CN101311140A - Method for preparing charcoal/charcoal heating element of high resistance and high purity - Google Patents
Method for preparing charcoal/charcoal heating element of high resistance and high purity Download PDFInfo
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- CN101311140A CN101311140A CNA2008100180263A CN200810018026A CN101311140A CN 101311140 A CN101311140 A CN 101311140A CN A2008100180263 A CNA2008100180263 A CN A2008100180263A CN 200810018026 A CN200810018026 A CN 200810018026A CN 101311140 A CN101311140 A CN 101311140A
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Abstract
The invention relates to a preparation method for a carbon/a carbon heating unit with high resistance and high purity; in the method, carbon cloth and short carbon fiber web fetus are adopted to be alternately laminated or wound into a cylinder to form horizontal fabric which is added with vertical fabric along the thickness direction by adopting a needling technique to prepare a prefabricated body of the heating unit with a three-direction structure; the prefabricated body is processed with furfural acetone resin or phenolic resin vacuum pressure impregnation and curing treatment, charring at normal pressure and other densification techniques until the density reaches 1.55g/cm<3> and then high-temperature vacuum purification is carried out below 2,000 DGE C and the carbon/the carbon heating unit with high resistance and high purity can be produced after mechanical processing. The carbon/the carbon heating unit of the invention has outstanding features of high resistance and high purity and has the advantages of short production period, low production period and long service life, which is mainly applicable to a U-shaped heating unit of a polysilicon hydrogenation furnace as well as a large cylindrical heating unit of a polysilicon pulling furnace.
Description
Technical field
The invention belongs to polysilicon hydrogenation furnace and silicon single crystal lifting furnace heating element technical field, be specifically related to a kind of preparation method of high resistance and high purity charcoal/carbon/carbon heating body.
Background technology
Polysilicon, silicon single crystal, silicon sheet material are the most important main functionality materials of semi-conductor industry, are first function electronic materials, so far all being made by silicon chip more than 95% of integrated circuit (IC) chip and classes of semiconductors device in the world.Hydrogenation furnace, the silicon single crystal lifting furnace of producing polysilicon all need supporting charcoal/carbon/carbon heating body, require to have higher resistance value (0.08～0.2 Ω) and high purity (ash content≤50ppm) usually.
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 well heater " and combine with no latitude cloth and make full charcoal fiber three way structure well 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 well heater precast body, 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 the vacuum impregnation technical scheme when acetone-furfural resin or resin impregnating, dipping efficient on the low side 30%.
Russia makes polysilicon hydrogenation furnace and the silicon single crystal lifting furnace adopts charcoal cloth lamination or coiling precast body with charcoal/carbon/carbon heating body, through isothermal method chemical vapor infiltration technology densified, does not pass through high temperature purification treatment.Its weak point is: (1) charcoal cloth lamination precast body is prone to the thickness direction lamination defect in process of production, and yield rate is low; (2) the ash oontent height is generally 2000～4000ppm, is unsuitable for the applications that requires purity high.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, and provide a kind of with short production cycle, the preparation method of high resistance and high purity charcoal/carbon/carbon heating body that cost is low, high and high polysilicon hydrogenation furnace and the silicon single crystal lifting furnace heating element of purity with the preparation resistance value, the work-ing life of prolongation heating element.
For achieving the above object, the technical solution adopted in the present invention is: a kind of preparation method of high resistance and high purity charcoal/carbon/carbon heating body is characterized in that may further comprise the steps:
(1) employing charcoal cloth and short carbon fiber net tire alternative stacked or alternately circumvolution round shape constitute the in-plane fiber, adopt needling process to introduce vertical fibers at thickness direction, make three way structure heating element precast body, and its density is 0.25～0.65g/cm
3
(2) acetone-furfural resin or resol vacuum-impregnating by pressure solidifies densified: earlier with acetone-furfural resin or resol preheating, and the heating element precast body in the step (1) packed into vacuumize in the impregnating autoclave, preheating, suck acetone-furfural resin or resol, at pressure is to flood 2-6 hour under 1.0～4.0MPa, after Vent presses, inserts resin return tube inflated with nitrogen, pressure is to eject unnecessary resin under the 0.2Mpa, and dip treating finishes; Be cured processing again;
(3) the normal pressure charing is handled: the charcoal/carbon/carbon heating body precast body that will flood solidification treatment is packed in the charring furnace, carries out the charing processing under nitrogen protection, makes charcoal/carbon/carbon heating body goods;
(4) charcoal in step (3)/carbon/carbon heating body extrudate density＜1.55g/cm
3The time, repeating step (2), step (3); As its density 〉=1.55g/cm
3The time, densification technique finishes;
(5) lesser temps, condition of high vacuum degree purification process: the charcoal in the step (4)/carbon/carbon heating body goods are packed in the vacuum induction furnace, carry out purification process, temperature is 1400～2000 ℃, and vacuum tightness is 1-40Pa;
(6) to charcoal/carbon/carbon heating body milling machine, machined into after the process purification process in the step (5), drilling machine boring promptly makes high resistance and high purity charcoal/carbon/carbon heating body, and described high resistance is meant that resistance value is 0.08～0.2 Ω, and described high purity is meant ash content≤50ppm.
