CN100389094C - Prepn process of composite material of carbon fiber and asphalt transition layer - Google Patents
Prepn process of composite material of carbon fiber and asphalt transition layer Download PDFInfo
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- CN100389094C CN100389094C CNB200610104438XA CN200610104438A CN100389094C CN 100389094 C CN100389094 C CN 100389094C CN B200610104438X A CNB200610104438X A CN B200610104438XA CN 200610104438 A CN200610104438 A CN 200610104438A CN 100389094 C CN100389094 C CN 100389094C
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Abstract
The present invention relates to preparation process of composite material of carbon fiber and asphalt transition layer. The carbon fiber prefab is first coated with intermediate phase asphalt powder and soaked under inert gas protection inside stainless steel tank in a dipping oven, and then carbonized through raising temperature and maintaining under inert gas protection in a carbonizing oven and deposited through chemical vapor permeation process in a chemical vapor depositing oven to prepare the C/C composite material with intermediate phase asphalt transition layer. The intermediate phase asphalt form the combining interface of medium strength between the carbon fiber and the pyrolytic carbon base, and this raise the mechanical performance of the composite material. The present invention has relatively low preparation temperature, 600-800 deg.c, and lowered preparation cost.
Description
Technical field
The present invention relates to the preparation method, the particularly preparation method of mesophase pitch transition layer matrix material of a kind of carbon fiber and RESEARCH OF PYROCARBON matrix transition layer matrix material.
Background technology
Carbon/carbon compound material has a lot of excellent properties, but its poor toughness, fragility height have limited it as the widespread use of structure properties product at military affairs and aviation field.Document [Hariom Dwivedi, Rakesh B.Mathur, Tersem L.Dhami, Om P.Bahl, Marc Monthioux, Sahendra P.Sharma.Evidence for the benefit of adding a carbon interphase in anall-carbon composite.Carbon, 44 (4), 2006,699-709] reported the method that carbon fiber and bitumencarb basal body interface place add the RESEARCH OF PYROCARBON interface transition layer in carbon/carbon compound material, and point out that interpolation carbon interfacial layer can make the carbon/carbon compound material toughness of preparation improve in all carbon/carbon compound materials, fragility reduces, and whole mechanical property is greatly improved.Its main theoretical foundation is: 1) surfaceness of carbon fiber and surface functional group change after deposition one deck RESEARCH OF PYROCARBON, thereby have changed the condition of surface of carbon fiber; 2) sedimentary RESEARCH OF PYROCARBON is one deck porous, low-density interfacial layer, and these characteristics help the deflection matrix and destroy the tiny crack that produces, and realize crack deflection, make the mechanical property of material increase; 3) the RESEARCH OF PYROCARBON interfacial layer is one deck porous organization, and it helps main crack growth is secondary crackle, thereby slows down the velocity of diffusion and the intensity of crackle, and material opposing destructive ability is strengthened.The method for preparing the RESEARCH OF PYROCARBON transition layer is to adopt chemical Vapor deposition process (hereinafter to be referred as CVD), realizes by the parameters such as depositing temperature, depositing time, presoma kind and flow velocity of controlling CVD technology.For different presomas, the depositing temperature scope of CVD is 800～1300 ℃, so this preparation method needs high temperature service, and is very high for the requirement of depositing device, and increases preparation cost.
Summary of the invention
Need high temperature service to cause the high deficiency of preparation cost in order to overcome prior art for preparing RESEARCH OF PYROCARBON transition layer, the invention provides the preparation method of a kind of carbon fiber and pyrolysis asphalt transition layer matrix material, by mesophase pitch as carbon fiber in the carbon/carbon compound material and RESEARCH OF PYROCARBON matrix transition layer, preparation process does not need high temperature service, reaches the purpose that reduces preparation cost.
