JPH0471879B2 - - Google Patents

Description

[Detailed description of the invention]

(Industrial Application Field) The present invention relates to a method and apparatus for producing SiC whiskers, and in particular to high-performance materials used in composite materials such as fiber-reinforced plastics (FRP), fiber-reinforced metals (FRM), and fiber-reinforced ceramics (FRC). This paper proposes a method and equipment for continuously and efficiently producing high-quality SiC whiskers on an industrial scale using a gas phase method. (Prior art) Currently known methods for producing SiC whiskers include a solid phase method using solid raw materials of carbon and silicon, a gaseous method of carbon and silicon, or a gaseous reaction of carbon and silicon with a solid, or a gaseous mixture thereof. There is a law. The solid phase method is a method of leading to the following reaction from solid SiO ₂ and C: SiO ₂ +CSiO+CO SiO+3COSiC+2CO ₂ C0 ₂ +C2CO, and is a technology in which so-called gaseous SiO and CO are reacted to precipitate and grow SiC whiskers. be. For example, the technology disclosed in Japanese Patent Publication No. 59-9516, which belongs to the solid-phase method, uses rice husk ash as the Si source and carbon black as the C source, and the This method involves heating to 1700℃. Furthermore, the technology disclosed in JP-A-61-227993 proposes a method of heating at a temperature of 1400 to 1700°C in a non-oxidizing atmosphere using silicic anhydride as a Si source and activated carbon as a C source. are doing. As a manufacturing apparatus used to carry out the above-mentioned solid phase method, for example, Japanese Utility Model Publication No. 59-38447 discloses a reaction vessel for producing SiC whiskers made of graphite material, and Publication No. 227999 discloses a furnace body having a passage with a temperature gradient along the longitudinal direction, a raw material filling area provided along the passage, and a plurality of sample storage units having a whisker generation area and an exhaust pipe. We are proposing an SiC whisker manufacturing device consisting of a container and a container. On the other hand, gas phase methods include a method in which a gaseous silicon halide such as silicon tetrachloride is reacted with a gaseous carbon compound such as carbon tetrachloride as a Si source at high temperature in a hydrogen stream, methyltrichlorosilane, etc. A method using thermal decomposition of organic silane is known. For example, the technology disclosed in Japanese Patent Publication No. 59-45635 introduces a silicon halide gas and a carbon halide gas into a heated reaction tube via a carrier gas (H ₂ ), and Alternatively, β-
This is a method for growing SiC whiskers, and in Japanese Patent Publication No. 59-45636, a porcelain tube or a graphite tube filled with carbon powder is inserted into a jacket tube.
We are proposing a method for producing SiC whiskers by generating a mixed gas of silicon tetrachloride and hydrogen while heating to 1300℃. (Problems to be Solved by the Invention) The above two conventional techniques shown as solid-phase methods have the following problems: (1) In addition to producing a large amount of granular SiC as a by-product, unreacted particulates of the raw material remain; These generated
Since it is mixed in SiC whiskers, high-purity whiskers suitable as reinforcing materials for metals and ceramics cannot be obtained. Therefore, additional complicated steps are required to separate and purify these particulates, and the yield of whiskers is also low. (2) Due to the slow reaction rate, it is difficult to continuously produce large amounts of high aspect ratio whiskers. (3) Reaction temperature is high. There were other problems. In addition, regarding the equipment used for such solid phase method,
All of them are batch-type production devices, which not only cannot perform continuous production, but also require a large number of reaction vessels in order to perform large-volume and efficient production, resulting in a large-scale device. Next, the above two conventional techniques described as gas phase methods both have a problem in that the silicon halide used as the raw material is expensive. Furthermore, these conventional methods do not include any specific disclosure or suggestion regarding continuous production means on an industrial scale. An object of the present invention is to develop a technique that can overcome the problems of the above-mentioned conventional techniques of the solid phase method and the gas phase method. (Means for Solving the Problems) As a method for efficiently producing high-purity SiC whiskers suitable as reinforcing materials on an industrial scale, the present invention provides SiC whiskers by vapor phase synthesis of silicon sulfide and a carbon compound. To produce whiskers, a gas containing hydrogen sulfide is introduced into a silicon sulfide gas generation chamber maintained at a temperature of 1000 to 1400℃, and is brought into contact with and reacts with the metal silicon layer loaded in the generation chamber. By this, silicon sulfide gas is generated, and then the generated silicon sulfide gas is heated to 1000℃.
