Method for preparing bulk C—AlN composite aerogel with high strength and high temperature resistance

Patent metadata

Field	Value
Publication number	US-9869422-B2
Application number	US-201314406685-A
Country	US
Kind code	B2
Filing date	Jun 17, 2013
Priority date	Jun 18, 2012
Publication date	Jan 16, 2018
Grant date	Jan 16, 2018

Abstract

Provided is a method for preparing a bulk C—AlN composite aerogel with high strength and high temperature resistance, which includes: evenly stirring aluminum chloride crystals, water, ethanol and epoxy propane, to obtain a clear aluminum oxide sol solution, then adding formaldehyde and resorcinol to the solution and performing even stirring, to obtain an RF/Al 2 O 3 composite aerogel sol solution, leaving the gel to stand, treating the sample by using a supercritical CO 2 drying method, and finally heat-treating the sample at a high temperature under the condition of nitrogen, to obtain the bulk C—AlN composite aerogel with high strength and high temperature resistance. The composite aerogel prepared by using this method has advantages of high integrity, high specific surface area, intact structure, low heat conductivity, low density, and high strength.

First claim

What is claimed is:

1. A method for preparing a bulk C—AlN composite aerogel with high strength and high temperature resistance, the method comprising the following steps:
(1) evenly stirring aluminum chloride crystals, distilled water, anhydrous ethanol and epoxy propane, to obtain a clear aluminum oxide sol solution;
(2) adding formaldehyde (referred to as F for short) and resorcinol (referred to as R for short) to the aluminum oxide sol solution obtained in Step (1) and performing even stirring, to obtain an RF/Al 2 O 3 composite aerogel sol solution;
(3) pouring the RF/Al 2 O 3 composite aerogel sol solution in Step (2) into a mold for reaction to form a gel;
(4) adding at least one of anhydrous ethanol and deionized water to the gel obtained in Step (3) for aging replacement;
(5) placing the wet gel after aging replacement in Step (4) in an oven at 60° C. to 75° C., aging the wet gel for 5 to 10 d, and then drying the wet gel using a supercritical CO 2 drying method; and
(6) heat-treating the sample after drying in Step (5) under the condition of nitrogen, to obtain the bulk C—AlN composite aerogel with high strength and high temperature resistance;
wherein:
in Step (1), a molar ratio of aluminum chloride crystals, distilled water, anhydrous ethanol and epoxy propane is 1:(50 to 70):(20 to 30):(8 to 13);
in Step (2), a molar ratio of aluminum chloride crystals:resorcinol:formaldehyde is (1 to 5):1:2;
in the supercritical CO 2 drying method of Step (5), CO 2 is used for protection, a reaction temperature is 45° C. to 50° C., pressure of a high pressure reactor is controlled at 8 to 12 MPa, and reaction time is 2 to 3 d; and
in Step (6), a heat treatment temperature ranges from 1500° C. to 1700° C., and heat treatment time is 1 h to 10 h.

2. The preparation method according to claim 1 , wherein in Step (3), time for reaction to form a gel is 2 to 10 h.

3. The preparation method according to claim 1 , wherein in Step (4), the number of times of replacement of the anhydrous ethanol and/or deionized water in the process of aging replacement is 3 to 5, and replacement time is 12 to 24 h each time.

4. The preparation method according to claim 1 , wherein:
in Step (1), the molar ratio of aluminum chloride crystals, distilled water, anhydrous ethanol and epoxy propane is 1:(50 to 70):(20 to 30):(9 to 13);
in the supercritical CO 2 drying method of Step (5), the pressure of the high pressure reactor is controlled at 8 to 11 MPa; and
in Step (6), the heat treatment time is 2 h to 5 h.

5. The preparation method according to claim 1 , wherein:
in Step (3), time for reaction to form a gel is 2 to 10 h; and
in Step (4), the number of times of replacement of the anhydrous ethanol and/or deionized water in the process of aging replacement is 3 to 5, and replacement time is 12 to 24 h each time.

6. The preparation method according to claim 4 , wherein:
in Step (3), time for reaction to form a gel is 2 to 10 h; and
in Step (4), the number of times of replacement of the anhydrous ethanol and/or deionized water in the process of aging replacement is 3 to 5, and replacement time is 12 to 24 h each time.

7. A method for preparing a bulk C—AlN composite aerogel with high strength and high temperature resistance, the method comprising the following steps:
(1) evenly stirring aluminum chloride crystals, distilled water, anhydrous ethanol and epoxy propane, to obtain a clear aluminum oxide sol solution;
(2) adding formaldehyde (referred to as F for short) and resorcinol (referred to as R for short) to the aluminum oxide sol solution obtained in Step (1) and performing even stirring, to obtain an RF/Al 2 O 3 composite aerogel sol solution;
(3) pouring the RF/Al 2 O 3 composite aerogel sol solution in Step (2) into a mold for reaction to form a gel;
(4) adding at least one of anhydrous ethanol and deionized water to the gel obtained in Step (3) for aging replacement;
(5) placing the wet gel after aging replacement in Step (4) in an oven at 60° C. to 75° C., aging the wet gel for 5 to 10 d, and then taking the wet gel out for drying; and
(6) heat-treating the sample after drying in Step (5) under the condition of nitrogen, to obtain the bulk C—AlN composite aerogel with high strength and high temperature resistance;
wherein:
in Step (1), a molar ratio of aluminum chloride crystals, distilled water, anhydrous ethanol and epoxy propane is 1:(50 to 70):(20 to 30):(8 to 13); and
in Step (2), a molar ratio of aluminum chloride crystals:resorcinol:formaldehyde is (3 to 5):1:2..

Assignees

• Nanjing University Of Technology

Inventors

• Shen Xiaodong
• Zhong ya
• Cui Sheng

Classifications

• C01B21/072 Primary

  with aluminium · CPC title

• C04B2235/422

  Carbon · CPC title

• C04B35/581

  based on aluminium nitride · CPC title

• C01B32/00

  Carbon; Compounds thereof (C01B21/00, C01B23/00 take precedence; percarbonates C01B15/10; carbon black C09C1/48) · CPC title

• C04B2235/444

  Halide containing anions, e.g. bromide, iodate, chlorite · CPC title