JP2000159575A - Glassy carbon pipe and its production - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a glassy carbon pipe useful as the inner tube of a CVD device for producing semiconductors, etc., not containing a filler contaminating the CVD, and suitable as a large diameter member for which high heat resistance and corrosion resistance are required, and to provide a method for producing the same. SOLUTION: This method for producing a glassy carbon pipe comprises molding pipe raw materials containing a thermoplastic resin 3 by a centrifugal molding method and then applying a carbonization treatment to the obtained thermosetting resin molded product. Therein, the thermosetting resin as the pipe raw material has a curing property that a time for reaching a curing degree of 10% (T10) at 115 deg.C is 5-60 min, and further has a flowing property of >=60 mm at 100 deg.C in the disk type flow test of JIS-K6911. The method can give the glassy carbon pipe having a diameter of >=15 mm and substantially not containing a filler.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a glassy carbon pipe and a method for manufacturing the same, and more particularly, to a glassy carbon pipe excellent in heat resistance, gas impermeability and corrosion resistance, which is used for manufacturing semiconductors. TECHNICAL FIELD The present invention relates to a glassy carbon pipe suitable as an inner tube of a CVD apparatus and a method for producing the same.

[0002]

2. Description of the Related Art Quartz glass is generally used for members requiring heat resistance, gas impermeability and corrosion resistance, such as an inner tube of a CVD apparatus for semiconductor production. However, quartz glass has a problem that it is easily corroded by a fluorine-based gas or a mixed solution of nitric acid and hydrofluoric acid for cleaning, and its life is extremely short.

Therefore, glassy carbon is expected as a material to replace quartz glass. Glassy carbon is a carbon material obtained by carbonizing a thermosetting resin such as a phenol resin or a furan resin or cellulose at a high temperature range of about 1000 ° C. or more, and has a heat resistance higher than that of quartz glass. In addition to this, it has the characteristics that the mechanical strength and hardness are equivalent to that of quartz glass, the gas permeability is extremely low, and the corrosion resistance to the above-mentioned chemicals is extremely excellent.

Accordingly, materials containing glassy carbon as a main component have been used in various fields as structural members having high heat resistance. However, in order to obtain a glassy carbon pipe, it is necessary to manufacture a thermosetting resin pipe as a precursor thereof. Unlike a thermoplastic resin, a thermosetting resin has a low viscosity in a molten state. It is difficult to obtain a pipe-shaped molded body by using a method of extrusion molding, compression molding, injection molding or the like of a molding method in which a thermoplastic resin is usually used alone with a thermoplastic resin. In particular, the inner tube used for the CVD apparatus has, for example, an approximate diameter of 400 m.
m, a length of 1000 mm, and a thickness of 3 to 5 mm with open pipes at both ends, and it was extremely difficult to form such a shape using only a thermosetting resin.

[0005] Since thermosetting resins have poor moldability, they are usually molded after being mixed with various fillers. For example, if an inorganic filler such as magnesia, talc, mica, or the like is added to a thermosetting resin at a high concentration and mixed, a high-strength pipe suitable for a cable tube or the like can be formed by extrusion molding. Further, when a carbon fiber non-woven fabric is impregnated with a liquid resin and compression-molded, a carbon fiber / thermosetting resin composite having high strength and elastic modulus can be obtained. That is, when used as a thermosetting resin molded article without carbonization, the use of the above filler is preferable because it can improve the mechanical properties of the resin material and can save the amount of expensive resin used. Met.

However, in order to obtain glassy carbon, it is necessary to carbonize these thermosetting resin molded products in a high-temperature inert atmosphere. In this case, if a filler is contained, the following problem occurs. Cause serious problems.
That is, since liquid resin generally shrinks by more than 10% during carbonization, when a resin composite pipe containing a filler is carbonized, cracks occur at the interface between the glassy carbon portion and the filler portion with little dimensional change. As a result, there is a problem that gas impermeability and corrosion resistance, which are characteristics of glassy carbon, are significantly impaired. For example, in the case of the above-mentioned carbon fiber-thermosetting resin composite (so-called precursor of carbon-carbon composite material), a member obtained by carbonizing the composite contains many cracks and voids. And carbonization had to be repeated several times.

