CN101100384A - Nanocomposite silicon carbide ceramics and preparation method thereof - Google Patents
Nanocomposite silicon carbide ceramics and preparation method thereof Download PDFInfo
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Abstract
本发明公开了一种纳米复合碳化硅陶瓷的制备方法，以碳化硅、钇铝石榴石和纳米颗粒组成主原料，包括以下步骤：1)将上述主原料、粘结剂、水溶性高分子混合物溶胶和分散剂加入去离子水中，球磨混合后，配制成固相含量为30％～60％水基碳化硅浆料；2)采用喷雾造粒工艺对水基碳化硅浆料进行喷雾干燥，得碳化硅造粉粒；3)对碳化硅造粉粒采用二步方式成型，获得高密度的碳化硅素坯；4)将上述碳化硅素坯放在真空无压烧结炉中烧结。本发明还公开了上述方法所制备的纳米复合碳化硅陶瓷。该方法工艺简便，所制备的碳化硅陶瓷性能优越。
The invention discloses a method for preparing nano-composite silicon carbide ceramics. The main raw materials are composed of silicon carbide, yttrium aluminum garnet and nanoparticles, and the steps are as follows: 1) sol and dispersant in deionized water, mixed by ball milling, and prepared into a water-based silicon carbide slurry with a solid phase content of 30% to 60%; 2) spray-drying the water-based silicon carbide slurry by a spray granulation process to obtain carbonized Silicon powder granules; 3) The silicon carbide powder granules are molded in two steps to obtain high-density silicon carbide green bodies; 4) The silicon carbide green bodies are sintered in a vacuum pressureless sintering furnace. The invention also discloses the nanocomposite silicon carbide ceramic prepared by the above method. The process is simple and convenient, and the prepared silicon carbide ceramic has superior performance.
Description
Technical field
The present invention relates to a kind of silicon carbide ceramics and preparation method thereof, specifically, is a kind of nanometer composite silicon carbide ceramic and preparation method thereof.
Background technology
Silicon carbide ceramics has many good characteristics as a kind of high-temperature structural ceramics, and is good etc. as wear resistance, high thermal conductivity and electric insulating quality, semiconductive and electric conductivity, heat-resisting, corrosion-resistant and high-temperature mechanics and thermal property.Silicon carbide ceramics has been widely used in industrial circle and national defense industry such as machinery, electronics, petrochemical complex, metallurgy, and has been confirmed as the 4th kind of basic material since metal, aluminum oxide, Wimet in the world.Though silicon carbide ceramics has many performances, also be applied in a lot of fields, its room temperature strength is low, toughness not enough, moulding is relatively more difficult, thereby has limited its application.Meanwhile, various fields such as the national defence in the high speed development, space technology, automobile, the energy constantly propose new requirement to structured material.Therefore have only the toughness reinforcing means of the various enhancings of employing to prepare carborundum based material, improve its intensity and toughness, could satisfy the requirement that silicon carbide ceramics is used in leading-edge fields such as national defence, space technologies better.Prepare high-strength, high-ductility, high multifrequency nature such as hard, corrosion-resistant, high temperature resistant, wear-resisting in the composite silicon carbide ceramic material of the excellent performance of one, become the main flow of thyrite research and development.
Nanosecond science and technology are as a kind of emerging science and technology, just more and more cause people's attention and attention.Because nano material has some fundamental characteristics such as small-size effect, surface and interfacial effect, quantum size effect, caused nano material all to demonstrate special performances at aspects such as many physics such as fusing point, vapour pressure, transformation temperature, optical property, chemical reaction character, magnetic, superconduction and viscous deformation and chemistry.Nano ceramics makes bill of material reveal the characteristic of a lot of excellences because grain-size is very little, as normal temperature superplasticity, intensity raising when keeping original conventional ceramic materials fracture toughness, sintering temperature reduction etc.But the crystal grain recrystallization that stupalith must occur when pyroprocessing brings obstacle for the preparation of single phase nano stupalith, and the conception of nano heterogeneous ceramic is arisen at the historic moment.Nano heterogeneous ceramic with heterogeneous phase nano particle equably disperse in ceramic matrix, can play effect simultaneously to the strengthening and toughening of material.Nano particle by to the pinning of matrix crystal boundary, strengthening effect and form the intensity that dislocation network increases stupalith in the matrix crystal boundary, increases the toughness of stupalith by crackle bridging, crack deflection, crackle bending in ceramic matrix.
