CN104177087A - Method for preparing silicon carbide bonded silicon nitride composite material by using microwave sintering process - Google Patents
Method for preparing silicon carbide bonded silicon nitride composite material by using microwave sintering process Download PDFInfo
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- CN104177087A CN104177087A CN201410405551.6A CN201410405551A CN104177087A CN 104177087 A CN104177087 A CN 104177087A CN 201410405551 A CN201410405551 A CN 201410405551A CN 104177087 A CN104177087 A CN 104177087A
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- silicon nitride
- silicon carbide
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Abstract
The invention relates to a method for preparing a silicon carbide bonded silicon nitride composite material by using a microwave sintering process. The method is characterized by comprising the following steps: mixing the following components in percentage by weight: 50-80 percent of silicon carbide particles, 5-25 percent of silicon carbide powder, 5-30 percent of silicon powder, 1-4 percent of carboxymethyl cellulose and 1-5 percent of water, and molding; putting a molded blank body into a vacuum microwave sintering furnace, vacuumizing until the pressure intensity in the microwave sintering furnace is less than or equal to 20Pa, filling nitrogen, and sintering for 0.5-5 hours in a nitrogen atmosphere at 1300-1600 DEG C so as to obtain the silicon carbide bonded silicon nitride composite material. The method is short in production cycle and high in production efficiency; and the prepared silicon carbide bonded silicon nitride composite material is uniform in phase distribution and relatively high in strength, and has excellent thermal shock resistance, oxidation resistance, high-temperature creep resistance and erosion resistance.
Description
Technical field
The invention belongs to silicon nitride combined silicon carbide technical field of composite materials.Relate in particular to a kind of microwave sintering legal system of using for the method for silicon nitride combined silicon carbide matrix material.
Background technology
The microhardness of silicon nitride and silicon carbide is only second to a few superhard materials such as diamond, cubic boron nitride, norbide, in addition silicon carbide has fabulous thermal conductivity and very low coefficient of thermal expansion, makes silicon nitride combined silicon carbide matrix material have good heat-shock resistance.Meanwhile, silicon nitride combined silicon carbide material has good chemical property, almost can bear the corrosion of mineral acid He some alkali lye of all (except for hydrofluoric acid).In industrial application, the erosion of the anti-melting non-ferrous metal of silicon nitride combined silicon carbide, is not soaked by aluminum and its alloy liquation, high-temperature electric good insulating.
Research is found, the folding strength of silicon nitride combined silicon carbide matrix material room temperature is the twice of clay silicon carbide articles, and owing to not containing setting phase, hot strength can reach 4 times of clay-carborundum goods, compare with clay silicon carbide articles, it has good oxidation-resistance.So, using under harsh environment, silicon nitride combined silicon carbide matrix material is widely used.
Above advantage has a wide range of applications silicon nitride combined silicon carbide matrix material in metallurgical and manufacturing, such as having obtained good effect in aspect application such as iron-smelting blast furnace, aluminium cell, ceramic kiln furnitures.
At present, the preparation of silicon nitride combined silicon carbide matrix material is mainly by pass into the method for nitrogen in High Temperature Furnaces Heating Apparatus thermal treatment base substrate, by heating unit in stove, generate heat, under thermal-radiating effect, make to be heated containing the SiC base substrate of elemental silicon, the elemental silicon of base substrate inside and nitrogen react and generate Si
3n
4siC particle is combined, can obtain silicon nitride combined silicon carbide matrix material thus.The silicon nitride combined silicon carbide matrix material that this conventional method of preparing silicon nitride combined silicon carbide material finally obtains is just outside has more silicon nitride to generate, and inner silicon nitride growing amount is less, even do not have, reduced thus the homogeneity of silicon nitride combined silicon carbide composite structure and tissue.In use, composite inner and outside volume expansivity there are differences, and will cause material in Thermal Cycling, to occur peeling off and the problems such as crackle.
Summary of the invention
The present invention is intended to overcome prior art deficiency, and object is to provide a kind of by microwave sintering legal system method for silicon nitride combined silicon carbide matrix material high with production efficiency with short production cycle; The silicon nitride combined silicon carbide matrix material thing of preparing by the method is evenly distributed mutually, and intensity is higher, and heat-shock resistance, oxidation-resistance, high-temperature creep resistance and erosion-resisting characteristics are good.
