CN105948777B - A kind of density is 0.5~0.8g/cm3Carbon/carbon compound material preparation method - Google Patents

A kind of density is 0.5~0.8g/cm3Carbon/carbon compound material preparation method Download PDF

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CN105948777B
CN105948777B CN201610422517.9A CN201610422517A CN105948777B CN 105948777 B CN105948777 B CN 105948777B CN 201610422517 A CN201610422517 A CN 201610422517A CN 105948777 B CN105948777 B CN 105948777B
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carbon
compound material
carbon compound
density
low
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CN105948777A (en
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郭领军
寇钢
李贺军
彭坚
李伟
刘宁坤
霍彩霞
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Wuxi Bozhi Composite Materials Co ltd
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Northwestern Polytechnical University
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
    • C04B35/83—Carbon fibres in a carbon matrix
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
    • C04B35/521—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained by impregnation of carbon products with a carbonisable material
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/448—Sulphates or sulphites
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/5216—Inorganic
    • C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5248—Carbon, e.g. graphite
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density

Abstract

It is 0.5~0.8g/cm the present invention relates to a kind of density3Carbon/carbon compound material preparation method, the carbon/carbon compound material of low-density is impregnated using copper sulfate solution, by introducing a certain amount of metallic copper element catalyst in immersion-heating-drying-pyrolytic-original position carbothermic reduction reaction normal direction low-density carbon/carbon compound material, promote its in-situ growing carbon nano tube in isothermal chemical vapor deposition processes.Then the low-density carbon/carbon compound material containing carbon nanotube is placed in thermal gradient chemical vapor infiltration furnace and carries out final densification, obtains the carbon/carbon compound material of low porosity.

