CN100400471C - Method for manufacture thermal field charcoal/charcoal draft tube for single crystal silicon pulling furnace - Google Patents
Method for manufacture thermal field charcoal/charcoal draft tube for single crystal silicon pulling furnace Download PDFInfo
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- CN100400471C CN100400471C CNB2006100431879A CN200610043187A CN100400471C CN 100400471 C CN100400471 C CN 100400471C CN B2006100431879 A CNB2006100431879 A CN B2006100431879A CN 200610043187 A CN200610043187 A CN 200610043187A CN 100400471 C CN100400471 C CN 100400471C
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Abstract
This invention involves a preparation method for thermal field carbon/carbon draft tube used for silicon drawing furnace. The method comprises acupuncturing to three way draft tube prefabricated structure by using carbon cloth hoop-wound with thin carbon fiber network, densifying by chemical vapor deposition, phenolic resin impregnation and charring and combination of hot isostatic pressing and asphalt impregnation charring process repeatedly until the product density >= 1.83 g/cm3, purifying the product at high temperature under Freon and chlorine, and machining to obtain the final product. The invention can improve strength of carbon/carbon draft tube, prolong its life and reduce its replacement rate, and has good process consistency and feasibility, and low cost.
Description
Technical field
The invention belongs to monocrystalline silicon draw machines guide shell technical field, be specifically related to the preparation method of a kind of monocrystalline silicon draw machines with thermal field charcoal/charcoal draft tube.
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 all use 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, at high temperature flows into by the gas flow guiding tube at protective gas such as hydrogen or argon gas, young brilliant through 1400-1600 ℃ of high-temperature fusion, and traction crystal grain is grown up gradually and drawn 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 gas flow guiding tube of CZ monocrystal stove, lining, liner plate, heating element, thermal insulation layer, crucible etc. are all made with high purity graphite.Working temperature is at 1400-1600 ℃ 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.The gas flow guiding tube mainly plays the guide functions of high-temperature gas, and general 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 uses the thermal field guide shell substantially by the graphite manufacturing at present, because graphite products intensity is low, the high temperature heat-resistant shock stability is poor, the thermal conductivity height, 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 single crystal silicon semiconductor production development.
Summary of the invention
The objective of the invention is at above-mentioned the deficiencies in the prior art, the preparation method of the monocrystalline silicon draw machines of simple, fine and close respond well, the material use properties excellence of a kind of technology with thermal field charcoal/charcoal draft tube is provided, to improve the strength of stability and the resistance to heat shocks energy of guide shell, reduce the thermal conductivity of guide shell, prevent that environment reacts in guide shell and the monocrystalline silicon draw machines, improve the work-ing life of guide shell, reduce turnover rate.
For achieving the above object, the technical solution adopted in the present invention is: a kind of monocrystalline silicon draw machines preparation method of thermal field charcoal/charcoal draft tube is characterized in that this method may further comprise the steps:
(1) adopt charcoal cloth and thin carbon fiber network tread ring to twine back acupuncture mutually and make accurate three way structure guide shell precast body, and at the perverse introducing fortifying fibre of guide shell precast body vertical direction pin, guide shell precast body volume density is 0.2-0.6g/cm
3
(2) chemical vapour deposition densification technique feeds propylene or Sweet natural gas in chemical vapor deposition stove under 800-1100 ℃ of condition, the flow of propylene or Sweet natural gas is 1.0-5.0m
3/ h packs the guide shell precast body in the step (1) in the chemical vapor deposition stove into, carries out vapour deposition;
(3) resin impregnating charing densification technique: at pressure is under the 1.5-3.0MPa, dipping solidifies in vacuum-pressure resin impregnation curing oven with packing into through the guide shell precast body after the chemical vapour deposition in the step (2), the guide shell precast body floods and solidifies back commentaries on classics charring furnace charing processing, make the guide shell goods, solidification value is 150-220 ℃, and carbonization temperature is 800-1100 ℃;
(4) hot isostatic pressing bituminizing charing densification technique; At pressure is under the 50-100MPa, handles carrying out the charing of hot isostatic pressing bituminizing through the guide shell goods after the resin impregnating charing densification in the step (3), and carbonization temperature is 550-750 ℃;
(5) guide shell extrudate density＜1.83g/cm that charing is handled through the hot isostatic pressing bituminizing in the step (4)
3The time, repeating step (4); Up to guide shell extrudate density 〉=1.83g/cm
3The time, densification technique finishes, and feeds at purifying furnace under the condition of chlorine and freonll-11, packs into and carries out purification process in the purifying furnace finishing fine and close guide shell goods, and cleansing temp is 2000-2500 ℃;
(6) to the guide shell goods machined into after the process purification process in the step (5), promptly make the monocrystalline silicon draw machines thermal field charcoal/charcoal draft tube.
