CN104230368A - Pitch-based carbon fiber nonwoven felt insulation board and manufacturing method thereof - Google Patents

Pitch-based carbon fiber nonwoven felt insulation board and manufacturing method thereof Download PDF

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CN104230368A
CN104230368A CN201410512417.6A CN201410512417A CN104230368A CN 104230368 A CN104230368 A CN 104230368A CN 201410512417 A CN201410512417 A CN 201410512417A CN 104230368 A CN104230368 A CN 104230368A
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carbon fiber
woven mat
asphalt base
fiber non
base carbon
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CN104230368B (en
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郑淑云
陈惠龙
朴成军
王红伟
张作桢
李里
崔欣
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Liaoning Aoyida New Materials Co ltd
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LIAONING AOYIDA ADVANCED MATERIAL Co Ltd
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Abstract

The invention relates to a pitch-based carbon fiber nonwoven felt insulation board and a manufacturing method of the pitch-based carbon fiber nonwoven felt insulation board. The pitch-based carbon fiber nonwoven felt insulation board comprises a pitch-based carbon fiber nonwoven felt insulation board main body which is a plate obtained by cutting, laminating, forming, curing, carbonizing/graphitizing pitch-based carbon fiber nonwoven felt after being mixed with a mixed liquid of an organic binder and a solvent, and the pitch-based carbon fiber nonwoven felt is obtained by carrying out spinning, preoxidation and carbonization on pitch. Carbon material binder layers and graphite paper/carbon fiber sheets are in sequence arranged on the main body and the lower surfaces of the pitch-based carbon fiber nonwoven felt insulation board from inside to outside, and a finished product is cured and carbonized. Compared with the prior art, the invention has the benefits that (1) thermal insulation and heat insulation properties are good; (2) the density is 0.1-0.4 g/cm<3>, the strength is high and the self-supporting property is good, (3) oxidation and air flow scouring are resisted because surface treatment is carried out to facilitate a long service life; (4) the process is simple, the production cost is low, the thickness can be decided once, and the product is not easy to crack and good in stability.

Description

Asphalt base carbon fiber non-woven mat warming plate and manufacture method thereof
Technical field
The present invention relates to heat-insulating heat-preserving material technical field, particularly relate to the asphalt base carbon fiber non-woven mat warming plate and manufacture method thereof that use in the stoves such as crystal growing furnace and crystal pulling apparatus, ceramic sintering furnace, vacuum high-temperature heat treatment furnace.
Background technology
The carbon-fiber heat-insulation material used in current domestic high-temperature vacuum furnace is divided into two classes: a class is carbon fiber flexible felt, and a class is the hard felt of carbon fiber.
Carbon fiber flexible felt heat-insulating heat-preserving material generally adopts soft carbon felt (Nomex), and the heat-insulating heat-preserving material of this structure exists low, yielding, the easy efflorescence of intensity, effect of heat insulation difference and dismounting, installs shortcomings such as wasting time and energy.And carbon fiber hard felt heat-insulating heat-preserving material overcomes the shortcoming existing for soft carbon felt, as crystal furnace, ceramic sintering furnace, the high temperature furnace used heat-insulating heat-preserving material such as gaseous phase deposition stove is widely used.
The hard felt of carbon fiber mainly contains viscose base, PAN base and asphaltic base three kinds, although viscose base carbon fibre thermal conductivity is less, its the most applicable lagging material that does of theoretical analysis, but its antioxidant property and intensity are all not as good as asphalt base carbon fiber, and its yield is extremely low, expensive, limit its use to a great extent.PAN base carbon fibre due to raw material cheap, production technique is simple, domestic a lot of producer all with, but it is after pyroprocessing, fiber brittle, easily produces carbon fiber chip, larger harm is caused to furnace atmosphere, and carbon fiber section indentation, can form sharp-pointed section, larger to human health damage.Asphalt base carbon fiber carbon content is high, and volatilization is few, and purity is high, and thermal conductivity is relatively little, and intensity is high should not rupture, even if carbon fiber fracture, the section broken to form is rounder and more smooth minimum to human health damage.The lagging material using asphalt base carbon fiber to produce has the following advantages: 1) excellent heat-proof quality; 2) carbon content is high, and volatile matter is few, pollutes little; 3) higher intensity.
