Hierarchical organic-inorganic composites synthesized by electrospinning fibers within a non-conductive and a conductive pre-ceramic gel

Patent metadata

Field	Value
Publication number	US-12398073-B2
Application number	US-202117477892-A
Country	US
Kind code	B2
Filing date	Sep 17, 2021
Priority date	Sep 18, 2020
Publication date	Aug 26, 2025
Grant date	Aug 26, 2025

Abstract

Methods for the production of ceramic composites in which three-dimensional (3D) printed organic polymer fibers are embedded in an amorphous inorganic ceramic matrix are provided. The composites are made by electrospinning the organic polymer fibers and collecting them in a liquid or gel collector. Ceramic precursors added to the liquid collector after the fibers are collected, or present in the gel collector during the electrospinning, are then cured to form a solid ceramic matrix around the organic polymer fibers to produce an organic polymer fiber-reinforced ceramic.

First claim

What is claimed is:

1. A method of making a fiber-reinforced ceramic, the method comprising:
electrospinning a water-insoluble organic polymer fiber;
collecting the electrospun water-insoluble organic polymer fiber in a collector, wherein the collector is a liquid or gel, to disperse the electrospun water-insoluble organic polymer fiber in the collector;
adding inorganic ceramic precursors to the collector, wherein the inorganic ceramic precursors are added to the collector before, during, or after collecting the electrospun water-insoluble organic polymer fiber in the collector;
adding an inorganic curing agent into the collector; and
curing the inorganic ceramic precursors and the inorganic curing agent to form an organic polymer fiber-reinforced ceramic.

2. The method of claim 1 , wherein the inorganic ceramic precursors comprise potassium silicate, sodium silicate, or a mixture thereof, the inorganic curing agent comprises metakaolin, and the organic polymer fiber-reinforced ceramic is an organic polymer fiber-reinforced geopolymer.

3. The method of claim 2 , wherein the organic polymer fiber-reinforced geopolymer has an electrospun water-insoluble organic polymer fiber concentration of least 0.1 weight percent, based on the weight of the geopolymer.

4. The method of claim 2 , wherein the organic polymer fiber-reinforced geopolymer has an electrospun water-insoluble organic polymer fiber concentration in the range from 0.1 weight percent to 1 weight percent, based on the weight of the geopolymer.

5. The method of claim 1 , wherein the water-insoluble organic polymer fiber is a polyacrylonitrile fiber.

6. The method of claim 5 , wherein the inorganic ceramic precursors comprise potassium silicate, sodium silicate, or a mixture thereof, the inorganic curing agent comprises metakaolin, and the organic polymer fiber-reinforced ceramic is a polyacrylonitrile fiber-reinforced geopolymer.

7. The method of claim 1 , wherein the inorganic ceramic precursors are added to the collector after the electrospun water-insoluble organic polymer fiber is dispersed in the collector.

8. The method of claim 7 , wherein the collector consists of only deionized water.

9. The method of claim 7 , wherein the inorganic ceramic precursors comprise potassium silicate, sodium silicate, or a mixture thereof, the inorganic curing agent comprises metakaolin, and the organic-polymer fiber-reinforced ceramic is an organic polymer fiber-reinforced geopolymer.

10. The method of claim 9 , wherein the water-insoluble organic polymer fiber is a polyacrylonitrile fiber.

11. The method of claim 1 , wherein the inorganic ceramic precursors are added to the collector before the electrospun water-insoluble organic polymer fiber is dispersed in the collector.

12. The method of claim 11 , wherein the inorganic ceramic precursors comprise potassium silicate, sodium silicate, or a mixture thereof, the inorganic curing agent comprises metakaolin, and the organic polymer fiber-reinforced ceramic is an organic polymer fiber-reinforced geopolymer.

13. The method of claim 12 , wherein the water-insoluble organic polymer fiber is a polyacrylonitrile fiber.

14. A method of making a fiber-reinforced ceramic, the method comprising:
electrospinning a water-soluble organic polymer fiber;
collecting the electrospun water-soluble organic polymer fiber in a gel collector comprising inorganic ceramic precursors to disperse the electrospun water-soluble organic polymer fiber in the gel collector, wherein the water-soluble organic polymer fiber is not a polyethylene oxide fiber;
adding an inorganic curing agent into the gel collector; and
curing the inorganic ceramic precursors and the inorganic curing agent to form an organic polymer fiber-reinforced ceramic.

15. The method of claim 14 , wherein the inorganic ceramic precursors comprise potassium silicate, sodium silicate, or a mixture thereof, the inorganic curing agent comprises metakaolin, and the organic polymer fiber-reinforced ceramic is an organic polymer fiber-reinforced geopolymer.

16. The method of claim 15 , wherein the water-soluble organic polymer fiber comprises polyacrylamide or poly(methacrylic acid).

17. The method of claim 15 , wherein the organic polymer fiber-reinforced geopolymer has an electrospun organic polymer fiber concentration of least 0.1 weight percent, based on the weight of the geopolymer.

18. The method of claim 15 , wherein the organic polymer fiber-reinforced geopolymer has an electrospun organic polymer fiber concentration in the range from 0.1 weight percent to 1 weight percent, based on the weight of the geopolymer.

Assignees

• Univ Northwestern

Inventors

• Guo Ping
• Akono Ange-Therese
• Xu Yunzhi

Classifications

• C04B16/0658

  Polyacrylonitrile · CPC title

• D01D5/003

  the material being a polymer solution or dispersion (D01D5/0053 takes precedence) · CPC title

• D01F6/18

  from polymers of unsaturated nitriles, e.g. polyacrylonitrile, polyvinylidene cyanide · CPC title

• Y02P40/10

  Production of cement, e.g. improving or optimising the production methods; Cement grinding · CPC title

• C04B28/006

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