CN101638322B - Method for preparing carbon/carbon heat shields used for polysilicon hydriding furnances - Google Patents
Method for preparing carbon/carbon heat shields used for polysilicon hydriding furnances Download PDFInfo
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- CN101638322B CN101638322B CN2009100225409A CN200910022540A CN101638322B CN 101638322 B CN101638322 B CN 101638322B CN 2009100225409 A CN2009100225409 A CN 2009100225409A CN 200910022540 A CN200910022540 A CN 200910022540A CN 101638322 B CN101638322 B CN 101638322B
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Abstract
The invention discloses a method for preparing carbon/carbon heat shields used for polysilicon hydriding furnances, comprising the following steps: adopting carbon cloths and short carbon fiber mesh tires to be hoop wound alternately to form plane fibers and introducing reinforcing fibers in the vertical direction to prepare three-dimensional heat shield preforms, carrying out the followings on the three-dimensional heat shield preforms in sequence: chemical vapor infiltration and densification processes, resin or pitch impregnation and carbonization treatment, high-temperature purification treatment and mechanical processing, and carrying out chemical vapor deposition coating treatment on the surfaces of the carbon/carbon heat shields undergoing mechanical processing, thus obtaining the high-purity carbon/carbon heat shields. The method is simple in processes, short in cycle and low in cost, can improve the product purity under the premise of not reducing the heat insulation of the carbon/carbon heat shields obviously, can greatly improve the heat shock resistance and structural stability, can effectively enhance the erosion resistibility and corrosion resistance under the atmospheres of SiCl4 and HCl of the heat shield products and prolongs the service lives.
Description
Technical field
The invention belongs to polysilicon hydrogenation furnace and use the lagging material technical field, be specifically related to the preparation method of a kind of polysilicon hydrogenation furnace with charcoal/charcoal thermoscreen.
Background technology
At present, the main method of producing polysilicon is the improvement Siemens Method, adopts the polysilicon of improvement Siemens Method production to account for more than 80% of global polysilicon ultimate production.Produce in the polysilicon process at the improvement Siemens Method, hydrogenation furnace is the major equipment of the recycle system of reaction product recovery, is about to byproduct of reaction SiCl
4With H
2Reaction generates SiHCl
3Raw material utilizes again.In the hydrogenation furnace, SiCl
4With H
2Mixed gas under 1250 ℃ of conditions, react, thermoscreen is the outside lagging material of Heating element, also is for above-mentioned reaction a homothermic zone to be provided.Therefore require the thermoscreen thermal insulation good, the purity height does not pollute polysilicon product, high anti-the washing away of intensity.The hydrogenation furnace continuous operating time is more than 2000 hours, so will have influence on the continuous operating time of hydrogenation furnace the work-ing life of thermoscreen.
Chinese patent ZL200610043184.5; Name is called and discloses the employing needled carbon cloth in " monocrystalline silicon draw machines and polysilicon smelting furnace are with the preparation method of thermal field charcoal/charcoal thermoscreen " and combine with no latitude cloth and process three way structure thermoscreen precast body; Matrix adopting asphalt carbon and resin charcoal double element carbon matrix; And under the condition of 2000～2500 ℃ of logical chlorine or freonll-11, carry out purification process; Its weak point does not adopt vacuum pressed dipping technique scheme when being (1) bituminizing, dipping efficient is on the low side 30%, and the cycle grows up to this height; (2) do not carry out coating after the machining and handle, surface irregularity, fine and close inadequately, anti-air scour ability and corrosion resistance are relatively poor.
Russia's preparation polysilicon hydrogenation furnace adopts charcoal cloth lamination to twine precast body with charcoal/charcoal thermoscreen, and pure chemistry gas-phase permeation technology is fine and close, and top coat is handled.This chemical vapor infiltration technology method for densifying cycle is long, and efficient is low, and cost is high.The about 1000mm of its product diameter, dimensions is less, can not satisfy the demand of hydrogenation furnace to the large size development gradually.
