CN102660768B - The preparation technology of carbon/carbon composite material crucible for a kind of monocrystaline silicon stove - Google Patents
The preparation technology of carbon/carbon composite material crucible for a kind of monocrystaline silicon stove Download PDFInfo
- Publication number
- CN102660768B CN102660768B CN201210166266.4A CN201210166266A CN102660768B CN 102660768 B CN102660768 B CN 102660768B CN 201210166266 A CN201210166266 A CN 201210166266A CN 102660768 B CN102660768 B CN 102660768B
- Authority
- CN
- China
- Prior art keywords
- crucible
- carbon
- gas
- composite material
- precast body
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The invention discloses the preparation technology of a kind of monocrystaline silicon stove carbon/carbon composite material crucible, the method adopts the precast body of polyacrylonitrile-based carbon fibre establishment, with natural gas, propylene, the mist of oil liquefied gas is carbon source, nitrogen or argon gas are carrier gas, in the samming thermal field forming at vertical tank type multiple cvd furnace, the upper air on timing for cutting replace tubes road and lower air inlet, utilize the pressure differential of the inside and outside gas of crucible, realize equal warm therapy, pressure differential method, forced draft method combines, realize the quick densifying of crucible base substrate entirety, crucible is after 300 to 350 hours, density reachable is to 1.6g/cm3Above, more traditional unhindered settling technique shortens sedimentation time greatly, has reduced production cost. After crucible is machined, for monocrystaline silicon stove thermal field, carbon/carbon composite material crucible has improved 3 to 5 times compared with the high temperature insostatic pressing (HIP) graphite crucible life-span, and cost performance is obviously better than graphite crucible, greatly reduces cost and the labour intensity of monocrystalline silicon production.
Description
Technical field
The present invention relates to the preparation technology of a kind of monocrystaline silicon stove carbon/carbon composite material crucible.
Background technology
The equipment of preparing at present monocrystalline silicon employing is pulling of silicon single crystal stove, concrete production process is that high-purity polysilicon silica flour is contained in silica crucible, then silica crucible is put into the graphite crucible of heating collet, in monocrystaline silicon stove, pass into hydrogen or argon gas as protective gas, by silica flour heating and melting, temperature general control is controlled at 1400 DEG C-1700 DEG C, by guide shell, the seed crystal of monocrystalline silicon is inserted in melt, seed crystal drawing bar and crucible do rotation counter motion, in the melt of polycrystalline silica flour, constantly there is like this crystal grain to separate out, and being arranged in around seed crystal according to the sequence rules of seed crystal atom, along with the upwards lifting of drawing bar generates silicon single crystal rod. because the intensity of the crucible of graphite is poor, general graphite crucible only has 30 heats left and right service life, and the many dependence on import of isostatic pressing formed graphite crucible, makes monocrystalline silicon production cost higher.
In recent years along with carbon/carbon composite is in the promotion and application aspect civil equipment, there is company to adopt carbon/carbon composite material crucible to replace isostatic pressing formed graphite crucible, carbon/carbon composite material crucible is the precast body that is compiled into crucible taking carbon fiber as raw material, adopt CVD(chemical meteorology deposition), CVI(chemical vapor infiltration) or the method such as impregnation technology, with carbon matrix fortifying fibre structure, through on probation, carbon/carbon composite material crucible has improved 3 to 5 times compared with the high temperature insostatic pressing (HIP) graphite crucible life-span, cost performance is obviously better than graphite crucible, greatly reduce cost and the labour intensity of monocrystalline silicon production.
Industrial, generally adopt free CVD or CVI technique, precast body is freely put in cvd furnace, and gas is entered by bottom, and discharge on top, and preparation density is at 1.5g/cm3Above carbon/carbon composite, the reaction time is many more than 600 hours, and relative cost is higher; If adopt depositing operation to combine with impregnation technology, technique is loaded down with trivial details on the one hand, and the composite obtaining is on the other hand inconsistent because of the carbon matrix structure of fibrous inside, and the thermophysical property of material itself be there are differences, and has affected the life-span of material.
Summary of the invention
The object of the invention is provides a kind of preparation technology that can realize quick density and the low monocrystaline silicon stove of cost carbon/carbon composite material crucible for above-mentioned technical problem.
