CN114988856A - Composite quartz ceramic feeding cone for pulling single crystal and manufacturing method thereof - Google Patents
Composite quartz ceramic feeding cone for pulling single crystal and manufacturing method thereof Download PDFInfo
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- CN114988856A CN114988856A CN202210774272.1A CN202210774272A CN114988856A CN 114988856 A CN114988856 A CN 114988856A CN 202210774272 A CN202210774272 A CN 202210774272A CN 114988856 A CN114988856 A CN 114988856A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000010453 quartz Substances 0.000 title claims abstract description 27
- 239000000919 ceramic Substances 0.000 title claims abstract description 19
- 239000002131 composite material Substances 0.000 title claims abstract description 19
- 239000013078 crystal Substances 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 10
- 239000003999 initiator Substances 0.000 claims abstract description 10
- 239000000178 monomer Substances 0.000 claims abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 7
- 239000004576 sand Substances 0.000 claims abstract description 7
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- 239000005350 fused silica glass Substances 0.000 claims abstract description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 238000012360 testing method Methods 0.000 claims description 9
- 239000011268 mixed slurry Substances 0.000 claims description 8
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical group CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000006004 Quartz sand Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims description 3
- 239000010963 304 stainless steel Substances 0.000 claims description 3
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical group CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 3
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 claims description 3
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical group C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 3
- 238000013461 design Methods 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- 239000004310 lactic acid Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 3
- XJKVPKYVPCWHFO-UHFFFAOYSA-N silicon;hydrate Chemical compound O.[Si] XJKVPKYVPCWHFO-UHFFFAOYSA-N 0.000 claims description 2
- FIMIAMLAWXOMGM-UHFFFAOYSA-N N-cyano-N-(2-methylpropyl)formamide Chemical compound C(=O)N(CC(C)C)C#N FIMIAMLAWXOMGM-UHFFFAOYSA-N 0.000 claims 1
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 239000000377 silicon dioxide Substances 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 4
- 230000035939 shock Effects 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 2
- YDVJBLJCSLVMSY-UHFFFAOYSA-N carbamoyl cyanide Chemical compound NC(=O)C#N YDVJBLJCSLVMSY-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000005816 glass manufacturing process Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
- C04B2235/3873—Silicon nitrides, e.g. silicon carbonitride, silicon oxynitride
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6023—Gel casting
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Abstract
The invention relates to a composite quartz ceramic feeding cone for pulling a single crystal and a preparation method thereof, wherein the composite quartz ceramic feeding cone comprises the following components: fused silica sand, silicon nitride, a monomer, a cross-linking agent, an initiator, a pH regulator, silica sand and water. The preparation method comprises the following steps: preparing slurry, preparing a gel system, manufacturing a blank, drying a cone and sintering. The invention has the beneficial effects that: the service life of the single crystal charging quartz cone is prolonged; the product is formed in one step, and the manufacturing cost is reduced.
Description
Technical Field
The invention relates to the technical field of quartz ceramic feeding cones, in particular to a composite quartz ceramic feeding cone for pulling a single crystal and a manufacturing method thereof.
Background
With the continuous development of the industrialization process, the demand for energy sources is more and more increased. But the current mainstream energy sources: petroleum, natural gas and coal are all non-renewable energy sources. The development of science and technology is continuous, and the technical bottleneck of renewable energy sources is being broken step by step. The development of renewable energy sources is urgent and important. The monocrystalline silicon solar cell is a green, environment-friendly and clean renewable new energy source with the mature technology and higher photoelectric conversion rate at present, the monocrystalline silicon used by the solar cell needs to be added with silicon materials for many times in the manufacturing process at present, and quartz glass cones are matched to finish feeding in the feeding process.
In addition, the existing products have the following problems:
1. the existing product adopts a quartz glass manufacturing process, the manufacturing process is cutting and processing of quartz large blocks, the process difficulty is high, and the production cost is high.
2. The existing product has poor thermal shock stability, high density, easy occurrence of cracks and crack extension blocks and short service cycle.
Disclosure of Invention
The invention aims to solve the technical problems of high difficulty in technological process, high cost and poor thermal shock stability of a product, and provides a composite quartz ceramic charging cone for pulling a single crystal and a manufacturing method thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a composite quartz ceramic feeding cone for pulling a single crystal comprises the following components:
fused silica sand, silicon nitride, a monomer, a cross-linking agent, an initiator, a pH regulator, silica sand and water.
