CN107500769B - C/TiB2Surface treatment method of composite material - Google Patents
C/TiB2Surface treatment method of composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 76
- 229910033181 TiB2 Inorganic materials 0.000 claims abstract description 39
- 238000004381 surface treatment Methods 0.000 claims abstract description 20
- 239000011812 mixed powder Substances 0.000 claims abstract description 15
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 14
- 239000004917 carbon fiber Substances 0.000 claims abstract description 14
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 11
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 11
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 17
- 239000010936 titanium Substances 0.000 claims description 14
- 239000011863 silicon-based powder Substances 0.000 claims description 13
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 12
- 239000005011 phenolic resin Substances 0.000 claims description 12
- 229920001568 phenolic resin Polymers 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000000498 ball milling Methods 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000000748 compression moulding Methods 0.000 claims description 5
- 238000000280 densification Methods 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 238000005475 siliconizing Methods 0.000 claims description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 238000013329 compounding Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 abstract description 11
- 229910008484 TiSi Inorganic materials 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract description 2
- 239000011226 reinforced ceramic Substances 0.000 abstract description 2
- 230000000087 stabilizing effect Effects 0.000 abstract description 2
- 229910052710 silicon Inorganic materials 0.000 description 9
- 239000000463 material Substances 0.000 description 5
- 238000005728 strengthening Methods 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 229910008479 TiSi2 Inorganic materials 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000003733 fiber-reinforced composite Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002289 liquid silicon infiltration Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
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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
- C04B35/563—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 boron carbide
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
- C04B41/5133—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal with a composition mainly composed of one or more of the refractory metals
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
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- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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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
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
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Abstract
The invention belongs to the surface of a carbon fiber reinforced ceramic matrix compositeThe field of treatment, in particular to a C/TiB2A surface treatment method of composite material. With B4C powder embedded C/TiB2Treating the composite material at 950-1100 ℃ in vacuum; mixing Ti powder and NH4Cl、Al2O3Uniformly mixing the powder to obtain mixed powder; embedding treated C/TiB with the resulting mixed powder2And (3) reacting the composite material for 3-5 hours at the temperature of 1200-1300 ℃ in vacuum, and then naturally cooling. The method of the invention firstly deposits a layer B on the surface of the composite material4C, then obtaining TiSi by reacting Ti powder with residual silicon2And at the same time can be connected with surface B4C reacting to obtain TiB2Further stabilizing the properties of the composite material.
Description
Technical Field
The invention belongs to the field of surface treatment of carbon fiber reinforced ceramic matrix composite materials, and particularly relates to C/TiB2A surface treatment method of composite material.
Background
TiB2The boride ceramic which is expected to be widely applied due to excellent performance has good conductivity, high melting point, hardness and corrosion resistance, so that the boride ceramic has wide application in the aspects of manufacturing evaporation vessels, molten metal crucibles, cathodes of aluminum electrolysis cells, spark plugs, other electrodes, materials of contact switches and the like; after the composite material is compounded with a carbon material, the ablation resistance is improved, and the composite material has the characteristics of small material specific gravity, high thermal shock stability, good conductivity and friction and wear resistance, is low in preparation cost, and is a carbon/ceramic composite material with excellent performance.
Often in the actual preparation process for enhancing C/TiB2The densification degree of the silicon-based alloy needs to be siliconized, and the liquid silicon infiltration method has the advantages of simple process, short preparation period, low cost, near net shape, easy industrial production and the like, so that related research is greatly influenced at home and abroadThere is a great concern. Studies have shown that residual Si content affects C/TiB2And the high-temperature mechanical property and the oxidation resistance of the composite material. When the volume fraction of the residual Si is high, part of the fibers can be corroded by silicon, and meanwhile, the fibers have large volume expansion and more cracks, so that the material is easy to expand along the cracks when stressed, and the mechanical property is poor. However, the treatment of the residual silicon is less researched at present, and although research shows that the silicon can be removed by corrosion with concentrated mixed acid, the method has the defect of easy damage to the composite material. Therefore, a surface treatment method for fiber reinforced composite materials is needed to reduce the content of residual Si on the basis of ensuring the excellent mechanical properties of the composite materials.
