CN114890805A - Preparation process of carbon-carbon crucible in continuous graphitizing furnace - Google Patents
Preparation process of carbon-carbon crucible in continuous graphitizing furnace Download PDFInfo
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Abstract
The invention discloses a preparation process of a carbon-carbon crucible in a continuous graphitizing furnace, which belongs to the technical field of carbon fiber composite materials and comprises 10 steps of prefabricated part, pretreatment, CVI hardening, CVI densification, high-temperature heat treatment, rough turning, dipping-carbonization, finish machining, CVD and metal coating, wherein the ash content of a finished carbon-carbon crucible product prepared by the process is 20-50ppm, the service life of the product is ensured, the process improves the carbon yield, shortens the construction period, reduces the cost and can resist the high temperature of 3000 ℃.
Description
Technical Field
The invention belongs to the technical field of carbon fiber composite materials, and particularly relates to a preparation process of a carbon-carbon crucible in a continuous graphitizing furnace.
Background
The continuous graphitization furnace is a furnace for producing graphitized products in a continuous output manner, and the acheson furnace widely used at present is a discontinuous furnace for periodic production, and due to the discontinuous production, the defects such as low productivity, fluctuation in quality, high power consumption, bad operating environment and the like are brought, so the continuous furnace becomes an important subject and a target for global attention and research and development. The performance of the crucible essential in the continuous graphitizing furnace is crucial, the carbon/carbon crucible is a composite material of carbon fibers and a fabric reinforced carbon matrix thereof, and has the characteristics of excellent heat resistance, excellent high-temperature mechanical property, light specific gravity, good ablation resistance and excellent frictional wear resistance.
The carbon fiber ash refers to inorganic residues left after carbon fibers are ablated at high temperature, and researches show that the content of the inorganic residues directly influences the exertion of the mechanical properties of the carbon fibers, but the ash content of a product obtained by the existing carbon crucible production process is generally about 200, the high-content ash can seriously influence the mechanical properties of a finished product, and the existing carbon crucible produced can only generally resist the high temperature of about 1500 ℃, and cannot meet the increasing temperature requirement of a graphitization furnace.
Therefore, a preparation process of the carbon-carbon crucible in the continuous graphitizing furnace, which reduces ash content, improves high temperature resistance, improves carbon yield and reduces cost, is needed.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preparation process of a carbon-carbon crucible in a continuous graphitizing furnace, wherein the ash content of a finished carbon-carbon crucible product prepared by the process is 20-50ppm, the service life of the product is ensured, the process improves the carbon yield, shortens the construction period, reduces the cost and can resist the high temperature of 3000 ℃.
In order to realize the purpose, the invention adopts the technical scheme that:
a preparation process of a carbon-carbon crucible in a continuous graphitizing furnace comprises the following steps:
1) performing a prefabricated part: alternately superposing a layer of carbon fiber plain cloth and a layer of short fiber net tire, and continuously winding and needling to obtain a prefabricated member;
2) pretreatment: pretreating the prefabricated member obtained in the step 1), preserving heat for 2-5h at 1800-;
3) CVI hardening: after the pretreatment of the step 2), placing the prefabricated member into a deposition furnace for CVI treatment at the temperature of 1000-;
4) CVI densification: after the hardening treatment in the step 3), removing the anti-deformation perforated graphite inner membrane in the prefabricated part, and performing CVI densification by adopting gas phase liquefaction at the temperature of 1000-;
5) high-temperature treatment: after the densification in the step 4), carrying out high-temperature treatment at 2800-;
6) rough turning: performing rough turning treatment after high-temperature treatment to obtain a prefabricated part product, and turning the single side with the allowance of 2-5 mm;
7) impregnation-carbonization: preheating the prefabricated part product in a preheating tank at the preheating temperature of 250-;
8) finish machining: after dipping and carbonization, finish turning is carried out firstly, and then finish milling is carried out, so that the dimension meets the requirement of a drawing;
9) CVD: after the fine processing, carrying out CVD processing at the temperature of 1100-1200 ℃, introducing natural gas at the temperature of 10-30L/min and nitrogen at the temperature of 1-3L/min, and introducing the gas at the furnace pressure of 1000-2000Pa for 40-60 h;
10) metal coating: and after CVD treatment, preparing a metal Ir coating on the surface by adopting a laser induced liquid phase deposition method to obtain a carbon-carbon crucible finished product.
