WO1991004954A1

WO1991004954A1 - Carbon fiber-reinforced composite carbon material having excellent thermal shock resistance and production thereof

Info

Publication number: WO1991004954A1
Application number: PCT/JP1989/001034
Authority: WO
Inventors: Soukan Miki; Toshiharu Hiraoka; Touru Hosikawa
Original assignee: Toyo Tanso Co., Ltd.
Priority date: 1989-10-06
Filing date: 1989-10-06
Publication date: 1991-04-18

Abstract

A carbon fiber-reinforced carbon composite material of the invention comprises highly pure carbide felt internally impregnated with graphitized pyrolytic carbon. This composite material has an excellent thermal shock resistance and is favorable as, particularly, the first wall of an apparatus for confining nuclear fusion plasma or a member of a rocket.

Description

Specification

Patent application title: Carbon fiber reinforced carbon composite excellent in thermal shock resistance and method for producing the same

The present invention relates to a carbon material, a method for producing the same, and a use thereof, and more particularly, to a carbon material having a small amount of outgas and erosion and having excellent heat shock resistance, a method for producing the same, and a use thereof. The present invention provides, for example, a first wall structural material of a fusion plasma confinement device, a locating member, a target member, a protective material for a sputtering device (a beam concentrator used in a sputtering device, Beam shielding materials such as wall protection materials), boats for plasma-enhanced chemical vapor deposition (hereinafter referred to as “CVD”) facing the plasma, electrodes for ion implanters, other plasma, electro-beam (EB), The present invention relates to a carbon composite material suitable for a protective material, a jig, an armor material, an electrode, and the like facing a neutron beam (NB) and an ion beam (IB).

Background art

For convenience of explanation, under the most severe conditions among the uses according to the present invention The first wall material of the fusion plasma confinement device used will be described as a typical example.

Graphite material is composed of a simple substance and has features such as a low atomic number and a high melting point, so it has been used as the first wall material of fusion plasma confinement devices.Currently, isotropic high-density graphite is used. It is the mainstream. Further, graphite resistant to thermal shock compared with Sera Mi poke general, also has low vapor pressure (2 5 0 0 'C at about ^{_{5 X 1 0 - fa at m}} ) because it has characteristics such as nuclear fusion apparatus It is in good agreement with the requirements of However, despite these advantages, graphite has the following problems. In other words, there is a danger that the plasma temperature will drop due to the release of the gate gas, and finally, a disruption (plasma collapse) will occur. (2) Difficulty based on erosion, such as spattering and sublimation, which results in material consumption. (3) Even though it is resistant to thermal shock, the thermal conditions of the fusion reactor are severe and may cause cracks, separation, etc.と When 14 MeV neutrons are irradiated in the presence of a temperature gradient, cracks may be generated and propagated due to internal stress caused by deformation induced by irradiation. .

In addition to the isotropic high-density graphite, carbon arrowhead reinforced carbon composites (referred to as C / C composites) have been used, but conventional C / C composites have been used. It is made by soaking coal tar bite, resin, etc. into a matrix, which has the problem that the matrix portion is selectively and significantly consumed when EB irradiation is performed.

Such problems arise more or less not only in the first wall material, but also in rocket nozzles and other uses.

The problem to be solved by the present invention is to solve the above-mentioned drawbacks of the conventional carbon material and to provide a composite material which is high in purity, contains little gas and erosion, and has excellent thermal shock resistance. Disclosure of the invention

(i) depositing pyrolytic carbon (hereinafter referred to as "Py C") inside the carbonaceous flute, particularly to the deeper part thereof; and (ii) particularly preferably purifying the carbonaceous flute in one apparatus. It is to use a production method that performs continuous treatment, PyC deposition, and graphitization.