The technical solution adopted for the present invention to solve the technical problems is: the preparation method of carbon fiber and pyrolysis asphalt transition layer matrix material comprises the steps:
1) at first the 3K carbon cloth is carried out cutting according to designed size, lamination and Z make the prefabricated carbon fiber body to puncture together then, and choosing intermediate phase content, to account for the mesophase pitch powder of pitch weight 85% standby;
2) above-mentioned prefabricated carbon fiber body is placed in the stainless steel impregnating autoclave, behind above-mentioned mesophase pitch powder embedding precast body, puts into the dipping stove;
3) to the dipping stove evacuation, and with rare gas element feeding dipping stove displacement furnace air, after the dipping stove is incubated 0.5～1.5h after heating to 200～400 ℃, feed the rare gas element of 0.5～1MPa and continue insulation, pressurize 0.5～1.5h, powered-down, cut-out inertia source of the gas naturally cool to room temperature then;
4) the stainless steel impregnating autoclave is taken out from the dipping stove, the upper end is pushed down with the stainless steel cover plate, put into carbide furnace, and behind one deck carbon dust of stainless steel cover plate upper berth, to the carbide furnace heat temperature raising, in 2h, be raised to 250 ℃ and be incubated 0.5～1.5h naturally by room temperature, adopt different temperature rise rate temperature-gradient methods, insulation then, between 250～800 ℃, temperature rise rate is controlled in 5～25 ℃/h scope, each stage insulation 0.5～2.5h, whole carbonization process is protected with rare gas element, and the pressure of rare gas element is 0.5～1MPa;
5) the mesophase pitch carbon transition layer carbon/carbon compound material after the taking-up carbonization from impregnating autoclave is put into chemical vapor deposition stove then and is deposited with chemical vapor infiltration, makes mesophase pitch transition layer carbon/carbon compound material finished product.
The invention has the beneficial effects as follows, because by in carbon/carbon compound material, adopting mesophase pitch as carbon fiber in the carbon/carbon compound material and RESEARCH OF PYROCARBON matrix transition layer, can alleviate carbon fiber and the unmatched characteristic of RESEARCH OF PYROCARBON matrix thermal expansivity, thereby form weak in junction, carbon fiber interface in conjunction with the strong interfacial bond characteristic that weakens carbon fiber and RESEARCH OF PYROCARBON, construct the moderate interface of bonding strength, improved the mechanical property of material.And mesophase pitch is as the method that adopts dipping for preparing of carbon fiber in the carbon/carbon compound material and RESEARCH OF PYROCARBON matrix transition layer, adopt the chemical Vapor deposition process RESEARCH OF PYROCARBON to compare with prior art as transition layer, prepare and temperature requiredly be reduced to 600～800 ℃ by 800～1300 ℃, whole process of preparation does not need high temperature deposition equipment, thereby has reduced preparation cost.
The invention will be further described below in conjunction with drawings and Examples.
Description of drawings
Fig. 1 is the prepared carbon/carbon compound material fracture scanning electron microscope pattern photo of the preparation method of carbon fiber of the present invention and pyrolysis asphalt transition layer matrix material.
Fig. 2 is preparation method's mesophase pitch transition layer carbonization process temperature curve of carbon fiber of the present invention and pyrolysis asphalt transition layer matrix material.
Embodiment
Embodiment 1, at first the 3K carbon cloth carried out cutting according to 80mm * 80mm size, and lamination and Z make the prefabricated carbon fiber body of 80mm * 80mm * 5mm to puncture together then.
The mesophase pitch powder of choosing softening temperature and be 290 ℃ is standby, and intermediate phase content accounts for 85% of pitch weight.
Above-mentioned prefabricated carbon fiber body is placed in the stainless steel impregnating autoclave of Φ 130 * 120mm, behind above-mentioned mesophase pitch powder embedding precast body, puts into the dipping stove.
After checking that the sealing of flooding stove is intact, to the dipping stove evacuation, when vacuum tightness reaches 5 * 10
-3During MPa, with N
2Feed dipping stove displacement furnace air, according to the aforesaid operations process dipping stove is vacuumized once more then, to guarantee that remaining atmosphere is N in the dipping stove
2In confirming the dipping stove is N
2After, to dipping stove heat temperature raising, setting the heating terminal temperature is 330 ℃.The dipping stove freely heats up, during asphalt melting, liquid bitumen, fully enters in the hole of precast body inside the adsorption of its generation by negative pressure and carbon fiber.Reach behind 330 ℃ of design temperatures behind the insulation 1h, feed the N of 0.5MPa
2, and under 330 ℃ of temperature, pressure 0.5MPa, continue insulation, pressurize 1h, then powered-down, cut off N
2Source of the gas naturally cools to room temperature.
