CN102660768A - Preparation technology of carbon/carbon composite material crucible for monocrystalline silicon furnace - Google Patents
Preparation technology of carbon/carbon composite material crucible for monocrystalline silicon furnace Download PDFInfo
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- CN102660768A CN102660768A CN2012101662664A CN201210166266A CN102660768A CN 102660768 A CN102660768 A CN 102660768A CN 2012101662664 A CN2012101662664 A CN 2012101662664A CN 201210166266 A CN201210166266 A CN 201210166266A CN 102660768 A CN102660768 A CN 102660768A
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Abstract
The invention discloses a preparation technology of a carbon/carbon composite material crucible for a monocrystalline silicon furnace, and the preparation technology comprises the following steps of: adopting a polyacrylonitrile nitrile base carbon fiber-woven performing body, taking mixed gas of natural gas, propylene, liquefied petroleum as a carbon source and nitrogen or argon as carrier gas, in a uniform temperature thermal field formed by a vertical pot type deposition furnace, timely switching the upper gas charging and lower gas charging of a pipeline, due to the pressure difference of the gas inside and outside the crucible, and in combination with a uniform temperature method, a differential-pressure method and a compulsive gas current method, realizing the quick densifying of the whole crucible blank body, wherein after 300-350 hours, the intensity of the crucible can reach to more than 1.6g/cm<3>, compared with the conventional free deposition technology, the preparation technology can be used for greatly shortening the deposition time, and reduces the production cost. After being mechanically machined, the crucible is used for a thermal field of the monocrystalline silicon furnace, compared with the hot isostatic pressure graphite crucible, the carbon/carbon composite material crucible has the advantages that the service life is prolonged by 3-5 times, the cost performance is obviously better than that of the graphite crucible, and the production cost and labor intensity of the monocrystalline silicon are greatly reduced.
Description
Technical field
The present invention relates to the preparation technology of a kind of monocrystaline silicon stove with the carbon/carbon composite crucible.
Background technology
The equipment of preparation silicon single crystal employing is the pulling of silicon single crystal stove at present, and concrete production process is that high-purity polysilicon silica flour is contained in the quartz crucible, then quartz crucible is put into the plumbago crucible of heating collet; In monocrystaline silicon stove, feed hydrogen or argon gas as shielding gas, with the silica flour heating and melting; Temperature generally is controlled at 1400 ℃-1700 ℃; Insert in the melt through the seed crystal of guide shell with silicon single crystal, seed crystal drawing bar and crucible are done the rotation reversing motion, constantly have crystal grain to separate out like this in the melt of polycrystalline silica flour; And according to being arranged in around the seed crystal of the sequence rules of seed crystal atom, along with upwards promoting of drawing bar generates silicon single crystal rod.Because the intensity of the crucible of graphite is relatively poor, general plumbago crucible has only about 30 heats work-ing life, and the many dependence on import of isostatic pressing formed graphite crucible, makes that the monocrystalline silicon production cost is higher.
In recent years along with carbon/carbon composite in the promotion and application aspect the civil equipment; Had company to adopt the carbon/carbon composite crucible to replace the isostatic pressing formed graphite crucible, the carbon/carbon composite crucible is to be the precast body that raw material is compiled into crucible with the thomel, adopts CVD (chemical meteorology deposition); Methods such as CVI (chemical vapor infiltration) or impregnation technology; With carbon matrix fortifying fibre structure, through on probation, the carbon/carbon composite crucible has improved 3 to 5 times than the hot isostatic pressing plumbago crucible life-span; Cost performance obviously is superior to plumbago crucible, greatly reduces the cost and the labour intensity of monocrystalline silicon production.
In the industry, generally adopt free CVD or CVI technology, promptly precast body is freely put in cvd furnace, and gas is advanced by the bottom, and discharge on top, and preparation density is at 1.5g/cm
3Above carbon/carbon composite, the reaction times is many more than 600 hours, and relative cost is higher; If adopt depositing operation to combine with impregnation technology, technology is loaded down with trivial details on the one hand, and the matrix material that obtains on the other hand is inconsistent because of the carbon matrix structure of fibrous inside, makes the heat physical properties of material itself there are differences, and has influenced the life-span of material.
