CN105819450A - Silicon nitride ceramic tail gas hood for polycrystalline silicon reducing furnace and preparation method of tail gas hood - Google Patents
Silicon nitride ceramic tail gas hood for polycrystalline silicon reducing furnace and preparation method of tail gas hood Download PDFInfo
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Abstract
The invention relates to a silicon nitride ceramic tail gas hood for a polycrystalline silicon reducing furnace and a preparation method of the tail gas hood. The preparation method comprises the steps that 80%-92% of silicon nitride powder and 8%-20% of a sintering auxiliary are weighed by weight, wet-mixed through ethyl alcohol and refined until the size of all granules is smaller than 1 micrometer, spray granulation is conducted, and the granules obtained through spray serve as raw materials for preparing the silicon nitride ceramic tail gas hood; the granules obtained through spray are subjected to dry pressing by a hydraulic machine and then subjected to isostatic cool pressing to obtain a pipe-barrel-shaped green body with a bottom, the green body is placed in a degumming sintering furnace to be presintered after being dried, green body milling is conducted, grooves or holes are formed in the cylindrical side wall, the green body is placed in an air pressure sintering furnace to be sintered, the sintered ceramic green body is subjected to finish machining, and then the finished silicon nitride ceramic tail gas hood is obtained. Compared with the prior art, the tail gas hood has the advantages of resisting high temperature, corrosion, thermal shock and the like, cannot generate harmful impurities and can ensure the purity of a polycrystalline silicon product.
Description
Technical field
The present invention relates to a kind of polycrystalline silicon reducing furnace tail gas cover, especially relate to a kind of polycrystalline silicon reducing furnace silicon nitride ceramics tail gas cover and preparation method thereof.
Background technology
Increasing along with China environmental protection dynamics, the application of clean energy resource increasingly comes into one's own, photovoltaic generation is installed more and more at home, wherein polysilicon domestic production capacity is in continuous expansion, produce polysilicon and have three kinds of techniques, domestic production polysilicon producer commonly used improved Siemens technique at present, its ultimate principle is with the high-purity hydrogen high-purity trichlorosilane of reduction on the HIGH-PURITY SILICON core of about 1100 DEG C, the polysilicon deposition generated is on silicon core, a large amount of hydrogen chloride is produced in reduction process, the products such as Silicon chloride., this production technology produces polysilicon process compared with other and has energy-conservation, the advantages such as consumption reduction.It is that hydrogen reacts polycrystalline silicon reducing furnace that improved Siemens produces the key equipment of polysilicon, in reduction furnace, high-purity trichlorosilane reduces in hydrogen atmosphere and generates polysilicon, it is slow with hydrogen reaction rate, about about 1/3rd participate in reaction every time, generate polysilicon, remaining is discharged from reduction furnace tail gas hole together with byproduct hydrogen chloride, Silicon chloride. and the hydrogen produced, return to blood circulation participates in again reduction reaction, it is made fully to be utilized, reduce trash discharge, effectively control to pollute.
Improved Siemens produces the key equipment of polysilicon at present is that hydrogen reacts polycrystalline silicon reducing furnace, its tail gas hole is most on polycrystalline silicon reduction furnace base plate, several tail gas holes are had on general chassis, simultaneously in producing polysilicon process, the most often occurring silicon rod rod problem in stove, the little silico briquette fallen down is easily advanced into tail gas hole, blocking tail gas hole, circular response is caused to be normally carried out, in order to avoid this problem occurs, therefore general one tail gas closure assembly of installation on tail gas hole.
Tail gas cover generally uses mesh-like structure, material generally uses rustless steel or alloy material, owing to having a large amount of high temperature corrosion gas by tail gas hole during there is reduction reaction in stove, rustless steel or alloy material are corroded, and the life-span is the shortest, need often to change, cost is the highest, and easily produce objectionable impurities, take in burner hearth, have influence on the quality of polysilicon.
Chinese patent CN203890069U discloses a kind of labyrinth type high purity graphite tail gas cover, is used for discharging polysilicon reducing furnace tail gas and settling oarse-grained free silica.Described labyrinth type tail gas cover includes outer housing and inner cover two parts；Described tail gas cover has labyrinth type gas channel；Described outer housing is top closure, plays the rounding tubular that on top end face certain depth, milling is empty from bottom face, and outer housing bottom has the air inlet that multiple circumference is uniform；The rounded pipeline of described inner cover, its underpart inserts interface with concentric locating outer housing and the boss structure of inner cover, its bottom with offgas duct；Outer housing forms silicon grain storing ring after assembling with inner cover at boss；The air-flow forming certain lift between outer housing inwall and interior cover outer wall rises circuit；Form air-flow circuit of turning back between inner cover top end face and outer housing roof and air-flow is introduced exhaust pipe.This patent carries out new structure design to tail gas cover, and the raw material of employing is high purity graphite, and on the one hand price is higher, is on the other hand difficult to machine-shaping.