Disclosure of Invention
The invention aims to provide a C/TiB2A surface treatment method for composite material includes depositing a layer B on the surface of composite material4C, then obtaining TiSi by reacting Ti powder with residual silicon2And at the same time can be connected with surface B4C reacting to obtain TiB2Further stabilizing the properties of the composite material.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
C/TiB2Method for surface treatment of composite material, said C/TiB2The composite material is C/TiB prepared by melt siliconizing densification treatment2The composite material comprises the following processing steps:
(1) with B4C powder embedded C/TiB2Treating the composite material at 900-1100 ℃ in vacuum;
(2) mixing Ti powder and NH4Cl、Al2O3Uniformly mixing the powder to obtain mixed powder;
(3) embedding the C/TiB treated in the step (1) with the mixed powder obtained in the step (2)2And (3) reacting the composite material for 3-5 hours at the temperature of 1200-1300 ℃ in vacuum, and then naturally cooling.
Preferably, in the step (1), the treatment time is 5-6 h.
Preferably, in the step (2), the Ti powder and NH are4Cl、Al2O3The mass ratio of (1) to (12-22) is (75-85) to (3) to (12-85); placing the three into a ball milling tank, and carrying out ball milling for 0.5-1 h to obtain mixed powder.
In the present invention, C/TiB2The composite material can be prepared by one of the following two methods.
The first method comprises the following steps:
(A) dispersing the liquid phenolic resin in absolute ethyl alcohol, and ensuring that the content of the liquid phenolic resin in the dispersion liquid is 5-12 wt%;
(B) press against TiB2The mass ratio of the powder to the absolute ethyl alcohol is (0.5-1.2): 1, and TiB is added2Adding the powder into the solution obtained in the step (A), and uniformly stirring at 40-60 ℃;
(C) carbon fiber powder and TiB2Adding carbon fiber powder into the solution obtained in the step (B) according to the mass ratio of (0.1-0.2): 1, and continuously stirring at 60-80 ℃ until the slurry is viscous and cannot be stirred;
(D) drying the slurry, granulating and sieving, putting the obtained granular powder into a mould, and performing compression molding to obtain a blank body;
(E) coating the blank with silicon powder or a composition of the silicon powder and the titanium powder, placing the blank in a graphite crucible, and reacting for 1-3 hours at 1550-1650 ℃ in vacuum to obtain C/TiB2A composite material.
The second method comprises the following steps:
(I) dispersing the liquid phenolic resin in absolute ethyl alcohol, and ensuring that the content of the liquid phenolic resin in the dispersion liquid is 2-5 wt%;
(II) mixing TiO2Powder and B4Adding the powder C into the solution obtained in the step (I), and uniformly stirring at 40-60 ℃; wherein the TiO is2Powder and B4The mass ratio of the total amount of the C powder to the absolute ethyl alcohol is (0.5-1.2) to 1, and TiO2Powder and B4The mass ratio of the C powder is (1.2-2.8) to 1;
(III) carbon fiber powder and TiO2Adding carbon fiber powder into the solution obtained in the step (II) according to the mass ratio of (0.07-0.14) to 1, and continuously stirring at 60-80 ℃ until the slurry is viscous and cannot be stirred;
(IV) drying the slurry, granulating and sieving, putting the obtained granular powder into a mould, and performing compression molding to obtain a blank body;
(V) reacting and sintering the blank obtained in the step (IV) for 2-3 h at the temperature of 1800-1900 ℃ in vacuum to obtain C/TiB2Compounding the green body;
(VI) composition C/TiB using silicon powder or both silicon powder and titanium powder2Placing the composite blank in a graphite crucible, and reacting for 1-3 h at 1550-1650 ℃ in vacuum to obtain C/TiB2A composite material.