The hard felt of current domestic carbon fiber mainly adopts PAN base soft carbon felt to flood the moulding process of mold pressing or soft carbon felt dipping layering stickup (graphite paper and carbon fiber interval are pasted).The shortcoming that dipping former compression technology exists is that goods interlaminar strength is low, the easy delamination splitting of goods under applied at elevated temperature condition, and work-ing life is short, and because intensity is relatively low, it is convenient not to remove and install; Adopt the hard felt that layering stickup shaping mode is made, although intensity increases, the thermal conductivity of goods increases, and heat-insulating property is deteriorated, and reduces effect of heat insulation.The heat conductivility impact of orientation on lagging material of fiber is relatively more remarkable, and when hot-fluid is parallel to fiber direction, it is less that hot-fluid is subject to resistance, and thermal conductivity is larger; And hot-fluid perpendicular to fiber direction time, the resistance be subject to is larger, and thermal conductivity is less.Nomex hardening product all has the carbon fibre tow of longitudinal stretching, therefore some carbon fiber is parallel with direction of heat flow, and therefore thermal conductivity is relatively large, and the lagging material energy consumption of relative two dimensional structure is large.
Summary of the invention
The invention provides a kind of asphalt base carbon fiber non-woven mat warming plate, it has the characteristics such as excellent heat-proof quality, low heat capacity, low density and high strength, be the lagging material being specially adapted to the High Temperature Furnaces Heating Apparatuss such as vacuum heat treatment furnace, monocrystalline crystal pulling furnace, ceramic sintering furnace, invention also provides the manufacture method of asphalt base carbon fiber non-woven mat warming plate.
In order to achieve the above object, the present invention realizes by the following technical solutions:
Asphalt base carbon fiber non-woven mat warming plate, comprise asphalt base carbon fiber non-woven mat warming plate body, described asphalt base carbon fiber non-woven mat warming plate body be after being mixed with the mixed solution of organic binder bond+solvent by asphalt base carbon fiber non-woven mat through cutting, stacked, shaping, solidify, sheet material obtained after carbonization/graphitization processing, asphalt base carbon fiber non-woven mat is obtained through spinning, preoxidation and carbonization by pitch, and the weight ratio of asphalt base carbon fiber non-woven mat, binding agent, solvent is: 100:30 ~ 200:18 ~ 600.
Described asphalt base carbon fiber non-woven mat warming plate body single or double is through surface treatment, and handled surface sets gradually carbon material adhesive layer and graphite paper/carbon cloth from inside to outside, and finished product is through solidification, carbonizing treatment.
Described organic binder bond is one or more in resol, epoxy resin, furane resin, urea-formaldehyde resin, vinyl ester resin, polymeric amide, acrylic resin, polyethylene, polypropylene, ethylene propylene copolymer, polystyrene, pitch and tar.
Described solvent is one or more in methyl alcohol, ethanol, propyl alcohol, ethylene glycol, propylene glycol, furfuryl alcohol, furfural, acetone, benzene, toluene.
Described carbon material adhesive layer is formed by the brushing of carbon material binding agent, carbon material binding agent by can char-forming material, dispersion agent, short cut or ground carbon fiber, Graphite Powder 99, carborundum powder and silica flour by weight ratio mixing and stirring make, the weight ratio of each component is: can char-forming material 40 ~ 100 weight part, dispersion agent 40 ~ 160 weight part, shortly to cut or ground carbon fiber 5 ~ 20 weight part, Graphite Powder 99 25 ~ 50 weight part, carborundum powder 10 ~ 30 weight part, silica flour 5 ~ 20 weight part; Wherein graphite powder particle diameter is 10-600 μm, and carborundum powder granularity is 200-1000 order, and silicon particle size is 200-1000 order.
Described can char-forming material be one in resol, epoxy resin, furane resin, urea-formaldehyde resin, vinyl ester resin, polymeric amide, acrylic resin, polyethylene, polypropylene, ethylene propylene copolymer, polystyrene, pitch or tar, two or more combination; Described dispersion agent is one in methyl alcohol, ethanol, propyl alcohol, ethylene glycol, propylene glycol, furfuryl alcohol, furfural, acetone, furfuralcohol, furtural, benzene or toluene, two or more combination.
