KR20180083125A - The Carbon nano tube and Alumina mixed paper, the method of manufacturing it and the heat treatment tray - Google Patents
The Carbon nano tube and Alumina mixed paper, the method of manufacturing it and the heat treatment tray Download PDFInfo
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- KR20180083125A KR20180083125A KR1020170005190A KR20170005190A KR20180083125A KR 20180083125 A KR20180083125 A KR 20180083125A KR 1020170005190 A KR1020170005190 A KR 1020170005190A KR 20170005190 A KR20170005190 A KR 20170005190A KR 20180083125 A KR20180083125 A KR 20180083125A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
- D21H13/36—Inorganic fibres or flakes
- D21H13/46—Non-siliceous fibres, e.g. from metal oxides
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
- D21H13/36—Inorganic fibres or flakes
- D21H13/46—Non-siliceous fibres, e.g. from metal oxides
- D21H13/50—Carbon fibres
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Abstract
Description
The present invention relates to a composite paper comprising carbon fibers and alumina fibers, a method for producing the same, and a heat treatment tray.
Cemented carbides are used in various fields because of their high hardness and abrasion resistance. In order to obtain such mechanical properties, the sintered body should be sintered to a solid state free of free carbon or eta (η) phase and free from internal defects such as pores or impurities. The sintering process is performed at about 1,400 ° C. The carbon plate is used as a refractory for supporting the formed product during sintering. However, the carbon plate is adhered due to the reaction with the cemented carbide or the carbon is diffused into the carbide product.
Most and carbide tool areas in the cemented carbide and to prevent the reaction of the carbon plate characters release agent Al 2 O 3 powder and AlN powder is used, the method and put the adhesive on the carbon plate in the form of applying an Al 2 O 3 and AlN powder When the gas is generated in the adhesive, not only the formation of pores in the product is easy, but also the atmosphere in the furnace is affected, and it is also difficult to sinter to a normal state free from free carbon or eta (?) Phase. In this case, it is difficult to apply and remove Al 2 O 3 powder and AlN powder, and there is a possibility that the refractories are mixed into the product and interposed as impurities in the process, and a solution for producing high quality carbide cutting tools is needed.
On the other hand, in the case of the carbon fiber paper used as the releasing paper, the fixing reaction between the carbon plate and the cemented carbide does not occur, the gas is not generated in the sintering at high temperature and the reaction with the cemented carbide is not affected, It is possible to simplify the process. However, the manufacturing process of carbon fiber paper is complicated, and the phenol resin used in the manufacturing process is expensive due to environmental pollution and carbonization process, resulting in a high product cost. Due to a slight reaction with cemented carbide, some high value- Free Carbon) is generated, and it is difficult to apply to a product such as a plate where the product itself is broken well and is bent.
Thus, the inventors of alumina (Al 2 O 3) fibers and using a carbon nanotube, an existing six-stage process for the production of composite paper (wet nonwoven fabric manufacturing process, the impregnation step, the drying process, the compression process, the cutting process, the carbonized A method for manufacturing a sintered paper for sintering which can reduce the production cost by simplifying the production process and shortening the production time by a four step process (a wet nonwoven fabric manufacturing process, a drying process, a compression process, and a cutting process) in the process (FIG. 1) And completed the present invention.
The present invention has been made to solve the above-mentioned problems, and it is an object of the present invention to provide a carbon nanotube and alumina composite paper, a manufacturing method thereof, and a heat treatment tray.
In order to achieve the above object, the present invention provides a method for producing a carbon nanotube, comprising: dissociating and mixing a carbon nanotube and an alumina fiber to obtain a slurry; Adding a surfactant to the slurry; Adding polyvinyl alcohol and a dispersant to the slurry to which the surfactant is added; And a step of thermally pressing the slurry containing the polyvinyl alcohol and the dispersant in the form of a composite sheet, followed by thermocompression bonding, characterized in that it is a method of producing a fiber-composite paper comprising carbon nanotubes and alumina .
The dissociated carbon nanotubes and alumina fibers may be added in a weight ratio of 1: 7 to 90: 96.
