CN103755375B - Binding agent used for carbon materials in high-temperature furnace and application method - Google Patents
Binding agent used for carbon materials in high-temperature furnace and application method Download PDFInfo
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- CN103755375B CN103755375B CN201410051014.6A CN201410051014A CN103755375B CN 103755375 B CN103755375 B CN 103755375B CN 201410051014 A CN201410051014 A CN 201410051014A CN 103755375 B CN103755375 B CN 103755375B
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Abstract
The invention provides a binding agent used for carbon materials in a high-temperature furnace and an application method. A preparation method of the binding agent comprises a step of evenly mixing carbonized materials, a dispersing agent, short or milled carbon fibers, short or milled graphite powder, silicon carbide powder and silica powder according to a certain proportion, so as to obtain the binding agent. The binding agent is particularly suitable for binding and surface treating of carbon fiber heat insulating materials in a polycrystalline silicon ingot casting funace, a single crystal silicon stretching furnace, a ceramic sintering furnace, a high temperature heat treatment furnace and other high-temperature furnaces. The binding agent is adopted to paste graphite paper or carbon cloth on a rigid carbon fiber heat insulation material; then curing treatment and carbonation treatment are performed to obtain the rigid carbon fiber heat insulating material pasted with graphite paper or carbon cloth; as the binding agent can prevent permeation of gas in furnaces and solves the problem of loss caused by reaction resulting from direct contact between the gas and the carbon fibers; the airflow washing resistance and certain oxidation resistance can be achieved; the service life of rigid carbon fiber heat insulating materials at a high-temperature environment is effectively prolonged; the energy-saving and cost-reducing effects are achieved; the production efficiency is improved; a great amount of cost is lowered for enterprises.
Description
Technical field
The present invention relates to carbon fiber thermal insulating material technical field, relate generally to making and the using method of the bonding binding agent of carbon material in High Temperature Furnaces Heating Apparatus, particularly as stickup and the surface treatment binding agent of carbon fiber thermal insulating material in the High Temperature Furnaces Heating Apparatuss such as polycrystalline silicon ingot casting, silicon single crystal stretching, ceramic sintering furnace, high temperature heat treatment furnace.
Background technology
Along with the progress of science and technology, there is great demand in the fields such as photovoltaic solar, military affairs, national defence and scientific research to crystalline silicon, rare metal and magneticsubstance.And the production of these materials all has direct or indirect relation with High Temperature Furnaces Heating Apparatus, vacuum oven.In addition, in industrial technical field, workpiece or raw-material pyroprocessing are all completed in vacuum high temperature furnace or inert atmosphere furnace.High temperature in-furnace temperature is general all more than 1350 DEG C, this just proposes very harsh requirement to lagging material---not only required high insulating effect to save the energy but also require high temperature resistant pollution-free, the life-span is long, carbon fiber thermal insulating material is due to its superior insulative properties, lower volume, low volatile, high strength and become the preferred material of soak.
Carbon fiber thermal insulating material is in rare gas element or vacuum, and the thermotolerance high due to it and extremely low vapour pressure, even can use under the ultrahigh-temperature of about 3000 DEG C.But, in practical service environment, consume due to the metallic impurity reaction of the oxidizing gas in stove or gasification, efflorescence, embrittlement and sex change.Such as, in polycrystalline silicon ingot or purifying furnace, the SiO produced in carbon fiber thermal insulating material and ingot furnace, metal impurities gas reaction, the constantly consumption of carbon fiber thermal insulating material surface, efflorescence, embrittlement, more seriously foreign gas penetrates into the inner sex change with its reaction of lagging material, carbon fiber thermal insulating material is made to lose heat-insulating property, life-span reduces greatly, and the dust produced after lagging material efflorescence disperses in stove, polluted product workpiece, cause product foreign matter content to increase, have a strong impact on quality product.