While maintaining the temperature above, the SiC whiskers are transferred to a SiC whisker synthesis chamber maintained at 1130 to 1500℃, and brought into contact with carbon compounds in the synthesis chamber to precipitate and grow SiC whiskers. We propose a method for producing SiC whiskers, which is characterized by discharge from below. An apparatus suitably used in carrying out such a manufacturing method is one whose interior is divided into a silicon sulfide gas generation chamber and a SiC whisker synthesis chamber, and a gas transfer passage is provided to communicate between the two chambers. Both of these compartments are comprised of cylindrical reaction vessels each equipped with a heating device that can individually control the temperature, and the silicon sulfide gas generation chamber is equipped with a dispersion plate. A gas inlet for introducing hydrogen sulfide-containing gas is provided below, and a metal silicon charging port is provided above the dispersion plate.
We proposed an SiC whisker manufacturing device in which the whisker synthesis chamber is equipped with at least a carbon compound supply port, a whisker discharge port, and a gas discharge port in order to solve the above-mentioned technical problems. FIG. 1 shows a typical example of the essential parts of the apparatus of the present invention, in which a silicon sulfide gas generation chamber 1 is partitioned and formed in the upper part of the reaction vessel, and the lower part separated by a partition wall 14 is shown in FIG. The SiC whisker synthesis chamber 2 is divided into sections, and a cylindrical gas transfer passage 3 is provided at the center of the partition wall 14 to project upward and communicate the two defined chambers 1 and 2. Inside the silicon sulfide gas generation chamber 1, there is a porous gas distribution plate 4 for holding charged metal silicon particles (raw material) 13, and in the space below this gas distribution plate 4, A gas introduction port 5 for introducing hydrogen sulfide-containing gas, which is a reaction gas, is opened through a gas introduction pipe 5a inserted from above the container, and a raw material charging port 8 is provided in the space above the gas distribution plate 4. is opened through a raw material supply pipe 8a disposed from above the container. A carbon compound supply port 9 is opened in the SiC whisker synthesis chamber 2 through a carbon supply pipe 9a disposed from above the container. At the bottom of this synthesis chamber, there are provided a whisker outlet 11 for taking out the synthesized SiC whiskers and a gas outlet 12 for discharging hydrogen sulfide gas and unreacted gas generated during the synthesis of SiC whiskers. be. Further, the silicon sulfide generation chamber 1 and the SiC whisker synthesis chamber 2 are provided with heating devices 7a and 7b whose temperature can be controlled individually. Figures 2 to 5 show the silicon sulfide generation chamber 1 and
This figure shows another specific example of the apparatus of the present invention, showing a modification of the arrangement with the SiC whisker synthesis chamber 2, the arrangement of the gas transfer passage 3, and the arrangement of the gas introduction pipe 5a. First, the apparatus shown in FIG.
A SiC whisker synthesis chamber 2 is partitioned at the lower part of the partition wall 14, and a cylindrical gas transfer passage 3 is provided in the center of the partition wall 14 to project upward and connect the two partitioned chambers 1 and 2. This is the same as the example shown in the first diagram. The configuration that differs from the example in FIG. 1 is in the arrangement of the hydrogen sulfide-containing gas inlet 5 having an opening under the gas distribution plate 4. In this example, the gas introduction port 5 is used to introduce hydrogen sulfide-containing gas as a reaction gas. The opening 5 is a gas introduction pipe 5a inserted into the room from the side of the container.