The polyvinyl alcohol may be added in an amount of 3 to 5% by weight based on the total weight of the slurry.
The dispersant may be a polyamine.
The present invention is a fiber composite paper comprising carbon nanotubes and alumina produced by the method according to the present invention.
The present invention is characterized in that the carbon nanotube of the present invention is a heat treatment tray including a sintered fiber-composite paper comprising alumina and a cemented carbide.
The cemented carbide may be WC Ni-based or WC-Co-based.
The carbon nanotube and alumina fiber composite papers according to the present invention can suppress the adhesion reaction between the cemented carbide and do not require a separate binder because of the nature of the bundle of carbon nanotubes, And further control the carburization reaction by controlling the content ratio of carbon nanotubes. It is possible to manufacture various types of products due to the characteristics of flexible paper.
Figure 1 is a diagram illustrating process steps for making conventional composite paper.
2 is a view illustrating process steps for producing a composite paper according to the present invention.
Fig. 3 is a photograph of the surface of the composite paper of Examples 1 to 4 according to the present invention, taken by means of a field emission scanning electron microscope. Fig.
4 is a cross-sectional view of a cemented carbide after sintering of a WC Ni-based cemented carbide on a composite paper according to Examples 5 to 7 according to the present invention, using an observation microscope.
5 is a photograph of the surface of a cemented carbide after sintering the WC Ni-based cemented carbide on the composite paper of Examples 8 to 10 according to the present invention.
Fig. 6 is a cross-sectional view of a corroded cemented carbide after sintering of a WC Ni-based cemented carbide on a composite paper of Examples 8 to 10 according to the present invention, using an observation microscope.
7 is a photograph of the surface of a cemented carbide before and after sintering the WC Co-based cemented carbide on the composite paper of Examples 11 to 14 according to the present invention.
8 is a cross-sectional view of a cemented carbide after sintering of a WC Co-based cemented carbide on a composite paper of Examples 11 to 14 according to the present invention, using an observation microscope.
FIG. 9 is a photograph of the surface of the composite paper of Examples 11 to 14 according to the present invention before and after the heat treatment by a field emission scanning electron microscope. FIG.
Disclosure of the Invention The present invention relates to a method for producing carbon nanotubes by dissociating and mixing carbon nanotubes and alumina fibers to obtain a slurry; Adding a surfactant to the slurry; Adding polyvinyl alcohol and a dispersant to the slurry to which the surfactant is added; And a step of thermally pressing a slurry containing the polyvinyl alcohol and a dispersant in the form of a composite sheet, followed by thermocompression bonding. The present invention also provides a method for producing a fiber composite paper comprising carbon nanotubes and alumina.
The dissociated carbon nanotubes and alumina fibers may be added in a weight ratio of 1: 7 to 90: 96.
The surfactant may be added in an amount of 3 to 7 wt% based on the total weight of the alumina fiber, preferably 5 wt%.
The polyvinyl alcohol may be added in an amount of 3 to 5% by weight based on the total weight of the slurry. When the amount is less than 3 wt%, the dispersibility may be decreased. If the amount is more than 5 wt%, aggregation may occur.
The polyvinyl alcohol acts as a binder between the fibers to temporarily bind the fibers.
The dispersant may be a polyamine.
The dispersant may be added in an amount of 3 to 7 wt%, preferably 5 wt%, based on the total weight of the slurry.
The polyamine bonds in a molecular state between the fibers to improve the dispersion state.
In one embodiment of the present invention, the carbon nanotubes and the alumina fibers are each dissociated, and then the carbon nanotubes are added to the alumina fibers at 1 to 7 wt% relative to the alumina fibers. Carburization can be controlled by the content ratio of the carbon nanotubes. The composite slurry of carbon nanotubes and alumina fibers was agitated using a surfactant, polyvinyl alcohol was added in an amount of 3 to 5 wt% based on the composite slurry and stirred, and an aqueous solution of the dispersant was added to the composite slurry. Composite slurry was prepared in the form of a composite sheet, followed by drying and thermocompression to produce a uniform thickness, thereby preparing a carbon nanotube and alumina fiber composite paper.