Owing to adopting technique scheme, the technical solution used in the present invention is: first the simple substance silica flour of the carborundum powder of the silicon-carbide particle of 50 ~ 80wt%, 5 ~ 25wt%, 5 ~ 30wt%, the carboxymethyl cellulose of 1 ~ 4wt% and the water of 1 ~ 5wt% are mixed to moulding.Base substrate after moulding is inserted in vacuum microwave sintering oven, first be evacuated to the pressure≤20Pa in described microwave agglomerating furnace, be filled with nitrogen, then sintering 0.5 ~ 5 hour under nitrogen atmosphere and 1300 ~ 1600 ℃ of conditions, obtains silicon nitride combined silicon carbide matrix material again.
The particle diameter of described silicon-carbide particle is 7 ~ 0.1mm, the SiC content >=95wt% of silicon-carbide particle.
The particle diameter of described carborundum powder is 5 ~ 100 μ m, the SiC content >=95wt% of carborundum powder.
The particle diameter of described simple substance silica flour is 5 ~ 100 μ m, the Si content >=95wt% of simple substance silica flour
Purity >=the 99.9Vol% of described nitrogen.
Owing to adopting technique scheme, the present invention compared with prior art has following positively effect:
The present invention, by the method for microwave sintering, utilizes catalysis and the non-thermal effect of microwave, promotes the solid phase diffusion between material, and the density of the finished product and mechanical property are apparently higher than normal sintering product; Meanwhile, microwave radiation can promote densification, promotes grain growing, accelerates the effects such as chemical reaction.In sintering, microwave, not only as a kind of heating energy source, is also a kind of activated sintering process.High-frequency electrical field energy promotes the migration in the charged room of Grain Surface, thereby crystal grain is produced, is similar to the viscous deformation that diffusion is wriggled, thereby has promoted the carrying out of sintering.And microwave sintering heat-up rate is fast, sintering time is short, can significantly improve production efficiency.
Most importantly, during microwave sintering, material is from inside, to start to heat up and heating, first the process that so just makes elemental silicon and nitrogen reaction produce silicon nitride is started by inside, prolongation along with sintering time, the generation of silicon nitride is carried out to outside by inside gradually, and after sintering process finishes, silicon nitride is evenly distributed in composite inner mutually.The present invention can overcome that volume effect that the silicon nitride due to billet surface that conventional sintering technique causes generates is stopped up pore in base substrate, nitrogen can not be diffused into base substrate inside and silicon nitride generates the technological deficiency that is mainly present in billet surface effectively.
Therefore, of the present invention with short production cycle high with production efficiency, prepared silicon nitride combined silicon carbide matrix material thing is evenly distributed mutually, not only has higher intensity, and has good heat-shock resistance, oxidation-resistance, high-temperature creep resistance and erosion-resisting characteristics.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, not the restriction to its protection domain.
For avoiding repetition, now the related technical parameter unification of this embodiment is described below, in embodiment, repeat no more:
The particle diameter of described silicon-carbide particle is 7 ~ 0.1mm, the SiC content >=95wt% of silicon-carbide particle.
The particle diameter of described carborundum powder is 5 ~ 100 μ m, the SiC content >=95wt% of carborundum powder.
The particle diameter of described simple substance silica flour is 5 ~ 100 μ m, the Si content >=95wt% of simple substance silica flour
Purity >=the 99.9Vol% of described nitrogen.
embodiment 1
A kind of microwave sintering legal system of using is for the method for silicon nitride combined silicon carbide matrix material.First the simple substance silica flour of the carborundum powder of the silicon-carbide particle of 50 ~ 60wt%, 20 ~ 25wt%, 15 ~ 30wt%, the carboxymethyl cellulose of 1 ~ 2wt% and the water of 1 ~ 3wt% are mixed to moulding.Base substrate after moulding is inserted in vacuum microwave sintering oven, first be evacuated to the pressure≤20Pa in described microwave agglomerating furnace, be filled with nitrogen, then sintering 0.5 ~ 1.5 hour under nitrogen atmosphere and 1300 ~ 1400 ℃ of conditions, obtains silicon nitride combined silicon carbide matrix material again.
