CN107935614A - Carbon ceramic composite material and preparation method thereof - Google Patents
Carbon ceramic composite material and preparation method thereof Download PDFInfo
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- CN107935614A CN107935614A CN201711235448.1A CN201711235448A CN107935614A CN 107935614 A CN107935614 A CN 107935614A CN 201711235448 A CN201711235448 A CN 201711235448A CN 107935614 A CN107935614 A CN 107935614A
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- C04B35/806—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- 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
- C04B35/56—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 carbides or oxycarbides
- C04B35/565—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 carbides or oxycarbides based on silicon carbide
- C04B35/573—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 carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
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- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
Abstract
The invention belongs to carbon ceramic composite material preparation field, and in particular to a kind of carbon ceramic composite material and preparation method thereof.It includes the following steps：(1) pretreatment carbon fiber is obtained in carbon fiber surface cladding binding paste, wherein, the binding paste is dissolved in solvent by binding agent to be made；(2) ceramic powder containing carbon dust and silica flour is prepared, the wherein molar ratio of silicon and carbon is more than 1: 1；(3) the pretreatment carbon fiber is woven to obtain netted pretreatment carbon fiber precast body, the ceramic powder is filled in the gap of the netted pretreatment carbon fiber precast body, forms carbon ceramic composite material precast body；(4) sinter the carbon ceramic composite material precast body and obtain carbon ceramic composite material, thus obtained carbon ceramic composite material has more preferable toughness and compression strength, and it is small as friction material wear extent.
Description
Technical field
The invention belongs to carbon ceramic composite material preparation field, and in particular to a kind of carbon ceramic composite material and preparation method thereof.
Background technology
Carbon ceramic composite material is carbon fibre reinforced silicon carbide ceramic composite, its with density is low, antioxygenic property is good,
The features such as corrosion-resistant, and there is the advantages such as carbon disk density is low, brake is steady, wear weight loss rate is small as brake material, therefore
More and more concerns and research are caused in friction material field.Its traditional preparation process mainly includes chemical vapor deposition
Method and liquid immersion method, chemical vapour deposition technique are first to prepare carbon disk (carbon fiber is woven into the shape designed by product), so
It is repeated multiple times afterwards in a certain temperature conditions to be fumigated containing silicane hydroxide, until densification, this method process cycle are up to 2-
3 months, energy consumption was big, of high cost.Liquid immersion method is first to prepare carbon disk and polysilane or polysilane carbon, then in vacuum, nitrogen
Or under conditions of the protection of argon gas, polysilane or Polycarbosilane are penetrated into carbon disk, then be heat-treated, it is repeated multiple times, until fine and close
Change, the preparation process of polysilane or Polycarbosilane is complex and high cost in this method.Therefore a kind of inexpensive, fast short-term training is developed
The carbon ceramic composite material preparation method of type has become the hot spot of research and important development is sent to.
3D printing technique is the advanced manufacturing technology to grow up the late 1980s, it can direct basis
Product design data, quickly produce the exemplar, mould or model of new product, greatly shorten the process-cycle of product, and reduction is ground
This is made.3D printing technique is applied to the preparation of carbon ceramic composite material can make up problem existing in the prior art well.
Answered for this reason, Chinese patent literature CA106927847A discloses a kind of fiber reinforced ceramic based on 3D printing technique
Condensation material manufacturing process and device.Its forming method includes：(1) the main printhead of ceramic fibre sustainable supply is continuously strengthened, together
When, ceramic slurry is supplied to main printhead by slurry inlet B, and compressed gas is passed through from A mouthfuls, there is provided homogeneous pressure；(2) it is leading
Ceramic slurry at print head nozzle wraps continuous fiber and is extruded under the pressure of compressed gas at nozzle, (3) initiator
Eject from initiator nozzle mouth, be sprayed onto in the form of mist state on the ceramic slurry printed, ceramic slurry is in UV illumination
Penetrate under the double action with initiator and solidify, thus print current cross-section；(4) after model is completed when the section of preceding layer,
Lifting gear will decline a lift height together with workbench, repeat the above steps, until part is completed；(5) will printing
The part of completion irradiates curing in the UV lamp, and carries out degreasing and high temperature sintering to the part after curing, that is, obtains fiber increasing
The shaping of strong ceramic matric composite.The fiber reinforced ceramic zero with certain toughness and intensity can be obtained by this method
Part, but the interface bonding energy force difference in this method between continuous fiber and ceramic slurry, its toughness and intensity have much room for improvement, and
As friction material, its wear extent is big.
