CN105712730B - A kind of preparation method of the hard felt of dead size C/C complex heat-preservation - Google Patents
A kind of preparation method of the hard felt of dead size C/C complex heat-preservation Download PDFInfo
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- CN105712730B CN105712730B CN201410729467.XA CN201410729467A CN105712730B CN 105712730 B CN105712730 B CN 105712730B CN 201410729467 A CN201410729467 A CN 201410729467A CN 105712730 B CN105712730 B CN 105712730B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000004321 preservation Methods 0.000 title claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 106
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 80
- 239000004744 fabric Substances 0.000 claims abstract description 31
- 239000010439 graphite Substances 0.000 claims abstract description 29
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000002131 composite material Substances 0.000 claims abstract description 13
- 238000000746 purification Methods 0.000 claims abstract description 13
- 238000002803 maceration Methods 0.000 claims abstract description 12
- 238000003475 lamination Methods 0.000 claims abstract description 10
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 9
- 239000004917 carbon fiber Substances 0.000 claims abstract description 9
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000465 moulding Methods 0.000 claims abstract description 8
- 238000007598 dipping method Methods 0.000 claims abstract description 7
- 238000004381 surface treatment Methods 0.000 claims abstract description 7
- 229920005989 resin Polymers 0.000 claims abstract description 5
- 239000011347 resin Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000003763 carbonization Methods 0.000 claims description 9
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 7
- 238000005470 impregnation Methods 0.000 claims description 7
- 229920001568 phenolic resin Polymers 0.000 claims description 7
- 239000005011 phenolic resin Substances 0.000 claims description 7
- 239000000835 fiber Substances 0.000 claims description 5
- 238000007788 roughening Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000007711 solidification Methods 0.000 claims description 5
- 230000008023 solidification Effects 0.000 claims description 5
- 238000005255 carburizing Methods 0.000 claims description 4
- 229920000297 Rayon Polymers 0.000 claims description 2
- 239000010426 asphalt Substances 0.000 claims description 2
- 230000001680 brushing effect Effects 0.000 claims description 2
- 229920002239 polyacrylonitrile Polymers 0.000 claims 1
- 230000004888 barrier function Effects 0.000 abstract 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 9
- 238000009413 insulation Methods 0.000 description 5
- 239000004743 Polypropylene Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- -1 polypropylene Polymers 0.000 description 4
- 229920001155 polypropylene Polymers 0.000 description 4
- 230000002708 enhancing effect Effects 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 238000003754 machining Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- IUHFWCGCSVTMPG-UHFFFAOYSA-N [C].[C] Chemical group [C].[C] IUHFWCGCSVTMPG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
Abstract
The present invention relates to a kind of preparation methods of the hard felt of dead size C/C composite material complex heat-preservation, include the following steps：Prepare finger gauge；It chooses carbon fiber and is prepared into carbon felt, carbon cloth；Resin is chosen as maceration extract, flexible graphite paper is as surface treatment；Carbon felt, carbon cloth and flexible graphite paper are subjected to dipping process respectively；The lamination formed by carbon felt, carbon cloth and flexible graphite paper is subjected to curing molding；The product for obtaining curing molding is carbonized, high temperature purification processing.Method of the invention is easy to operate, at low cost, and the period is short, and gas barrier properties are good, high mechanical strength, good product consistency.
Description
Technical field
It is compound with C/C composite material that the present invention relates to the preparation methods of compound hard felt more particularly to a kind of high temperature industrial furnace
The preparation method of hard felt.
