Thermistor material and method of preparing the same

Patent metadata

Field	Value
Publication number	US-9805847-B2
Application number	US-201414762078-A
Country	US
Kind code	B2
Filing date	Jan 24, 2014
Priority date	Jan 30, 2013
Publication date	Oct 31, 2017
Grant date	Oct 31, 2017

Abstract

A thermistor material and a method for preparing a thermistor material are provided. The thermistor material is prepared by mixing and heating a mixture containing BaTiO 3 , B 2 O 3 , SiO 2 , Li 2 O, P 2 O 5 , Cs 2 O, Nd 2 O 3 , Al 2 O 3 and TiO 2 .

First claim

What is claimed is:

1. A method for preparing a thermistor material, comprising steps of:
providing a first mixture comprising BaTiO 3 , B 2 O 3 , SiO 2 , Li 2 O, P 2 O 5 , Cs 2 O and Nd 2 O 3 , wherein with respect to 100 weight parts of the first mixture, BaTiO 3 is about 94.85 weight parts to about 97.75 weight parts, B 2 O 3 is about 0.4 weight parts to about 2.5 weight parts, SiO 2 is about 0.5 weight parts to about 0.9 weight parts, Li 2 O is about 0.08 weight parts to about 0.2 weight parts, P 2 O 5 is about 0.2 weight parts to about 0.3 weight parts, Cs 2 O is about 0.6 weight parts to about 0.725 weight parts, and Nd 2 O 3 is about 0.325 weight parts to about 0.565 weight parts;
sintering the first mixture at about 800 degree Celsius to about 900 degree Celsius to form a first powder material;
mixing the first powder material with a second mixture comprising Al 2 O 3 and TiO 2 , wherein with respect to 100 weight parts of BaTiO 3 , Al 2 O 3 is about 0.06 weight parts to about 0.08 weight parts, and TiO 2 is about 0.07 weight parts to about 0.08 weight parts to form a second power material;
granulating, pelleting and molding the second powder material to form a molded material; and
subjecting the molded material to a heat treatment.

2. The method of claim 1 , further comprising:
subjecting the first mixture to milling prior to the sintering step, and
subjecting the second power material to milling prior to the granulating step.

3. The method of claim 1 , wherein in the mixing step, the first powder material is mixed with the second mixture and a sintering additive.

4. The method of claim 3 , wherein the sintering additive comprises an acid silica sol.

5. The method of claim 1 , wherein the granulating step is performed by using an organic binder.

6. The method of claim 5 , wherein the organic binder comprises a polyvinyl alcohol solution having a concentration of about 5 wt % to about 6 wt %, and with respect to 100 weight parts of the second powder material, the polyvinyl alcohol solution is about 0.1 weight parts to about 0.2 weight parts.

7. The method of claim 1 , wherein the heat treatment comprises:
a first heat treatment at a first temperature of about 580 degree Celsius to about 600 degree Celsius;
a second heat treatment at a second temperature of about 1150 degree Celsius to about 1180 degree Celsius;
a third heat treatment at a third temperature of about 1200 degree Celsius to about 1270 degree Celsius; and
a fourth heat treatment at a fourth temperature of about 1100 degree Celsius to about 1175 degree Celsius.

8. The method of claim 7 , wherein the first heat treatment is performed for about 60 minutes to about 120 minutes, the second heat treatment is performed for about 20 minutes to about 40 minutes, the third heat treatment is performed for about 50 minutes to about 70 minutes, and the fourth heat treatment is performed for about 50 minutes to about 70 minutes.

9. The method of claim 7 , wherein the first temperature is achieved with a temperature increasing rate of about 4.0° C./min to about 5.2° C./min, the third temperature is achieved with a temperature increasing rate of about 3.0° C./min to about 10° C./min, and the fourth temperature is achieved with a temperature decreasing rate of about 1.1° C./min to about 3.5° C./min.

10. The method of claim 7 , wherein the heat treatment further comprises:
a fifth heat treatment at about 600 degree Celsius to about 610 degree Celsius for about 90 minutes to about 110 minutes.