Charcoal cloth in the above-mentioned steps (1) is 12K charcoal cloth, and K represents tow thousand radicals; Monocrystalline silicon draw machines in the above-mentioned steps (6) is 150-800m with the diameter of thermal field charcoal/charcoal draft tube, and height is 100-600mm.
The present invention uses on the device basic of monocrystalline silicon draw machines at traditional monocrystalline silicon draw machines, introduce carbon/carbon composite and replace traditional graphite guide shell as guide shell, the tensile strength that guide shell uses carbon/carbon composite as 70MPa about, compressive strength is about 200MPa, flexural strength is about 90MPa, shearing resistance is about 50MPa, and the tensile strength of graphite guide shell material is about 14MPa, compressive strength is about 45MPa, flexural strength is about 20MPa, shearing resistance is about 15MPa, adopt advanced carbon/carbon composite compact technology, the densification technique that chemical vapour deposition and resin impregnating charing and the charing of hot isostatic pressing bituminizing combine makes density 〉=1.83g/cm
3Charcoal/charcoal draft tube guide shell goods.This product structure strength of stability height, resistance to heat shocks can be good, 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 guide shell greatly, reduces turnover rate.
The present invention compared with prior art has the following advantages:
(1) adopt charcoal cloth and thin carbon fiber network tread ring to twine the accurate three way structure guide shell of back acupuncture precast body mutually, adopt the acupuncture technology to introduce fortifying fibre in vertical direction, can strengthen guide shell intensity and the thermal shock of the high temperature repeatedly test of bearing environment in the monocrystalline silicon draw machines;
(2) adopt chemical vapour deposition and resin impregnating charing and the charing of the hot isostatic pressing bituminizing densification technique that combines, fine and close respond well, guide shell extrudate density height, it is good with intensity, the process consistency of thermal field charcoal/charcoal draft tube effectively to improve monocrystalline silicon draw machines, exploitativeness is strong, and cost is low;
(3) monocrystalline silicon draw machines that makes with this Technology has in light weight with thermal field charcoal/charcoal draft tube, volume is little, thin thickness, improve 2-3 work-ing life doubly, as the monocrystalline silicon draw machines charcoal/charcoal draft tube, prolong the number of times that product reduces the replacing parts work-ing life significantly, thereby improve usage ratio of equipment, reduce maintenance cost;
When (4) using charcoal/charcoal draft tube as monocrystalline silicon draw machines, 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 well heater;
(6) monocrystalline silicon draw machines that makes with this Technology thermal field charcoal/charcoal draft tube purity height as the monocrystalline silicon draw machines charcoal/charcoal draft tube, 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 sectional view of thermal field charcoal/charcoal draft tube for the monocrystalline silicon draw machines that adopts the present invention's preparation.
