CN112723898A - Preparation method of carbon/carbon liner for natural gas chemical vapor deposition furnace - Google Patents

Preparation method of carbon/carbon liner for natural gas chemical vapor deposition furnace Download PDF

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CN112723898A
CN112723898A CN202011630446.4A CN202011630446A CN112723898A CN 112723898 A CN112723898 A CN 112723898A CN 202011630446 A CN202011630446 A CN 202011630446A CN 112723898 A CN112723898 A CN 112723898A
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carbon
chemical vapor
vapor deposition
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resin
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高大恩
邵海成
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Inner Mongolia Pate New Material Technology Co ltd
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Inner Mongolia Pate New Material Technology Co ltd
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Abstract

The invention discloses a preparation method of a carbon/carbon liner for a natural gas chemical vapor deposition furnace, which adopts a carbon fiber needling body as a prefabricated body material and adopts the technical processes of resin brushing treatment, chemical vapor deposition densification and complete set assembly. The method comprises the following specific steps: firstly, adopting a carbon fiber needling body as a prefabricated body material; secondly, hardening and shaping; thirdly, preparing and brushing resin impregnation liquid; fourthly, curing/carbonizing treatment; fifthly, chemical vapor deposition is carried out to compact; sixthly, assembling into a complete set. The invention adopts the carbon/carbon composite material as the liner of the natural gas chemical vapor deposition furnace, has the characteristics of high temperature resistance, high strength, good heat-insulating property, difficult layering and the like, has simple process, low manufacturing cost, long service life and difficult deformation, greatly improves the service life and the safety performance of the chemical vapor deposition furnace, simultaneously can protect the electrodes of the deposition furnace and reduce the replacement rate of electrode materials.

