CN1887803A - Prepn process of heat isolating C/C screen for monocrystal silicon drawing furnace and polycrystal silicon smelting furnace - Google Patents
Prepn process of heat isolating C/C screen for monocrystal silicon drawing furnace and polycrystal silicon smelting furnace Download PDFInfo
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- CN1887803A CN1887803A CN 200610043184 CN200610043184A CN1887803A CN 1887803 A CN1887803 A CN 1887803A CN 200610043184 CN200610043184 CN 200610043184 CN 200610043184 A CN200610043184 A CN 200610043184A CN 1887803 A CN1887803 A CN 1887803A
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Abstract
The present invention relates to preparation process of heat isolating C/C screen for monocrystal silicon drawing furnace and polycrystal silicon smelting furnace. The preparation process includes preparing 3D heat isolating screen prefab with carbon fiber; dipping the prefab in mid-temperature pitch or furfural acetone resin and charring repeatedly to reach the compactness of 1.30 g/cu cm; high temperature purifying the heat isolating screen through introducing chlorine and Freon; and final machining to obtain the heat isolating C/C screen for monocrystal silicon drawing furnace and polycrystal silicon smelting furnace. The heat isolating C/C screen for monocrystal silicon drawing furnace and polycrystal silicon smelting furnace has effectively lowered thermal conductivity coefficient, low cost and long service life.
Description
Technical field
The invention belongs to monocrystalline silicon draw machines and polysilicon smelting furnace with process furnace thermoscreen technical field, be specifically related to a kind of monocrystalline silicon draw machines and polysilicon smelting furnace preparation method with charcoal/charcoal thermoscreen.
Background technology
Single crystal growing furnace is that stainless steel is made except body of heater, and the heat-generating system of the inside and strut member comprise that crucible all uses graphite piece.The manufacture order crystal silicon promptly is in inert gas environment, with graphite heater polycrystalline silicon material is melted, with Grown by CZ Method dislocation-free monocrystalline.Silicon single crystal is to be raw material with the high purity silica flour, and under protective atmosphere conditions such as hydrogen or argon gas, growing up gradually through 1400-1600 ℃ of high-temperature fusion young brilliant traction crystal grain draws moulding.In the pulling process, plumbago crucible is together with quartz crucible transmission mechanism low speed rotation bottom furnace chamber, vertical pulling method that Here it is (CZ method).Because the resistance to elevated temperatures of graphite and good chemical stability, the thermoscreen of CZ monocrystal stove, crucible, lining, liner plate, well heater, thermal insulation layer, guide shell etc. are all made with high purity graphite.Working temperature is at 1400-1600 ℃, owing to plumbago crucible shields in the quartz crucible outside, so its temperature is at 1600-1700 ℃ in the CZ method stove.The vertical pulling method basic characteristics are with a high-purity silica pot splendid attire molten silicon.Primary process is that high purity polycrystalline silicon piece and micro-doping agent are placed in the quartz crucible, quartz crucible places in the plumbago crucible, external graphite heater, heat fused under vacuum or high-purity argon gas environment, the control proper temperature, seed crystal is inserted melt, make the fusion polysilicon become silicon single crystal by the Siliciumatom of the seed crystal crystallization and freezing that puts in order.Because working temperature is generally at 1400 ℃～1600 ℃ in this characteristics, stove.Graphite thermoscreen outsourcing charcoal felt mainly has been a heat-blocking action.The graphite thermoscreen is general, and what use is high purity graphite, requires three height, i.e. high purity, high strength, high-density, density 〉=1.8g/cm
3, require purity very high, and do not allow to contain metallic impurity, non-volatile free ions, atomic impurity under the high temperature, promptly grey calibration≤50PPM.