Through after the above-mentioned art breading, stainless steel impregnating autoclave upper end is pushed down with the stainless steel cover plate, put into the carbide furnace carbonization, and on the cover board spread one deck carbon dust with the expansion that weakens the carbonization process appearance, prevent atmospheric oxidation.To the carbide furnace heat temperature raising, be raised to 250 ℃ and be incubated 1h naturally by room temperature in the 2h; Temperature rise rate with 10 ℃/h is raised to 350 ℃ of insulation 1h from 250 ℃ then; Temperature rise rate with 5 ℃/h is raised to 450 ℃ of insulation 2h from 350 ℃; Temperature rise rate with 15 ℃/h is raised to 600 ℃ of insulation 1h from 450 ℃; Be raised to 800 ℃ of insulation 2h with the temperature rise rate of 25 ℃/h from 600 ℃, temperature curve is referring to Fig. 2.Whole carbonization process N
2Atmosphere is protected, N
2Pressure is 0.5MPa.
Mesophase pitch carbon transition layer carbon/carbon compound material from the stainless steel impregnating autoclave after the taking-up carbonization, put into chemical vapor deposition stove then and deposit, to reach the density requirements of mesophase pitch transition layer carbon/carbon compound material finished product with chemical vapor infiltration.From the mesophase pitch transition layer carbon/carbon compound material fracture scanning electron microscopic observation that contains shown in Figure 1, can see the mesophase pitch carbon transition layer that centers on carbon fibre growth at the carbon fiber edge.
Embodiment 2, at first the 3K carbon cloth carried out cutting according to 60mm * 60mm size, and lamination and Z make the prefabricated carbon fiber body of 60mm * 60mm * 4mm to puncture together then.
Choosing of mesophase pitch powder with embodiment 1.
Above-mentioned prefabricated carbon fiber body is placed in the stainless steel impregnating autoclave of Φ 130 * 120mm, behind above-mentioned mesophase pitch powder embedding precast body, puts into the dipping stove.
After checking that the sealing of flooding stove is intact, to the dipping stove evacuation, when vacuum tightness reaches 5 * 10
-3During MPa, with rare gas element Ar
2Feed dipping stove displacement furnace air, according to the aforesaid operations process dipping stove is vacuumized once more then, to guarantee that remaining atmosphere is rare gas element Ar in the dipping stove
2In confirming the dipping stove is inert atmosphere Ar
2After, to dipping stove heat temperature raising, setting the heating terminal temperature is 200 ℃.The dipping stove freely heats up, during asphalt melting, liquid bitumen, fully enters in the hole of precast body inside the adsorption of its generation by negative pressure and carbon fiber.Reach behind 200 ℃ of design temperatures behind the insulation 1.5h, feed the Ar of 0.5MPa
2, and under 200 ℃ of temperature, pressure 0.5MPa, continue insulation, pressurize 1.5h, then powered-down, cut off rare gas element Ar
2Source of the gas naturally cools to room temperature.
Through after the above-mentioned art breading, stainless steel impregnating autoclave upper end is pushed down with the stainless steel cover plate, put into the carbide furnace carbonization, and on the cover board spread one deck carbon dust.To the carbide furnace heat temperature raising, be raised to 250 ℃ and be incubated 1h naturally by room temperature in the 2h; Temperature rise rate with 10 ℃/h is raised to 350 ℃ of insulation 1h from 250 ℃ then; Temperature rise rate with 5 ℃/h is raised to 450 ℃ of insulation 2h from 350 ℃; Temperature rise rate with 15 ℃/h is raised to 600 ℃ of insulation 1h from 450 ℃; Be raised to 800 ℃ of insulation 2h with the temperature rise rate of 25 ℃/h from 600 ℃, temperature curve is referring to Fig. 2.Whole carbonization process Ar
2Atmosphere is protected, Ar
2Pressure is 0.5MPa.
Mesophase pitch carbon transition layer carbon/carbon compound material from the stainless steel impregnating autoclave after the taking-up carbonization, put into chemical vapor deposition stove then and deposit, to reach the density requirements of mesophase pitch transition layer carbon/carbon compound material finished product with chemical vapor infiltration.
Embodiment 3, at first the 3K carbon cloth carried out cutting according to 70mm * 70mm size, and lamination and Z make the prefabricated carbon fiber body of 70mm * 70mm * 6mm to puncture together then.
Choosing of mesophase pitch powder with embodiment 1.
