CN105480957A - Method for preparing non-grinding high-purity fully granulated silicon nitride powder by adopting direct nitriding method - Google Patents
Method for preparing non-grinding high-purity fully granulated silicon nitride powder by adopting direct nitriding method Download PDFInfo
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/068—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with silicon
- C01B21/0682—Preparation by direct nitridation of silicon
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Abstract
The invention relates to a method for preparing non-grinding high-purity non-fiber fully granulated silicon nitride powder by adopting the direct nitriding method. According to the method, silicon powder with the purity of 99.990-99.999% and D50 of 800-1000 meshes is taken as the raw material, and high-purity nitrogen with the purity of 99.999% and high-purity argon with the purity of 99.999% are adopted as the environmental atmosphere. According to the method, on the basis of effectively controlling the shape of silicon nitride powder by adopting the silicon powder direct nitriding technology, the silicon nitride powder is incompact in shape and can be directly used as a demolding agent of polycrystalline silicon without grinding, so that the product cost is reduced on the premise of meeting the demolding requirement.
Description
Technical field
The present invention relates to a kind of method that direct nitridation method prepares solar energy polycrystalline silicon crucible coating layer beta-silicon nitride powder.
Background technology
High purity silicon nitride silicon powder is mainly for the preparation of solar energy polycrystalline silicon quartz crucible for ingot casting coating and high-performance silicon nitride ceramics preparation raw material.
Due to Si
3n
4be strong covalent bond, self-diffusion coefficient is low, and its resistance to elevated temperatures and chemical stability good, and N element belongs to electrically inactive element, less on the electric property impact of polysilicon, do not infiltrate between silicon nitride and silicon melt meanwhile, polysilicon discord crucible is sticked together, and the easy demoulding, does not ftracture.Therefore, generally Si is used in current polycrystalline silicon industry
3n
4as coated material.Sun power polysilicon has higher requirement to purity, in order to prevent being mixed into of impurity, therefore also requires higher to the purity of silicon nitride coating.Common silica flour direct nitridation method is prepared silicon nitride and is had that equipment is simple, cost is low, the feature such as stable and controllable for quality, but the silicon nitride particle that direct nitridation method was produced is bonded to bulk in the past, need grinding, the electric energy of at substantial on the one hand, increases preparation cost, on the other hand, the ball-milling medium of denuding in process of lapping can be mixed in product, thus reduces the purity of product.Moreover because high-purity silicon powder easily generates the totally different crystal grain of two kinds of shape characteristics in nitridation process simultaneously, one is macrofiber shape, and one is particulate state, fibrous crystal grain can produce adverse influence to the quality of the preparation of coating and polysilicon.
Summary of the invention
Goal of the invention:
The invention provides the preparation of a kind of direct nitridation method to exempt to grind high-purity method without the full particulate state beta-silicon nitride powder of fiber, its objective is the problem that solution is in the past existing.
Technical scheme:
In order to above-mentioned purpose, the solution of the present invention is: adopting purity be 99.990 ~ 99.999%, D50 to be 800 order ~ 1000 object silica flours is raw material, and the high pure nitrogen of 99.999% and the high-purity argon gas of 99.999% are ambiance.
High purity prepared by the present invention is as follows without the preparation process of fiber full particulate state beta-silicon nitride powder:
One, silica flour is put into atmosphere furnace, material layer thickness control is at 15 ~ 30mm
Two, close fire door and gas channel, vacuumize
Three, high pure nitrogen air-flow is passed into
Four, in stream of nitrogen gas, furnace temperature is risen to 1300 ~ 1340 DEG C, be incubated 90 ~ 120 minutes
Five, close stream of nitrogen gas, vacuumize, pass into high-purity argon gas air-flow
Six, in high-purity argon gas air-flow, furnace temperature is risen to 1450 ~ 1480 DEG C
Seven, close high-purity argon gas air-flow, vacuumize, pass into high pure nitrogen air-flow
Eight, under high pure nitrogen air-flow 1450 ~ 1480 DEG C of conditions, be incubated 600 minutes and above time, make it complete nitrogenize
Nine, be down to room temperature, obtain exempting from grinding high purity without the full granular nitrogen SiClx of fiber
Advantageous effect:
Direct nitridation method preparation exempt to grind high-purity method without the full particulate state beta-silicon nitride powder of fiber, it not only reduces costs, and this method can obtain exempt from grind high purity without the full particulate state beta-silicon nitride powder of fiber, this powder can be used for solar energy polycrystalline silicon crucible coating layer.