Further, the filler component has a lower corrosion resistance than glassy carbon, and furthermore, there is a possibility that impurities caused by the filler itself may be scattered in the CVD apparatus to contaminate the CVD film. It is not suitable for use in inner tubes and the like.

[0008] Accordingly, there is a strong demand for the development of a glassy carbon pipe containing no filler, and a pipe having a glassy carbon content of 95% or more, more preferably a pipe consisting essentially of glassy carbon. Therefore, development of a glassy carbon pipe which can be suitably used particularly for a CVD apparatus and a method for producing the same have been desired.

Accordingly, the present inventors have intensively studied a molding method of a thermosetting resin containing no filler based on the prior art.
As a result, they have found that it is possible to obtain a pipe-shaped thermosetting resin molded article by injection molding or compression molding, which are conventionally used. However, in order to facilitate removal of the resin member from the mold, at least an angle of 0.5 °
Preferably, it is necessary to form a taper of one degree, and furthermore, the size and shape change in the carbonization step after molding are added. Therefore, the inner diameter of the glassy carbon pipe as the final product is not uniform, and the inner diameter of both ends is not uniform. It was found that the variation in the inner diameter exceeded 1% of the length. This means
It is not preferable because it is impossible to form a cylindrical member having an industrially useful cylindrical body, that is, a cylindrical member having the same inner diameter throughout. In addition, since injection molding and compression molding are originally unsuitable for pipe molding, productivity is low, and furthermore, resin pipes which are the precursors of large-diameter glassy carbon pipes as described above are molded. To do so, an extremely large mold was required, and it was practically difficult to manufacture it on an industrial scale at low cost.

[0010] Due to the above-mentioned circumstances, in the case of a glassy carbon pipe containing no filler, if it is attempted to obtain a cylindrical pipe having a constant inner diameter by compression molding or injection molding, a taper for die cutting is required. A pipe that is so short and thin that processing does not need to be performed on the mold,
Those having a diameter of less than 15 mm and a diameter of less than 15 mm are the limits in manufacturing technology. For a pipe having a diameter or length exceeding this, it is necessary to apply a taper process to the mold, so that there is inevitably a difference in the inner diameter of the pipe exceeding 1% of the length. In addition, it was difficult to form a thermosetting resin containing no filler into a pipe by extrusion.

In addition to the molding methods mentioned above, centrifugal molding methods are disclosed in JP-A-6-247770 and JP-A-4-149067 as methods suitable for pipe molding. However, the methods disclosed in these publications are methods using a filler, and there is no method using no filler or a description suggesting the method. In fact, the present inventors have attempted to form a glassy carbon pipe simply by removing the filler from the methods disclosed in these publications, but the formed body is liable to foam. Strict temperature control was required, and it was difficult to obtain a molded article without voids with good productivity and reproducibility. Also,
Even when a good molded product is obtained, many voids are formed in the molded product due to the vapor of the solvent remaining in the subsequent curing or carbonization process and the generated gas, and it is excellent in gas impermeability and corrosion resistance It was difficult to obtain vitreous carbon.

Further, a reference ("Carbon", 1996, vo
l.34, No.6, pp.789-796), a liquid phenolic resin is continuously applied to the outer surface of a rotating metal cylinder in a spray form while removing the solvent and performing a curing reaction of the resin. A method for obtaining a precursor resin pipe of carbonaceous carbon is disclosed. However, the glassy carbon pipe exemplified in the above technical literature has an inner diameter of 12.7 mm,
There is no disclosure of a method for producing larger diameter pipes. When the present inventors tried this method, they precisely controlled many factors such as resin supply speed, cylindrical rotation speed, resin curing reaction and temperature for controlling the amount of solvent evaporation, and the like. However, a resin pipe having a uniform thickness could not be obtained.