Above-mentioned prefabricated carbon fiber body is placed in the stainless steel impregnating autoclave of Φ 130 * 120mm, behind above-mentioned mesophase pitch powder embedding precast body, puts into the dipping stove.
After checking that the sealing of flooding stove is intact, to the dipping stove evacuation, when vacuum tightness reaches 5 * 10
-3During MPa, with rare gas element He
2Feed dipping stove displacement furnace air, according to the aforesaid operations process dipping stove is vacuumized once more then, to guarantee that remaining atmosphere is rare gas element He in the dipping stove
2In confirming the dipping stove is inert atmosphere He
2After, to dipping stove heat temperature raising, setting the heating terminal temperature is 380 ℃.The dipping stove freely heats up, during asphalt melting, liquid bitumen, fully enters in the hole of precast body inside the adsorption of its generation by negative pressure and carbon fiber.Reach behind 380 ℃ of design temperatures behind the insulation 1h, feed the He of 1MPa
2, and under 380 ℃ of temperature, pressure 1MPa, continuing insulation, pressurize 1h, powered-down, cut-out inertia source of the gas naturally cool to room temperature then.
Through after the above-mentioned art breading, stainless steel impregnating autoclave upper end is pushed down with the stainless steel cover plate, put into the carbide furnace carbonization, and on the cover board spread one deck carbon dust.To the carbide furnace heat temperature raising, be raised to 250 ℃ and be incubated 1h naturally by room temperature in the 2h; Temperature rise rate with 10 ℃/h is raised to 350 ℃ of insulation 1h from 250 ℃ then; Temperature rise rate with 5 ℃/h is raised to 450 ℃ of insulation 2h from 350 ℃; Temperature rise rate with 15 ℃/h is raised to 600 ℃ of insulation 1h from 450 ℃; Be raised to 800 ℃ of insulation 2h with the temperature rise rate of 25 ℃/h from 600 ℃, temperature curve is referring to Fig. 2.Whole carbonization process He
2Atmosphere is protected, He
2Pressure is 0.5MPa.
Mesophase pitch carbon transition layer carbon/carbon compound material from the stainless steel impregnating autoclave after the taking-up carbonization, put into chemical vapor deposition stove then and deposit, to reach the density requirements of mesophase pitch transition layer carbon/carbon compound material finished product with chemical vapor infiltration.
Embodiment 4, at first the 3K carbon cloth carried out cutting according to 90mm * 90mm size, and lamination and Z make the prefabricated carbon fiber body of 80mm * 80mm * 6mm to puncture together then.
Choosing of mesophase pitch powder with embodiment 1.
Above-mentioned prefabricated carbon fiber body is placed in the stainless steel impregnating autoclave of Φ 130 * 120mm, behind above-mentioned mesophase pitch powder embedding precast body, puts into the dipping stove.
After checking that the sealing of flooding stove is intact, to the dipping stove evacuation, when vacuum tightness reaches 5 * 10
-3During MPa, with N
2Feed dipping stove displacement furnace air, according to the aforesaid operations process dipping stove is vacuumized once more then, to guarantee that remaining atmosphere is N in the dipping stove
2In confirming the dipping stove is N
2After, to dipping stove heat temperature raising, setting the heating terminal temperature is 400 ℃.The dipping stove freely heats up, during asphalt melting, liquid bitumen, fully enters in the hole of precast body inside the adsorption of its generation by negative pressure and carbon fiber.Reach behind 400 ℃ of design temperatures behind the insulation 0.5h, feed the N of 1MPa
2, and under 400 ℃ of temperature, pressure 1MPa, continue insulation, pressurize 0.5h, then powered-down, cut off N
2Source of the gas naturally cools to room temperature.
Through after the above-mentioned art breading, stainless steel impregnating autoclave upper end is pushed down with the stainless steel cover plate, put into the carbide furnace carbonization, and on the cover board spread one deck carbon dust.To the carbide furnace heat temperature raising, be raised to 250 ℃ and be incubated 1h naturally by room temperature in the 2h; Temperature rise rate with 10 ℃/h is raised to 350 ℃ of insulation 1h from 250 ℃ then; Temperature rise rate with 5 ℃/h is raised to 450 ℃ of insulation 2h from 350 ℃; Temperature rise rate with 15 ℃/h is raised to 600 ℃ of insulation 1h from 450 ℃; Be raised to 800 ℃ of insulation 2h with the temperature rise rate of 25 ℃/h from 600 ℃, temperature curve is referring to Fig. 2.Whole carbonization process N
2Atmosphere is protected, N
2Pressure is 1MPa.