In other words, the present inventor used a conventional carbonaceous melt to solve the above-mentioned disadvantages of lead materials and C / C composite materials, and to achieve higher purity and higher purity which could not be achieved by the conventional method.鋭 Intensive research has been conducted in order to develop a more economical method for producing C / C composites with less thermal gas and erosion and excellent thermal shock resistance. Result, hydrocarbons, in particular d -C _e, rather preferably is CH *, P and C ₃ hydrocarbon gas such as H ₈ if Ku hydrocarbon compound to the carbonaceous Fuyuru preparative deep layer is thermally decomposed y C It has been found that a C / C composite material with high purity, little art gas and erosion, and excellent thermal shock resistance can be obtained when osmotic precipitation is performed. At this time, high-purity treatment, PyC impregnation treatment, and graphitization treatment are performed sequentially in one device, resulting in cost of moving goods, breakage during the process, energy loss due to cooling and heating cycle of the device. Establish an economical manufacturing method while reducing the consumption of halogens due to high purification, reducing the consumption of halogens due to high purification, and reducing the consumption of exhaust and wastewater. It has been found that a revolutionary manufacturing method can be developed to obtain a C / C composite material with high purity, low art gas and erosion, and excellent thermal shock resistance that could not be achieved by conventional methods. Here, the present invention has been completed.

It should be particularly noted that, according to the study of the present inventor, PyC was immersed in the deep part of this kind of carbonaceous fiber, so that the bulk density was large, especially the amount of art gas and erosion was small, and the heat resistance was low. It has been found that a composite material having high impact properties can be obtained, and a new fact that a composite material having such properties is extremely effective as the first wall for fusion is found. The composite material of the present invention in which PyC is impregnated to such a deep part has a bulk density. It is a dense composite material of 1.40 g / o3 or more, which is an extremely strong solid block. In this case, even if PyC is immersed in the carbonaceous float, the above characteristics are extremely low only in the surface layer.

First, the configuration of a C / C composite material using PyC as a matrix based on the carbonaceous melt according to the present invention will be described.

The C / C composite material according to the present invention is obtained by impregnating PyC into the inside of an air-permeable carbonaceous material. As described above, in the C / C composite material of the present invention, by allowing Pyc to penetrate into the carbonaceous flute and bead out, a strong adhesion between the carbonaceous filter and PyC is obtained, and the excellent properties of PyC are obtained. Cracking, separation, cracking, etc. can be prevented by the heat shock resistance.

As the carbonaceous filtrate, any of those conventionally used can be used, and more specifically, for example, those using organic fiber as a starting material, coal, petroleum tar, pitch, etc. Typical examples include raw materials, synthetic fibers such as polybutyl alcohol and polyacrylonitrile, and raw materials of rayon.

The present inventors have conducted intensive studies on PyC immersion using the above-mentioned raw materials, and as a result, the rayon-based carbonaceous ferrite was obtained under the same conditions.

(Temperature, hydrocarbon concentration, degree of vacuum, gas flow) PyC soaked As a result, it was found that the amount of deposited PyC was the largest. This fact is thought to be due to the fact that the shape of the lay-based carbon fiber differs from other carbon fibers in that the cross-sectional structure shows a polygonal shape and the largest specific surface area. Is not clear. Therefore, it was found that the use of a rayon-based carbonaceous material as a base material for the immersion of PyC to the desired density can shorten the PyC immersion treatment time, and is very economically advantageous.

The bulk density of the carbonaceous float used in the present invention is desirably 0.03 to 0.3 [g / ci]. If it does not reach 0.03 (g / ci), the time required for PyC infiltration becomes long, and the content of carbon fiber is too small to achieve the intended purpose as a reinforced composite material.

If it is larger than 0.3 (g / ci), the so-called "pseudo-isotropic" characteristic, which is a feature of the carbonaceous flute itself, is lost. It is needless to say that the isotropic method is advantageous in that the heat diffusion is performed uniformly and the heat load is reduced.

The results of measuring the relationship between the bulk density of the carbonaceous felt used in the present invention and the degree of PyC leaching are shown below. It is In this measurement Te temperature 1 1 0 0, total pressure 2 Torr (C ₃ Η ₈ gas 6, Eta ₂ gas 7 0 £ STP / rain) was conducted under the reaction conditions. The results are as follows. TP 0034

However, at 0.03 or less, the deposition speed is very slow.