The content of the invention
Therefore, the technical problem to be solved in the present invention is to overcome the carbon being prepared in the prior art based on the prior art
The defects of toughness of ceramic composite material, big compression strength difference and wear extent, so as to provide a kind of preparation side of carbon ceramic composite material
Method, the carbon ceramic composite material obtained by this method have more preferable toughness and compression strength, and it is as friction material wear extent
It is small.
Technical scheme is as follows：
A kind of preparation method of carbon ceramic composite material, includes the following steps：(1) obtained in carbon fiber surface cladding binding paste
To pretreatment carbon fiber, wherein, the binding paste is dissolved in solvent by binding agent to be made；(2) prepare and contain carbon dust and silicon
The molar ratio of the ceramic powder of powder, wherein silicon and carbon is more than 1: 1；(3) the pretreatment carbon fiber is woven to obtain netted
Pretreatment carbon fiber precast body, the ceramic powder is filled in the gap of the netted pretreatment carbon fiber precast body
In, form carbon ceramic composite material precast body；(4) sinter the carbon ceramic composite material precast body and obtain carbon ceramic composite material.
The step (3) includes, and the pretreatment carbon fiber is woven to obtain netted pretreatment carbon fiber layer, will
The ceramic powder is filled in the gap of the pretreatment carbon fiber layer, forms carbon ceramic composite material layer；Repetitive operation, obtains
If the carbon ceramic composite material precast body overlapped to form by dried layer carbon ceramic composite material layer.
In the step (1), it is calculated in mass percent, the concentration of the binding paste is 5%-40%, the binding agent
For the one or more in epoxy resin, phenolic resin or modified coal tar pitch.
In the step (1), the solvent is acetone, n-hexane or gasoline.
In the step (4), the temperature of sintering is 1500-1800 DEG C, time 0.5h-3.0h.
In the step (4), the pressure of sintering is 10MPa-200MPa.
In the step (2), the ceramic powder further includes the binding agent for accounting for the ceramic powder gross mass 2%-5%.
The ceramic powder further includes the one or more in pure boron, diboron trioxide or boric acid, wherein, boron accounts for the pottery
The 1%-3% of porcelain powder gross mass.
Carbon dust in the ceramic powder is one kind in activated carbon, tar asphalt, furane resins, phenolic resin or carbon black
It is or a variety of.
Silica flour in the ceramic powder is polycrystalline silica flour.
The preparation method is 3D printing method, including, (1) described pretreatment carbon fiber sustainable supply is beaten at least one
Head is printed, meanwhile, the ceramic powder sustainable supply to remaining printhead；(2) the pre- place is sprayed according to setting program, printhead
Carbon fiber is managed, braiding obtains netted pretreatment carbon fiber precast body, and the ceramic powder is filled in netted by remaining printhead
Pretreatment carbon fiber precast body gap in, thus print carbon ceramic composite material precast body；(3) it is compound to sinter the carbon pottery
Prefabricated body obtains carbon ceramic composite material.
The step (2) includes, and according to setting program, printhead sprays the pretreatment carbon fiber, and braiding obtains netted
Pretreatment carbon fiber layer, the ceramic powder is filled in the gap of netted pretreatment carbon fiber by remaining printhead, by
This prints the pretreatment carbon fiber layer filled with ceramic powder, i.e. carbon ceramic composite material layer；Repetitive operation, if obtaining by dried layer
The carbon ceramic composite material precast body that carbon ceramic composite material layer overlaps to form.
The carbon ceramic composite material that a kind of preparation method by carbon ceramic composite material as described above is prepared.
Technical solution of the present invention, has the following advantages that：
1. the preparation method of carbon ceramic composite material provided by the invention, is included in carbon fiber surface cladding binding paste and obtains
Carbon fiber is pre-processed, and the molar ratio of silicon and carbon is more than 1: 1 in ceramic powder, and binding paste is coated on the surface one of carbon fiber
Aspect improves the process operability of carbon fiber knitting forming, on the other hand, sintering process of the pretreatment carbon fiber in step (4)
In, the binding agent in the binding paste of carbon fiber surface can carbonize, and after binding agent charing is 45%-65% containing carbon content, its
It can react with silica flour unnecessary in ceramic powder, so that the surface chemistry between reinforced carbon fiber and ceramic powder combines,
And then improve toughness, compression strength and the wearability of carbon ceramic composite material.