As described above, various methods of producing a glassy carbon pipe have been studied. However, a method of producing a pipe which can be formed even with a small amount of filler and can cope with a large diameter is not sufficient. In addition, there has not been provided an inner tube of a CVD apparatus which has both heat resistance, gas impermeability, corrosion resistance, and durability and has low contamination.

[0014]

SUMMARY OF THE INVENTION The present invention has been made in view of the above circumstances, and is intended to provide a glass pipe made of glassy carbon with low contamination which is optimal as an inner tube of a CVD apparatus for semiconductor production. And furthermore,
An object of the present invention is to provide a glassy carbon pipe having a large diameter and a uniform thickness, which cannot be manufactured by a conventional method, and a method for manufacturing the same.

[0015]

Means for Solving the Problems The manufacturing method of the present invention which has solved the above-mentioned problems is that a pipe material containing a thermosetting resin is formed into a thermosetting resin molded product by a centrifugal molding method, and the thermosetting resin molded product is produced. A pipe made of glassy carbon by subjecting the pipe to a carbonization treatment, wherein the thermosetting resin as a raw material of the pipe is a degree of cure at 115 ° C. of 10% (T
The gist of the present invention is to use a thermosetting resin having a curability of 10) of 5 to 60 minutes and a flowability of not less than 60 mm at 100 ° C. in a disk flow test of JIS-K6911. In addition, according to the method of the present invention, even if 99% by weight or more of the pipe raw material is a thermosetting resin, it can be formed into a pipe shape.

Further, the glass-like carbon pipe of the present invention which has solved the above-mentioned problems has a gist of 15 mm or more in diameter and substantially containing no filler.

[0017]

BEST MODE FOR CARRYING OUT THE INVENTION The present inventors have conducted intensive studies with the aim of solving the above-mentioned problems, and as a result, if a thermosetting resin having a specific curability and fluidity is used, a filler is mixed. The present inventors have found that a pipe-shaped molded body can be obtained by a centrifugal molding method, and have arrived at the present invention.

The thermosetting resin used as a raw material for the pipe in the present invention has a curability of not less than 5 minutes and not more than 60 minutes at 115 ° C. at a resin curing degree of 10% (T10), and the JIS-K6911 circle. It is a thermosetting resin having a fluidity of 60 mm or more at 100 ° C. in a plate-type flow test.

As the curability of the thermosetting resin, it is necessary that the raw material of the pipe be plastically deformed into a cylindrical shape along the mold before completing the curing reaction.
It is necessary that 10 is 5 minutes or more. If the above T10 is less than 5 minutes, curing of the resin is completed before the pipe raw material is deformed into a cylindrical shape along the mold, or a gas component contained in the raw material or generated during molding. Since the curing of the resin is completed before the gas components dissipate, a resin molded body having a desired shape and free from bubbles and cracks cannot be obtained. T10 is desirably 10 minutes or more, and if the time until the completion of curing is increased, molding can be performed with a smaller centrifugal force (small number of rotations). However, a resin having an excessively long curing time is not preferable because a large amount of gas is generated at the time of the curing reaction in the rotary mold to cause the molded body to foam and easily contain bubbles.
It is necessary to be within 0 minutes, more preferably within 40 minutes.

In the method of the present invention, centrifugal molding is performed while heating the molding raw material to a temperature higher than the temperature at which the curing reaction of the resin occurs, so that the thermosetting resin used as the raw material has appropriate fluidity at the molding temperature. Must have. In the present invention, JI
S-K6911 having a fluidity value of 60 mm or more when subjected to a disk-type flow test at 100 ° C. is used. Here, the flow test is performed at 100 ° C. for the following reason.
Usually, the curing reaction of a thermosetting resin starts at about 100 ° C., and the fluidity of the resin gradually decreases as the reaction proceeds. Therefore, in order to shape the resin into a cylindrical shape, it is essential that the resin undergoes a certain flow deformation at this temperature, and in order to evaluate this property, a disk-type flow test of JIS-K6911 must be performed. Perform at ° C.