Though the exploitation of nano complex phase ceramic material and toughness reinforcing enhancing theory and method are well developed, but still have following problem:
1) mechanical mixing be use at most at present, the easiest method for preparing composite granule, but because nano-powder has bigger specific surface area, in the drying process after ball milling, very easily produce reunion, sedimentation, cause the nano particle can not homodisperse, influence the performance of nano heterogeneous ceramic the most at last.
2) present sintering processings such as the more use hot pressed sintering of the sintering of nano heterogeneous ceramic, HIP sintering, discharge plasma sintering, these modes have very high requirement to agglomerating plant, and complex process, and the cost height is difficult to realize industrialization production.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of nanometer composite silicon carbide ceramic and preparation method thereof, and this method technology is easy, low-cost, adopts the silicon carbide ceramics of this method preparation to have characteristics such as hardness height, bending strength is big, fracture toughness property is good.
In order to solve the problems of the technologies described above, the invention provides a kind of preparation method of nanometer composite silicon carbide ceramic, with weight percent is that 75%～85% silicon carbide, 5%～10% yttrium aluminum garnet and 10%～15% nano particle are formed main raw material, may further comprise the steps successively:
1), above-mentioned main raw material, binding agent, mixture of water-soluble polymer colloidal sol and dispersion agent are added in the deionized water, ball milling mixed after 5～20 hours, and being mixed with solid load is 30%～60% water base silicon carbide slurry; The weight of described binding agent, mixture of water-soluble polymer colloidal sol and dispersion agent is respectively 0.5%～3%, 0.5%～2% and 0.5%～1.5% of main raw material;
2), adopt atomizing granulating technology that above-mentioned water base silicon carbide slurry is carried out spraying drying, the silicon carbide amyloplastid; Slurry flow is 3～7Kg/h, and the hot blast inlet temperature is 200～250 ℃;
3), above-mentioned silicon carbide amyloplastid is adopted the two steps mode moulding of 100MPa dry-pressing precompressed and 250MPa cold isostatic pressing end pressing, obtain highdensity silicon carbide biscuit;
4) above-mentioned silicon carbide biscuit is placed in the vacuum non-pressure sintering furnace, is warming up to 1900～2000 ℃ of insulations 0.5～1 hour, be cooled to 1760～1850 ℃ of insulations 0.5～5 hour again, sintering finishes, and gets nanometer composite silicon carbide ceramic.
Improvement as the preparation method of nanometer composite silicon carbide ceramic of the present invention: nano particle is at least a in nanometer silicon carbide, nano titanium carbide and the Nano titanium nitride.Binding agent is resol or dextrin, and mixture of water-soluble polymer colloidal sol is polyvinyl alcohol (PVA), and dispersion agent is polyoxyethylene glycol (PEG) or Tetramethylammonium hydroxide (TMAH).
In the present invention, solid load is that 30%～60% water base silicon carbide slurry refers to: (main raw material+binding agent+mixture of water-soluble polymer colloidal sol+dispersion agent) ÷ (main raw material+binding agent+mixture of water-soluble polymer colloidal sol+dispersion agent+deionized water)=30%～60%.
The present invention also provides simultaneously according to the prepared nanometer composite silicon carbide ceramic of above-mentioned any one method.
The preparation method of nanometer composite silicon carbide ceramic of the present invention has the following advantages:
(1) in step 1), rely on ball milling to mix, make nano particle and submicron (micron) powder uniform mixing, thereby prepared the homodisperse slurry of nano particle.
(2) in step 2) in, utilize atomizing granulating technology directly to be sprayed to the slurry that mixes in the warm air, at very short time inner drying, avoided the reunion again of nano particle and settlement separate, keep the original homogeneity of slurry, realized the preparation of the homodisperse composite granule of nano particle.In this step, by adjusting hot blast inlet temperature and slurry flow, thereby water ratio, flowability and the intensity of control granulation ball are finally prepared and are flowed and the good silicon carbide granulating powder of processability.