Further, the carbon fiber plain cloth and the short fiber net tire in the step 1) respectively have the following weight percentages: 75-85% and 15-25%.
Further, the needling density in the step 1) is as follows: the middle tubular part is 30-35 needles/cm 2 (ii) a The upper part of the thickened port part is 35 to 40 needles/cm 2 (ii) a The lower thickened part and the bottom plate are 35-40 needles/cm 2 Interlayer density of 15-17 layers/cm 3 (ii) a The apparent bulk density of the resulting preform was: the middle tubular part is 0.45-0.5g/cm 3 (ii) a The upper thickened port part is more than or equal to 0.6g/cm 3 (ii) a The lower thickened part and the bottom plate are 0.5-0.53g/cm 3 。
Further, the flow rate of the natural gas in the step 3) is 40-80L/min, and the flow rate of the nitrogen is 4-8L/min.
Further, the density of the hardened prefabricated member in the step 3) is 0.9-1.0g/cm 3 。
Further, the flow rate of the natural gas in the step 4) is 50-80L/min, and the flow rate of the nitrogen is 5-8L/min.
Further, the density of the densified prefabricated part in the step 4) is more than or equal to 1.3g/cm 3 If the density is not more than or equal to 1.3g/cm 3 And performing CVI densification for the second time until the set index is reached.
Further, the density of the prefabricated part after dipping and carbonization in the step 7) is more than or equal to 1.7g/cm 3 If the density is not more than 1.7g/cm 3 And carrying out second impregnation-carbonization until reaching the set index.
The invention has the beneficial effects that: (1) the ash content of the finished carbon-carbon crucible product prepared by the method is 20-50ppm, the service life of the product is guaranteed, the carbon yield is improved, the construction period is shortened, the cost is reduced, and the finished carbon-carbon crucible product can resist the high temperature of 3000 ℃;
(2) the high-temperature pretreatment is adopted in the invention to eliminate some resin, impurities and the like remained in the prefabricated member in the manufacturing process of the prefabricated member and reduce the ash content of the finished product;
(3) the CVI hardening is adopted in the invention to ensure that the product has corresponding strength and prevent the product from deforming; CVI hardening and densification are carried out twice in order to guarantee the service life of the deposition furnace;
(4) in the prior art, impurities in the carbon material generally begin to volatilize after 2400 ℃, the invention adopts high-temperature treatment to prevent the impurities from entering the product in the production process, causing corrosion to the product and further purifying, thereby influencing the service life of the product, and the use temperature of the product is 3000 ℃, so that the stress can be eliminated in advance, and the product is prevented from deforming in the use process;
(5) according to the invention, rough turning is adopted because the density of the product is high after the CVI process, when the density of the product is higher, a density gradient is formed inside and outside the product, the higher the surface density is, the hole sealing can be realized on the surface of the product, a layer of hole sealing on the surface can be turned off by rough turning, and the subsequent impregnation carbonization efficiency is improved;
(6) the invention adopts asphalt impregnation, has higher carbon yield, and can solve the technical problem that thick products can only be deposited on the surface by vapor deposition and can not be deposited in the products;
(7) the invention adopts the metal coating and the Ir metal coating, can resist the high temperature of 3000 ℃, can form a compact metal layer on the surface, and prevents gas and impurities thereof from entering the product to corrode the product;
(8) the carbon-carbon crucible prepared by the invention has long service life, and the most important of the service life of the product is product density, surface coating and graphitization degree.
