JPS59135208A - Production of electroconductive composition - Google Patents

Abstract

PURPOSE:To produce an electroconductive composition, by reacting a compound containing both a cyano group and a double bond at a high temperature. CONSTITUTION:A 6-C or lower compound having both a cyano group and a double bond of the formula (wherein X, Y, and Z are each H, or a halogen, cyano, or alkyl), e.g., acrylonitrile, chloroacrylonitrile, or tetracyanoethylene), preferably after diluting to a concentration of about 10-30wt% with an inert gas, is reacted at 500-3,200 deg.C to obtain an electro-conductive composition. It is possible to conduct this reaction at lower temperature by using a catalyst such as alumina, iron, or vanadium.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method of manufacturing an electrically conductive composition. Although carbon-based conductive compositions can be produced by various methods, gas phase pyrolysis is considered to be one of the most important methods, and many specific methods have been proposed so far. One example is the thermal decomposition of compounds such as methane, propane, propylene, benzene, and acetylene at high temperatures, but the reaction temperature is generally high and usually 9
It requires a temperature of 00°C or more to 2500°C and is energy consuming. Moreover, within this range, it is difficult to obtain a highly conductive product in the low temperature region.

In the present invention, a method is proposed in which a composition having sufficiently high conductivity can be obtained even by low-temperature reaction of a compound having a cyan group and a double bond. As mentioned above, the purpose of the present invention is to produce a conductive composition, but in addition to being used alone, it can also be used as a coating layer for other heat-resistant materials such as carbon, ceramics, metals, etc.

In addition, the conductive composition in a3 of the present invention is metal 4K 7%
In addition to compositions that exhibit high electrical conductivity in semiconductor regions, we also provide compositions that exhibit high electrical conductivity in semiconductor regions.

The method of the present invention is described above in detail. The gist of the present invention σ) is that a compound having a cyano group and a double bond is
00℃ 1N (1N)

Specific examples of compounds containing a cyano group and a 12Φ bond (31, acryloni l-, IJ
Ru, Metak IJ l] 21~Ril, j for~Raciano-[
-tyrene, ri IJ ["iacryl"] is a hydrocarbon having 21~lyl, and its bulk, 11 Φ bond, C is also good, and other fatty hχ hydrocarbons of A,
Used in combination with alicyclic hydrocarbons, Z apricot group hydrocarbons, unsaturated hydrocarbons, etc. (J: It). During the reaction, C in the reaction atmosphere of nitrogen, helium, norgon, hydrogen, etc.
Inert gas usually 3-4098, preferably 10 3
0% σ) l'a lu i This dilution yields -C and 11.

These scum-like rivers j)l'l chopsticks 500・-320
The reaction is carried out at a temperature of 0°C, (1' good (t = 600 - 2000°C, and (f, i L < 700 - 100"C. Reaction 4i is thought to proceed by various mechanisms. First, there is a knee-heavy combination, and then cyclization occurs due to the ring closure of Dino′], and roughly -1 of the reaction eddy current occurs.
, = Dehydrocyclization and other anti-1,6 reactions occur in a complex manner with Wr ('', I don't think that even higher temperatures (higher temperature) will lead to further cyclization. In addition to this, there are other reactions. A mechanism that prevents cleavage into radicals is also considered.Depending on the reaction products (and reaction conditions), various structures may be mixed:
, considered a complex composition.

The reaction time depends on the conditions f4+ and 2, or about 0 seconds at 700'C (or ε). 1) It will have a certain effect over time. .

Method No. 1 of the present invention (according to which a new compound containing nitrogen is first formed at a low temperature stage. When the temperature is −1−, the nitrogen content decreases, and the so-called gutsufu (l -Structure I is considered to approach.In this case, conventional gas phase pyrolysis j
Compared to the production of large trees, the reaction speed is slow, so the low-temperature reaction 1-is j] 1-711 It is low-temperature reaction.
- from the inkstone fish - (also highly valued.