2. the preparation method of carbon ceramic composite material provided by the invention, binding agent is further included in ceramic powder, binding agent exists
There is higher carbon content, charcoal and unnecessary pasc reaction, so as to improve the interface between carbon fiber and silicon carbide ceramics after charing
Chemical bond.
3. the preparation method of carbon ceramic composite material provided by the invention, added in ceramic powder pure boron, diboron trioxide or
Boric acid, on the one hand can reduce the temperature of sintering, easy to produce；On the other hand, in sintering process, diboron trioxide and boric acid are equal
It can generate pure boron, pure boron meeting and adhere to the charcoal reaction after the resin charing of carbon fiber surface, improve carbon fiber and ceramic powder
Between bond strength, and then improve product folding resistance, compression strength and wearability.
4. the preparation method of carbon ceramic composite material provided by the invention, the carbon dust in this powder of making pottery selects activated carbon, tar
The characteristics of one or more in pitch, furane resins, phenolic resin or carbon black, they are active big, phosphorus content is high, a side
Face can reduce the temperature of sintering, easy to produce, on the other hand can increase the bond strength between carbon dust and silica flour, improve carbon
Toughness, compression strength and the abrasivity of ceramic composite material.
5. the preparation method of carbon ceramic composite material provided by the invention, since the carbon dust in slurry and silica flour are uniformly distributed
In the gap of netted pretreatment carbon fiber layer, then carbon dust and silica flour can fully react in sintering process, and it is equal to obtain distribution
Even carborundum, and then obtain the good carbon ceramic composite material of homogeneity.
6. the preparation method of carbon ceramic composite material provided by the invention, the system of carbon ceramic material is carried out using 3D printing technique
It is standby, the raising of speed can be performed with the upgrading and order of 3D printing equipment, performs the increase of 3D printing head quantity, more
The reduction process-cycle.
7. the preparation method of carbon ceramic composite material provided by the invention, using the generation carbon that can inexpensively react at high temperature
The carbon dust and silica flour of SiClx, reduce production cost.
8. the preparation method of carbon ceramic composite material provided by the invention, the system of carbon ceramic material is carried out using 3D printing technique
It is standby, the setting program of 3D printer can be set according to needs of production, to obtained netted pretreatment carbon fiber precast body
The size of mesopore, braiding order and shape are set, and then obtain different carbon ceramic composite materials, and this method is simple, just
In realization.
9. the structure for the carbon ceramic composite material that the present invention obtains has more preferable designability and uniformity.
Embodiment
Technical scheme will be clearly and completely described below, it is clear that described embodiment is this hair
Bright part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not having
Have and make all one for being obtained under the premise of creative work his embodiments, belong to the scope of protection of the invention.
The manufacturer of polycrystalline silica flour is upper marine fry dried food ingredients powder body material Co., Ltd.
Embodiment 1
The pretreatment of carbon fiber：Epoxy resin is dissolved in the binding paste for obtaining that mass fraction is 5% in acetone soln, will
Impregnated carbon fiber obtains pretreatment carbon fiber in binding paste.
The preparation of ceramic powder：Silicon powder particle is made in 308g polycrystalline silica flours and 122g activated carbons are uniformly mixed.
Input setting program in the operating system of 3D printer, pretreatment carbon fiber sustainable supply a to printhead,
Printhead sprays pretreatment carbon fiber and is woven to obtain netted pretreatment carbon fiber layer according to setting program, meanwhile, ceramics
Ceramic powder is filled in netted pretreatment carbon fibre by powder sustainable supply to another printhead, the printhead according to setting program
In the gap for tieing up layer, the pretreatment carbon fiber layer filled with ceramic powder, i.e. carbon ceramic composite material layer are thus printed, completes one
After layer, lifting gear declines the thickness of a layering, two printheads and lifting gear repetitive operation with workbench together, obtains
If to the dried layer carbon ceramic composite material layer overlapped, if the dried layer carbon ceramic composite material that will be overlapped by way of suture
Layer fixation obtains carbon ceramic composite material precast body, puts it into graphite jig, and graphite jig is put into vacuum high-temperature sintering
It it is 1500 DEG C in temperature, after pressure keeps the temperature 30min under conditions of being 200MPa, epoxy resin is herein under argon gas protection in stove
Under the conditions of carbonize after carbon content be 50%, remove pressure, when vacuum high-temperature sintering furnace temperature is down to less than 200 DEG C, can general
Obtained carbon ceramic composite material takes out.
