JPH09110528A - Production of glass-like carbon material containing silicon - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for producing a glass-like carbon material containing silicon having a uniform and minute composite structure containing a silicon component as a continuous phase in an atomic level, and having an excellent oxidation resistant property. SOLUTION: This method for producing a glass-like carbon material containing silicon is to dilute an aminosilane compound containing a single Si atom in a molecule (preferably 3-aminopropyltriethoxysilane) by mixing with an organic solvent having a high residual ratio after a carbonization (preferably furfuryl alcohol, furfural or their mixture), drip the diluted solution into a thermosetting resin liquid while agitating and mixing, form and cure the obtained resin composition containing the aminosilane into a prescribed shape, and burn under a non oxidizing atmosphere at >=800 deg.C for carbonizing treatment.

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to a modified glassy carbon material having a homogeneous and dense composite structure structure containing a Si component as a continuous phase, and particularly a Si-containing glassy carbon material having excellent oxidation resistance. Manufacturing method.

[0002] A glassy carbon material is a heterogeneous carbon material having a macroscopically vitreous and dense structure obtained by firing and carbonizing a thermosetting resin compact, and is gas-free compared to general carbon materials. Because of its excellent permeability, abrasion resistance, corrosion resistance, self-lubricating property, surface smoothness and robustness,
Utilizing its characteristics, it is useful for various industrial members in various fields. In recent years, attention has been paid to non-contaminating material properties that do not allow minute carbon particles to be detached from tissue, and practical use in the semiconductor field where contamination is averse, such as electrodes for plasma etching of silicon wafers and members for ion implantation equipment. Have been.

[0003]

2. Description of the Related Art However, a glassy carbon material is fragile in its material and, like a general carbon material, has a material defect peculiar to a carbon material that is rapidly oxidized in a high temperature oxidizing atmosphere and deteriorates its physical properties. is there. For this reason, conventionally, attempts have been made to improve the physical properties by combining a ceramic component in a glassy carbon structure. In the initial stage, a method was used in which ceramic particles such as SiC were mixed with a thermosetting resin as a raw material by a dry method or a wet method, and a molded body obtained by curing this was carbonized by firing. Cannot be uniformly dispersed in the carbon structure, and because grain boundaries exist between the ceramic particles and the carbon structure, material destruction may occur under severe usage conditions,
There is a problem that the phenomenon that the ceramic particles come off occurs.

For this reason, there has been proposed a method of obtaining a Si-containing glassy carbon material having a uniform structure by mixing a silicon-containing compound with a thermosetting resin to prepare a raw material system. For example, JP-A-61-1111 discloses a liquid silicon compound,
Disclosed is a method for producing an oxidation resistant carbon material by carbonizing a liquid organic compound having a functional group and carbonized by heating, and a precursor substance containing Si, O and C in which a catalyst for polymerization or crosslinking is solubilized. Has been done. In this method, a silicic acid polymer obtained by dealkalization of water glass as a liquid silicon compound, an ester of a silicic acid with an organic compound having a hydroxyl group, a Si ester such as ethyl silicate, a reaction product of silicon tetrachloride and ethanol, etc. The use of sulfuric acid, hydrochloric acid, organic peroxides, organic sulfonic acids, etc. as a catalyst is an essential requirement.

However, the above-mentioned method is intended to produce a carbon material containing a relatively large amount of Si component (C / Si atomic ratio: 0.5 to 19). Due to the large amount, the silicon compounds bond with each other in the process of forming the precursor material containing Si, O and C to form fine agglomerates, which are the same as S in the carbonized structure.
i It tends to have a non-uniform texture that is dispersed as a granular material. Also, multiple S such as siloxane bond (Si-0-Si)
Even when a polymerized ester in which i atoms are chained is used as a silicon source, a heterogeneous structure is likewise caused by agglomeration.
Even if the blending amount with respect to the liquid organic compound is reduced, it is not possible to obtain a continuous phase carbonaceous structure in which Si is not dispersed in a particle state. In addition, when the catalyst used in combination is a strong acid such as sulfuric acid or hydrochloric acid, the gelation reaction proceeds rapidly and the homogeneity of the structure is impaired, and when using a catalyst such as sodium ethylate or organic sulfonic acid, the contained inorganic components remain. It becomes an impurity and becomes a factor to reduce the purity.