The technical solution used in the present invention:
A preparation technology for carbon/carbon composite material crucible for monocrystaline silicon stove, comprises the steps:
(1), taking carbon fiber as raw material, be woven into respectively net tire and charcoal cloth, and make it to be combined into felt by acupuncture, felt is fastened on the mould of crucible shape, on it, covers one deck charcoal cloth, then cover one deck net tire, so crossover is placed and is made it compound by acupuncture, and obtaining density is 0.4g/cm3-0.6g/cm3The three-dimensional crucible precast body of standard;
(2) described crucible precast body being put into cvd furnace deposits, on the support baseboard of described cvd furnace and furnace roof, be provided with respectively 1-4 road gas passage, the inlet, outlet state of the gas passage on described support baseboard and furnace roof can instantaneously switch, and concrete steps are:
A. described crucible precast body is upside down on the support baseboard in described cvd furnace, makes the gas port of the gas passage on support baseboard be housed in crucible precast body inside completely;
B. keeping temperature in cvd furnace is 850 DEG C-1150 DEG C, taking the mist of natural gas, propylene, oil liquefied gas as carbon source, controls furnace pressure at 1-7kPa, controls carbon source total amount at 2-8m3, controlling carrier gas (nitrogen or argon gas) total amount and carbon source total amount ratio is 3: 2, keeps the pressure differential of the inside and outside 500Pa-1kPa of crucible;
C. in vapor deposition processes, the inlet, outlet state of described gas passage switched once every 30 to 100 hours, and deposition 300-350 hour, makes carbon carbon composite crucible density reach 1.6g/cm3Above;
(3) crucible depositing in step (2) carries out graphitization processing at 1800-2500 DEG C.
Described carbon fiber is T-700 polyacrylonitrile-based carbon fibre.
In the mist of described natural gas, propylene, oil liquefied gas, three's ratio regulates according to setting temperature, and concrete grammar is:, natural gas, propylene, oil liquefied gas three's volume ratio is: 1:4:3 when 850 DEG C≤the temperature≤960 DEG C; , three's volume ratio is: 3:5:3 when 960 DEG C < the temperature≤1020 DEG C; , three's volume ratio is 2:1:2 when 1020 DEG C < the temperature≤1150 DEG C.
The present invention compared with prior art possesses following characteristics:
(1) in preparation process of the present invention, adopt the mist of natural gas, propylene, oil liquefied gas as carbon source, with respect to single carbon source, increase the temperature range of chemical reaction, greatly increase the precursor concentration of the RESEARCH OF PYROCARBON of different phase, when being conducive to large and small molecule RESEARCH OF PYROCARBON, form and deposition, improved the density of material part.
(2) the T-700 polyacrylonitrile-based carbon fibre adopting in the present invention, than other carbon fibers, has higher strength and modulus, improves know clearly stretch-proof and the crushing strength of crucible, thereby has improved service life.
(3) in the present invention, crucible precast body is inverted and is put in cvd furnace, in course of reaction, having realized equal warm therapy, pressure differential method, forced draft method combines, realized the quick densifying of crucible base substrate entirety, crucible is after deposition 300 to 350 hours, and density reachable is to 1.6g/cm3Above, more traditional unhindered settling technique shortens sedimentation time greatly, has reduced production cost. After crucible is machined, for monocrystaline silicon stove thermal field, carbon/carbon composite material crucible has improved 3 to 5 times compared with the high temperature insostatic pressing (HIP) graphite crucible life-span, and cost performance is obviously better than graphite crucible, greatly reduces cost and the labour intensity of monocrystalline silicon production.
(4) in this technique, change intake method by timing for cutting, having overcome single direction carbon-source gas is unfavorable for that RESEARCH OF PYROCARBON is in precast body inside deposition on the one hand, the structure that makes on the other hand deposit carbon form at carbon fiber surface can realize complementation, can avoid the composite of " hollow " structure.