The structure is arranged through. Also, the above
The carbon compound supply port 9 having an opening in the SiC whisker synthesis chamber 2 is opened through a carbon supply pipe 9a disposed on the side of the container. Furthermore, in this example, a generated nucleating material supply port 10 is provided for supplying the generated nucleating material used as needed in the present invention, and this supply port 10 is provided from the side of the container for supplying the nucleating material. It is formed through a pipe 10a. The other configurations are the same as those shown in the first figure. The apparatus shown in FIG. 3 has a silicon sulfide gas generation chamber 1 partitioned in the upper part of a reaction vessel, and a SiC whisker synthesis chamber 2 partitioned in the lower part separated by a partition wall 14. A cylindrical transfer passage 3 which communicates the two defined chambers 1 and 2 is provided in a manner to protrude upward. The difference with the device shown in the first figure is that the transfer channel 3 is located at the periphery rather than at the center. Accordingly, a carbon compound supply port 9 having an opening in the SiC whisker synthesis chamber 2 is a pipe 9a inserted from above the container so as to penetrate the silicon sulfide gas generation chamber 1.
It is established through. There are no differences in other configurations. The apparatus shown in FIG. 4 has a silicon sulfide gas generation chamber 1 partitioned in the upper part of a reaction vessel, and a SiC whisker synthesis chamber 2 partitioned in the lower part separated by a partition wall 14. It is the same as the one shown in the first figure in that a cylindrical transfer passage 3 is provided in an upwardly projecting manner for communicating the two defined chambers 1 and 2. The difference between the two configurations lies in the arrangement of the gas introduction port 5 and the carbon compound supply port 9. That is, the gas inlet 5
is opened below the gas distribution plate 4 through a gas introduction pipe 5a inserted from below the container so as to penetrate the SiC whisker synthesis chamber 2, and the carbon compound supply port 9 is connected to the SiC whisker synthesis chamber 2 from below the container. This is because the inserted carbon compound supply pipe 9a is opened to the upper part of the room. The other configurations are exactly the same as those shown in the first figure. The apparatus shown in FIG. 5 has a silicon sulfide gas generation chamber 1 sectioned at the bottom of a reaction vessel, and an SiC whisker synthesis chamber 2 sectioned at the upper part separated by a partition wall 14, and the area around the partition wall 14 is partitioned. A cylindrical transfer passageway 3 that connects the two defined chambers 1 and 2 is provided in an upwardly projecting manner. In the silicon sulfide gas generation chamber 1 located at the bottom, metal silicon particles (raw material) are charged.
A gas distribution plate 4 is attached to hold the gas 13, and a gas introduction port 5 for introducing hydrogen sulfide-containing gas is opened under the gas distribution plate 4 through a gas introduction pipe 5a inserted from below the container. On the other hand, on the gas distribution plate 4, a raw material charging port 8 is connected to a raw material supply pipe 8 similarly arranged from the side of the container.
It is opened through a. Furthermore, a carbon compound supply port 9 is opened in the SiC whisker synthesis chamber 2 located at the top through a carbon supply pipe 9a disposed from above the container. In addition, on the side of the SiC whisker synthesis chamber 2 located at the top, there is an outlet 11 for taking out the synthesized SiC whiskers.
