CN107573076B - High-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece - Google Patents

High-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece Download PDF

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CN107573076B
CN107573076B CN201710838753.3A CN201710838753A CN107573076B CN 107573076 B CN107573076 B CN 107573076B CN 201710838753 A CN201710838753 A CN 201710838753A CN 107573076 B CN107573076 B CN 107573076B
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silicon carbide
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李双
魏春城
刘爱菊
孟子霖
张茜
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Shandong University of Technology
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Abstract

The invention relates to a composite ceramic, in particular to a high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece, belonging to the technical field of ceramic materials. The composition phase of the heterogeneous ceramic special-shaped piece comprises a titanium silicon carbide phase, a silicon carbide phase and a silicon phase, wherein the content of the titanium silicon carbide phase accounts for 15-25% of the total mass of the heterogeneous ceramic special-shaped piece, the content of the silicon carbide phase accounts for 65-85% of the total mass of the heterogeneous ceramic special-shaped piece, and the balance is the silicon phase. The complex phase ceramic special-shaped piece comprises the following components in percentage by mass: 50-60% of carbon black, 25-35% of titanium carbide powder, 10-15% of titanium powder, 1-3% of dispersing agent and 3-5% of plasticizer. The titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece has higher density, good mechanical property, and particularly higher bending strength and fracture toughness.

Description

High-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece
Technical Field
The invention relates to a composite ceramic, in particular to a high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece, belonging to the technical field of ceramic materials.
Background
The silicon carbide ceramic material has excellent performances of light weight, high strength, good heat conductivity, low expansion coefficient, high hardness, oxidation resistance and the like, and has very good dimensional stability in severe environmental disturbance including severe changes of temperature and humidity or exposure to corrosive and other environments in which chemical reactions are easy to occur, so that the silicon carbide ceramic material is widely applied to industries of aviation, aerospace, automobiles, machinery, petrifaction, metallurgy, electronics and the like. Most silicon carbide products belong to high value-added products, and the market prospect is wide, so the silicon carbide ceramic is valued by many countries and is always the key point of research in the material academia, and a researcher is concerned about how to prepare silicon carbide ceramic components with high toughness and complex shapes.
Silicon carbide is a compound with strong covalent bond (the covalent bond component accounts for 88%), the diffusion coefficient is quite low under the high-temperature sintering condition, and sintering is difficult to compact, so that a material with excellent mechanical property is difficult to prepare. The fracture toughness of single-phase silicon carbide ceramics is generally lower, and the problem is solved by a mode that short fibers, nano particles and the like are added in the material preparation process to be used as reinforcements to prepare composite materials in the industry at present; however, problems associated with fiber/particle agglomeration, high temperature damage, interfacial strength, etc. during introduction of the second phase reinforcement reduce its toughening effect. In addition, the common preparation methods of the silicon carbide ceramic at present mainly comprise hot pressing sintering, hot isostatic pressing sintering, reaction sintering, normal pressure sintering, chemical vapor deposition, vapor infiltration, polymer precursor conversion and the like. The sintering temperature of the sintering processes such as normal pressure sintering, hot pressing sintering, hot isostatic pressing sintering and the like reaches 2000 ℃, the sintering shrinkage rate is about 15%, and the preparation of the silicon carbide product with a complex shape is difficult to realize. Silicon carbide ceramics have high hardness and rigidity, high processing difficulty and long period, so that sintered products are required to have high dimensional accuracy.
The titanium silicon carbide has good thermal shock resistance, high conductivity, good oxidation resistance and high-temperature thermal stability, and reflects the dual advantages of metal and ceramic, so the titanium silicon carbide has good application prospect. Silicon titanium carbide is a material with typical plastic characteristics in ternary materials, has a layered structure similar to graphite, can obviously improve the expansion path in the crack propagation process, and is expected to prepare a structure and function integrated ceramic matrix composite material with excellent performance, so the silicon titanium carbide ceramic is a research hotspot in the field of ceramic materials.