In order to solve the problem, the practice usual at present pastes graphite paper at heat insulation material surface, and prevent surface from consuming, this just needs adhibit quality good, the high temperature resistant and binding agent of good endurance.
Summary of the invention
The invention provides a kind of high-temperature agglomerant and the using method thereof that are applicable to high-density rigid carbon-fiber lagging material, adopt the rigid carbon-fiber lagging material of adhesive treatment of the present invention, because it can prevent from furnace gas from permeating and completely cut off gas directly contacting with carbon fiber and reacting and cause loss, make it have anti-airflow scouring and certain oxidation-resistance, greatly can improve the life-span of rigid carbon-fiber lagging material.And the graphite paper using this binding agent to paste/carbon cloth Reusability there will not be, and graphite paper/carbon cloth comes off, peeling.
In order to achieve the above object, the present invention realizes by the following technical solutions:
Carbon material binding agent in a kind of High Temperature Furnaces Heating Apparatus, by can char-forming material, dispersion agent, shortly to cut or ground carbon fiber, Graphite Powder 99, carborundum powder, silica flour are mixed in proportion to stir and make, the weight ratio of each component is: can char-forming material 40-100 part, dispersion agent 40-160 part, short cut or ground carbon fiber 5-20 part, Graphite Powder 99 25-50 part, carborundum powder 10-30 part, silica flour 5-20 part;
Described can char-forming material be one, two or more combination of resol, epoxy resin, furane resin, urea-formaldehyde resin, vinyl ester resin, polymeric amide, acrylic resin, polyethylene, polypropylene, ethylene propylene copolymer, polystyrene, pitch or tar;
Described dispersion agent is one in methyl alcohol, ethanol, propyl alcohol, ethylene glycol, propylene glycol, furfuryl alcohol, furfural, acetone, benzene or toluene, two or more combination;
Described shortly to cut or ground carbon fiber is one, two or more combination of asphalt base carbon fiber, viscose-based carbon fiber or polypropylene cyano group carbon fiber; Describedly shortly to cut or ground carbon fiber mean length is 10-1200 μm, more preferably mean length is 50-400 μm;
Described Graphite Powder 99 is natural flake graphite; Described Graphite Powder 99 granularity is 10-600 μm, and more preferably granularity is 30-300 μm;
Described carborundum powder granularity is 200-1000 order, and more preferably granularity is at 300-800 order;
Described silicon particle size is 200-1000 order, and more preferably granularity is at 300-800 order.
In described High Temperature Furnaces Heating Apparatus, the using method of carbon material binding agent, comprises the steps:
(1) carry out cut edge, Xiu Jiao, planing surface and machine to rigid carbon-fiber lagging material and add process, make goods reach surfacing, the chip purging surface makes surface without tiny carbon fiber; Then carry out cleaning and skimming treatment with dehydrated alcohol, then dry for standby at 110 ~ 130 DEG C in an oven;
(2) graphite paper or carbon cloth is cut according to the graphite paper used or carbon cloth size; Graphite paper thickness is 0.1-5mm;
(3) on the rigid carbon-fiber lagging material of drying and graphite paper or carbon cloth, brush described binding agent 1 ~ 4 time, its brushing method is: after front initial adhesion agent of once brushing is dried, then after brush once; After the rigid carbon-fiber lagging material of having brushed and graphite paper or carbon cloth dry, they are fit together, and bubble is discharged in roll extrusion, then uses clamp; Described consumption of binder is according to 150-1300g/m
2.
(4) solidify, the rigid carbon-fiber lagging material of upper fixture and graphite paper or carbon cloth are put into baking oven, makes binding agent at 150 ~ 350 DEG C of solidification 1 ~ 5.5h, be formed with the solidifying product of certain bonding strength;
(5) carbonization, puts into carbonizing treatment 1-6h under the rare gas element of 1000 DEG C-1800 DEG C or vacuum atmosphere, can obtain the rigid carbon-fiber lagging material that graphite paper or carbon cloth are pasted in surface by solidifying product.
