CN100497753C - Preparation method of carbon/carbon thermal insulation cover for monocrystalline silicon draw machines - Google Patents
Preparation method of carbon/carbon thermal insulation cover for monocrystalline silicon draw machines Download PDFInfo
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- CN100497753C CN100497753C CNB2007100179153A CN200710017915A CN100497753C CN 100497753 C CN100497753 C CN 100497753C CN B2007100179153 A CNB2007100179153 A CN B2007100179153A CN 200710017915 A CN200710017915 A CN 200710017915A CN 100497753 C CN100497753 C CN 100497753C
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Abstract
The invention discloses a preparing method of carbon/carbon thermal insulation cover of single-crystal silicon drawing oven, which comprises the following steps: toroidal-binding with carbon fiber weftless cloth and thin carbon fabric net tyre; needling radially; producing pseudo three-dimensional thermal insulation cover preformed body with low density; vacuum-dipping with furfural ketone resin; hardening; charring; proceeding fine and close fro 2-4 times repeatedly; reaching density not less than 1. 2g/cm3; ending; leading into chlorine gas or Freon; proceeding high-temperature purified treatment; machining; getting the product. This invention possesses the advantages of simple craft, low cost and long durability.
Description
Technical field
The invention belongs to monocrystalline silicon draw machines with stay-warm case material technology field, be specifically related to the preparation method of a kind of monocrystalline silicon draw machines with carbon/carbon thermal insulation cover.
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 single crystal 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 stay-warm case 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 monocrystalline silico briquette 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 fusion silicon single crystal 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 stay-warm case outsourcing charcoal felt mainly has been a heat-blocking action.The graphite stay-warm case 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.
At present monocrystalline silicon draw machines with stay-warm case substantially by the graphite manufacturing because graphite products intensity is low, the thermal conductivity height, the high temperature heat-resistant shock stability is poor, and work-ing life is short, changes frequent, large size product shaping difficulty makes it be difficult to satisfy the requirement of single crystal silicon semiconductor production development.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, and the preparation method that a kind of technology is simple, density suitable, the monocrystalline silicon draw machines of material use properties excellence is used carbon/carbon thermal insulation cover is provided.
For achieving the above object, the technical solution adopted in the present invention is: a kind of monocrystalline silicon draw machines preparation method of carbon/carbon thermal insulation cover is characterized in that this method may further comprise the steps:
(1) adopting the charcoal fiber not have latitude cloth and thin carbon fiber network tire replaces hoop and twines the full carbon fiber pseudo-three-dimensional structure of radially acupuncture precast body;
(2) adopt the fine and close precast body of acetone-furfural resin dipping charing, dipping went out jar after 3 hours in impregnating autoclave under the condition of vacuumizing, and changed charring furnace again over to and carried out charing processing, fine and close 2-4 time repeatedly;
(3) stay-warm case precast body extrudate density 〉=1.20g/cm
3The time densification technique finish, under the condition that feeds chlorine and freonll-11, stay-warm case precast body goods are carried out high temperature purification treatment;
(4) promptly make the monocrystalline silicon draw machines carbon/carbon thermal insulation cover after the mechanical workout.
Adopt 12K charcoal fiber not have latitude cloth hoop in the described step (1) and twine radially needling structure precast body, adopt radially acupuncture, prevent layering and cracking in the manufacturing processed, the precast body volume density is at 0.25～0.35g/cm
3, K represents tow thousand radicals.
Carbonization temperature in the described step (2) is 800-1100 ℃.Vacuum pressure in the described step (2) is-0.094～-0.098Mpa.
High temperature purification treatment temperature in the described step (3) is 2000～2500 ℃.
Promptly making monocrystalline silicon draw machines in the described step (4) after the mechanical workout is 500～1100mm with the diameter of carbon/carbon thermal insulation cover, highly is 200～1500mm, and thickness is 20～100mm.
The present invention is on the device basic of traditional monocrystalline silicon draw machines, introduce carbon/carbon composite and replace traditional graphite stay-warm case as stay-warm case, the tensile strength that stay-warm case uses carbon/carbon composite as 50MPa about, compressive strength is about 120MPa, flexural strength is about 70MPa, shearing resistance is about 40MPa, thermal conductivity is about 10W/mk (300K), and the tensile strength of graphite stay-warm case material is about 14MPa, compressive strength is about 45MPa, flexural strength is about 20MPa, and shearing resistance is about 15MPa, and thermal conductivity is about 60W/mk (300K).Adopt acetone-furfural resin vacuum impregnation, charring process, make density 〉=1.20g/cm
3The stay-warm case goods.This product structure is stable, and thermal conductivity is low, is difficult for reacting with the interior environment of monocrystalline silicon draw machines, can improve the work-ing life of product greatly, reduces turnover rate.