Mesophase pitch carbon transition layer carbon/carbon compound material from the stainless steel impregnating autoclave after the taking-up carbonization, put into chemical vapor deposition stove then and deposit, to reach the density requirements of mesophase pitch transition layer carbon/carbon compound material finished product with chemical vapor infiltration.
Claims (1)
1. the preparation method of carbon fiber and pyrolysis asphalt transition layer matrix material is characterized in that comprising the steps:
1) at first the 3K carbon cloth is carried out cutting, lamination and Z make the prefabricated carbon fiber body to puncture together then, and it is standby to choose the mesophase pitch powder, and wherein intermediate phase accounts for 85% of pitch weight;
2) above-mentioned prefabricated carbon fiber body is placed in the stainless steel impregnating autoclave, behind above-mentioned mesophase pitch powder embedding precast body, puts into the dipping stove;
3) to the dipping stove evacuation, and with rare gas element feeding dipping stove displacement furnace air, after the dipping stove is incubated 0.5～1.5h after heating to 200～400 ℃, feed the rare gas element of 0.5～1MPa and continue insulation, pressurize 0.5～1.5h, powered-down, cut-out inertia source of the gas naturally cool to room temperature then;
4) the stainless steel impregnating autoclave is taken out from the dipping stove, the upper end is pushed down with the stainless steel cover plate, put into carbide furnace, and behind one deck carbon dust of stainless steel cover plate upper berth, to the carbide furnace heat temperature raising, in 2h, be raised to 250 ℃ and be incubated 0.5～1.5h naturally by room temperature, adopt different temperature rise rate temperature-gradient methods, insulation then, between 250～800 ℃, temperature rise rate is controlled in 5～25 ℃/h scope, each stage insulation 0.5～2.5h, whole carbonization process is protected with rare gas element, and the pressure of rare gas element is 0.5～1MPa;
5) the mesophase pitch carbon transition layer carbon/carbon compound material after the taking-up carbonization from impregnating autoclave is put into chemical vapor deposition stove then and is deposited with chemical vapor infiltration.
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| CN101591178B (en) * | 2008-05-30 | 2012-08-08 | 鞍山塞诺达碳纤维有限公司 | Method for manufacturing rigid carbon fiber heat insulating material and surface treatment method |
| CN102093068A (en) * | 2010-11-18 | 2011-06-15 | 西北工业大学 | Method for preparing intermediate phase pitch-based carbon/carbon composite |
| CN102180696B (en) * | 2011-03-08 | 2013-11-20 | 宁波方力密封件有限公司 | Carbon-based composite material and production process thereof |
| CN104446588B (en) * | 2014-12-15 | 2016-08-31 | 湖北三江航天红阳机电有限公司 | A kind of prefabricated carbon fiber body liquid impregnation density method |
| US10017426B2 (en) * | 2016-04-01 | 2018-07-10 | Honeywell International Inc. | High density carbon-carbon friction materials |
| CN108117405A (en) * | 2017-12-27 | 2018-06-05 | 江西嘉捷信达新材料科技有限公司 | The interface modification method of C-base composte material |
| CN108727053B (en) * | 2018-06-04 | 2020-11-24 | 中钢集团新型材料（浙江）有限公司 | Preparation method of high-performance carbon-carbon composite carbon material |
| CN111807853B (en) * | 2020-07-07 | 2021-05-28 | 湖南碳谷新材料有限公司 | Carbon-carbon composite material and preparation process and application thereof |
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| CN113292352B (en) * | 2021-04-30 | 2022-09-23 | 北京化工大学 | Preparation method of unidirectional high-thermal-conductivity carbon/carbon composite material |
| CN114455950B (en) * | 2022-01-06 | 2023-08-15 | 韶关赛普超硬材料科技有限公司 | Method for preparing graphite carrier boat from lignin-rich plant |
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Effective date of registration: 20221108 Address after: No. 25, Yangbei Road, Luoshe Town, Huishan District, Wuxi City, Jiangsu Province, 214154 Patentee after: Wuxi Bozhi Composite Materials Co.,Ltd. Address before: 710072 No. 127 Youyi West Road, Shaanxi, Xi'an Patentee before: Northwestern Polytechnical University |
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