JPS6385010A - Production of carbon film - Google Patents

Abstract

PURPOSE:To obtain a thin and uniform carbon film useful for electrode for cells, various electronic materials readily, by producing a high polymer film from benzene by electrolytic oxidation polymerization method and then carbonizing. CONSTITUTION:Benzene is dissolved in a solvent containing a supporting electrolyte, an electric current is made to flow between two electrodes and benzene is subjected to electrolytic oxidation polymerization. Polyphenylene formed on the anode plate is washed and dried to give a polyphenylene film. Then the high polymer film is heat-treated in an inert gas and carbonized to give the aimed carbon film.

Description

DETAILED DESCRIPTION OF THE INVENTION [Technical Field] The present invention relates to a novel method for producing carbon films.

[Prior art]

Carbon film is a substance that is attracting attention as an electrode material and conductive material. Conventional manufacturing methods include applying graphite oxide produced by treating natural graphite in a strong oxidizing solution to a substrate, drying it and then carbonizing it in a reducing atmosphere to obtain a film; A method of manufacturing a carbon film by forming a sheet of colloidal expanded graphite obtained by electrolyzing in sulfuric acid to form an intercalation compound and rapidly heating it, and a method of shaping carbon and graphite powder by physically compressing them. , carbon vapor deposition method, etc. Recently, methods have been used in which a polymer film is used as a starting material and carbonized as it is, or if it is a soluble polymer, it is dissolved in an appropriate solvent and then cast onto a glass plate or the like and carbonized. However, with this method, the thickness of the film cannot be controlled;
It also has drawbacks such as difficulty in obtaining a uniform film. Therefore,
An industrial method for producing a relatively thin and uniform carbon film has not been established.

[Purpose of the invention]

An object of the present invention is to provide a method for manufacturing a carbon film using a method different from that of the prior art.

[Structure of the invention]

The present invention is a method for manufacturing a carbon film by dissolving benzene in a solvent containing a supporting electrolyte and passing electricity between two electrodes to carbonize a polyphenylene film formed on an anode plate. In this method, the film thickness can be easily controlled by the amount of electricity applied, and the produced polymer is carbonized in a solid phase with good yield, so the film thickness can be reduced to 2 to 30 μm while maintaining most of the film shape. It is possible to make a carbon film of about 100%. The specific manufacturing method will be described below.

Example (1) 20 x 20 Il in the center of a 5Q + Ill Mitsuro flask
Platinum and nickel plate electrodes of 1Wl were suspended, and aluminum chloride 48 and tetrachloride were added while nitrogen gas was flowing.
Dissolve n-butylammonium sail 58 in 351 nitromethane or nitrobenzene, and add benzene 2+I to this.
I was added, and a constant DC current of 48 mA was applied with the platinum electrode as positive and the nickel electrode as negative. The reamer on the gold-platinum plate was washed with acetone and heated dilute hydrochloric acid for 0.5 to 3 hours, and dried at 100°C. Approximately 10 μm in about 0.5 hours, 1
It becomes more than 20μI in ~2 hours. Place the obtained film on a platinum or quartz boat and heat it for 3 minutes while flowing argon gas.
A desired carbon film is obtained by heat treatment at 800 or 1000° C. for 1 hour at a heating rate of ° C./win.

The film number ratio is 75 to 80X, and although it shrinks somewhat, the film maintains its shape.

Example (2) Platinum and nickel electrodes were suspended in the same reaction vessel as in (1),
0.5 g of cupric chloride and 0.78 g of lithium arsenic hexafluoride are suspended in 35 ml of nitrobenzene. Approximately 41 g of benzene is added to this, and a constant current of 8 mA is applied with the platinum electrode set as positive and the nickel electrode set as negative.

After 1 hour, the polymer on the platinum electrode plate is washed with acetone to obtain a polyphenylene film. Anions doped into the polymer can be removed by reversing the aggressiveness of the reaction or soaking it in aqueous ammonia. The thickness of the film is 10-12 μm in 1 hour. Next, the obtained film is carbonized in the same manner as above. The yield was about 85χ when treated at 800°C, which is higher than in Example (1).

〔Effect of the invention〕

The thin and uniform carbon film obtained by the present invention is
It is expected to be used in battery electrodes and various electronic materials.

Claims (1)

[Claims] A method of producing a carbon film by carbonizing a polymer film synthesized from benzene using the electrolytic oxidation polymerization method.