JP-A-5-43319 discloses a glassy state in which ultrafine ceramics obtained by uniformly mixing a thermosetting resin and an organometallic compound in a liquid state and heating (calcining) are highly dispersed. A carbon composite material is disclosed.
In the present invention, as the organometallic compound serving as a silicon source, S
Polycarbosilanes and polysilanes that give iC, Si
A Ti-containing polycarbosilane which gives —Ti—C—O, S
Polysilazanes that give i _x N _y , Si—N—C or Si ₂ N ₄ —SiC have been used. However, when a polymer such as polycarbosilane or polysilane having a plurality of silane bonds is mixed with a thermosetting resin to form a raw material system, the ceramics source is in a state of being dispersed as a molecule, so that fine metal carbide particles and fine particles are formed after heat treatment. It is unavoidable that grain boundaries are generated, and a glassy carbon structure in which ceramics and carbon exhibit a homogeneous continuous phase cannot be obtained.

In addition, Japanese Patent Laid-Open No. 5-339006 discloses a polymerization or cross-linking catalyst which uses a liquid silicon compound and a liquid organic compound which has a functional group and produces carbon by heating as a raw material, and uniformly solubilizes it. A β-type silicon carbide-carbon mixture, which is obtained by subjecting the resulting precursor substance to heating or carbonization in a non-oxidizing atmosphere and further firing the resulting intermediate product at a higher temperature in a non-oxidizing atmosphere. In the method for producing a powder, the raw material and the catalyst do not substantially contain an impurity element, the intermediate molded product has a carbon / silicon molar ratio of 2.5 to 3.5, and the carbonization in the mixed powder is Silicon and carbon are homogeneously mixed, the amount of carbon is 3 to 28% by weight, and the content of each impurity element in the mixed powder is 1 pp.
A method for producing a high-purity β-type silicon carbide-carbon mixed powder having a size of m or less has been proposed. However, this method is for producing a SiC-C-based powder for a sintered body, and is not a production technique for a Si-containing carbon compact whose main component is a glassy carbon structure.

In view of the above situation, the present applicant has previously proposed -O-
Obtained by firing and carbonizing a molded body of a thermosetting resin crosslinked with Si-O-, and atomic level Si is distributed as a uniform continuous phase in the range of 0.1 to 15% by weight in the glassy carbon structure. The SiC-containing glassy carbon material having a texture property, a thermosetting resin, and a hydrolyzate of a Si alkoxide having a single Si atom in one molecule are stirred and mixed in an organic solvent to produce a crosslinking reaction. A method (Japanese Patent Application No. 7-155177) was developed, in which the gelled product obtained by (1) is cured and molded, and then the cured molded body is subjected to firing and carbonization treatment at a temperature of 800 ° C. or higher in a non-oxidizing atmosphere. 1
An aminosilane compound containing a single Si atom in the molecule is dropped into a thermosetting resin solution and mixed by stirring to mold and cure the mixed solution, and then the cured molded article is heated in a non-oxidizing atmosphere at 80
We proposed a method for producing a Si-containing glassy carbon material, which is characterized by performing a firing carbonization treatment at a temperature of 0 ° C. or higher (Japanese Patent Application No. 7-234696).

[0009]

[Problems to be Solved by the Invention] Japanese Patent Application No. 7-23469
According to the method of the invention of No. 6, a silane compound having an amino group as a Si source and containing a single Si atom in one molecule is selected and directly mixed with a thermosetting resin liquid. Even if it is made into a large-sized molded body, it is free from cracks, pores and dimensional deformation, and S
Si of composite structure in which i is homogeneously dispersed in the structure at the atomic level
It becomes possible to manufacture a glassy carbon material containing.

In the above method, the amino group preferentially bonds with the thermosetting resin in preference to the alkoxy group in the step of dropping the aminosilane compound containing Si atom into the thermosetting resin solution, and the dehydration condensation reaction proceeds. Since this dehydration condensation is an exothermic reaction, the temperature in the reaction system rises rapidly. Therefore, if the thermosetting resin is left as it is, the curing of the thermosetting resin is promoted to increase the viscosity, and it becomes difficult to obtain a uniform component mixture system. Especially Si in glassy carbon material
When the dropping amount of the aminosilane compound is increased in order to increase the content, heat generation becomes remarkable, and voids and segregation of Si components are likely to occur in the structure of the molded body that is the precursor of the glassy carbon.