Charcoal cloth described in the step (1) is 3～24K plain weave charcoal cloth, and wherein K represents tow thousand radicals.
Preheating temperature is 40～80 ℃ described in the step (2), and the described vacuum tightness that vacuumizes is 200～1000Pa, and described solidification treatment temperature is 160～230 ℃, and pressure is 1.0～4.0Mpa.
Nitrogen flow is 600～1200L/h described in the step (3), and described charing treatment temp is 850～1200 ℃.
The resistivity of the charcoal/carbon/carbon heating body goods of preparation is 30～50 μ Ω/m in the step (5).
High resistance and high purity charcoal/carbon/carbon heating body described in the step (6) is the U-shaped heating element of polysilicon hydrogenation furnace.The width of described U-shaped heating element is 60～200mm, highly is 1000～4000mm.
High resistance and high purity charcoal/carbon/carbon heating body described in the step (6) is the round shape heating element of silicon single crystal lifting furnace.The diameter of described round shape heating element is
400～
2000mm highly is 600～2000mm.
The present invention compared with prior art has the following advantages:
(1) adopts acupuncture 3～24K charcoal cloth and short carbon fiber net tire alternative stacked to make three way structure heating element 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 anti-stratified ability of precast body densification technique process;
(2) when acetone-furfural resin or resin impregnating, adopt the technical scheme that vacuumizes, air emptying in precast body or the charcoal/carbon/carbon heating body hole can be able to be improved dipping efficient 30%, shortened the production cycle of charcoal/carbon/carbon heating body, reduced manufacturing cost;
(3) adopt the higher resin charcoal unit matrix of resistance value, can effectively improve the resistance value of charcoal/carbon/carbon heating body and the homogeneity of resistance thereof; And resin charcoal sealing of hole is good, and erosion resistance is strong, can prolong the work-ing life of charcoal/carbon/carbon heating body;
(4) adopt lesser temps high vacuum purification process, can guarantee not reduce under the prerequisite of charcoal/carbon/carbon heating body resistance value, can remove impurity again, reach the high purity (requirement of ash content≤50ppm).
Embodiment
The present invention will be further described below in conjunction with embodiment.
Embodiment 1
(1) employing charcoal cloth and short carbon fiber net tire alternative stacked or alternately circumvolution round shape constitute the in-plane fiber, adopt needling process to introduce vertical fibers at thickness direction, make three way structure heating element precast body, and its density is 0.25g/cm
3
(2) acetone-furfural resin or resol vacuum-impregnating by pressure is solidified densified: earlier with 40 ℃ of acetone-furfural resin or resol preheatings, and the heating element precast body in the step (1) packed into vacuumize in the impregnating autoclave, vacuum tightness 200Pa, preheating temperature is 50 ℃, sucks acetone-furfural resin or resol, is to flood 2 hours under the 1.0MPa at pressure, after Vent presses, insert resin return tube inflated with nitrogen, pressure is to eject unnecessary resin under the 0.2Mpa, and dip treating finishes.Be cured processing again, pressure is 160 ℃ for the 1.0MPa temperature;
(3) the normal pressure charing is handled: the charcoal/carbon/carbon heating body that will flood solidification treatment is packed in the charring furnace, and under nitrogen protection, its flow is that 600L/h carries out the charing processing, and carbonization temperature is 850 ℃, makes charcoal/carbon/carbon heating body goods;
(4) charcoal/carbon/carbon heating body extrudate density＜1.55g/cm
3The time, repeating step (2), step (3); As its density 〉=1.55g/cm
3The time, densification technique finishes;
(5) lesser temps condition of high vacuum degree purification process: charcoal/carbon/carbon heating body goods are packed in the vacuum induction furnace, and temperature is 1400 ℃, and vacuum tightness is 1Pa, carries out lesser temps condition of high vacuum degree purification process;
(6) to charcoal/carbon/carbon heating body milling machine, machined into after the process purification process in the step (5), drilling machine boring promptly makes high resistance and high purity charcoal/carbon/carbon heating body, the U-shaped heating element that can be used for polysilicon hydrogenation furnace also can be used for the round shape heating element of silicon single crystal lifting furnace.