Preferably, the solid content of the liquid phenolic resin is more than or equal to 50 wt%.
Preferably, the length of the carbon fiber powder is 30-50 μm.
Preferably, the drying temperature is 60-100 ℃.
Preferably, the powder is sieved by a sieve of 60-100 meshes.
Preferably, the pressure of the compression molding is controlled to be 150-250 MPa.
Preferably, when the silicon powder and the titanium powder are combined, the mass ratio of the silicon powder to the titanium powder is (1.8-2.5) to 1.
The invention provides a C/TiB2The surface treatment method of the composite material realizes the treatment of C/TiB by using a two-step method2Removing residual silicon on the surface of the composite material by firstly removing C/TiB2Composite material surface deposition B4C powder, then Ti powder is used to remove residual silicon, and the residual silicon reacts with the C powder to generate TiSi2In which Al is used2O3The powder is used for reducing the activity of Ti powder at high temperature, NH4Cl is used for dispersing powder and preventing agglomeration, so that the mechanical property of the composite material is improved, and meanwhile, Ti powder and B can also be mixed4C reaction to produce TiB2The performance of the composite material is further stabilized, the densification degree is improved, and the surface strengthening treatment of the material is realized.
Detailed Description
The present invention will be further described with reference to the following specific examples. It should be understood that the following examples are illustrative only and are not intended to limit the scope of the present invention.
Example 1
The preparation of C/TiB was carried out as follows2The composite material comprises the following steps:
(I) dispersing liquid phenolic resin (solid content is 50 wt%) in absolute ethyl alcohol, and ensuring that the content of the liquid phenolic resin in the dispersion liquid is 2 wt%;
(II) mixing TiO2Powder and B4Adding the powder C into the solution obtained in the step (I), and uniformly stirring at 40 ℃; wherein the TiO is2Powder and B4The mass ratio of the total amount of the C powder to the absolute ethyl alcohol is 1: 1, and the TiO powder2Powder and B4The mass ratio of the C powder is 1.2: 1;
(III) mixing carbon fiber powder (with a length of 45 mu m) and TiO2Adding carbon fiber powder into the solution obtained in the step (II) according to the mass ratio of the powder of 0.14: 1, and continuously stirring at 60 ℃ until the slurry is viscous and cannot be stirred;
(IV) placing the slurry in a drying box, and drying at 90 ℃; after granulation and 100-mesh sieve, placing the powder particles in a mould, and pressing under 180MPa to form a blank;
(V) reacting and sintering the blank obtained in the step (4) for 2 hours at the temperature of 1800 ℃ in vacuum to obtain C/TiB2Compounding the green body;
(VI) coating C/TiB with mixed powder of silicon powder and titanium powder (the mass ratio of Si to Ti is 1.8: 1)2Placing the composite blank in a graphite crucible, keeping the temperature at 1550 ℃ in vacuum for 2h to increase densification, and naturally cooling to obtain the C/TiB2A composite material.
The C/TiB prepared by the method2The composite material is subjected to surface treatment, and the treatment steps are as follows:
(1) with B4C powder is used for embedding C/TiB obtained by siliconizing2Reacting the composite material for 6 hours at the temperature of 950 ℃ in vacuum, and strengthening the surface of the composite material;
(2) ti powder and NH in a mass ratio4Cl∶Al2O3= 80: 3: 17, mixing Ti powder and NH4Cl、Al2O3Placing the powder in a ball milling tank, and carrying out ball milling for 45min to obtain mixed powder;
(3) using the step (a)2) The obtained mixed powder is embedded with the C/TiB treated in the step (1)2The composite material is reacted for 4 hours at the temperature of 1200 ℃ in vacuum, and then naturally cooled.
Example 2
C/TiB2The composite was prepared as in example 1.