Describedly shortly to cut or ground carbon fiber is one in asphalt base carbon fiber, viscose-based carbon fiber or polypropylene cyano group carbon fiber, two or more combination, carbon fiber mean length is 10 ~ 1200 μm.
Described asphalt base carbon fiber non-woven mat warming plate body single or double is through coating dipping or vapour deposition process, and finished product is overall through solidification, carbonizing treatment.
The manufacture method of asphalt base carbon fiber non-woven mat warming plate, comprises the steps:
1) spinning being carried out to pitch, forming non-woven mat, then pre-oxidation treatment by receiving after silk, then carry out carbonization and obtain asphalt base carbon fiber non-woven mat;
2) mixed solution that asphalt base carbon fiber non-woven mat and organic binder bond+solvent are formed fully mixes, and makes binding agent mixed solution fully infiltrate asphalt base carbon fiber non-woven mat by the mode spraying, brush or flood;
3) by the size cutting as requested of asphalt base carbon fiber non-woven mat, be laid on bed die after stacked, when reaching required thickness, premolding is complete, is then fixed on by mold in stacked good preformed board, pressurizes fixed for preformed board thick compacting;
4) solidification treatment: by step 3) obtained asphalt base carbon fiber non-woven mat preformed board puts into baking oven together with mould, at 130 ~ 350 DEG C of temperature, be cured process;
5) carbonization/greying/carbonization+graphitization processing: by the preformed board demoulding after solidification treatment, then puts into carbonization under vacuum oven or inert atmosphere, carbonization temperature 700 ~ 1200 DEG C; Or carrying out graphitization processing, graphitization temperature is 1800 ~ 2500 DEG C; Or at 700 ~ 1200 DEG C of temperature graphitization processing at 1800 ~ 2500 DEG C of temperature again after carbonization; Obtained asphalt base carbon fiber non-woven mat warming plate body.
Asphalt base carbon fiber non-woven mat warming plate manufacture method, comprises the steps:
1) spinning being carried out to pitch, forming non-woven mat, then pre-oxidation treatment by receiving after silk, then carry out carbonization and obtain asphalt base carbon fiber non-woven mat;
2) mixed solution that asphalt base carbon fiber non-woven mat and organic binder bond+solvent are formed fully mixes, and makes binding agent mixed solution fully infiltrate asphalt base carbon fiber non-woven mat by the mode spraying, brush or flood;
3) asphalt base carbon fiber non-woven mat and the size cutting as requested of graphite paper/carbon cloth, on graphite paper/carbon cloth, brushing carbon material binding agent forms carbon material adhesive layer;
4) get the graphite paper/carbon cloth cut, cated one side is upwards laid on bed die, lays stacked asphalt base carbon fiber non-woven mat thereon, and when reaching required thickness, the asphalt base carbon fiber non-woven mat warming plate premolding of one side process is complete; As needed double treatment, then separately get the graphite paper/carbon cloth cut, cated one faces down is put in asphalt base carbon fiber non-woven mat, finally installs mould pressurizing by fixed for preformed board thick compacting;
5) solidification treatment: by step 4) obtained asphalt base carbon fiber non-woven mat preformed board puts into baking oven together with mould, is warmed up to 130 ~ 350 DEG C, at this temperature thermostatically heating 1 ~ 5.5h with the temperature rise rate of 1 ~ 15 DEG C/min;
6) carbonization/greying/carbonization+graphitization processing: by the preformed board demoulding after solidification treatment, then puts into carbonization under vacuum oven or inert atmosphere, carbonization temperature 700 ~ 1200 DEG C; Or carrying out graphitization processing, graphitization temperature is 1800 ~ 2500 DEG C; Or at 700 ~ 1200 DEG C of temperature graphitization processing at 1800 ~ 2500 DEG C of temperature again after carbonization; Obtained asphalt base carbon fiber non-woven mat warming plate.
Compared with prior art, the invention has the beneficial effects as follows:
1) fiber direction of asphalt base carbon fiber non-woven mat warming plate of the present invention meets two-dimensional arrangements, and vertical with direction of heat flow, and be heat insulation optimum orientation, therefore heat insulation property is good;
2) density reaches 0.1-0.4g/cm 3, intensity is high, and self-supporting is good, has more advantage when making large size product;
3) after surface treatment, anti-oxidant, anti-airflow scouring, long service life;
4) technique is simple, and cost of manufacture is low, can be once fixed thick, and product is not easy to crack, good stability.