Detailed description of the invention
The present embodiment monocrystaline silicon stove comprises following step by the preparation technology of carbon/carbon composite material crucible:
(1) taking the polyacrylonitrile-based carbon fibre of T-700 as raw material, be woven into respectively net tire and charcoal cloth, and make it to be combined into felt by acupuncture, felt is fastened on the mould of crucible shape, on it, cover one deck charcoal cloth, cover one deck net tire, so crossover is placed and is made it compound by acupuncture again, and obtaining density is 0.45g/cm3The three-dimensional crucible precast body of standard;
(2) described crucible precast body is put into cvd furnace and deposit, be provided with respectively 3 road gas passages on the support baseboard of described cvd furnace and furnace roof, the inlet, outlet state of described gas passage can instantaneously switch, and concrete steps are:
A. described crucible precast body is upside down on the support baseboard in described cvd furnace, makes the gas port of the gas passage on support baseboard be housed in crucible precast body inside completely;
B. keeping temperature in cvd furnace is within the scope of 950 DEG C-1050 DEG C, and actual temp value will change instant adjusting according to furnace pressure, controls furnace pressure at 3.5kPa, taking the mist of natural gas, propylene, oil liquefied gas as carbon source, controls carbon source total amount at 5m3/ h, controls carrier gas nitrogen total amount 7.5m3/ h, the pressure differential of the inside and outside 600Pa of maintenance crucible;
In the mist of described natural gas, propylene, oil liquefied gas, three's ratio regulates according to setting temperature, and concrete grammar is:, natural gas, propylene, oil liquefied gas three's volume ratio is: 1:4:3 when 850 DEG C≤the temperature≤960 DEG C; , three's volume ratio is: 3:5:3 when 960 DEG C < the temperature≤1020 DEG C; , three's volume ratio is 2:1:2 when 1020 DEG C < the temperature≤1150 DEG C;
C. in vapor deposition processes, if from furnace bottom air inlet furnace roof give vent to anger, if furnace roof air inlet furnace bottom give vent to anger, inlet, outlet state can instantaneously switch, described gas passage switched an inlet, outlet state every 50 hours, deposited 350 hours, made carbon carbon composite crucible density reach 1.6g/cm3Above;
(3) crucible depositing in step (2) is carried out to graphitization processing at 1800-2500 DEG C, improve on the one hand the degree of graphitization of material, the chemical stability and the thermophysical property that improve, remove on the other hand volatile impurity, carbon/carbon composite material crucible after treatment, can be directly used in the thermal field of monocrystaline silicon stove.
Claims (2)
1. a preparation technology for carbon/carbon composite material crucible for monocrystaline silicon stove, is characterized in that comprising the steps:
(1), taking carbon fiber as raw material, be woven into respectively net tire and charcoal cloth, and make it to be combined into felt by acupuncture, felt is fastened on the mould of crucible shape, on it, covers one deck charcoal cloth, then cover one deck net tire, so crossover is placed and is made it compound by acupuncture, and obtaining density is 0.4g/cm3-0.6g/cm3The three-dimensional crucible precast body of standard;
(2) described crucible precast body is put into cvd furnace and deposit, be provided with respectively 1-4 road gas passage on the support baseboard of described cvd furnace and furnace roof, the inlet, outlet state of described gas passage can instantaneously switch, and concrete steps are:
A. described crucible precast body is upside down on the support baseboard in described cvd furnace, makes the gas port of the gas passage on support baseboard be housed in crucible precast body inside completely;
B. keeping temperature in cvd furnace is 850 DEG C-1150 DEG C, taking the mist of natural gas, propylene, oil liquefied gas as carbon source, controls furnace pressure at 1-7kPa, controls carbon source total amount at 2-8m3, controlling carrier gas total amount and carbon source total amount ratio is 3: 2, keeps the pressure differential of the inside and outside 500Pa-1kPa of crucible;
C. in vapor deposition processes, described gas passage switched an inlet, outlet state every 30 to 100 hours, and deposition 300-350 hour, makes carbon carbon composite crucible density reach 1.6g/cm3Above;
(3) crucible depositing in step (2) carries out graphitization processing at 1800-2500 DEG C;
Wherein, in the mist of described natural gas, propylene, oil liquefied gas, three's ratio regulates according to setting temperature, and concrete grammar is:, natural gas, propylene, oil liquefied gas three's volume ratio is: 1:4:3 when 850 DEG C≤the temperature≤960 DEG C; , three's volume ratio is: 3:5:3 when 960 DEG C < the temperature≤1020 DEG C; , three's volume ratio is 2:1:2 when 1020 DEG C < the temperature≤1150 DEG C.