For solving this problem, need to research and develop the polycrystalline silicon reducing furnace tail gas cover of a kind of suitable material.
Summary of the invention
Defect that the purpose of the present invention is contemplated to overcome above-mentioned prior art to exist and polycrystalline silicon reducing furnace silicon nitride ceramics tail gas cover of a kind of high temperature resistant, corrosion-resistant, anti-thermal shock and preparation method thereof is provided.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of polycrystalline silicon reducing furnace silicon nitride ceramics tail gas cover, including the raw material of following weight percentage: silicon nitride powder 80～92%, sintering aid 8～20%.
Described silicon nitride powder is α phase silicon nitride, and described α phase silicon nitride α phase content is more than 92%.The mean diameter of described α phase silicon nitride is 0.01～1.5um.
Described sintering aid is nanometer level RE oxide or nanosize metal oxide.The combination of one or more in lanthana, yittrium oxide, cerium oxide or tantalum oxide of the described rare earth oxide；One or both the combination in aluminium oxide or magnesium oxide of the described metal-oxide；Described metal-oxide or the purity of rare earth oxide are more than or equal to 99.99%.
The preparation method of described polycrystalline silicon reducing furnace silicon nitride ceramics tail gas cover, comprises the following steps:
(1) according to the percentage by weight following raw material of weighing: silicon nitride powder 80～92%, sintering aid 8～20%, it is 30～50wt% through ethanol wet-mixed, control slip content, micronization processes 30～60 hours, to particle diameter all less than 1um, mist projection granulating, after pelletize, particle diameter is 30～200um, and spraying gained particle is as the raw material preparing silicon nitride ceramics tail gas cover；
(2) by dry-pressing formed through hydraulic press for above-mentioned spraying gained particle, the most again through cold isostatic compaction, obtain the foim base substrate at the bottom of band, by (being dried more than 12 hours in the baking oven of 150 DEG C) after body drying, it is placed on presintering in degumming sintering furnace, then carries out biscuit Milling Machining, in cylinder side wall fluting or hole, it is placed on sintering in gas pressure sintering stove again, the most again the ceramic body after sintering is carried out polish, i.e. obtain silicon nitride ceramics tail gas cover finished product.
Micronization processes includes Ball-stirring mill and ball milling.
Described cold isostatic compaction pressure is 180～250Mpa.
In degumming sintering furnace, the temperature of presintering is 1100～1250 DEG C.
In air pressure stove, the condition of sintering is: sintering temperature is 1700～1850 DEG C, sinters 2～4 hours in 3-8MPa nitrogen atmosphere.
Polish device therefor is surface grinding machine, universal cutter grinder and brill Milling Machining center, and after polish, final surface roughness requirements is at below 1.6um.
Compared with prior art, the present invention has the following advantages and beneficial effect:
1, silicon nitride ceramic material has the characteristics such as high temperature resistant, corrosion-resistant, anti-thermal shock, can be greatly prolonged service life 1100 DEG C of normal uses, and the life-span, at least more than 1 year, reduces maintenance of equipment rate.
2, the present invention uses silicon nitride ceramics as tail gas cover material, will not produce objectionable impurities, it is ensured that the purity of polysilicon product.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
Take α phase silicon nitride raw material 1600 grams, α phase content is 93%, mean diameter 0.9um, adds 160 grams of (purity 99.99% of yittrium oxide, mean diameter 90nm), 40 grams of (purity 99.99% of cerium oxide, mean diameter 70nm), aluminium oxide 200 grams (purity 99.99%, mean diameter 80nm), through ethanol wet-mixed, ethanol addition at 4.5 kilograms, micronization processes 40 hours, detection particle diameter, at 0.8um, is then spray-dried；After pelletize, raw material particle size is at 50-180um, then is loaded in rubber mold by the raw material handled well, seals, carries out cold isostatic compaction, is pressed into the foim base substrate at the bottom of band.Briquetting pressure is 220MPa, next the biscuit of the silicon nitride ceramics tail gas cover suppressed is placed 150 DEG C of baking ovens 18 hours, it is then placed within presintering in degumming sintering furnace, sintering temperature 1100 DEG C, takes out after cooling, it is placed on Milling Machining center, lateral walls at presintering pipe fitting etc. point fluting (or hole), are then charged into gas pressure sintering stove, carry out gas pressure sintering, sintering temperature is at 1820 DEG C, and nitrogen pressure is at 5Mpa.Maximum temperature sintering time is 4 hours, and the silicon nitride base substrate after sintering carries out surface grinding machine processing plane, universal cutter grinder chamfering, grinding machine of universal processing inside and outside circle, makes surface roughness be worked into 1.6um.