In order to avoid such a phenomenon, Japanese Patent Application No. 7-
In the invention of No. 234696, although a mixed solution of a thermosetting resin liquid and an aminosilane compound is cooled and stored, a curing reaction due to heat generation is suppressed, and then a means for giving a slow flow to enhance the homogeneity of the mixed state is taken. However, this method alone cannot obtain a sufficient heat generation suppressing effect under the compounding conditions such that the Si content in the glassy carbon material exceeds 5% by weight, and it is difficult to always form a homogeneous component mixture system.

[0012] The inventor of the present invention, as a result of continuous improvement research in order to solve the above problems, results in Japanese Patent Application No. 7-234696.
In the method of No. 3, when an aminosilane compound containing a single Si atom in one molecule is mixed and diluted in advance with an organic solvent having a high carbonization residual ratio and then dropped into a thermosetting resin liquid, the reaction between the amino group and the resin proceeds. It has been found that even if the Si source is relaxed and the Si source is in a high mixing ratio, the components can be uniformly mixed while effectively suppressing heat generation.

The present invention has been developed on the basis of the above-mentioned findings, and its object to be solved is to provide a high oxidation resistance Si-containing glass-like glass having a uniform and dense composite structure structure in which Si is distributed as a continuous phase. It is an object of the present invention to provide a manufacturing method for industrially obtaining a carbon material without material defects.

[0014]

A method for producing a Si-containing glassy carbon material according to the present invention for solving the above problems has a high carbonization residual ratio of an aminosilane compound containing a single Si atom in one molecule. After mixing and diluting with an organic solvent, the diluted solution is dropped into a thermosetting resin liquid and stirred and mixed, and the obtained aminosilane-containing resin composition is molded and cured into a predetermined shape, and then the molded body is subjected to a non-oxidizing atmosphere. The constitutional feature is that the carbonization treatment is performed at a temperature of 800 ° C. or higher.

[0015]

BEST MODE FOR CARRYING OUT THE INVENTION In the present invention, an aminosilane compound is a raw material component serving as a Si source for dispersing and compounding Si in a glassy carbon structure at the atomic level, and an aminosilane compound containing a single Si atom in one molecule is selected. Is used for. A polysilane in which two or more Si atoms are bonded in one molecule is likely to cause an aggregation phenomenon in the mixing step with the thermosetting resin liquid, and has an organic functional group other than an amino group, such as a methyl group or a vinyl group. Since the silane compound does not directly react with the thermosetting resin, it is separated during the mixing, and the association and the multimerization (polymerization) occur to make it impossible to disperse Si at the atomic level.

The aminosilane compound containing a single Si atom in one molecule is represented by the following general formula (Formula 1), and is usually
It is commercially available as an amine-based silane coupling agent.

[0017]

Embedded image

As the amine-based silane coupling agent containing an alkoxy group, 3-aminopropyltriethoxysilane (SiC ₉ H ₂₃ NO ₃ ), N- (2-aminoethyl) -3 is used.
-Aminopropyltrimethoxysilane (SiC ₈ H ₂₂ N ₂ O ₃ ),
N- (2-aminoethyl) -3-aminopropylmethyldimethoxysilane (SiC ₈ H ₂₂ N ₂ O ₂ ), p- [N- (2-aminoethyl) aminomethyl] phenethyltrimethoxysilane (SiC ₁₄ H _{2 6} N ₂ O _3), 4- aminobutyl dimethylmethoxysilane _{(SiC 7 H 19 NO),} 4- aminobutyl triethoxysilane _{(SiC 10 H 2 5 NO 3} ), N- (2- aminoethyl) -3
-Aminopropyltris (2-ethylhexiso) silane
(SiC ₂₉ H _{6 4} N ₂ O ₃ ), p-aminophenyltrimethoxysilane (SiC ₉ H ₁₅ NO ₃ ), p-aminophenyltriethoxysilane (SiC ₉ H ₁₅ NO ₃ ), 3- (1-amino Propoxy) 3,3
-Dimethyl-1-propenyltrimethoxysilane (SiC ₁₁
H _{2 5} NO _4), 3- aminopropyl tris (methoxyethoxy) silane _{(SiC 18 H 4 1 NO 9} ), 3- aminopropyldimethylethoxysilane _{(SiC 7 H 19 NO),} 3- aminopropyl methyl diethoxy Silane (SiC ₈ H ₂₁ NO ₂ ), 3-aminopropyltrimethoxysilane (SiC ₉ H ₂₃ NO ₃ ), ω-aminoundecyltrimethoxysilane (SiC ₁₄ H _{3 3} NO ₃ ), 1-
Trimethoxysilyl-2- (p, m-aminomethyl) phenylethane (SiC ₁₂ H _{2 1} NO ₃ ), 6- (aminohexylaminopropyl) trimethoxysilane (SiC ₁₂ H _{3 0} N ₂ O ₃ ), N
- (triethoxysilylpropyl) urea (SiC ₁₀ H _{1 4} N
₂ O _4), trimethoxysilylpropyl diethylene triamine _{(SiC 10 H 2 7 N 3} O 3) , etc. are exemplified.