Disclosure of Invention
The invention provides a complex phase ceramic material with excellent mechanical property in order to overcome the defects in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme: the composition phase of the multiphase ceramic special-shaped part comprises a titanium silicon carbide phase, a silicon carbide phase and a silicon phase, wherein the content of the titanium silicon carbide phase accounts for 15-25% of the total mass of the multiphase ceramic special-shaped part, the content of the silicon carbide phase accounts for 65-85% of the total mass of the multiphase ceramic special-shaped part, and the balance is the silicon phase.
The content of the titanium silicon carbide can influence the performance of the silicon carbide complex phase ceramic, and the silicon carbide complex phase ceramic has better comprehensive performances such as strength, toughness, hardness and the like in the range; the titanium silicon carbide has a graphite-like layered structure, and a crack propagation path is bent in the fracture process, so that a large amount of fracture energy can be consumed, so that the strength, toughness and other parameters of the complex-phase ceramic are improved due to the increase of the content, but the hardness of the titanium silicon carbide is lower, and the hardness parameter of the complex-phase ceramic can be obviously reduced when the content is too high.
In the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece, the complex phase ceramic special-shaped piece comprises the following components in percentage by mass: 50-60% of carbon black, 25-35% of titanium carbide powder, 10-15% of titanium powder, 1-3% of dispersing agent and 3-5% of plasticizer.
Carbon black provides a carbon source in the complex phase ceramic special-shaped piece and reacts with liquid phase silicon to generate silicon carbide; when the content of the carbon black is too high (the content exceeds 60 percent), the carbon-silicon reaction is accompanied with obvious volume expansion, and microcracks are easy to generate in the complex phase ceramic, so that the mechanical properties such as strength, toughness and the like are reduced; when the carbon black is too low (the content is lower than 50%), the silicon content in the complex phase ceramic is increased, and the density and hardness of the complex phase ceramic are lower. Reacting titanium carbide and titanium powder with liquid-phase silicon to generate titanium silicon carbide; if the contents of titanium carbide and titanium powder are too high, the content of titanium silicon carbide is higher, and the hardness of the complex phase ceramic is insufficient; if the contents of titanium carbide and titanium powder are too low, the content of titanium silicon carbide is low, the complex phase ceramic lacks the strengthening and toughening effects of the lamellar reinforcement, and the strength and toughness are low. In the invention, the titanium carbide, the titanium powder and the carbon black need to be dispersed by adding a dispersing agent, so that the titanium carbide, the titanium powder and the carbon black exist in the form of single particles as much as possible. The preparation process requires that the blank after grouting forming has certain strength, and the strength is derived from the combination effect of the plasticizer; when the plasticizer content is low, the strength of the blank is low, and the blank is easy to crack after being dried; when the content is too high, the moisture in the green body is slowly lost, and the drying period is longer. In the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped part, the mass ratio of titanium carbide powder to titanium powder is 2-3: 1. The titanium carbide powder, the titanium powder and the liquid-phase silicon react to generate titanium silicon carbide, in order to generate a proper amount of titanium silicon carbide phase, the mass ratio of the titanium carbide powder to the titanium powder needs to be strictly controlled at 2-3:1, otherwise the residual silicon carbide powder or the titanium powder can influence the performance of the multiphase ceramic special-shaped part.
In the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped part, the particle size of titanium carbide powder is 1-3 mu m. When the particle size of the titanium carbide powder is too large, the particle size of the generated titanium silicon carbide is larger, and the mechanical properties such as strength, toughness and the like of the material can be reduced; however, the submicron powder and the nanometer powder which are less than 1 micron have extremely high raw material cost.
In the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped part, the particle size of titanium powder is 2-5 mu m. When the particle size of the titanium powder is too large, the generated titanium silicon carbide has larger particle size, and the mechanical properties such as strength, toughness and the like of the material can be reduced; the raw material cost of titanium powder less than 2 microns is extremely high.