Description

Preparation method of carbon/carbon liner for natural gas chemical vapor deposition furnace
Technical Field
The invention relates to a preparation method of carbon/carbon liner for a chemical vapor deposition furnace, belonging to the field of thermal field materials for high-temperature furnaces.
Background
At present, a carbon/carbon composite material is densified by adopting chemical vapor deposition furnace equipment, a carbon fiber preform is placed in a chemical vapor deposition furnace, organic carbon source gas is introduced under the conditions of high temperature and vacuum, carbon atoms are deposited in a gap of the preform through the cracking reaction of the gas, so that the preform achieves the purpose of densification, and a novel material (namely the carbon/carbon composite material) is formed; the carbon/carbon composite material has the characteristics of high strength, high temperature resistance and small specific gravity, is widely applied to the fields of aerospace, photovoltaics and high technology, and has wide market development prospect.
When the chemical vapor deposition furnace is used for carrying out densification treatment on the carbon/carbon composite material, the organic carbon source gas comprises propylene, propane, natural gas and other organic carbon-containing micromolecule gases, and when the gas with the cracking temperature of below 1000 ℃ is used as the carbon source gas, the heat-resistant steel material can be used as the inner container of the deposition furnace. However, when high-cracking-temperature gas such as natural gas is used as carbon source gas, the cracking temperature of the gas exceeds 1000 ℃, and heat-resistant steel and other metal alloy materials are difficult to meet the high-temperature use requirement of the deposition furnace, so that a carbon/carbon composite material with good high-temperature resistance, low density and high strength is required to be used as an inner container material to meet the use requirement of the chemical vapor deposition furnace.
Therefore, a large-sized chemical vapor deposition furnace using natural gas as a carbon source gas has a high demand for a preparation method of a furnace liner which is simple in process, high-temperature resistant, high in strength, good in heat insulation performance and not easy to layer. The traditional heat-resistant steel and metal alloy materials are difficult to meet the use requirements. The carbon/carbon composite material has the characteristics of low density, high temperature resistance, high mechanical strength, high impact toughness and the like, can be applied to the liner material of a large-size chemical vapor deposition furnace using natural gas as carbon source gas, can greatly improve the service life and the safety performance of the chemical vapor deposition furnace, can protect the electrode of the deposition furnace, and reduces the replacement rate of the electrode material.
Disclosure of Invention
The invention aims to solve the technical problems of poor heat resistance, low high-temperature strength, easy deformation and short service life of the existing large-size chemical vapor deposition furnace liner material taking natural gas as carbon source gas, and provides a preparation method of a carbon/carbon liner for a natural gas chemical vapor deposition furnace, which has the advantages of simple process, low density, good compact effect, high mechanical strength and excellent heat resistance, by utilizing the characteristics of high temperature resistance, high strength, good heat-insulating property and difficult layering of a carbon/carbon composite material.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of carbon/carbon liner for a natural gas chemical vapor deposition furnace is characterized by comprising the following steps:
the method comprises the following steps: the carbon fiber needling body is adopted as a preform material, and the density of the preform is controlled to be 0.20g/cm3-0.60g/cm3
Step two: and (3) setting the preform adopted in the step one in a curing furnace, heating to 150-300 ℃ under the condition that the heating rate is 2-50 ℃/h, then preserving heat for 1-10 h for setting treatment, and naturally cooling.
Step three: and (3) coating the inner surface and the outer surface of the preform subjected to the shaping treatment in the step two and the end surface of the preform with resin, wherein the coating is carried out twice, the first coating is carried out by adopting a pure resin solution, the blank after the coating is dried in the air for 10h-24h and then is subjected to second coating treatment, the second coating solution is prepared by resin and graphite powder according to the weight ratio of (2-20) to 1, and then the preform is dried in the air for 10h-24 h.
Step four: and (3) hoisting the blank coated with the resin in the third step into a carbonization furnace for curing/carbonization treatment, heating to 150-250 ℃ under the condition that the heating rate is 2-50 ℃/h, preserving heat for 2-6 h for curing treatment, then heating to 850-1000 ℃ under the condition that the heating rate is 2-50 ℃/h, preserving heat for 2-6 h for carbonization treatment, taking the product out of the furnace, cleaning the surface, and treating the carbon shell of the surface to be clean.
Step five: hoisting the blank subjected to surface cleaning in the fourth step into a deposition furnace for chemical vapor deposition densification, wherein propylene or natural gas is used as a carbon source gas, and the gas flow is 5m3/h-100m3H, heating to 850-1200 ℃ under the condition that the heating rate is 2 ℃/h-50 ℃/h, then preserving the heat for 50-300 h for densification treatment, naturally cooling, and when the density is more than or equal to 1.0g/cm3The next procedure is carried out.
Step six: and C, assembling the carbon/carbon liner subjected to densification treatment in the fifth step to obtain the carbon/carbon liner for the natural gas chemical vapor deposition furnace.
The preparation method of the carbon/carbon liner for the natural gas chemical vapor deposition furnace is characterized in that the carbon fiber needling body in the step one comprises a PAN-based 1K-24K carbon cloth or a PAN-based short fiber net tire alternately laminated needling preform, the thickness of the preform is 5mm-100mm, the inner diameter is phi 2000 mm-phi 6000mm, and the height is 100mm-2000 mm.
