CN101478841A - Carbon/carbon heating body preparation method for polysilicon hydrogenation furnace - Google Patents
Carbon/carbon heating body preparation method for polysilicon hydrogenation furnace Download PDFInfo
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- CN101478841A CN101478841A CNA2008102365461A CN200810236546A CN101478841A CN 101478841 A CN101478841 A CN 101478841A CN A2008102365461 A CNA2008102365461 A CN A2008102365461A CN 200810236546 A CN200810236546 A CN 200810236546A CN 101478841 A CN101478841 A CN 101478841A
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Abstract
The invention discloses a method for preparing carbon/carbonate heating unit applied to a polysilicon hydrogenation furnace, wherein, a pinpricked plain wave carbon cloth quasi-three-needle structure prefabricated body is adopted; the prefabricated body is compacted through chemical vapor infiltration and the compaction processing is carried out repeatedly for several times; when the density is bigger than or equal to 1.30g/cm<3>, the compacting craft is over; mechanical processing is carried out after a high temperature treatment; then, CVD coating is carried out on the surface to obtain the carbon/carbonate heating unit. The method for preparing carbon/carbonate heating unit applied to a polysilicon hydrogenation furnace has the advantage that with the adoption of a craft method of chemical vapor infiltration, the carbon/carbonate heating unit is compactly obtained, thus can effectively improve purity and resistance of the heating unit in respect of the heating unit applied to the polysilicon hydrogenation furnace, improve anti-scouring capability and anticorrosion capacity of the heating unit, prolong service life of the heating unit and lower replacement rate of the heating unit.
Description
Technical field
The invention belongs to polysilicon hydrogenation furnace heater technical field, be specifically related to the preparation method of a kind of polysilicon hydrogenation furnace with charcoal/carbon/carbon heating body.
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 total output.When the improvement Siemens Method was produced polysilicon product, hydrogenation furnace was that the circulatory system is the step that product reclaims, and was about to generate the accessory substance SiCl that the polysilicon product reaction produces
4With H
2Reaction generates SiHCl
3Raw material utilizes again.In the hydrogenation furnace, under 1250 ℃ of conditions, SiCl
4With H
2Mist enter in the stove with the speed of 30m/s and react, furnace pressure reaches 0.6MPa.Therefore require heater purity height, do not pollute polysilicon product, have higher resistance value (0.06～0.25 Ω), high anti-the washing away of intensity.The hydrogenation furnace continuous operating time is more than 2000 hours, so will have a strong impact on the continuous operating time of hydrogenation furnace the useful life of heater.
Chinese patent ZL200610043185X, name is called and discloses the employing needled carbon cloth in " monocrystalline silicon draw machines and polysilicon smelting furnace with the preparation method of charcoal/charcoal heater " and combine with no latitude cloth and make full charcoal fiber three-dimensional structure heater precast body, matrix adopting asphalt carbon and resin charcoal double element carbon matrix, and under the condition in 2000～2500 ℃ of logical chlorine and fluorine Lyons, carry out purification process, its weak point is that (1) all is made of long charcoal fiber owing to the heater precast body, electric conductivity asphalt carbon component is preferably arranged again in the carbon matrix, and temperature surpasses the purification process more than 2000 ℃, the resistance value of its charcoal/carbon/carbon heating body only is 0.016～0.020 Ω, than the little order of magnitude of required value; (2) do not adopt vacuum pressed dipping technique scheme when furfural acetone resin or resin impregnating, dipping efficient on the low side 30%.
Russia makes polysilicon hydrogenation furnace and adopts charcoal cloth lamination precast body with charcoal/carbon/carbon heating body, through isothermal method chemical vapor infiltration technology densified, its weak point is: (1) charcoal cloth lamination precast body is prone to the thickness direction lamination defect in process of production, and rate of finished products is low; (2) the content of ashes height is generally 2000～4000ppm, is unsuitable for the applications that requires purity high.
Germany makes polysilicon hydrogenation furnace and adopts no latitude cloth lamination precast body with charcoal/carbon/carbon heating body, makes rectangular flat plate with the bituminizing pressurization, uses the graphite bolt that two rectangular flat plate are connected with the high purity graphite piece and makes.Its weak point: (1) graphite bolt strength is lower, adopts bolted to connect, and causes the coupling part contact resistance bigger, causes the heater local temperature inhomogeneous in the course of the work, thereby causes the inhomogeneous of the interior thermal field of hydrogenation furnace; (2) heater is that three parts are formed, and comparatively inconvenience is installed, and damages easily.