Detailed Description
For a better understanding of the present invention, embodiments of the present invention are described in detail below with reference to examples, but those skilled in the art will understand that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention.
Example 1:
a preparation process of a carbon-carbon crucible in a continuous graphitizing furnace comprises the following steps:
1) performing a prefabricated part: alternately superposing and continuously winding and needling a layer of carbon fiber plain cloth and a layer of short fiber net tire to obtain a prefabricated member, wherein the carbon fiber plain cloth and the short fiber net tire respectively comprise the following components in percentage by weight: 75% and 25%, wherein the needling density is as follows: the middle tubular part is 30 needles/cm 2 (ii) a The upper part of the thickened port part is 40 needles/cm 2 (ii) a The lower thickened part and the bottom plate are 35 needles/cm 2 The interlayer density was 15 layers/cm 3 (ii) a To obtainThe apparent bulk density of the preform of (a): middle tubular part 0.45g/cm 3 (ii) a The upper part of the thickened port part is 0.6g/cm 3 (ii) a The lower thickened part and the bottom plate are 0.5g/cm 3 ；
2) Pretreatment: pretreating the prefabricated member obtained in the step 1), preserving heat for 2 hours at 2500 ℃, and introducing nitrogen for protection during treatment;
3) CVI hardening: after the pretreatment of the step 2), placing the prefabricated member into a deposition furnace for CVI treatment, introducing natural gas at 1000 ℃, 40L/min and nitrogen at 4L/min, keeping the furnace pressure at 3000pa, introducing the gas for 100h, placing an anti-deformation perforated graphite inner membrane in the prefabricated member during the treatment, placing a carbon plate or graphite paper with the thickness of 20mm on the top layer of the prefabricated member after hardening, wherein the density of the prefabricated member after hardening is 1.0g/cm 3 ；
4) CVI densification: after the hardening treatment in the step 3), removing the internal anti-deformation perforated graphite inner membrane of the prefabricated part, and performing CVI densification by adopting gas phase liquefaction at the temperature of 1000 ℃, introducing 80L/min of natural gas and 8L/min of nitrogen, wherein the furnace pressure is 3000pa, the ventilation time is 150h, and the density of the densified prefabricated part is 1.3g/cm 3 ；
5) High-temperature treatment: after the densification in the step 4), carrying out 2800 ℃ high-temperature treatment, keeping the temperature for 10h, and filling nitrogen for protection in the process;
6) rough turning: after high-temperature treatment, rough turning treatment is carried out to obtain a prefabricated part product, and the single-side allowance is turned by 2 mm;
7) impregnation-carbonization: preheating the prefabricated part product in a preheating tank at 300 ℃ for 5h, heating the asphalt material in a melting tank to 250 ℃, pumping the asphalt material into a dipping tank at 5MPa and 250 ℃, dipping the preheated prefabricated part product in the dipping tank, carbonizing the prefabricated part product in a carbonization furnace at 900 ℃, preserving the temperature for 10h, and keeping the density of the dipped and carbonized prefabricated part to be 1.7g/cm 3 ；
8) Finish machining: after dipping and carbonization, finish turning is carried out firstly, and then finish milling is carried out, so that the dimension meets the requirement of a drawing;
9) CVD: after fine processing, carrying out CVD processing at 1100 ℃, introducing natural gas 30L/min and nitrogen 3L/min, keeping the furnace pressure at 2000pa, and introducing the gas for 40 h;
10) metal coating: and after CVD treatment, preparing a metal Ir coating on the surface by adopting a laser induced liquid phase deposition method to obtain a carbon-carbon crucible finished product.