Background technique
Carbon/carbon composite material thermal-insulation felt is widely used in the high temperature work such as monocrystalline silicon growing furnace, polycrystalline silicon ingot or purifying furnace, sintering furnace
In industry equipment, the energy consumption that performance and service life run hot industry equipment, cost control, product quality etc. has crucial make
With.Insulation quilt is divided into soft felt and two kinds of hard felt, the shape that soft felt is not fixed, and it is bigger and infrequently to be commonly used in furnace inner space
The type of furnace of dismounting；Hard felt can be designed to the product of accurate dimension, can directly be assembled with fastener etc. in shove charge, assembly letter
It is single.The insulation quilt of polycrystalline ingot furnace is substantially all at present selects hard felt.Hard felt can be divided into whole hard felt and multiple according to structure type
Hard felt is closed, the precast body that whole hard felt uses is net tire needling structure, and good integrity, intensity is high, long service life, but it is manufactured
It is at high cost, and be affected by needle prick shape state, if needle pierce it is too deep if material thermal insulation property it is poor, if needle pierces uneven pole
Easily there is Large Area Cracking phenomenon, and depth of needling and density are undetectable variables, are easy to cause Product Status unstable
It is fixed；The thickness of the mat of 5mm/10mm thickness or so as required is generally bonded by MULTILAYER COMPOSITE felt, such compound felt
Preparation Method is simple, raw material technical maturity, period are short, at low cost, but its globality poor, and intensity is lower, density uniformity is poor,
Carbon dust, layering are easy in use process.
Summary of the invention
The object of the present invention is to provide it is a kind of use high osmosis, large arch dam phenolic resin for maceration extract, double rods
Extruding pulling equipment is gumming device, and carbon cloth is enhancing structure, the high temperature industrial furnace C/C that flexible graphite paper is surface-treated
The preparation method method of the compound hard felt of composite material.
The invention is realized in this way a kind of preparation method of the hard felt of dead size C/C composite material complex heat-preservation, including with
Lower step：
(1) finger gauge is prepared；
(2) it chooses carbon fiber and is prepared into carbon felt, carbon cloth；
(3) resin is chosen as maceration extract, and flexible graphite paper is as surface treatment；
(4) carbon felt, carbon cloth and flexible graphite paper are subjected to dipping process respectively；
(5) lamination formed by carbon felt, carbon cloth and flexible graphite paper is subjected to curing molding；
(6) product that step (5) obtain curing molding is carbonized, high temperature purification processing.
The finger gauge scale error answers≤0.02mm, the pressure >=2MPa that can be born.
The carbon fiber is that asphalt base carbon fiber, the fine base carbon fibre of polypropylene or viscose-based carbon fiber, carbon felt volume are close
Degree is 0.10~0.20g/cm3, 6K carbon cloth surface density is 250~350g/m2, preparation method is plain weave.
The flexible graphite paper need to be covered with groined type gas circuit by surface roughening treatment and surface.
The resin is phenolic resin, and solid content is 40~50%, viscosity 10-20mpa.s.
The carbon felt impregnation equipment, allows carbon felt to first pass through steeping vat, after dipping process is completed under the traction of double rods, together
When the residual quantity of maceration extract in carbon felt is quantitatively controlled by controlling the distance between double rods.
The mode that the impregnation of carbon cloth and flexible graphite paper is all made of quantitative brushing carries out.
Curing process is carried out using hot press, the lamination includes two layers of flexible graphite paper and is placed in the two sides soft graphite
Multilayer temporary location between paper, the multilayer temporary location include one layer of carbon felt arranging from bottom to top and several by one layer
Carbon felt and one layer of carbon cloth combination layer stacked on top of one another.
The solidification temperature of the curing process is 140~180 DEG C, 2~4h of curing time；The carbonization temperature of the carbonization treatment
750~900 DEG C, 2~4h of carbonization time of degree, heating rate≤30 DEG C/h；The high temperature purification of the high temperature purification processing handles temperature
Degree is 1500~2000 DEG C, handles 2~6h of time, heating rate≤100 DEG C/h.
The beneficial effects of the invention are as follows：
(1) present invention realizes the same stepping of hot-press solidifying, structure enhancing and surface treatment by dead size forming technique
Row, simplifies manufacturing procedure, shortens manufacturing cycle, reduce process costs.
