IP Library Granted Patent US 9,666,878
Granted Patent B2
US 9,666,878 · App. 14/801,438 · Granted May 30, 2017

Method for fabricating catalytic 3D network material

Inventors: Chun-Hsien Tsai (Miaoli County, TW); Ting-Chuan Lee (Miaoli County, TW); Chun-Jung Tsai (Miaoli County, TW); Ching-Tung Hsu (Miaoli County, TW); Chia-Hung Li (Miaoli County, TW); Jui-Yu Jao (Miaoli County, TW); Wen-Hui Liu (Miaoli County, TW); Ya-Han Wu (Miaoli County, TW)
Assignee: TAIWAN CARBON NANO TECHNOLOGY CORPORATION
H01M4/96
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Quick Facts
Patent No.
US 9,666,878
App. No.
14/801,438
Granted
May 30, 2017
Kind
B2
Abstract

A method for fabricating a catalytic 3-dimensional network material comprises steps: mixing an aqueous solvent with a nitrogen-containing carbon material whose surface is doped with nitrogen atoms to form a first dispersion liquid, and mixing the first dispersion liquid with ammonium carboxymethyl cellulose to form a first gel; undertaking a freeze-drying process of the first gel to remove water from the first gel to form a first product; and undertaking a low-temperature heating process of the first product at a temperature of 50-380° C. to cure the first product into a 3D network material doped with nitrogen atoms. The catalytic 3D network material of the present invention has a very high specific surface area to increase the catalytic efficiency.

Claims (25)

1. A method for fabricating a catalytic 3-dimensional network material, comprising the steps of:

Step 1 A: placing a carbon material in a container filled with ammonium, heating the container to a temperature 500-1000° C. to decompose the ammonium gas and release nitrogen atoms, which attach to the carbon material to form a nitrogen-containing carbon material, mixing an aqueous solvent with the nitrogen-containing carbon material whose surface is doped with nitrogen atoms to form a first dispersion liquid, and mixing the first dispersion liquid with ammonium carboxymethyl cellulose to form a first gel;

Step 2 A: undertaking a freeze-drying process of the first gel to remove water from the first gel to form a first product; and

Step 3 A: undertaking a low-temperature heating process of the first product at a temperature of 50-380.degree. C. to cure the first product into a 3D network material doped with nitrogen atoms.

2. The method for fabricating a catalytic 3-dimensional network material according to claim 1 , wherein the carbon material is selected from a group consisting of carbon nanotube, graphene and carbon nanoribbon.

3. The method for fabricating a catalytic 3-dimensional network material according to claim 1 , wherein in Step 1 A, a weight ratio of the nitrogen-containing carbon material and the aqueous solvent ranges from 0.01:100 to 50:100; a weight ratio of the ammonium carboxymethyl cellulose and the first dispersion liquid ranges from 0.1:100 to 50:100.

4. The method for fabricating a catalytic 3-dimensional network material according to claim 1 , wherein a first surfactant is added into the first gel; the first surfactant is sodium dodecyl sulfate (SDS) or sodium dodecyl benzene sulphonate (SDBS).

5. The method for fabricating a catalytic 3-dimensional network material according to claim 4 , wherein a weight ratio of the nitrogen-containing carbon material and the aqueous solvent ranges from 0.01:100 to 50:100; a weight ratio of the ammonium carboxymethyl cellulose and the aqueous solvent ranges from 0.1:100 to 80:100; a weight ratio of the first surfactant and the aqueous solvent ranges from 0.01:100 to 50:100.

6. The method for fabricating a catalytic 3-dimensional network material according to claim 1 , wherein glycerol is added into the first gel; a weight ratio of the glycerol and the ammonium carboxymethyl cellulose ranges from 0.01:1 to 5:1.

7. The method for fabricating a catalytic 3-dimensional network material according to claim 1 , wherein the freeze-drying process is undertaken at a temperature ranging from 0 to −200° C.