When the value of the fluidity of the forming raw material is less than 60 mm, it is extremely difficult to form a desired cylindrical shape even when a large centrifugal force is applied while heating. If the fluidity of the molding material is 60 mm or more, it can be formed into a cylindrical shape by centrifugal molding.
mm or more is preferable because molding can be performed at a lower rotation speed and in a shorter time.

There is no particular upper limit on the value of the fluidity of the forming raw material. However, since a resin having extremely high fluidity generally contains a relatively large amount of a low molecular weight oligomer component, a large amount of gas is generated during a curing reaction in a rotary mold to easily foam a molded body, and the curing reaction takes a long time. Therefore, the value of the fluidity is desirably 150 mm or less.

As described above, by setting the curing reactivity and fluidity of the raw material of the pipe to a specific range, a filler material which has been impossible by centrifugal molding conventionally is not contained, and substantially no glassy carbon is used. It has become possible to manufacture even pipes.

The raw material for the pipe used in the present invention may have a fluidity and a degree of hardening within the above ranges, and may be in the form of a powder or a liquid or a solution containing a solvent. In the method, powdered pipe feedstock is preferred. The reason is that if a liquid pipe raw material or a solution pipe raw material dissolved in a solvent is used, even if the fluidity and the degree of hardening are within the above range, the gas and solvent vapor generated in the centrifugal molding process may cause This is because the molded body is easily foamed, and voids are easily generated in the glassy carbon pipe as the final product.

In order to obtain a glassy carbon pipe suitable for an inner tube of a CVD apparatus by the method of the present invention, a pipe containing 95% or more of a thermosetting resin having the above-mentioned fluidity and curing degree is used. It is preferable to use a raw material, and it is more preferable to use a pipe raw material in which the thermosetting resin is 99% or more and the remainder is inevitable impurities because contamination during use can be reduced.

As the thermosetting resin contained in the raw material of the pipe, all generally known thermosetting resins such as a phenol resin and a furan resin can be used, and the phenol resin is not particularly limited. It is more preferable for the reasons described below. That is, the phenolic resin has a higher material yield after carbonization than other resins, and therefore has less dimensional change. Therefore, it is suitable for obtaining a glassy carbon pipe having a desired shape and dimensions. The fluidity and degree of cure of the pipe raw material can be controlled by adjusting the amount of thermosetting resin, the amount of catalyst, and the polymerization reaction time, and also by the type and amount of filler and solvent. It is possible.

In producing a thermosetting resin molded article by a centrifugal molding method, a pipe raw material containing a thermosetting resin is charged into a substantially cylindrical mold rotatable in a circumferential direction,
The substantially cylindrical mold may be heated to the curing temperature of the resin while rotating to produce a substantially cylindrical thermosetting resin molded body.

In manufacturing the thermosetting resin pipe, it is recommended to use a centrifugal molding apparatus as shown in FIG. In FIG. 1, reference numeral 1 denotes a cylindrical mold, and at least one end thereof needs to have an opening so that gas generated during a resin curing reaction can escape to the outside.
This mold 1 can be rotated at high speed by a motor or a pulley. In addition, it is desirable to adopt a structure that can be divided from the viewpoint of facilitating removal of the resin pipe. As the material of the mold, metal, ceramic, resin, or the like can be used, but metal is preferable in terms of strength and ease of processing.

In FIG. 2, reference numeral 4 is a schematic explanatory view of a mold for obtaining a pipe having flanges formed at both ends.
By molding using this mold 4, a resin pipe 5 having both ends flanged can be obtained, and by carbonizing the same, a glassy carbon pipe having both ends flanged can be obtained at low cost. be able to. According to the method of the present invention, the outer diameter and length of the glassy carbon pipe are determined only by the inner diameter and length of the cylindrical mold, so that a long pipe having a large outer diameter can be easily manufactured. Also, the thickness of the pipe can be easily controlled by changing the amount of resin loaded in the mold.