Accompanying drawing explanation
In Fig. 1 high-purity silicon powder nitrogenize product, threadiness and granular nitrogen silicon carbide particle coexist powder SEM image;
The nitrogenize of Fig. 2 high-purity silicon powder is without fiber full particulate state beta-silicon nitride powder SEM image.
Embodiment
In conjunction with concrete enforcement example, the invention will be further described.
Embodiment 1:
1. be 99.990%, D50 by purity be that atmosphere furnace put into by 800 order silica flours, the bed of material is thick is 30mm;
2. close fire door and gas channel, vacuumize;
3. high pure nitrogen air-flow is passed into;
4. in high pure nitrogen air-flow, furnace temperature is risen to 1340 DEG C, be incubated 120 minutes;
5. close high pure nitrogen air-flow, vacuumize, pass into high-purity argon gas air-flow;
6. in high-purity argon gas air-flow, furnace temperature is risen to 1450 DEG C;
7. close high-purity argon gas air-flow, vacuumize, pass into high pure nitrogen air-flow;
8. under high pure nitrogen air-flow and 1450 DEG C of conditions, 600 minutes are incubated;
9. be down to 27 DEG C, obtain exempting from grinding high purity without the full granular nitrogen SiClx of fiber;
Embodiment 2:
1. be 99.990%, D50 by purity be that atmosphere furnace put into by 800 order silica flours, the bed of material is thick is 20mm;
2. close fire door and gas channel, vacuumize;
3. high pure nitrogen air-flow is passed into;
4. in high pure nitrogen air-flow, furnace temperature is risen to 1320 DEG C, be incubated 100 minutes;
5. close high pure nitrogen air-flow, vacuumize, pass into high-purity argon gas air-flow;
6. in high-purity argon gas air-flow, furnace temperature is risen to 1450 DEG C;
7. close high-purity argon air-flow, vacuumize, pass into high pure nitrogen air-flow;
8. under high pure nitrogen air-flow and 1450 DEG C of conditions, 600 minutes are incubated;
9. be down to 24 DEG C, obtain exempting from grinding high purity without the full granular nitrogen SiClx of fiber;
Embodiment 3:
1. be 99.999%, D50 by purity be that atmosphere furnace put into by 1000 order silica flours, the bed of material is thick is 15mm;
2. close fire door and gas channel, vacuumize;
3. high pure nitrogen air-flow is passed into;
4. in high pure nitrogen air-flow, furnace temperature is risen to 1320 DEG C, be incubated 110 minutes;
5. close high pure nitrogen air-flow, vacuumize, pass into high-purity argon gas air-flow;
6. in high-purity argon gas air-flow, furnace temperature is risen to 1460 DEG C;
7. close argon gas stream, vacuumize, pass into high pure nitrogen air-flow;
8. under high pure nitrogen air-flow and 1480 DEG C of conditions, 650 minutes are incubated;
9. be down to 20 DEG C, obtain exempting from grinding high purity without the full granular nitrogen SiClx of fiber;
Embodiment 4:
1. be 99.999%, D50 by purity be that atmosphere furnace put into by 1000 order silica flours, the bed of material is thick is 20mm;
2. close fire door and gas channel, vacuumize;
3. high pure nitrogen air-flow is passed into;
4. in high pure nitrogen air-flow, furnace temperature is risen to 1320 DEG C, be incubated 120 minutes;
5. close stream of nitrogen gas, vacuumize, pass into high-purity argon gas air-flow;
6. in high-purity argon gas air-flow, furnace temperature is risen to 1480 DEG C;
7. close high-purity argon air-flow, vacuumize, pass into high pure nitrogen air-flow;
8. under high pure nitrogen air-flow and 1480 DEG C of conditions, 650 minutes are incubated;
9. be down to 25 DEG C, obtain exempting from grinding high purity without the full granular nitrogen SiClx of fiber;
Embodiment 5:
1. be 99.999%, D50 by purity be that atmosphere furnace put into by 1000 order silica flours, the bed of material is thick is 25mm;
2. close fire door and gas channel, vacuumize;
3. high pure nitrogen air-flow is passed into;
4. in stream of nitrogen gas, furnace temperature is risen to 1330 DEG C, be incubated 120 minutes;
5. close stream of nitrogen gas, vacuumize, pass into high-purity argon gas air-flow;
6. in high-purity argon gas air-flow, furnace temperature is risen to 1480 DEG C;
7. close argon gas stream, vacuumize, pass into high pure nitrogen air-flow;
8. under high pure nitrogen air-flow and 1480 DEG C of conditions, 650 minutes are incubated;
9. be down to 22 DEG C, obtain exempting from grinding high purity without the full granular nitrogen SiClx of fiber;
Embodiment 6:
1. be 99.990%, D50 by purity be that atmosphere furnace put into by 1000 order silica flours, the bed of material is thick is 15mm;
2. close fire door and gas channel, vacuumize;
3. high pure nitrogen air-flow is passed into;
4. in stream of nitrogen gas, furnace temperature is risen to 1300 DEG C, be incubated 90 minutes;
5. close stream of nitrogen gas, vacuumize, pass into high-purity argon gas air-flow;
6. in high-purity argon gas air-flow, furnace temperature is risen to 1480 DEG C;
7. close argon gas stream, vacuumize, pass into high pure nitrogen air-flow;
8. under high pure nitrogen air-flow and 1480 DEG C of conditions, 650 minutes are incubated;
Be down to 25 DEG C, obtain exempting from grinding high purity without the full granular nitrogen SiClx of fiber.
