CN103193495A - Production method of insulation materials used for crystal pulling furnace - Google Patents
Production method of insulation materials used for crystal pulling furnace Download PDFInfo
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- CN103193495A CN103193495A CN2013100648630A CN201310064863A CN103193495A CN 103193495 A CN103193495 A CN 103193495A CN 2013100648630 A CN2013100648630 A CN 2013100648630A CN 201310064863 A CN201310064863 A CN 201310064863A CN 103193495 A CN103193495 A CN 103193495A
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Abstract
The invention provides a production method of insulation materials used for a crystal pulling furnace. The method comprises: selecting carbonized or graphitized carbon fiber composite, immersing the carbon fiber composite or coating the surface of the carbon fiber composite for 1-3 times with organic composite resin, drying for later use; curing, coating a hole sealing agent on the surface of the carbon fiber composite, drying for later use; selecting carbonized or graphitized carbon fibrofelt, immersing the carbon fibrofelt or coating surfaces of the carbon fibrofelt with the organic composite resin, drying for later use; respectively coating an adhesive on surfaces of the treated carbon fiber composite and the carbon fibrofelt, winding and fitting the two materials, fixing by using a mold, curing; sending the product into a high temperature furnace for carbonization and graphitization, performing surface treatment, sending into a purifying furnace, purifying in inert gas and chlorine, and taking out to obtain the finish product. The method solves problems of difficultly controlled production technology and poor quality of finished products in prior art.
Description
Technical field
The present invention relates to the carbon-fiber heat-insulation material technical field, relate in particular to a kind of production method as the carbon-fiber heat-insulation material that uses in the stoves such as crystal growing furnace and crystal pulling apparatus, ceramic post sintering stove, vacuum high-temperature heat treatment furnace, further relate to a kind of crystal pulling furnace with the production method of lagging material.
Background technology
Carbon fiber is fibrous carbon material, have high specific strength, high ratio modulus, high temperature resistant, anti-ablation, antifatigue, creep resistance, conduction, heat conduction, a series of excellent properties such as density is low and thermal expansivity is little, be the most important strongthener of advanced configuration matrix material, having a wide range of applications aspect spaceship, aerospacecraft, satellite, military project and the high-grade sports goods.The key factor that influences carbon fiber and graphiteization is greying equipment and high-temperature heat treatment technology, and people utilize different hot industrial source to develop the greying that multiple graphitizing furnace carries out carbon fiber for this reason.Present domestic silicon single crystal polysilicon industry is in the ascendant, silicon single crystal and polycrystalline silicon furnace increase day by day with the lagging material demand, this lagging material mainly is carbon-fibre composite, domestic carbon fiber class heat-insulation and heat-preservation material development, production start to walk evening, product specification is low, kind is few, and most of kind is mainly used in heat treatment industry.The silicon single crystal of domestic use and polycrystalline silicon furnace use the heat-insulation and heat-preservation material mainly from external import.External supplier is German western Cree Inc. and Japanese Wu Yu company, the product carbon content height of these two companies, and ash content is little, and the resistance to compression bending strength is good, and heat preservation and insulation is good, but price is higher relatively, is unfavorable for saving cost.
Number of patent application is 200910043408.6 Chinese patent, it discloses a kind of technology is simple, thermal conductivity is little high temperature furnace-grade curing carbon fiber thermal insulating material and production technique thereof, it is characterized in that it is made through precast body preparation-density-Re purifying-machining of shaking by carbon fiber, processes such as it need not be bonding in precast body preparation, dipping, curing and charing, simple and the energy-conserving and environment-protective of its technology, the precast body internal carbon fibers is crisscross, cohesive force is stronger, can delamination, Stability Analysis of Structures, thermal conductivity≤0.8W/mK, excellent thermal insulation performance; Product is made of high-strength carbon fiber and carbon element matrix, have premium propertiess such as high specific strength, high temperature resistant, corrosion-resistant, good heat insulating, having fire-resistant, insulation dual nature concurrently, and can carry certain heavy burden, is the desirable upgrading products that substitute high temperature furnace used relevant graphite product and soft charcoal felt.But this method has following defective: the production technique journey is comparatively complicated, and the cycle is longer, and processing parameter is difficult for controlling, and raw material and intermediates are easily ablated in the production process, so final product quality is difficult to guarantee, and production cost is higher; This method gained finished product oxidation-resistance is relatively poor, and heat preservation and insulation is relatively poor, and the staple fibre of gained finished product easily comes off, and work-ing life is short etc.