The present invention is a fiber composite paper comprising carbon nanotubes and alumina produced by the method according to the present invention.
The present invention is characterized in that the carbon nanotube of the present invention is a heat treatment tray including a sintered fiber-composite paper comprising alumina and a cemented carbide.
The cemented carbide may be WC Ni-based or WC-Co-based.
The sintering may be performed by using WC Ni or WC Co cemented carbide for carbon nanotube and alumina fiber composite paper at a temperature of 1,150 to 1,400 ° C.
The method for producing a carbon fiber composite paper comprising carbon nanotubes and alumina according to the present invention comprises the steps of (1) a conventional 6-step process for producing a composite paper (a wet nonwoven fabric manufacturing process, an impregnation process, a drying process, a compression process, a cutting process, 1) can be manufactured by a simple four step process (a wet nonwoven fabric manufacturing process, a drying process, a pressing process, and a cutting process) (FIG. 2), and a time and cost can be minimized because a heat treatment process is not necessary.
Further, the carbon fiber composite paper comprising carbon nanotubes and alumina produced by the method according to the present invention has the following advantages.
① Reduction of production cost by simplifying the production process of sintered release paper and shortening the time
( 2 ) Alumina (Al 2 O 3 ) fibers with excellent thermal stability and carbon nanotubes can be used as sintering supports at high temperature (1,400 ° C) during sintering.
③ Carbon nanotubes tend to exist in the form of bundles due to strong Van der Waals interaction between the tube and the tube, so no binder is needed.
④ Because there are many pores, it is easy to remove wax and remove gas when sintering cemented carbide.
⑤ Thinner thickness minimizes deformation of cemented carbide due to releasing paper
⑥ Flexible and applicable to various products, especially heat treatment trays
Hereinafter, preferred embodiments of the present invention will be described in detail. It should be understood, however, that the invention can be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. It should be noted that the embodiments of the present invention described below are intended to sufficiently convey the spirit of the present invention to those skilled in the art.
< Example 1 ~ 4> Preparation of carbon nanotube and alumina fiber composite paper
Carbon nanotubes (CNT, JEIO Jeno Tube 8) were dissociated at a speed of 1,800 rpm using a pulper. The alumina fibers (MAFTEC ALS, MITSUBISHI, INC.) Were pulverized to a size of 1 to 3 mm and dissociated at a speed of 2,500 rpm using a pulper. The dissociated carbon nanotubes were added to 1 to 3 mm of alumina fibers in an amount of 1 to 7% by weight relative to the alumina fibers. Carbon nanotube content ratio can control carburization. The composite slurry of carbon nanotubes and alumina fibers was stirred in a stirrer at a speed of 1,500 rpm for 30 minutes. A surfactant (Hansol Chem., Co., Ltd) was added in an amount of 5% by weight based on the alumina fiber and stirred for 18 minutes. An aqueous solution of polyvinyl alcohol (PVA) was prepared and added to the composite slurry. When polyvinyl alcohol aqueous solution was added, 3 to 5% by weight of polyvinyl alcohol was added to the composite slurry, and the mixture was stirred. A dispersant (polyamine, HANWET HF-59, Hansol Chem., Co., Ltd.) was added to the composite slurry at 5 wt% and maintained for 10 minutes. The composite slurry was prepared in the form of a composite sheet using a wet nonwoven production equipment (Wet-laid) and then dried at 150 ° C for 2 minutes using a net dryer (2 m / min). In order to produce the sheet with a constant thickness, the carbon nanotube and the alumina fiber composite paper were prepared by thermocompression at a temperature of 0.5-1 bar to 150-160 ° C.
Fig. 3 is a microscope-magnified image of carbon nanotube and alumina fiber composite papers of Examples 1 to 4, in which alumina fibers, carbon nanotubes, and PVA were prepared according to the addition amounts in Table 1 below. It can be confirmed that the small carbon nanotubes are bonded between the alumina fibers to serve as a binder, thereby maintaining the shape at the time of high-temperature sintering. .