Further, a gas outlet 12 is provided at the bottom of the synthesis chamber 2 for discharging hydrogen sulfide gas and unreacted gas generated during the synthesis of SiC whiskers. Furthermore, the silicon sulfide gas generation chamber 1 and
The SiC whisker synthesis chamber 2 is provided with heating devices 7a and 7b whose temperature can be controlled individually. (Operation) The basic principle of the idea of the present invention is to bring silicon sulfide into contact with a mixed gas of hydrogen sulfide and hydrogen to create silicon sulfide gas, and to react with propylene gas (C ₃ H ₆ ) to form SiC. This idea is based on the research of Egashira et al., who confirmed it in the laboratory as a whisker vapor phase synthesis method. , Shohachi Kawazumi, “Ceramic Industry Association Journal” 93.535
~540 (1985)] is known. According to this study, the above method is thought to be based on the following reaction. Overall reaction formula: Si+1/3C ₃ H ₆ →SiC+H ₂ (1) When SiS is used as an intermediate; Si+H ₂ S→SiS+H ₂ SiS+1/3C ₃ H ₆ →SiC+H ₂ S (2) When SiS ₂ is used as an intermediate Case: Si+2H ₂ S→SiS ₂ +2H ₂ SiS+1/3C ₃ H ₆ +H ₂ →SiC+2H ₂ S This known method based on desk experiments yields whiskers with a larger aspect ratio than the conventional technique described above, and the starting materials are inexpensive. It has excellent characteristics such as fast whisker growth, high purity whiskers, and no particulate matter. However, according to the explanation in the above-mentioned "References," this method is a batch method research using a small tube furnace, and the technology is not developed for specific measures to enable continuous and mass production, which are essential for industrialization. It was considered unsuitable for continuous and mass production due to the lack of disclosure and various constraints. As a result of extensive research based on the basic principle shown in the above reference, the present inventors separated a series of manufacturing processes into a silicon sulfide gas generation process and a SiC whisker precipitation and growth process. By adopting a method in which reaction zones corresponding to each process are defined and provided, and the defined chambers are communicated with each other through gas transfer passages to facilitate handling of intermediate reaction products, the above-mentioned problem of the conventional technology can be solved. They overcame the various problems encountered and completed the technology to continuously and efficiently produce high-quality whiskers on an industrial scale. The present invention will be explained in detail below with reference to the drawings. The method of the present invention consists of a first step of generating silicon sulfide gas and a second step of precipitating SiC whiskers from the gas. The first step is a step in which metal silicon 13, which is one of the raw materials loaded into the silicon sulfide gas generation chamber 1, is brought into contact with hydrogen sulfide-containing gas to generate silicon sulfide gas. The metal silicon 13
A raw material charging port 8 is provided in the silicon sulfide gas generation chamber 1.
It is charged continuously or intermittently through the process. Silicon sulfide gas generation chamber 1 occupying a part of the reaction vessel
The device is provided with a transfer passage 3 serving as a generated gas outlet and a hydrogen sulfide-containing gas inlet 5 above and below an internal gas distribution plate 4, and deposits and holds the metal silicon 13 on this gas distribution plate 4. Note that metal silicon 13 is charged into this silicon sulfide gas generation chamber 1 through a raw material charging port 8 . The metal silicon 13 to be charged preferably has a particle size of 2 mm or less. If the size is too large, the reaction efficiency will be poor. Further, if the particle size is less than 0.04 mm, there is a possibility that it will be scattered along with the gas from the transfer passage 3 for discharging the generated gas. Therefore, the particle size of metal silicon 13 is
It is desirable to use one with a size of 0.04 to 2 mm. Regarding the material of the silicon sulfide gas generation chamber 1, since the inside of the container reaches a high temperature of 1000°C or more,
It is desirable to use heat-resistant materials such as alumina, mullite, silicon carbide, and carbon. After charging the metal silicon 13 as a raw material, hydrogen sulfide-containing gas is introduced from the hydrogen sulfide-containing gas inlet 5 opened into the silicon sulfide gas generation chamber 1, and the metal silicon 13 is deposited. While passing through the layer, silicon sulfide gas is generated by causing a contact reaction, and the next SiC whisker is passed through the gas transfer passage 3 which serves as a generated gas discharge port provided in the silicon sulfide gas generation chamber 1. Transfer to synthesis room 2 while keeping it warm (>1000℃). Note that the first stage silicon sulfide gas generation chamber 1
In order to generate silicon sulfide gas, it is necessary to maintain the inside of the gas generation chamber 1 at a temperature of 1000°C or higher,
More preferably, the boiling point of silicon disulfide is 1130
It is desirable to keep the temperature above ℃. However, since the melting point of metallic silicon is 1414°C, metallic silicon will melt at a temperature higher than this, so the temperature inside the container will decrease.