In the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece, the dispersing agent is one or more of polyvinyl alcohol, tetramethyl ammonium hydroxide, polyacrylic acid, ammonium citrate and polyethylene glycol, the dispersing medium is one or two of absolute ethyl alcohol and deionized water, and the dispersing mode is high-frequency ultrasonic dispersion.
In the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece, the plasticizer is one or more of sodium carboxymethylcellulose, epoxy resin, organic silicon and polyvinyl alcohol.
Preferably, the plasticizer is sodium carboxymethylcellulose, and the viscosity of the sodium carboxymethylcellulose is 800-1200 Pa.s. If the viscosity is too low, the binding force is affected, but the viscosity is higher, and the production cost is greatly increased, so through experimental research, the sodium carboxymethylcellulose with the viscosity of 800-1200 Pa.s can not only ensure lower production cost, but also ensure better binding force.
The invention also provides a preparation method of the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped part, which comprises the following steps:
1) uniformly dispersing carbon black, titanium carbide powder, titanium powder, a dispersing agent and a plasticizer in proportion, and then carrying out high-speed ball milling to obtain ceramic slurry;
2) slowly injecting the ceramic slurry into a gypsum mold after vacuum degassing, and drying to obtain a special-shaped blank;
3) and (3) moving the biscuit of the special-shaped part into a vacuum sintering furnace, uniformly spreading high-purity silicon powder above the biscuit, and then carrying out infiltration-reaction sintering at the sintering temperature of 1650-1700 ℃ for 1-2 hours to obtain the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped part.
The invention adopts the plaster mold, can mold parts with complex shapes, and only needs to process the required mold.
In the preparation method of the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped part, the medium for ball milling is high-hardness silicon carbide balls.
In the preparation method of the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped part, the surface of a gypsum mould is coated with a layer of coating, and the coating comprises the following components in parts by mass: 3-8 parts of microcrystalline wax, 3-5 parts of lanolin magnesium soap, 0.5-2 parts of modified water glass, 3-8 parts of rosin, 20-30 parts of solvent oil and 20-30 parts of mineral oil. According to the invention, the surface of the gypsum mould is covered by coating the coating with the reasonable formula, and the gypsum is separated from water and harmful components in the slurry by utilizing the hydrophobicity of an oil product, so that the contact probability of harmful substances in the slurry and the gypsum mould is reduced, and the occurrence of corrosion reaction is prevented. Meanwhile, the influence of the oil immersion on the water absorption performance of the surface of the mold is reduced as much as possible.
Preferably, the plaster mold comprises the following components in parts by mass: 20-30 parts of carbon fiber, 5-10 parts of silicate, 8-15 parts of rosin, 2-6 parts of phenolic resin, 2-8 parts of adhesive, 1-5 parts of quartz sand, 3-8 parts of sodium polyphosphate and 3-15 parts of water reducing agent. The invention further improves the density of the multiphase ceramic special-shaped piece by further improving the gypsum mould. The gypsum mold disclosed by the invention has the advantages that the strength, including dry compressive strength and wet compressive strength, of the gypsum mold is improved by adding a proper amount of carbon fiber and silicate. According to continuous research, the gypsum mold prepared from the conventional common calcium sulfate is easy to have fine cracks, and the gypsum mold disclosed by the invention is not only free from cracks, but also has the dry compressive strength increased by 35% and the wet compressive strength increased by 54% compared with the common gypsum mold. Further improving the density of the titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece after molding.
In the preparation method of the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped part, the silicon spreading amount above the biscuit is 1.2-1.4 times of the silicon amount required by silicon-carbon chemical reaction.
In the preparation method of the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped part, a hearth is vacuumized to 10-20 Pa when the temperature is lower than 800 ℃ in the sintering process, and argon or nitrogen is filled into the hearth when the temperature reaches above 800 ℃. The melting point of silicon is 1450 ℃, the liquid phase silicon is good in fluidity when the temperature is continuously raised to 1650-1700 ℃, can quickly permeate into a ceramic body, but is volatilized rapidly if the temperature exceeds 1700 ℃, and the effect is influenced; silicon carbide is easy to generate oxidation reaction at high temperature and is changed into silicon dioxide, the vacuumizing and the nitrogen filling are both used for removing oxygen and avoiding oxidation, the vacuum degree is higher at low temperature, so that the hearth is vacuumized to 10-20 Pa until the hearth is heated to 800 ℃, and after the hearth reaches 800 ℃, the argon or the nitrogen is filled.