Summary of the invention
The purpose of this invention is to provide a kind of crystal pulling furnace with the production method of lagging material, be difficult to control problems such as final product quality difference with production technique in the solution prior art.
The present invention is achieved by the following technical solutions: this crystal pulling furnace production method of lagging material, and its technical essential is may further comprise the steps:
(1) selects 900 ~ 2400 ℃ of carbonizations or graphited carbon-fibre composite; After carbon-fibre composite soaked 1 ~ 3h or brushing surface 1 ~ 3 time with organic compound resin, drying for standby; Behind 150 ~ 180 ℃ of curing 3 ~ 5h, the fibre composite surface applied hole sealing agent after curing, drying for standby;
(2) select 900 ~ 2400 ℃ of carbonizations or graphited carbon fiber felt; After carbon fiber felt soaked 1 ~ 3h or brushing surface 1 ~ 3 time with organic compound resin, drying for standby;
(3) carbon-fibre composite after the curing of coating hole sealing agent applies sizing agent respectively with the carbon fiber felt surface of handling, and two kinds of materials that apply sizing agent is twined fit together, and after fixing with mould, solidifies 3 ~ 10h at 150 ~ 180 ℃;
(4) product after will solidifying is sent into High Temperature Furnaces Heating Apparatus and is carried out carbonization, greying at 900 ~ 2400 ℃;
(5) paste graphite paper or carbon cloth at product surface spray coating coating or at product surface after the greying, send into purifying furnace after the surface treatment, in rare gas element, chlorine 2200 ℃ carry out purifying after, taking-up gets product;
The carbon-fibre composite of step (1) is selected from a kind of of polyacrylonitrile carbon fiber, viscose carbon fiber, asphalt-based carbon fiber, and the linear density of carbon-fibre composite is 0.111 ~ 0.666tex;
The hole sealing agent of step (1) is by the resol of 10 ~ 50wt%, the Resins, epoxy of 3 ~ 50wt%, the furane resin of 1 ~ 10wt%, the furfuryl resin of 1 ~ 10wt% and the solvent composition of surplus;
The carbon fiber felt of step (2) is selected from a kind of of pan based fibers felt, viscose base fibrefelt, pitch-based fiber felt, and fiber linear density is 0.111 ~ 0.666tex;
The sizing agent of step (3) is selected from a kind of of resol, furane resin, furfuryl resin, Resins, epoxy, and content is 10 ~ 70wt%;
The coating of step (5) is by the resol of 5 ~ 20wt%, the Resins, epoxy of 1 ~ 10wt%, and the furfuryl resin of 0 ~ 5wt%, the furane resin of 0 ~ 5wt%, the Graphite Powder 99 of 1 ~ 10wt%, balance solvent is formed;
Described solvent is selected from a kind of of methyl alcohol, ethanol, acetone, ethyl acetate, butylacetate;
Described organic compound resin is selected from a kind of of resol, furane resin, furfuryl resin, Resins, epoxy, and content is 5 ~ 30wt%.
The carbon fiber felt of described step (2) is selected from 900 ~ 2400 ℃ of carbonizations, graphited polyacrylonitrile-based carbon felt.
Beneficial effect of the present invention is as follows: in the production process product is carried out surface treatment, not only improved anti-airflow scouring performance and work-ing life but also can prevent the ablation of raw material and intermediates effectively, production process is safety and stability more, has reduced production cost; Adopt hole sealing agent, the coating of specific proportioning to guarantee the surface-treated effect; Select specified temp carbonization, graphited carbon-fibre composite and carbon fiber felt for use, further improved final product quality; Strict control temperature and time has shortened the production cycle in the production process; The technical process simple controllable; Lagging material carbon content, resistance to compression bending strength, thermal conductivity, thermal expansivity, the ash that uses the inventive method the to produce index of grading all is better than similar products at home and abroad, and production cost is low, the cost performance height can substitute similar imported product fully, has greatly market potential.