Be that stainless steel is made except body of heater in the polysilicon smelting furnace in addition, the heat-generating system of the inside and strut member comprise that crucible all uses graphite piece.It promptly is in atmosphere surrounding that the production polysilicon adopts the improvement Siemens Method more, with graphite heater 1400-1600 ℃ high temperature silicon materials is melted, with halogen family gas reduction purifying polycrystalline silicon material.Because the resistance to elevated temperatures of graphite and good chemical stability, the thermoscreen of polysilicon smelting furnace, well heater etc. are all made with high purity graphite.Working temperature is at 1400-1600 ℃ in the improvement Siemens Method stove.Graphite thermoscreen outsourcing charcoal felt mainly has been a heat-blocking action.The graphite thermoscreen is general, and what use is high purity graphite, requires three height, i.e. high purity, high strength, high-density, density 〉=1.8g/cm
3, require purity very high, and do not allow to contain metallic impurity, non-volatile free ions, atomic impurity under the high temperature, promptly grey calibration≤50PPM.
Monocrystalline silicon draw machines and polysilicon smelting furnace use the thermal field thermoscreen substantially by the graphite manufacturing at present, because graphite products intensity height, thermal conductivity is low, the high temperature heat-resistant shock stability is poor, work-ing life is short, changes frequently, and purity is also lower, large size product shaping difficulty makes it be difficult to satisfy the requirement of polycrystalline silicon semiconductor production development.
Summary of the invention
The objective of the invention is at above-mentioned the deficiencies in the prior art, the monocrystalline silicon draw machines of simple, fine and close respond well, the material use properties excellence of a kind of technology and the polysilicon smelting furnace preparation method with charcoal/charcoal thermoscreen is provided, to improve the thermoscreen strength of stability, the thermal conductivity that reduces thermoscreen is low, avoiding thermoscreen and polysilicon to smelt furnace inner environment reacts, improve the work-ing life of thermoscreen, reduce the turnover rate of thermoscreen.
For achieving the above object, the technical solution adopted in the present invention is: a kind of monocrystalline silicon draw machines and the polysilicon smelting furnace preparation method of charcoal/charcoal thermoscreen is characterized in that this method may further comprise the steps:
(1) adopt needled carbon cloth to combine with no latitude cloth and make full charcoal fiber three way structure thermoscreen precast body, thermoscreen precast body volume density is 0.3-0.5g/cm
3, adopt the acupuncture technology to introduce fortifying fibre in thermoscreen precast body vertical direction;
(2) pitch or acetone-furfural resin dipping charing densification technique: at pressure is under the 1.0-1.5MPa, with pack in impregnating autoclave dipping 5 hours of the thermoscreen precast body in the step (1), the thermoscreen precast body floods back commentaries on classics charring furnace and carries out the charing processing, make the thermoscreen goods, carbonization temperature is 800-1100 ℃;
(3) thermoscreen extrudate density＜1.30g/cm
3The time, repeating step (2); Thermoscreen extrudate density 〉=1.30g/cm
3The time, densification technique finishes, and feeds at purifying furnace under the condition of chlorine and freonll-11, the thermoscreen goods is packed into carry out purification process in the purifying furnace, and cleansing temp is 2000-2500 ℃;
(4), promptly make monocrystalline silicon draw machines and polysilicon smelting furnace charcoal/charcoal thermoscreen to the thermoscreen goods machined into after the process purification process in the step (3).
Needled carbon cloth in the above-mentioned steps (1) is the 12K needled carbon cloth, and wherein K represents tow thousand radicals; Monocrystalline silicon draw machines in the above-mentioned steps (4) and polysilicon smelting furnace are 300-1800mm with the diameter of thermal field charcoal/charcoal thermoscreen, and height is 300-2000mm.
The present invention is on the device basic of traditional monocrystalline silicon draw machines and polysilicon smelting furnace, introduce carbon/carbon composite and replace traditional graphite thermoscreen as thermoscreen, the tensile strength that thermoscreen uses carbon/carbon composite as 40MPa about, compressive strength is about 150MPa, flexural strength is about 60MPa, shearing resistance is about 40MPa, thermal conductivity is about 10w/m * k (300K), and the tensile strength of graphite thermoscreen material is about 14MPa, compressive strength is about 45MPa, flexural strength is about 20MPa, shearing resistance is about 15MPa, and thermal conductivity is about 60w/m * k (300K), adopts advanced carbon/carbon composite compact technology, mid-temperature pitch or acetone-furfural resin impregnated carbon metallization processes make density 〉=1.30g/cm
3The thermoscreen goods.This thermoscreen Stability Analysis of Structures thermal conductivity is low, is difficult for smelting furnace inner environment with polysilicon and reacts, and can improve the work-ing life of thermoscreen greatly, reduces the thermoscreen turnover rate.