Description

A kind of density is 0.5~0.8g/cm3Carbon/carbon compound material preparation method
Technical field
The invention belongs to field of composite material preparation, being related to a kind of density is 0.5~0.8g/cm3Carbon/carbon compound material Preparation method.
Background technique
Carbon/carbon compound material has excellent mechanical behavior under high temperature and preferable Burning corrosion resistance energy, can be in aerospace Field is widely used.But in the preparation process of carbon/carbon compound material, the generation of unavoidable internal void, is caused always There are a large amount of larger-size porosity defects in composite inner.And the service performance of carbon/carbon compound material mainly with its density It is closely bound up with porosity.In general, the method for reducing carbon/carbon compound material porosity mainly has extension densification time and more It is secondary to repeat to densify.But with the increase of densification time, the closed pore inside carbon/carbon compound material can not be eliminated or reduce. The biggish hole inside precast body that is formed as of closure hole is difficult to be pyrolyzed carbon filling, and is pyrolyzed in the small place of hole Carbon can deposit faster, and with the increase of sedimentation time, the small gap around big gap is all pyrolyzed carbon filling, and big gap is also It is not completely filled and has just been closed to form lipostomous hole, subsequent pyrolytic carbon cannot be introduced into these closure holes.Therefore, it to drop Hole inside low carbon/carbon compound material, it is necessary to reduce hole or elimination before forming closure hole.It is closed the shape of hole At being because there is non-uniform gap of taking measurements greatly inside precast body, in densification process, larger-size gap is difficult to It is pyrolyzed carbon filling.Therefore, the density of carbon/carbon compound material is improved by extending the densification time or densification being repeated several times Effect be often not satisfactory.
Summary of the invention
Technical problems to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes that a kind of density is 0.5~0.8g/cm3Carbon/carbon it is multiple The preparation method of condensation material is filled by the in-situ growing carbon nano tube in low-density carbon/carbon compound material or carbon nanocoils Hole reduces the pore-size in precast body, during pyrocarbon, and meanwhile it is heavy in carbon fiber and carbon nano tube surface Product achievees the purpose that reduce carbon/carbon compound material inner void and reduces carbon carbon composite porosity.
Technical solution
A kind of density is 0.5~0.8g/cm3Carbon/carbon compound material preparation method, it is characterised in that steps are as follows:
Step 1 is activated: carbon/carbon compound material is ultrasonically treated in 5.0~15.0wt% nitric acid solution 30min is dried after being ultrasonically treated in deionized water；
Step 2 introduces metal copper in carbon/carbon compound material:
A: will through step 1, treated that carbon/carbon compound material is soaked into 10.0~50.0wt% copper-bath, heating 20~60min is kept the temperature after to 100 DEG C；
B: carbon/carbon compound material is placed in tube type resistance furnace, is evacuated to -0.05MPa and is passed through 0.2~0.8L/min's H2, tube type resistance furnace is warming up to 800 DEG C with the rate of 10 DEG C/min under normal pressure and keeps the temperature 3~10h；Then room is cooled to the furnace Temperature, obtains the low-density carbon/carbon compound material containing nano copper particle, and realization deposits nano copper particle in carbon/carbon compound material；
Step 3, in-situ growing carbon nano tube: the low-density carbon/carbon compound material containing nano copper particle is placed in isothermal It learns in gaseous phase deposition stove, is 900~1200 DEG C in temperature, the time is in-situ growing carbon nano tube under the conditions of 10~50h；
Step 4: carbon/carbon compound material handled by step 3 is placed in the cause carried out in thermal gradient chemical vapor infiltration furnace Densification process, obtains low porosity and density is not less than 1.8g/cm3Carbon/carbon compound material.
In the step 1 be ultrasonically treated 10min twice, 80 DEG C at a temperature of dried.
The nitric acid solution concentration is 5.0~15.0wt%.
The copper-bath concentration is 10.0wt%~50.0wt%.
Beneficial effect
A kind of density proposed by the present invention is 0.5~0.8g/cm3Carbon/carbon compound material preparation method, utilize sulfuric acid Copper liquor impregnates the carbon/carbon compound material of low-density, anti-by immersion-heating-drying-pyrolytic-original position carbon thermal reduction It answers and introduces a certain amount of metallic copper element catalyst in the carbon/carbon compound material of normal direction low-density, promote it in isothermal chemistry gas In-situ growing carbon nano tube in phase deposition process.The low-density carbon/carbon compound material containing carbon nanotube is then placed in hot ladder Final densification is carried out in degree chemical vapor deposition stove, obtains the carbon/carbon compound material of low porosity.
Detailed description of the invention
Fig. 1 is the carbon nanotube grown in low-density carbon/carbon compound material
Carbon nanotube when Fig. 2 is that sample does not densify completely, in carbon/carbon compound material in macrovoid
Fig. 3 is carbon nanotube of the sample after densification, in carbon/carbon compound material in big gap
Specific embodiment
Now in conjunction with embodiment, attached drawing, the invention will be further described:
Embodiment one
The present embodiment is a kind of preparation method of low porosity carbon/carbon compound material, and detailed process is:
Step 1: being 0.5g/cm by the density after using acetone to be cleaned by ultrasonic3Carbon/carbon compound material immerse concentration be Surface activation process 30min is carried out in 5.0wt% nitric acid solution.It is finally ultrasonically treated 10min in deionized water, repeats two It is secondary, 80 DEG C at a temperature of dried；
Step 2: by step 1 processing after carbon/carbon compound material be soaked into concentration be 10.0wt% copper-bath in, 20min is kept the temperature after being heated to 100 DEG C, is then placed on being dried in 90 DEG C of baking ovens；
Step 3: step 2 gained carbon/carbon compound material being placed in tube type resistance furnace and is heat-treated；By tube type resistance furnace It is evacuated to the H that -0.05MPa is passed through 0.2L/min2, tube type resistance furnace is warming up to 800 DEG C and keeps the temperature 10h；Then cold with furnace But to room temperature, to realize that density be 0.5g/cm3Carbon/carbon compound material in introduce a certain amount of metallic copper catalytic elements；
Step 4: step 3 gained carbon/carbon compound material in-situ growing carbon nano tube: being placed in isothermal chemical vapor deposition stove Middle in-situ growing carbon nano tube, temperature are 900 DEG C, time 20h；
Step 5: the low-density carbon/carbon compound material of carbon nanotubes obtained above final densification: being placed in hot ladder It spends in chemical vapor deposition stove, densification is carried out using traditional dense technique, finally obtains porosity less than 3.75% Carbon/carbon compound material.
Embodiment two
The present embodiment is a kind of preparation method of low porosity carbon/carbon compound material, and detailed process is:
Step 1: being 0.6g/cm by the density after using acetone to be cleaned by ultrasonic3Carbon/carbon compound material immerse concentration be Surface activation process 15min is carried out in 10.0% nitric acid solution.It is finally ultrasonically treated 10min in deionized water, is repeated twice, 80 DEG C at a temperature of dried；；
Step 2: by step 1, treated that carbon/carbon compound material is soaked into that concentration is in the copper-bath of 20.0wt%, 40min is kept the temperature after being heated to 100 DEG C.It is dried being placed in 90 DEG C of baking ovens immersed with the carbon/carbon compound material of copper-bath It is dry；
Step 3: step 2 gained carbon/carbon compound material being placed in tube type resistance furnace and is heat-treated；By tube type resistance furnace It is evacuated to the H that -0.05MPa is passed through 0.8L/min2, tube type resistance furnace is warming up to 800 DEG C and keeps the temperature 5h；Then sample is with furnace It is cooled to room temperature, to realize that density be 0.6g/cm3Carbon/carbon compound material in introduce a certain amount of metallic copper catalysis member Element；
Step 4: in-situ growing carbon nano tube: by the low-density carbon/carbon compound material obtained above containing nano copper particle It is placed in in-situ growing carbon nano tube in isothermal chemical vapor deposition stove, temperature is 1000 DEG C, time 50h；
Step 5: the low-density carbon/carbon compound material of carbon nanotubes obtained above final densification: being placed in hot ladder It spends in chemical vapor deposition stove, densification is carried out using traditional dense technique, obtains carbon/carbon that porosity further decreases Composite material.
Embodiment three
The present embodiment is a kind of preparation method of low porosity carbon/carbon compound material, and detailed process is:
Step 1: being 0.8g/cm by the density after using acetone to be cleaned by ultrasonic3Carbon/carbon compound material immerse concentration be Surface activation process 30min is carried out in 15% nitric acid solution.It is finally ultrasonically treated 10min in deionized water, is repeated twice, It is dried at a temperature of 80 DEG C；
Step 2: by step 1, treated that carbon/carbon compound material is soaked into that concentration is in the copper-bath of 50.0wt%, 60min is kept the temperature after being heated to 100 DEG C, is dried being placed in 90 DEG C of baking ovens immersed with the carbon/carbon compound material of copper-bath It is dry；；
Step 3: step 2 gained carbon/carbon compound material being placed in tube type resistance furnace and is heat-treated；By tube type resistance furnace It is evacuated to the H that -0.05MPa is passed through 0.5L/min2, tube type resistance furnace is warming up to 800 DEG C and keeps the temperature 3h；Then furnace cooling To room temperature, a certain amount of metallic copper catalytic elements are introduced into low-density carbon/carbon compound material to realize；
Step 4: in-situ growing carbon nano tube: by the low-density carbon/carbon compound material obtained above containing nano copper particle It is placed in isothermal chemical vapor deposition stove and carries out in-situ growing carbon nano tube, temperature is 1200 DEG C, time 10h；
Step 5: the low-density carbon/carbon compound material of carbon nanotubes obtained above final densification: being placed in hot ladder It spends in chemical vapor deposition stove, densification is carried out using traditional dense technique, obtains carbon/carbon composite wood of porosity reduction Material.