Accompanying drawing explanation
Fig. 1 is the structural representation of the asphalt base carbon fiber non-woven mat warming plate through monoplanar surface process of the present invention.
Fig. 2 is the structural representation through two-sided surface-treated asphalt base carbon fiber non-woven mat warming plate of the present invention.
Fig. 3 is the process flow sheet of asphalt base carbon fiber non-woven mat impregnated with adhesive mixed solution of the present invention.
Fig. 4 is the premolding schematic diagram of asphalt base carbon fiber non-woven mat warming plate (without surface treatment) of the present invention.
Fig. 5 is the premolding schematic diagram of asphalt base carbon fiber non-woven mat warming plate (through surface treatment) of the present invention.
In figure: 1. asphalt base carbon fiber non-woven mat 2. Extruded roller 3. binding agent solvent liquid pool 4. axle 5. mold 6. asphalt base carbon fiber non-woven mat preformed board 7. bed die 8. carbon material adhesive layer 9. graphite papers/carbon cloth 10. asphalt base carbon fiber non-woven mat warming plate bodies
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described further:
Seeing Fig. 1-Fig. 2, is the structural representation through single or double surface-treated asphalt base carbon fiber non-woven mat warming plate of the present invention.Asphalt base carbon fiber non-woven mat warming plate of the present invention, comprise asphalt base carbon fiber non-woven mat warming plate body 10, described asphalt base carbon fiber non-woven mat warming plate body 10 be after being mixed with the mixed solution of organic binder bond+solvent by asphalt base carbon fiber non-woven mat 1 through cutting, stacked, shaping, solidify, sheet material obtained after carbonization/graphitization processing, asphalt base carbon fiber non-woven mat 1 is obtained through spinning, preoxidation and carbonization by pitch, and the weight ratio of asphalt base carbon fiber non-woven mat 1, binding agent, solvent is: 100:30 ~ 200:18 ~ 600.
Described asphalt base carbon fiber non-woven mat warming plate body 10 single or double is through surface treatment, and handled surface sets gradually carbon material adhesive layer 8 and graphite paper/carbon cloth 9 from inside to outside, and finished product is through solidification, carbonizing treatment.
Described organic binder bond is one or more in resol, epoxy resin, furane resin, urea-formaldehyde resin, vinyl ester resin, polymeric amide, acrylic resin, polyethylene, polypropylene, ethylene propylene copolymer, polystyrene, pitch and tar.
Described solvent is one or more in methyl alcohol, ethanol, propyl alcohol, ethylene glycol, propylene glycol, furfuryl alcohol, furfural, acetone, benzene, toluene.
Described carbon material adhesive layer 8 is formed by the brushing of carbon material binding agent, carbon material binding agent by can char-forming material, dispersion agent, short cut or ground carbon fiber, Graphite Powder 99, carborundum powder and silica flour by weight ratio mixing and stirring make, the weight ratio of each component is: can char-forming material 40 ~ 100 weight part, dispersion agent 40 ~ 160 weight part, shortly to cut or ground carbon fiber 5 ~ 20 weight part, Graphite Powder 99 25 ~ 50 weight part, carborundum powder 10 ~ 30 weight part, silica flour 5 ~ 20 weight part; Wherein graphite powder particle diameter is 10-600 μm, preferred 30-300 μm; Carborundum powder granularity is 200-1000 order, preferred 300-800 order; Silicon particle size is 200-1000 order, preferred 300-800 order.
Described can char-forming material be one in resol, epoxy resin, furane resin, urea-formaldehyde resin, vinyl ester resin, polymeric amide, acrylic resin, polyethylene, polypropylene, ethylene propylene copolymer, polystyrene, pitch or tar, two or more combination; Described dispersion agent is one in methyl alcohol, ethanol, propyl alcohol, ethylene glycol, propylene glycol, furfuryl alcohol, furfural, acetone, furfuralcohol, furtural, benzene or toluene, two or more combination.
Describedly shortly to cut or ground carbon fiber is one in asphalt base carbon fiber, viscose-based carbon fiber or polypropylene cyano group carbon fiber, two or more combination, carbon fiber mean length is 10 ~ 1200 μm, preferred 50-400 μm.