This carbonaceous fiber is subjected to a high-purity treatment, and then a dense and high-density PyC is placed inside the carbonaceous fiber with a bulk density of 1.4 (g / of) or more, preferably 1.4 to 2, 0 '[g / ci). In this case, it is preferable that PyC is particularly dense and high in purity. Here, high purity means that the total ash content is 1 Oppm or less. At this time, if the purity is out of the above range,

PyC itself tends to contaminate the equipment due to impurities.

To further explain the bulk density of the C / C composite material of the present invention, it is desirable that this be 1.4 [g / ci) or more.

If it does not reach 1.4 (s / ci), the strength will be weak as already mentioned above, but the thermal conductivity, which is essential for other heat-resistant and shock-resistant properties, is too low. There is a risk that the lock may occur.

However, the theoretical density of PyC itself is about 2.26 (g / ci), and since it has carbon fibers, it is larger than this value in principle. In practice, there is a slight pore space in the product, so in reality, the upper limit is about 2.05 to 2.10 [g Zcrf j]. To infiltrate and precipitate PyC to this extent, the deposition efficiency is greatly reduced, the reaction time becomes longer, and it is economically disadvantageous. Taking these factors into consideration, it is generally preferable to keep the bulk density of the composite at 1.4 or more and around 2.0 in terms of heat diffusion, strength, and resistance to thermal load from plasma. For reference, polarizing microscope photographs of cross sections near the surface of the C / C composite material having a bulk density of 1.6 (g / αϋ) and 1.9 μg / ci) are shown in FIGS. 1 and 2, respectively.

Another advantage of the C / C composite of the present invention is that the felt itself is so-called "pseudo-isotropic". In other words, although PyC penetrates into the carbonaceous fiber, the C / C composite material is substantially substantially formed because PyC is substantially uniformly deposited in the carbon fiber constituting the fiber. " It is "pseudo-isotropic". This isotropic property plays an important role in uniformly dispersing heat and reducing thermal load. Here, “pseudo-isotropic” means that PyC itself is a strongly anisotropic carbon material, but the carbon fibers constituting the flute exist randomly in all directions, ie, isotropic. When PyC is deposited on the surface of the carbon fiber, the composite itself exhibits substantially isotropic properties in terms of thermal conductivity, expansion coefficient, and other physical properties as a whole. It is said that it becomes.

The method itself for infiltrating PyC in the present invention is well known in other fields, as described in the literature such as “Introduction to Carbon Materials” (published by the Japan Society for Carbon Materials, January, 1974). The general embodiment is described as follows.The pyrolysis of a carbon-generating material, for example, a hydrocarbon gas or a hydrocarbon compound having 1 to 8 carbon atoms, especially a carbon compound having 3 carbon atoms, deposits PyC on a substrate. It has been infiltrated. On the other hand, the hydrocarbon concentration for concentration control (usually using H ₂ gas as a diluting gas) is 3 to 30% or 5 to 15%, and the total pressure is 100 Torr, preferably. It is desirable to operate under the condition of 50 Torr or less.

When such an operation is performed, hydrocarbons form giant carbon compounds near the surface of the substrate by dehydration, thermal decomposition, polymerization, etc., which are deposited on the substrate, deposited, and further dehydrogenated. This leads to the formation of a dense PyC film, or permeation and impregnation. However, 0 _z, because the co-existence of H ₂ 0 is an adverse effect, arbitrariness preferred is better to avoid. The temperature range for the deposition is generally a wide range from 800 to 250 ΐ, but PyC is deposited in a relatively low temperature range of less than 130 ° C to immerse as much as possible. It is desirable to use a conventional method of isolating, such as the conventional isothermal method, temperature gradient method, and pressure gradient method. There is a pulse method for the purpose of shortening time and densification as a more recent method.

In the present invention, the conditions for infiltrating the PyC and the method of soaking are not important at all, and various formation methods may be used as long as the PyC having the above-mentioned predetermined requirements is permeated and deposited in the deep part of the carbonaceous float. Either one can be used, but one embodiment is as follows.

