Method for production of mono-dispersed and crystalline TiO.sub.2 ultrafine powders for aqueous TiOCl.sub.2 solution using homogeneous precipitation

• US 6,001,326 A
• Filed: 09/28/1998
• Issued: 12/14/1999
• Est. Priority Date: 07/16/1998
• Status: Expired due to Term

• Current Assignee: Korea Atomic Energy Research Institute (Government of The Republic of Korea)
• Original Assignee: Korea Atomic Energy Research Institute (Government of The Republic of Korea)
• Inventors: Jeong, Yong Hwan, Kim, Kyeong Ho, Park, Soon Dong, Kim, Sun-Jae, Kuk, Il Hiun
• Primary Examiner(s): Straub, Gary P.
• Assistant Examiner(s): Nguyen, Cam N.
• Application Number:
  US09/162,009
• Time in Patent Office: 442 Days
• Field of Search: 423/598, 423/608, 423/610, 423/611, 423/612
• US Class Current: 423/598
• CPC Class Codes: C01G 23/0536 by hydrolysing chloride-containing salts
• CPC Class Codes: C01P 2004/03 obtained by SEM
• CPC Class Codes: C01P 2004/52 highly monodisperse size distribution
• CPC Class Codes: C01P 2006/12 Surface area

Abstract

A method for production of mono-dispersed and crystalline titanium dioxide ultra fine powders comprises preparing an aqueous titanyl chloride solution, diluting the aqueous titanyl chloride solution to a concentration of between about 0.2 to 1.2 mole and heating the diluted aqueous titanyl chloride solution and maintaining the solution in a temperature range of between 15 to 155° C. to precipitate titanium dioxide. The aqueous titanyl chloride solution is prepared by adding ice pieces of distilled water or icing distilled water to undiluted titanium tetrachloride.

Claims

1. A method for production of mono-dispersed and crystalline titanium dioxide (TiO₂) ultrafine powders comprising the steps of:

(a) preparing an aqueous titanyl chloride (TiOCl₂) solution in a concentration of greater than or equal to 1.5M, by adding ice pieces of distilled water or icy distilled water to the undiluted titanium tetrachloride (TiCl₄);

(b) diluting the above aqueous titanyl chloride solution to a specific concentration within the range of 0.2 to 1.2M by adding an adequate amount of distilled water;

(c) obtaining crystalline titanium dioxide, which precipitates, by heating the above diluted aqueous titanyl chloride solution and maintaining the temperature within a range of 15-155°

C.; and

(d) fabricating the mono-dispersed and crystalline titanium dioxide ultrafine powders by filtrating, washing and drying the above titanium dioxide precipitates.

2. The method for production of mono-dispersed and crystalline titanium dioxide ultrafine powders according to claim 1, wherein the precipitation reaction of (c) step is carried out with the addition of ethanol of higher than or equal to 1 volume % after (b) step.

3. The method for production of mono-dispersed and crystalline titanium dioxide ultrafine powders according to claim 2, wherein the added ethanol is evaporated completely during (c) step.

4. The method for production of mono-dispersed and crystalline titanium dioxide ultrafine powders according to claim 1, wherein pressure of higher than 4 bar is applied to the titanium dioxide precipitates for 48 hours or more between (c) step and (d) step.

5. A method for production of mono-dispersed and crystalline titanium dioxide ultrafine powders comprising the steps of:

(a) preparing an aqueous titanyl chloride solution in a concentration of greater than or equal to 1.5M, by adding ice pieces of distilled water or icy distilled water to the undiluted titanium tetrachloride;

(b) diluting the above aqueous titanyl chloride solution to a specific concentration within the range of 0.2 to 1.2M with an adequate amount of distilled water;

(c) obtaining crystalline titanium dioxide, which precipitates, by heating the above diluted aqueous titanyl chloride solution and maintaining the temperature within a range of 75-155°

C. for 20 minutes to 3 hours; and

(d) fabricating the mono-dispersed and crystalline titanium dioxide ultrafine powders by filtrating, washing and drying the above titanium dioxide precipitates.

6. The method for production of mono-dispersed and crystalline titanium dioxide ultrafine powders according to claim 5, wherein the precipitation reaction of (c) step is carried out with the addition of ethanol of higher than or equal to 1 volume % after (b) step.

7. The method for production of mono-dispersed and crystalline titanium dioxide ultrafine powders according to claim 6, wherein the added ethanol is evaporated completely during (c) step.

8. The method for production of mono-dispersed and crystalline titanium dioxide ultrafine powders according to claim 5, wherein pressure of higher than 4 bar is applied to the titanium dioxide precipitates for 48 hours or more between (c) step and (d) step.

9. A method for production of mono-dispersed and crystalline titanium dioxide ultrafine powders comprising the steps of;

(a) preparing an aqueous titanyl chloride solution in a concentration of greater than or equal to 1.5M, by adding ice pieces of distilled water or icy distilled water to the undiluted titanium tetrachloride;

(b) diluting the above aqueous titanyl chloride solution to a specific concentration within the range of 0.2 to 1.2M with an adequate amount of distilled water;

(c) obtaining crystalline titanium dioxide, which precipitates, by heating the above diluted aqueous titanyl chloride solution and maintaining the temperature within a range of 15-70°

C. for 2 to 60 hours; and

(d) fabricating the mono-dispersed and crystalline titanium dioxide ultrafine powders by filtrating, washing and drying the above titanium dioxide precipitates.

10. The method for production of mono-dispersed and crystalline titanium dioxide ultrafine powders according to claim 9, wherein the precipitation reaction of (c) step is carried out with the addition of ethanol of higher than or equal to 1 volume % after (b) step.

11. The method for production of mono-dispersed and crystalline titanium dioxide ultrafine powders according to claim 10, wherein the added ethanol is evaporated completely during (c) step.

12. The method for production of mono-dispersed and crystalline titanium dioxide ultrafine powders according to claim 9, wherein pressure of higher than 4 bar is applied to the titanium dioxide precipitates for 48 hours or more between (c) step and (d) step.