C/TiB2The surface treatment steps of the composite material are as follows:
(1) with B4C powder is used for embedding C/TiB obtained by siliconizing2Reacting the composite material for 5 hours at the temperature of 1000 ℃ in vacuum, and strengthening the surface of the composite material;
(2) ti powder and NH in a mass ratio4Cl∶Al2O3= 85: 3: 12, mixing Ti powder and NH4Cl、Al2O3Placing the powder in a ball milling tank, and carrying out ball milling for 60min to obtain mixed powder;
(3) embedding the C/TiB treated in the step (1) with the mixed powder obtained in the step (2)2The composite material is reacted for 3 hours at the temperature of 1300 ℃ in vacuum, and then naturally cooled.
Example 3
C/TiB2The composite was prepared as in example 1.
C/TiB2The surface treatment steps of the composite material are as follows:
(1) with B4C powder is used for embedding C/TiB obtained by siliconizing2Reacting the composite material for 5.5 hours at the temperature of 900 ℃ in vacuum, and strengthening the surface of the composite material;
(2) ti powder and NH in a mass ratio4Cl∶Al2O3= 75: 3: 22, mixing Ti powder and NH4Cl、Al2O3Placing the powder in a ball milling tank, and carrying out ball milling for 30min to obtain mixed powder;
(3) embedding the C/TiB treated in the step (1) with the mixed powder obtained in the step (2)2The composite material is reacted for 5 hours at the temperature of 1250 ℃ in vacuum, and then naturally cooled.
C/TiB2The residual silicon content and the performance data of the composite material before and after the treatment by the method of the invention are shown in the following table.
From the above table, it can be seen that: the method of the invention not only reduces C/TiB2The residual silicon content of the composite material also realizes C/TiB2And the mechanical property of the composite material is improved.
Claims (10)
1. C/TiB2A method for surface treatment of a composite material, characterized in that the C/TiB is2The composite material is C/TiB prepared by melt siliconizing densification treatment2The composite material comprises the following processing steps:
(1) with B4C powder embedded C/TiB2Treating the composite material at 900-1100 ℃ in vacuum;
(2) mixing Ti powder and NH4Cl、Al2O3Uniformly mixing the powder according to the mass ratio of (75-85) to (3) to (12-22) to obtain mixed powder;
(3) embedding the C/TiB treated in the step (1) with the mixed powder obtained in the step (2)2And (3) reacting the composite material for 3-5 hours at the temperature of 1200-1300 ℃ in vacuum, and then naturally cooling.
2. The surface treatment method according to claim 1, characterized in that: in the step (1), the treatment time is 5-6 h.
3. The surface treatment method according to claim 1, characterized in that: in the step (2), Ti powder and NH are added4Cl、Al2O3The three are placed in a ball milling tank, and ball milling is carried out for 0.5-1 h to obtain mixed powder.
4. The surface treatment method according to claim 1, wherein C/TiB2The preparation process of the composite material comprises the following steps:
(A) dispersing the liquid phenolic resin in absolute ethyl alcohol, and ensuring that the content of the liquid phenolic resin in the dispersion liquid is 5-12 wt%;
(B) press against TiB2The mass ratio of the powder to the absolute ethyl alcohol is (0.5-1.2): 1, and TiB is added2Adding the powder into the solution obtained in the step (A), and uniformly stirring at 40-60 ℃;
(C) carbon fiber powder and TiB2Adding carbon fiber powder into the solution obtained in the step (B) according to the mass ratio of (0.1-0.2): 1, and continuously stirring at 60-80 ℃ until the slurry is viscous and cannot be stirred;
(D) drying the slurry, granulating and sieving, putting the obtained granular powder into a mould, and performing compression molding to obtain a blank body;
(E) coating the blank with silicon powder or a composition of the silicon powder and the titanium powder, placing the blank in a graphite crucible, and reacting for 1-3 hours at 1550-1650 ℃ in vacuum to obtain C/TiB2A composite material.