The pipe raw material 3 is loaded into the cylindrical mold 1 as shown in FIG. The loading of the resin may be performed with the mold stationary or while rotating. The rotation speed of the mold varies depending on the diameter of the mold and the properties and reactivity of the resin, but is at least twice the gravity, preferably 10 times.
It is desirable to set so that gravity of G or more is generated.

In the present invention, the raw material for the pipe is charged into a centrifugal molding die, and the resin is heated to a temperature at which the curing reaction proceeds while rotating the die. When the pipe raw material has the above properties, the resin is melted by heating, and a compressive force acts by centrifugal force generated by rotation of the mold, whereby the pipe is formed into a pipe shape having a substantially constant inner diameter and a uniform wall thickness. Volatile components contained in the resin and gaseous components generated during the molding process can be dissipated from the resin surface not in contact with the mold. In addition, since the resin on the outside of the pipe directly contacts the inner surface of the rotating mold, the outer surface of the pipe can be formed into a shape substantially equal to the inner surface of the mold.

In the molding method of the present invention, the mold is heated to a temperature higher than the temperature at which the curing reaction of the resin starts while rotating the mold loaded with the resin. (Heating furnace) 2 may be used.

Since various gases including steam are generated during the curing reaction of the thermosetting resin, degassing is important during molding. When a large-diameter pipe such as an inner tube is formed by a general method such as compression molding, degassing is practically impossible. Further, if the molded body is taken out of the mold at a stage where the curing reaction is insufficient to suppress generation of gas, the molded body is deformed in the curing step, so that the shape cannot be maintained.

On the other hand, in the method of the present invention, since a compressive force acts on the resin by centrifugal force due to the rotation of the mold, a pipe having a uniform thickness can be formed. Since the surface not in contact with the mold is open to the atmosphere, the generated gas can be easily dissipated outside the molded body.
In addition, since the resin is heated to a temperature at which a curing reaction occurs while being rotationally molded, it is possible to keep the shape of the pipe without being deformed even after being taken out of the mold. The molding temperature depends on the properties and reactivity of the resin, but is set to 100 ° C. or higher, preferably 120 ° C. or higher.

There is no particular limitation on the method of the carbonization treatment performed after the pipe formation of the thermosetting resin, and the resin molded body is heated to 800 ° C. or more, preferably 1000 ° C. or more in a non-oxidizing atmosphere. The heat treatment can be performed at a temperature. Further, if necessary, before the carbonization treatment, a post-curing treatment may be performed in which the resin molded body is heated at 100 ° C. to 300 ° C. in air or a non-oxidizing atmosphere.

According to the method of the present invention, the diameter is 15
It is possible to manufacture a vitreous carbon pipe having a large diameter of not less than mm (further, not less than 60 mm) and substantially containing no filler.

Hereinafter, the present invention will be described in more detail with reference to Examples. However, the following Examples are not intended to limit the present invention, and any changes in the design based on the gist of the preceding and following aspects will be described. Are included within the technical scope of

[0038]

EXAMPLE 1 The time to reach a degree of cure of 10% (T10) was 25 minutes at 115 ° C., and JIS-K6911 at 100 ° C.
A powdery phenol resin having a disk flow test value of 140 mm was used as a raw material.

The mold used had an inner diameter of 8 with both ends open.
It has a cylindrical shape of 0 mm, a length of 300 mm, and a thickness of 15 mm, and has a structure that can be divided into two by a plane including a center line. 300 g of resin is charged into the mold, and 25 g / min.
While rotating at a speed of 00 rotations, the temperature was raised from room temperature to 120 ° C. for 30 minutes by a heater installed outside the mold, then maintained at this temperature for 10 minutes, and further increased to 160 ° C. for 6 minutes.
The temperature was raised in 0 minutes, and a curing reaction was performed at 160 ° C. for 30 minutes. Thereafter, the mixture was allowed to cool, stopped at 80 ° C., and removed from the mold. As a result, a pipe having a thickness of about 2 mm and a substantially uniform thickness without cracks could be obtained.

The pipe was cured at 230 ° C. for 48 hours, and no change in appearance such as cracks or voids was observed except for blackening due to the curing. further,
When the carbonization treatment was performed at 1500 ° C., a glassy carbon pipe having the shape at the time of curing was obtained.