Charcoal cloth in the above-mentioned steps (1) is 3K plain weave charcoal cloth, and wherein K represents tow thousand radicals.
The purity of charcoal in the above-mentioned steps (5)/carbon/carbon heating body goods is ash content≤50ppm, and resistivity is 30 μ Ω/m, and resistance value is 0.08 Ω.
Polysilicon hydrogenation furnace in the above-mentioned steps (6) is 60mm with the width of U-shaped heating element, highly is 1000mm; The silicon single crystal lifting furnace with the diameter of round shape heating element is
400mm highly is 600mm.
Embodiment 2
(1) employing charcoal cloth and short carbon fiber net tire alternative stacked or alternately circumvolution round shape constitute the in-plane fiber, adopt needling process to introduce vertical fibers at thickness direction, make three way structure heating element precast body, and its density is 0.45g/cm
3
(2) acetone-furfural resin or resol vacuum-impregnating by pressure is solidified densified: earlier with 60 ℃ of acetone-furfural resin or resol preheatings, and the heating element precast body in the step (1) packed into vacuumize in the impregnating autoclave, vacuum tightness 600Pa, preheating temperature is 60 ℃, sucks acetone-furfural resin or resol, is to flood 4 hours under the 2.5MPa at pressure, after Vent presses, insert resin return tube inflated with nitrogen, pressure is to eject unnecessary resin under the 0.2Mpa, and dip treating finishes; Be cured processing again, pressure is 2.5Mpa, and temperature is 200 ℃;
(3) the normal pressure charing is handled: the charcoal/carbon/carbon heating body that will flood solidification treatment is packed in the charring furnace, and under nitrogen protection, its flow is that 900L/h carries out the charing processing, and carbonization temperature is 1000 ℃, makes charcoal/carbon/carbon heating body goods;
(4) charcoal/carbon/carbon heating body extrudate density＜1.55g/cm
3The time, repeating step (2), step (3); As its density 〉=1.55g/cm
3The time, densification technique finishes;
(5) lesser temps condition of high vacuum degree purification process: charcoal/carbon/carbon heating body goods are packed in the vacuum induction furnace, and temperature is 1700 ℃, and vacuum tightness is 20Pa, carries out lesser temps condition of high vacuum degree purification process;
(6) to charcoal/carbon/carbon heating body milling machine, machined into after the process purification process in the step (5), drilling machine boring promptly makes high resistance and high purity charcoal/carbon/carbon heating body, the U-shaped heating element that can be used for polysilicon hydrogenation furnace also can be used for the round shape heating element of silicon single crystal lifting furnace.
Charcoal cloth in the above-mentioned steps (1) is 12K plain weave charcoal cloth, and wherein K represents tow thousand radicals.
The purity of charcoal in the above-mentioned steps (5)/carbon/carbon heating body goods is ash content≤50ppm, and resistivity is 40 μ Ω/m, and resistance value is 0.14 Ω.
Polysilicon hydrogenation furnace in the above-mentioned steps (6) is 130mm with the width of U-shaped heating element, highly is 3000mm; The silicon single crystal lifting furnace with the diameter of round shape heating element is
1200mm highly is 1200mm.