Summary of the invention
Technical problem to be solved by this invention is at above-mentioned deficiency of the prior art, the preparation method of the simple polysilicon hydrogenation furnace of a kind of technology with charcoal/carbon/carbon heating body is provided, fine and close respond well to prepare, has high resistance and high purity, thermal shock resistance and structural stability are good, and the polysilicon hydrogenation furnace of long service life charcoal/carbon/carbon heating body.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind of polysilicon hydrogenation furnace preparation method of charcoal/carbon/carbon heating body is characterized in that preparation process is:
(1) adopt charcoal cloth and short carbon fiber net tire alternative stacked, constitute plane fibers, introduce vertical fibers at the thickness direction employing needling process of plane fibers, make three-dimensional structure heater precast body, the density of precast body is 0.25～0.65g/cm
3
(2) chemical gas-phase permeation compaction technology: adopt the graphite frock with the inside and outside typing of the three-dimensional structure heater precast body in the step (1), with propylene or natural gas be raw material high temperature 850-1200 ℃ of following cracking, three-dimensional structure heater precast body is carried out gas-phase permeation compaction handles;
(3) condition of high vacuum degree high temperature purification treatment technology: the density 〉=1.30g/cm of the three-dimensional structure heater precast body in the step (2)
3The time, in vaccum sensitive stove, described three-dimensional structure heater precast body being carried out the condition of high vacuum degree high temperature purification treatment, described high temperature is meant that temperature is 1500-2300 ℃, described condition of high vacuum degree is meant vacuum degree≤40Pa; Density＜the 1.30g/cm of the three-dimensional structure heater in the step (2)
3The time, return to step (2);
(4) mechanical processing technique: to process drilling machine boring in the step (3) with milling machine through the charcoal/carbon/carbon heating body of condition of high vacuum degree high temperature purification treatment;
(5) chemical vapor deposited coatings being carried out on the charcoal after machining/carbon/carbon heating body surface in the step (4) handles, promptly make high resistance and high-purity polycrystalline hydrogenation furnace charcoal/carbon/carbon heating body, described high resistance is meant that resistance value is 0.06～0.25 Ω, and described high-purity is meant ash content≤800ppm.
Charcoal cloth described in the above-mentioned steps (1) is 6-48K plain weave charcoal cloth, and wherein K represents tow thousand radicals.
The resistivity of the charcoal/carbon/carbon heating body in the above-mentioned steps (3) after the condition of high vacuum degree high temperature purification treatment is 25～60 μ Ω m.
The treatment temperature of surface chemistry vapour deposition coating is 900-1200 ℃ described in the above-mentioned steps (5).
The width of described charcoal/carbon/carbon heating body is 60～200mm, highly is 1000～4000mm.
The present invention compared with prior art has the following advantages:
(1) adopts acupuncture 6～48K charcoal cloth and short carbon fiber net tire alternative stacked to make three-dimensional structure heater precast body, suitably reduce long stapled content, improved the resistance value of charcoal/carbon/carbon heating body; And short carbon fiber net tire provides the silk source of acupuncture vertical fibers, has increased the content of vertical fibers, has improved the ability of the anti-layering of precast body densification technique process;
(2) densification technique of employing chemical vapor infiltration, fine and close respond well, the deposit carbon Stability Analysis of Structures has good dimensional stability.
(3) adopt 1500-2300 ℃ high vacuum high temperature purification treatment, under the prerequisite that does not reduce charcoal/carbon/carbon heating body resistance value, can improve product purity again, and can improve thermal shock resistance and structural stability greatly.
(4) the heater product after the machine work is carried out surface chemistry vapour deposition (CVD) coating and handle, can effectively improve the erosion resistibility of heater product and at SiCl
4, the corrosion resistance in the HCl atmosphere.
(5) global formation, it is convenient to install, and not fragile, the useful life of energy significant prolongation charcoal/carbon/carbon heating body.
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
Description of drawings
Fig. 1 is a process chart of the present invention.
Fig. 2 uses the front view of charcoal/carbon/carbon heating body for the polysilicon hydrogenation furnace of the present invention's preparation.
Fig. 3 is the left view of Fig. 2.
Fig. 4 prepares polysilicon hydrogenation furnace is used the graphite frock with charcoal/carbon/carbon heating body structural representation for the present invention.
Embodiment
Embodiment 1
(1) adopt 6K charcoal cloth and short carbon fiber net tire alternative stacked to constitute the in-plane fiber, adopt needling process to introduce vertical fibers at thickness direction, make three-dimensional structure heater precast body, its density is 0.65g/cm
3
(2) chemical vapor infiltration technology adopts the graphite frock to finalize the design inside and outside the heater precast body, guarantees finished size; Under 850 ℃ of temperature, be that raw material carries out the gas-phase permeation compaction processing to precast body with the propylene;
(3) charcoal/carbon/carbon heating body extrudate density＜1.30g/cm
3The time, repeating step (2) is as its density 〉=1.30g/cm
3The time, densification technique finishes;
(4) condition of high vacuum degree high temperature purification treatment: charcoal/carbon/carbon heating body goods are packed in the vaccum sensitive stove, and treatment temperature is 1500 ℃, vacuum degree≤5Pa;
(5) machining: to process drilling machine boring in the step (4) with milling machine through charcoal/carbon/carbon heating body after the purification process;
(6) chemical vapour deposition (CVD) (being CVD) coating is carried out on the heater surface and handle, under 900 ℃, to be raw material with the propylene carry out the CVD carbon coating to the surface promptly makes polysilicon hydrogenation furnace with charcoal/carbon/carbon heating body.