Below by example the present invention is described in further detail, but following example only is the present invention's example wherein that do not represent the rights protection scope that the present invention limits, the scope of the present invention is as the criterion with claims.
Embodiment
Example 1
A kind of crystal pulling furnace production method of lagging material, its production process is as follows:
(1) the polyacrylonitrile-radical short carbon fiber material (0.666tex) after the greying under 2400 ℃ of temperature of ∮ 360mm * ∮ 390mm * 115mm0 is soaked 3h, drying for standby with organic compound resin; Organic compound resin is selected from resol, furfuryl resin, furane resin, Resins, epoxy etc. a kind of, preferred resol (solvent is methyl alcohol);
Behind 150 ℃ of curing 3h, polyacrylonitrile-radical short carbon fiber material surface applied one deck hole sealing agent after curing, dry that standby (hole sealing agent is by the resol of 10 ~ 50wt%, the Resins, epoxy of 3 ~ 50wt%, the furane resin of 1 ~ 10wt%, the furfuryl resin of 1 ~ 10wt% and the methyl alcohol of surplus are formed).
(2) the polyacrylonitrile-radical graphite fibre felt (0.666tex) after 2400 ℃ of greyings is soaked 1 ~ 3h, drying for standby with organic compound resin.
It is a kind of of 20 ~ 30% resol, furfuryl resin, furane resin, Resins, epoxy that organic compound resin is selected from content, preferred resol.
(3) carbon-fibre composite after the curing of coating hole sealing agent applies resol respectively with the carbon fiber felt surface of handling, and two kinds of materials that apply sizing agent is twined fit together, after fixing with mould, at 150 ~ 180 ℃ of cure under pressure 5h.
(4) product after will solidifying is sent into High Temperature Furnaces Heating Apparatus carry out greying under 2400 ℃.
(5) after the greying at product surface spray coating Graphite Powder 99 or resol (solvent is methyl alcohol), send into purifying furnace after the surface treatment, in nitrogen, argon gas, chlorine 2400 ℃ carry out purifying after, take out and namely to get the finished product that is of a size of ∮ 360mm * ∮ 430mm * 1150mm.
(6) finished-product material behind the purifying is machined into the used thermal insulation material of crystal pulling furnace according to the drawing needs.
Example 2
(1) graphited viscose base short carbon fiber material (0.244tex) under 2400 ℃ of temperature of ∮ 45mm0 * ∮ 350mm * 500mm is soaked 2h, drying for standby in furfuryl resin (solvent is ethanol); Behind 150 ℃ of processing 3h, at short carbon fiber material surface applied one deck resol, dry standby.
(2) with 2400 ℃ of graphited viscose foundation stone China ink fibrefelts, in furfuryl resin (solvent is ethanol), soak 2h, dry standby.
(3) the surperficial and graphite felt surface applied resol at the viscose base short carbon fiber material of coating resol; Two kinds of materials windings that were coated with sizing agent are fit together, after fixing with mould, cure under pressure 5h under 150 ~ 180 ℃ of temperature.
(4) product after will solidifying is sent into High Temperature Furnaces Heating Apparatus and is carried out greying at 2400 ℃.
(5) after the greying at product surface spray coating Graphite Powder 99 or resol (solvent is methyl alcohol), send into purifying furnace after the surface treatment, in nitrogen, argon gas, chlorine 2200 ℃ carry out purifying after, take out and namely to get the finished product that is of a size of ∮ 530mm * ∮ 350mm * 500mm.
(6) finished-product material behind the purifying is machined into the used thermal insulation material of crystal pulling furnace according to the drawing needs.
Example 3
Carbon-fibre composite is selected from that polyacrylonitrile-radical short carbon fiber material (0.666tex) course of processing after the carbonized graphiteization is with example 1 under 2400 ℃ of temperature of ∮ 400mm * ∮ 380mm * 730mm, and final dimension is ∮ 480mm * ∮ 380mm * 730mm.