Germany Xi Geli prepares polysilicon hydrogenation furnace with charcoal/charcoal thermoscreen, adopts no latitude cloth lamination precast body, makes rectangular flat plate with the bituminizing pressurization; Use the anistree splicing of bolt hoop; Its shortcoming is that jointing positions has seam, and poor sealing can't be born big pressure in the hydrogenation furnace; And comparatively inconvenience is installed, damages easily.The thermoscreen product of this structure polysilicon enterprise is at home tried out, and has bigger design defect, can not satisfy the thermoscreen functional requirement fully.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of technology simple to above-mentioned deficiency of the prior art, and the cycle is short, and lower-cost polysilicon hydrogenation furnace is with the preparation method of charcoal/charcoal thermoscreen.This method can improve product purity again under the prerequisite that does not significantly reduce charcoal/charcoal thermoscreen thermal insulation, and can improve heat-shock resistance and structural stability greatly, can effectively improve the erosion resistibility of thermoscreen product and at SiCl
4, the corrosion resistance in the HCl atmosphere, increase the service life.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind of polysilicon hydrogenation furnace is characterized in that with the preparation method of charcoal/charcoal thermoscreen the preparation process is:
(1) adopt 6-48K charcoal cloth and short carbon fiber net tire to replace hoop and twine the formation plane fibers, adopt needling process to introduce fortifying fibre in vertical charcoal cloth direction, processing volume density is 0.25～0.55g/cm
3Three way structure thermoscreen precast body, needling density 25～45 pins/cm
2, wherein, K represents tow thousand radicals;
(2) chemical gas-phase permeation compaction technology: with propylene or Sweet natural gas is the cracking under high temperature 850-1200 ℃ condition of charcoal source gas; Three way structure thermoscreen precast body is carried out gas-phase permeation compaction handle, make the volume density>=0.40g/cm of three way structure thermoscreen precast body
3
(3) resin or bituminizing, charing treatment process: this operation is divided two kinds of methods: a kind of for resin or pitch vacuum impregnation charing, in the vacuum impregnation jar, vacuum tightness≤-vacuum state of 0.090MPa under, to volume density>=0.40g/cm
3Three way structure thermoscreen precast body dipping go out jar after 2-4 hour, change charring furnace again over to and carry out charing and handle, process charcoal/charcoal thermoscreen precast body; A kind of is resin or pitch pressure impregnation solidifying, carbonizing, in the pressure impregnation jar, is under the condition of 1.5～2.0Mpa, to volume density>=0.40g/cm at pressure
3Three way structure thermoscreen precast body dipping go out jar after 3-5 hour, be cured processing again, change charring furnace then over to and carry out charing and handle charcoal/charcoal thermoscreen precast body; Wherein, the solidification treatment temperature is 190 ℃, and carbonization temperature is 800-1000 ℃, and said resin is acetone-furfural resin or resol;
(4) high temperature purification treatment technology: repeating step (3), as the volume density>=1.0g/cm of charcoal/charcoal thermoscreen precast body
3The time, in purifying furnace, under the condition of feeding chlorine or freonll-11 charcoal/charcoal thermoscreen precast body is carried out high temperature purification treatment, the high temperature purification treatment temperature is 2300-2800 ℃;
(5) charcoal/charcoal thermoscreen precast body through high temperature purification treatment in the step (4) is machined, process charcoal/charcoal thermoscreen;
(6) charcoal/charcoal thermoscreen after machining in the step (5) is carried out the chemical vapour deposition top coat and handle, promptly make highly purified charcoal/charcoal thermoscreen, said high purity is meant ash content≤50ppm.
Charcoal cloth described in the above-mentioned steps (1) is plain weave, twill or satin weave charcoal cloth.
The chemical gas-phase permeation compaction treatment temp is 850-1200 ℃ described in the above-mentioned steps (2).
Chemical vapour deposition top coat treatment temp is 900-1200 ℃ described in the above-mentioned steps (6).
The thermal conductivity of charcoal described in the above-mentioned steps (6)/charcoal thermoscreen is 5～30W/mK.
The diameter of charcoal described in the above-mentioned steps (6)/charcoal thermoscreen is 1000～1800mm.
The present invention compared with prior art has the following advantages:
(1) adopts acupuncture 6～48K plain weave, twill or satin weave charcoal cloth and short carbon fiber net tire to replace the hoop winding and make three way structure thermoscreen precast body, improved the intensity and the thermal insulation of charcoal/charcoal thermoscreen; And short carbon fiber net tire provides radially vertical fibers, has improved the anti-stratified ability of precast body densification technique process;
(2) adopt chemical vapor infiltration sclerosis precast body, the densification technique that combines is handled in resin or bituminizing charing, and technology is simple, and the cycle is short, and cost is lower.
(3) adopt 2300-2800 ℃ high temperature purification treatment, under the prerequisite that does not significantly reduce charcoal/charcoal thermoscreen thermal insulation, can improve product purity again, and can improve heat-shock resistance and structural stability greatly.
(4) the thermoscreen product after the machining is carried out surface C VD coating and handle, can effectively improve the erosion resistibility of thermoscreen product and at SiCl
4, the corrosion resistance in the HCl atmosphere, increase the service life.
(5) hoop global formation highly passes through from buckle, and it is convenient to install, and not fragile, the work-ing life of ability significant prolongation charcoal/charcoal thermoscreen.