Claims (2)

1. a kind of preparation method of carbon/carbon compound material, it is characterised in that steps are as follows:
Step 1 is activated: being 0.5~0.8g/cm by density3Carbon/carbon compound material in 5.0~15.0wt% nitric acid solution In carry out ultrasonic treatment 30min, in deionized water be ultrasonically treated after dry；
Step 2 introduces metal copper in carbon/carbon compound material:
A: will through step 1, treated that carbon/carbon compound material is soaked into 10.0~50.0wt% copper-bath, be heated to 20~60min is kept the temperature after 100 DEG C；
B: carbon/carbon compound material is placed in tube type resistance furnace, is evacuated to the H that -0.05MPa is passed through 0.2~0.8L/min2, often Tube type resistance furnace is warming up to 800 DEG C with the rate of 10 DEG C/min and keeps the temperature 3~10h by pressure；Then it cools to room temperature with the furnace, obtains To the low-density carbon/carbon compound material containing nano copper particle, realization deposits nano copper particle in carbon/carbon compound material；
Step 3, in-situ growing carbon nano tube: the low-density carbon/carbon compound material containing nano copper particle is placed in isothermal chemistry gas It is 900~1200 DEG C in temperature, the time is in-situ growing carbon nano tube under the conditions of 10~50h in phase cvd furnace；
Step 4: carbon/carbon compound material handled by step 3 being placed in thermal gradient chemical vapor infiltration furnace and is carried out at densification Reason, obtains low porosity and density is not less than 1.8g/cm3Carbon/carbon compound material.
2. the preparation method of carbon/carbon compound material according to claim 1, it is characterised in that: in deionization in the step 1 In water be ultrasonically treated 10min twice, 80 DEG C at a temperature of dried.
CN201610422517.9A 2016-06-14 2016-06-14 A kind of density is 0.5~0.8g/cm3Carbon/carbon compound material preparation method Active CN105948777B (en)

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Publication number Priority date Publication date Assignee Title
CN107010978B (en) * 2017-03-24 2020-04-03 西北工业大学 Preparation method of carbon nanotube reinforced pyrolytic carbon material
CN113480321B (en) * 2021-05-07 2022-09-13 西北工业大学 Core-shell structure carbon nanotube reinforced carbon/carbon composite material and preparation method thereof

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CN101376597A (en) * 2008-09-25 2009-03-04 中南大学 Preparation of in situ carbon nano-tube enhanced carbon / carbon composite material
CN102776404A (en) * 2012-07-07 2012-11-14 西北工业大学 Preparation method of carbon/carbon-copper composite material
CN105645962A (en) * 2016-01-06 2016-06-08 天津大学 Preparation method of high-temperature-resistant oxidation-resistant heat-conducting carbon fiber/silicon carbide composite material

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CN1868869A (en) * 2006-06-07 2006-11-29 西北工业大学 Method of growing carbon nanometer pipe on carbon cloth base
CN101376597A (en) * 2008-09-25 2009-03-04 中南大学 Preparation of in situ carbon nano-tube enhanced carbon / carbon composite material
CN102776404A (en) * 2012-07-07 2012-11-14 西北工业大学 Preparation method of carbon/carbon-copper composite material
CN105645962A (en) * 2016-01-06 2016-06-08 天津大学 Preparation method of high-temperature-resistant oxidation-resistant heat-conducting carbon fiber/silicon carbide composite material

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