Embodiment 3
(1) employing charcoal cloth and short carbon fiber net tire alternative stacked or alternately circumvolution round shape constitute the in-plane fiber, adopt needling process to introduce vertical fibers at thickness direction, make three way structure heating element precast body, and its density is 0.65g/cm
3
(2) acetone-furfural resin or resol vacuum-impregnating by pressure is solidified densified: earlier with 80 ℃ of acetone-furfural resin or resol preheatings, and the heating element precast body in the step (1) packed into vacuumize in the impregnating autoclave, vacuum tightness 1000Pa, preheating temperature is 80 ℃, sucks acetone-furfural resin or resol, is to flood 6 hours under the 4.0MPa at pressure, after Vent presses, insert resin return tube inflated with nitrogen, pressure is to eject unnecessary resin under the 0.2Mpa, and dip treating finishes; Be cured processing again, pressure is 4.0Mpa, and temperature is 230 ℃;
(3) the normal pressure charing is handled: the charcoal/carbon/carbon heating body that will flood solidification treatment is packed in the charring furnace, and under nitrogen protection, its flow is that 1200L/h carries out the charing processing, and carbonization temperature is 1200 ℃, makes charcoal/carbon/carbon heating body goods;
(4) charcoal/carbon/carbon heating body extrudate density＜1.55g/cm
3The time, repeating step (2), step (3); As its density 〉=1.55g/cm
3The time, densification technique finishes;
(5) lesser temps condition of high vacuum degree purification process: charcoal/carbon/carbon heating body goods are packed in the vacuum induction furnace, and temperature is 2000 ℃, and vacuum tightness is 40Pa, carries out lesser temps condition of high vacuum degree purification process;
(6) to charcoal/carbon/carbon heating body milling machine, machined into after the process purification process in the step (5), drilling machine boring promptly makes high resistance and high purity charcoal/carbon/carbon heating body, the U-shaped heating element that can be used for polysilicon hydrogenation furnace also can be used for the round shape heating element of silicon single crystal lifting furnace.
Charcoal cloth in the above-mentioned steps (1) is 24K plain weave charcoal cloth, and wherein K represents tow thousand radicals.
The purity of charcoal in the above-mentioned steps (5)/carbon/carbon heating body goods is ash content≤50ppm, and resistivity is 50 μ Ω/m, and resistance value is 0.2 Ω.
Polysilicon hydrogenation furnace in the above-mentioned steps (6) is 200mm with the width of U-shaped heating element, highly is 4000mm; The silicon single crystal lifting furnace with the diameter of round shape heating element is
2000mm highly is 2000mm.
Claims (9)
1, a kind of preparation method of high resistance and high purity charcoal/carbon/carbon heating body is characterized in that may further comprise the steps:
(1) employing charcoal cloth and short carbon fiber net tire alternative stacked or alternately circumvolution round shape constitute the in-plane fiber, adopt needling process to introduce vertical fibers at thickness direction, make three way structure heating element precast body, and its density is 0.25～0.65g/cm
3
(2) acetone-furfural resin or resol vacuum-impregnating by pressure solidifies densified: earlier with acetone-furfural resin or resol preheating, and the heating element precast body in the step (1) packed into vacuumize in the impregnating autoclave, preheating, suck acetone-furfural resin or resol, at pressure is to flood 2-6 hour under 1.0～4.0MPa, after Vent presses, inserts resin return tube inflated with nitrogen, pressure is to eject unnecessary resin under the 0.2Mpa, and dip treating finishes; Be cured processing again;
(3) the normal pressure charing is handled: the charcoal/carbon/carbon heating body precast body that will flood solidification treatment is packed in the charring furnace, carries out the charing processing under nitrogen protection, makes charcoal/carbon/carbon heating body goods;
(4) charcoal in step (3)/carbon/carbon heating body extrudate density＜1.55g/cm
3The time, repeating step (2), step (3); As its density 〉=1.55g/cm
3The time, densification technique finishes;
(5) lesser temps, condition of high vacuum degree purification process: the charcoal in the step (4)/carbon/carbon heating body goods are packed in the vacuum induction furnace, carry out purification process, temperature is 1400～2000 ℃, and vacuum tightness is 1-40Pa;
(6) to charcoal/carbon/carbon heating body milling machine, machined into after the process purification process in the step (5), drilling machine boring promptly makes high resistance and high purity charcoal/carbon/carbon heating body, and described high resistance is meant that resistance value is 0.08～0.2 Ω, and described high purity is meant ash content≤50ppm.
2, the preparation method of high resistance and high purity charcoal/carbon/carbon heating body according to claim 1 is characterized in that charcoal cloth described in the step (1) is 3～24K plain weave charcoal cloth, and wherein K represents tow thousand radicals.
3, the preparation method of high resistance and high purity charcoal/carbon/carbon heating body according to claim 1, it is characterized in that preheating temperature is 40～80 ℃ described in the step (2), the described vacuum tightness that vacuumizes is 200～1000Pa, and described solidification treatment temperature is 160～230 ℃, and pressure is 1.0～4.0Mpa.
