CN102924084B - Method for preparing silicon carbide ceramic product by adopting pre-oxidizing process - Google Patents
Method for preparing silicon carbide ceramic product by adopting pre-oxidizing process Download PDFInfo
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- CN102924084B CN102924084B CN201210477673.7A CN201210477673A CN102924084B CN 102924084 B CN102924084 B CN 102924084B CN 201210477673 A CN201210477673 A CN 201210477673A CN 102924084 B CN102924084 B CN 102924084B
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Abstract
The invention discloses a method for preparing a silicon carbide ceramic product by adopting a pre-oxidizing process, comprising the following steps: (1) mixing the silicon carbide powder with the particle size of 50-100 microns, the silicon carbide powder with the particle size of 100-150 microns and the silicon carbide powder with the particle size of 150-200 microns uniformly, heating the mixture to 200-700 DEG C by a resistance furnace, and pre-oxidizing for 1-3 hours to obtain the pre-oxidized powder; (2) adding phenolic resin into the pre-oxidized powder, mixing the phenolic resin and the pre-oxidized powder uniformly, putting the mixture into a pugging machine for mixing, wrapping by plastic, and ageing for 3-4 hours to obtain mud; (3) putting the mud into an extruder for extruding to obtain a pipe billet, moving the pipe billet into a vacuum sintering furnace, and preserving the heat at 1,400-,1600 DEG C for 1-2 hours to obtain the extruded silicon carbide ceramic product. The technology for preparing the silicon carbide ceramic product by adopting the pre-oxidizing process has the advantages of simple process and stable performance, and the obtained product has a clean interface and is suitable for industrial scale production.
Description
Technical field
The present invention relates to pressureless sintering method and prepare the technical field of extrusion molding silicon carbide.
Background technology
Density is little, Young's modulus is large, thermal conductivity is high, thermal expansivity is low because having for thyrite, anti-thermal shock and oxidation susceptibility good, and moderate, corrosion-resistant and excellent performances such as semi-conductor of hot strength and obtain and study widely and apply: its Application Areas comprises: one, can be used for high-temperature structural material, as engine parts and blade of gas turbine, kiln rolling bar, refractory materials etc.; Two, because its high elastic coefficient and low density determined that it has very high specific rigidity, can be used for the structured material in aerospace field; Three, because its thermal expansivity can match and characteristic of semiconductor with Si, GaAs, therefore can be used as electronic package material and make electronic component; Four, because carbon and silicon have lower ordination number, silicon carbide also can be used as the structured material of reactor.
For silicon carbide, the forming technique having developed at present has: compression molding, etc. static pressure, extrusion molding, injection molding and flow casting molding.Wherein, extrusion molding is used powder size range is wide and receive much concern.More external major companies ripe application high-efficiency and continuous extrusion technique is produced, yet domestic this technology is not yet stable and ripe at present.Along with China joined WTO and each phase field are further opened, it is the task of top priority with the comprehensive competitive power that improves China enterprise that Speeding up development has the independently silicon carbide products technology of preparing of intellecture property.
At present, silicon carbide is very restricted because Cost Problems makes its application.The research and development that reduce stupalith cost are by the difficult task that is 21 century stupalith field face.Wherein, serialization, the high extruding shaping technique of automatization will be one of powerful measure addressing this problem.
By closing the preoxidation of batch silicon carbide powder, it adds plastic forming agent and react also removal completely with zone of oxidation in pressureless sintering to make extruded product, and because newborn silicon carbide is closely connected with raw material powder, makes the raising of extruded product intensity.
Summary of the invention
The object of the present invention is to provide a kind of method of pressureless sintering silicon carbide extruded product.