Examples of the amine-based silane coupling agent containing no alkoxy group include 3-aminopropyltrimethylsilane (SiC ₆ H ₁₇ N) and 3-aminopropyldiethylmethylsilane (SiC ⁸ H ²¹ N). To be

It is preferable to use these aminosilane compounds having a molecular weight as low as possible because organic components other than Si are thermally decomposed and volatilized during carbonization. Therefore, the most suitable amino group-containing silane compound for the present invention is 3
-Aminopropyltriethoxysilane.

The above-mentioned aminosilane compound containing a single Si atom in one molecule (hereinafter, simply referred to as "aminosilane compound")
Is mixed with an organic solvent having a high carbonization residual ratio to dilute. The organic solvent having a high carbonization residue rate refers to an organic solvent having a small amount of volatile components and having a high ratio of remaining as a carbide when a solid material is subjected to a baking treatment. Examples of this type of organic solvent include furfuryl alcohol, furfural, phenol, furan, tetrahydrofuran, etc., which have a particularly good affinity with the thermosetting resin liquid to be dripped and are converted into glassy carbon by a firing treatment. Furfuryl alcohol, furfural or a mixture thereof is preferably used. On the other hand, when a volatile organic solvent such as acetone or alcohol is used, breakage is likely to occur due to significant volume shrinkage at the stage of molding and curing the thermosetting resin liquid that has been dropped and mixed, and the residual solvent component is It volatilizes during curing and pores are generated inside the tissue.

The organic solvent having a high carbonization residual ratio slightly reacts in the process of mixing with the aminosilane compound, but does not cause a thickening phenomenon which hinders uniform mixing. The degree of dilution of the aminosilane compound with the organic solvent is not particularly limited, but it is preferable to adjust the dilution ratio to about 0.5 to 3 times.

The diluted solution prepared by mixing and diluting the aminosilane compound with the organic solvent having a high carbonization residual ratio is then added dropwise to the thermosetting resin liquid. The thermosetting resin liquid serves as a carbon source that is converted into glassy carbon by firing and carbonizing treatment, and for example, liquid phenol resin, furan resin, polyimide resin, polycarbodiimide resin, polyacrylonitrile resin, pyrene- A phenanthrene-based resin, a polyvinyl chloride-based resin, an epoxy-based resin, a mixed resin thereof, or the like can be used. In particular, when the resin is fired at a temperature of 800 ° C. in a non-oxidizing atmosphere, the residual carbon content is high, and when mixed with the silicon source component, the amino group in the silane compound acts to slowly perform the dehydration condensation reaction. An initial condensate of a phenolic resin or a furan-based resin, or a mixed resin solution thereof, which produces the above is preferably used.

The dropping of the diluted solution into the thermosetting resin liquid is carried out under sufficient stirring and cooling conditions. When the dropping and mixing are advanced, the amino group in the aminosilane compound is bonded to the thermosetting resin in preference to other functional groups (alkoxy groups), and the dehydration condensation reaction proceeds. For example, when 3-aminopropyltriethoxysilane is dropped into a phenol resin solution and mixed with stirring, a two-step reaction as shown in Chemical formulas 2 and 3 below proceeds.

[0025]

Embedded image

[0026]

Embedded image

Although the aminosilane compound is dispersed in the thermosetting resin while generating heat through the above reaction, in the present invention, the aminosilane compound is diluted with the organic solvent having a high carbonization residual ratio and the thermosetting resin is dispersed. Since it is dropped in the liquid, the progress of the violent reaction is moderated, and the extreme heat generation is effectively suppressed. Therefore, even if the aminosilane compound is added to the thermosetting resin liquid in a high blending ratio, the viscosity of the reaction system does not increase, and a homogeneously mixed aminosilane-containing resin composition is always formed while maintaining good fluidity. . Further, at this stage, the alkoxy group in the aminosilane compound hardly reacts with the thermosetting resin, and the amino group is bonded to the resin component to form a peculiar form in which the molecule is enlarged around Si.
For this reason, since the reactivity of the alkoxy group is relatively decreased, the reaction between the alkoxy group and the resin component is suppressed, and at the same time, the aggregation caused by the polymerization of aminosilanes is suppressed, so that the mixed solution does not contain aggregated particles. It exhibits a very homogeneous continuous phase.