In the preparation method of the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece, the temperature is reduced to room temperature after infiltration-reaction sintering, and the attached silicon balls are removed by sand blasting on the surface of the ceramic by a sand blasting machine.
Compared with the prior art, the invention has the following advantages:
1) the composition phases of the titanium silicon carbide-silicon carbide composite ceramic comprise a titanium silicon carbide phase and a silicon carbide phase, and the chemical synthesis of the two composition phases and the sintering process of the composite ceramic are synchronously carried out: wherein the titanium silicon carbide phase is generated by the reaction of titanium carbide powder, titanium powder and liquid-phase silicon, and the silicon carbide phase is generated by the reaction of carbon black and liquid-phase silicon; meanwhile, the two kinds of powder are tightly combined with liquid-phase silicon to realize sintering densification. Therefore, the process has simple process route, shortens the production flow and reduces the production cost.
2) The generated titanium silicon carbide phase has a layered structure similar to graphite, and can effectively change a crack propagation path so as to improve the fracture toughness of the silicon carbide ceramic. Particularly, the titanium silicon carbide phase has obvious plasticity characteristics at high temperature, and can effectively prevent the brittle fracture of the silicon carbide ceramic. The fracture toughness of the prepared titanium silicon carbide-silicon carbide composite ceramic is as high as 5-6.5 MPa.m1/2
3) The adopted slip casting method can mold ceramic special-shaped pieces with complex shapes, realizes the complication and light weight of silicon carbide parts, and meets the diversified requirements on the silicon carbide parts. The reasonable proportion of the plaster mold and the coating on the surface of the plaster mold further improve the density of the formed titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece.
4) The adopted infiltration reaction method can completely fill residual air holes in the biscuit with liquid-phase silicon, and the prepared silicon carbide ceramic is almost completely compact and has the characteristics of low sintering temperature and net size forming. The density of the prepared titanium silicon carbide-silicon carbide composite ceramic is about 99-99.5%,
drawings
FIG. 1 is an SEM photograph of a mixed powder prepared in example 1 of the present invention.
FIG. 2 is an SEM image of a polished surface of a TiSiC-SiC composite ceramic prepared in example 1 of the present invention.
FIG. 3 is a graph showing the morphology of a silicon titanocarbide phase produced by the infiltration reaction in example 1 of the present invention.
Detailed Description
The following is a description of specific embodiments of the present invention with reference to the drawings, and the technical solutions of the present invention will be further described, but the present invention is not limited to these embodiments.
Example 1
1) Uniformly dispersing 110g of carbon black, 55g of titanium carbide powder (with the average particle size of 2 microns), 22g of titanium powder (with the average particle size of 3 microns), 4g of polyvinyl alcohol and 6g of sodium carboxymethylcellulose in deionized water, and then carrying out ball milling for 24 hours to obtain ceramic slurry;
2) transferring the ceramic slurry into a vacuum container, vacuumizing under 10Pa to remove gas, slowly injecting the slurry into a gypsum mold, demolding, and drying for 3 days to obtain a special-shaped biscuit;
3) moving the shaped blank into a vacuum sintering furnace, uniformly spreading a certain amount of high-purity silicon powder (the silicon amount is 1.3 times of the silicon amount required by the chemical reaction of silicon and carbon) above the blank, then carrying out infiltration-reaction sintering at the sintering temperature of 1680 ℃, keeping the temperature for 1.5 hours (in the sintering process, when the temperature is lower than 800 ℃, vacuumizing a hearth to 15Pa, and when the temperature reaches above 800 ℃, filling argon gas into the hearth), finally cooling to room temperature, and carrying out sand blasting on the surface of the ceramic by using a sand blasting machine to remove attached silicon balls, thus obtaining the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic shaped part. The composition phase of the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece obtained in the embodiment contains 17% of titanium silicon carbide phase, 72% of silicon carbide phase and 11% of silicon phase.