Described asphalt base carbon fiber non-woven mat warming plate body single or double is through coating dipping or vapour deposition process, and finished product is overall through solidification, carbonizing treatment.
Seeing Fig. 3, is the process flow sheet of asphalt base carbon fiber non-woven mat impregnated with adhesive mixed solution of the present invention.The manufacture method of not surface treated asphalt base carbon fiber non-woven mat warming plate of the present invention and asphalt base carbon fiber non-woven mat warming plate body 10, comprises the steps:
1) spinning being carried out to pitch, forming non-woven mat, then pre-oxidation treatment by receiving after silk, then carry out carbonization and obtain asphalt base carbon fiber non-woven mat 1;
2) mixed solution that asphalt base carbon fiber non-woven mat 1 and organic binder bond+solvent are formed fully mixes, and makes binding agent mixed solution fully infiltrate asphalt base carbon fiber non-woven mat 1 by the mode spraying, brush or flood; (see Fig. 3)
3) by asphalt base carbon fiber non-woven mat 1 size cutting as requested, be laid on bed die 7 after stacked, when reaching required thickness, premolding is complete, is then fixed on by mold 5 in stacked good preformed board 6, pressurizes fixed for preformed board 6 thick compacting; (see Fig. 4)
4) solidification treatment: by step 3) obtained asphalt base carbon fiber non-woven mat preformed board 6 puts into baking oven together with mould 5,7, at 130 ~ 350 DEG C of temperature, be cured process;
5) carbonization/greying/carbonization+graphitization processing: by preformed board 6 demoulding after solidification treatment, then puts into carbonization under vacuum oven or inert atmosphere, carbonization temperature 700 ~ 1200 DEG C; Or carrying out graphitization processing, graphitization temperature is 1800 ~ 2500 DEG C; Or at 700 ~ 1200 DEG C of temperature graphitization processing at 1800 ~ 2500 DEG C of temperature again after carbonization; Obtained asphalt base carbon fiber non-woven mat warming plate body 10.
For increasing the surface property of asphalt base carbon fiber non-woven mat warming plate, the asphalt base carbon fiber non-woven mat warming plate body 10 after to above-mentioned shaping carbonization/greying is needed to carry out surface treatment, by once shaped, graphite paper/carbon cloth 9 can be compounded on asphalt base carbon fiber non-woven mat warming plate body 10, or the process such as machining rear surface subsides graphite paper/carbon cloth 9, coating dipping, vapour deposition are carried out to the asphalt base carbon fiber non-woven mat warming plate body 10 after above-mentioned carbonization/greying.Wherein through the manufacture method of the asphalt base carbon fiber non-woven mat warming plate of once shaped composite graphite paper/carbon cloth 9, comprise the steps:
1) spinning being carried out to pitch, forming non-woven mat, then pre-oxidation treatment by receiving after silk, then carry out carbonization and obtain asphalt base carbon fiber non-woven mat 1;
2) mixed solution that asphalt base carbon fiber non-woven mat 1 and organic binder bond+solvent are formed fully mixes, and makes binding agent mixed solution fully infiltrate asphalt base carbon fiber non-woven mat 1 by the mode spraying, brush or flood;
3) asphalt base carbon fiber non-woven mat 1 and graphite paper/carbon cloth 9 size cutting as requested, on graphite paper/carbon cloth 9, brushing carbon material binding agent forms carbon material adhesive layer 8;
4) graphite paper/carbon cloth 9 cut is got, cated one side is upwards laid on bed die 7, lay stacked asphalt base carbon fiber non-woven mat 1 thereon, when reaching required thickness, the asphalt base carbon fiber non-woven mat warming plate premolding of one side process is complete; As needed double treatment, then separately get the graphite paper/carbon cloth 9 cut, cated one faces down be put into premolding after asphalt base carbon fiber non-woven mat 1 on, finally install mould 5 and pressurize fixed for preformed board 6 thick compacting; (see Fig. 5)
5) solidification treatment: by step 4) obtained asphalt base carbon fiber non-woven mat preformed board 6 puts into baking oven together with mould 5,7, is warmed up to 130 ~ 350 DEG C, at this temperature thermostatically heating 1 ~ 5.5h with the temperature rise rate of 1 ~ 15 DEG C/min;
6) carbonization/greying/carbonization+graphitization processing: by preformed board 6 demoulding after solidification treatment, then puts into carbonization under vacuum oven or inert atmosphere, carbonization temperature 700 ~ 1200 DEG C; Or carrying out graphitization processing, graphitization temperature is 1800 ~ 2500 DEG C; Or at 700 ~ 1200 DEG C of temperature graphitization processing at 1800 ~ 2500 DEG C of temperature again after carbonization; Obtained asphalt base carbon fiber non-woven mat warming plate.