(2) 1600 DEG C of high-temperature heat conductivities of composite felt prepared by the present invention are 0.3-0.4w/m.k, compressive strength >=0.5MPa.
It (3) is raw material present invention employs carbon felt, maceration extract is recyclable to be reused, and cost of material is lower.
(4) present invention employs special dipping equipment, realize uniformity, the controllability of product density.
It (5) is enhancing structure present invention employs carbon cloth, phenolic resin is maceration extract, product strength height, long service life.
(6) present invention employs protective film designs, ensure that the bright and clean, beautiful of product surface.
(7) the method for the present invention can be according to product requirement, design thickness scale cun and lamination quantity, without changing former material gauge
Mass production can be realized in lattice.
(8) present invention devises special spliced tooling, ensure that large size product flatness requirement.
Detailed description of the invention
Fig. 1 is carbon felt gumming device schematic diagram group；
Fig. 2 is schematic diagram of laminated structure.
Wherein, 1- maceration extract；2- dipping tank；3- carbon felt；The bis- rods of 4- squeeze pulling equipment；5- carbon cloth；6- flexible graphite paper；
7- carbon felt.
Specific embodiment
Dead size C/C thermal-insulation hard felt preparation method of the present invention is made combined with specific embodiments below further specific
Description.
Embodiment one,
(1) according to product specification, finger gauge is prepared first, finger gauge 40 ± 0.02mm of size, the pressure that can be born >=
2MPa；
(2) it chooses the fine base carbon fibre of polypropylene and is prepared into 10mm carbon felt, 6K carbon cloth, carbon felt bulk density is 0.10g/cm3,
6K carbon cloth surface density is 280g/m2, preparation method is plain weave；
(3) phenolic resin that selection solid content is 45%, viscosity is 12mpa.s is as maceration extract, the flexible stone of 0.6mm thickness
Flexible graphite paper is carried out surface roughening and is covered with groined type gas circuit by black paper as surface treatment；
(4) allow carbon felt to first pass through steeping vat as shown in Fig. 1 using impregnation equipment, after leaching is completed under the traction of double rods
Glue process, controlling the distance between double rods is 50% carbon felt thickness；Respectively according to 200g/m2With 100g/m2Dosage brush carbon cloth
The rough surface on two surfaces and flexible graphite paper；
(5) illustrate graph structure according to lamination, as shown in Fig. 2, by two layers of flexible graphite paper, three layers of carbon cloth and four layers of 10mm
Carbon felt is combined with each other, and is placed on the hot press for having placed finger gauge etc. to be solidified；
(6) it will be solidified in product, be carbonized, high temperature purification processing, solidification temperature is 140~180 DEG C, curing time 2
~4h；750~900 DEG C of carburizing temperature, 2~4h of carbonization time, heating rate≤30 DEG C/h；High temperature purification treatment temperature is 1500
~2000 DEG C, handle 2~6h of time, heating rate≤100 DEG C/h；
(7) according to drawing requirement, process is machining, and obtaining density is 0.20g/cm3The hard felt of C/C complex heat-preservation.
Embodiment two,
(1) according to product specification, finger gauge is prepared first, finger gauge 20 ± 0.02mm of size, the pressure that can be born >=
2MPa；
(2) it chooses the fine base carbon fibre of polypropylene and is prepared into 10mm carbon felt, 6K carbon cloth, carbon felt bulk density is 0.15g/cm3,
6K carbon cloth surface density is 280g/m2, preparation method is plain weave.；
(3) phenolic resin that selection solid content is 45%, viscosity is 12mpa.s is as maceration extract, the flexible stone of 0.6mm thickness
Flexible graphite paper is carried out surface roughening and is covered with groined type gas circuit by black paper as surface treatment；
(4) allow carbon felt to first pass through steeping vat as shown in Fig. 1 using impregnation equipment, after leaching is completed under the traction of double rods
Glue process, controlling the distance between double rods is 40% carbon felt thickness；Respectively according to 200g/m2With 100g/m2Dosage brush carbon cloth
The rough surface on two surfaces and flexible graphite paper；
(5) illustrate graph structure according to lamination, as shown in Fig. 2, by two layers of flexible graphite paper, one layer of carbon cloth and two layers of 10mm
Carbon felt is combined with each other, and is placed on the hot press for having placed finger gauge etc. to be solidified；
(6) it will be solidified in product, be carbonized, high temperature purification processing, solidification temperature is 140~180 DEG C, curing time 2
~4h；750~900 DEG C of carburizing temperature, 2~4h of carbonization time, heating rate≤30 DEG C/h；High temperature purification treatment temperature is 1500
~2000 DEG C, handle 2~6h of time, heating rate≤100 DEG C/h；
(7) according to drawing requirement, process is machining, and obtaining density is 0.25g/cm3The hard felt of C/C complex heat-preservation.