Example 2
1) Uniformly dispersing 100g of carbon black, 60g of titanium carbide powder (with the average particle size of 2 microns), 24g of titanium powder (with the average particle size of 4 microns), 6g of polyvinyl alcohol and 10g of sodium carboxymethylcellulose in deionized water, and then carrying out ball milling for 24 hours to obtain ceramic slurry;
2) transferring the ceramic slurry into a vacuum container, vacuumizing under 10Pa to remove gas, slowly injecting the slurry into a gypsum mold, demolding, and drying for 3 days to obtain a special-shaped biscuit;
3) moving the shaped blank into a vacuum sintering furnace, uniformly spreading a certain amount of high-purity silicon powder (the silicon amount is 1.3 times of the silicon amount required by the chemical reaction of silicon and carbon) above the blank, then carrying out infiltration-reaction sintering at 1660 ℃, keeping the temperature for 1 hour (the hearth is vacuumized to 12Pa when the temperature is lower than 800 ℃ in the sintering process, and is filled with nitrogen when the temperature reaches above 800 ℃), finally cooling to room temperature, and carrying out sand blasting on the ceramic surface by using a sand blasting machine to remove attached silicon balls, thus obtaining the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic shaped piece. The composition phase of the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece obtained in the embodiment contains 20% of titanium silicon carbide phase, 67% of silicon carbide phase and 13% of silicon phase.
Example 3
1) Uniformly dispersing 120g of carbon black, 50g of titanium carbide powder (with the average particle size of 1 micron), 17g of titanium powder (with the average particle size of 2 microns), 5g of polyvinyl alcohol and 8g of sodium carboxymethylcellulose in deionized water, and then carrying out ball milling for 24 hours to obtain ceramic slurry;
2) transferring the ceramic slurry into a vacuum container, vacuumizing under 10Pa to remove gas, slowly injecting the slurry into a gypsum mold, demolding, and drying for 3 days to obtain a special-shaped biscuit;
3) moving the shaped blank into a vacuum sintering furnace, uniformly spreading a certain amount of high-purity silicon powder (the silicon amount is 1.3 times of the silicon amount required by the chemical reaction of silicon and carbon) above the blank, then carrying out infiltration-reaction sintering at the sintering temperature of 1690 ℃, keeping the temperature for 1 hour (the hearth is vacuumized to 18Pa when the temperature is lower than 800 ℃ in the sintering process, argon is filled in the hearth when the temperature reaches above 800 ℃), finally cooling to room temperature, carrying out sand blasting on the ceramic surface by using a sand blasting machine to remove attached silicon balls, and obtaining the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic shaped piece. The composition phase of the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece obtained in the embodiment contains 18% of titanium silicon carbide phase, 73% of silicon carbide phase and 9% of silicon phase.
Example 4
1) Dispersing 115g of carbon black, 54g of titanium carbide powder (with the average particle size of 3 microns), 21g of titanium powder (with the average particle size of 5 microns), 3g of polyvinyl alcohol and 7g of sodium carboxymethylcellulose uniformly in deionized water, and then carrying out ball milling for 24 hours to obtain ceramic slurry;
2) transferring the ceramic slurry into a vacuum container, vacuumizing under 10Pa to remove gas, slowly injecting the slurry into a gypsum mold, demolding, and drying for 3 days to obtain a special-shaped biscuit;
3) moving the shaped blank into a vacuum sintering furnace, uniformly spreading a certain amount of high-purity silicon powder (the silicon amount is 1.4 times of the silicon amount required by the silicon-carbon chemical reaction) above the blank, then carrying out infiltration-reaction sintering, wherein the sintering temperature is 1650 ℃, the heat preservation time is 2 hours (the furnace chamber is vacuumized to 10Pa when the temperature is lower than 800 ℃ in the sintering process, and nitrogen is filled in the furnace chamber when the temperature reaches above 800 ℃), finally cooling to room temperature, and carrying out sand blasting on the ceramic surface by using a sand blasting machine to remove attached silicon balls, thus obtaining the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic shaped piece. The composition phase of the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece obtained in the embodiment contains 16% of titanium silicon carbide phase, 74% of silicon carbide phase and 10% of silicon phase.