More preferably: as stated above, rigid carbon-fiber lagging material is first pasted one or more layers carbon cloth and pastes graphite paper again, effect is better.
Advantage of the present invention according to requirements rigid carbon-fiber lagging material is carried out to the stickup of graphite paper/carbon cloth, prevent from furnace gas from permeating and completely cut off gas directly contacting with carbon fiber and reacting and cause loss, anti-airflow scouring, there is certain oxidation-resistance, effectively extend carbon fiber thermal insulating material work-ing life in high temperature environments, energy-saving and cost-reducing, improve production efficiency, for enterprise can save great amount of cost.And the graphite paper using this binding agent to paste/carbon cloth Reusability there will not be, and graphite paper/carbon cloth comes off, peeling.
Embodiment
Below by embodiment, the method for preparation and use of carbon material binding agent of the present invention and example are described in further detail.
Carbon material binding agent in High Temperature Furnaces Heating Apparatus, by can the material of carbonization, dispersion agent, shortly to cut or ground carbon fiber, Graphite Powder 99, carborundum powder and silica flour mix and obtain, as described below:
(1) can char-forming material, as one, two or more combination of resol, epoxy resin, furane resin, urea-formaldehyde resin, vinyl ester resin, polymeric amide, acrylic resin, polyethylene, polypropylene, ethylene propylene copolymer, polystyrene, pitch, tar;
(2) dispersion agent as methyl alcohol, ethanol, propyl alcohol, ethylene glycol, propylene glycol, furfuryl alcohol, furfural, acetone, benzene, toluene one, two or more combination;
(3) carbon fiber, as one, two or more combination of asphalt base carbon fiber, viscose-based carbon fiber, polypropylene cyano group carbon fiber, carbon fiber mean length is 10-1200 μm, and more preferably mean length is 50-400 μm.
(4) crystalline graphite powder, particle diameter is 10-600 μm, and more preferably particle diameter is at 30-300 μm.
(5) carborundum powder, granularity is 200-1000 order, and more preferably granularity is at 300-800 order.
(6) silica flour, granularity is 200-1000 order, and more preferably granularity is at 300-800 order.
The ratio mixing by weight of the above raw material of carbon material binding agent is obtained, 40-100 part can char-forming material, 40-160 part dispersion agent, 5-20 part is short cuts or ground carbon fiber, 25-50 part crystalline flake graphite, 10-30 part carborundum powder and 5-20 part silica flour, mixed according to the above ratio, can be obtained carbon material binding agent.Above raw material all can obtain from commercially available prod.
Then above-mentioned binding agent is used to paste graphite paper/carbon cloth to rigid carbon-fiber heat insulation material surface, graphite paper thickness is generally at 0.1-5mm, more preferably graphite paper thickness is at 0.2-1.5mm, more preferably graphite paper thickness is at 0.2-1.0mm, solidify the rigid carbon-fiber lagging material that carbonizing treatment obtains surperficial subsides graphite paper/carbon cloth again, because it can prevent from furnace gas from permeating and completely cut off gas directly contacting with carbon fiber and reacting and cause loss, make it have anti-airflow scouring and certain oxidation-resistance, greatly can improve the life-span of rigid carbon-fiber lagging material.
The concrete steps of pasting the rigid carbon-fiber lagging material of graphite paper/carbon cloth are as follows:
(1) prepared by carbon material binding agent: prepare described binding agent by above-mentioned raw materials and parts by weight of component, for subsequent use.
(2) carry out the process such as cut edge, Xiu Jiao, planing surface and machine add to rigid carbon-fiber lagging material, make goods reach surfacing, the chip purging surface makes surface without tiny carbon fiber, and rigid carbon-fiber lagging material density is 0.1 ~ 0.4g/cm
3; Then washes of absolute alcohol and skimming treatment is used, then dry for standby at 110 ~ 130 DEG C in an oven.