< Example 5 ~ 7> For carbon nanotube and alumina fiber composite paper WC Ni Cemented carbide sintering treatment (1,150 ℃)
Examples 5 to 7 (CNT paper-1-3) of carbon nanotube and alumina fiber composite paper were prepared by the method of Example 1 according to the addition amounts and conditions of the following Table 2, respectively. Carbon fiber paper (Himc) was prepared and covered with Examples 5 to 7 prepared on graphite as a sintered body and as a control group, respectively. Also, Al 2 O 3 powder was applied on graphite according to the conventional process as a control group. Graphite covered with Examples 5 to 7, graphite coated with Al 2 O 3 powder as a control group, and graphite covered with carbon fiber paper were sintered at a temperature of 1,150 ° C and WC Ni cemented carbide was sintered. Respectively.
As a result, there were no differences in the hardness and density of the carbon fiber paper (Himc Carbon paper) and Examples 5 to 7 (CNT paper-1 to 3) compared to Al 2 O 3 powder application (Al 2 O 3 pow) , The carbon level has risen. Particularly, in Examples 5 to 7, discoloration did not occur even after sintering, and strength was maintained and reusable.
Furthermore, the same carbon fibrosis is (Himc Carbon paper) and Example 5 ~ 7 (CNT paper-1 ~ 3) cross-section a case where a result (Fig. 4), Al 2 0 3 powder coating observed with the actual micrograph of the tissue Respectively.
< Example 8 ~ 10> For carbon nanotube and alumina fiber composite paper WC Ni Cemented carbide sintering treatment (1,390 ℃)
Examples 8 to 10 (CNT paper-4 to 6) of carbon nanotube and alumina fiber composite paper were prepared according to the method of Example 1, respectively, in accordance with the addition amounts and conditions of Table 2 below. Graphite covered with Examples 8 to 10, graphite coated with Al 2 O 3 powder as a control group, and graphite covered with carbon fiber paper (Himc) were sintered at a temperature of 1,390 ° C and WC Ni cemented carbide was sintered Are shown in Table 4. < tb >< TABLE >
As a result, the hardness and density of the Al 2 0 3 powder coating (Al 2 0 3 pow), the carbon fibrosis (Himc Carbon paper) and Example 8 ~ 10 (CNT paper-4 ~ 6) were the same. Carbon number and saturation magnetization (MS) of Carbon fibrous species and Examples 8 to 10 were increased, and in Examples 8 to 10, the increase was smaller than that of carbon fiber paper.
Al 2 0 3 powder coating (Al 2 0 3 pow), a result of observing this carbon fibrosis (Himc Carbon paper) and Examples 8-10 (CNT paper-4 ~ 6) (Fig. 5) Example 8-10 Was not different from that of Al 2 O 3 powder and showed no discoloration of sintered body. In the case of the carbon fiber paper, after the sintering, there was a hole in the area where the sintered body and the paper came into contact with each other. In Examples 8 to 10, no holes were formed after the sintering but the marks remained. In particular, Example 8 (CNT paper- It was confirmed that the strength was maintained even after that.
In addition, Al 2 0 3 powder coating (Al 2 0 3 pow), the carbon fibrosis (Himc Carbon paper) and Example 8 ~ 10 (CNT paper-4 ~ 6) surface unevenness by using a cemented carbide surface pretreatment step portion kkami of The solution was exposed to the carbide specimens for about 30 seconds and the surface was corroded and observed (Fig. 6), confirming that the tissues were the same in all the papers.
< Example 11 ~ 14> For carbon nanotube and alumina fiber composite paper WC Co (0.3 μm, 9.5%) Cemented carbide sintering treatment (1,400 ℃)
Examples 11 to 14 (CNT paper-7 to 10) of carbon nanotube and alumina fiber composite paper were respectively prepared by the method of Example 1 according to the addition amounts and conditions of Table 5 below. Graphite coated with Al 2 O 3 powder and carbon fiber paper (Himc) coated with the graphite covered with the produced Examples 11 to 14 (CNT paper-7 to 10), the graphite coated with Al 2 O 3 powder and the carbon fiber paper (0.3 μm, 9.5%) cemented carbide, and their properties are shown in Table 6.