The preparation method of the carbon/carbon liner for the natural gas chemical vapor deposition furnace is characterized in that in the shaping treatment in the step two, a shaping tool is sleeved in a cylinder of the prefabricated body, the tool is made of a wooden product, the outer diameter of the tool is smaller than the inner diameter of the prefabricated body by 4mm, and the height of the tool is consistent with the height of the prefabricated body.
The preparation method of the carbon/carbon liner for the natural gas chemical vapor deposition furnace is characterized in that resin coating technology is carried out on the inner surface and the outer surface of the prefabricated body and the end face of the prefabricated body in the third step, the resin comprises one of phenolic resin, epoxy resin and furfuryl ketone resin, the particle size of graphite powder is less than 800 meshes, and the coating quantity of resin solution or mixed solution of the resin and the graphite powder is 0.1Kg-10Kg per square meter of the surface area of the prefabricated body.
The preparation method of the carbon/carbon liner for the natural gas chemical vapor deposition furnace is characterized in that the carbon/carbon liner assembly in the sixth step adopts upper and lower section self-fastening type assembly, or H-shaped clamping groove assembly, or direct overlapping assembly set.
The final density of the carbon/carbon liner for the natural gas chemical vapor deposition furnace prepared by the technical scheme is more than or equal to 1.0g/cm3Compressive strength of>80MPa, purity less than or equal to 1000ppm, strong airflow scouring resistance and oxidation resistance, and difficult layering.
Compared with the prior art, the invention has the following advantages:
1. compared with the traditional chemical vapor deposition furnace inner container, the carbon/carbon composite material adopted by the invention as the chemical vapor deposition furnace inner container has the characteristics of high temperature resistance, high strength, good heat insulation performance and difficult layering.
2. The hardening and shaping treatment process adopted by the carbon fiber needling preform can ensure that the preform is not easy to deform in the subsequent treatment process, and the densification efficiency of the preform can be greatly improved by adopting the secondary resin and the mixed liquid of the resin and the graphite powder for coating treatment.
Drawings
FIG. 1 is a block diagram of the process flow for preparing the carbon/carbon liner for the natural gas chemical vapor deposition furnace according to the invention.
Detailed Description
Example 1
The method comprises the following steps: the method is characterized in that 1K PAN-based carbon fibers are used as main raw materials, a carbon fiber needling body is used as a prefabricated body material, the thickness of the prefabricated body is 5mm, the inner diameter is phi 2000mm, and the height is 2000 mm. The density of the preform is controlled to be 0.20g/cm3
Step two: and (2) performing setting treatment on the prefabricated body adopted in the step one in a curing furnace, sleeving a setting tool in a prefabricated body cylinder, wherein the tool is made of a wooden product, the outer diameter of the tool is less than 4mm than the inner diameter of the prefabricated body, the height of the tool is consistent with the height of the prefabricated body, heating to 150 ℃ under the condition that the heating rate is 2 ℃/h, then performing heat preservation for 10h, performing setting treatment, and naturally cooling.
Step three: and (3) coating the inner surface and the outer surface of the prefabricated part subjected to the sizing treatment in the step two and the end surface of the prefabricated part with resin, wherein the resin is phenolic resin, the first coating is performed with pure phenolic resin solution, and the coating amount of the resin solution is 0.1Kg per square meter of the surface area of the prefabricated part. And airing the coated blank in air for 10 hours, then carrying out secondary coating treatment, wherein secondary coating solution is prepared by phenolic resin and graphite powder according to the weight ratio of 2:1, the particle size of the graphite powder is below 800 meshes, the coating amount of the mixed solution of the resin and the graphite powder is 10Kg per square meter of the surface area of the preform, and then continuously airing in air for 10 hours.
Step four: and (3) hoisting the blank coated with the resin in the third step into a carbonization furnace for curing/carbonization treatment, heating to 150 ℃ under the condition that the heating rate is 2 ℃/h, preserving heat for 2h for curing treatment, then heating to 850 ℃ under the condition that the heating rate is 2 ℃/h, preserving heat for 2h for carbonization treatment, taking the product out of the furnace, cleaning the surface, and treating the carbon crust of the surface to be clean.
Step five: hoisting the blank subjected to surface cleaning in the fourth step into a deposition furnace for chemical gasThe phase deposition is compact, propylene is used as a carbon source gas, and the gas flow is 5m3H, heating to 850 ℃ under the condition that the heating rate is 2 ℃/h, then preserving heat for 300h for densification treatment, naturally cooling, and when the density is more than or equal to 1.0g/cm3The next procedure is carried out.
Step six: and C, carrying out self-buckled assembly on the upper section and the lower section of the carbon/carbon liner subjected to densification treatment in the fifth step to obtain the carbon/carbon liner for the natural gas chemical vapor deposition furnace.
The final density of the carbon/carbon liner for the natural gas chemical vapor deposition furnace prepared by the technical scheme is 1.0g/cm3The compression strength is 85MPa, the purity is 900ppm, the airflow scouring resistance and the oxidation resistance are strong, and the delamination is not easy to occur.
Example 2
The method comprises the following steps: the method is characterized in that 12K PAN-based carbon fibers are used as main raw materials, a carbon fiber needling body is used as a prefabricated body material, the thickness of the prefabricated body is 50mm, the inner diameter is phi 4000mm, and the height is 1000 mm. The density of the preform is controlled at 0.40g/cm3