If the aminosilane-containing resin composition thus formed is left to stand as it is, the curing reaction proceeds due to the heat storage effect, and the heterogeneous composition is likely to be mixed and dispersed. It is preferable to carry out an operation of suppressing the above and giving a slow flow again in the molding stage to enhance the homogeneity of the mixed state.

The aminosilane-containing resin composition is, if necessary, vacuum-deaerated to remove air to be occluded and then molded into a predetermined shape. The molding means is usually cast molding or centrifugal molding, but it is also possible to apply compression molding, extrusion molding, transfer molding, etc. at the semi-cured stage. The molded body thus molded is heated to a temperature of 70 to 150 ° C. and hardened to obtain a glassy carbon precursor.

Then, the cured molded article is transferred to a heating furnace maintained in a non-oxidizing atmosphere and subjected to a firing carbonization treatment in a temperature range of 800 ° C. or higher, preferably in a temperature range of 1000 to 2500 ° C. At the stage of the calcination and carbonization treatment, the thermosetting resin component and the residue of the organic solvent having a high carbonization residual rate are both converted into glassy carbon.

The Si-containing glassy carbon material produced in the above process is a carbonaceous structure obtained by substantially carbonizing a thermosetting resin compact by firing and carbonization.
i has a composite texture property in which it is distributed as a uniform continuous phase in the glassy carbon structure. This texture is Si
Unlike the composite structure in which the components are dispersed in the form of fine particles, it exhibits an alloy-like continuous solid solution phase in which there are no grain boundaries between Si and C, and macroscopically it has a structure structure of glassy carbon alone. Substantially no difference was observed, while microscopically, it had a unique composite morphology in which a part of C of the glassy carbon structure was substituted and bonded to Si. In particular, according to the present invention, a high-quality Si-containing glassy carbon material having high strength and high oxidation resistance with no material defects even in a high compounding region in which the Si content in the glassy carbon structure exceeds 5% by weight. Can be obtained.

[0032]

EXAMPLES Examples of the present invention will be specifically described below in comparison with comparative examples. However, the scope of the invention is not limited to these examples.

Examples 1 to 3 3-aminopropyltriethoxysilane (TSL8345 manufactured by Toshiba Silicone Co., Ltd.) was used as a Si source, and 0.5 times volume of furfuryl alcohol was mixed with this and sufficiently stirred,
A uniform diluted solution was made. This diluted solution was added dropwise to the phenol resin initial condensate [PR-940 manufactured by Sumitomo Durez Co., Ltd.] in a running water cooling tank under stirring, and the stirring and mixing operation was continued for 1 hour. At this time, the dropping amount of the dilute solution was changed so that the Si content in the glassy carbon structure finally became 7,
It was set to be 10 and 15% by weight. Put the agitated and mixed aminosilane-containing resin composition in the refrigerator (2 ° C) and
Cool and store for 8 hours, then gently stir again with a stirrer,
The solution was kept in the fluidized state over time. Then, the solution was poured into the mold and subjected to defoaming treatment in a vacuum device, followed by 7
The resin component was cured by heating to 0 to 150 ° C. The obtained cured molded article was transferred to a heating furnace maintained in a nitrogen atmosphere,
It was heated to 2000 ° C. at a heating rate of 10 ° C./hr and carbonized by firing. Thus, Si-containing glassy carbon materials having different Si contents (300 mm in length and width, 5 mm in thickness) were manufactured. No cracks or pores were found in the structure of each of the obtained Si-containing glassy carbon materials, and the surface condition was a glassy smooth surface.

The bulk density, bending strength and oxidation resistance at high temperature of each Si-containing glassy carbon material obtained were measured,
The results are shown in Table 1. The oxidation resistance was shown as the weight loss rate when the test piece was treated with a dry air flow at temperatures of 750 ° C. and 950 ° C. for 40 minutes.