Technical scheme of the present invention is: preoxidation is prepared the method for pushing silicon carbide ceramic product, and its step is as follows:
(1) by 15-30 weight part granularity, be that the carborundum powder that the carborundum powder of 50-100 μ m, carborundum powder that 15-30 weight part granularity is 100-150 μ m and 20-50 weight part granularity are 150-200 μ m mixes, then in resistance furnace, be heated to 200-700 ℃, preoxidation 1-3 hour, makes preoxidation powder;
(2) in preoxidation powder, add the resol of 10-30 weight part, after mixing, put into pug mill and mix; Finally by plastic wraps, undertaken oldly, the time is 3-4 hour, makes pug;
(3) pug is put into extrusion machine and extrude, obtain tube billet, tube billet is moved in vacuum sintering furnace, under the condition of 1400-1600 ℃, be incubated 1-2 hour, make extruding silicon carbide ceramic product.
The invention has the beneficial effects as follows: the silicon carbide powder of size fractionated is criticized also after evenly mixing through closing, make it preoxidation in resistance furnace, powder surface generate continuously and have a certain thickness silicon dioxide layer, in sintering, can carry out complete reaction with the plastic forming agent adding, plastic forming agent is disappeared, newborn silicon carbide layer is tightly sintered together raw material powder, and pressureless sintering product properties is improved.Preoxidation extruded carbon SiClx technology of preparing, technique is simple, stable performance, resulting product interface cleanness, is applicable to technical scale.
Embodiment
embodiment 1
Batching weighing 2.0kg, wherein the particulate carborundum powder of 80 μ m is 0.6kg; The middle grain carborundum powder of 115 μ m is 0.5kg; The coarse grain carborundum powder of 180 μ m is 0.6kg; Resol 0.3kg.
First silicon carbide powder is closed and criticize, put into mixer mixing 1.0hr, then above compound is put into resistance furnace 500 ℃ of preoxidation 2.5 hours.
Above-mentioned compound is put into satellite gear mill, while mix, pour resol into, until mix.Then above-mentioned pug being put into pug mill mixes; Last plastic wraps is carried out old, and the time is 3.5hrs.
Above pug is put into extrusion machine and is extruded, and obtains tube billet.This blank is moved in vacuum sintering furnace in 1600 ℃ of insulation 1.5hrs, acquisition finished product.The bending strength that records this material is 272MPa.
embodiment 2
Batching weighing 2.0kg, wherein the particulate carborundum powder of 60 μ m is 0.5kg; The middle grain carborundum powder of 125 μ m is 0.5kg; The coarse grain carborundum powder of 170 μ m is 0.6kg; Resol 0.4kg.
First silicon carbide powder is closed and criticize, put into mixer mixing 1.5hrs, then above compound is put into resistance furnace 600 ℃ of preoxidation 3.0 hours.
Then compound is put into satellite gear mill, while mix, poured into resol, until mix.Then above-mentioned pug being put into pug mill mixes; Last plastic wraps is carried out old, and the time is 4.0hr.
Above pug is put into extrusion machine and is extruded, and obtains tube billet.This blank is moved in vacuum sintering furnace in 1600 ℃ of insulation 2.0hrs, acquisition finished product.The bending strength that records this material is 265MPa.
embodiment 3
Preoxidation is prepared the method for pushing silicon carbide ceramic product, it is characterized in that its step is as follows:
(1) by 15 weight part granularities, be that the carborundum powder that the carborundum powder of 50 μ m, carborundum powder that 15 weight part granularities are 100 μ m and 20 weight part granularities are 150 μ m mixes, then in resistance furnace, be heated to 200 ℃, preoxidation 1 hour, makes preoxidation powder;
(2) in preoxidation powder, add the resol of 10 weight parts, after mixing, put into pug mill and mix; Finally by plastic wraps, undertaken oldly, the time is 3 hours, makes pug;
(3) pug is put into extrusion machine and extrude, obtain tube billet, tube billet is moved in vacuum sintering furnace, under the condition of 1400 ℃, be incubated 1 hour, make extruding silicon carbide ceramic product.