Step two: and (2) performing setting treatment on the prefabricated body adopted in the step one in a curing furnace, sleeving a setting tool in a prefabricated body cylinder, wherein the tool is made of a wooden product, the outer diameter of the tool is less than 4mm than the inner diameter of the prefabricated body, the height of the tool is consistent with the height of the prefabricated body, heating to 250 ℃ under the condition that the heating rate is 20 ℃/h, then performing setting treatment for 5h, and naturally cooling.
Step three: and (3) coating the inner surface and the outer surface of the preform subjected to the shaping treatment in the step two and the end surface with resin, wherein the resin is epoxy resin, the first coating is performed with pure epoxy resin solution, and the coating amount of the resin solution is 5Kg per square meter of the surface area of the preform. And airing the coated blank in air for 15 hours, then carrying out secondary coating treatment, wherein the secondary coating solution is prepared by epoxy resin and graphite powder according to the weight ratio of 10:1, the particle size of the graphite powder is below 1000 meshes, the coating amount of the mixed solution of the resin and the graphite powder is 5Kg per square meter of the surface area of the preform, and then continuously airing in air for 15 hours.
Step four: and (3) hoisting the blank coated with the resin in the third step into a carbonization furnace for curing/carbonization treatment, heating to 200 ℃ under the condition that the heating rate is 25 ℃/h, preserving heat for 4h for curing treatment, then heating to 900 ℃ under the condition that the heating rate is 25 ℃/h, preserving heat for 4h for carbonization treatment, taking the product out of the furnace, cleaning the surface, and treating the carbon crust of the surface.
Step five: hoisting the blank subjected to surface cleaning in the fourth step into a deposition furnace for chemical vapor deposition densification, wherein natural gas is used as a carbon source gas, and the gas flow is 50m3H, heating to 1050 ℃ under the condition that the heating rate is 25 ℃/h, then preserving the heat for 100h for densification treatment, naturally cooling, and when the density is more than or equal to 1.0g/cm3The next procedure is carried out.
Step six: and C, assembling the carbon/carbon liner subjected to densification treatment in the fifth step through an H-shaped clamping groove to obtain the carbon/carbon liner for the natural gas chemical vapor deposition furnace.
The final density of the carbon/carbon liner for the natural gas chemical vapor deposition furnace prepared by the technical scheme is 1.10g/cm3The compression strength is 90MPa, the purity is 600ppm, the airflow scouring resistance and the oxidation resistance are strong, and the delamination is not easy to occur.
Example 3
The method comprises the following steps: the method is characterized in that 24K PAN-based carbon fibers are used as main raw materials, a carbon fiber needling body is used as a prefabricated body material, the thickness of the prefabricated body is 100mm, the inner diameter is phi 6000mm, and the height is 100 mm. The density of the preform is controlled at 0.60g/cm3
Step two: and (2) performing setting treatment on the prefabricated body adopted in the step one in a curing furnace, sleeving a setting tool in a prefabricated body cylinder, wherein the tool is made of a wooden product, the outer diameter of the tool is less than 4mm than the inner diameter of the prefabricated body, the height of the tool is consistent with the height of the prefabricated body, heating to 300 ℃ under the condition that the heating rate is 50 ℃/h, then performing setting treatment for 1h, and naturally cooling.
Step three: and (3) coating resin on the inner surface and the outer surface of the preform subjected to the shaping treatment in the step two and the end surface of the preform, wherein the resin is furfuryl ketone resin, the first coating is performed by adopting a pure furfuryl ketone resin solution, and the coating amount of the resin solution is 10Kg per square meter of the surface area of the preform. And airing the coated blank in air for 24 hours, then carrying out secondary coating treatment, wherein a secondary coating solution is prepared by furfuryl ketone resin and graphite powder according to the weight ratio of 20:1, the particle size of the graphite powder is less than 1200 meshes, the coating amount of a mixed solution of the resin and the graphite powder is 0.1Kg per square meter of the surface area of the preform, and then continuously airing in air for 24 hours.
Step four: and (3) hoisting the blank coated with the resin in the third step into a carbonization furnace for curing/carbonization treatment, heating to 250 ℃ under the condition that the heating rate is 50 ℃/h, preserving heat for 6h for curing treatment, then heating to 1000 ℃ under the condition that the heating rate is 50 ℃/h, preserving heat for 6h for carbonization treatment, taking the product out of the furnace, cleaning the surface, and treating the carbon crust of the surface.
Step five: hoisting the blank subjected to surface cleaning in the fourth step into a deposition furnace for chemical vapor deposition densification, wherein natural gas is used as a carbon source gas, and the gas flow is 100m3H, heating to 1200 ℃ under the condition that the heating rate is 50 ℃/h, then preserving heat for 50h for densification treatment, naturally cooling, and when the density is more than or equal to 1.0g/cm3The next procedure is carried out.
Step six: and D, directly stacking and assembling the carbon/carbon liner subjected to densification treatment in the step five to obtain the carbon/carbon liner for the natural gas chemical vapor deposition furnace.
The final density of the carbon/carbon liner for the natural gas chemical vapor deposition furnace prepared by the technical scheme is 1.20g/cm3The compression strength is 105MPa, the purity is 500ppm, the airflow scouring resistance and the oxidation resistance are strong, and the delamination is not easy to occur.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, changes and equivalent structural changes made to the above embodiment according to the technical spirit of the present invention still fall within the protection scope of the technical solution of the present invention.