It is desirable to maintain the temperature within the range of 1000-1400°C. Therefore, a heating device 7a such as an electric furnace is installed in the silicon sulfide gas generation chamber 1 and the transfer passage 3 for transferring the silicon sulfide gas so that the internal temperature thereof is maintained in the range of 1000 to 1400°C. It is necessary to provide The hydrogen sulfide-containing gas may be hydrogen sulfide alone, an inert gas such as argon or helium, a reducing gas such as hydrogen, or a mixture thereof. When hydrogen sulfide-containing gas is blown into the silicon sulfide gas generation chamber 1, it is desirable to operate the metal silicon 13 loaded therein so that it gradually changes from an initial fixed bed to a fluidized bed. This is because a fluidized bed is preferable in terms of reaction efficiency. however,
It is undesirable that the metal silicon 13 particles are scattered from the gas transfer passage 3 together with the blown gas into the next SiC whisker synthesis chamber 2 without reacting. In this sense, in order to efficiently generate silicon sulfide gas, it is desirable to further adjust the gas velocity below the porous gas distribution plate 4 on which metal silicon is deposited. The degree of this adjustment varies depending on the particle size of the metal silicon 13, but it is preferably 10 times or less the speed at which the metal silicon layer starts to fluidize. If this value is exceeded, there is a high possibility that the metal silicon 13 particles will be scattered from the generated gas outlet 6. Next, in the second step of the present invention, the silicon sulfide gas produced in the first step is transferred to a defined chamber formed by dividing the inside of the same reaction vessel, that is, the internal temperature is reduced through heating equipment. kept at 1130~1500℃
A carbon compound is introduced into the SiC whisker synthesis chamber 2, and a carbon compound is introduced into the synthesis chamber 2 through a carbon compound supply pipe 9a.
This is a step in which whiskers are precipitated and grown by supplying SiC through the SiC whisker synthesis chamber 2 and bringing them into contact within the SiC whisker synthesis chamber 2. At this time, the generated nucleating material may be supplied through the generated nucleating material supply port 10 if necessary. Examples of the carbon compounds include paraffin hydrocarbons such as methane, ethane, propane, butane, and pentane; olefin hydrocarbons such as ethylene, propylene, butylene, and amylene; acetylene hydrocarbons such as acetylene, arylene, and butyne;
Aromatic hydrocarbons such as benzene, naphthalene and anthracene, alicyclic hydrocarbons such as cycloparaffin and cycloolefin, or mixtures thereof can be used. In addition, these carbon compounds may be supplied in any of the gas, liquid, or solid states, but those that are liquid or solid at room temperature are made into fine particles and slurried using water or an organic solvent. From the viewpoint of handling, it is preferable to use a solid state, a state dispersed in the carrier gas, a solution dissolved in an organic solvent or the like, or a state modified into a gas state by heating. Note that the carbon compound used in the present invention is
As mentioned above, it is possible to select from a wide range of types and forms, but in terms of reaction efficiency, whisker yield, ease of handling, etc., methane, ethane, propane, ethylene, propylene,
It is desirable to use acetylene, arylene, etc. On the other hand, the nucleating materials supplied as needed include metals such as iron, nickel, titanium, manganese, cobalt, copper, vanadium, chromium, aluminum, and silicon, as well as oxides, carbides, nitrides, and sulfides of these metals. Inorganic substances such as halides, sulfates, sulfates, or metal alcoholates such as ethyl silicate and ethyl titanate, general formula M (C ₅ H ₅ ) ₂ [M: Fe, Ni, Ti, Mn, Co, Cu ，
Organometallic compounds such as metallocenes represented by V, Cr] or mixtures thereof can be used. The conditions at the time of supply of these generation nucleating materials are as follows:
It can be in any state such as gas, liquid, or solid, but