In the PyC immersion treatment, the temperature is preferably lower than 130 ° C. and the pressure is lower than 100 Torr, preferably lower than 50 Torr.

At higher temperatures, PyC tends to break out on the surface of the substrate, forming closed pores in the PyC film near the surface, making it no longer possible to soak. If the pressure is higher than 100 Torr, the gas diffusion becomes worse, the raw material gas does not sufficiently reach the inside of the base material flute, and there is also a tendency that closed pores are formed on the surface.

As the carbonaceous felt used in the present invention, various kinds of conventionally known ones can be used. In particular, it is preferable to immerse PyC in highly purified water. Purification at this time means that the amount of impurities is small, and it is usually preferable that the total ash content be 1 O ppm or less.

In this case, the purifying method is as follows. Means of contacting with rogen gas to convert metals, which are built up as impurities, into halides with higher vapor pressure

(For example, Japanese Patent Application No. 61-2422131), the power is not limited to this. Examples of the halogen-containing gas used at this time include halogen-containing gases such as chlorine or fluorine and a gas of a compound thereof, and more specifically, 2-fluorinated gas, fluorine gas, and the like. Is mentioned.

It is preferable to purify the carbonaceous fur- ter as high as possible to the inside, so it is effective to perform it before applying PyC treatment. In other words, in order to purify the interior of the felt, the effect is small unless the halogen compound enters the interior of the felt and the halogenated and vaporized impurities are not removed to the outside of the felt. For this purpose, the order of the steps is to carry out Py C treatment after purifying the gas permeable carbonaceous frit in advance.

In addition, it may be preferable to fluctuate the pressure in the reaction vessel to increase or decrease the pressure in order to more quickly and reliably purify the product. The effect is particularly large when the air permeability of the flute is large.

In general, high purification is carried out under reduced pressure conditions in the reaction system, for example, while maintaining the total pressure at 100 Torr or less, to remove carbonaceous filtrate from 150 to 200 • Keep the temperature at C and distribute the halogen compound. Increase or decrease the pressure in the reaction system as necessary. In any case, the amount of impurities can be easily reduced to 10 ppm or less by the method of the present invention. Next, a method for producing a C / C composite material according to the present invention will be described. As a method for producing the C / C composite material of the present invention, basically, a carbonaceous material is highly purified, and then PyC is infiltrated into the inside of the material. Thereafter, it is graphitized at a high temperature of at least 250, preferably at least 280 to improve the thermal conductivity.

Since PyC is a particularly graphitizable material, the improvement in thermal conductivity by heat treatment is very remarkable.

In the present invention, a method in which each step is performed under reduced pressure or high vacuum using high-frequency heating means is a preferable representative example, and a preferable specific example is a method using an apparatus shown in FIG. . The method using this device will be described in more detail as follows.

First, after the air inside the vessel was replaced with N _z gas and air with N ₂ gas from the gas supply pipe (8), Metsu圧from the gas discharge pipe (1), or a non-oxidizing atmosphere evacuated and pressurized And

Next, a voltage is gradually applied to the induction coil (5) to heat the susceptor (6), and the radiant heat causes the heated carbonaceous felt (4) to be heated.

0 to 20000, and adjust the halogen gas from the gas supply pipe (8). For example, supply 2-fluorocarbon (the flow rate is reduced by the amount of carbon material to be heated in the vessel, for example, about 17 Q. NTP / kg) for about 2 to 10 hours.

The inside of the container is kept at 10 O Torr or less, preferably at 50 Torr or less, from the start of heating.