(3) according to the graphite paper used/carbon cloth size cutting graphite paper/carbon cloth.Graphite paper thickness is generally at 0.1-5mm, and more preferably graphite paper thickness is at 0.2-1.5mm, and more preferably graphite paper thickness is at 0.2-1.0mm.
(4) brush binding agent 1 ~ 4 time on the rigid carbon-fiber lagging material of drying and graphite paper/carbon cloth, its brushing method is: after front initial sizing agent of once brushing dries, then after brush once; After the sample of having brushed dries, they are bonded together, and bubble is discharged in roll extrusion, then uses clamp.Consumption of binder is according to 150-1300g/m
2, more preferably 230-900g/m
2.
(5) solidify, the rigid carbon-fiber lagging material of upper fixture and graphite paper or carbon cloth are put into baking oven, makes binding agent at 150 ~ 350 DEG C of solidification 1 ~ 5.5h, be formed with the solidifying product of certain bonding strength.
(6) carbonization, puts into carbonizing treatment 1-6h under the rare gas element of 1000 DEG C-1800 DEG C or vacuum atmosphere, can obtain the rigid carbon-fiber lagging material that graphite paper/carbon cloth is pasted on surface by solidifying product.
More preferably: as stated above, rigid carbon-fiber lagging material is first pasted one or more layers carbon cloth and pastes graphite paper again, effect is better.Concrete using method is described below:
The using method of carbon material binding agent in described High Temperature Furnaces Heating Apparatus, comprises the steps (describing to paste one deck carbon cloth and graphite paper):
(1) be 0.1 ~ 0.4g/cm to density
3rigid carbon-fiber lagging material carry out cut edge, Xiu Jiao, planing surface and machine and add process, make goods reach surfacing, the chip purging surface makes surface without tiny carbon fiber; Then carry out cleaning and skimming treatment with dehydrated alcohol, then dry for standby at 110 ~ 130 DEG C in an oven;
(2) according to the graphite paper used, carbon cloth size cutting graphite paper or carbon cloth; Graphite paper thickness is 0.1-5mm, and more preferably graphite paper thickness is at 0.2-1.5mm, and more preferably graphite paper thickness is at 0.2-1.0mm;
(3) at the rigid carbon-fiber lagging material of drying and graphite paper, carbon cloth brushes described binding agent 1 ~ 4 time, its brushing method is: after front initial adhesion agent of once brushing is dried, then after brush once; After the rigid carbon-fiber lagging material of having brushed and graphite paper, carbon cloth dry, rigid carbon-fiber lagging material, carbon cloth, graphite paper are fit together, and bubble is discharged in roll extrusion, then uses clamp; Described consumption of binder is according to 150-1300g/m
2, more preferably 230-900g/m
2.
(4) solidify, the rigid carbon-fiber lagging material of upper fixture is put into baking oven, make binding agent at 150 ~ 350 DEG C of solidification 1 ~ 5.5h, be formed with the solidifying product of certain bonding strength;
(5) carbonization, puts into carbonizing treatment 1-6h under the rare gas element of 1000 DEG C-1800 DEG C or vacuum atmosphere, can obtain the rigid carbon-fiber lagging material that carbon cloth and graphite paper are pasted in surface by solidifying product.
Example 1
(1) isotropic asphalt base carbon fiber production inflexibility carbon fiber thermal insulating material is adopted, density 0.16g/cm
3, machine is carried out to lagging material and adds, make its surfacing and it is purged, then use washes of absolute alcohol surface, then it is for subsequent use to dry 2h in an oven at 110 ~ 130 DEG C.
(2) each components by weight of binding agent is resol: ethanol: asphalt base carbon fiber: Graphite Powder 99: carborundum powder: silica flour=55:45:10:25:10:10, mixes obtained carbon material binding agent.