Through accompanying drawing and embodiment, technical scheme of the present invention is done further detailed description below.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Embodiment 1
(1) adopts 12K plain weave charcoal cloth and short carbon fiber net tire to replace hoop and twine, adopt needling process to introduce vertical fibers, process three way structure heating element precast body, needling density 35～40 pins/cm at thickness direction
2, its volume density is 0.45g/cm
3
(2) chemical vapor infiltration technology under 940 ℃ of temperature, is that charcoal source gas carries out the gas-phase permeation compaction processing to precast body with the propylene;
(3) resin or pitch vacuum impregnation charing, charcoal/charcoal thermoscreen product volume density>=0.50g/cm
3The time, carry out acetone-furfural resin, resol or pitch vacuum impregnation and handle, vacuum tightness≤-0.094MPa, carry out 900 ℃ of charings after the dipping and handle;
(4) high temperature purification treatment: repeating step (3), as its volume density>=1.20g/cm
3The time, densification technique finishes, and under the condition of 2600 ℃ of feeding chlorine or freonll-11, goods is carried out high temperature purification treatment;
(5) mechanical workout: to using machined into through charcoal/charcoal thermoscreen after the purification process in the step (4);
(6) the CVD coating being carried out on the thermoscreen surface and handle, under 960 ℃, is that charcoal source gas carries out the CVD carbon coating to the surface and promptly makes polysilicon hydrogenation furnace with charcoal/charcoal thermoscreen with the propylene.
Polysilicon hydrogenation furnace in the above-mentioned steps (6) uses the diameter of charcoal/charcoal thermoscreen to be 1000mm.
Embodiment 2
(1) adopts 6K twill charcoal cloth and short carbon fiber net tire to replace hoop and twine, adopt needling process to introduce vertical fibers, process three way structure heating element precast body, needling density 25～30 pins/cm at thickness direction
2, its volume density is 0.25g/cm
3
(2) chemical vapor infiltration technology under 850 ℃ of temperature, is that charcoal source gas carries out the gas-phase permeation compaction processing to precast body with the propylene;
(3) resin or pitch vacuum impregnation charing, charcoal/charcoal thermoscreen product volume density>=0.40g/cm
3The time, carry out acetone-furfural resin, resol or pitch vacuum impregnation and handle, vacuum tightness≤-0.090MPa, carry out 800 ℃ of charings after the dipping and handle;
(4) high temperature purification treatment: repeating step (3), as its volume density>=1.0g/cm
3The time, densification technique finishes, and under the condition of 2300 ℃ of feeding chlorine or freonll-11, goods is carried out high temperature purification treatment;
(5) mechanical workout: to using machined into through charcoal/charcoal thermoscreen after the purification process in the step (4);
(6) the CVD coating being carried out on the thermoscreen surface and handle, under 900 ℃, is that charcoal source gas carries out the CVD carbon coating to the surface and promptly makes polysilicon hydrogenation furnace with charcoal/charcoal thermoscreen with the propylene.
Polysilicon hydrogenation furnace in the above-mentioned steps (6) uses the diameter of charcoal/charcoal thermoscreen to be 1500mm.
Embodiment 3
(1) adopts 48K satin weave charcoal cloth and short carbon fiber net tire to replace hoop and twine, adopt needling process to introduce vertical fibers, process three way structure heating element precast body, needling density 40～45 pins/cm at thickness direction
2, its volume density is 0.55g/cm
3
(2) chemical vapor infiltration technology under 1200 ℃ of temperature, is that charcoal source gas carries out the gas-phase permeation compaction processing to precast body with the Sweet natural gas;
(3) resin or the charing of pitch pressure impregnation, charcoal/charcoal thermoscreen product volume density>=0.60g/cm
3The time, carrying out acetone-furfural resin, resol or pitch pressure impregnation and handle, 1.5～2.0MPa pressure goes out jar about dipping 4h down, and acetone-furfural resin, resol are cured, and treatment temp is 190 ℃, carries out 1000 ℃ of charings afterwards and handles;
(4) high temperature purification treatment: repeating step (3), as its volume density>=1.3g/cm
3The time, densification technique finishes, and under the condition of 2800 ℃ of feeding chlorine or freonll-11, goods is carried out high temperature purification treatment;
(5) mechanical workout: to using machined into through charcoal/charcoal thermoscreen after the purification process in the step (4);
(6) the CVD coating being carried out on the thermoscreen surface and handle, under 1200 ℃, is that charcoal source gas carries out the CVD carbon coating to the surface and promptly makes polysilicon hydrogenation furnace with charcoal/charcoal thermoscreen with the Sweet natural gas.