embodiment 2
A kind of microwave sintering legal system of using is for the method for silicon nitride combined silicon carbide matrix material.First the simple substance silica flour of the carborundum powder of the silicon-carbide particle of 60 ~ 70wt%, 10 ~ 20wt%, 10 ~ 25wt%, the carboxymethyl cellulose of 3 ~ 4wt% and the water of 4 ~ 5wt% are mixed to moulding.Base substrate after moulding is inserted in vacuum microwave sintering oven, first be evacuated to the pressure≤20Pa in described microwave agglomerating furnace, be filled with nitrogen, then sintering 1.5 ~ 3.0 hours under nitrogen atmosphere and 1400 ~ 1500 ℃ of conditions, obtains silicon nitride combined silicon carbide matrix material again.
embodiment 3
A kind of microwave sintering legal system of using is for the method for silicon nitride combined silicon carbide matrix material.First the simple substance silica flour of the carborundum powder of the silicon-carbide particle of 70 ~ 80wt%, 5 ~ 10wt%, 5 ~ 20wt%, the carboxymethyl cellulose of 2 ~ 3wt% and the water of 3 ~ 4wt% are mixed to moulding.Base substrate after moulding is inserted in vacuum microwave sintering oven, first be evacuated to the pressure≤20Pa in described microwave agglomerating furnace, be filled with nitrogen, then sintering 3 ~ 5 hours under nitrogen atmosphere and 1500 ~ 1600 ℃ of conditions, obtains silicon nitride combined silicon carbide matrix material again.
This embodiment compared with prior art has following positively effect:
This embodiment, by the method for microwave sintering, is utilized catalysis and the non-thermal effect of microwave, promotes the solid phase diffusion between material, and the density of the finished product and mechanical property are apparently higher than normal sintering product; Meanwhile, microwave radiation can promote densification, promotes grain growing, accelerates the effects such as chemical reaction.In sintering, microwave, not only as a kind of heating energy source, is also a kind of activated sintering process.High-frequency electrical field energy promotes the migration in the charged room of Grain Surface, thereby crystal grain is produced, is similar to the viscous deformation that diffusion is wriggled, thereby has promoted the carrying out of sintering.And microwave sintering heat-up rate is fast, sintering time is short, can significantly improve production efficiency.
Most importantly, this embodiment is when microwave sintering, material is from inside, to start to heat up and heating, first the process that so just makes elemental silicon and nitrogen reaction produce silicon nitride is started by inside, prolongation along with sintering time, the generation of silicon nitride is carried out to outside by inside gradually, and after sintering process finishes, silicon nitride is evenly distributed in composite inner mutually.This embodiment can overcome that volume effect that the silicon nitride due to billet surface that conventional sintering technique causes generates causes pore in base substrate to stop up, nitrogen can not be diffused into base substrate inside and silicon nitride generates the technological deficiency that is mainly present in billet surface effectively.
Therefore, with short production cycle and the production efficiency of this embodiment is high, prepared silicon nitride combined silicon carbide matrix material thing is evenly distributed mutually, not only has higher intensity, and has good heat-shock resistance, oxidation-resistance, high-temperature creep resistance and erosion-resisting characteristics.
Claims (5)
- One kind by microwave sintering legal system the method for silicon nitride combined silicon carbide matrix material, it is characterized in that first the water of the carboxymethyl cellulose of the simple substance silica flour of the carborundum powder of the silicon-carbide particle of 50 ~ 80wt%, 5 ~ 25wt%, 5 ~ 30wt%, 1 ~ 4wt% and 1 ~ 5wt % being mixed moulding;Base substrate after moulding is inserted in vacuum microwave sintering oven, first be evacuated to the pressure≤20Pa in described microwave agglomerating furnace, be filled with nitrogen, then sintering 0.5 ~ 5 hour under nitrogen atmosphere and 1300 ~ 1600 ℃ of conditions, obtains silicon nitride combined silicon carbide matrix material again.