Gradually cooled when the highly purified operation completes adjusted to about 1 0 0 0 ~ 1 3 0 0 ΐ, is rather to be a hydrocarbon gas such as C ₃ Eta _8, while the hydrocarbon compound is thermally decomposed Infiltrate PyC inside the flute. In the meantime, if necessary, the temperature can be lowered once, the product can be taken out, and the state of drought, deposition, and soaking of pyrolytic carbon inside the float can be observed and measured. This intermediate chucking operation can be repeated several times to produce a product having the required bulk density. However, the conditions can be determined empirically for products with regular shapes and sizes, so it is possible to perform certain operations.However, it is more reliable to carry out repeated immersion operations for irregularly shaped products, etc. It is. Thereafter, it is heat-treated at 250 ° C. or more, preferably 280 ° C. or more, to be graphitized.

Stop energization, return to normal pressure and normal temperature while filling and replacing the vessel with N ₂ gas.

In the step of removing impurities, that is, in the step of high purification, the vacuum high-frequency heating furnace according to the present invention is extremely convenient. That is, heated The first advantage of contacting the carbonaceous fur- tle with halogen under reduced or high vacuum is that the consumption is very small. Under reduced pressure or high vacuum, the halogen gas expands and is used, so the utilization efficiency is high and the contact with the flute is good. Therefore, according to the experimental study of the inventor of the present invention, 1 Compared to 0 £ NTP / kg, using the device shown in Fig. 3 can reduce the consumption of 3 £ NTP / kg and the consumption of halogen gas to about 1/3. Another advantage is that the impurities in the halogen and / or hydrogenated furl are under reduced pressure, so they are easy to volatilize and desorb to the outside, and are faster despite the use of small amounts of halogen gas. Higher purity is obtained.

In the present invention, it is desirable to maintain the pressure in the vessel at the time of high purification or graphitization with the purification within 100 Torr or less. The pressure in the vessel is the force indicated on the pressure gauge as the sum (total pressure) of the vapor pressures (partial pressures) of the various compounds of the halide, chlorinated and / or fluorinated impurities. When the pressure is higher than 0 Torr, the decompression effect is reduced, so that the time required for high purification is long, and the effect of the purity reduction is not so large.

As one application example of the practice of the present invention, when the pressure in the reaction vessel is raised or lowered during high-purity operation by changing the pressure inside the reaction vessel, the diffusion and replacement of the halogen gas into the deep part of the flute and the deep part From In some cases, the elimination and substitution of the halogenated product may be complete, which is more effective.

Since the high-purification treatment, the PyC treatment, and the graphitization treatment are successively performed under vacuum, the c / c composite material of the present invention has a small amount of art gas. In addition, the amount of art gas is reduced by PyC treatment. This point is disclosed in Japanese Patent Application No. 62-304405 filed earlier by the present applicant.

By thermally treating PyC at a temperature of 250 ° C. or higher, preferably 280 ° C. or higher, it becomes very graphitic, and the bond between graphite crystals becomes stronger. In addition, the thermal conductivity of the C / C composite material having a bulk density of 1.4 [g Zcii!] Or more is 100 CKCal / m · hr ♦] or more. Very strong against erosion such as sputtering due to plasma irradiation.

In the present invention, various shapes can be produced by further utilizing the flexibility of the felt. For example, it can be said that the C / C composite material of the present invention can be subjected to PyC immersion treatment after being formed into a crucible shape or a curved shape.

In this case, since the felt is flexible and flexible, an appropriate jig (matrix) is made, and along with this, a very small amount of binder resin such as phenolic resin is placed. Attach the soaked melt, cure it with 150 to 200 After temporarily fixing the crossing points of the fusible fibers, or by removing it from the matrix, the resin is carbonized by burning. Even if the obtained melt molded product is transferred to the PyC extraction process performed at a higher temperature, PyC precipitates in the space while maintaining its shape, and products of any shape can be used. Can be obtained. In this case, the amount of resin used is very small, and furthermore,

As PyC is formed, it has virtually no effect on the properties of the product.