Embodiment
Embodiment 1
(1) adopt 12K charcoal cloth and thin carbon fiber network tread ring to twine the accurate three way structure guide shell of back acupuncture precast body mutually, guide shell precast body volume density is 0.6g/cm
3, adopt the acupuncture technology to introduce fortifying fibre in guide shell precast body vertical direction, wherein, K represents tow thousand radicals;
(2) chemical vapour deposition densification technique feeds propylene in chemical vapor deposition stove under 900 ℃ of conditions, the flow of propylene is 1.5m
3/ h packs the guide shell precast body in the step (1) in the chemical vapor deposition stove into, carries out vapour deposition;
(3) resin impregnating charing densification technique: at pressure is under the 1.9MPa, dipping solidifies in vacuum-pressure resin impregnation curing oven with packing into through the guide shell precast body after the chemical vapour deposition in the step (2), the guide shell precast body floods and solidifies back commentaries on classics charring furnace charing processing, make the guide shell goods, solidification value is 150 ℃, and carbonization temperature is 900 ℃;
(4) hot isostatic pressing bituminizing charing densification technique; At pressure is under the 100MPa, handles carrying out the charing of hot isostatic pressing bituminizing through the guide shell goods after the resin impregnating charing densification in the step (3), and carbonization temperature is 750 ℃;
(5) guide shell extrudate density＜1.83g/cm that charing is handled through the hot isostatic pressing bituminizing in the step (4)
3The time, repeating step (4); Guide shell extrudate density 〉=1.83g/cm
3The time, densification technique finishes, and feeds at purifying furnace under the condition of chlorine and freonll-11, the guide shell goods is packed into carry out purification process in the purifying furnace, and cleansing temp is 2500 ℃;
(6) to the guide shell goods machined into after the process purification process in the step (5), promptly making its diameter is 300mm, and height is the monocrystalline silicon draw machines thermal field charcoal/charcoal draft tube of 500mm.
The tensile strength of the used carbon/carbon composite of this guide shell is 75MPa after tested, and compressive strength is 210MPa, and flexural strength is 85MPa, and shearing resistance is 55MPa.
Embodiment 2
(1) adopt 12K charcoal cloth and thin carbon fiber network tread ring to twine the accurate three way structure guide shell of back acupuncture precast body mutually, guide shell precast body volume density is 0.5g/cm
3, adopt the acupuncture technology to introduce fortifying fibre in guide shell precast body vertical direction, wherein, K represents tow thousand radicals;
(2) chemical vapour deposition densification technique feeds propylene in chemical vapor deposition stove under 950 ℃ of conditions, the flow of propylene is 2.5m
3/ h packs the guide shell precast body in the step (1) in the chemical vapor deposition stove into, carries out vapour deposition;
(3) resin impregnating charing densification technique: at pressure is under the 1.8MPa, dipping solidifies in vacuum-pressure resin impregnation curing oven with packing into through the guide shell precast body after the chemical vapour deposition in the step (2), the guide shell precast body floods and solidifies back commentaries on classics charring furnace charing processing, make the guide shell goods, solidification value is 200 ℃, and carbonization temperature is 1000 ℃;
(4) hot isostatic pressing bituminizing charing densification technique; At pressure is under the 100MPa, handles carrying out the charing of hot isostatic pressing bituminizing through the guide shell goods after the resin impregnating charing densification in the step (3), and carbonization temperature is 650 ℃;
(5) guide shell extrudate density＜1.83g/cm that charing is handled through the hot isostatic pressing bituminizing in the step (4)
3The time, repeating step (4); Guide shell extrudate density 〉=1.83g/cm
3The time, densification technique finishes, and feeds at purifying furnace under the condition of chlorine and freonll-11, the guide shell goods is packed into carry out purification process in the purifying furnace, and cleansing temp is 2400 ℃;
(6) to the guide shell goods machined into after the process purification process in the step (5), promptly making its diameter is 400mm, and height is the monocrystalline silicon draw machines thermal field charcoal/charcoal draft tube of 350mm.
The tensile strength of the used carbon/carbon composite of this guide shell is 80MPa after tested, and compressive strength is 220MPa, and flexural strength is 95MPa, and shearing resistance is 60MPa.