Further, for the purpose of evaluating the uniformity of the pipe, the variation of the inner diameter was measured by the following method. That is,
The pipe was divided into four equal parts in the length direction, the difference between the maximum value and the minimum value of the inner diameter of each part was determined, and the value (percentage) divided by the entire length of the pipe was defined as the change in the inner diameter. The variation in the inner diameter of the pipe of this example was 0.4%.

Example 2 A phenol resin pipe was molded using the same resin raw material and apparatus as in Example 1 except that a two-piece mold having a diameter of 350 mm and a length of 1000 mm was used. The obtained pipe can be cured while keeping its shape, and when carbonized at 1500 ° C., there is no change in appearance except for the change in dimensions due to shrinkage, and there is no shrinkage of uniform wall thickness. It could be made as a pipe. The variation in the inner diameter of this pipe was 0.8%.

Example 3 A phenolic resin having different curing reactivity and fluidity was prepared by changing the catalyst concentration or the polymerization time, and a resin pipe was molded using the same apparatus as in Example 1;
Time curing was performed, and carbonization was further performed at 1500 ° C. Table 1 shows the properties [curability (T10) and fluidity] of the raw material resin and the properties of the obtained glassy carbon pipe.

[0044]

[Table 1]

No. Examples 1 to 4 are examples using the resin according to the present invention.
%, And a crack-free glassy carbon pipe could be obtained.

No. Nos. 5 to 7 are comparative examples using resins that do not satisfy the conditions according to the present invention. The resin of No. 5 is T
Since the curing speed was too high in 10 minutes for 4 minutes, the curing was completed before it was deformed into a cylindrical shape, and a pipe having a uniform thickness could not be obtained. In addition, degassing from the resin was insufficient, cracks occurred in the pipe after carbonization, and the inside diameter of the pipe was uneven.

No. Resin No. 6 is within the range of the present invention at T10 of 13 minutes, but is a comparative example having a disc-type flow test value of 58 mm, which is smaller than the range of the present invention. Also, the pipe was not formed into a cylindrical shape, and a pipe having a uniform thickness could not be obtained. In addition, degassing from the resin is insufficient,
The resin molding contained many air bubbles. Cracks also occurred in the pipe after the carbonization treatment.

No. Resin No. 7 was a comparative example in which the curing time was too long, with T10 being 62 minutes, and a large amount of foaming occurred inside the molded body due to the gas generated at the time of molding, and significantly large unevenness also occurred in the pipe inner diameter. . In addition, cracks and foaming occurred during curing and carbonization, so that a glassy carbon pipe could not be obtained.

Example 4 The time to reach T10 was 24 minutes at 115 ° C.
A thermosetting resin molded body was manufactured in the same manner as in Example 1 except that a powdery phenol resin having a disk-type flow test value of JIS-K6911 of 104 mm at 100 ° C was used as a raw material.

The pipe was cured at 230 ° C. for 48 hours, but no change in appearance such as cracks or voids was observed other than blackening due to curing. In addition, 1
When the carbonization treatment was performed at 500 ° C., a glassy carbon pipe having the shape at the time of curing could be obtained.

When a dense resin pipe is formed by completely removing the gas component contained in the resin raw material and the gas component generated during the molding, the bulk density of the molded pipe and the true density of the resin match. It is thought that. Therefore, the ratio of the bulk density of the resin pipe to the true density of the resin (specific density)
Is an index of moldability. The specific density of the thermosetting resin molded product obtained in this example was more than 0.99. Therefore, it is considered that the resin pipe obtained in the present example had gas components contained in the resin raw material and gas components generated during molding almost completely removed. The variation in the inner diameter of the carbon pipe obtained in this example was 0.1%.

Example 5 A phenol resin pipe was formed using the same resin raw material and apparatus as in Example 4 except that a two-piece mold having a diameter of 350 mm and a length of 1000 mm was used. This pipe can be hardened while maintaining its shape, and when carbonized at 1500 ° C, there is no change in appearance except for dimensional change due to shrinkage, and there is no shrinkage of uniform thickness and glass-like carbon pipe. And could be.