Polysilicon hydrogenation furnace in the above-mentioned steps (6) is 60mm with the width of charcoal/carbon/carbon heating body, highly is 1000mm.
Embodiment 2
(1) adopt 12K charcoal cloth and short carbon fiber net tire alternative stacked to constitute the in-plane fiber, adopt needling process to introduce vertical fibers at thickness direction, make three-dimensional structure heater precast body, its density is 0.45g/cm
3
(2) chemical vapor infiltration technology adopts the graphite frock to finalize the design inside and outside the heater precast body, guarantees finished size; Under 1040 ℃ of temperature, be that raw material carries out the gas-phase permeation compaction processing to precast body with the natural gas;
(3) charcoal/carbon/carbon heating body extrudate density＜1.30g/cm
3The time, repeating step (2) is as its density 〉=1.30g/cm
3The time, densification technique finishes;
(4) condition of high vacuum degree high temperature purification treatment: charcoal/carbon/carbon heating body goods are packed in the vaccum sensitive stove, and temperature is 2000 ℃, vacuum degree≤20Pa;
(5) machining: to process drilling machine boring in the step (4) with milling machine through charcoal/carbon/carbon heating body after the purification process;
(6) chemical vapor deposited coatings is carried out on the heater surface and handle, under 980 ℃, to be raw material with the propylene carry out the CVD carbon coating to the surface promptly makes polysilicon hydrogenation furnace with charcoal/carbon/carbon heating body.
Polysilicon hydrogenation furnace in the above-mentioned steps (6) is 100mm with the width of charcoal/carbon/carbon heating body, highly is 2000mm.
Embodiment 3
(1) adopt 48K charcoal cloth and short carbon fiber net tire alternative stacked to constitute the in-plane fiber, adopt needling process to introduce vertical fibers at thickness direction, make three-dimensional structure heater precast body, its density is 0.25g/cm
3
(2) chemical vapor infiltration technology adopts the graphite frock to finalize the design inside and outside the heater precast body, guarantees finished size; Under 1200 ℃ of temperature, be that raw material carries out the gas-phase permeation compaction processing to precast body with the natural gas;
(3) charcoal/carbon/carbon heating body extrudate density＜1.30g/cm
3The time, repeating step (2) is as its density 〉=1.30g/cm
3The time, densification technique finishes;
(4) condition of high vacuum degree high temperature purification treatment: charcoal/carbon/carbon heating body goods are packed in the vaccum sensitive stove, and temperature is 2300 ℃, vacuum degree≤40Pa;
(5) machining: to process drilling machine boring in the step (4) with milling machine through charcoal/carbon/carbon heating body after the purification process;
(6) chemical vapor deposited coatings is carried out on the heater surface and handle, under 1200 ℃, to be raw material with the natural gas carry out the CVD carbon coating to the surface promptly makes polysilicon hydrogenation furnace with charcoal/carbon/carbon heating body.
Polysilicon hydrogenation furnace in the above-mentioned steps (6) is 200mm with the width of charcoal/carbon/carbon heating body, highly is 4000mm.
The above; it only is preferred embodiment of the present invention; be not that the present invention is imposed any restrictions, everyly any simple modification that above embodiment did, change and equivalence changed, all still belong in the protection range of technical solution of the present invention according to the technology of the present invention essence.
Claims (5)
1. a polysilicon hydrogenation furnace is characterized in that preparation process is with the preparation method of charcoal/carbon/carbon heating body:
(1) adopt charcoal cloth and short carbon fiber net tire alternative stacked, constitute plane fibers, introduce vertical fibers at the thickness direction employing needling process of plane fibers, make three-dimensional structure heater precast body, the density of precast body is 0.25～0.65g/cm
3
(2) chemical gas-phase permeation compaction technology: adopt the graphite frock with the inside and outside typing of the three-dimensional structure heater precast body in the step (1), with propylene or natural gas be raw material high temperature 850-1200 ℃ of following cracking, three-dimensional structure heater precast body is carried out gas-phase permeation compaction handles;
(3) condition of high vacuum degree high temperature purification treatment technology: the density 〉=1.30g/cm of the three-dimensional structure heater precast body in the step (2)
3The time, in vaccum sensitive stove, described three-dimensional structure heater precast body being carried out the condition of high vacuum degree high temperature purification treatment, described high temperature is meant that temperature is 1500-2300 ℃, described condition of high vacuum degree is meant vacuum degree≤40Pa; Density＜the 1.30g/cm of the three-dimensional structure heater in the step (2)
3The time, return to step (2);
(4) mechanical processing technique: to process drilling machine boring in the step (3) with milling machine through the charcoal/carbon/carbon heating body of condition of high vacuum degree high temperature purification treatment;
(5) chemical vapor deposited coatings being carried out on the charcoal after machining/carbon/carbon heating body surface in the step (4) handles, promptly make high resistance and high-purity polycrystalline hydrogenation furnace charcoal/carbon/carbon heating body, described high resistance is meant that resistance value is 0.06～0.25 Ω, and described high-purity is meant ash content≤800ppm.