4, the preparation method of high resistance and high purity charcoal/carbon/carbon heating body according to claim 1 is characterized in that nitrogen flow is 600～1200L/h described in the step (3), and described charing treatment temp is 850～1200 ℃.
5, the preparation method of high resistance and high purity charcoal/carbon/carbon heating body according to claim 1 is characterized in that the resistivity of the charcoal/carbon/carbon heating body goods of preparation in the step (5) is 30～50 μ Ω/m.
6, the preparation method of high resistance and high purity charcoal/carbon/carbon heating body according to claim 1 is characterized in that high resistance and high purity charcoal/carbon/carbon heating body described in the step (6) is the U-shaped heating element of polysilicon hydrogenation furnace.
7, the preparation method of high resistance and high purity charcoal/carbon/carbon heating body according to claim 1 is characterized in that high resistance and high purity charcoal/carbon/carbon heating body described in the step (6) is the round shape heating element of silicon single crystal lifting furnace.
8, the preparation method of high resistance and high purity charcoal/carbon/carbon heating body according to claim 6, the width that it is characterized in that described U-shaped heating element is 60～200mm, highly is 1000～4000mm.
9, the preparation method of high resistance and high purity charcoal/carbon/carbon heating body according to claim 7 is characterized in that the diameter of described round shape heating element is
Highly be 600～2000mm.
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| CN101541111B (en) * | 2009-04-22 | 2010-10-13 | 蒋建纯 | U-shaped heating element of silicon tetrachloride hydrogenation furnace and manufacturing process thereof |
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| CN101638321B (en) * | 2009-05-15 | 2012-06-06 | 西安超码科技有限公司 | Method for preparing carbon/carbon composite profiles |
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| CN104244475A (en) * | 2013-06-09 | 2014-12-24 | 浙江昱辉碳纤维材料有限公司 | Processing method of carbon fiber heating pad |
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| CN101541111B (en) * | 2009-04-22 | 2010-10-13 | 蒋建纯 | U-shaped heating element of silicon tetrachloride hydrogenation furnace and manufacturing process thereof |
| CN101638321B (en) * | 2009-05-15 | 2012-06-06 | 西安超码科技有限公司 | Method for preparing carbon/carbon composite profiles |
| CN101608983B (en) * | 2009-07-23 | 2011-05-18 | 攀钢集团钢铁钒钛股份有限公司 | Preparation method of chemical analysis sample of titanium product and titanium alloy and preparation device thereof |
| CN102167611A (en) * | 2011-01-27 | 2011-08-31 | 无锡市弟兆碳材料有限公司 | Method for preparing carbon/carbon composite material plate |
| 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 |
| CN104244475A (en) * | 2013-06-09 | 2014-12-24 | 浙江昱辉碳纤维材料有限公司 | Processing method of carbon fiber heating pad |
| CN104244475B (en) * | 2013-06-09 | 2016-04-20 | 嘉兴启晟碳材料有限公司 | Processing method of carbon fiber heating pad |
| CN103342574A (en) * | 2013-07-25 | 2013-10-09 | 华东理工大学 | Enhanced block carbon nanofiber (CNF)/carbon composite material and preparation method thereof |
| CN105712728A (en) * | 2014-12-04 | 2016-06-29 | 航天睿特碳材料有限公司 | Method for preparing carbon-carbon composite material thermal insulation cylinder from soft felt |
| CN105712729A (en) * | 2014-12-04 | 2016-06-29 | 航天睿特碳材料有限公司 | Preparation method for crucible cover plate for polycrystalline ingot furnace |
| CN113175565A (en) * | 2021-06-09 | 2021-07-27 | 湖南汇达新材料有限公司 | Thin-wall high-strength carbon-carbon composite material pipeline and preparation method thereof |
| CN114804906A (en) * | 2022-05-27 | 2022-07-29 | 陕西美兰德炭素有限责任公司 | High-purity carbon/carbon composite material and preparation method and application thereof |
| CN114804906B (en) * | 2022-05-27 | 2023-02-14 | 陕西美兰德炭素有限责任公司 | High-purity carbon/carbon composite material and preparation method and application thereof |
| CN115286414A (en) * | 2022-08-17 | 2022-11-04 | 陕西美兰德炭素有限责任公司 | Preparation method of carbon bottom heater for monocrystalline silicon drawing furnace |
| CN115286414B (en) * | 2022-08-17 | 2023-08-18 | 陕西美兰德新材料股份有限公司 | Preparation method of charcoal bottom heater for monocrystalline silicon drawing furnace |
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