CN109265179A - A kind of silicon nitride material - Google Patents

A kind of silicon nitride material Download PDF

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Publication number
CN109265179A
CN109265179A CN201811441790.1A CN201811441790A CN109265179A CN 109265179 A CN109265179 A CN 109265179A CN 201811441790 A CN201811441790 A CN 201811441790A CN 109265179 A CN109265179 A CN 109265179A
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silicon nitride
oxide
nitride material
average grain
grain diameter
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吴强德
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Jiaxing Chai Fuel Technology Co Ltd
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Jiaxing Chai Fuel Technology Co Ltd
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Abstract

The present invention relates to a kind of silicon nitride material, the silicon nitride material is made of each raw material of following weight percent: silicon nitride 70~85%, nano-silicon nitride 5~15%, catalyst 8~15% and tungsten carbide 0.5~5%；The preparation method of thermal insulating disc cover made of the silicon nitride material, comprising the following steps: weigh silicon nitride, nano-silicon nitride, sintering aid and tungsten carbide by above-mentioned weight percent, ball milling mixing is uniform；Base-material is made in mixing drying；After compression moulding, tubular biscuit is obtained；Appropriate size is processed on lathe；The biscuit processed is put into sintering furnace, nitrogen sintering is filled with；Stop heating, cooling opens fire door in normal pressure, and natural cooling obtains blank；Blank is carried out to end face processing on grinding machine to get finished product.