Summary of the invention
The objective of the invention is provides a kind of preparation technology that can realize the low monocrystaline silicon stove of quick density and cost with the carbon/carbon composite crucible to above-mentioned technical problem.
The technical scheme that the present invention adopts:
A kind of monocrystaline silicon stove comprises the steps: with the preparation technology of carbon/carbon composite crucible
(1) is raw material with the thomel, is woven into net tire and charcoal cloth respectively, and make it to be combined into felt through acupuncture; Be fastened felt on the mould of crucible shape, cover one deck charcoal cloth on it, cover one deck net tire again; So crossover is placed and is made it compound through acupuncture, and obtaining density is 0.4 g/cm
3-0.6 g/cm
3The three-dimensional crucible precast body of standard;
(2) said crucible precast body being put into cvd furnace deposits; Be provided with 1-4 road gas passage on the support base plate of said cvd furnace and the furnace roof respectively; The inlet, outlet state of the gas passage on said support base plate and the furnace roof can instantaneously switch, and concrete steps are:
A. said crucible precast body is upside down on the support base plate in the said cvd furnace, it is inner to make the gas port that supports the gas passage on the base plate be housed in the crucible precast body fully;
B. keeping that temperature is 850 ℃-1150 ℃ in the cvd furnace, is carbon source with the mixed gas of Sweet natural gas, propylene, oil liquefied gas, and the control furnace pressure is at 1-7kPa, and control carbon source total amount is at 2-8m
3, control carrier gas (nitrogen or argon gas) total amount and carbon source total amount ratio are 3: 2, keep the pressure difference of the inside and outside 500Pa-1kPa of crucible;
C. in vapor deposition processes, the inlet, outlet state of said gas passage whenever switched once at a distance from 30 to 100 hours, deposited 300-350 hour, made carbon-carbon composite crucible density reach 1.6g/cm
3More than;
(3) crucible that deposited in the step (2) carries out graphitization processing at 1800-2500 ℃.
Said thomel is the T-700 PAN-based carbon fiber.
Three's ratio is regulated according to setting temperature in the mixed gas of said Sweet natural gas, propylene, oil liquefied gas, and concrete grammar is: in the time of 850 ℃≤temperature≤960 ℃, Sweet natural gas, propylene, oil liquefied gas three's volume ratio is: 1:4:3; 960 ℃ < during temperature≤1020 ℃, three's volume ratio is: 3:5:3; 1020 ℃ < three's volume ratio is 2:1:2 during temperature≤1150 ℃.
The present invention compared with prior art possesses following characteristics:
(1) the present invention prepare adopt Sweet natural gas, propylene, oil liquefied gas in the process mixed gas as carbon source; With respect to single carbon source; Increased the TR of chemical reaction; Increase the precursor concentration of the RESEARCH OF PYROCARBON of different steps greatly, formed when helping large and small molecule RESEARCH OF PYROCARBON and deposition, improved the partial density of material.
(2) the T-700 PAN-based carbon fiber that adopts among the present invention has higher intensity and modulus than other thomels, improves the know clearly stretch-proof and the crushing strength of crucible, thereby has improved work-ing life.
(3) the crucible precast body is inverted in cvd furnace and is put among the present invention; Realized that in reaction process equal warm therapy, pressure differential method, forced draft method combine; Realized the whole quick densifying of crucible base substrate, crucible is after deposition 300 to 350 hours, and density can reach 1.6g/cm
3More than, more traditional unhindered settling technology shortens depositing time greatly, has reduced production cost.Crucible is used for the monocrystaline silicon stove thermal field after mechanical workout, the carbon/carbon composite crucible has improved 3 to 5 times than the hot isostatic pressing plumbago crucible life-span, and cost performance obviously is superior to plumbago crucible, greatly reduces the cost and the labour intensity of monocrystalline silicon production.