8. The method for fabricating a catalytic 3-dimensional network material according to claim 1 , wherein the low-temperature heating process is preferably undertaken at a temperature of 80-350° C., for 1 minute to 10 hours.

9. A method for fabricating a catalytic 3-dimensional network material, comprising the steps of:

Step 1 B: mixing a carbon material with an aqueous solvent to form a second dispersion liquid, and mixing the second dispersion liquid with ammonium carboxymethyl cellulose to form a second gel;

Step 2 B: undertaking a freeze-drying process of the second gel to remove water from the second gel to form a second product;

Step 3 B: undertaking a low-temperature heating process of the second product at a temperature of 50-380° C. to cure the second product into a third product; and

Step 4 B: placing the third product in a container filled with ammonium, and keeping the container at a temperature of 500-1000° C. to form a 3D network material doped with nitrogen atoms.

10. The method for fabricating a catalytic 3-dimensional network material according to claim 9 , wherein in Step 1 B, an acidifying process of the carbon material is used to obtain an acidified carbon material; the acidified carbon material is mixed with the aqueous solvent to form the second dispersion liquid.

11. The method for fabricating a catalytic 3-dimensional network material according to claim 10 , wherein a weight ratio of the acidified carbon material and the aqueous solvent ranges from 0.01:100 to 50:100; a weight ratio of the ammonium carboxymethyl cellulose and the aqueous solvent ranges from 0.1:100 to 100:100.

12. The method for fabricating a catalytic 3-dimensional network material according to claim 9 , wherein the carbon material is selected from a group consisting of carbon nanotube, graphene and carbon nanoribbon.

13. The method for fabricating a catalytic 3-dimensional network material according to claim 9 , wherein in Step 1 B, a weight ratio of the carbon material and the aqueous solvent ranges from 0.01:100 to 50:100; a weight ratio of the ammonium carboxymethyl cellulose and the second dispersion liquid ranges from 0.1:100 to 100:100.

14. The method for fabricating a catalytic 3-dimensional network material according to claim 9 , wherein a second surfactant is added into the second gel; the second surfactant is sodium dodecyl sulfate (SDS) or sodium dodecyl benzene sulphonate (SDBS).

15. The method for fabricating a catalytic 3-dimensional network material according to claim 14 , wherein a weight ratio of the carbon material and the aqueous solvent ranges from 0.01:100 to 50:100; a weight ratio of the ammonium carboxymethyl cellulose and the aqueous solvent ranges from 0.1:100 to 100:100; a weight ratio of the second surfactant and the aqueous solvent ranges from 0.01:100 to 50:100.

16. The method for fabricating a catalytic 3-dimensional network material according to claim 9 , wherein glycerol is added into the second gel; a weight ratio of the glycerol and the ammonium carboxymethyl cellulose ranges from 0.01:1 to 5:1.

17. The method for fabricating a catalytic 3-dimensional network material according to claim 9 , wherein the freeze-drying process is undertaken at a temperature ranging from 0 to −200° C.

18. The method for fabricating a catalytic 3-dimensional network material according to claim 9 , wherein the low-temperature heating process is preferably undertaken at a temperature of 80-350° C., for 1 minute to 10 hours.

Assignments (2)
CHANGE OF NAME Recorded Sep 2, 2016
From: TAIWAN CARBON NANOTUBE TECHNOLOGY CORPORATION
To: TAIWAN CARBON NANO TECHNOLOGY CORPORATION
Reel/Frame 039910/0013 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 24, 2015
From: TSAI, CHUN-HSIEN; LEE, TING-CHUAN; TSAI, CHUN-JUNG; HSU, CHING-TUNG; LI, CHIA-HUNG; JAO, JUI-YU; LIU, WEN-HUI; WU, YA-HAN
To: TAIWAN CARBON NANOTUBE TECHNOLOGY CORPORATION
Reel/Frame 036172/0172 →
Priority Claims (1)
TW 104114680 A · May 8, 2015 · national
Continuity (1)
Related Publication 20160329572A1 · Nov 10, 2016