Embodiment three,
(1) according to product specification, finger gauge is prepared first, finger gauge 65 ± 0.02mm of size, the pressure that can be born >=
2MPa；
(2) it chooses the fine base carbon fibre of polypropylene and is prepared into 5mm and 10mm carbon felt, 6K carbon cloth, carbon felt bulk density is
0.20g/cm3, 6K carbon cloth surface density is 280g/m2, preparation method is plain weave.；
(3) phenolic resin that selection solid content is 45%, viscosity is 12mpa.s is as maceration extract, the flexible stone of 0.6mm thickness
Flexible graphite paper is carried out surface roughening and is covered with groined type gas circuit by black paper as surface treatment；
(4) allow carbon felt to first pass through steeping vat as shown in Fig. 1 using impregnation equipment, after leaching is completed under the traction of double rods
Glue process, controlling the distance between double rods is 70% carbon felt thickness；Respectively according to 200g/m2With 100g/m2Dosage brush carbon cloth
The rough surface on two surfaces and flexible graphite paper；
(5) illustrate graph structure according to lamination, as shown in Fig. 2, by two layers of flexible graphite paper, six layers of carbon cloth, six layers of 10mm
Carbon felt and one layer of 5mm carbon felt are combined with each other, and are placed on the hot press for having placed finger gauge etc. to be solidified；
(6) it will be solidified in product, be carbonized, high temperature purification processing, solidification temperature is 140~180 DEG C, curing time 2
~4h；750~900 DEG C of carburizing temperature, 2~4h of carbonization time, heating rate≤30 DEG C/h；High temperature purification treatment temperature is 1500
~2000 DEG C, handle 2~6h of time, heating rate≤100 DEG C/h；
(7) according to drawing requirement, process is machining, and obtaining density is 0.30g/cm3The hard felt of C/C complex heat-preservation.
In above embodiments, before hot-press solidifying molding, by the upper of the lamination formed by carbon felt, carbon cloth and flexible graphite paper
Lower two surfaces should add protective film, it is ensured that product appearance is not damaged.
In carbonization, high-temperature process, every layer is required to shape righting tool between product, if single-piece shape righting tool is unable to satisfy greatly
The preparation requirement of sized products, need to carry out splicing to shape righting tool, and stitching portion side should be fastened using carbon carbon item and carbon carbon
Part connection, guarantees the globality of tooling.
Claims (6)
1. a kind of preparation method of the hard felt of dead size C/C composite material complex heat-preservation, it is characterised in that：Include the following steps：
(1) finger gauge is prepared；The finger gauge scale error answers≤0.02mm, the pressure >=2MPa that can be born；
(2) it chooses carbon fiber and is prepared into carbon felt, carbon cloth；The carbon fiber is asphalt base carbon fiber, polyacrylonitrile-based carbon fibre
Or viscose-based carbon fiber, carbon felt bulk density are 0.10~0.20g/cm3, 6K carbon cloth surface density is 250~350g/m2, establishment side
Method is plain weave；
(3) resin is chosen as maceration extract, and flexible graphite paper is as surface treatment；The flexible graphite paper need to be by surface
Roughening treatment and surface are covered with groined type gas circuit；
(4) carbon felt, carbon cloth and flexible graphite paper are subjected to dipping process respectively；
(5) lamination formed by carbon felt, carbon cloth and flexible graphite paper is subjected to curing molding；
(6) product that step (5) obtain curing molding is carbonized, high temperature purification processing.