Those that are liquid or solid at room temperature can be made into fine particles and made into a slurry with water or an organic solvent, or dispersed in the carrier gas mentioned above, or dissolved in water or an organic solvent or heated. It is desirable for handling to make it into a gaseous state. As explained above, the production nuclei used in the present invention can be selected from a wide range of types and forms, but the reaction efficiency, whisker yield, ease of handling, and even after whisker production are Organic metal compounds containing iron, nickel, manganese, etc. are desirable from the viewpoint of ease of removing generated nuclei. Now, at the stage of using this SiC whisker synthesis chamber 2, in order to generate SiC whiskers by the reaction between silicon sulfide gas and carbon compounds,
It is necessary to cause both to react in a gas phase. For this reason, the temperature inside the SiC whisker synthesis chamber 2 needs to be at least 1130° C., which is the boiling point of silicon sulfide. On the other hand, if the temperature is too high, the SiC whisker production reaction becomes difficult to occur, so the upper limit is set at 1500°C. The temperature inside the so-called SiC whisker synthesis chamber 2 is set in the range of 1130 to 1500°C. This SiC whisker synthesis chamber 2 is provided with a heating device 7b such as an electric furnace to heat and maintain the interior within the above temperature range. In addition, the material of the SiC whisker synthesis chamber 2 itself is alumina, mullite, silicon carbide,
A heat-resistant material such as carbon is preferred. In the first step, the content of hydrogen sulfide in the hydrogen sulfide-containing gas blown into the silicon sulfide gas generation chamber 1 is adjusted using an inert gas, a reducing gas, or a mixed gas thereof. Also,
Through this adjustment, the concentration of the generated silicon sulfide gas can be adjusted, and furthermore, the gas flow rate within the SiC whisker synthesis chamber 2 can also be controlled. The carbon compound supplied into the SiC whisker synthesis chamber 2 acts to synthesize SiC by reacting with silicon sulfide gas, and deposits SiC whiskers using the side wall of the synthesis chamber 2 as a medium (substrate). Let it grow gradually. Further, the generation nucleating material supplied as needed at this stage is suspended in the form of fine particles in the SiC whisker synthesis chamber 2, and acts as a nucleus or substrate for the precipitation and growth of SiC whiskers.
Therefore, the generated SiC whiskers are generated using the generated nuclei as seeds, and gradually grow while being fluidized along the flow of the silicon sulfide gas and the reaction is completed. (Example) An example using the apparatus shown in FIG. 1 will be described below. Metallic silicon 13 with an average particle size of 0.5 mm is placed on the gas distribution plate 4 in the silicon sulfide gas generation chamber 1 whose interior is maintained at 1200°C, and a predetermined amount of hydrogen sulfide-containing gas is blown into the chamber from the gas inlet 5. is. As the hydrogen sulfide-containing gas, a mixture of hydrogen sulfide gas and hydrogen gas was used. The generated silicon sulfide gas is transferred to the SiC whisker synthesis chamber 2 whose interior is maintained at 1300°C through the gas transfer passage 3 while being kept warm, and at the same time, propylene gas as a carbon compound and the necessary A predetermined amount of ferrocene gas was introduced as a nucleating material depending on the conditions. Note that these various gases were continuously supplied in predetermined amounts. The precipitated and grown SiC whiskers are discharged from the whisker outlet 11 provided at the bottom of the whisker synthesis chamber 2.
The gas was discharged and collected using a rotary valve 15 while being sealed. obtained in this way
SiC whiskers were analyzed using X-rays, and the length and
The diameter etc. were measured using a microscope. In addition, the yield of SiC whiskers was calculated from the weight of whiskers obtained per unit time and the weight of propylene gas charged. These results are summarized in Table 1.
In addition, in Examples 1 to 4 shown in the same table, the amount of hydrogen sulfide-containing gas used, the content of hydrogen sulfide, propylene,
Each amount of ferrocene used and silicon sulfide gas generation chamber 1
This is an example in which the SiC whisker was manufactured by changing the temperature inside the whisker synthesis chamber 2.