Embodiment 2
The pretreatment of carbon fiber：Phenolic resin is dissolved in mass fraction is obtained in the solution of n-hexane 500ml as 40%
Impregnated carbon fiber, is obtained pretreatment carbon fiber by binding paste in binding paste.
The preparation of ceramic powder：364g polycrystalline silica flours are made silicon powder particle, 74g tar asphalts and 50g carbon blacks to mix
It is even.
Input setting program in the operating system of 3D printer, pretreatment carbon fiber sustainable supply a to printhead,
Printhead drives pretreatment of fiber to be woven to obtain netted pretreatment of fiber layer according to setting program, meanwhile, ceramic powder
Ceramic powder is filled in netted pretreatment carbon fiber layer by sustainable supply to another printhead, the printhead according to setting program
Gap in, thus print the pretreatment carbon fiber layer filled with ceramic powder, i.e. carbon ceramic composite material layer, complete one layer
Afterwards, lifting gear declines the thickness of a layering, two printheads and lifting gear repetitive operation with workbench together, obtains
If the dried layer carbon ceramic composite material layer overlapped, if the dried layer carbon ceramic composite material layer that will be overlapped by way of suture
Fixation obtains carbon ceramic composite material precast body, puts it into graphite jig, and graphite jig is put into vacuum high-temperature sintering stove
In, it is 1800 DEG C in temperature, after pressure keeps the temperature 3h under conditions of being 150MPa, phenolic resin is in this condition under argon gas protection
Carbon content after lower charing is 65%, removes pressure, when vacuum high-temperature sintering furnace temperature is down to below 200 DEG C, will can obtain
Carbon ceramic composite material take out.
Embodiment 3
The pretreatment of carbon fiber：Modified coal tar pitch is dissolved in the bonding for obtaining that mass fraction is 10% in gasoline solution 500ml
Impregnated carbon fiber, is obtained pretreatment carbon fiber by slurry in binding paste.
The preparation of ceramic powder：336g polycrystalline silica flours are made silicon powder particle, 120g carbon blacks and 14g modified coal tar pitches to mix
Even granulation.
Input setting program in the operating system of 3D printer, pretreatment carbon fiber sustainable supply a to printhead,
Printhead drives pretreatment of fiber to be woven to obtain netted pretreatment of fiber layer according to setting program, meanwhile, ceramic powder
Ceramic powder is filled in netted pretreatment carbon fiber layer by sustainable supply to another printhead, the printhead according to setting program
Gap in, thus print the pretreatment carbon fiber layer filled with ceramic powder, i.e. carbon ceramic composite material layer, complete one layer
Afterwards, lifting gear declines the thickness of a layering, two printheads and lifting gear repetitive operation with workbench together, obtains
If the dried layer carbon ceramic composite material layer overlapped, if the dried layer carbon ceramic composite material layer that will be overlapped by way of suture
Fixation obtains carbon ceramic composite material precast body, puts it into graphite jig, and graphite jig is put into vacuum high-temperature sintering stove
In, it is 1560 DEG C in temperature, after pressure keeps the temperature 1h under conditions of being 30MPa, modified coal tar pitch is on this condition under argon gas protection
Carbon content after charing is 60%, remove pressure, when vacuum high-temperature sintering furnace temperature is down to below 200 DEG C, will can be obtained
Carbon ceramic composite material takes out.
Embodiment 4
The pretreatment of carbon fiber：Modified coal tar pitch is dissolved in the bonding for obtaining that mass fraction is 30% in gasoline solution 500ml
Impregnated carbon fiber, is obtained pretreatment carbon fiber by slurry in binding paste.
The preparation of ceramic powder：294g polycrystalline silica flours are made silicon powder particle, 120g carbon blacks and 8.5g epoxy resin to mix
Uniformly it is granulated.