(4) in this technology; Through regularly switching intake method; Having overcome the single direction carbon-source gas is unfavorable for RESEARCH OF PYROCARBON in the precast body inside deposition on the one hand, makes deposit carbon can realize complementation in the structure that carbon fiber surface forms on the other hand, can avoid the matrix material of " hollow " structure.
Embodiment
The present embodiment monocrystaline silicon stove comprises following step with the preparation technology of carbon/carbon composite crucible:
(1) PAN-based carbon fiber with T-700 is a raw material; Be woven into net tire and charcoal cloth respectively, and make it to be combined into felt, be fastened felt on the mould of crucible shape through acupuncture; Cover one deck charcoal cloth on it; Cover one deck net tire again, so crossover is placed and is made it compound through acupuncture, and obtaining density is 0.45 g/cm
3The three-dimensional crucible precast body of standard;
(2) said crucible precast body is put into cvd furnace and deposit, be provided with 3 road gas passages respectively on the support base plate of said cvd furnace and the furnace roof, the inlet, outlet state of said gas passage can instantaneously switch, and concrete steps are:
A. said crucible precast body is upside down on the support base plate in the said cvd furnace, it is inner to make the gas port that supports the gas passage on the base plate be housed in the crucible precast body fully;
B. keep that temperature is in 950 ℃ of-1050 ℃ of scopes in the cvd furnace, the actual temp value will change instant the adjusting according to furnace pressure, and the control furnace pressure is at 3.5kPa, is carbon source with the mixed gas of Sweet natural gas, propylene, oil liquefied gas, and control carbon source total amount is at 5m
3/ h, control carrier gas nitrogen total amount 7.5m
3/ h, the pressure difference of the inside and outside 600Pa of maintenance crucible;
Three's ratio is regulated according to setting temperature in the mixed gas of said Sweet natural gas, propylene, oil liquefied gas, and concrete grammar is: in the time of 850 ℃≤temperature≤960 ℃, Sweet natural gas, propylene, oil liquefied gas three's volume ratio is: 1:4:3; 960 ℃ < during temperature≤1020 ℃, three's volume ratio is: 3:5:3; 1020 ℃ < three's volume ratio is 2:1:2 during temperature≤1150 ℃;
C. in vapor deposition processes, if from the furnace bottom air inlet then furnace roof give vent to anger, if the furnace roof air inlet then furnace bottom give vent to anger; The inlet, outlet state can instantaneously switch; Said gas passage whenever switched an inlet, outlet state at a distance from 50 hours, deposited 350 hours, made carbon-carbon composite crucible density reach 1.6g/cm
3More than;
(3) crucible that deposited in the step (2) is carried out graphitization processing at 1800-2500 ℃; Improve the degree of graphitization of material on the one hand; The chemicalstability and the heat physical properties that improve; Remove volatile impurity on the other hand, the carbon/carbon composite crucible after the processing can directly be used for the thermal field of monocrystaline silicon stove.
Claims (3)
1. a monocrystaline silicon stove is characterized in that comprising the steps: with the preparation technology of carbon/carbon composite crucible
(1) is raw material with the thomel, is woven into net tire and charcoal cloth respectively, and make it to be combined into felt through acupuncture; Be fastened felt on the mould of crucible shape, cover one deck charcoal cloth on it, cover one deck net tire again; So crossover is placed and is made it compound through acupuncture, and obtaining density is 0.4 g/cm
3-0.6 g/cm
3The three-dimensional crucible precast body of standard;
(2) said crucible precast body is put into cvd furnace and deposit, be provided with 1-4 road gas passage on the support base plate of said cvd furnace and the furnace roof respectively, the inlet, outlet state of said gas passage can instantaneously switch, and concrete steps are:
A. said crucible precast body is upside down on the support base plate in the said cvd furnace, it is inner to make the gas port that supports the gas passage on the base plate be housed in the crucible precast body fully;
B. keeping that temperature is 850 ℃-1150 ℃ in the cvd furnace, is carbon source with the mixed gas of Sweet natural gas, propylene, oil liquefied gas, and the control furnace pressure is at 1-7kPa, and control carbon source total amount is at 2-8m
3, control carrier gas total amount and carbon source total amount ratio are 3: 2, keep the pressure difference of the inside and outside 500Pa-1kPa of crucible;
C. in vapor deposition processes, said gas passage whenever switched an inlet, outlet state at a distance from 30 to 100 hours, deposited 300-350 hour, made carbon-carbon composite crucible density reach 1.6g/cm
3More than;
(3) crucible that deposited in the step (2) carries out graphitization processing at 1800-2500 ℃.