2. according to the preparation method of the described a kind of polysilicon hydrogenation furnace of claim 1 with charcoal/carbon/carbon heating body, it is characterized in that charcoal cloth described in the step (1) is 6-48K plain weave charcoal cloth, wherein K represents tow thousand radicals.
3. according to the preparation method of the described a kind of polysilicon hydrogenation furnace of claim 1 with charcoal/carbon/carbon heating body, the resistivity that it is characterized in that the charcoal/carbon/carbon heating body after the condition of high vacuum degree high temperature purification treatment in the step (3) is 25～60 μ Ω m.
4. according to the preparation method of the described a kind of polysilicon hydrogenation furnace of claim 1 with charcoal/carbon/carbon heating body, the treatment temperature that it is characterized in that surface chemistry vapour deposition coating described in the step (5) is 900-1200 ℃.
5. according to the preparation method of the described a kind of polysilicon hydrogenation furnace of arbitrary claim among the claim 1-4 with charcoal/carbon/carbon heating body, it is characterized in that: the width of described charcoal/carbon/carbon heating body is 60～200mm, highly is 1000～4000mm.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101541111B (en) * | 2009-04-22 | 2010-10-13 | 蒋建纯 | U-shaped heating element of silicon tetrachloride hydrogenation furnace and manufacturing process thereof |
| CN102490259A (en) * | 2011-12-30 | 2012-06-13 | 湖南南方搏云新材料有限责任公司 | Mould device for producing U-shaped heating body blank |
| 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 |
| CN105367105A (en) * | 2015-11-27 | 2016-03-02 | 西北工业大学 | Method for preparing thick-walled ceramic-matrix composite material through mechanical processing assisted CVI (Chemical Vapor Infiltration) |
| CN106278343A (en) * | 2016-07-29 | 2017-01-04 | 烟台鲁航炭材料科技有限公司 | A kind of manufacture method of giant chemical vapour deposition resistance furnace C/C heater |
| 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 |
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| CN115974571A (en) * | 2022-12-28 | 2023-04-18 | 湖南金博碳基材料研究院有限公司 | Heating cylinder device and preparation method thereof |
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| JP2000351689A (en) * | 1999-06-08 | 2000-12-19 | Toyo Tanso Kk | Carbon fiber-reinforced carbon composite material coated with pyrolyzed carbon and part for single crystal-pulling device |
| CN100366581C (en) * | 2006-07-20 | 2008-02-06 | 西安超码科技有限公司 | Making process of C/C heater for monocrystal silicon drawing furnace and polycrystal silicon smelting furnace |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101541111B (en) * | 2009-04-22 | 2010-10-13 | 蒋建纯 | U-shaped heating element of silicon tetrachloride hydrogenation furnace and manufacturing process thereof |
| 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 |
| CN102490259A (en) * | 2011-12-30 | 2012-06-13 | 湖南南方搏云新材料有限责任公司 | Mould device for producing U-shaped heating body blank |
| CN105367105A (en) * | 2015-11-27 | 2016-03-02 | 西北工业大学 | Method for preparing thick-walled ceramic-matrix composite material through mechanical processing assisted CVI (Chemical Vapor Infiltration) |
| CN106278343A (en) * | 2016-07-29 | 2017-01-04 | 烟台鲁航炭材料科技有限公司 | A kind of manufacture method of giant chemical vapour deposition resistance furnace C/C heater |
| 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 |
| CN110016803A (en) * | 2019-04-04 | 2019-07-16 | 碳翁(北京)科技有限公司 | A kind of high temperature resistant fibre electroheating and its application |
| CN115974571A (en) * | 2022-12-28 | 2023-04-18 | 湖南金博碳基材料研究院有限公司 | Heating cylinder device and preparation method thereof |
| CN115974571B (en) * | 2022-12-28 | 2023-11-24 | 湖南金博碳基材料研究院有限公司 | Heating tube device and preparation method thereof |
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