(3) introduce yttrium aluminum garnet as sintering aid, reduced sintering temperature, avoided nano particle under higher temperature, to grow up rapidly, thereby suppressed the growth of nanocrystal.
(4) adopt the vacuum non-pressure sintering technology, technology is easy, more can adapt to suitability for industrialized production.
(5) nano particle in the nanometer complex phase silicon carbide ceramics can suppress the growth of carborundum grain, make silicon carbide whisker particle size tiny evenly (Fig. 2), median size is between 0.5～2 μ m, thereby improved the intensity of material, nano particle has increased the toughness of material by crackle bridging, crack deflection, crackle bending simultaneously.According to the silicon carbide ceramics that the present invention makes, its body is close to be 3.10～3.30g/cm
3, hardness is 20～28GPa, and bending strength is 450～700MPa, and fracture toughness property is 6～8MPam
1/2
(6) preparation method of nanometer composite silicon carbide ceramic of the present invention, technology is easy, low-cost, can adapt to suitability for industrialized production.
Description of drawings
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described in further detail.
Fig. 1 is a step 2) the pattern synoptic diagram of the silicon carbide amyloplastid of gained;
Fig. 2 is that the crystalline substance of nanometer composite silicon carbide ceramic section of final gained is as synoptic diagram.
Embodiment
Below umber among all embodiment all represent weight part.
Embodiment 1: a kind of preparation method of nanometer composite silicon carbide ceramic, form main raw material with 85 parts of silicon carbide, 5 parts of yttrium aluminum garnets, 5 parts of nanometer silicon carbides and 5 parts of nano titanium carbides, and carry out following steps successively:
1), above-mentioned main raw material, 2 parts of resol, 0.5 part of PVA and 1 part of PEG are added in 200 parts of deionized waters, ball milling mixed after 5 hours, was mixed with water base silicon carbide slurry;
2), adopt atomizing granulating technology that above-mentioned water base silicon carbide slurry is carried out spraying drying, the silicon carbide amyloplastid; The processing condition of mist projection granulating are as follows: slurry flow is 6Kg/h, and the hot blast inlet temperature is 200 ℃;
3), above-mentioned silicon carbide amyloplastid is adopted the two steps mode moulding of 100MPa dry-pressing precompressed and 250MPa cold isostatic pressing end pressing, obtain highdensity silicon carbide biscuit;
4) above-mentioned silicon carbide biscuit is placed in the vacuum non-pressure sintering furnace, is warming up to 1900 ℃ of insulations 1 hour, be cooled to 1760 ℃ of insulations 5 hours again, sintering finishes, and gets nanometer composite silicon carbide ceramic.
The body of this nanometer composite silicon carbide ceramic is close to be 3.10～3.30g/cm
3, hardness is 20～28GPa, and bending strength is 450～700MPa, and fracture toughness property is 6～8MPam
1/2
Embodiment 2: a kind of preparation method of nanometer composite silicon carbide ceramic, form main raw material with 80 parts of silicon carbide, 8 parts of yttrium aluminum garnets, 5 parts of nanometer silicon carbides, 2 parts of nano titanium carbides and 5 parts of Nano titanium nitrides, and carry out following steps successively:
1), above-mentioned main raw material, 3 parts of resol, 2 parts of PVA and 1.5 parts of PEG are added in 150 parts of deionized waters, ball milling mixed after 10 hours, was mixed with water base silicon carbide slurry;
2), adopt atomizing granulating technology that above-mentioned water base silicon carbide slurry is carried out spraying drying, the silicon carbide amyloplastid; The processing condition of mist projection granulating are as follows: slurry flow is 4Kg/h, and the hot blast inlet temperature is 225 ℃;
3), above-mentioned silicon carbide amyloplastid is adopted the two steps mode moulding of 100MPa dry-pressing precompressed and 250MPa cold isostatic pressing end pressing, obtain highdensity silicon carbide biscuit;
4) above-mentioned silicon carbide biscuit is placed in the vacuum non-pressure sintering furnace, is warming up to 1950 ℃ of insulations 0.7 hour, be cooled to 1800 ℃ of insulations 3 hours again, sintering finishes, and gets nanometer composite silicon carbide ceramic.