Example 2:
a preparation process of a carbon-carbon crucible in a continuous graphitizing furnace comprises the following steps:
1) performing a prefabricated part: alternately superposing and continuously winding and needling a layer of carbon fiber plain cloth and a layer of short fiber net tire to obtain a prefabricated member, wherein the carbon fiber plain cloth and the short fiber net tire respectively comprise the following components in percentage by weight: 85% and 15%, wherein the needling density is as follows: the middle tubular part is 35 needles/cm 2 (ii) a The upper part of the thickened port part is 35 needles/cm 2 (ii) a The lower thickened part and the bottom plate are 40 needles/cm 2 The interlayer density was 17 layers/cm 3 (ii) a The apparent bulk density of the resulting preform was: middle tubular part 0.5g/cm 3 (ii) a The upper part of the thickened port part is 0.75g/cm 3 (ii) a The lower thickened part and the bottom plate are 0.53g/cm 3 ；
2) Pretreatment: pretreating the prefabricated member obtained in the step 1), preserving heat for 5 hours at 2000 ℃, and introducing nitrogen for protection during treatment;
3) CVI hardening: after the pretreatment of the step 2), putting the prefabricated member into a deposition furnace for CVI treatment at the temperature of 1200 ℃, introducing natural gas for 60L/min and nitrogen for 6L/min, the furnace pressure is 2500pa, the ventilation time is 200h, arranging an anti-deformation open-pore graphite inner membrane in the prefabricated member during the treatment, placing a carbon plate or graphite paper with the thickness of 30mm on the upper part of the topmost layer, and setting the density of the hardened prefabricated member to be 0.9g/cm 3 ；
4) CVI densification: after the hardening treatment in the step 3), removing the internal anti-deformation perforated graphite inner membrane of the prefabricated part, performing CVI densification by adopting gas phase liquefaction at the temperature of 1200 ℃, introducing 50L/min of natural gas and 5L/min of nitrogen, wherein the furnace pressure is 3500pa, the ventilation time is 250h, and the density of the densified prefabricated part is 1.5g/cm 3 ；
5) High-temperature treatment: after the densification in the step 4), performing 3200 ℃ high-temperature treatment, preserving heat for 5 hours, and filling nitrogen for protection in the process;
6) rough turning: after high-temperature treatment, rough turning treatment is carried out to obtain a prefabricated part product, and the single-side allowance is turned by 5 mm;
7) impregnation-carbonization: preheating the prefabricated part product in a preheating tank at 250 ℃ for 10h, heating the asphalt material in a melting tank to 350 ℃, pumping the asphalt material into a dipping tank at 10MPa and 350 ℃, dipping the preheated prefabricated part product in the dipping tank, carbonizing the prefabricated part product in a carbonization furnace at 1500 ℃ for 5h, and keeping the temperature of the dipped and carbonized prefabricated part for 1.8g/cm 3 ；
8) Finish machining: after dipping and carbonization, finish turning is carried out firstly, and then finish milling is carried out, so that the dimension meets the requirement of a drawing;
9) CVD: after fine processing, carrying out CVD processing at 1200 ℃, introducing natural gas 10L/min and nitrogen 1L/min, keeping the furnace pressure at 1000pa, and introducing the gas for 60 h;
10) metal coating: and after CVD treatment, preparing a metal Ir coating on the surface by adopting a laser induced liquid phase deposition method to obtain a carbon-carbon crucible finished product.