Example 4
Carbon-fibre composite is selected from that polyacrylonitrile-radical short carbon fiber material (0.666tex) course of processing after the carbonized graphiteization is with example 1 under 2400 ℃ of temperature of ∮ 440mm * ∮ 520mm * 1000mm, and final dimension is ∮ 440mm * ∮ 620mm * 1000mm.
Example 5
Carbon-fibre composite is selected from that polyacrylonitrile-radical short carbon fiber material (0.666tex) course of processing after the carbonized graphiteization is with example 1 under 2400 ℃ of temperature of ∮ 700mm * 30mm, and final dimension is ∮ 700mm * 50mm.
Example 6
Carbon-fibre composite is selected from that polyacrylonitrile-radical short carbon fiber material (0.666tex) course of processing after the carbonized graphiteization is with example 1 under 2400 ℃ of temperature of ∮ 720mm * 10mm, and final dimension is ∮ 720mm * 20mm.
Example 7
Carbon-fibre composite is selected from that polyacrylonitrile-radical short carbon fiber material (0.666tex) course of processing after the carbonized graphiteization is with example 1 under 2400 ℃ of temperature of ∮ 830mm * 20mm, and final dimension is ∮ 830mm * 60mm.
Carbon-fibre composite, carbon fiber felt are available from the outstanding carbon materials of Shanghai black horse company limited, Shenyang cartel non-woven company limited, Fushun City Tianyuan technical cloth company limited, Liaoyuan City China foreign non-woven fabrics company limited.
The lagging material that embodiment 1 ~ 7 produces compared with prior art has better thermal conductivity.Described carbonization in the present invention refers to that the pyroprocessing temperature is the product below 1600 ℃; Greying refers to that the pyroprocessing temperature is the product more than 1600 ℃.
Above-mentioned example 1 ~ 7 gained finished product parameter is as shown in the table:
Claims (2)
1. the production method of a crystal pulling furnace usefulness lagging material is characterized in that, may further comprise the steps:
(1) selects 900 ~ 2400 ℃ of carbonizations or graphited carbon-fibre composite; After carbon-fibre composite soaked 1 ~ 3h or brushing surface 1 ~ 3 time with organic compound resin, drying for standby; Behind 150 ~ 180 ℃ of curing 3 ~ 5h, the fibre composite surface applied hole sealing agent after curing, drying for standby;
(2) select 900 ~ 2400 ℃ of carbonizations or graphited carbon fiber felt; After carbon fiber felt soaked 1 ~ 3h or brushing surface 1 ~ 3 time with organic compound resin, drying for standby;
(3) carbon-fibre composite after the curing of coating hole sealing agent applies sizing agent respectively with the carbon fiber felt surface of handling, and two kinds of materials that apply sizing agent is twined fit together, and after fixing with mould, solidifies 3 ~ 10h at 150 ~ 180 ℃;
(4) product after will solidifying is sent into High Temperature Furnaces Heating Apparatus and is carried out carbonization, greying at 900 ~ 2400 ℃;
(5) the product surface spray coating coating after carbonization, greying, paste graphite paper or carbon cloth, send into purifying furnace after the surface treatment, in rare gas element, chlorine 2200 ℃ carry out purifying after, taking-up gets product;
The carbon-fibre composite of step (1) is selected from a kind of of polyacrylonitrile carbon fiber, viscose carbon fiber, asphalt-based carbon fiber, and the linear density of carbon-fibre composite is 0.111 ~ 0.666tex;
The hole sealing agent of step (1) is by the resol of 10 ~ 50wt%, the Resins, epoxy of 3 ~ 50wt%, the furane resin of 1 ~ 10wt%, the furfuryl resin of 1 ~ 10wt% and the solvent composition of surplus;
The carbon fiber felt of step (2) is selected from a kind of of pan based fibers felt, viscose base fibrefelt or pitch-based fiber felt, and fiber linear density is 0.111 ~ 0.666tex;
The sizing agent of step (3) is selected from a kind of of resol, furane resin, furfuryl resin or Resins, epoxy, and content is 10 ~ 70wt%;
The coating of step (5) is by the resol of 5 ~ 20wt%, the Resins, epoxy of 1 ~ 10wt%, and the furfuryl resin of 0 ~ 5wt%, the furane resin of 0 ~ 5wt%, the Graphite Powder 99 of 1 ~ 10wt%, balance solvent is formed;
Described solvent is selected from a kind of of methyl alcohol, ethanol, acetone, ethyl acetate or butylacetate;
Described organic compound resin is selected from a kind of of resol, furane resin, furfuryl resin or Resins, epoxy, and content is 5 ~ 30wt%.