11. The method of claim 1 , wherein the sintering step comprises:
a first sintering at a fifth temperature of about 500 degree Celsius to about 620 degree Celsius, and
a second sintering at a sixth temperature of about 800 degree Celsius to about 900 degree Celsius.

12. The method of claim 11 , wherein the first sintering step is performed for about 50 minutes to about 70 minutes, the second sintering step is performed for about 60 minutes to about 70 minutes, and the fifth temperature is increased to the sixth temperature with a temperature increasing rate of about 4.2° C./min to about 5.2° C./min.

13. The method of claim 1 , wherein the granulating step is carried out via spray granulation, and in the granulating step, the second powder material is granulated into granulated particles having an average diameter of about 200 μm to about 1000 μm.

14. The method of claim 1 , wherein the pelleting step is carried out under a pressure of about 20 MPa to about 30 MPa.

15. The method of claim 1 , further comprising steps of:
maintaining at a seventh temperature of about 1125 degree Celsius to about 1250 degree Celsius for about 1 hour to about 1.5 hours; and
cooling.

16. The method of claim 15 , wherein the seventh temperature is achieved with a temperature increasing rate of about 250° C./h to about 300° C./h, and the cooling step is performed with a temperature decreasing rate of about 300° C./h to about 350° C./h.

17. The method of claim 1 , wherein the BaTiO 3 is prepared by steps of:
mixing a barium salt, a titanate and an oxalic acid solution under a pH of about 2.5 to about 3.5 to form a first solution;
subjecting the first solution to co-precipitation to form a titanium barium oxalate precursor; and
calcinating the titanium barium oxalate precursor at about 720 degree Celsius to about 820 degree Celsius for about 0.8 hours to about 1.2 hours.

18. A thermistor material prepared by mixing and heating a mixture, wherein the mixture comprises BaTiO 3 , B 2 O 3 , SiO 2 , Li 2 O, P 2 O 5 , Cs 2 O, Nd 2 O 3 , Al 2 O 3 and TiO 2 ,
wherein with respect to 100 weight parts of BaTiO 3 , B 2 O 3 is about 1.05 weight parts to about 2.64 weight parts, SiO 2 is about 0.52 weight parts to about 0.94 weight parts, Li 2 O is about 0.084 weight parts to about 0.21 weight parts, P 2 O 5 is about 0.21 weight parts to about 0.32 weight parts, Cs 2 O is about 0.63 weight parts to about 0.764 weight parts, Nd 2 O 3 is about 0.343 weight parts to about 0.596 weight parts, Al 2 O 3 is about 0.06 weight parts to about 0.08 weight parts, and TiO 2 is about 0.04 weight parts to about 0.08 weight parts.

19. The thermistor material of claim 18 , wherein with respect to 100 weight parts of BaTiO 3 , B 2 O 3 is about 1.08 weight parts to about 2.60 weight parts, SiO 2 is about 0.55 weight parts to about 0.90 weight parts, Li 2 O is about 0.088 weight parts to about 0.20 weight parts, P 2 O 5 is about 0.25 weight parts to about 0.30 weight parts, Cs 2 O is about 0.65 weight parts to about 0.75 weight parts, Nd 2 O 3 is about 0.35 weight parts to about 0.55 weight parts, Al 2 O 3 is about 0.06 weight parts to about 0.08 weight parts, and TiO 2 is about 0.04 weight parts to about 0.08 weight parts.

Assignees

• Byd Co Ltd

Inventors

• Zhao Yanshuai
• Zhou Wei

Classifications

• H01C17/06533

  composed of oxides · CPC title

• C04B35/62685

  characterised by the order of addition of constituents or additives · CPC title

• C04B2235/5427

  millimeter or submillimeter sized, i.e. larger than 0,1 mm · CPC title

• C04B2235/3201

  Alkali metal oxides or oxide-forming salts thereof · CPC title

• C04B2235/6567

  Treatment time · CPC title