A method for manufacturing a composite quartz ceramic feeding cone for pulling a single crystal comprises the following steps:
the method comprises the following steps: preparing slurry, namely mixing fused quartz sand, silicon nitride and water according to the weight ratio of 10-15: 0.1-0.5: 2, adding zirconia ball mill according to the proportion, adding 8-50mm zirconia ball stones in the ball mill, and ball milling for 10-20 hours to obtain slurry with the particle size (D50) of 5.0-13.0um, wherein the slurry can be used after 20-30 hours of aging;
step two: preparing a gel system, namely preparing the slurry prepared in the step one, the monomer, the cross-linking agent and the initiator according to a ratio of 100: 3-8: mixing at a ratio of 0.3-1:0.5-2 to prepare gel system slurry, and adjusting the pH to 6-8 by using a pH regulator;
step three: blank preparation: putting the gel system slurry obtained in the step two and 10-200-mesh quartz sand into a mixer according to the proportion of 2:1-1.5 for mixing for 50-120 minutes, wherein the water content of the mixed material is 6-12%, vacuumizing the mixed slurry for 30-60 minutes, then pressure-pouring the mixed slurry into a quartz cone 304 stainless steel mold finished according to the size design, standing the mixture in a 60-80 ℃ water bath for 30-80 minutes, taking out the mixture, and demolding to obtain a blank meeting the size requirement;
step four: cone drying and sintering: and (3) placing the formed blank in a drying box, heating to 120-1250 ℃ for drying by 30-60 small tests according to the heating rate of 5 ℃/small tests, sintering for 10-15 hours by using a sintering kiln at 1050-1250 ℃ after drying is finished, and obtaining the composite quartz cone product for single crystal charging meeting the requirements after the test is qualified.
Preferably, the monomer is hydroxyethyl methacrylate or acrylamide.
Preferably, the crosslinking agent is trimethylolpropane triacrylate or N-N methylenebisacrylamide.
Preferably, the initiator is hexanazo-isobutyryl-cyano-formamide or ammonium persulfate.
Preferably, the pH regulator is lactic acid or ammonia water.
The invention has the following advantages: the composite quartz ceramic charging cone is produced by adding silicon nitride in a quartz ceramic injection-solidification forming mode, the product is formed in one step by an in-situ curing technology, the size precision is high, the thermal shock stability of the product is good, cracks cannot be further extended after the surface cracks appear due to proper porosity and different particle size collocation in the product, and the service cycle is prolonged.
Detailed Description
The present invention will be described in further detail with reference to examples.
Embodiment 1, the present application relates to a composite quartz ceramic cone and a method for manufacturing the same:
1. slurry preparation, melting quartz sand: silicon nitride: water is mixed according to the weight ratio of 10-15: 0.1-0.5: 2, adding zirconia ball mill according to the proportion, adding 8-50mm zirconia ball stones in the ball mill, and ball milling for 10-20 hours to obtain slurry with the particle size (D50) of 5.0-13.0um, wherein the slurry can be used after 20-30 hours of aging;
2. preparing a gel system, namely, adopting a water-based low-toxicity gel system, taking hydroxyethyl methacrylate as a monomer, taking trimethylolpropane triacrylate as a cross-linking agent, taking azoisobutyryl cyano formamide as an initiator, taking lactic acid or ammonia water as a pH regulator, and mixing the prepared slurry: monomer (b): a crosslinking agent: the initiator is prepared according to the proportion of 100: 3-8: mixing at a ratio of 0.3-1:0.5-2 to prepare gel system slurry, and adjusting the pH to 6-8 by using a pH regulator;
3. blank preparation: putting the slurry and 10-200 mesh quartz sand into a mixer according to the proportion of 2:1-1.5 for mixing for 50-120 minutes, wherein the water content of the mixed material is 6-12%, vacuumizing the mixed slurry for 30-60 minutes, then pressure-pouring the mixed slurry into a quartz cone 304 stainless steel mold finished according to the size design, standing the mixed slurry in a 60-80 ℃ water bath for 30-80 minutes, taking out the mixed slurry and demolding to obtain a blank meeting the size requirement;
4. cone drying and sintering: and (3) placing the formed blank in a drying box, heating to 120-1250 ℃ for drying by 30-60 small tests according to the heating rate of 5 ℃/small tests, sintering for 10-15 hours by using a sintering kiln at 1050-1250 ℃ after drying is finished, and obtaining the composite quartz cone product for single crystal charging meeting the requirements after the test is qualified.