[Table] (Effects of the Invention) As can be seen from the above explanation and the results of the examples, when SiC whiskers are manufactured according to the method described above using the apparatus according to the present invention, high quality
SiC whiskers can be manufactured continuously and efficiently. In particular, according to the present invention, it is possible to control the concentration and generation amount of silicon sulfide gas by changing the amount of hydrogen sulfide-containing gas charged into the silicon sulfide gas generation chamber and the content rate of hydrogen sulfide. Further, by changing the amount of raw materials, the amount of the hydrogen sulfide-containing gas, and the temperature inside each compartment, it is possible to continuously produce on an industrial scale while controlling the amount, length, diameter, etc. of whiskers. In addition, in the present invention, a generated nucleating material can be used as needed, and when this is used, the whiskers that are generated grow using the generated nucleating material fine particles that exist in a suspended state in the whisker synthesis chamber as nuclei. Therefore, the generation conditions are uniform, and compared to SiC whiskers that grow using the surface of a fixed substrate as a nucleus, SiC whiskers are more uniform in length and diameter.
Whiskers are obtained continuously. Furthermore, the Si source material of the present invention is metallic silicon, which is cheaper than the silicon halide gas used in the conventional technology. ，
Suitable for use as composite reinforcing material such as FRC.

[Brief explanation of drawings]

Figures 1 to 5 all relate to the present invention.
FIG. 1 is a cross-sectional view showing a preferred example of a SiC whisker production apparatus, in which FIG. 1 shows an example in which a gas inlet and a raw material supply port are arranged from above, and FIG. Fig. 3 shows an example in which the gas inlet and carbon compound supply port are arranged on the side, and Fig. 4 shows an example in which the gas transfer passage is arranged in the periphery. FIG. 5 shows an example of an arrangement in which the SiC whisker synthesis chamber is in the upper part and the silicon sulfide gas generation chamber is in the lower part. 1... Silicon sulfide gas generation chamber, 2... SiC whisker synthesis chamber, 3... Transfer passage, 4... Gas distribution plate, 5... Hydrogen sulfide-containing gas inlet, 5a... Gas introduction pipe, 7a , 7b... heating device, 8...
...Raw material (Si) charging port, 8a...Raw material supply pipe,
9... Carbon compound supply port, 9a... Carbon compound supply pipe, 10... Nucleus material supply port. 10a...
Nuclear material supply pipe, 11... Whisker outlet, 12... Gas outlet, 13... Metallic silicon, 14... Partition wall.

Claims (1)

[Claims] 1. In producing SiC whiskers by vapor phase synthesis of silicon sulfide and a carbon compound, a gas containing hydrogen sulfide is heated to a silicon sulfide gas maintained at a temperature of 1000 to 1400°C. Silicon sulfide gas is generated by introducing the silicon sulfide gas into the generation chamber, contacting and reacting with the metal silicon layer loaded in the generation chamber, and then heating the generated silicon sulfide gas to 1000℃.
While maintaining the temperature above, the SiC whiskers are transferred to a SiC whisker synthesis chamber maintained at 1130 to 1500℃, and brought into contact with carbon compounds in the synthesis chamber to precipitate and grow SiC whiskers. A method for producing SiC whiskers, which is characterized by discharging from below. 2 The interior is divided into a silicon sulfide gas generation chamber and a SiC whisker synthesis chamber, and a gas transfer passage is provided to communicate between the two chambers, and a heating device is attached to each of these chambers. A dispersion plate is disposed in the silicon sulfide gas generation chamber, and a gas inlet for introducing hydrogen sulfide-containing gas is disposed below the dispersion plate. A metal silicon charging port is provided on the distribution plate, while the SiC
1. A SiC whisker manufacturing apparatus, characterized in that a whisker synthesis chamber is provided with at least a carbon compound supply port, a whisker discharge port, and a gas discharge port.