Through inspection silicon nitride ceramics tail gas cover technical specification: density reaches solid density 98.9%, hardness 1490MPa, bending strength 800MPa, reach to design requirement.
Embodiment 2
Take α phase silicon nitride raw material 1650 grams, α phase content is 94%, mean diameter 0.8um, adds 200 grams of (purity 99.99% of yittrium oxide, mean diameter 90nm), 50 grams of (purity 99.99% of cerium oxide, mean diameter 70nm), magnesium oxide 100 grams (purity 99.99%, mean diameter 60nm), through ethanol wet-mixed, ethanol addition at 4 kilograms, micronization processes 35 hours, detection particle diameter, at 0.7um, is then spray-dried；After pelletize, raw material particle size is at 30-150um, then is loaded in rubber mold by the raw material handled well, seals, carries out cold isostatic compaction, is pressed into the foim at the bottom of band.Briquetting pressure is 200MPa, next the biscuit of the silicon nitride ceramics tail gas cover suppressed is placed 150 DEG C of baking ovens 24 hours, it is then placed within presintering in degumming sintering furnace, sintering temperature 1150 DEG C, takes out after cooling, it is placed on Milling Machining center, lateral walls at presintering pipe fitting etc. point fluting (or hole), are then charged into gas pressure sintering stove, carry out gas pressure sintering, sintering temperature is at 1850 DEG C, and nitrogen pressure is at 6Mpa.Maximum temperature sintering time is 3 hours, and the silicon nitride base substrate after sintering carries out surface grinding machine processing plane, universal cutter grinder chamfering, grinding machine of universal processing inside and outside circle, makes surface roughness be worked into 1.6um.
Through inspection silicon nitride ceramics tail gas cover technical specification: density reaches solid density 98.9%, hardness 1510MPa, bending strength 750MPa, reach to design requirement.
Embodiment 3
Take α phase silicon nitride raw material 1700 grams, α phase content is 92%, mean diameter 0.85um, add 150 grams of (purity 99.99% of yittrium oxide, mean diameter 90nm), 50 grams of (purity 99.99% of cerium oxide, mean diameter 70nm), 50 grams of (purity 99.99% of magnesium oxide, mean diameter 40nm) and 50 grams of (purity 99.99% of aluminium oxide, mean diameter 50nm), through ethanol wet-mixed, ethanol addition at 4.1 kilograms, micronization processes 4 hours, detection particle diameter, at 0.85um, is then spray-dried；After pelletize, raw material particle size is at 40-150um, then is loaded in rubber mold by the raw material handled well, seals, carries out cold isostatic compaction, is pressed into the foim base substrate at the bottom of band.Briquetting pressure is 240MPa, next the biscuit of the silicon nitride ceramics tail gas cover suppressed is placed 150 DEG C of baking ovens 36 hours, it is then placed within presintering in degumming sintering furnace, sintering temperature 1130 DEG C, takes out after cooling, it is placed on Milling Machining center, lateral walls at presintering pipe fitting etc. point fluting (or hole), are then charged into gas pressure sintering stove, carry out gas pressure sintering, sintering temperature is at 1820 DEG C, and nitrogen pressure is at 4Mpa.Maximum temperature sintering time is 4 hours, and the silicon nitride base substrate after sintering carries out surface grinding machine processing plane, universal cutter grinder chamfering, grinding machine of universal processing inside and outside circle, makes surface roughness be worked into 1.6um.
Through inspection silicon nitride ceramics tail gas cover technical specification: density reaches solid density 98.9%, hardness 1500MPa, bending strength 760MPa, reach to design requirement.
The above-mentioned description to embodiment is to be understood that for ease of those skilled in the art and use invention.These embodiments obviously easily can be made various amendment by person skilled in the art, and General Principle described herein is applied in other embodiments without through performing creative labour.Therefore, the invention is not restricted to above-described embodiment, those skilled in the art should be within protection scope of the present invention according to the announcement of the present invention, the improvement made without departing from scope and amendment.
Claims (10)
1. a polycrystalline silicon reducing furnace silicon nitride ceramics tail gas cover, it is characterised in that include the raw material of following weight percentage: silicon nitride powder 80～92%, sintering aid 8～20%.
A kind of polycrystalline silicon reducing furnace silicon nitride ceramics tail gas cover the most according to claim 1, it is characterised in that described silicon nitride powder is α phase silicon nitride, and described α phase silicon nitride α phase content is more than 92%.
A kind of polycrystalline silicon reducing furnace silicon nitride ceramics tail gas cover the most according to claim 2, it is characterised in that the mean diameter of described α phase silicon nitride is 0.01～1.5um.
A kind of polycrystalline silicon reducing furnace silicon nitride ceramics tail gas cover the most according to claim 1, it is characterised in that described sintering aid is nanometer level RE oxide or nanosize metal oxide.