Example 3:
a preparation process of a carbon-carbon crucible in a continuous graphitizing furnace comprises the following steps:
1) performing a prefabricated part: alternately superposing and continuously winding and needling a layer of carbon fiber plain cloth and a layer of short fiber net tire to obtain a prefabricated member, wherein the carbon fiber plain cloth and the short fiber net tire respectively comprise the following components in percentage by weight: 80% and 20%, wherein the needling density is as follows: the middle tubular part is 32 needles/cm 2 (ii) a The upper part is thickened at the port part of 36 needles/cm 2 (ii) a The lower thickened part and the bottom plate are 38 needles/cm 2 The interlayer density was 16 layers/cm 3 (ii) a The apparent bulk density of the resulting preform was: middle tubular part 0.43g/cm 3 (ii) a The upper part of the thickened port part is 0.75g/cm 3 (ii) a The lower thickened part and the bottom plate are 0.52g/cm 3 ；
2) Pretreatment: pretreating the prefabricated member obtained in the step 1), preserving heat for 4 hours at 1800 ℃, and introducing nitrogen for protection during treatment;
3) CVI hardening: after the pretreatment of the step 2), putting the mixture into a deposition furnace for CVI treatment at the temperature of 1150 ℃, introducing 80L/min of natural gas and 8L/min of nitrogen, controlling the furnace pressure to 2800pa and introducing the gas for 140hDuring treatment, the prefabricated member is internally provided with an anti-deformation perforated graphite inner membrane, a carbon plate or graphite paper with the thickness of 25mm is placed on the upper part of the topmost layer, and the density of the hardened prefabricated member is 0.96g/cm 3 ；
4) CVI densification: after the hardening treatment in the step 3), removing the internal anti-deformation open-pore graphite inner film of the prefabricated part, performing CVI densification by adopting gas phase liquefaction at the temperature of 1100 ℃, introducing 70L/min of natural gas and 7L/min of nitrogen, introducing 3250pa of furnace pressure, introducing for 200h, and ensuring that the density of the densified prefabricated part is 1.45g/cm 3 ；
5) High-temperature treatment: after the densification in the step 4), carrying out high-temperature treatment at 3000 ℃, preserving heat for 5-10h, and filling nitrogen for protection in the process;
6) rough turning: after high-temperature treatment, rough turning treatment is carried out to obtain a prefabricated part product, and the single-side allowance is turned by 4 mm;
7) impregnation-carbonization: preheating the prefabricated part product in a preheating tank at 280 ℃ for 8h, heating the asphalt material in a melting tank to 300 ℃, pumping the asphalt material into a dipping tank at the pressure of 8MPa and the temperature of 260 ℃, dipping the preheated prefabricated part product in the dipping tank, carbonizing the prefabricated part product in a carbonization furnace at the carbonization temperature of 1200 ℃ for 7h, and keeping the temperature of the dipped and carbonized prefabricated part to be 1.75g/cm in density 3 ；
8) Finish machining: after dipping and carbonization, finish turning is carried out firstly, and then finish milling is carried out, so that the dimension meets the requirement of a drawing;
9) CVD: after finish machining, carrying out CVD treatment at the temperature of 1150 ℃, introducing natural gas at 20L/min and nitrogen at 2L/min, keeping the furnace pressure at 1800pa, and introducing the gas for 55 h;
10) metal coating: and after CVD treatment, preparing a metal Ir coating on the surface by adopting a laser induced liquid phase deposition method to obtain a carbon-carbon crucible finished product.
Comparative example 1:
comparative example 1 is different from example 1 in that the pretreatment of step 2) is omitted and other technical contents are the same as example 1.
Comparative example 2:
comparative example 2 is different from example 1 in that the temperature of the high temperature treatment of step 5) is changed from 3000 c to 2000 c, and the other technical contents are the same as example 1.
Comparative example 3:
comparative example 3 differs from example 1 in that the metallic Ir coating in step 10) is replaced by a conventional coating, the other technical contents being the same as in example 1.
The carbon-carbon crucibles prepared in examples 1 to 3 and comparative examples 1 to 3 were subjected to technical index tests, and the test results are shown in table 1.
TABLE 1
2. High temperature test
The carbon-carbon crucibles prepared in examples 1 to 3 and comparative examples 1 to 3 were put into a continuous graphitization furnace to work, various carbon materials were continuously produced into graphitized articles at 3000 ℃ under the protection of various inert atmospheres, and after one cycle of production was completed, the properties of the carbon-carbon crucibles were measured, and the measurement results are shown in table 2.
TABLE 2
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments. Those skilled in the art should appreciate that many modifications and variations are possible in light of the above teaching without departing from the scope of the invention.