In sum, we take silica flour Direct-Nitridation technique effectively controlling, on the basis of silicon nitride powder shape, to make beta-silicon nitride powder be loose shape, directly can be used as the releasing agent of polysilicon without the need to grinding, on the basis meeting demoulding requirement, reduce the cost of product.
Claims (2)
1. direct nitridation method preparation exempts to grind high-purity method without the full particulate state beta-silicon nitride powder of fiber, it is characterized in that: the present invention adopts purity to be 99.990 ~ 99.999%, D50 be 800 order ~ 1000 object silica flours as raw material, adopt 99.999% high pure nitrogen and 99.999% high-purity argon gas as ambiance.
2. direct nitridation method preparation according to claim 1 exempts to grind high-purity method without the full particulate state beta-silicon nitride powder of fiber, it is characterized in that:
Preparation process of the present invention is as follows: get the raw materials ready according to the ratio in claim 1;
(1), by silica flour put into atmosphere furnace, silica flour layer thickness control is at 15 ~ 30mm;
(2), close fire door and gas channel, vacuumize;
(3), pass into high pure nitrogen air-flow, gas outflow controls at 0.3 ~ 1.0L/Min;
(4), in stream of nitrogen gas, furnace temperature is risen to 1300 ~ 1340 DEG C, be incubated 90 ~ 120 minutes;
(5), close stream of nitrogen gas, vacuumize, pass into high-purity argon gas air-flow, gas outflow controls at 0.3 ~ 1.0L/Min
(6), in high-purity argon gas air-flow, furnace temperature is risen to 1450 ~ 1480 DEG C;
(7), close high-purity argon gas air-flow, vacuumize, pass into high pure nitrogen air-flow, gas outflow controls at 0.3 ~ 1.0L/Min;
(8), under high pure nitrogen air-flow and furnace temperature 1450 ~ 1480 DEG C of conditions be incubated 600 minutes and above time, until make the complete nitrogenize of silica flour, be then down to room temperature, obtain exempting from grinding high purity without the full granular nitrogen SiClx of fiber.
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Cited By (5)
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| CN109627050A (en) * | 2018-12-25 | 2019-04-16 | 宁波宝斯达坩埚保温制品有限公司 | A kind of quartz crucible inner surface coating and preparation method thereof |
| CN112408992A (en) * | 2020-12-11 | 2021-02-26 | 安阳亨利高科实业有限公司 | Production method of high alpha-phase silicon nitride powder |
| CN112794294A (en) * | 2021-01-05 | 2021-05-14 | 段文轩 | Preparation of high-purity zinc nitride powder material |
| WO2022011830A1 (en) * | 2020-07-14 | 2022-01-20 | 中材高新氮化物陶瓷有限公司 | Preparation method for silicon nitride powder |
| CN115650183A (en) * | 2022-10-28 | 2023-01-31 | 福建新航凯材料科技有限公司 | Silicon nitride production process and equipment |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109627050A (en) * | 2018-12-25 | 2019-04-16 | 宁波宝斯达坩埚保温制品有限公司 | A kind of quartz crucible inner surface coating and preparation method thereof |
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| CN112408992B (en) * | 2020-12-11 | 2022-08-02 | 安阳亨利高科实业有限公司 | Production method of high alpha-phase silicon nitride powder |
| CN112794294A (en) * | 2021-01-05 | 2021-05-14 | 段文轩 | Preparation of high-purity zinc nitride powder material |
| CN115650183A (en) * | 2022-10-28 | 2023-01-31 | 福建新航凯材料科技有限公司 | Silicon nitride production process and equipment |
| CN115650183B (en) * | 2022-10-28 | 2023-12-19 | 福建新航凯材料科技有限公司 | Silicon nitride production process and equipment |
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