The C / C composite material of the present invention has a high purity as described above, has a small amount of art gas and erosion, and has excellent properties such as thermal shock resistance. This is mainly described in the specification, but as other uses, the material for rocket nozzle, the material for the target, and the Protective materials (beam shielding, beam shielding materials such as chamber-wall protective materials), plasma CVD boats facing plasma, electrodes for ion implanters facing ion beams, etc. Other plasma, EB, NB, IB, It can be used for protective materials, jigs, armor materials and electrodes, etc. facing

In addition, the epoch-making properties inherent in PyC (impermeability, carbon powder does not adhere, does not scatter, hardly wets molten metal, etc.) Due to the synergistic effect of the present invention, the C / C composite of the present invention can be used for various applications other than the above.

Fig. 1 and Fig. 2 are polarization micrographs of the cross section of the C / C composite material. Fig. 3 is a side cross section of an example of a vacuum / high frequency heating type high-purity C / C composite production apparatus according to the present invention. Is schematically shown. However, the numbers in Fig. 3 indicate the following.

(1) ... Gas exhaust pipe (6) Susceptor

(2) Insulation material (7) Insulation tray

(3) Insulation material (8) Gas supply pipe

(4) Heat insulation material to be heated (9) Water-cooled jacket

(5) High frequency coil

FIG. 4 is a drawing showing an example in which the composite material of the present invention is used for a rocket nozzle (10 is a stainless steel outer cylinder, (12) is a composite material of the present invention, and (13) is a light showing a screw). Best form to apply

Hereinafter, the present invention will be described specifically with reference to Examples, but the present invention is not limited to these Examples.

Example 1 <High purification process>

Rayon-based carbonaceous felt having a size of 200 × 200 × 10 × 10 and a bulk density of 0.09 [g / cA] was first highly purified using the apparatus shown in FIG. That is, at the stage where the carbonaceous felt was put into a container and heated to 180 Torr under a reduced pressure of 180 Torr, ethane difluoride was allowed to flow from the gas supply pipe (8) to filter the carbonaceous felt. Impurities, especially metal impurities, were volatilized and removed as halogenated compounds with high vapor pressure. The gas supply time was 3 hours.

After the high purification process is completed, then feed the C ₃ H ₈ gas and H _z gas from the gas supply pipe (8), impregnated with PyC inside Fell up by the following conditions.

Reaction conditions: Temperature 1 1 0 0 Te, total pressure 2 Torr (C ₃ H ₈ gas 6,

H ₂ gas 7 0 £ STP no min)

The bulk density of the C / C composite was adjusted by changing the processing time (100-350 hr).

Graphitization process>

After the completion of the PyC treatment, the temperature was raised to 290 O'C and maintained for 3 hours under a decompression pressure of 80 Torr.

Let the temperature rise from room temperature to 100,000, 400,700, Each of the samples was held for 30 minutes, and the gas release characteristics were evaluated based on the total amount of gas release at each temperature. For the test specimen, the C / C composite material obtained above was processed to a dimension of 1 x 10 x 10 x 10 and used.

Heat load test>

The heat load test was evaluated by an electron beam irradiation test, assuming a plasma dislocation.

As a test specimen for measurement, the C / C composite material obtained above was processed into a size of 30 × 30 × 10 mm and used.

Electron beam irradiation conditions:

Acceleration voltage: 120 KV

Rusting frequency; 350 K H Z

Heat flow velocity: about 100 MWZnf ·

Heating time; 200 ms

Comparative example

For comparison with the C / C composite material of the present invention, a C / C composite material was obtained by immersing the same amount of coal tar bite in the same rayon-based carbonaceous material as above.

As a process, coal tar bitches were immersed and fired four times, and then graphitized. Thereafter, a high purification treatment was performed. The conditions for the graphitization and the purification treatment were the same as above. C / C for comparison The bulk density of the composite was 1.7 μg / ci). The test pieces for gas release test and heat load test were the same as above. Furthermore, it was compared with isotropic high-density graphite (IG-110U manufactured by Toyo Tanso Co., Ltd.).

Table 1 shows the test results.

(Α in Table 1)

(2) in Table 1

(3) in the table

From Table 1, it can be said that a C / C composite material with a bulk density of 1.4 to 2.0 [g / ci] impregnated with PyC is very effective in achieving the intended purpose.

