Uncalcined geopolymer-based refractory material and method for its preparation

Patent metadata

Field	Value
Publication number	US-11866368-B2
Application number	US-202117474908-A
Country	US
Kind code	B2
Filing date	Sep 14, 2021
Priority date	Sep 14, 2020
Publication date	Jan 9, 2024
Grant date	Jan 9, 2024

Abstract

An uncalcined geopolymer-based refractory material is provided, comprising a matrix of a geopolymer obtainable by polymerization of a mixture consisting of mineral powder, fly ash, and metakaolin; and SiC whiskers embedded in the geopolymer matrix. The material has excellent mechanical properties and high resistance to high temperatures and exhibits a ductile fracture mechanism instead of a brittle fracture mechanism.

First claim

What is claimed is:

1. An uncalcined geopolymer-based refractory material, comprising:
a matrix of a geopolymer obtained by polymerization of a mixture consisting of mineral powder, fly ash, and metakaolin; and
silicon carbide whiskers embedded in the geopolymer matrix, the silicon carbide whiskers being pure silicon carbide whiskers or boron nitride coated silicon carbide whiskers,
wherein a mass ratio of the mineral powder to the fly ash to the metakaolin is in a range of (35-45):(25-35):(25-35).

2. The material of claim 1 , wherein, the silicon carbide whiskers are present in the geopolymer matrix in an amount of 0.8 to 1.2 wt. %.

3. The material of claim 2 , wherein, the silicon carbide whiskers have a diameter of 0.1 to 2.5 μm and a length of 2 to 50 μm.

4. The material of claim 3 , wherein, the boron nitride coated silicon carbide whiskers have a 50 to 250 nm thick boron nitride coating.

5. The material of claim 1 , wherein, the silicon carbide whiskers have a diameter of 0.1 to 2.5 μm and a length of 2 to 50 μm.

6. The material of claim 5 , wherein, the boron nitride coated silicon carbide whiskers have a 50 to 250 nm thick boron nitride coating.

7. The material of claim 1 , wherein, the mineral powder is high-calcium mineral powder and the fly ash is Class F fly ash.

8. A method for preparing the uncalcined geopolymer-based refractory material of claim 1 , the method comprising steps of:
(a) mixing the mineral powder, the fly ash, the metakaolin, and the silicon carbide whiskers by ball milling to form a milled material;
(b) mixing the milled material with a sodium water glass solution and water to form a slurry; and
(c) curing the slurry to obtain the uncalcined geopolymer-based refractory material.

9. The method of claim 8 , further comprising: before the step (a), subjecting the silicon carbide whiskers to a dispersion treatment comprising:
mixing the silicon carbide whiskers with a dispersant solution by ultrasonic vibration, followed by drying;
wherein, the dispersant solution is a 95 wt. % aqueous solution of 2-amino-2-methyl-1-propanol.

10. The method of claim 8 , wherein, in the step (a), the mineral powder, the fly ash, the metakaolin, and the SiC whiskers are ball milled together with zirconium oxide beads having a diameter of 5 mm at a rotation speed of 150 rpm for 25 min.

11. The method of claim 8 , wherein, the sodium water glass used in the step (b) has an SiO 2 /Na 2 O modulus in the range from 1.5 to 3.5, and wherein, a ratio of a mass of sodium silicate in the sodium water glass solution to a total mass of the mineral powder, the fly ash, and the metakaolin is 0.15:1, and a ratio of a total mass of the water used and the water in the sodium water glass solution to a total mass of the mineral powder, the fly ash, and the metakaolin is 0.4:1.

12. The method of claim 8 , wherein, in the step (c), the slurry obtained in the step (b) is cured by placing it in a mold inside a curing chamber for 24 h at 95±5% relative humidity and 23±0.5° C. and then maintaining it inside the curing chamber after removal from the mold for 7 days under the same temperature and humidity conditions.

13. The method of claim 8 , wherein, the silicon carbide whiskers are present in the geopolymer matrix in an amount of 0.8 to 1.2 wt. %.

14. The method of claim 13 , wherein, the silicon carbide whiskers are composed of pure silicon carbide only or boron nitride coated silicon carbide, and have a diameter of 0.1 to 2.5 μm and a length of 2 to 50 μm.

15. The method of claim 14 , wherein, the boron nitride coated silicon carbide whiskers have a 50 to 250 nm thick boron nitride coating.

16. The method of claim 13 , further comprising: before the step (a), subjecting the silicon carbide whiskers to a dispersion treatment comprising:
mixing the silicon carbide whiskers with a dispersant solution by ultrasonic vibration, followed by drying;
wherein, the dispersant solution is a 95 wt % aqueous solution of 2-amino-2-methyl-1-propanol.

17. The method of claim 8 , wherein, the silicon carbide whiskers are composed of pure silicon carbide only or boron nitride coated silicon carbide, and have a diameter of 0.1 to 2.5 μm and a length of 2 to 50 μm.

18. The method of claim 17 , wherein, the boron nitride coated silicon carbide whiskers have a 50 to 250 nm thick boron nitride coating.

19. The method of claim 17 , further comprising: before the step (a), subjecting the silicon carbide whiskers to a dispersion treatment comprising:
mixing the silicon carbide whiskers with a dispersant solution by ultrasonic vibration, followed by drying;
wherein, the dispersant solution is a 95 wt % aqueous solution of 2-amino-2-methyl-1-propanol.

20. The method of claim 8 , wherein, the mineral powder is high-calcium mineral powder and the fly ash is Class F fly ash; and wherein a mass ratio of mineral powder:fly ash metakaolin is (35-45):(25-35):(25-35).

Assignees

• Univ Shenzhen

Inventors

• Xing Feng
• Fang Yuan
• Wang Aoxuan

Classifications

• C04B28/006 Primary

  containing mineral polymers, e.g. geopolymers of the Davidovits type · CPC title

• C04B14/324

  Silicon carbide · CPC title

• C04B14/383

  Whiskers · CPC title

• C04B35/66 Primary

  Monolithic refractories or refractory mortars, including those whether or not containing clay {(making or repairing of linings F27D1/16)} · CPC title

• C04B2235/349

  Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite · CPC title