Zino method of the present invention (the conductive composition obtained is transferred to another shrine 11)
Table...1 As a base when used as a coating layer, 6-E,
Inorganic materials such as garnos, nitride, silicon nitride, sapphire, silicone, aluminum, stainless steel, copper and other metal materials, granoite, carbon fiber such as carbon fiber, etc. are used. It is of course possible to use the crystalline substrate used in the full polymerization of Toshi C-cho Pitaxy X, as well as the substrate used in the Graph A epitaxial process.

Although the present invention typically embodies a thermal stage reaction without the use of a catalytic IJ, catalytic processes are also possible.

As a catalyst - C is aluminum, iron, Pal 1~, Niracle,
Hanodium, small metals, alloys thereof, oxides, carbides and other compounds are used.

By using a catalyst, the temperature of the reaction can be further lowered8.
I can do 11. Roughly plasma polymerization hand d1 (for jf (J) can also be used.

Although the conductive composition obtained according to the present invention is generally obtained as a 14-layer material on a substrate, fibrous or even fibrous products are of course within the scope of the present invention. Included.

The electrical conductivity of the conductive material obtained according to the present invention is 5JJ, which is 1,1 and 1% as compared with doping and interspersion.
Other known compounds can be used, such as fj-ton, Y'm arsenic fluoride, and anzushin chloride.
.

The method of the present invention will be explained in detail using Examples above.

Example 1 Insert a quartz plate (-1 yen 15 mm) into a quartz plate as a base for this reaction, and heat it to l'600'C using an electric furnace. -Doji, this includes acryloni 1~lyl, methacrylic 1''21heryl, two 1~nocyano-[-1-lene, methane, zo[-1bi1
Non, alebren, ()-=henotane, benzene, ?
tl-nitrile, cyF lentrinomine, 2-vinylpyridine, d3 and chloroacrylonitrile
100 ml/'m of raw material gas containing 20% by volume separately.
Ingredients were used immediately for 2 hours. After repulsion, the quartz JK substrate was taken out and the reaction products were observed with the naked eye. With acrylonitrile, methacrylonitrile, tetracyanoethylene, J3, and chloroacrylonitrile, a reaction product with metallic luster was formed on the substrate, but with the other raw materials, no surface coating layer was formed.

Example 2 Acrylonitrile was diluted to 5% with argon to 50%
The reaction was carried out on a quartz plate placed in a reaction tube heated to 600, 800, or 1500° C. at a rate of ml/min.

After one hour of reaction, the quartz plate used as a substrate was taken out, and the product on the substrate was taken for elemental analysis. The results were as follows.

Firing temperature Atomic ratio °C Carbon Nitrogen Water 600 5.5 1.0 0.6800 6
．． 8.1. OO,4 15008,,31,00,1 If the reaction temperature is low, nitrogen-rich products are obtained. The results of measuring the electrical conductivity of the reaction product were as follows.

Reaction temperature Electric conductivity 600℃ 0.02' S/cm 800℃
80 S/cm1500'C900S/cm Example 3 A magnetic boat coated with ferrous chloride was placed in a reaction tube with an inner diameter of 20 cm, the temperature was raised to 1000°C, and acrylonitrile was added to the reaction tube for 1 hour.
The reaction was carried out for 2 hours at a flow rate of 5 cm/min. After the repulsion, the magnetic boat was taken out and observed, and it was found that whiskers 6 mm in length were growing densely.

Patent Applicant Director of the Agency of Industrial Science and Technology Slate M-Procedural Amendment (Method) September 8, 1981 Kazuo Wakasugi, Commissioner of the Patent Office 1, Indication of Case Patent Application No. 136831 of 1982''''□ 1 l--(-1, i "Title of the invention" column-6 in the specification) ・', -\di:, (jt', 1

Claims (1)

[Scope of Claims] (1) A compound containing a cyan group and a double bond containing 500 to 3
A method for producing a conductive composition, characterized in that the reaction is carried out at a temperature of 20-0°C. (2. The method according to claim 1, wherein the compound containing a cyano group and a double bond is represented by the following general formula and has 6 or less carbon atoms. Here, X, Y, and Z are atomic groups selected from hydrogen, halogen, cyano group, and argyl group. , α-chloroacrylonitrile or β-chloroacryloni-lyl.