2. a kind of monocrystaline silicon stove according to claim 1 is characterized in that with the preparation technology of carbon/carbon composite crucible said thomel is the T-700 PAN-based carbon fiber.
3. a kind of monocrystaline silicon stove according to claim 1 is with the preparation technology of carbon/carbon composite crucible; It is characterized in that three's ratio is regulated according to setting temperature in the mixed gas of said Sweet natural gas, propylene, oil liquefied gas; Concrete grammar is: in the time of 850 ℃≤temperature≤960 ℃, Sweet natural gas, propylene, oil liquefied gas three's volume ratio is: 1:4:3; 960 ℃ < during temperature≤1020 ℃, three's volume ratio is: 3:5:3; 1020 ℃ < three's volume ratio is 2:1:2 during temperature≤1150 ℃.
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| CN103193498A (en) * | 2013-04-07 | 2013-07-10 | 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 |
| CN105695954A (en) * | 2016-01-22 | 2016-06-22 | 山东国晶新材料有限公司 | Method for strengthening mechanical properties of single crystal furnace thermal field material |
| US9409337B2 (en) | 2013-11-08 | 2016-08-09 | Georgia Tech Research Corporation | Polyacrylonitrile/cellulose nano-structure fibers |
| CN106245117A (en) * | 2016-08-29 | 2016-12-21 | 湖南省鑫源新材料股份有限公司 | Monoblock type carbon carbon crucible and manufacture 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 |
| CN109097823A (en) * | 2017-06-20 | 2018-12-28 | 常州市永达五金工具厂 | Monocrystalline silicon growing silica crucible inner cylinder and its carbon fiber sintering tube and their preparation method |
| 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 |
| 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 |
| CN111892417A (en) * | 2020-08-25 | 2020-11-06 | 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 |
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| 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 |
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| US9771669B2 (en) | 2013-11-08 | 2017-09-26 | Georgia Tech Research Corporation | Use, stabilization and carbonization of polyacrylonitrile/carbon composite fibers |
| US9409337B2 (en) | 2013-11-08 | 2016-08-09 | Georgia Tech Research Corporation | Polyacrylonitrile/cellulose nano-structure fibers |
| US11773514B2 (en) | 2014-10-08 | 2023-10-03 | Georgia Tech Research Corporation | Method for making high strength and high modulus carbon fibers |
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| CN105695954A (en) * | 2016-01-22 | 2016-06-22 | 山东国晶新材料有限公司 | Method for strengthening mechanical properties of single crystal furnace thermal field material |
| 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 |
| CN106245117A (en) * | 2016-08-29 | 2016-12-21 | 湖南省鑫源新材料股份有限公司 | Monoblock type carbon carbon crucible and manufacture method thereof |
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| 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 |
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| CN115652282A (en) * | 2022-11-16 | 2023-01-31 | 湖南碳峰材料科技有限公司 | Composite CVD graphite material and preparation method and application thereof |
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| CN115745646A (en) * | 2022-11-28 | 2023-03-07 | 湖南博云新材料股份有限公司 | Preparation method of carbon/carbon composite material |
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| CN117265641A (en) * | 2023-11-20 | 2023-12-22 | 内蒙古鼎泰万邦新材料有限公司 | Braided crucible preform and manufacturing method |
| 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 |
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