Input setting program in the operating system of 3D printer, pretreatment carbon fiber sustainable supply a to printhead,
Printhead drives pretreatment of fiber to be woven to obtain netted pretreatment of fiber layer according to setting program, meanwhile, ceramic powder
Ceramic powder is filled in netted pretreatment carbon fiber layer by sustainable supply to another printhead, the printhead according to setting program
Gap in, thus print the pretreatment carbon fiber layer filled with ceramic powder, i.e. carbon ceramic composite material layer, complete one layer
Afterwards, lifting gear declines the thickness of a layering, two printheads and lifting gear repetitive operation with workbench together, obtains
If the dried layer carbon ceramic composite material layer overlapped, if the dried layer carbon ceramic composite material layer that will be overlapped by way of suture
Fixation obtains carbon ceramic composite material precast body, puts it into graphite jig, and graphite jig is put into vacuum high-temperature sintering stove
In, temperature be 1780 DEG C, pressure be 180MPa under conditions of keep the temperature 2.5h after, modified coal tar pitch carbonize on this condition after contain
Charcoal amount is 55%, removes pressure, and when vacuum high-temperature sintering furnace temperature is down to below 200 DEG C, can make pottery obtained carbon composite wood
Material takes out.
Embodiment 5
The pretreatment of carbon fiber：Modified coal tar pitch is dissolved in the bonding for obtaining that mass fraction is 10% in gasoline solution 500ml
Impregnated carbon fiber, is obtained pretreatment carbon fiber by slurry in binding paste.
The preparation of ceramic powder：Silicon powder particle, 120g carbon blacks, 24.3g modified coal tar pitches and boron is made in 336g polycrystalline silica flours
9.8g is uniformly mixed granulation.
Input setting program in the operating system of 3D printer, pretreatment carbon fiber sustainable supply a to printhead,
Printhead drives pretreatment of fiber to be woven to obtain netted pretreatment of fiber layer according to setting program, meanwhile, ceramic powder
Ceramic powder is filled in netted pretreatment carbon fiber layer by sustainable supply to another printhead, the printhead according to setting program
Gap in, thus print the pretreatment carbon fiber layer filled with ceramic powder, i.e. carbon ceramic composite material layer, complete one layer
Afterwards, lifting gear declines the thickness of a layering, two printheads and lifting gear repetitive operation with workbench together, obtains
If the dried layer carbon ceramic composite material layer overlapped, if the dried layer carbon ceramic composite material layer that will be overlapped by way of suture
Fixation obtains carbon ceramic composite material precast body, puts it into graphite jig, and graphite jig is put into vacuum high-temperature sintering stove
In, temperature be 1560 DEG C, pressure be 30MPa under conditions of keep the temperature 1h after, modified coal tar pitch carbonize on this condition after contain charcoal
Measure as 60%, remove pressure, when vacuum high-temperature sintering furnace temperature is down to below 200 DEG C, the carbon ceramic composite material that will can obtain
Take out.
Embodiment 6
The pretreatment of carbon fiber：Epoxy resin is dissolved in the binding paste for obtaining that mass fraction is 5% in acetone soln, will
Impregnated carbon fiber obtains pretreatment carbon fiber in binding paste.
The preparation of ceramic powder：Silicon powder particle is made in 308g polycrystalline silica flours and 122g activated carbons are uniformly mixed.
Input setting program in the operating system of 3D printer, pretreatment carbon fiber sustainable supply a to printhead,
Printhead drives pretreatment of fiber to be woven to obtain netted pretreatment of fiber layer according to setting program, meanwhile, ceramic powder
Ceramic powder is filled in netted pretreatment carbon fiber layer by sustainable supply to another printhead, the printhead according to setting program
Gap in, thus print the pretreatment carbon fiber layer filled with ceramic powder, i.e. carbon ceramic composite material layer, complete one layer
Afterwards, lifting gear declines the thickness of a layering, two printheads and lifting gear repetitive operation with workbench together, obtains
If the dried layer carbon ceramic composite material layer overlapped, if the dried layer carbon ceramic composite material layer that will be overlapped by way of suture
Fixation obtains carbon ceramic composite material precast body, puts it into graphite jig, and graphite jig is put into vacuum high-temperature sintering stove
In, argon gas protection under, in temperature be 1500 DEG C under the conditions of keep the temperature 30min after, epoxy resin carbonize on this condition after contain
Charcoal amount is 50%, removes pressure, and when vacuum high-temperature sintering furnace temperature is down to below 200 DEG C, can make pottery obtained carbon composite wood
Material takes out.