2. the preparation method of the hard felt of dead size C/C composite material complex heat-preservation according to claim 1, it is characterised in that：
The resin is phenolic resin, and solid content is 40~50%, viscosity 10-20mpas.
3. the preparation method of the hard felt of dead size C/C composite material complex heat-preservation according to claim 1, it is characterised in that：
Using impregnation equipment, carbon felt is allowed to first pass through steeping vat, after complete dipping process under the traction of double rods, while by controlling double rods
Between distance quantitatively control the residual quantity of maceration extract in carbon felt.
4. the preparation method of the hard felt of dead size C/C composite material complex heat-preservation according to claim 1, it is characterised in that：
The mode that the impregnation of carbon cloth and flexible graphite paper is all made of quantitative brushing carries out.
5. the preparation method of the hard felt of dead size C/C composite material complex heat-preservation according to claim 1, it is characterised in that：
Curing process is carried out using hot press, the lamination includes two layers of flexible graphite paper and is placed between the two layers of flexible graphite paper
Multilayer temporary location, the multilayer temporary location include one layer of carbon felt arranging from bottom to top and several by one layer of carbon felt and one
Layer carbon cloth combination layer stacked on top of one another.
6. the preparation method of the hard felt of dead size C/C composite material complex heat-preservation according to claim 1, it is characterised in that：
The solidification temperature of the curing molding is 140~180 DEG C, 2~4h of curing time；The carburizing temperature 750 of the carbonization treatment~
900 DEG C, 2~4h of carbonization time, heating rate≤30 DEG C/h；The high temperature purification treatment temperature of the high temperature purification processing is 1500
~2000 DEG C, handle 2~6h of time, heating rate≤100 DEG C/h.
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| CN107083020A (en) * | 2017-05-19 | 2017-08-22 | 常熟市奥欣复合材料有限公司 | The recycling method of carbon fiber and its product |
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| CN108129155B (en) * | 2017-12-29 | 2021-03-05 | 湖南省鑫源新材料股份有限公司 | Composite structure carbon-carbon heat-preservation cylinder and preparation method thereof |
| CN109505132A (en) * | 2018-12-29 | 2019-03-22 | 湖南九华碳素高科有限公司 | It is a kind of for making the dipping method of carbon fiber hard composite felt |
| CN111016137B (en) * | 2019-12-24 | 2021-08-13 | 山东众途复合材料有限公司 | Method for preparing carbon fiber heat-insulating hard felt by using water-soluble phenolic resin as curing agent |
| CN111584151B (en) * | 2020-05-26 | 2021-10-01 | 杭州幄肯新材料科技有限公司 | Carbon fiber/carbon/graphite composite carbon felt and method for enhancing heat conduction and electric conduction performance of polymer composite material |
| CN111892417B (en) * | 2020-08-25 | 2021-05-14 | 内蒙古中晶科技研究院有限公司 | Carbon fiber composite material and preparation method thereof |
| CN113026349A (en) * | 2021-03-12 | 2021-06-25 | 上海瑟赫新材料科技有限公司 | Heat-preserving and heat-insulating carbon felt and preparation method thereof |
| CN113619216A (en) * | 2021-08-31 | 2021-11-09 | 南通大学 | Kapok felt, carbon cloth composite non-woven felt, needling reinforcing method and application |
| CN116892056B (en) * | 2023-08-07 | 2024-04-16 | 江苏超芯星半导体有限公司 | Thermal insulation structure for silicon carbide single crystal growth and manufacturing method and application thereof |
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