Example 5
1) Uniformly dispersing 120g of carbon black, 55g of titanium carbide powder (with the average particle size of 2 microns), 26g of titanium powder (with the average particle size of 2 microns), 3g of polyvinyl alcohol and 7g of sodium carboxymethylcellulose in deionized water, and then carrying out ball milling for 24 hours to obtain ceramic slurry;
2) transferring the ceramic slurry into a vacuum container, vacuumizing under 10Pa to remove gas, slowly injecting the slurry into a gypsum mold, demolding, and drying for 3 days to obtain a special-shaped biscuit;
3) moving the shaped blank into a vacuum sintering furnace, uniformly spreading a certain amount of high-purity silicon powder (the silicon amount is 1.2 times of the silicon amount required by the chemical reaction of silicon and carbon) above the blank, then carrying out infiltration-reaction sintering at the sintering temperature of 1700 ℃, keeping the temperature for 1 hour (the hearth is vacuumized to 20Pa when the temperature is lower than 800 ℃ in the sintering process, and argon is filled in the hearth when the temperature reaches above 800 ℃), finally cooling to room temperature, and carrying out sand blasting on the ceramic surface by using a sand blasting machine to remove attached silicon balls, thus obtaining the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic shaped piece.
Example 6
The difference from the embodiment 1 is only that the surface of the plaster mold in the embodiment is coated with a layer of coating, and the coating comprises the following components in parts by mass: 6 parts of microcrystalline wax, 4 parts of lanolin magnesium soap, 1.5 parts of modified water glass, 5 parts of rosin, 25 parts of solvent oil and 25 parts of mineral oil; and the gypsum mould in the embodiment is prepared from the following components in parts by mass: 25 parts of carbon fiber, 8 parts of silicate, 12 parts of rosin, 3 parts of phenolic resin, 5 parts of adhesive, 3 parts of quartz sand, 5 parts of sodium polyphosphate and 8 parts of water reducing agent.
Example 7
The difference from the embodiment 2 is only that the surface of the plaster mold in the embodiment is coated with a layer of coating, and the coating comprises the following components in parts by mass: 4 parts of microcrystalline wax, 4 parts of lanolin magnesium soap, 1 part of modified water glass, 6 parts of rosin, 22 parts of solvent oil and 28 parts of mineral oil; and the gypsum mould in the embodiment is prepared from the following components in parts by mass: 22 parts of carbon fiber, 6 parts of silicate, 10 parts of rosin, 5 parts of phenolic resin, 6 parts of adhesive, 4 parts of quartz sand, 6 parts of sodium polyphosphate and 10 parts of water reducing agent.
Example 8
The difference from the embodiment 3 is only that the surface of the plaster mold in the embodiment is coated with a layer of coating, and the coating comprises the following components in parts by mass: 8 parts of microcrystalline wax, 3 parts of lanolin magnesium soap, 2 parts of modified water glass, 3 parts of rosin, 30 parts of solvent oil and 20 parts of mineral oil; and the gypsum mould in the embodiment is prepared from the following components in parts by mass: 30 parts of carbon fiber, 5 parts of silicate, 15 parts of rosin, 2 parts of phenolic resin, 8 parts of adhesive, 1 part of quartz sand, 8 parts of sodium polyphosphate and 3 parts of water reducing agent.
Example 9
The difference from the embodiment 4 is only that the surface of the plaster mold in the embodiment is coated with a layer of coating, and the coating comprises the following components in parts by mass: 3 parts of microcrystalline wax, 5 parts of lanolin magnesium soap, 0.5 part of modified water glass, 8 parts of rosin, 20 parts of solvent oil and 30 parts of mineral oil.