The body of this nanometer composite silicon carbide ceramic is close to be 3.10～3.30g/cm for body is close
3, hardness is 20～28GPa, and bending strength is 450～700MPa, and fracture toughness property is 6～8MPam
1/2
Embodiment 3: a kind of preparation method of nanometer composite silicon carbide ceramic, form main raw material with 75 parts of silicon carbide, 10 parts of yttrium aluminum garnets, 5 parts of nanometer silicon carbides, 5 parts of nano titanium carbides and 5 parts of Nano titanium nitrides, and carry out following steps successively:
1), above-mentioned main raw material, 0.5 part of dextrin, 1 part of PVA and 0.5 part of TMAH are added in 90 parts of deionized waters, ball milling mixed after 20 hours, was mixed with water base silicon carbide slurry;
2), adopt atomizing granulating technology that above-mentioned water base silicon carbide slurry is carried out spraying drying, the silicon carbide amyloplastid; The processing condition of mist projection granulating are as follows: slurry flow is 3Kg/h, and the hot blast inlet temperature is 250 ℃;
3), above-mentioned silicon carbide amyloplastid is adopted the two steps mode moulding of 100MPa dry-pressing precompressed and 250MPa cold isostatic pressing end pressing, obtain highdensity silicon carbide biscuit;
4) above-mentioned silicon carbide biscuit is placed in the vacuum non-pressure sintering furnace, is warming up to 2000 ℃ of insulations 0.5 hour, be cooled to 1850 ℃ of insulations 0.5 hour again, sintering finishes, and gets nanometer composite silicon carbide ceramic.
The body of this nanometer composite silicon carbide ceramic is close to be 3.10～3.30g/cm
3, hardness is 20～28GPa, and bending strength is 450～700MPa, and fracture toughness property is 6～8MPam
1/2
Embodiment 4: a kind of preparation method of nanometer composite silicon carbide ceramic, form main raw material with 85 parts of silicon carbide, 5 parts of yttrium aluminum garnets and 10 parts of nanometer silicon carbides, and carry out following steps successively:
1), above-mentioned main raw material, 0.5 part of resol, 1 part of PVA and 0.5 part of TMAH are added in 200 parts of deionized waters, ball milling mixed after 5 hours, was mixed with water base silicon carbide slurry;
2), adopt atomizing granulating technology that above-mentioned water base silicon carbide slurry is carried out spraying drying, the silicon carbide amyloplastid; The processing condition of mist projection granulating are as follows: slurry flow is 5Kg/h, and the hot blast inlet temperature is 225 ℃;
3), above-mentioned silicon carbide amyloplastid is adopted the two steps mode moulding of 100MPa dry-pressing precompressed and 250MPa cold isostatic pressing end pressing, obtain highdensity silicon carbide biscuit;
4) above-mentioned silicon carbide biscuit is placed in the vacuum non-pressure sintering furnace, is warming up to 1900 ℃ of insulations 1 hour, be cooled to 1760 ℃ of insulations 5 hours again, sintering finishes, and gets nanometer composite silicon carbide ceramic.