Description

A kind of silicon nitride material
Technical field
The present invention relates to a kind of silicon nitride material, inolrganic chemicals technical fields.
Background technique
International photovoltaic industry is being grown rapidly, and polysilicon market is in the ascendant.Currently, along with the production of polysilicon, The processing problem of silicon tetrachloride in process tail gas is increasingly prominent, it is possible to create serious problem of environmental pollution.Simultaneously with city Field intensified competition, promotes manufacturer constantly to pay attention to recycling for silicon tetrachloride.
Processing unit of the polysilicon hydrogenation furnace as process tail gas, process conditions are very harsh.Silicon tetrachloride need to be It is reacted under 1200 DEG C of high temperature, in-furnace temperature may instantaneously reach 1400 DEG C.Electrode is needed in 100 DEG C or less the normal works of ability simultaneously Make, this 1100 DEG C or so temperature difference improves very high requirement to the material of the thermal insulating disc cover of guard electrode.Industry generally uses Quartz, aluminium oxide and silicon nitride material.Quartz has phase transformation at 1200 DEG C or so and volume is caused to vary widely, and aluminium oxide is due to it Thermal expansion coefficient it is larger can not long period high frequency time bear so high temperature gradient, the two reasons and lead to thermal insulating disc cover Frequently replacement.Although the silicon nitride heat shield disk service life of external import is long, selling at exorbitant prices, Lead Time is long, can not be at home Market is universal to be used.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of silicon nitride materials.
The technical scheme to solve the above technical problems is that a kind of silicon nitride material, the silicon nitride material by Each raw material of following weight percent forms: silicon nitride 70~85%, nano-silicon nitride 5~15%, catalyst 8~15% and carbon Change tungsten 0.5~5%.
Silicon nitride material beneficial effect of the present invention is: nano-silicon nitride can enable after being added must silicon nitride surface It increases, interparticle contact area increases, and diffusion length is short, and solution modeling is also relatively easy；Excessive nano-silicon nitride will lead to Bad grasp is shunk, while cost can be increased, so control is advisable in 15%；The catalyst contained, is on the one hand capable of providing The liquid phase of good fluidity promotes silicon nitride sintering, on the other hand can be precipitated from the glass phase of silicon nitride crystal boundary in cooling high The crystal of fusing point improves the elevated temperature strength of silicon nitride.
Based on the above technical solution, the present invention can also be improved as follows.
Further, the average grain diameter of the common silicon nitride is 0.1~5 μm, the average grain diameter < of the nano-silicon nitride 100nm, 2 μm of the average grain diameter < of the tungsten carbide.
Beneficial effect using above-mentioned further scheme is can to stay in nitridation silicon wafer using the tungsten carbide of submicron order On the one hand boundary inhibits the abnormal growth of silicon nitride grain, on the other hand improves the elevated temperature strength of crystal boundary.
Further, the catalyst by weight percent metal oxide 20~80% and rare earth oxide 20~80% Composition.
Beneficial effect using above-mentioned further scheme is, on the one hand can lower silicon nitride sintering when the temperature that occurs of liquid phase, Promote the sintering densification process of beta-silicon nitride powder；On the other hand, the addition of rare earth oxide can change liquid phase generated Viscosity, promote the generation of needle-shaped silicon nitride grain, improve the intensity and toughness of silicon nitride.
Further, the metal oxide is aluminium oxide and/or magnesia, and the rare earth oxide is yttrium oxide, oxidation One of ytterbium, cerium oxide, lanthana or samarium oxide or any several mixture.
Beneficial effect using above-mentioned further scheme be formed by liquid phase in temperature-fall period can with fusing point compared with High crystalline solid is precipitated, to improve the elevated temperature strength of Grain-Boundary Phase.
Further, 5 μm of average grain diameter < of the aluminium oxide or magnesia, 5 μ of average grain diameter < of the rare earth oxide m。
Beneficial effect using above-mentioned further scheme is, on the one hand, is easier to broken form new table in high-energy ball milling The sintering activity of powder is improved in face, promotes the formation of liquid phase；On the other hand, it can be uniformly mixed with silicon nitride powder, reduce nitrogen The component segregation of SiClx.
Further, the average grain diameter of the tungsten carbide is 0.1~1 μm.
Beneficial effect using above-mentioned further scheme is, stays in silicon nitride crystal boundary using size in the numberical range Tungsten carbide can best inhibit the abnormal growth of silicon nitride grain, improve the elevated temperature strength of crystal boundary.
Specific embodiment
Embodiment 1
Each raw material: silicon nitride (average grain diameter is 0.1~5 μm) 80%, nano silicon nitride is weighed by weight percent below Silicon (average grain diameter < 100nm) 7%, catalyst are Al2O3 (5 μm of average grain diameter <) 4%, Y2O36%, tungsten carbide (average grain 5 μm of diameter <) it is 0.5%, it puts it into high-strength aluminum oxide ceramic container, the high straight alcohol of solvent is added, is put into silicon nitride abrading-ball, Roller ball mill 30 hours, mixing was placed in 120 DEG C of temperature of baking oven and dries, and sundries is weeded out after drying, be placed in rubber mold into Row cold isostatic compaction, briquetting pressure 180MPa, obtains biscuit.Biscuit is put into sintering after being machined to accurate dimension on lathe Heat up pressure sintering in a nitrogen atmosphere in furnace.Specific temperature-rise period are as follows: when temperature rises to 1350 DEG C, pressure adds to 0.4MPa, It is kept for 30 minutes, when being continuously heating to 1800 DEG C, pressure adds to 5MPa, is kept for 2 hours.Stop heating, cools to 150 DEG C with the furnace When release, obtain blank after natural cooling.Then bed processing end face is regrinded, so that its end face is met tolerance fit, obtains i.e. finished product.
Through examining, the technical indicator of thermal insulating disc cover obtained are as follows: bending strength 700MPa, fracture toughness 7.1MPa M1/2, density are not less than 3.21g/cm3, hardness HRA92.6.
Embodiment 2
Each raw material: silicon nitride 65%, nano-silicon nitride 15%, catalyst: Al2O3 are weighed by weight percent below 8%, La2O3 (5 μm of average grain diameter <) 7%, tungsten carbide (5 μm of average grain diameter <) are 5%, and the high straight alcohol of solvent is added, is added The grinding agent polyethylene glycol of total mass of raw material 1% is put into aluminium oxide abrading-ball, and roller ball mill 40 hours, mixing was placed in 80 DEG C of temperature Baking oven in dry, sundries is weeded out after drying.Cold isostatic compaction is carried out in base-material merging polyurethane mould, briquetting pressure is 200MPa obtains biscuit.Biscuit is put into sintering furnace heating pressurization in a nitrogen atmosphere after being machined to accurate dimension on lathe Sintering.Specific temperature-rise period are as follows: when temperature rises to 1400 DEG C, pressure adds to 1MPa, is kept for 30 minutes, is continuously heating to 1850 DEG C When, pressure adds to 3MPa, is kept for 2 hours.Stop heating, release when cooling to 150 DEG C with the furnace, obtains blank after natural cooling. Then bed processing end face is regrinded, its end face is made to meet tolerance fit to get finished product.
Through examining, the technical indicator of thermal insulating disc cover obtained are as follows: bending strength 800MPa, fracture toughness 5.5MPa M1/2, density are not less than 3.27g/cm3, hardness HRA92.1.
Embodiment 3
Each raw material: silicon nitride 74%, nano-silicon nitride 12%, catalyst: MgO2 are weighed by weight percent below 6%, the high straight alcohol of solvent is added in CeO2 (5 μm of average grain diameter <) 6%, tungsten carbide 1%, and distilled water is added, and it is total that raw material is added The grinding agent polyethylene glycol of quality 1% places into aluminium oxide abrading-ball, and roller ball mill 20 hours, mixing was placed in 180 DEG C of temperature of baking It is dried in case, sundries is weeded out after drying.Cold isostatic compaction is carried out in base-material merging polyurethane mould, briquetting pressure is 120MPa obtains biscuit.Biscuit is put into sintering furnace heating pressurization in a nitrogen atmosphere after being machined to accurate dimension on lathe Sintering.Specific temperature-rise period are as follows: when temperature rises to 1500 DEG C, pressure adds to 1MPa, is kept for 60 minutes, is continuously heating to 1900 DEG C When, pressure adds to 3MPa, is kept for 3 hours.Stop heating, release when cooling to 150 DEG C with the furnace, obtains blank after natural cooling. Then bed processing end face is regrinded, its end face is made to meet tolerance fit to get finished product.
Through examining, the technical indicator of thermal insulating disc cover obtained are as follows: bending strength 800MPa, fracture toughness 9.3MPa M1/2, density are not less than 3.20g/cm3, hardness HRA91.3.
Embodiment 4
Each raw material: silicon nitride 85% is weighed by weight percent below, nano-silicon nitride 5%, catalyst: The high straight alcohol of solvent is added in Al2O35%, Yb2O3 (5 μm of average grain diameter <) 3%, tungsten carbide 2%, and total mass of raw material is added 3% grinding agent polyvinyl alcohol is put into aluminium oxide abrading-ball, and Ball-stirring mill ball milling 3 hours, mixing obtained base after being spray-dried Material.Cold isostatic compaction is carried out in base-material merging polyurethane mould, briquetting pressure 200MPa obtains biscuit.Biscuit is in lathe On be machined to accurate dimension after be put into sintering furnace the pressure sintering that heats up in a nitrogen atmosphere.Specific temperature-rise period are as follows: temperature liter When to 1480 DEG C, pressure adds to 1MPa, is kept for 20 minutes, and when being continuously heating to 1750 DEG C, pressure adds to 3MPa, is kept for 2 hours. Stop heating, release when cooling to 150 DEG C with the furnace, obtains blank after natural cooling.Then bed processing end face is regrinded, its end face is made Meet tolerance fit to get finished product.
Through examining, the technical indicator of thermal insulating disc cover obtained are as follows: bending strength 800MPa, fracture toughness 6.0MPa M1/2, density are not less than 3.20g/cm3, hardness HRA91.6.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims (5)