- 2. the microwave sintering legal system of using according to claim 1 is for the method for silicon nitride combined silicon carbide matrix material, and the particle diameter that it is characterized in that described silicon-carbide particle is 7 ~ 0.1mm, the SiC content >=95wt% of silicon-carbide particle.
- 3. the microwave sintering legal system of using according to claim 1 is for the method for silicon nitride combined silicon carbide matrix material, and the particle diameter that it is characterized in that described carborundum powder is 5 ~ 100 μ m, the SiC content >=95wt% of carborundum powder.
- 4. the microwave sintering legal system of using according to claim 1 is for the method for silicon nitride combined silicon carbide matrix material, and the particle diameter that it is characterized in that described simple substance silica flour is 5 ~ 100 μ m, the Si content >=95wt% of simple substance silica flour.
- 5. the microwave sintering legal system of using according to claim 1, for the method for silicon nitride combined silicon carbide matrix material, is characterized in that the purity >=99.9Vol% of described nitrogen.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104446637A (en) * | 2014-12-08 | 2015-03-25 | 武汉科技大学 | Silicon nitride combined silicon carbide material based on molten salt medium pore-forming and preparation method of material |
| CN106083055A (en) * | 2016-06-08 | 2016-11-09 | 武汉钢铁股份有限公司 | A kind of annular furnace Si N Al C complex fire resistant ceramics furnace base plate and preparation method |
| CN109400189A (en) * | 2018-11-30 | 2019-03-01 | 河南华西耐火材料有限公司 | A kind of blast furnace crucibe nitrogen composite casting material and preparation method thereof |
| CN109503171A (en) * | 2018-12-18 | 2019-03-22 | 宜兴高等职业技术学校 | A kind of silicon nitride combined silicon carbide brick and preparation method thereof |
| CN115231925A (en) * | 2022-07-20 | 2022-10-25 | 洛阳理工学院 | Method for preparing calcium hexaluminate combined silicon carbide ceramic by microwave |
| CN116178026A (en) * | 2022-12-05 | 2023-05-30 | 山西华钠碳能科技有限责任公司 | Sagger for sintering battery material and preparation method and application thereof |
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| CN1131134A (en) * | 1995-03-10 | 1996-09-18 | 薛天瑞 | Method for producing high strength silicon nitride products based on silicon carbide |
| CN1609057A (en) * | 2004-11-12 | 2005-04-27 | 清华大学 | Fast microwave sintering process of combined silicon nitride-silicon carbide refractorg material |
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2014
- 2014-08-18 CN CN201410405551.6A patent/CN104177087A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1131134A (en) * | 1995-03-10 | 1996-09-18 | 薛天瑞 | Method for producing high strength silicon nitride products based on silicon carbide |
| CN1609057A (en) * | 2004-11-12 | 2005-04-27 | 清华大学 | Fast microwave sintering process of combined silicon nitride-silicon carbide refractorg material |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104446637A (en) * | 2014-12-08 | 2015-03-25 | 武汉科技大学 | Silicon nitride combined silicon carbide material based on molten salt medium pore-forming and preparation method of material |
| CN106083055A (en) * | 2016-06-08 | 2016-11-09 | 武汉钢铁股份有限公司 | A kind of annular furnace Si N Al C complex fire resistant ceramics furnace base plate and preparation method |
| CN109400189A (en) * | 2018-11-30 | 2019-03-01 | 河南华西耐火材料有限公司 | A kind of blast furnace crucibe nitrogen composite casting material and preparation method thereof |
| CN109503171A (en) * | 2018-12-18 | 2019-03-22 | 宜兴高等职业技术学校 | A kind of silicon nitride combined silicon carbide brick and preparation method thereof |
| CN115231925A (en) * | 2022-07-20 | 2022-10-25 | 洛阳理工学院 | Method for preparing calcium hexaluminate combined silicon carbide ceramic by microwave |
| CN116178026A (en) * | 2022-12-05 | 2023-05-30 | 山西华钠碳能科技有限责任公司 | Sagger for sintering battery material and preparation method and application thereof |
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Application publication date: 20141203 |