A kind of polycrystalline silicon reducing furnace silicon nitride ceramics tail gas cover the most according to claim 4, it is characterised in that the described rare earth oxide combination of one or more in lanthana, yittrium oxide, cerium oxide or tantalum oxide；One or both the combination in aluminium oxide or magnesium oxide of the described metal-oxide；Described metal-oxide or the purity of rare earth oxide are more than or equal to 99.99%.
6. the preparation method of a polycrystalline silicon reducing furnace silicon nitride ceramics tail gas cover as claimed in claim 1, it is characterised in that comprise the following steps:
(1) according to the percentage by weight following raw material of weighing: silicon nitride powder 80～92%, sintering aid 8～20%, it is 30～50wt% through ethanol wet-mixed, control slip content, micronization processes 30～60 hours, to particle diameter all less than 1um, mist projection granulating, after pelletize, particle diameter is 30～200um, and spraying gained particle is as the raw material preparing silicon nitride ceramics tail gas cover；
(2) by dry-pressing formed through hydraulic press for above-mentioned spraying gained particle, the most again through cold isostatic compaction, obtain the foim base substrate at the bottom of band, after body drying, it is placed on presintering in degumming sintering furnace, then carries out biscuit Milling Machining, in cylinder side wall fluting or hole, it is placed on sintering in gas pressure sintering stove again, the most again the ceramic body after sintering is carried out polish, i.e. obtain silicon nitride ceramics tail gas cover finished product.
The preparation method of a kind of polycrystalline silicon reducing furnace silicon nitride ceramics tail gas cover the most according to claim 6, it is characterised in that described cold isostatic compaction pressure is 180～250Mpa.
The preparation method of a kind of polycrystalline silicon reducing furnace silicon nitride ceramics tail gas cover the most according to claim 6, it is characterised in that in degumming sintering furnace, the temperature of presintering is 1100～1250 DEG C.
The preparation method of a kind of polycrystalline silicon reducing furnace silicon nitride ceramics tail gas cover the most according to claim 6, it is characterised in that the condition of sintering is in air pressure stove: sintering temperature is 1700～1850 DEG C, sinters 2～4 hours in 3-8MPa nitrogen atmosphere.
The preparation method of a kind of polycrystalline silicon reducing furnace silicon nitride ceramics tail gas cover the most according to claim 6, it is characterised in that after polish, final surface roughness requirements is at below 1.6um.
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| CN201610187498.6A CN105819450A (en) | 2016-03-29 | 2016-03-29 | Silicon nitride ceramic tail gas hood for polycrystalline silicon reducing furnace and preparation method of tail gas hood |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109608204A (en) * | 2019-01-31 | 2019-04-12 | 山东工业陶瓷研究设计院有限公司 | A kind of high rigidity Si3N4Ceramic radome high-efficiency and precision preparation for processing |
| CN117185821A (en) * | 2023-11-06 | 2023-12-08 | 中材高新氮化物陶瓷有限公司 | Silicon nitride ceramic and preparation method thereof |
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| CN101962297A (en) * | 2010-10-20 | 2011-02-02 | 北京中材人工晶体研究院有限公司 | Preparation method of silicon nitride ceramics ring for polysilicon reduction furnace |
| CN104119079A (en) * | 2014-08-04 | 2014-10-29 | 上海泛联科技股份有限公司 | Sintering method for improving performance consistency of silicon nitride material |
| CN204550073U (en) * | 2015-04-09 | 2015-08-12 | 景德镇晶达新材料有限公司 | The anti-lost silicon device in a kind of polysilicon reducing furnace tail gas hole |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101962297A (en) * | 2010-10-20 | 2011-02-02 | 北京中材人工晶体研究院有限公司 | Preparation method of silicon nitride ceramics ring for polysilicon reduction furnace |
| CN104119079A (en) * | 2014-08-04 | 2014-10-29 | 上海泛联科技股份有限公司 | Sintering method for improving performance consistency of silicon nitride material |
| CN204550073U (en) * | 2015-04-09 | 2015-08-12 | 景德镇晶达新材料有限公司 | The anti-lost silicon device in a kind of polysilicon reducing furnace tail gas hole |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109608204A (en) * | 2019-01-31 | 2019-04-12 | 山东工业陶瓷研究设计院有限公司 | A kind of high rigidity Si3N4Ceramic radome high-efficiency and precision preparation for processing |
| CN117185821A (en) * | 2023-11-06 | 2023-12-08 | 中材高新氮化物陶瓷有限公司 | Silicon nitride ceramic and preparation method thereof |
| CN117185821B (en) * | 2023-11-06 | 2024-01-30 | 中材高新氮化物陶瓷有限公司 | Silicon nitride ceramic and preparation method thereof |
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Application publication date: 20160803 |