The present invention compared with prior art has the following advantages:
(1) adopt 12K charcoal fibrous ring to twining radially needling structure precast body, the thermal shock of the high temperature repeatedly test that can strengthen the intensity of stay-warm case and bear environment in the monocrystalline silicon draw machines;
(2) adopt acetone-furfural resin vacuum impregnation, charing densification technique, compactness extent is suitable, can effectively reduce monocrystalline silicon draw machines and use thermal conductivity, the process consistency of carbon/carbon thermal insulation cover good, and exploitativeness is strong, and cost is low;
(3) monocrystalline silicon draw machines that makes with this Technology has in light weightly with carbon/carbon thermal insulation cover, and volume is little, and thin thickness improves 2-3 work-ing life doubly, reduces the number of times of changing parts, thereby improves usage ratio of equipment, reduces maintenance cost;
(4) existing installation has the fixed working volume, and because carbon/carbon composite has excellent performance, compares 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 formed product difficulty, price is higher, and because carbon/carbon composite has excellent performance, can adopt charcoal/raw material of wood-charcoal material when producing large diameter product;
(6) monocrystalline silicon draw machines that makes with this Technology carbon/carbon thermal insulation cover purity height as the monocrystalline silicon draw machines carbon/carbon thermal insulation cover, is compared with the conventional graphite product, can avoid polluted product, improves the purity and the quality of product;
Description of drawings
Fig. 1 uses the structural representation of carbon/carbon thermal insulation cover for the monocrystalline silicon draw machines of the present invention's preparation.
Embodiment
The present invention will be further described below in conjunction with embodiment.
Embodiment 1
(1) adopting the charcoal fiber not have latitude cloth and thin carbon fiber network tire replaces hoop and twines the full carbon fiber pseudo-three-dimensional structure of radially acupuncture precast body; Precast body density is at 0.25g/cm
3
(2) adopt the fine and close precast body of acetone-furfural resin dipping charing, dipping went out jar in about 3 hours in impregnating autoclave under the pressure of-0.094MPa, changed 900 ℃ of charring furnaces over to and carried out charing and handle;
(3) stay-warm case precast body extrudate density 〉=1.20g/cm
3The time densification technique finish, stay-warm case precast body goods are carried out high temperature purification treatment feeding under chlorine and 00 ℃ of condition of Freon 21.
(4) can make diameter after the mechanical workout is 750mm, highly is 1000mm, and thickness is the monocrystalline silicon draw machines carbon/carbon thermal insulation cover of 30mm.
The tensile strength of the used carbon/carbon composite of this stay-warm case is 40MPa after tested, and compressive strength is 90MPa, and flexural strength is 55MPa, and shearing resistance is 30MPa, and thermal conductivity is 6W/mk (300K).
Embodiment 2
(1) adopting the charcoal fiber not have latitude cloth and thin carbon fiber network tire replaces hoop and twines the full carbon fiber pseudo-three-dimensional structure of radially acupuncture precast body; Precast body density is at 0.30g/cm
3
(2) adopt the fine and close precast body of acetone-furfural resin dipping charing, dipping went out jar in about 3 hours in impregnating autoclave under the pressure of-0.096MPa, changed 950 ℃ of charring furnaces over to and carried out charing and handle;
(3) stay-warm case precast body extrudate density 〉=1.20g/cm
3The time densification technique finish, stay-warm case precast body goods are carried out high temperature purification treatment feeding under chlorine and 00 ℃ of condition of Freon 23.
(4) can make diameter after the mechanical workout is 900mm, highly is 1200mm, and thickness is the monocrystalline silicon draw machines carbon/carbon thermal insulation cover of 50mm.
The tensile strength of the used carbon/carbon composite of this stay-warm case is 45MPa after tested, and compressive strength is 110MPa, and flexural strength is 65MPa, and shearing resistance is 35MPa, and thermal conductivity is 8W/mk (300K).
Embodiment 3
(1) adopting the charcoal fiber not have latitude cloth and thin carbon fiber network tire replaces hoop and twines the full carbon fiber pseudo-three-dimensional structure of radially acupuncture precast body; Precast body density is at 0.35g/cm
3
(2) adopt the fine and close precast body of acetone-furfural resin dipping charing, dipping went out jar in about 3 hours in impregnating autoclave under the pressure of-0.098MPa, changed 1100 ℃ of charring furnaces over to and carried out charing and handle;
(3) stay-warm case precast body extrudate density 〉=1.20g/cm
3The time densification technique finish, stay-warm case precast body goods are carried out high temperature purification treatment feeding under chlorine and 500 ℃ of conditions of freon-12.