Embodiment 3
(1) adopt 12K charcoal cloth and thin carbon fiber network tread ring to twine the accurate three way structure guide shell of back acupuncture precast body mutually, guide shell precast body volume density is 0.4g/cm
3, adopt the acupuncture technology to introduce fortifying fibre in guide shell precast body vertical direction, wherein, K represents tow thousand radicals;
(2) chemical vapour deposition densification technique feeds Sweet natural gas in chemical vapor deposition stove under 950 ℃ of conditions, the flow of Sweet natural gas is 3.0m
3/ h packs the guide shell precast body in the step (1) in the chemical vapor deposition stove into, carries out vapour deposition;
(3) resin impregnating charing densification technique: at pressure is under the 2.5MPa, dipping solidifies in vacuum-pressure resin impregnation curing oven with packing into through the guide shell precast body after the chemical vapour deposition in the step (2), the guide shell precast body floods and solidifies back commentaries on classics charring furnace charing processing, make the guide shell goods, solidification value is 220 ℃, and carbonization temperature is 1000 ℃;
(4) hot isostatic pressing bituminizing charing densification technique; At pressure is under the 80MPa, to step
(3) carry out the charing of hot isostatic pressing bituminizing through the guide shell goods after the resin impregnating charing densification in and handle, carbonization temperature is 680 ℃;
(5) guide shell extrudate density＜1.83g/cm that charing is handled through the hot isostatic pressing bituminizing in the step (4)
3The time, repeating step (4); Guide shell extrudate density 〉=1.83g/cm
3The time, densification technique finishes, and feeds at purifying furnace under the condition of chlorine and freonll-11, the guide shell goods is packed into carry out purification process in the purifying furnace, and cleansing temp is 2200 ℃;
(6) to the guide shell goods machined into after the process purification process in the step (5), promptly making its diameter is 350mm, and height is the monocrystalline silicon draw machines thermal field charcoal/charcoal draft tube of 380mm.
The tensile strength of the used carbon/carbon composite of this guide shell is 88MPa after tested, and compressive strength is 225MPa, and flexural strength is 85MPa, and shearing resistance is 65MPa.
Claims (3)
1. a monocrystalline silicon draw machines is characterized in that this method may further comprise the steps with the preparation method of thermal field charcoal/charcoal draft tube:
(1) adopt charcoal cloth and thin carbon fiber network tread ring to twine back acupuncture mutually and make accurate three way structure guide shell precast body, and introduce fortifying fibre in the acupuncture of guide shell precast body vertical direction, guide shell precast body volume density is 0.2-0.6g/cm
3
(2) chemical vapour deposition densification technique feeds propylene or Sweet natural gas in chemical vapor deposition stove under 800-1100 ℃ of condition, the flow of propylene or Sweet natural gas is 1.0-5.0m
3/ h packs the guide shell precast body in the step (1) in the chemical vapor deposition stove into, carries out vapour deposition;
(3) resin impregnating charing densification technique: at pressure is under the 1.5-3.0MPa, dipping solidifies in vacuum-pressure resin impregnation curing oven with packing into through the guide shell precast body after the chemical vapour deposition in the step (2), the guide shell precast body floods and solidifies back commentaries on classics charring furnace charing processing, make the guide shell goods, solidification value is 150-220 ℃, and carbonization temperature is 800-1100 ℃;
(4) hot isostatic pressing bituminizing charing densification technique; At pressure is under the 50-100MPa, handles carrying out the charing of hot isostatic pressing bituminizing through the guide shell goods after the resin impregnating charing densification in the step (3), and carbonization temperature is 550-750 ℃;
(5) guide shell extrudate density＜1.83g/cm that charing is handled through the hot isostatic pressing bituminizing in the step (4)
3The time, repeating step (4); Up to guide shell extrudate density 〉=1.83g/cm
3The time, densification technique finishes, and feeds at purifying furnace under the condition of chlorine and freonll-11, packs into and carries out purification process in the purifying furnace finishing fine and close guide shell goods, and cleansing temp is 2000-2500 ℃;
(6) to the guide shell goods machined into after the process purification process in the step (5), promptly make the monocrystalline silicon draw machines thermal field charcoal/charcoal draft tube.
2. the monocrystalline silicon draw machines according to claim 1 preparation method of thermal field charcoal/charcoal draft tube, it is characterized in that: the charcoal cloth in the step (1) is 12K charcoal cloth, and wherein K represents tow thousand radicals.
3. the monocrystalline silicon draw machines according to claim 1 preparation method of thermal field charcoal/charcoal draft tube, it is characterized in that: the monocrystalline silicon draw machines in the step (6) is 150-800mm with the diameter of thermal field charcoal/charcoal draft tube, height is 100-600mm.
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| CN101637815B (en) * | 2009-05-15 | 2010-12-29 | 西安超码科技有限公司 | Method for preparing carbon/carbon screws used for high-temperature smelting metals |
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