Polysilicon hydrogenation furnace in the above-mentioned steps (6) uses the diameter of charcoal/charcoal thermoscreen to be 1800mm.
The above; It only is preferred embodiment of the present invention; Be not that the present invention is done any restriction, every technical spirit changes any simple modification, change and the equivalence that above embodiment did according to the present invention, all still belongs in the protection domain of technical scheme of the present invention.
Claims (5)
1. a polysilicon hydrogenation furnace is characterized in that with the preparation method of charcoal/charcoal thermoscreen the preparation process is:
(1) adopt 6-48K charcoal cloth and short carbon fiber net tire to replace hoop and twine the formation plane fibers, adopt needling process to introduce fortifying fibre in vertical charcoal cloth direction, processing volume density is 0.25～0.55g/cm
3Three way structure thermoscreen precast body, needling density 25～45 pins/cm
2, wherein, K represents tow thousand radicals;
(2) chemical gas-phase permeation compaction technology: with propylene or Sweet natural gas is the cracking under high temperature 850-1200 ℃ condition of charcoal source gas; Three way structure thermoscreen precast body is carried out gas-phase permeation compaction handle, make the volume density>=0.40g/cm of three way structure thermoscreen precast body
3
(3) resin or bituminizing, charing treatment process: this operation is divided two kinds of methods: a kind of for resin or pitch vacuum impregnation charing, in the vacuum impregnation jar, vacuum tightness≤-vacuum state of 0.090MPa under, to volume density>=0.40g/cm
3Three way structure thermoscreen precast body dipping go out jar after 2-4 hour, change charring furnace again over to and carry out charing and handle, process charcoal/charcoal thermoscreen precast body; A kind of is resin or pitch pressure impregnation solidifying, carbonizing, in the pressure impregnation jar, is under the condition of 1.5～2.0MPa, to volume density>=0.40g/cm at pressure
3Three way structure thermoscreen precast body dipping go out jar after 3-5 hour, be cured processing again, change charring furnace then over to and carry out charing and handle, process charcoal/charcoal thermoscreen precast body; Wherein, the solidification treatment temperature is 190 ℃, and carbonization temperature is 800-1000 ℃, and said resin is acetone-furfural resin or resol;
(4) high temperature purification treatment technology: repeating step (3), as the volume density>=1.0g/cm of charcoal/charcoal thermoscreen precast body
3The time, in purifying furnace, under the condition of feeding chlorine or freonll-11 charcoal/charcoal thermoscreen precast body is carried out high temperature purification treatment, the high temperature purification treatment temperature is 2300-2800 ℃;
(5) charcoal/charcoal thermoscreen precast body through high temperature purification treatment in the step (4) is machined, process charcoal/charcoal thermoscreen;
(6) charcoal/charcoal thermoscreen after machining in the step (5) is carried out the chemical vapour deposition top coat and handle, promptly make highly purified charcoal/charcoal thermoscreen, said high purity is meant ash content≤50ppm; Said chemical vapour deposition top coat treatment temp is 900-1200 ℃.
2. according to the preparation method of the described a kind of polysilicon hydrogenation furnace of claim 1, it is characterized in that charcoal cloth described in the step (1) is plain weave, twill or satin weave charcoal cloth with charcoal/charcoal thermoscreen.
3. according to the preparation method of the described a kind of polysilicon hydrogenation furnace of claim 1, it is characterized in that the chemical gas-phase permeation compaction treatment temp is 850-1200 ℃ described in the step (2) with charcoal/charcoal thermoscreen.
4. according to the preparation method of the described a kind of polysilicon hydrogenation furnace of claim 1, it is characterized in that the thermal conductivity of charcoal described in the step (6)/charcoal thermoscreen is 5～30W/mK with charcoal/charcoal thermoscreen.
5. according to the preparation method of the described a kind of polysilicon hydrogenation furnace of claim 1, it is characterized in that the diameter of charcoal described in the step (6)/charcoal thermoscreen is 1000～1800mm with charcoal/charcoal thermoscreen.
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| CN102093068A (en) * | 2010-11-18 | 2011-06-15 | 西北工业大学 | Method for preparing intermediate phase pitch-based carbon/carbon composite |
| CN102167325B (en) * | 2010-12-27 | 2012-07-25 | 湖南南方搏云新材料有限责任公司 | Carbon/carbon heat screen of polysilicon hydrogenation furnace and manufacture method thereof |
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| 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 |
| CN113915021B (en) * | 2021-09-29 | 2022-11-22 | 湖北瑞宇空天高新技术有限公司 | Cylindrical prefabricated body, light high-temperature-resistant composite piston and preparation method thereof |
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