5. The surface treatment method according to claim 1, wherein C/TiB2The preparation process of the composite material comprises the following steps:
(I) dispersing the liquid phenolic resin in absolute ethyl alcohol, and ensuring that the content of the liquid phenolic resin in the dispersion liquid is 2-5 wt%;
(II) mixing TiO2Powder and B4Adding the powder C into the solution obtained in the step (I), and uniformly stirring at 40-60 ℃; wherein the TiO is2Powder and B4The mass ratio of the total amount of the C powder to the absolute ethyl alcohol is (0.5-1.2) to 1, and TiO2Powder and B4The mass ratio of the C powder is (1.2-2.8) to 1;
(III) carbon fiber powder and TiO2Adding carbon fiber powder into the solution obtained in the step (II) according to the mass ratio of (0.07-0.14) to 1, and continuously stirring at 60-80 ℃ until the slurry is viscous and cannot be stirred;
(IV) drying the slurry, granulating and sieving, putting the obtained granular powder into a mould, and performing compression molding to obtain a blank body;
(V) reacting and sintering the blank obtained in the step (IV) for 2-3 h at the temperature of 1800-1900 ℃ in vacuum to obtain C/TiB2Compounding the green body;
(VI) using silicon powder or silicon powder and titanium powderComposition C/TiB of2Placing the composite blank in a graphite crucible, and reacting for 1-3 h at 1550-1650 ℃ in vacuum to obtain C/TiB2A composite material.
6. The surface treatment method according to claim 4 or 5, characterized in that: the solid content of the liquid phenolic resin is more than or equal to 50 wt%; the length of the carbon fiber powder is 30-50 mu m.
7. The surface treatment method according to claim 4 or 5, characterized in that: the drying temperature is 60-100 ℃.
8. The surface treatment method according to claim 4 or 5, characterized in that: sieving the powder by a sieve of 60-100 meshes.
9. The surface treatment method according to claim 4 or 5, characterized in that: the pressure of the pressing forming is controlled to be 150-250 MPa.
10. The surface treatment method according to claim 4 or 5, characterized in that: when the silicon powder and the titanium powder are combined, the mass ratio of the silicon powder to the titanium powder is (1.8-2.5) to 1.
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| CN108947536A (en) * | 2018-07-05 | 2018-12-07 | 重庆文理学院 | A kind of high-densit B-Ti-C system ceramics of strong ultrasonic wave added method preparation even tissue |
| CN110282977B (en) * | 2019-06-17 | 2021-01-08 | 东北大学 | B4C/TiB2Preparation method of layered composite ceramic material |
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| CN114315367B (en) * | 2021-12-28 | 2023-03-17 | 北京理工大学 | Titanium diboride-boron carbide-titanium carbide composite ceramic material and hot-pressing preparation method thereof |
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| JPS61146775A (en) * | 1984-12-18 | 1986-07-04 | 日立化成工業株式会社 | Carbon fiber reinforced carbon material |
| CN102424597A (en) * | 2011-09-26 | 2012-04-25 | 宁波伏尔肯机械密封件制造有限公司 | Preparation method of C/C-SIC ceramic composite material |
| CN103288468A (en) * | 2013-05-14 | 2013-09-11 | 大连理工大学 | Preparation method for fiber reinforced carbon-silicon carbide-zirconium carbide-based composite material |
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| JPS61146775A (en) * | 1984-12-18 | 1986-07-04 | 日立化成工業株式会社 | Carbon fiber reinforced carbon material |
| CN102424597A (en) * | 2011-09-26 | 2012-04-25 | 宁波伏尔肯机械密封件制造有限公司 | Preparation method of C/C-SIC ceramic composite material |
| CN103288468A (en) * | 2013-05-14 | 2013-09-11 | 大连理工大学 | Preparation method for fiber reinforced carbon-silicon carbide-zirconium carbide-based composite material |
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