Example 2

PyC-soaked carbon fiber felt composite prepared in the same manner as in Example 1 (bulk density 1.79 g / crf, bending strength 660 g / crf, compression strength 1450 kg {α} The inner diameter of the narrow part was 15 讓, the total length was 50 m, and the outermost stainless steel cylinder was shrink-fitted.

Fig. 4 shows a cross-sectional view of this nozzle. The injection gas at the time of the test was about 280 * C at the throat section, the pressure was about 36 atm, and the injection speed was about 1200 seconds. After the injection for 30 seconds, the wear amount of the nozzle was measured.

For comparison, a carbon-carbon composite material (CFRC) obtained by immersing the same carbon fiber in fluorinated resin, firing, carbonizing, and graphitizing twice in a conventional manner, and Isotropic lead material (bulk specific gravity: 1.77 g / cd. Compressive strength: 800 kg / di, thermal conductivity: lOOkcal / m · hr · * C) [Toyo Tanso IG — 110 U] is cut into the same shape. Using. The results are shown below. Average lubrication rate (m / _m / sec) Nozzle of the present invention 0.14

C F R C Nozzle 0.2 8

Graphite material alone Nozzle test medium rupture From the results in Table 2, when the carbon composite material according to the present invention was used, the throat portion had a small amount of wear despite severe thermal and mechanical shock, and was worn. It turns out that the degree of the degree was small.

Claims

The scope of the claims

(1) A carbon fiber reinforced carbon composite material in which pyrolytic carbonized graphite is impregnated inside a high-purity carbonaceous fiber.

(2) The composite material according to claim 1, wherein the total ash content is 1 O ppm or less.

(3) The composite material according to any one of (1) to (2), wherein the bulk density of the carbonaceous felt base material before soaking is 0.03 to 0.3 [g crf].

(4) The composite material has a bulk density of 1.4 g / ci) or more.

The composite material according to any one of 1 to 3.

(5) The composite according to any one of claims 1 to 4, wherein the composite has a bulk density of 1.4 to 2.0 (/ d).

(6) The method for producing a composite material according to any one of claims 1 to 5, wherein the pyrolytic carbon is soaked into the deep layer of the carbonaceous fiber.

(7) A method characterized in that pyrolysis carbon is deposited on the carbonaceous felt and immersed under a condition in which the temperature is kept at less than 1300 and the total pressure is less than 10 O Torr. Item 1. The method for producing a composite material according to Item 1.

(8) The composite material according to claim 6, wherein the air-permeable carbonaceous melt is continuously subjected to high-purification treatment, pyrolysis carbon immersion treatment, and graphitization treatment in the same apparatus. Production method.

(9) Each of the above treatments is performed using high-frequency heating means under reduced pressure or high vacuum. 9. The method for producing a composite material according to claim 8, wherein the method is performed.

Q0) The production method according to claim 8 or 9, wherein at least one of the purification and graphitization is performed under a pressure of 100 Torr or less.

5 01) In the purifying step under reduced pressure or high vacuum conditions, the lipogenation reaction and the elimination reaction of the lipogenation product are simultaneously carried out, according to claims 9 to 10, The manufacturing method described.

02) The first wall structural material of the fusion plasma containment device 10 comprising the composite material of claim 1.

(13) A protective material for a battling device comprising the composite material according to claim 1.

A beam-resistant protective material, such as an electron beam, a neutron beam, and an ion beam, comprising the composite material according to claim 1.

iis A beam-resistant jig made of the composite material according to claim 1, such as an electron beam, a neutron beam, or an ion beam.

(16) A beam-resistant armor material, such as an electron beam, a neutron beam, or an ion beam, comprising the composite material according to claim 1.

07) A beam-resistant electrode made of the composite material according to claim 1, such as an electron beam, a new 20-tron beam, or an ion beam.

08) Using a small amount of thermosetting resin to prepare carbonaceous 9. The method for producing a shaped composite material according to claim 6, wherein the shaped composite material is molded.

09) A heat-resistant member for a gas injection portion of a rocket nozzle comprising the composite material according to claim 1.