(3) according to the graphite paper that demand size cutting 0.5mm is thick, by the even scrubbing brush of carbon material binding agent brush on rigid carbon-fiber lagging material and graphite paper, according to 500g/m
2, then adhered on rigid carbon-fiber heat insulation material surface by graphite paper, roll extrusion has prevented bubble, then with clamp 200 DEG C of solidification 2h in baking oven.
(4) carbonization, carbonization 2h in the vacuum oven of 1800 DEG C, obtains the rigid carbon-fiber lagging material that graphite paper is pasted on surface.
Above-mentioned rigid carbon-fiber lagging material is used in polycrystalline silicon ingot or purifying furnace, use 4320h, heat insulation material surface is still better, there is not the phenomenons such as surface consumption, dry linting, embrittlement, graphite paper come off, and Ingot quality is higher and more stable, substantially increase the work-ing life of lagging material.
Example 2
(1) isotropic asphalt base carbon fiber production inflexibility carbon fiber thermal insulating material is adopted, density 0.18g/cm
3, machine is carried out to lagging material and adds, make its surfacing and it is purged, then use washes of absolute alcohol surface, then it is for subsequent use to dry 2h in an oven at 110 ~ 130 DEG C.
(2) each components by weight of binding agent is resol: ethanol: asphalt base carbon fiber: Graphite Powder 99: carborundum powder: silica flour=60:40:8:28:8:6, mixes obtained carbon material binding agent.
(3) according to the thick graphite paper of demand size cutting 0.5mm and carbon cloth, by the even scrubbing brush of carbon material binding agent brush on rigid carbon-fiber lagging material and carbon cloth, according to 480g/m
2, then adhered on rigid carbon-fiber heat insulation material surface by carbon cloth, roll extrusion has prevented bubble; Brush coating on carbon cloth and graphite paper again, according to 400g/m
2, then adhere on carbon cloth by graphite paper, roll extrusion has prevented bubble, then puts into 200 DEG C, baking oven solidification 2h by clamp.
(4) carbonization, carbonization 2h in the inert atmosphere furnace of 1200 DEG C, obtains the rigid carbon-fiber lagging material that one deck carbon cloth graphite paper is pasted on surface.
Above-mentioned rigid carbon-fiber lagging material is used in quenching furnance, use 7200h, heat insulation material surface is still better, its anti-airflow scouring better performances, there is not the phenomenons such as surface consumption, dry linting, embrittlement, carbon cloth graphite paper come off, and the quality product of producing is higher, does not occur the phenomenons such as workpiece contamination, substantially increases the work-ing life of lagging material.
Specific examples described in this specification sheets just illustrates the technical scheme of this patent but not the restriction to this patent.Based on other technical scheme of inventive concept, all within rights protection scope of the present invention.
Claims (3)
1. carbon material binding agent in a High Temperature Furnaces Heating Apparatus, it is characterized in that, by can char-forming material, dispersion agent, shortly to cut or ground carbon fiber, Graphite Powder 99, carborundum powder, silica flour are mixed in proportion to stir and make, the weight ratio of each component is: can char-forming material 40-100 part, dispersion agent 40-160 part, short cut or ground carbon fiber 5-20 part, Graphite Powder 99 25-50 part, carborundum powder 10-30 part, silica flour 5-20 part;
Described can char-forming material be one, two or more combination of resol, epoxy resin, furane resin, urea-formaldehyde resin, vinyl ester resin, polymeric amide, acrylic resin, polyethylene, polypropylene, ethylene propylene copolymer, polystyrene, pitch or tar;
Described dispersion agent is one in methyl alcohol, ethanol, propyl alcohol, ethylene glycol, propylene glycol, furfuryl alcohol, furfural, acetone, benzene or toluene, two or more combination;
Described shortly to cut or ground carbon fiber is one, two or more combination of asphalt base carbon fiber, viscose-based carbon fiber or polypropylene cyano group carbon fiber; Describedly shortly to cut or ground carbon fiber mean length is 10-1200 μm;
Described Graphite Powder 99 is natural flake graphite; Described Graphite Powder 99 granularity is 10-600 μm;
Described carborundum powder granularity is 200-1000 order;
Described silicon particle size is 200-1000 order.