2. the preparation technology of carbon/carbon composite material crucible for a kind of monocrystaline silicon stove according to claim 1, is characterized in that described carbon fiber is T-700 polyacrylonitrile-based carbon fibre.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210166266.4A CN102660768B (en) | 2012-05-26 | 2012-05-26 | The preparation technology of carbon/carbon composite material crucible for a kind of monocrystaline silicon stove |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210166266.4A CN102660768B (en) | 2012-05-26 | 2012-05-26 | The preparation technology of carbon/carbon composite material crucible for a kind of monocrystaline silicon stove |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102660768A CN102660768A (en) | 2012-09-12 |
| CN102660768B true CN102660768B (en) | 2016-05-04 |
Family
ID=46770341
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210166266.4A Expired - Fee Related CN102660768B (en) | 2012-05-26 | 2012-05-26 | The preparation technology of carbon/carbon composite material crucible for a kind of monocrystaline silicon stove |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102660768B (en) |
Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103193498B (en) * | 2013-04-07 | 2014-06-18 | 山东国晶新材料有限公司 | Narrow flow induction coupling chemical vapor deposition (CVD) densification method for rapidly preparing carbon/carbon composite material crucible |
| US9409337B2 (en) | 2013-11-08 | 2016-08-09 | Georgia Tech Research Corporation | Polyacrylonitrile/cellulose nano-structure fibers |
| EP3204542A4 (en) | 2014-10-08 | 2018-04-11 | Georgia Tech Research Corporation | High strength and high modulus carbon fibers |
| CN105695954B (en) * | 2016-01-22 | 2018-07-24 | 山东国晶新材料有限公司 | A method of enhancing thermal field of single crystal furnace material mechanical performance |
| CN106245117B (en) * | 2016-08-29 | 2019-02-01 | 湖南省鑫源新材料股份有限公司 | Monoblock type carbon carbon crucible and its manufacturing method |
| CN109097823B (en) * | 2017-06-20 | 2021-09-10 | 常州博科浩纳知识产权服务有限公司 | Quartz crucible inner cylinder body for monocrystalline silicon growth, carbon fiber sintering cylinder thereof and preparation methods thereof |
| CN109097824A (en) * | 2017-06-20 | 2018-12-28 | 常州市永达五金工具厂 | Monocrystalline silicon growing combined type silica crucible and preparation method thereof |
| CN108752031A (en) * | 2018-06-12 | 2018-11-06 | 甘肃新西北碳素科技有限公司 | A kind of method that carbon fiber prepares large-size carbon carbon crucible |
| CN111058087A (en) * | 2020-01-12 | 2020-04-24 | 陕西美兰德炭素有限责任公司 | Carbon/silicon carbide composite material feeding cylinder for repeatedly feeding single crystal silicon furnace |
| CN111892417B (en) * | 2020-08-25 | 2021-05-14 | 内蒙古中晶科技研究院有限公司 | Carbon fiber composite material and preparation method thereof |
| CN112457038A (en) * | 2020-11-13 | 2021-03-09 | 甘肃新西北碳素科技有限公司 | Preparation method of carbon/carbon composite material thin-wall cylinder |
| CN114411115A (en) * | 2021-12-09 | 2022-04-29 | 安徽绿能技术研究院有限公司 | Double-loop double-carbon-source rapid directional vapor deposition method |
| CN115094514B (en) * | 2022-08-15 | 2023-09-19 | 湖南泰坦未来科技有限公司 | Composite material crucible and preparation method thereof |
| CN115652282B (en) * | 2022-11-16 | 2024-04-05 | 湖南碳材科技有限公司 | Composite CVD graphite material and preparation method and application thereof |
| CN115745646B (en) * | 2022-11-28 | 2024-03-08 | 湖南博云新材料股份有限公司 | Preparation method of carbon/carbon composite material |
| CN117265641B (en) * | 2023-11-20 | 2024-01-30 | 内蒙古鼎泰万邦新材料有限公司 | Braided crucible preform and manufacturing method |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101235493A (en) * | 2007-11-16 | 2008-08-06 | 南京航空航天大学 | Real time measuring weight increase speed controlling chemical gas-phase deposition device and method |
| CN101319353A (en) * | 2008-05-20 | 2008-12-10 | 湖南金博复合材料科技有限公司 | Carbon/carbon composite material crucible pot and preparing technique thereof |
| EP2298699A1 (en) * | 2008-07-16 | 2011-03-23 | Hodogaya Chemical Co., Ltd. | Mass of carbon fibers, process for producing same, and composite material containing these |
| CN102030554A (en) * | 2010-11-02 | 2011-04-27 | 西安超码科技有限公司 | Method for compacting carbon/carbon composite material by using natural gas mixture CVI (Chemical Vapor Infiltration) |
| WO2012015044A1 (en) * | 2010-07-30 | 2012-02-02 | 保土谷化学工業株式会社 | Vapor grown carbon fiber aggregate |
