetrachloride solution into a strongly alkaline range;

(e) heating the titanium tetrachloride solution to a reaction temperature at normal pressure in a nitrogen-containing environment, and performing a stable hydro-thermal reflux reaction for the titanium tetrachloride solution; and

(f) after the hydro-thermal reflux reaction is completed, a product thereof is treated by an ion exchange resin until the product is substantially neutral, and then is dried to obtain barium titanate powders.

2. The method of claim 1, wherein at the step (a), the titanium tetrachloride solution has a concentration of 5–

20 wt %.

3. The method of claim 1, wherein at the step (b), the ammonium aqueous solution has a concentration of 20–

28 wt %.

4. The method of claim 1, wherein at the step (b), the molar ratio of ammonium to titanium tetrachloride is in the range of 4–

8.

5. The method of claim 1, wherein at the step (c), the molar ratio of barium hydroxide to titanium tetrachioride is between 1˜

1.4.

6. The method of claim 1, wherein at the step (d), the potassium hydroxide is in solid state with an amount that is enough to make pH value of the titanium tetrachloride solution larger than 12.

7. The method of claim 1, wherein at the step (e), the reaction temperature of the hydro-thermal reflux ranges from 80 to 102°

.

8. The method of claim 1, wherein at the step (e), the reaction time of the hydro-thermal reflux ranges from 1 to 5 hours.

9. The method of claim 1, wherein at the step (f), the drying temperature ranges from 100 to 120°

.