Claims (5)

1. A preparation method of carbon/carbon liner for a natural gas chemical vapor deposition furnace is characterized by comprising the following steps:
the method comprises the following steps: the carbon fiber needling body is adopted as a preform material, and the density of the preform is controlled to be 0.20g/cm3-0.60g/cm3
Step two: and (3) setting the preform adopted in the step one in a curing furnace, heating to 150-300 ℃ under the condition that the heating rate is 2-50 ℃/h, then preserving heat for 1-10 h for setting treatment, and naturally cooling.
Step three: and (3) coating the inner surface and the outer surface of the preform subjected to the shaping treatment in the step two and the end surface of the preform with resin, wherein the coating is carried out twice, the first coating is carried out by adopting a pure resin solution, the blank after the coating is dried in the air for 10h-24h and then is subjected to second coating treatment, the second coating solution is prepared by resin and graphite powder according to the weight ratio of (2-20) to 1, and then the preform is dried in the air for 10h-24 h.
Step four: and (3) hoisting the blank coated with the resin in the third step into a carbonization furnace for curing/carbonization treatment, heating to 150-250 ℃ under the condition that the heating rate is 2-50 ℃/h, preserving heat for 2-6 h for curing treatment, then heating to 850-1000 ℃ under the condition that the heating rate is 2-50 ℃/h, preserving heat for 2-6 h for carbonization treatment, taking the product out of the furnace, cleaning the surface, and treating the carbon shell of the surface to be clean.
Step five: hoisting the blank subjected to surface cleaning in the fourth step into a deposition furnace for chemical vapor deposition densification, wherein propylene or natural gas is used as a carbon source gas, and the gas flow is 5m3/h-100m3H, heating to 850-1200 ℃ under the condition that the heating rate is 2 ℃/h-50 ℃/h, then preserving the heat for 50-300 h for densification treatment, naturally cooling, and when the density is more than or equal to 1.0g/cm3The next procedure is carried out.
Step six: and assembling the carbon/carbon liner subjected to densification treatment in the fifth step to obtain the carbon/carbon liner for the natural gas chemical vapor deposition furnace.
2. The method for preparing the carbon/carbon liner for the natural gas chemical vapor deposition furnace according to claim 1, wherein the carbon fiber needled body in the step one comprises a PAN-based 1K-24K carbon cloth or a non-woven cloth and PAN-based short fiber net tire alternately laminated needled preform, the thickness of the preform is 5mm-100mm, the inner diameter is phi 2000 mm-phi 6000mm, and the height is 100mm-2000 mm.
3. The method for preparing the carbon/carbon liner for the natural gas chemical vapor deposition furnace according to the claim 1, wherein in the shaping treatment in the step two, a shaping tool is sleeved in a cylinder of the preform, the tool is made of a wood product, the outer diameter of the tool is less than 4mm than the inner diameter of the preform, and the height of the tool is consistent with the height of the preform.
4. The method for preparing the carbon/carbon liner for the natural gas chemical vapor deposition furnace according to the claim 1, wherein the inner surface and the outer surface of the preform in the third step are coated with resin, the resin comprises one of phenolic resin, epoxy resin and furfuryl ketone resin, the particle size of graphite powder is less than 800 meshes, and the coating amount of resin solution or the mixed solution of the resin and the graphite powder is 0.1Kg to 10Kg per square meter of the surface area of the preform.
5. The method for preparing the carbon/carbon liner for the natural gas chemical vapor deposition furnace according to claim 1, wherein the carbon/carbon liner assembly in the sixth step is an upper and lower self-fastening assembly, or an H-shaped clamping groove assembly, or a complete set of direct overlapping assembly.
The final density of the carbon/carbon liner for the natural gas chemical vapor deposition furnace prepared by the technical scheme is more than or equal to 1.0g/cm3Compressive strength of>80MPa, purity less than or equal to 1000ppm, strong airflow scouring resistance and oxidation resistance, and difficult layering.
CN202011630446.4A 2020-12-30 2020-12-30 Preparation method of carbon/carbon liner for natural gas chemical vapor deposition furnace Pending CN112723898A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113416086A (en) * 2021-06-18 2021-09-21 湖南金硅科技有限公司 Rotary furnace carbon ceramic furnace tube for CVD carbon vapor deposition, rotary furnace and preparation method of carbon ceramic furnace tube
CN115466528A (en) * 2022-08-03 2022-12-13 中南大学 Carbon black aerogel and preparation method thereof

Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1360887A (en) * 1971-06-25 1974-07-24 Bendix Corp Method of producing a carbon composite
JP2001048664A (en) * 1999-08-11 2001-02-20 Tokai Carbon Co Ltd Production of carbon fiber-reinforced carbon material
CN101747071A (en) * 2009-12-15 2010-06-23 王占双 Preparation of carbon/carbon mould for hot-pressed sintering furnace
CN102010231A (en) * 2010-10-24 2011-04-13 西安超码科技有限公司 Method for preparing low-density carbon/carbon composite material surface coating
CN102030555A (en) * 2010-11-18 2011-04-27 西安超码科技有限公司 Method for preparing thick carbon/carbon heat insulation cover for polysilicon hydrogenation furnace
CN102167611A (en) * 2011-01-27 2011-08-31 无锡市弟兆碳材料有限公司 Method for preparing carbon/carbon composite material plate
CN202323024U (en) * 2012-03-02 2012-07-11 烟台鲁航炭材料科技有限公司 Deposition chamber for chemical vapor deposition
CN103396139A (en) * 2013-08-05 2013-11-20 东莞市凯鹏复合材料有限公司 Manufacturing method of carbon/carbon crucible
CN104710184A (en) * 2013-12-12 2015-06-17 航天睿特碳材料有限公司 Gas phase rapid preparation method of U-type carbon/carbon heat-generating body
CN105712729A (en) * 2014-12-04 2016-06-29 航天睿特碳材料有限公司 Preparation method for crucible cover plate for polycrystalline ingot furnace
CN108191448A (en) * 2018-01-24 2018-06-22 航天睿特碳材料有限公司 A kind of method that winding process prepares carbon/carbon cylinder
CN210287519U (en) * 2019-07-02 2020-04-10 烟台鲁航炭材料科技有限公司 Rotating device for carbon-carbon composite material vapor deposition furnace
CN111960843A (en) * 2020-08-31 2020-11-20 陕西美兰德炭素有限责任公司 Method for shaping carbon fiber preform

Patent Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1360887A (en) * 1971-06-25 1974-07-24 Bendix Corp Method of producing a carbon composite
JP2001048664A (en) * 1999-08-11 2001-02-20 Tokai Carbon Co Ltd Production of carbon fiber-reinforced carbon material
CN101747071A (en) * 2009-12-15 2010-06-23 王占双 Preparation of carbon/carbon mould for hot-pressed sintering furnace
CN102010231A (en) * 2010-10-24 2011-04-13 西安超码科技有限公司 Method for preparing low-density carbon/carbon composite material surface coating
CN102030555A (en) * 2010-11-18 2011-04-27 西安超码科技有限公司 Method for preparing thick carbon/carbon heat insulation cover for polysilicon hydrogenation furnace
CN102167611A (en) * 2011-01-27 2011-08-31 无锡市弟兆碳材料有限公司 Method for preparing carbon/carbon composite material plate
CN202323024U (en) * 2012-03-02 2012-07-11 烟台鲁航炭材料科技有限公司 Deposition chamber for chemical vapor deposition
CN103396139A (en) * 2013-08-05 2013-11-20 东莞市凯鹏复合材料有限公司 Manufacturing method of carbon/carbon crucible
CN104710184A (en) * 2013-12-12 2015-06-17 航天睿特碳材料有限公司 Gas phase rapid preparation method of U-type carbon/carbon heat-generating body
CN105712729A (en) * 2014-12-04 2016-06-29 航天睿特碳材料有限公司 Preparation method for crucible cover plate for polycrystalline ingot furnace
CN108191448A (en) * 2018-01-24 2018-06-22 航天睿特碳材料有限公司 A kind of method that winding process prepares carbon/carbon cylinder
CN210287519U (en) * 2019-07-02 2020-04-10 烟台鲁航炭材料科技有限公司 Rotating device for carbon-carbon composite material vapor deposition furnace
CN111960843A (en) * 2020-08-31 2020-11-20 陕西美兰德炭素有限责任公司 Method for shaping carbon fiber preform

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
天津海关, 化学工业出版社 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113416086A (en) * 2021-06-18 2021-09-21 湖南金硅科技有限公司 Rotary furnace carbon ceramic furnace tube for CVD carbon vapor deposition, rotary furnace and preparation method of carbon ceramic furnace tube
CN115466528A (en) * 2022-08-03 2022-12-13 中南大学 Carbon black aerogel and preparation method thereof
CN115466528B (en) * 2022-08-03 2023-08-22 中南大学 Carbon black aerogel and preparation method thereof

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