The present invention compared with prior art has the following advantages:
(1) adopt the acupuncture 12K charcoal cloth full carbon fiber pseudo-three-dimensional structural heat-insulation screen precast body that combines with no latitude cloth, the thermal shock of high temperature repeatedly that can strengthen the intensity of well heater and bear polysilicon smelting furnace inner environment tests;
(2) adopt mid-temperature pitch or acetone-furfural resin impregnated carbon metallization processes, fine and close respond well, can effectively reduce monocrystalline silicon draw machines and polysilicon smelting furnace and use thermal conductivity, the process consistency of thermal field charcoal/charcoal thermoscreen good, exploitativeness is strong, and cost is low;
(3) monocrystalline silicon draw machines and the polysilicon smelting furnace that makes with this Technology has in light weight with the thermal field charcoal/charcoal thermoscreen, volume is little, thin thickness, improve 2-3 work-ing life doubly, as monocrystalline silicon draw machines and polysilicon smelting furnace charcoal/charcoal thermoscreen, prolong the number of times that product reduces the replacing parts work-ing life significantly, thereby improve usage ratio of equipment, reduce maintenance cost;
(4) as monocrystalline silicon draw machines and polysilicon smelting furnace during with charcoal/charcoal thermoscreen, existing installation has the fixed working volume, and because carbon/carbon composite has excellent performance, compare with the conventional graphite product, can do thinlyyer, thereby can utilize existing installation production more products, can save a large amount of new installation investment costs;
(5) when producing large diameter product, conventional graphite thermal field formed product difficulty, and because carbon/carbon composite has excellent performance when producing large diameter product, can adopt charcoal/charcoal thermoscreen;
(6) monocrystalline silicon draw machines and the polysilicon smelting furnace thermal field charcoal/charcoal thermoscreen purity height that makes with this Technology, as monocrystalline silicon draw machines and polysilicon smelting furnace charcoal/charcoal thermoscreen, compare with the conventional graphite product, can avoid polluted product, improve the purity and the quality of product;
Description of drawings
The sectional view that Fig. 1 uses charcoal/charcoal thermoscreen for the monocrystalline silicon draw machines and the polysilicon smelting furnace of employing the present invention preparation.
Embodiment
Embodiment 1
(1) adopt the 12K needled carbon cloth full charcoal fiber three way structure thermoscreen precast body that combines with no latitude cloth, thermoscreen precast body volume density is 0.3g/cm
3, adopt the acupuncture technology to introduce fortifying fibre in thermoscreen precast body vertical direction, wherein, K represents tow thousand radicals;
(2) pitch or acetone-furfural resin dipping charing densification technique: at pressure is under the 1.5MPa, with pack in impregnating autoclave dipping 5 hours of the thermoscreen precast body in the step (1), go out a jar commentaries on classics charring furnace after the thermoscreen precast body floods and carry out the charing processing, carbonization temperature is 1000 ℃;
(3) thermoscreen extrudate density＜1.30g/cm
3The time, repeating step (2); Thermoscreen extrudate density 〉=1.30g/cm
3The time, densification technique finishes, and feeds at purifying furnace under the condition of chlorine and freonll-11, the thermoscreen goods is packed into carry out purification process in the purifying furnace, and cleansing temp is 2500 ℃;
(4) to the thermoscreen goods machined into after the process purification process in the step (3), can make its diameter is 1100mm, and height is monocrystalline silicon draw machines and the polysilicon smelting furnace thermal field charcoal/charcoal thermoscreen of 1200mm.
The tensile strength of the used carbon/carbon composite of this thermoscreen is 40MPa after tested, and compressive strength is 150MPa, and flexural strength is 60MPa, and shearing resistance is 40MPa, and thermal conductivity is 10w/m * k (300K).