2. the using method of carbon material binding agent in High Temperature Furnaces Heating Apparatus according to claim 1, is characterized in that, comprise the steps:
(1) carry out cut edge, Xiu Jiao, planing surface and machine to rigid carbon-fiber lagging material and add process, make goods reach surfacing, the chip purging surface makes surface without tiny carbon fiber; Then carry out cleaning and skimming treatment with dehydrated alcohol, then dry for standby at 110 ~ 130 DEG C in an oven;
(2) graphite paper or carbon cloth is cut according to the graphite paper used or carbon cloth size; Graphite paper thickness is 0.1-5mm;
(3) on the rigid carbon-fiber lagging material of drying and graphite paper or carbon cloth, brush described binding agent 1 ~ 4 time, its brushing method is: after front initial adhesion agent of once brushing is dried, then after brush once; After the rigid carbon-fiber lagging material of having brushed and graphite paper or carbon cloth dry, they are fit together, and bubble is discharged in roll extrusion, then uses clamp; Described consumption of binder is according to 150-1300g/m
2;
(4) solidify, the rigid carbon-fiber lagging material of upper fixture and graphite paper or carbon cloth are put into baking oven, makes binding agent at 150 ~ 350 DEG C of solidification 1 ~ 5.5h, be formed with the solidifying product of certain bonding strength;
(5) carbonization, puts into carbonizing treatment 1-6h under the rare gas element of 1000 DEG C-1800 DEG C or vacuum atmosphere, can obtain the rigid carbon-fiber lagging material that graphite paper or carbon cloth are pasted in surface by solidifying product.
3. the using method of carbon material binding agent in High Temperature Furnaces Heating Apparatus according to claim 2, is characterized in that, by described method, rigid carbon-fiber lagging material is first pasted one or more layers carbon cloth and pastes graphite paper again.
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| CN104261853B (en) * | 2014-09-26 | 2016-01-20 | 辽宁奥亿达新材料有限公司 | Asphalt base carbon fiber non-woven mat heat-preservation cylinder and manufacture method thereof |
| CN108218460A (en) * | 2018-01-24 | 2018-06-29 | 航天睿特碳材料有限公司 | A kind of middle low-density surface of carbon/carbon composite Enhancement Method |
| CN108558268A (en) * | 2018-06-22 | 2018-09-21 | 西南石油大学 | A kind of fibre reinforced high temperature resistant adhesive and preparation method thereof |
| CN114804926B (en) * | 2022-04-27 | 2023-10-24 | 辽宁金谷炭材料股份有限公司 | Repairing method of composite heat-insulating material |
| CN115368146B (en) * | 2022-10-24 | 2023-02-21 | 山东红点新材料有限公司 | Non-asphalt-based adhesive for producing carbon products and preparation method thereof |
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| CN101591178A (en) * | 2008-05-30 | 2009-12-02 | 鞍山塞诺达碳纤维有限公司 | The manufacturing of rigid carbon-fiber heat-insulation material and surface treatment method |
| CN101671194A (en) * | 2009-09-23 | 2010-03-17 | 北京航空航天大学 | Preparation method of high temperature adhesive used for carbon-based composite material |
| CN101949481A (en) * | 2010-09-17 | 2011-01-19 | 西安超码科技有限公司 | Method for preparing wound heat-insulating drum |
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| CN101591178A (en) * | 2008-05-30 | 2009-12-02 | 鞍山塞诺达碳纤维有限公司 | The manufacturing of rigid carbon-fiber heat-insulation material and surface treatment method |
| CN101671194A (en) * | 2009-09-23 | 2010-03-17 | 北京航空航天大学 | Preparation method of high temperature adhesive used for carbon-based composite material |
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