2. method according to claim 1, it is characterized in that: the carbon fiber felt of described step (2) is selected from 900 ~ 2400 ℃ of carbonizations, graphited polyacrylonitrile-based carbon felt.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103642170A (en) * | 2013-11-25 | 2014-03-19 | 宜兴市飞舟高新科技材料有限公司 | Preparation method for carbon fiber composite material |
| CN104339730A (en) * | 2013-08-01 | 2015-02-11 | 甘肃郝氏炭纤维有限公司 | Sandwich cured carbon felt |
| CN105113001A (en) * | 2015-09-30 | 2015-12-02 | 吉林联科特种石墨材料有限公司 | Optimized preparation method of carbon-felt integrally-formed monocrystalline silicon growth furnace guide cylinder |
| CN106553429A (en) * | 2016-11-08 | 2017-04-05 | 扬州东润新材料科技有限公司 | The method of uniform rapid link between a kind of Carbon fiber thermal insulation hard carpet veneer |
| CN111409321A (en) * | 2020-03-31 | 2020-07-14 | 山东众途复合材料有限公司 | Preparation method of carbon fiber hard felt with density gradient |
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| CN101070250A (en) * | 2007-03-19 | 2007-11-14 | 华东理工大学 | Integrated nano carbon-fiber composite porous materila and preparing method |
| CN101613982A (en) * | 2008-06-27 | 2009-12-30 | 北京化工大学 | A kind of preparation method of carbon fiber paper for gas diffusion layer of fuel cell |
| CN102936148A (en) * | 2012-12-05 | 2013-02-20 | 湖南博云新材料股份有限公司 | Preparation method of carbon/carbon composite material for high-temperature furnace |
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2013
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Patent Citations (4)
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| CN1358162A (en) * | 1999-05-26 | 2002-07-10 | 吴羽化学工业株式会社 | Composite carbonaceous heat insualtor and its prepn. |
| CN101070250A (en) * | 2007-03-19 | 2007-11-14 | 华东理工大学 | Integrated nano carbon-fiber composite porous materila and preparing method |
| CN101613982A (en) * | 2008-06-27 | 2009-12-30 | 北京化工大学 | A kind of preparation method of carbon fiber paper for gas diffusion layer of fuel cell |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104339730A (en) * | 2013-08-01 | 2015-02-11 | 甘肃郝氏炭纤维有限公司 | Sandwich cured carbon felt |
| CN103642170A (en) * | 2013-11-25 | 2014-03-19 | 宜兴市飞舟高新科技材料有限公司 | Preparation method for carbon fiber composite material |
| CN105113001A (en) * | 2015-09-30 | 2015-12-02 | 吉林联科特种石墨材料有限公司 | Optimized preparation method of carbon-felt integrally-formed monocrystalline silicon growth furnace guide cylinder |
| CN106553429A (en) * | 2016-11-08 | 2017-04-05 | 扬州东润新材料科技有限公司 | The method of uniform rapid link between a kind of Carbon fiber thermal insulation hard carpet veneer |
| CN106553429B (en) * | 2016-11-08 | 2018-10-12 | 扬州东润新材料科技有限公司 | A kind of uniform method of rapid link between the hard carpet veneer of Carbon fiber thermal insulation |
| CN111409321A (en) * | 2020-03-31 | 2020-07-14 | 山东众途复合材料有限公司 | Preparation method of carbon fiber hard felt with density gradient |
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Application publication date: 20130710 |