As a result, the hardness and density of the Al 2 0 3 powder coating (Al 2 0 3 pow), the carbon fibrosis (Himc Carbon paper) and Examples 11 ~ 14 (CNT paper-7 ~ 10) was identical. In Examples 11 to 14, saturation magnetization (MS) values were slightly decreased as compared with Al 2 O 3 powder application, and as a result, the saturation magnetization (MS) values were decreased as compared with the former Respectively.
Al 2 0 3 powder coating (Al 2 0 3 pow), the carbon fibrosis (Himc Carbon paper) and Examples 11 to 14 As a result of observing the (CNT paper-7 ~ 10) ( Fig. 7), Al 2 0 3 powder There was no difference in application and texture, and discoloration of the sintered body did not occur. In Examples 11 to 14, no holes were formed after sintering, but marks were left on the portion where the paper came in contact, and the strength was maintained. Thus, it was confirmed that the application of the releasing agent was not necessary in the sintering process using Examples 11 to 14.
Al 2 O 3 powder (Al 2 O 3 pow), Himc Carbon paper and Examples 11 to 14 (CNT paper-7 to 10) were observed (FIG. 8) The same thing was confirmed.
In addition, when Examples 11 to 14 (CNT paper-7 to 10) were compared with each other before and after the heat treatment at a high temperature of 1,400 ° C (FIG. 9), the shape of the paper was maintained so that the carbon nanotubes It was judged to be suitable as material.
Claims (7)
Adding a surfactant to the slurry;
Adding polyvinyl alcohol and a dispersant to the slurry to which the surfactant is added; And
And a step of thermally pressing the slurry containing the polyvinyl alcohol and the dispersant in the form of a composite sheet, followed by thermocompression bonding.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110534746A (en) * | 2019-09-19 | 2019-12-03 | 华南农业大学 | A kind of tungsten carbide/carbon nano tube compound material and the preparation method and application thereof |
CN111673086A (en) * | 2020-05-27 | 2020-09-18 | 华南理工大学 | Porous fiber liquid absorption core with surface in-situ grown carbon nano tube and preparation method |
CN114940504A (en) * | 2022-06-06 | 2022-08-26 | 哈尔滨工业大学(威海) | Alumina micro-tube and preparation method thereof |
KR20230099895A (en) * | 2021-12-28 | 2023-07-05 | 주식회사 핫앤쿨 | Manufacture of Carbon Nanotubes and Carbon Fiber Composites |
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KR100628031B1 (en) | 2005-07-27 | 2006-09-26 | (주) 나노텍 | Thermally improve conductive carbon sheet base on mixed carbon material of expanded graphite powder and carbon nano tube powder |
KR100992154B1 (en) | 2008-09-19 | 2010-11-05 | 한국전자통신연구원 | Transparent Conductive Thin Film Using Carbon Nano Tube and Method for Preparation thereof |
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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KR100628031B1 (en) | 2005-07-27 | 2006-09-26 | (주) 나노텍 | Thermally improve conductive carbon sheet base on mixed carbon material of expanded graphite powder and carbon nano tube powder |
KR100992154B1 (en) | 2008-09-19 | 2010-11-05 | 한국전자통신연구원 | Transparent Conductive Thin Film Using Carbon Nano Tube and Method for Preparation thereof |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110534746A (en) * | 2019-09-19 | 2019-12-03 | 华南农业大学 | A kind of tungsten carbide/carbon nano tube compound material and the preparation method and application thereof |
CN111673086A (en) * | 2020-05-27 | 2020-09-18 | 华南理工大学 | Porous fiber liquid absorption core with surface in-situ grown carbon nano tube and preparation method |
KR20230099895A (en) * | 2021-12-28 | 2023-07-05 | 주식회사 핫앤쿨 | Manufacture of Carbon Nanotubes and Carbon Fiber Composites |
CN114940504A (en) * | 2022-06-06 | 2022-08-26 | 哈尔滨工业大学(威海) | Alumina micro-tube and preparation method thereof |
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