Following examples are implemented under premised on technical solution of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention are not limited to following embodiment.In following embodiment, method therefor is ordinary method if no special instructions.
[embodiment 1] asphalt-based carbon fiber non-woven mat warming plate manufacturing processed is as follows:
Spinning being carried out to pitch, forming non-woven mat, then pre-oxidation treatment by receiving after silk, then carry out carbonization and obtain asphalt base carbon fiber non-woven mat 1; Asphalt-based carbon fiber non-woven mat 1 is put into the binding agent mixing liquid pool 3 fully dipping of organic binder bond+solvent under the rotary action of cylinder axle 4, organic binder bond is resol, and solvent is ethanol; The weight ratio of binding agent mixed solution is resol: ethanol=40:60, then unnecessary binding agent is extruded by Extruded roller 2 by asphalt base carbon fiber non-woven mat 1, again by asphalt base carbon fiber non-woven mat 1 size cutting as requested, be laid on bed die 7 after stacked, shaping complete when reaching 70mm thickness, then mold 5 is fixed in stacked good preformed board 6, pressurizes fixed for preformed board 6 thick 45mm compacting; Obtained asphalt base carbon fiber non-woven mat preformed board 6 is put into baking oven together with mould 5,7, at 200 DEG C, is cured process.Again by asphalt base carbon fiber non-woven mat preformed board 6 demoulding after solidification treatment, put into vacuum oven carbonization, carbonization temperature 900 DEG C; Then graphitization processing, graphitization temperature is 2000 DEG C, produces not surface treated asphalt base carbon fiber non-woven mat warming plate and asphalt base carbon fiber non-woven mat warming plate body.
Obtained asphalt base carbon fiber non-woven mat warming plate density is 0.17g/cm 3, carbon content 99.5%, ash content 0.01%, thermal conductivity 0.31W/mK (sample thickness is 45mm, under nitrogen protection, and detection data when 1500 DEG C).
[example 2] is for increasing the surface property of asphalt base carbon fiber non-woven mat warming plate, be compounded on asphalt base carbon fiber non-woven mat warming plate body 10 by one-shot forming technique by disposable for graphite paper 9, produce surface treated asphalt base carbon fiber non-woven mat warming plate, specifically comprise the steps:
Spinning being carried out to pitch, forming non-woven mat, then pre-oxidation treatment by receiving after silk, then carry out carbonization and obtain asphalt base carbon fiber non-woven mat 1; Asphalt-based carbon fiber non-woven mat 1 is put into the binding agent mixing liquid pool 3 fully dipping of organic binder bond+solvent under the rotary action of cylinder axle 4, organic binder bond is resol, and solvent is ethanol; The weight ratio of binding agent mixed solution is resol: ethanol=40:60, then asphalt base carbon fiber non-woven mat 1 is extruded by unnecessary binding agent by Extruded roller 2.Asphalt base carbon fiber non-woven mat 1 and graphite paper 9 size cutting as requested, each components by weight of carbon material binding agent is resol: ethanol: asphalt base carbon fiber: Graphite Powder 99: carborundum powder: silica flour=56:44:12:20:8:6, mix obtained carbon material binding agent, on graphite paper 9, brushing carbon material binding agent forms carbon material adhesive layer 8; Get the graphite paper 9 cut, cated one side is upwards laid on bed die 7, lay stacked asphalt base carbon fiber non-woven mat 1 thereon, when reaching required thickness, premolding is complete, separately get the graphite paper 9 cut, cated one faces down be put into premolding after asphalt base carbon fiber non-woven mat 1 on, finally install mould 5 and pressurize fixed for preformed board 6 thick compacting;
Obtained asphalt base carbon fiber non-woven mat preformed board 6 is put into baking oven together with mould 5,7, is warmed up to 200 DEG C with the temperature rise rate of 3 DEG C/min, at this temperature thermostatically heating 2h, solidification carbon material adhesive layer 8; By preformed board 6 demoulding after solidification treatment, then put into vacuum oven carbonization, carbonization temperature 900 DEG C; Then graphitization processing, graphitization temperature is 2000 DEG C; Obtained surface treated asphalt base carbon fiber non-woven mat warming plate.