Comparative Examples 1 to 3 3-Aminopropyltriethoxysilane (TSL8345 manufactured by Toshiba Silicone Co., Ltd.) was used as a Si source, which was not diluted with an organic solvent and was directly stirred in a running water cooling tank. Phenolic resin initial condensate [PR-94 manufactured by Sumitomo Dures Co., Ltd.
0] and the stirring and mixing operation was continued for 1 hour. At this time, the dropping amount of the diluted solution was changed so that the Si content in the glassy carbon structure was finally set to 7, 10, 15% by weight. Other than that, the Si-containing glassy carbon material was manufactured under the same conditions as in Examples 1 to 3. In each of the Si-containing glassy carbon materials obtained, no cracks or pores were found in the structure, and the surface condition was smooth.
A slight segregation was observed in the dispersion of the components. The bulk density, bending strength, and oxidation resistance at high temperatures of each Si-containing glassy carbon material were measured, and the results are also shown in Table 1.

Example 4 The Si source was changed to 3-aminopropyldiethylmethylsilane, and the Si content was 1 under the same conditions as in Example 2.
A 0 wt% Si-containing glassy carbon material was produced. No cracks or pores were found in the structure of the obtained Si-containing glassy carbon material, and the surface state thereof was a glassy smooth surface. Table 1 shows the bulk density, bending strength, and oxidation resistance in a high temperature region measured for this Si-containing glassy carbon material.

Example 5 Furfural was used as an organic solvent for diluting 3-aminopropyltriethoxysilane, and the Si-containing glassy carbon material having a Si content of 10% by weight was produced under the same conditions as in Example 2. . No cracks or pores were found in the structure of the obtained Si-containing glassy carbon material, and the surface state thereof was a glassy smooth surface. Table 1 shows the bulk density, bending strength, and oxidation resistance in a high temperature region measured for this Si-containing glassy carbon material.

Comparative Example 4 A Si-containing glassy carbon material having a Si content of 10% by weight was produced under the same conditions as in Example 2 except that ethanol was used as an organic solvent for diluting 3-aminopropyltriethoxysilane. . In the obtained Si-containing glassy carbon material, many minute voids were recognized inside the structure.
Table 1 shows the bulk density, bending strength, and oxidation resistance in a high temperature region measured for this Si-containing glassy carbon material.

Comparative Example 5 A Si-containing glassy carbon material was produced under the same conditions as in Example 2 except that tetraethoxysilane was used as the Si source and ethanol was used as the diluting organic solvent.
At the stage of dropping into the phenol resin solution, the reaction system remarkably gelled, cracking occurred in the molded body during molding and curing, and the Si-containing glassy carbon material could not be obtained.

[0040]

[Table 1]

From the results shown in Table 1, the Si-containing glassy carbon material obtained by the production method of the present invention is improved in bending strength and oxidation resistance as compared with the comparative example product produced by the production method which deviates from the conditions of the present invention. It was recognized that

[0042]

Industrial Applicability As described above, according to the present invention, an Si-containing glassy carbon material having a homogeneous and dense composite structure containing an atomic level Si component as a continuous phase and having excellent oxidation resistance is industrially produced. Can be manufactured. Especially S
It is possible to easily obtain a high-quality Si-containing glassy carbon material which is always free of material defects even under the manufacturing conditions in which the i content is high. Therefore, a sufficiently stable use condition is guaranteed even under severe conditions in which desorption of fine particles from the tissue and oxidative damage are likely to occur, and therefore industrial members for various application fields including semiconductor members. It is extremely useful as a manufacturing technology.

────────────────────────────────────────────────── ───

[Procedure amendment]

[Submission date] March 4, 1996

[Procedure amendment 1]

[Document name to be amended] Statement

[Correction target item name] Name of invention

[Correction method] Change

[Correction contents]

Method of producing Si-containing glassy carbon material

Claims (2)

[Claims] 1. An aminosilane compound containing a single Si atom in one molecule is mixed and diluted with an organic solvent having a high carbonization residual ratio, and the diluted solution is dropped into a thermosetting resin liquid and mixed by stirring to obtain After the obtained aminosilane-containing resin composition is molded and cured into a predetermined shape, the molded body is subjected to 800 in a non-oxidizing atmosphere.
A method for producing a Si-containing glassy carbon material, which comprises performing a carbonization treatment at a temperature of ℃ or more. 2. The method for producing a Si-containing glassy carbon material according to claim 1, wherein the organic solvent having a high carbonization residual rate is furfuryl alcohol, furfural, or a mixture thereof.