Embodiment 2
(1) adopt the 12K needled carbon cloth full charcoal fiber three way structure thermoscreen precast body that combines with no latitude cloth, thermoscreen precast body volume density is 0.4g/cm
3, adopt the acupuncture technology to introduce fortifying fibre in thermoscreen precast body vertical direction, wherein, K represents tow thousand radicals;
(2) pitch or acetone-furfural resin dipping charing densification technique: at pressure is under the 1.5MPa, with pack in impregnating autoclave dipping 5 hours of the thermoscreen precast body in the step (1), go out a jar commentaries on classics charring furnace after the thermoscreen precast body floods and carry out the charing processing, carbonization temperature is 800 ℃;
(3) thermoscreen extrudate density＜1.30g/cm
3The time, repeating step (2); Thermoscreen extrudate density 〉=1.30g/cm
3The time, densification technique finishes, and feeds at purifying furnace under the condition of chlorine and freonll-11, the thermoscreen goods is packed into carry out purification process in the purifying furnace, and cleansing temp is 2400 ℃;
(4) to the thermoscreen goods machined into after the process purification process in the step (3), can make its diameter is 1000mm, and height is monocrystalline silicon draw machines and the polysilicon smelting furnace thermal field charcoal/charcoal thermoscreen of 1000mm.
The tensile strength of the used carbon/carbon composite of this thermoscreen is 45MPa after tested, and compressive strength is 180MPa, and flexural strength is 55MPa, and shearing resistance is 45MPa, and thermal conductivity is 12w/m * k (300K).
Embodiment 3
(1) adopt the 12K needled carbon cloth full charcoal fiber three way structure thermoscreen precast body that combines with no latitude cloth, thermoscreen precast body volume density is 0.5g/cm
3, adopt the acupuncture technology to introduce fortifying fibre in thermoscreen precast body vertical direction, wherein, K represents tow thousand radicals;
(2) pitch or acetone-furfural resin dipping charing densification technique: at pressure is under the 1.4MPa, with pack in impregnating autoclave dipping 5 hours of the thermoscreen precast body in the step (1), go out a jar commentaries on classics charring furnace after the thermoscreen precast body floods and carry out the charing processing, carbonization temperature is 1100 ℃;
(3) thermoscreen extrudate density＜1.30g/cm
3The time, repeating step (2); Thermoscreen extrudate density 〉=1.30g/cm
3The time, densification technique finishes, and feeds at purifying furnace under the condition of chlorine and freonll-11, the thermoscreen goods is packed into carry out purification process in the purifying furnace, and cleansing temp is 2000 ℃;
(4) to the thermoscreen goods machined into after the process purification process in the step (3), can make its diameter is 1000mm, and height is monocrystalline silicon draw machines and the polysilicon smelting furnace thermal field charcoal/charcoal thermoscreen of 1500mm.
The tensile strength of the used carbon/carbon composite of this thermoscreen is 45MPa after tested, and compressive strength is 160MPa, and flexural strength is 50MPa, and shearing resistance is 35MPa, and thermal conductivity is 8w/m * k (300K).
Claims (3)
1, a kind of monocrystalline silicon draw machines and the polysilicon smelting furnace preparation method of charcoal/charcoal thermoscreen is characterized in that this method may further comprise the steps:
(1) adopt needled carbon cloth to combine with no latitude cloth and make full charcoal fiber three way structure thermoscreen precast body, thermoscreen precast body volume density is 0.3-0.5g/cm
3, adopt the acupuncture technology to introduce fortifying fibre in thermoscreen precast body vertical direction;
(2) pitch or acetone-furfural resin dipping charing densification technique: at pressure is under the 1.0-1.5MPa, with pack in impregnating autoclave dipping 5 hours of the thermoscreen precast body in the step (1), the thermoscreen precast body floods back commentaries on classics charring furnace and carries out the charing processing, make the thermoscreen goods, carbonization temperature is 800-1100 ℃;
(3) thermoscreen extrudate density＜1.30g/cm
3The time, repeating step (2); Thermoscreen extrudate density 〉=1.30g/cm
3The time, densification technique finishes, and feeds at purifying furnace under the condition of chlorine and freonll-11, the thermoscreen goods is packed into carry out purification process in the purifying furnace, and cleansing temp is 2000-2500 ℃;
(4), promptly make monocrystalline silicon draw machines and polysilicon smelting furnace charcoal/charcoal thermoscreen to the thermoscreen goods machined into after the process purification process in the step (3).