(4) can make diameter after the mechanical workout is 1100mm, highly is 1500mm, and thickness is the monocrystalline silicon draw machines carbon/carbon thermal insulation cover of 100mm.
The tensile strength of the used carbon/carbon composite of this stay-warm case is 50MPa after tested, and compressive strength is 120Mpa, and flexural strength is 60Mpa, and shearing resistance is 40Mpa, and thermal conductivity is 10W/mk (300K).
Claims (5)
1, a kind of monocrystalline silicon draw machines preparation method of carbon/carbon thermal insulation cover is characterized in that this method may further comprise the steps:
(1) adopting the charcoal fiber not have latitude cloth and thin carbon fiber network tire replaces hoop and twines the full carbon fiber pseudo-three-dimensional structure of radially acupuncture precast body;
(2) adopt the fine and close precast body of acetone-furfural resin dipping charing, dipping went out jar after 3 hours in impregnating autoclave under the condition of vacuumizing, and changed charring furnace again over to and carried out charing processing, fine and close 2-4 time repeatedly;
(3) stay-warm case precast body extrudate density 〉=1.20g/cm
3The time densification technique finish, under the condition that feeds chlorine and freonll-11, stay-warm case precast body goods are carried out high temperature purification treatment, described high temperature purification treatment temperature is 2000～2500 ℃;
(4) promptly make the monocrystalline silicon draw machines carbon/carbon thermal insulation cover after the mechanical workout.
2, the monocrystalline silicon draw machines according to claim 1 preparation method of carbon/carbon thermal insulation cover, it is characterized in that adopting in the described step (1) 12K charcoal fiber not have latitude cloth hoop and twine radially needling structure precast body, adopt radially acupuncture, prevent layering and cracking in the manufacturing processed, the precast body volume density is at 0.25～0.35g/cm
3, K represents tow thousand radicals.
3, monocrystalline silicon draw machines according to claim 1 is characterized in that with the preparation method of carbon/carbon thermal insulation cover the carbonization temperature in the described step (2) is 800-1100 ℃.
4, the monocrystalline silicon draw machines according to claim 1 preparation method of carbon/carbon thermal insulation cover, it is characterized in that promptly making after the mechanical workout in the described step (4) monocrystalline silicon draw machines is 500～1100mm with the diameter of carbon/carbon thermal insulation cover, highly be 200～1500mm, thickness is 20～100mm.
5, monocrystalline silicon draw machines according to claim 1 is with the preparation method of carbon/carbon thermal insulation cover, it is characterized in that vacuum pressure in the described step (2) be-0.094～-0.098Mpa.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101463500B (en) * | 2008-03-03 | 2012-06-27 | 湖南金博复合材料科技有限公司 | High temperature furnace fire resistant heat preserving cover and technique for producing the same |
| CN101550017B (en) | 2009-05-12 | 2011-12-14 | 湖南金博复合材料科技有限公司 | High temperature furnace-grade curing carbon fiber thermal insulating material and production technology thereof |
| CN101948327B (en) * | 2010-08-17 | 2012-12-12 | 西安超码科技有限公司 | Method for preparing work hardening insulation quilt for high temperature furnace |
| CN102167611B (en) * | 2011-01-27 | 2013-02-27 | 无锡市弟兆碳材料有限公司 | Method for preparing carbon/carbon composite material plate |
| CN102731131B (en) * | 2012-07-13 | 2013-12-04 | 宜兴市飞舟高新科技材料有限公司 | High-performance fiber heat-insulating material prefabricating bodies and preparation method thereof |
| CN103482995B (en) * | 2013-08-06 | 2015-01-07 | 江苏天鸟高新技术股份有限公司 | Continuous carbon fiber reinforced crucible preform and preparation method thereof |
| CN104649701B (en) * | 2015-03-10 | 2015-11-04 | 李宇花 | A kind of preparation method of high-strength light carbon/carbon compound material |
| CN107031077A (en) * | 2017-04-27 | 2017-08-11 | 苏州宝骅密封科技股份有限公司 | A kind of vacuum infusion techniques for being used to prepare high tight ness rating seal |
| CN107199718B (en) * | 2017-04-27 | 2019-05-31 | 苏州宝骅密封科技股份有限公司 | A kind of impregnation technology being used to prepare high tightness sealing element |
| CN112626608A (en) * | 2020-12-01 | 2021-04-09 | 西安超码科技有限公司 | Carbon/carbon spliced heat-preservation cylinder for monocrystalline silicon straight pulling furnace and manufacturing method thereof |
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