embodiment 4
Preoxidation is prepared the method for pushing silicon carbide ceramic product, it is characterized in that its step is as follows:
(1) by 30 weight part granularities, be that the carborundum powder that the carborundum powder of 100 μ m, carborundum powder that 30 weight part granularities are 150 μ m and 50 weight part granularities are 200 μ m mixes, then in resistance furnace, be heated to 700 ℃, preoxidation 3 hours, makes preoxidation powder;
(2) in preoxidation powder, add the resol of 30 weight parts, after mixing, put into pug mill and mix; Finally by plastic wraps, undertaken oldly, the time is 4 hours, makes pug;
(3) pug is put into extrusion machine and extrude, obtain tube billet, tube billet is moved in vacuum sintering furnace, under the condition of 1600 ℃, be incubated 2 hours, make extruding silicon carbide ceramic product.
embodiment 5
Preoxidation is prepared the method for pushing silicon carbide ceramic product, it is characterized in that its step is as follows:
(1) by 20 weight part granularities, be that the carborundum powder that the carborundum powder of 80 μ m, carborundum powder that 20 weight part granularities are 120 μ m and 40 weight part granularities are 180 μ m mixes, then in resistance furnace, be heated to 500 ℃, preoxidation 2 hours, makes preoxidation powder;
(2) in preoxidation powder, add the resol of 20 weight parts, after mixing, put into pug mill and mix; Finally by plastic wraps, undertaken oldly, the time is 3 hours, makes pug;
(3) pug is put into extrusion machine and extrude, obtain tube billet, tube billet is moved in vacuum sintering furnace, under the condition of 1500 ℃, be incubated 2 hours, make extruding silicon carbide ceramic product.
embodiment 6
Preoxidation is prepared the method for pushing silicon carbide ceramic product, it is characterized in that its step is as follows:
(1) by 15-30 weight part granularity, be that the carborundum powder that the carborundum powder of 50-100 μ m, carborundum powder that 15-30 weight part granularity is 100-150 μ m and 20-50 weight part granularity are 150-200 μ m mixes, then in resistance furnace, be heated to 200-700 ℃, preoxidation 1-3 hour, makes preoxidation powder;
(2) in preoxidation powder, add the resol of 10-30 weight part, after mixing, put into pug mill and mix; Finally by plastic wraps, undertaken oldly, the time is 3-4 hour, makes pug;
(3) pug is put into extrusion machine and extrude, obtain tube billet, tube billet is moved in vacuum sintering furnace, under the condition of 1400-1600 ℃, be incubated 1-2 hour, make extruding silicon carbide ceramic product.
Claims (1)
1. preoxidation is prepared the method for silicon carbide ceramic product, it is characterized in that its step is as follows:
(1) by 15-30 weight part granularity, be that the carborundum powder that the carborundum powder of 50-100 μ m, carborundum powder that 15-30 weight part granularity is 100-150 μ m and 20-50 weight part granularity are 150-200 μ m mixes, then in resistance furnace, be heated to 200-700 ℃, preoxidation 1-3 hour, makes preoxidation powder;
(2) in preoxidation powder, add the resol of 10-30 weight part, after mixing, put into pug mill and mix; Finally by plastic wraps, undertaken oldly, the time is 3-4 hour, makes pug;
(3) pug is put into extrusion machine and extrude, obtain tube billet, tube billet is moved in vacuum sintering furnace, under the condition of 1400-1600 ℃, be incubated 1-2 hour, make extruding silicon carbide ceramic product.
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| CN114702317A (en) * | 2022-03-24 | 2022-07-05 | 湖南太子新材料科技有限公司 | Low-temperature sintering method of high-performance silicon carbide ceramic material |
| CN114956828B (en) * | 2022-05-17 | 2023-08-15 | 合肥商德应用材料有限公司 | Silicon carbide ceramic and preparation method and application thereof |
| CN116514554A (en) * | 2023-05-11 | 2023-08-01 | 中国科学院上海硅酸盐研究所 | Preparation method of high-compressive-strength silicon carbide ceramic |
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| JP2000109367A (en) * | 1998-10-02 | 2000-04-18 | Toshiba Ceramics Co Ltd | Heat treatment method for silicon carbide sintered body and heat-treated silicon carbide |
| CN101655330B (en) * | 2009-08-25 | 2011-11-09 | 山东理工大学 | Preparation method of ceramic tube for isothermal gradient heat exchanger |
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