2, monocrystalline silicon draw machines according to claim 1 and the polysilicon smelting furnace preparation method of charcoal/charcoal thermoscreen, it is characterized in that: the needled carbon cloth in the step (1) is the 12K needled carbon cloth, wherein K represents tow thousand radicals.
3, monocrystalline silicon draw machines according to claim 1 and the polysilicon smelting furnace preparation method of charcoal/charcoal thermoscreen, it is characterized in that: monocrystalline silicon draw machines in the step (4) and polysilicon smelting furnace are 300-1800mm with the diameter of thermal field charcoal/charcoal thermoscreen, and height is 300-2000mm.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100431845A CN100432021C (en) | 2006-07-20 | 2006-07-20 | Prepn process of heat isolating C/C screen for monocrystal silicon drawing furnace and polycrystal silicon smelting furnace |
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| CNB2006100431845A CN100432021C (en) | 2006-07-20 | 2006-07-20 | Prepn process of heat isolating C/C screen for monocrystal silicon drawing furnace and polycrystal silicon smelting furnace |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101805922A (en) * | 2010-04-27 | 2010-08-18 | 王敬 | Heat shielding and ingot furnace with same |
| CN101269981B (en) * | 2008-04-23 | 2010-12-15 | 西安超码科技有限公司 | Process for producing carbon/carbon heat insulation bottom board for high temperature furnace |
| CN102134744A (en) * | 2011-04-26 | 2011-07-27 | 安阳市凤凰光伏科技有限公司 | Heat insulation device of polycrystalline silicon ingot furnace |
| CN101638322B (en) * | 2009-05-15 | 2012-06-06 | 西安超码科技有限公司 | Method for preparing carbon/carbon heat shields used for polysilicon hydriding furnances |
| CN103183518A (en) * | 2011-12-27 | 2013-07-03 | 浙江昱辉阳光能源有限公司 | Method for preparing carbon/carbon composite material draft tube |
| CN104711679A (en) * | 2013-12-12 | 2015-06-17 | 航天睿特碳材料有限公司 | Single crystal furnace carbon/carbon composite material heat screen and preparation method thereof |
| CN112374904A (en) * | 2020-12-02 | 2021-02-19 | 福建康碳复合材料科技有限公司 | Carbon/carbon heat shield and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE60135080D1 (en) * | 2000-12-26 | 2008-09-11 | Asahi Glass Co Ltd | Solid polymer electrolyte material, liquid composition, solid polymer fuel cell and fluoropolymer |
| CN100460359C (en) * | 2005-03-21 | 2009-02-11 | 西安航天复合材料研究所 | Method for producing carbon/carbon skid of magnetic suspension train |
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2006
- 2006-07-20 CN CNB2006100431845A patent/CN100432021C/en active Active
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101269981B (en) * | 2008-04-23 | 2010-12-15 | 西安超码科技有限公司 | Process for producing carbon/carbon heat insulation bottom board for high temperature furnace |
| CN101638322B (en) * | 2009-05-15 | 2012-06-06 | 西安超码科技有限公司 | Method for preparing carbon/carbon heat shields used for polysilicon hydriding furnances |
| CN101805922A (en) * | 2010-04-27 | 2010-08-18 | 王敬 | Heat shielding and ingot furnace with same |
| CN102134744A (en) * | 2011-04-26 | 2011-07-27 | 安阳市凤凰光伏科技有限公司 | Heat insulation device of polycrystalline silicon ingot furnace |
| CN103183518A (en) * | 2011-12-27 | 2013-07-03 | 浙江昱辉阳光能源有限公司 | Method for preparing carbon/carbon composite material draft tube |
| CN104711679A (en) * | 2013-12-12 | 2015-06-17 | 航天睿特碳材料有限公司 | Single crystal furnace carbon/carbon composite material heat screen and preparation method thereof |
| CN112374904A (en) * | 2020-12-02 | 2021-02-19 | 福建康碳复合材料科技有限公司 | Carbon/carbon heat shield and preparation method thereof |
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| CN100432021C (en) | 2008-11-12 |
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