Example 10
The difference from the example 5 is only that the plaster mold in the example is made of the following components in parts by weight: 20 parts of carbon fiber, 10 parts of silicate, 8 parts of rosin, 6 parts of phenolic resin, 2 parts of adhesive, 5 parts of quartz sand, 3 parts of sodium polyphosphate and 15 parts of water reducing agent.
Example 11
The difference from the example 1 is only that in the example, 100g of carbon black, 66g of titanium carbide powder and 21g of titanium powder are adopted, namely the mass ratio of the titanium carbide powder to the titanium powder is 3.14: 1.
example 12
The difference from example 1 is only that in this example, 50g of titanium carbide powder and 27g of titanium powder, that is, the mass ratio of titanium carbide powder to titanium powder is 1.85: 1.
Comparative example 1
Silicon carbide ceramics common in the art.
Comparative example 2
The only difference from example 1 is that the sintering temperature in this comparative example 2 is 2000 ℃.
Comparative example 3
The only difference from example 1 is that in this comparative example 4 no silicon is laid over the biscuit.
The ceramic shaped articles of examples 1 to 12 and comparative examples 1 to 3 were subjected to performance tests, and the test results are shown in table 1.
Table 1: performance results for ceramic profiles of examples 1-12 and comparative examples 1-3
Figure BDA0001410195750000091
Figure BDA0001410195750000101
In conclusion, the titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece has higher density, good mechanical property and particularly higher bending strength and fracture toughness.
While the invention has been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.

Claims (6)

1. The high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece is characterized in that a composition phase of the complex phase ceramic special-shaped piece comprises a titanium silicon carbide phase, a silicon carbide phase and a silicon phase, wherein the content of the titanium silicon carbide phase accounts for 15-25% of the total mass of the complex phase ceramic special-shaped piece, the content of the silicon carbide phase accounts for 65-85% of the total mass of the complex phase ceramic special-shaped piece, and the balance is the silicon phase, and the complex phase ceramic special-shaped piece comprises the following components in percentage by mass: 50-60% of carbon black, 25-35% of titanium carbide powder, 10-15% of titanium powder, 1-3% of a dispersant and 3-5% of a plasticizer, wherein the mass ratio of the titanium carbide powder to the titanium powder is 2-3: 1;
the method for preparing the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped part comprises the following steps:
1) uniformly dispersing carbon black, titanium carbide powder, titanium powder, a dispersing agent and a plasticizer according to the proportion, and then carrying out high-speed ball milling to obtain ceramic slurry;
2) slowly injecting the ceramic slurry into a gypsum mold after vacuum degassing, and drying to obtain a special-shaped blank;
3) and (3) moving the biscuit of the special-shaped part into a vacuum sintering furnace, uniformly spreading high-purity silicon powder above the biscuit, and then carrying out infiltration-reaction sintering at the sintering temperature of 1650-1700 ℃ for 1-2 hours to obtain the high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped part.
2. The high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece according to claim 1, wherein the grain size of titanium carbide powder is 1-3 μm.
3. The high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece according to claim 1, wherein the particle size of titanium powder is 2-5 μm.
4. The high toughness titanium silicon carbide-silicon carbide complex phase ceramic special shaped piece according to claim 1, characterized in that the dispersant is one or more of polyvinyl alcohol, tetramethyl ammonium hydroxide, polyacrylic acid, ammonium citrate, polyethylene glycol, the dispersion medium is one or two of absolute ethyl alcohol and deionized water, and the dispersion mode is high frequency ultrasonic dispersion.
5. The high toughness silicon carbide-titanium carbide complex phase ceramic shaped piece according to claim 1, wherein said plasticizer is one or more of sodium carboxymethylcellulose, epoxy resin, organic silicon and polyvinyl alcohol.
6. The high toughness TiCSiC-SiC complex phase ceramic profile member as claimed in claim 5, wherein said plasticizer is sodium carboxymethylcellulose having a viscosity of 800-1200 Pa.s.
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