Obtained asphalt base carbon fiber non-woven mat warming plate density is 0.19g/cm 3, carbon content 99.5%, ash content 0.01%, thermal conductivity 0.31W/mK (sample thickness is 45mm, under nitrogen protection, and detection data when 1500 DEG C).
After the asphalt base carbon fiber non-woven mat warming plate of the disposable composite graphite paper produced according to above method uses 1 year on polycrystalline silicon ingot or purifying furnace, do not occur that graphite ply of paper is peeled off, the phenomenons such as foaming, the corrosion-free phenomenon of asphalt base carbon fiber non-woven mat warming plate body inside graphite ply of paper, significantly improves the life-span of asphalt base carbon fiber non-woven mat warming plate.
Asphalt base carbon fiber non-woven mat warming plate after surface treatment can to prevent in stove foreign gas directly and asphalt base carbon fiber non-woven mat warming plate surface contact, prevent corrosion and anti-airflow scouring, there is excellent anti-oxidant and corrosion resistance, the life-span of asphalt base carbon fiber non-woven mat warming plate can be significantly improved.

Claims (10)

1. asphalt base carbon fiber non-woven mat warming plate, comprise asphalt base carbon fiber non-woven mat warming plate body, it is characterized in that, described asphalt base carbon fiber non-woven mat warming plate body be after being mixed with the mixed solution of organic binder bond+solvent by asphalt base carbon fiber non-woven mat through cutting, stacked, shaping, solidify, sheet material obtained after carbonization/graphitization processing, asphalt base carbon fiber non-woven mat is obtained through spinning, preoxidation and carbonization by pitch, and the weight ratio of asphalt base carbon fiber non-woven mat, binding agent, solvent is: 100:30 ~ 200:18 ~ 600.
2. asphalt base carbon fiber non-woven mat warming plate according to claim 1, it is characterized in that, described asphalt base carbon fiber non-woven mat warming plate body single or double is through surface treatment, handled surface sets gradually carbon material adhesive layer and graphite paper/carbon cloth from inside to outside, and finished product is through solidification, carbonizing treatment.
3. asphalt base carbon fiber non-woven mat warming plate according to claim 1, it is characterized in that, described organic binder bond is one or more in resol, epoxy resin, furane resin, urea-formaldehyde resin, vinyl ester resin, polymeric amide, acrylic resin, polyethylene, polypropylene, ethylene propylene copolymer, polystyrene, pitch and tar.
4. asphalt base carbon fiber non-woven mat warming plate according to claim 1, is characterized in that, described solvent is one or more in methyl alcohol, ethanol, propyl alcohol, ethylene glycol, propylene glycol, furfuryl alcohol, furfural, acetone, benzene, toluene.
5. asphalt base carbon fiber non-woven mat warming plate according to claim 2, it is characterized in that, described carbon material adhesive layer is formed by the brushing of carbon material binding agent, carbon material binding agent is by can char-forming material, dispersion agent, shortly to cut or ground carbon fiber, Graphite Powder 99, carborundum powder and silica flour by weight ratio mixing and stirring are made, the weight ratio of each component is: can char-forming material 40 ~ 100 weight part, dispersion agent 40 ~ 160 weight part, shortly to cut or ground carbon fiber 5 ~ 20 weight part, Graphite Powder 99 25 ~ 50 weight part, carborundum powder 10 ~ 30 weight part, silica flour 5 ~ 20 weight part, wherein graphite powder particle diameter is 10-600 μm, and carborundum powder granularity is 200-1000 order, and silicon particle size is 200-1000 order.
6. asphalt base carbon fiber non-woven mat warming plate according to claim 5, it is characterized in that, described can char-forming material be one in resol, epoxy resin, furane resin, urea-formaldehyde resin, vinyl ester resin, polymeric amide, acrylic resin, polyethylene, polypropylene, ethylene propylene copolymer, polystyrene, pitch or tar, two or more combination; Described dispersion agent is one in methyl alcohol, ethanol, propyl alcohol, ethylene glycol, propylene glycol, furfuryl alcohol, furfural, acetone, furfuralcohol, furtural, benzene or toluene, two or more combination.