| CN102433543A (en) * | 2011-12-20 | 2012-05-02 | 西安超码科技有限公司 | Multi-deposition-chamber CVI (chemical vapor infiltration) device for compacting carbon/carbon crucible and method using same |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1796334A (en) * | 2004-12-27 | 2006-07-05 | 陈瑾惠 | Carbon/Carbon Composite material and mfg. method thereof |
-
2012
- 2012-05-26 CN CN201210166266.4A patent/CN102660768B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101235493A (en) * | 2007-11-16 | 2008-08-06 | 南京航空航天大学 | Real time measuring weight increase speed controlling chemical gas-phase deposition device and method |
| CN101319353A (en) * | 2008-05-20 | 2008-12-10 | 湖南金博复合材料科技有限公司 | Carbon/carbon composite material crucible pot and preparing technique thereof |
| EP2298699A1 (en) * | 2008-07-16 | 2011-03-23 | Hodogaya Chemical Co., Ltd. | Mass of carbon fibers, process for producing same, and composite material containing these |
| WO2012015044A1 (en) * | 2010-07-30 | 2012-02-02 | 保土谷化学工業株式会社 | Vapor grown carbon fiber aggregate |
| CN102030554A (en) * | 2010-11-02 | 2011-04-27 | 西安超码科技有限公司 | Method for compacting carbon/carbon composite material by using natural gas mixture CVI (Chemical Vapor Infiltration) |
| CN102433543A (en) * | 2011-12-20 | 2012-05-02 | 西安超码科技有限公司 | Multi-deposition-chamber CVI (chemical vapor infiltration) device for compacting carbon/carbon crucible and method using same |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102660768A (en) | 2012-09-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102660768B (en) | The preparation technology of carbon/carbon composite material crucible for a kind of monocrystaline silicon stove | |
| CN101643933B (en) | CZ method silicon single crystal growth furnace quartz crucible carbon protection crucible and manufacturing process thereof | |
| CN101319353B (en) | Carbon/carbon composite material crucible pot and preparing technique thereof | |
| CN110105075B (en) | High-purity carbon fiber reinforced silicon carbide composite material and preparation method thereof | |
| CN100400471C (en) | Method for manufacture thermal field charcoal/charcoal draft tube for single crystal silicon pulling furnace | |
| CN100432023C (en) | Method for manufacture thermal field charcoal/charcoal crucible for single crystal silicon pulling furnace | |
| CN207391600U (en) | A kind of growth apparatus of carborundum crystals | |
| CN102731119B (en) | Crucible using carbon/carbon/silicon carbide composite material and preparation method thereof | |
| CN112095150B (en) | Growth method of zinc selenide | |
| CN101386547B (en) | Carbon/carbon compound material heating element and production technology thereof | |
| CN100497753C (en) | Preparation method of carbon/carbon thermal insulation cover for monocrystalline silicon draw machines | |
| CN110396723A (en) | A kind of high-purity semi-insulating silicon carbide monocrystalline and its high efficiency preparation method and application | |
| WO2011060717A1 (en) | Method and apparatus for removing phosphorus and boron from polysilicon by continuously smelting | |
| CN103964883A (en) | Preparation method for thin wall or tapered member made from one-dimensional nanofiber reinforced and toughened carbon-ceramic composite | |
| CN102433543B (en) | Multi-deposition-chamber CVI (chemical vapor infiltration) device for compacting carbon/carbon crucible and method using same | |
| CN113151895B (en) | Large-diameter high-purity semi-insulating silicon carbide growth process | |
| CN105008278A (en) | Method for producing silicon carbide and silicon carbide | |
| CN201626998U (en) | Thermal field of czochralski silicon monocrystal | |
| CN101402455B (en) | Method for producing silicon carbide nano-stick with sublimation | |
| CN205856655U (en) | A kind of single-crystal silicon carbide stove | |
| CN101333685B (en) | Three-chamber continuous whisker-generating vacuum furnace for continuously preparing silicon carbide whisker | |
| CN102992800A (en) | Preparation method for carbon fiber prefabricated body in hot field S-shaped heater of polycrystalline silicon ingot furnace | |
| CN110512281A (en) | The method for quickly preparing silicon carbide | |
| CN106048728B (en) | A kind of method of growing high quality silicon carbide whisker | |
| CN203007475U (en) | Composite material guide cylinder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160504 Termination date: 20200526 |