The body of this nanometer composite silicon carbide ceramic is close to be 3.10～3.30g/cm
3, hardness is 20～28GPa, and bending strength is 450～700MPa, and fracture toughness property is 6～8MPam
1/2
What more than enumerate only is some specific embodiments of the present invention, obviously the invention is not restricted to above embodiment, and many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (4)
1, a kind of preparation method of nanometer composite silicon carbide ceramic is characterized in that with weight percent being that 75%～85% silicon carbide, 5%～10% yttrium aluminum garnet and 10%～15% nano particle are formed main raw material, may further comprise the steps successively:
1), above-mentioned main raw material, binding agent, mixture of water-soluble polymer colloidal sol and dispersion agent are added in the deionized water, ball milling mixed after 5～20 hours, and being mixed with solid load is 30%～60% water base silicon carbide slurry; The weight of described binding agent, mixture of water-soluble polymer colloidal sol and dispersion agent is respectively 0.5%～3%, 0.5%～2% and 0.5%～1.5% of main raw material;
2), adopt atomizing granulating technology that above-mentioned water base silicon carbide slurry is carried out spraying drying, the silicon carbide amyloplastid; Slurry flow is 3～7Kg/h, and the hot blast inlet temperature is 200～250 ℃;
3), above-mentioned silicon carbide amyloplastid is adopted the two steps mode moulding of 100MPa dry-pressing precompressed and 250MPa cold isostatic pressing end pressing, obtain highdensity silicon carbide biscuit;
4) above-mentioned silicon carbide biscuit is placed in the vacuum non-pressure sintering furnace, is warming up to 1900～2000 ℃ of insulations 0.5～1 hour, be cooled to 1760～1850 ℃ of insulations 0.5～5 hour again, sintering finishes, and gets nanometer composite silicon carbide ceramic.
2, the preparation method of nanometer composite silicon carbide ceramic according to claim 1 is characterized in that: described nano particle is at least a in nanometer silicon carbide, nano titanium carbide and the Nano titanium nitride.
3, the preparation method of nanometer composite silicon carbide ceramic according to claim 2, it is characterized in that: described binding agent is resol or dextrin, described mixture of water-soluble polymer colloidal sol is polyvinyl alcohol, and described dispersion agent is polyoxyethylene glycol or Tetramethylammonium hydroxide.
4, according to the prepared nanometer composite silicon carbide ceramic of any one method in the claim 1～3.
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| CN101653964B (en) * | 2009-09-10 | 2011-05-18 | 浙江立泰复合材料有限公司 | Cold isostatic pressing method of large-size cylindrical thin silicon carbide ceramic biscuit |
| CN101555144B (en) * | 2009-05-21 | 2012-02-01 | 浙江大学 | Silicon carbide short fiber toughened and strengthened silicon carbide ceramics and preparation method thereof |
| CN101525240B (en) * | 2009-04-23 | 2012-06-06 | 浙江大学 | Boride reinforced silicon carbide ceramics and preparation method thereof |
| CN106007721A (en) * | 2016-05-18 | 2016-10-12 | 淄博和润研磨材料科技有限公司 | Preparation method of silicon carbide ceramic grinding balls |
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| CN107459357A (en) * | 2017-09-06 | 2017-12-12 | 西安博尔新材料有限责任公司 | Silicon carbide composite powder body and its preparation method and application |
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| US5656218A (en) * | 1995-05-19 | 1997-08-12 | Industrial Technology Research Institute | Method for making high performance self-reinforced silicon carbide using a pressureless sintering process |
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| CN106045521A (en) * | 2016-05-27 | 2016-10-26 | 台州东新密封有限公司 | Method using hot pressed sintering to prepare dry-gas-seal rotating ring |
| CN107459357A (en) * | 2017-09-06 | 2017-12-12 | 西安博尔新材料有限责任公司 | Silicon carbide composite powder body and its preparation method and application |
| CN110064339A (en) * | 2019-05-07 | 2019-07-30 | 天津西敦津洋环保科技有限公司 | The preparation method of composite particles |
| CN111037710A (en) * | 2019-12-12 | 2020-04-21 | 湖南太子新材料科技有限公司 | Forming method of sagger for lithium battery positive electrode material |
| CN111138200A (en) * | 2020-01-11 | 2020-05-12 | 浙江东新新材料科技有限公司 | Multiphase composite reinforced low-friction silicon carbide ceramic sealing material and preparation method thereof |
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| CN114591086A (en) * | 2022-03-31 | 2022-06-07 | 中国兵器工业第五二研究所烟台分所有限责任公司 | Nano powder modified silicon carbide-boron carbide composite ceramic and preparation method thereof |
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| CN117819977A (en) * | 2024-03-06 | 2024-04-05 | 聚勒微电子科技(太仓)有限公司 | Silicon carbide composite ceramic material and preparation method and application thereof |
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