7. asphalt base carbon fiber non-woven mat warming plate according to claim 5, it is characterized in that, describedly shortly to cut or ground carbon fiber is one in asphalt base carbon fiber, viscose-based carbon fiber or polypropylene cyano group carbon fiber, two or more combination, carbon fiber mean length is 10 ~ 1200 μm.
8. asphalt base carbon fiber non-woven mat warming plate according to claim 1, is characterized in that, described asphalt base carbon fiber non-woven mat warming plate body single or double is through coating dipping or vapour deposition process, and finished product is overall through solidification, carbonizing treatment.
9. the manufacture method of asphalt base carbon fiber non-woven mat warming plate according to claim 1, is characterized in that, comprise the steps:
1) spinning being carried out to pitch, forming non-woven mat, then pre-oxidation treatment by receiving after silk, then carry out carbonization and obtain asphalt base carbon fiber non-woven mat;
2) mixed solution that asphalt base carbon fiber non-woven mat and organic binder bond+solvent are formed fully mixes, and makes binding agent mixed solution fully infiltrate asphalt base carbon fiber non-woven mat by the mode spraying, brush or flood;
3) by the size cutting as requested of asphalt base carbon fiber non-woven mat, be laid on bed die after stacked, when reaching required thickness, premolding is complete, is then fixed on by mold in stacked good preformed board, pressurizes fixed for preformed board thick compacting;
4) solidification treatment: by step 3) obtained asphalt base carbon fiber non-woven mat preformed board puts into baking oven together with mould, at 130 ~ 350 DEG C of temperature, be cured process;
5) carbonization/greying/carbonization+graphitization processing: by the preformed board demoulding after solidification treatment, then puts into carbonization under vacuum oven or inert atmosphere, carbonization temperature 700 ~ 1200 DEG C; Or carrying out graphitization processing, graphitization temperature is 1800 ~ 2500 DEG C; Or at 700 ~ 1200 DEG C of temperature graphitization processing at 1800 ~ 2500 DEG C of temperature again after carbonization; Obtained asphalt base carbon fiber non-woven mat warming plate body.
10. the manufacture method of asphalt base carbon fiber non-woven mat warming plate according to claim 2, is characterized in that, comprise the steps:
1) spinning being carried out to pitch, forming non-woven mat, then pre-oxidation treatment by receiving after silk, then carry out carbonization and obtain asphalt base carbon fiber non-woven mat;
2) mixed solution that asphalt base carbon fiber non-woven mat and organic binder bond+solvent are formed fully mixes, and makes binding agent mixed solution fully infiltrate asphalt base carbon fiber non-woven mat by the mode spraying, brush or flood;
3) asphalt base carbon fiber non-woven mat and the size cutting as requested of graphite paper/carbon cloth, on graphite paper/carbon cloth, brushing carbon material binding agent forms carbon material adhesive layer;
4) get the graphite paper/carbon cloth cut, cated one side is upwards laid on bed die, lays stacked asphalt base carbon fiber non-woven mat thereon, and when reaching required thickness, the asphalt base carbon fiber non-woven mat warming plate premolding of one side process is complete; As needed double treatment, then separately get the graphite paper/carbon cloth cut, cated one faces down is put in asphalt base carbon fiber non-woven mat, finally installs mould pressurizing by fixed for preformed board thick compacting;
5) solidification treatment: by step 4) obtained asphalt base carbon fiber non-woven mat preformed board puts into baking oven together with mould, is warmed up to 130 ~ 350 DEG C, at this temperature thermostatically heating 1 ~ 5.5h with the temperature rise rate of 1 ~ 15 DEG C/min;
6) carbonization/greying/carbonization+graphitization processing: by the preformed board demoulding after solidification treatment, then puts into carbonization under vacuum oven or inert atmosphere, carbonization temperature 700 ~ 1200 DEG C; Or carrying out graphitization processing, graphitization temperature is 1800 ~ 2500 DEG C; Or at 700 ~ 1200 DEG C of temperature graphitization processing at 1800 ~ 2500 DEG C of temperature again after carbonization; Obtained asphalt base carbon fiber non-woven mat warming plate.
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