Method for disentangling hollow carbon microfibers, electrically conductive transparent carbon microfibers aggregation film amd coating for forming such film

• US 5,853,877 A
• Filed: 05/31/1996
• Issued: 12/29/1998
• Est. Priority Date: 05/31/1996
• Status: Expired due to Term

• Current Assignee: Mitsubishi Materials Corporation
• Original Assignee: Hyperion Catalysis International Incorporated, Mitsubishi Materials Corporation
• Inventors: Shibuta, Daisuke
• Primary Examiner(s): Edwards, Newton
• Application Number:
  US08/656,067
• Time in Patent Office: 942 Days
• Field of Search: 428/357, 428/367, 428/375, 423/447.1, 423/447.2
• US Class Current: 428/357
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: B82Y 40/00 Manufacture or treatment of nanostructures
• CPC Class Codes: C01B 2202/22 Electronic properties
• CPC Class Codes: C01B 2202/34 Length
• CPC Class Codes: C01B 2202/36 Diameter
• CPC Class Codes: C01B 32/168 After-treatment
• CPC Class Codes: C09D 5/24 Electrically-conducting paints conductive materials H01B1/00
• CPC Class Codes: D01F 9/127 by thermal decomposition of hydrocarbon gases or vapours or other carbon-containing compounds in the form of gas or vapour, e.g. carbon monoxide, alcohols
• CPC Class Codes: H01B 1/04 mainly consisting of carbon-silicon compounds, carbon or silicon
• CPC Class Codes: Y10T 428/29 Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
• CPC Class Codes: Y10T 428/2918 including free carbon or carbide or therewith [not as steel]
• CPC Class Codes: Y10T 428/2933 Coated or with bond, impregnation or core

Abstract

This invention relates to a method for disentangling hollow carbon microfibers and to the dispersion of hollow carbon microfibers, preferably having an outer diameter of 3.5 to 70 nm and an aspect ratio of at least 5, to form transparent electrically conductive films. Hollow carbon microfibers, treated with strong acids such as sulfuric acid or oleum and an oxidizing agent such as nitric acid, are disentangled and dispersed homogeneously in a polar solvent. The slurry in which the microfibers are suspended can be coated on a substrate. The coating film is dried and a transparent electrically conductive film is formed. A carbon microfiber aggregation film with excellent transparency is obtained having a total transmittance of at least 80 percent and a haze value of at most 0.1%.

Claims

1. An electrically conductive transparent carbon microfibers aggregation film comprising hollow carbon microfibers, said microfibers being treated with a strong acid containing sulfur and an oxidizing agent, wherein said carbon microfibers have an outer diameter of 100 nm or less and said film has a total light transmittance of about 60% or more.

2. The electrically conductive transparent carbon microfibers aggregation film according to claim 1 which includes an additive such as a dispersing agent, a cross-linking agent, a stabilizer, an anti-settling agent, a coloring agent, or a charge adjusting agent.

7. The electrically conductive transparent carbon microfibers aggregation film of claim 1, wherein said carbon microfibers have an outer diameter of about 3.5 to 70 nm.

9. The electrically conductive transparent carbon microfibers aggregation film of claim 1, wherein said film has a thickness between about 0.05 to 5 microns.

10. The electrically conductive transparent film of claim 1, wherein said film has a total light transmittance of about 70% or more.

11. The electrically conductive transparent film of claim 1, wherein said film has a total light transmittance of about 85% or more.

14. The electrically conductive transparent film of claim 1, wherein said film has a haze value less than 1%.

15. The electrically conductive transparent film of claim 1, wherein said film has a haze value less than 0.5%.

16. The electrically conductive transparent film of claim 1, wherein said film has a haze value less than 0.1%.

17. A method of making the electrically conductive transparent film of claim 1, comprising the steps of:

(a) treating carbon microfibers with a strong acid containing sulfur and an oxidizing agent to form disentangled carbon microfibers; and

(b) forming said film from said disentangled carbon microfibers.

18. The method of claim 17, wherein said disentangled carbon microfibers are washed prior to forming said film.

19. The method of claim 17, wherein said film is formed by spin coating.

20. The method of claim 17, wherein said strong acid is sulfuric acid and said oxidizing agent is nitric acid.

3. An electrically conductive transparent film comprising a binder and hollow carbon microfibers, said microfibers being treated with a strong acid containing sulfur and an oxidizing agent, wherein said carbon microfibers have an outer diameter of 100 nm or less and said film has a total light transmittance of about 60% or more.

4. The electrically conductive transparent film according to claim 3 wherein the binder is selected from the group consisting of organosilanes, cellulose acetate, an olefinic polymer and an acrylic polymer.

5. The electrically conductive transparent film according to claim 3 having surface resistance in the range of about 10² -10¹⁰ Ω

/□

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6. The electrically conductive transparent carbon film according to claim 3 comprising hollow carbon microfibers having a total transmittance of about 60% or more and a haze value of about 0.5% or less.

8. The electrically conductive transparent film of claim 3, wherein said carbon microfibers have an outer diameter of about 3.5 to 70 nm.

12. The electrically conductive transparent film of claim 3, wherein said film has a total light transmittance of about 70% or more.

13. The electrically conductive transparent film of claim 3, wherein said film has a total light transmittance of about 85% or more.