1. a kind of silicon nitride material, which is characterized in that the silicon nitride material is made of each raw material of following weight percent: nitrogen SiClx 70~85%, nano-silicon nitride 5~15%, catalyst 8~15% and tungsten carbide 0.5~5%.
2. silicon nitride material according to claim 1, which is characterized in that the average grain diameter of the common silicon nitride is 0.1 ~5 μm, the average grain diameter < 100nm of the nano-silicon nitride, 2 μm of the average grain diameter < of the tungsten carbide.
3. silicon nitride material according to claim 1, which is characterized in that the sintering aid by weight percent metal Oxide 20~80% and rare earth oxide 20~80% form.
4. silicon nitride material according to claim 3, which is characterized in that the metal oxide is aluminium oxide and/or oxygen Change magnesium, the rare earth oxide is one of yttrium oxide, ytterbium oxide, cerium oxide, lanthana or samarium oxide or any several Mixture.
5. silicon nitride material according to claim 4, which is characterized in that the average grain diameter < of the aluminium oxide or magnesia 5 μm, 5 μm of the average grain diameter < of the rare earth oxide.
CN201811441790.1A 2018-11-29 2018-11-29 A kind of silicon nitride material Withdrawn CN109265179A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109678524A (en) * 2019-02-22 2019-04-26 苏州玄陶商务咨询有限公司 A kind of silicon nitride ceramics implantation material and preparation method thereof that performance is controllable
CN111196727A (en) * 2019-11-20 2020-05-26 中国科学院上海硅酸盐研究所 High-thermal-conductivity silicon nitride ceramic material and preparation method thereof
CN117819987A (en) * 2024-03-05 2024-04-05 呼伦贝尔市汇博环保科技有限公司 Method for preparing ceramic material by utilizing hazardous waste tail gas in polysilicon production

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109678524A (en) * 2019-02-22 2019-04-26 苏州玄陶商务咨询有限公司 A kind of silicon nitride ceramics implantation material and preparation method thereof that performance is controllable
CN109678524B (en) * 2019-02-22 2021-08-24 苏州玄陶商务咨询有限公司 Silicon nitride ceramic implant with controllable performance and preparation method thereof
CN111196727A (en) * 2019-11-20 2020-05-26 中国科学院上海硅酸盐研究所 High-thermal-conductivity silicon nitride ceramic material and preparation method thereof
CN111196727B (en) * 2019-11-20 2022-05-10 中国科学院上海硅酸盐研究所 High-thermal-conductivity silicon nitride ceramic material and preparation method thereof
CN117819987A (en) * 2024-03-05 2024-04-05 呼伦贝尔市汇博环保科技有限公司 Method for preparing ceramic material by utilizing hazardous waste tail gas in polysilicon production
CN117819987B (en) * 2024-03-05 2024-05-14 呼伦贝尔市汇博环保科技有限公司 Method for preparing ceramic material by utilizing hazardous waste tail gas in polysilicon production

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Application publication date: 20190125