Method for preparing infrared radiation ceramic material

Patent metadata

Field	Value
Publication number	US-12391618-B2
Application number	US-202217703052-A
Country	US
Kind code	B2
Filing date	Mar 24, 2022
Priority date	Mar 24, 2021
Publication date	Aug 19, 2025
Grant date	Aug 19, 2025

Abstract

A method for preparing an infrared radiation ceramic material includes mixing and ball milling raw materials of Fe 2 O 3 , MnO 2 and CuO in a mass ratio to obtain a mixed powder; pressing the mixed powder; adjusting laser spot, laser power and laser sintering time of a laser; irradiating or sintering by a first laser the pressed mixed powder in a crucible for a high-temperature solid-phase reaction to obtain an AB 2 O 4 type ferrite powder; obtaining a first mixture by mixing the AB 2 O 4 type ferrite powder and a cordierite powder in a mass ratio; adding a sintering aid and a nucleating agent for ball milling; obtaining a second mixture by mixing the first mixture and a binder for aging; pressing the second mixture; and irradiating or sintering the pressed second mixture by a second laser to obtain the infrared radiation ceramic material.

First claim

What is claimed is:

1. A method for preparing an infrared radiation ceramic material, comprising: mixing and ball milling raw materials of Fe 2 O 3 , MnO 2 and CuO in a mass ratio of x:(9-y):y to obtain a mixed powder, where 0<x<9, and 0<y<9; pressing the mixed powder; irradiating or sintering by a first laser with a first irradiating parameter the pressed mixed powder in a first crucible for a solid-phase reaction to obtain an AB 2 O 4 type ferrite powder; obtaining a first mixture by mixing the AB 2 O 4 type ferrite powder and a cordierite powder in a mass ratio of m:(100-m), where 0<m<100, and adding 0 to 5% of each of a sintering aid and a nucleating agent based on a total mass percent of the raw materials material for ball milling; obtaining a second mixture by mixing the first mixture with 1% to 5% of a binder based on the total mass percent of the raw materials and aging for 10 h or more; pressing the second mixture; and irradiating or sintering by a second laser with a second irradiating parameter the pressed second mixture in a second copper crucible for a solid-phase reaction to obtain the infrared radiation ceramic material, wherein each of the first irradiating parameter and the second irradiating parameter comprises at least one of laser spot, laser power and laser sintering time.

2. The method according to claim 1 , further comprising:
drying the raw materials of Fe 2 O 3 , MnO 2 and CuO at a temperature of 75° C. to 85° C. for 2 h or more,
wherein the mass ratio of Fe 2 O 3 , MnO 2 and CuO is such that the mixed powder comprises one or more of MnFe 2 O 4 , CuFe 2 O 4 , CuMn 2 O 4 , FeFe 2 O 4 and FeMn 2 O 4 .

3. The method according to claim 1 , wherein mixing and ball milling raw materials of Fe 2 O 3 , MnO 2 and CuO in a mass ratio of x:(9-y):y to obtain the mixed powder comprises:
dry ball milling the raw materials to obtain the mixed powder.

4. The method according to claim 1 , wherein mixing and ball milling raw materials of Fe 2 O 3 , MnO 2 and CuO in a mass ratio of x:(9-y):y to obtain the mixed powder comprises:
wet ball milling the raw materials with anhydrous ethanol, n-heptane, acetone or deionized water as a medium for 5 h or more in a ball milling tank, wherein a volume of the raw materials is not more than two thirds of a volume of the ball milling tank;
drying the ball milled materials at a temperature of 75° C. to 85° C. for 3 h or more to obtain the mixed powder; and
grinding the mixed powder evenly.

5. The method according to claim 1 , wherein ball milling is performed by a ball mill at a milling speed of 300 to 600 r/min, and a mass ratio of a milling ball to powders is 10:1 to 60:1.

6. The method according to claim 1 , wherein the binder comprises one or more of polyvinyl alcohol, methyl cellulose, polyhedral silsesquioxane, water glass, W-6C powder molding glue, hyperborosilicate, methoxysilane, polyurethane and silicone.

7. The method according to claim 1 , wherein each of the sintering aid and the nucleating agent comprises one or more of TiO 2 , TiC, ZnO, CeO 2 , and ZrO 2 .

8. The method according to claim 1 , wherein pressing is performed by hydraulic pressing at a pressure of 2 MPa to 15 MPa for 3 s to 10 s, or by isostatic pressing at a pressure of 100 MPa to 300 MPa for 3 s to 10 s.

9. The method according to claim 1 , further comprising:
removing the binder by heating the second mixture to a temperature of 300° C. to 500° C. at a heating rate of 2 to 5° C./min and maintaining the temperature for 10 to 24 h in a muffle furnace; or
removing the binder by laser irradiation with a spot diameter of 10 mm to 15 mm under a laser power of 30 W or less for 5 min to 20 min.

10. The method according to claim 1 , wherein irradiating and sintering is performed in at least one of vacuum, air, nitrogen, oxygen and argon;
wherein the laser spot is configured to cover a sample; and
wherein each of the first laser and second laser comprises a gas laser, a solid laser, a semiconductor diode laser, a fuel laser, a fiber laser, a free electron laser, or a diode-pumped solid laser.

11. The method according to claim 1 , wherein each of the first laser and the second laser power is in a range of 30 W to 1500 W).

12. The method according to claim 11 , wherein each of the first laser and the second laser power is in a range of 60 W to 200 W).

13. The method according to claim 1 , wherein each of the first laser and the second laser sintering time is in a range of 5 s to 20 min).

14. The method according to claim 13 , wherein each of the first laser and the second laser sintering time is in a range of 30 s to 3 min.

15. The method according to claim 1 , wherein irradiating or sintering is performed through laser with a wavelength of 900 to 1000 nm.

16. The method according to claim 15 , wherein irradiating or sintering is performed through laser with a wavelength of 980 nm.

17. The method according to claim 1 , further comprising:
cooling the AB 2 O 4 type ferrite powder or the infrared radiation ceramic material by room temperature cooling, liquid ammonia quenching or liquid nitrogen quenching.

18. The method according to claim 1 , wherein the infrared radiation ceramic material has a particle size of 0.1 μm to 2 μm.

19. The method according to claim 1 , wherein the first crucible comprises a copper crucible, an iron crucible, a ceramic crucible, or a corundum crucible.

20. The method according to claim 1 , wherein the first crucible is placed on a sample stage movable in at least one of x, y and z directions for continuous scanning sintering in a 3D printing mode.

Assignees

• Yunnan Huapu Quantum Mat Co Ltd
• Roi Optoelectronics Tech Co Ltd
• Chongqing Institute Of East China Normal Univ
• Univ East China Normal

Inventors

• Zeng Heping
• Hu Mengyun
• Shi shencheng

Classifications

• C04B2235/665

  Local sintering, e.g. laser sintering · CPC title

• C04B2235/658

  Atmosphere during thermal treatment · CPC title

• C04B2235/5445

  submicron sized, i.e. from 0,1 to 1 micron · CPC title

• C04B2235/5436

  micrometer sized, i.e. from 1 to 100 micron · CPC title

• C04B2235/3281

  Copper oxides, cuprates or oxide-forming salts thereof, e.g. CuO or Cu2O · CPC title