Embodiment 7
The pretreatment of carbon fiber：Modified coal tar pitch is dissolved in the bonding for obtaining that mass fraction is 10% in gasoline solution 500ml
Impregnated carbon fiber, is obtained pretreatment carbon fiber by slurry in binding paste.
The preparation of ceramic powder：Silicon powder particle, 120g carbon blacks, 24.3g modified coal tar pitches and boron is made in 336g polycrystalline silica flours
9.8g is uniformly mixed granulation.
Input setting program in the operating system of 3D printer, pretreatment carbon fiber sustainable supply a to printhead,
Printhead sprays pretreatment of fiber and is woven to obtain netted carbon fiber precast body according to setting program, meanwhile, ceramic powder
Ceramic powder is filled in netted carbon fiber precast body by sustainable supply to another printhead, the printhead according to setting program
In gap, carbon ceramic composite material precast body is thus printed, is put it into graphite jig, and graphite jig is put into vacuum height
It it is 1560 DEG C in temperature, after pressure keeps the temperature 1h under conditions of being 10MPa, modified coal tar pitch carbonizes on this condition in warm sintering furnace
Carbon content afterwards is 60%, removes pressure, when vacuum high-temperature sintering furnace temperature is down to below 200 DEG C, obtained carbon can be made pottery
Composite material takes out.
Embodiment 8
The pretreatment of carbon fiber：Modified coal tar pitch is dissolved in the bonding for obtaining that mass fraction is 10% in gasoline solution 500ml
Impregnated carbon fiber, is obtained pretreatment carbon fiber by slurry in binding paste.
The preparation of ceramic powder：Silicon powder particle, 120g carbon blacks, 24.8g modified coal tar pitches and boron is made in 336g polycrystalline silica flours
It is granulated 14.8g being uniformly mixed.
Pretreatment carbon fiber is woven to obtain netted pretreatment carbon fiber fibrous layer, ceramic powder is filled in institute
In the gap for stating pretreatment carbon fiber layer, carbon ceramic composite material layer is formed, repeats to weave and fills, if obtaining multiple by dried layer carbon pottery
The carbon ceramic composite material precast body that condensation material overlaps to form, puts it into graphite jig, and graphite jig is put into vacuum height
It is 1560 DEG C in temperature in warm sintering furnace, after pressure keeps the temperature 0.5h under conditions of being 30MPa, modified coal tar pitch charcoal on this condition
Carbon content after change is 60%, removes pressure, when vacuum high-temperature sintering furnace temperature is down to below 200 DEG C, the carbon that will can obtain
Ceramic composite material takes out.
Embodiment 9
The pretreatment of carbon fiber：Phenolic resin is dissolved in mass fraction is obtained in the solution of n-hexane 500ml as 40%
Impregnated carbon fiber, is obtained pretreatment carbon fiber by binding paste in binding paste.
The preparation of ceramic powder：Silicon powder particle is made in 364g polycrystalline silica flours, 277g tar asphalts are uniformly mixed.
Pretreatment carbon fiber is woven to obtain netted pretreatment carbon fiber fibrous layer, ceramic powder is filled in institute
In the gap for stating pretreatment carbon fiber layer, carbon ceramic composite material layer is formed, repeats to work out and fills, if obtaining multiple by dried layer carbon pottery
The carbon ceramic composite material precast body that condensation material overlaps to form, puts it into graphite jig, and graphite jig is put into vacuum height
It is 1800 DEG C in temperature in warm sintering furnace, after pressure keeps the temperature 0.5h under conditions of being 30MPa, phenolic resin charcoal on this condition
Carbon content after change is 65%, removes pressure, when vacuum high-temperature sintering furnace temperature is down to below 200 DEG C, the carbon that will can obtain
Ceramic composite material takes out.
Comparative example 1
Using preparation method in embodiment 3 in Chinese patent literature CA106927847A, carbon fibre reinforced silicon carbide is prepared
Ceramic composite, wherein ceramic powder select silicon carbide powder, and continuous reinforcing fiber selects carbon fiber.