The quartz ceramic cone produced by the gel injection molding is formed in one step by an in-situ curing technology, has high dimensional precision and good thermal shock stability, and can not extend cracks after the surface of the product has cracks due to proper porosity and different particle size collocation in the product, thereby improving the service cycle.
As another example, the monomer, the crosslinking agent and the initiator in the gel system may be acrylamide, N-N methylene bisacrylamide, ammonium persulfate and the like.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (6)
1. A composite quartz ceramic feeding cone for pulling a single crystal comprises the following components:
fused silica sand, silicon nitride, a monomer, a cross-linking agent, an initiator, a pH regulator, quartz sand and water.
2. A method for manufacturing a composite quartz ceramic feeding cone for pulling a single crystal comprises the following steps:
the method comprises the following steps: preparing slurry, namely mixing fused quartz sand, silicon nitride and water according to the weight ratio of 10-15: 0.1-0.5: 2, adding zirconia ball mill according to the proportion, adding 8-50mm zirconia ball stones in the ball mill, and ball milling for 10-20 hours to obtain slurry with the particle size (D50) of 5.0-13.0um, wherein the slurry can be used after 20-30 hours of aging;
step two: preparing a gel system, namely preparing the slurry prepared in the step one, the monomer, the cross-linking agent and the initiator according to a ratio of 100: 3-8: mixing 0.3-1:0.5-2 to prepare gel system slurry, and then adjusting the pH to 6-8 by using a pH regulator;
step three: blank preparation: putting the gel system slurry obtained in the step two and 10-200-mesh quartz sand into a mixer according to the proportion of 2:1-1.5 for mixing for 50-120 minutes, wherein the water content of the mixed material is 6-12%, vacuumizing the mixed slurry for 30-60 minutes, then pressure-pouring the mixed slurry into a quartz cone 304 stainless steel mold finished according to the size design, standing the mixture in a 60-80 ℃ water bath for 30-80 minutes, taking out the mixture, and demolding to obtain a blank meeting the size requirement;
step four: cone drying and sintering: and (3) placing the formed blank in a drying box, heating to 120-1250 ℃ for drying by 30-60 small tests according to the heating rate of 5 ℃/small tests, sintering for 10-15 hours by using a sintering kiln at 1050-1250 ℃ after drying is finished, and obtaining the composite quartz cone product for single crystal charging meeting the requirements after the test is qualified.
3. The composite quartz ceramic charging cone for czochralski single crystal according to claim 1 or 2, wherein: the monomer is hydroxyethyl methacrylate or acrylamide.
4. The composite quartz ceramic charging cone for czochralski single crystal according to claim 1 or 2, wherein: the cross-linking agent is trimethylolpropane triacrylate or N-N methylene bisacrylamide.
5. The composite quartz ceramic charging cone for czochralski single crystal according to claim 1 or 2, wherein: the initiator is hexanazo isobutyl cyano formamide or ammonium persulfate.
6. The composite quartz ceramic charging cone for czochralski single crystal according to claim 1 or 2, wherein: the pH regulator is lactic acid or ammonia water.
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| CN106336207A (en) * | 2016-08-26 | 2017-01-18 | 佛山市高明区明城镇新能源新材料产业技术创新中心 | Preparing method of silica ceramics of special-shaped structure |
| KR20180025717A (en) * | 2016-09-01 | 2018-03-09 | 국방과학연구소 | Method For Preparing Fused Silica Sintered Material Containing Silicon Nitride Using Gel-Casting Process |
| CN112725880A (en) * | 2020-12-21 | 2021-04-30 | 宁晋晶兴电子材料有限公司 | Feeding device |
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2022
- 2022-07-01 CN CN202210774272.1A patent/CN114988856A/en active Pending
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|---|---|---|---|---|
| CN101343775A (en) * | 2008-08-22 | 2009-01-14 | 宁晋晶兴电子材料有限公司 | Capacity increasing charging device for quartz crucible of monocrystalline silicon manufacturing stove |
| CN106278211A (en) * | 2016-08-26 | 2017-01-04 | 佛山市高明区明城镇新能源新材料产业技术创新中心 | A kind of preparation method of labyrinth quartz ceramic |
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