Claims (8)
1. A preparation process of a carbon-carbon crucible in a continuous graphitizing furnace is characterized by comprising the following steps:
1) performing a prefabricated part: alternately superposing a layer of carbon fiber plain cloth and a layer of short fiber net tire, and continuously winding and needling to obtain a prefabricated member;
2) pretreatment: pretreating the prefabricated member obtained in the step 1), preserving heat for 2-5h at 1800-;
3) CVI hardening: after the pretreatment of the step 2), placing the prefabricated member into a deposition furnace for CVI treatment at the temperature of 1000-;
4) CVI densification: after the hardening treatment in the step 3), removing the anti-deformation perforated graphite inner membrane in the prefabricated part, and performing CVI densification by adopting gas phase liquefaction at the temperature of 1000-;
5) high-temperature treatment: after the densification in the step 4), carrying out high-temperature treatment at 2800-;
6) rough turning: performing rough turning treatment after high-temperature treatment to obtain a prefabricated part product, and turning the single side with the allowance of 2-5 mm;
7) impregnation-carbonization: preheating the prefabricated part product in a preheating tank at the preheating temperature of 250-;
8) finish machining: after dipping and carbonization, finish turning is carried out firstly, and then finish milling is carried out, so that the dimension meets the requirement of a drawing;
9) CVD: after the fine processing, carrying out CVD processing at the temperature of 1100-1200 ℃, introducing natural gas at the temperature of 10-30L/min and nitrogen at the temperature of 1-3L/min, and introducing the gas at the furnace pressure of 1000-2000Pa for 40-60 h;
10) metal coating: and after CVD treatment, preparing a metal Ir coating on the surface by adopting a laser induced liquid phase deposition method to obtain a carbon-carbon crucible finished product.
2. The process for preparing a carbon-carbon crucible in a continuous graphitization furnace according to claim 1, wherein the weight percentages of the carbon fiber plain cloth and the short fiber net blank in the step 1) are respectively as follows: 75-85% and 15-25%.
3. The process for preparing a carbon-carbon crucible in a continuous graphitization furnace according to claim 1, wherein the needling density in step 1) is as follows: the middle tubular part is 30-35 needles/cm 2 (ii) a The upper part of the thickened port part is 35 to 40 needles/cm 2 (ii) a The lower thickened part and the bottom plate are 35-40 needles/cm 2 The density between layers is 15-17 layers/cm 3 (ii) a The apparent bulk density of the resulting preform was: the middle tubular part is 0.45-0.5g/cm 3 (ii) a The upper thickened port part is more than or equal to 0.6g/cm 3 (ii) a The lower thickened part and the bottom plate are 0.5-0.53g/cm 3 。
4. The process for preparing a carbon-carbon crucible in a continuous graphitization furnace as claimed in claim 1, wherein the natural gas is introduced at a flow rate of 40-80L/min and the nitrogen is introduced at a flow rate of 4-8L/min in step 3).
5. The process for preparing a carbon-carbon crucible in a continuous graphitization furnace as claimed in claim 1, wherein the density of the hardened preform in the step 3) is 0.9-1.0g/cm 3 。
6. The process for preparing a carbon-carbon crucible in a continuous graphitization furnace as claimed in claim 1, wherein the natural gas is introduced at a flow rate of 50-80L/min and the nitrogen is introduced at a flow rate of 5-8L/min in step 4).
7. The process for preparing a carbon-carbon crucible in a continuous graphitization furnace as claimed in claim 1, wherein the density of the densified preform in the step 4) is more than or equal to 1.3g/cm 3 If the density is not more than or equal to 1.3g/cm 3 And performing CVI densification for the second time until the set index is reached.
8. The process for preparing a carbon-carbon crucible in a continuous graphitization furnace as claimed in claim 1, wherein the density of the impregnated-carbonized preform in the step 7) is more than or equal to 1.7g/cm 3 If the density is not more than 1.7g/cm 3 And carrying out second impregnation-carbonization until reaching the set index.
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