Experimental example 1
The carbon ceramic composite material that embodiment 1-6 and comparative example are obtained is tested, the results are shown in Table 1：
Table 1
Obviously, the above embodiments are merely examples for clarifying the description, and the restriction not to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of change or
Change.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (13)
1. a kind of preparation method of carbon ceramic composite material, it is characterised in that include the following steps：
(1) pretreatment carbon fiber is obtained in carbon fiber surface cladding binding paste, wherein, the binding paste is dissolved by binding agent
It is made in solvent；
(2) ceramic powder containing carbon dust and silica flour is prepared, the wherein molar ratio of silicon and carbon is more than 1: 1；
(3) the pretreatment carbon fiber is woven to obtain netted pretreatment carbon fiber precast body, by the ceramic powder
It is filled in the gap of the netted pretreatment carbon fiber precast body, forms carbon ceramic composite material precast body；
(4) sinter the carbon ceramic composite material precast body and obtain carbon ceramic composite material.
2. the preparation method of carbon ceramic composite material according to claim 1, it is characterised in that the step (3) includes, right
The pretreatment carbon fiber is woven to obtain netted pretreatment carbon fiber layer, and the ceramic powder is filled in the pre- place
In the gap for managing carbon fiber layer, carbon ceramic composite material layer is formed；Repetitive operation, if obtaining overlapping by dried layer carbon ceramic composite material layer
The carbon ceramic composite material precast body of formation.
3. the preparation method of carbon ceramic composite material according to claim 1, it is characterised in that in the step (1), with matter
Percentage meter is measured, the concentration of the binding paste is 5%-40%, and the binding agent is epoxy resin, phenolic resin or modification drip
One or more in green grass or young crops.
4. the preparation method of carbon ceramic composite material according to claim 3, it is characterised in that described in the step (1)
Solvent is acetone, n-hexane or gasoline.
5. according to the preparation method of any carbon ceramic composite materials of claim 1-4, it is characterised in that the step (4)
In, the temperature of sintering is 1500-1800 DEG C, time 0.5h-3.0h.
6. the preparation method of carbon ceramic composite material according to claim 5, it is characterised in that in the step (4), sintering
Pressure be 10MPa-200MPa.
7. according to the preparation method of any carbon ceramic composite materials of claim 1-6, it is characterised in that the step (2)
In, the ceramic powder further includes the binding agent for accounting for the ceramic powder gross mass 2%-5%.
8. according to the preparation method of any carbon ceramic composite materials of claim 1-7, it is characterised in that the ceramic powder
The one or more in pure boron, diboron trioxide or boric acid are further included, wherein, boron accounts for the 1%- of the ceramic powder gross mass
3%.
9. according to the preparation method of any carbon ceramic composite materials of claim 1-8, it is characterised in that the ceramic powder
In carbon dust be activated carbon, tar asphalt, furane resins, phenolic resin or carbon black in one or more.
10. according to the preparation method of any carbon ceramic composite materials of claim 1-9, it is characterised in that the ceramic powder
Silica flour in body is polycrystalline silica flour.
11. according to the preparation method of any carbon ceramic composite materials of claim 1-10, it is characterised in that the preparation side
Method is 3D printing method, including,
(1) it is described pretreatment carbon fiber sustainable supply at least one printhead, meanwhile, the ceramic powder sustainable supply arrives it
Remaining printhead；
(2) according to setting program, printhead sprays the pretreatment carbon fiber, and braiding obtains netted pretreatment prefabricated carbon fiber
The ceramic powder is filled in the gap of netted pretreatment carbon fiber precast body, thus prints by body, remaining printhead
Carbon ceramic composite material precast body；
(3) sinter the carbon ceramic composite material precast body and obtain carbon ceramic composite material.
12. the preparation method of carbon ceramic composite material according to claim 11, it is characterised in that the step (2) includes,
According to setting program, printhead sprays the pretreatment carbon fiber, and braiding obtains netted pretreatment carbon fiber layer, remaining printing
The ceramic powder is filled in the gap of netted pretreatment carbon fiber by head, is thus printed filled with the pre- of ceramic powder
Treatment of Carbon layer, i.e. carbon ceramic composite material layer；Repetitive operation, if obtaining the carbon overlapped to form by dried layer carbon ceramic composite material layer
Ceramic composite material precast body.
The composite wood 13. carbon that a kind of preparation method by any carbon ceramic composite materials of claim 1-12 is prepared is made pottery
Material.
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