The specific density of the thermosetting resin molded article obtained in this example exceeded 0.99, and the appearance of the molded pipe was good as in the case of the carbon pipe of Example 4. The variation in the inner diameter of this pipe was 0.4%.

Example 6 A phenolic resin having different curing reactivity and fluidity was prepared by changing the catalyst concentration or the polymerization time, and a resin pipe was molded using the same apparatus as in Example 1;
Curing was performed for an hour, and carbonization was further performed at 1500 ° C. Table 2 shows the properties of the resin and the results of manufacturing the glassy carbon pipe.

[0055]

[Table 2]

No. Examples 1 to 5 are examples using the resin according to the present invention. In each case, a pipe made of glassy carbon having a variation in inner diameter of 1% or less and having no crack was obtained.

No. Nos. 6 to 9 are comparative examples using resins that do not satisfy the conditions according to the present invention. 6 and no. For the resin No. 8, the curing speed was too high at T10 of 4 minutes, so that the curing was completed before the resin was deformed into a cylindrical shape, and a pipe having a uniform thickness could not be obtained. In addition, degassing from the resin was insufficient, cracks occurred in the pipe after carbonization, and the inside diameter of the pipe was uneven.

No. Resin No. 7 is a comparative example in which T10 is 63 minutes and the curing time is too long, and a large amount of foaming occurs inside the molded body due to gas generated at the time of molding, and extremely large unevenness also occurs in the pipe inner diameter. . In addition, cracks and foaming occurred during curing and carbonization, so that a glassy carbon pipe could not be obtained.

No. The resin of No. 9 is within the range of the present invention at T10 of 8 minutes, but is a comparative example having a disk-type flow test value of 58 mm, which is smaller than the range of the present invention. Also, the pipe was not formed into a cylindrical shape, and a pipe having a uniform thickness could not be obtained. Further, degassing from the resin was insufficient, and the resin molded body contained many air bubbles. Cracks also occurred in the pipe after the carbonization treatment.

[0060]

Since the present invention is constructed as described above, the present invention relates to a glassy carbon pipe including an inner tube of a CVD apparatus for manufacturing a semiconductor, and a filler which causes contamination of the CVD apparatus. It is possible to provide a glassy carbon pipe suitable as a large-diameter member that does not contain the component and that is required to have high heat resistance and corrosion resistance, and a method for producing the same.

[Brief description of the drawings]

FIG. 1 is an explanatory view showing a centrifugal molding apparatus that can be used in the method of the present invention.

FIG. 2 is an explanatory view showing a molding die (a) that can be used in the method of the present invention and a glassy carbon pipe (b) obtained by the above-mentioned die.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Mold 2 Heater 3 Thermosetting resin 4 Mold for molding resin pipe with flange 5 Resin pipe with flange

 ────────────────────────────────────────────────── ─── Continuing from the front page (72) Inventor Setsu Nishizawa 1-5-5 Takatsukadai, Nishi-ku, Kobe F-term in Kobe Steel Research Institute Kobe Research Institute (reference) 4G032 AA07 AA13 BA04 GA06

Claims (3)

[Claims] 1. A method for producing a glassy carbon pipe by forming a pipe material containing a thermosetting resin into a thermosetting resin molded article by centrifugal molding, and subjecting the thermosetting resin molded article to a carbonization treatment. The thermosetting resin as a raw material of the pipe has a curability of reaching a curing degree of 10% (T10) at 115 ° C. of 5 to 60 minutes, and has a hardness of 100 in a disk flow test of JIS-K6911. A method for producing a glassy carbon pipe, characterized by using a thermosetting resin having a fluidity of 60 mm or more at a temperature of ° C. 2. The method according to claim 1, wherein 99% by weight or more of the raw material for the pipe is made of a thermosetting resin. 3. A glassy carbon pipe having a diameter of 15 mm or more and substantially containing no filler.