CN106145989A - A kind of preparation method of polycrystalline ingot furnace thermal field cover plate - Google Patents
A kind of preparation method of polycrystalline ingot furnace thermal field cover plate Download PDFInfo
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- CN106145989A CN106145989A CN201510136927.2A CN201510136927A CN106145989A CN 106145989 A CN106145989 A CN 106145989A CN 201510136927 A CN201510136927 A CN 201510136927A CN 106145989 A CN106145989 A CN 106145989A
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Abstract
The present invention provides the preparation method of a kind of polycrystalline ingot furnace thermal field cover plate, and the method comprises the following steps: (1) chooses carbon fiber, knitting forming, forms prefabricated carbon fiber body；(2) prefabricated carbon fiber body is put in resin impregnation liquid and impregnate；(3) hot-press solidifying, carbonization treatment will be carried out at goods；(4) will carry out densification at goods, high temperature purification processes；(5) coat of silicon carbide is prepared at product surface；(6) it is processed into product.The present invention is easy and simple to handle, good integrity, and during use, product is not stratified, does not ftractures, and service life is long.
Description
Technical field
The present invention relates to the preparation method of a kind of polycrystalline ingot furnace carbon/carbon (C/C) composite cover plate.
Background technology
C/C composite cover plate is widely used in the hot industry equipment such as polycrystalline silicon ingot or purifying furnace, and its performance directly affects silicon ingot matter
Amount, the energy consumption that hot industry equipment is run by its life-span and using effect, cost control etc. has pivotal role.Polycrystalline casting at present
The cover plate that ingot stove uses has graphite cover plate and C/C composite cover plate two kinds, and graphite cover plate is because its intrinsic fragility is in the process of use
In be easily broken off, and use and placement process in be intended to pay close attention to, be otherwise easily destroyed.C/C composite employs carbon
Fiber reinforcement, the shortcoming that cover plate avoids graphite cover plate to a certain extent.C/C composite cover plate is mainly carbon cloth layer at present
Cover clamp or carbon fiber felt acupuncture cover plate, carbon cloth laminated cover is not owing to having any fiber in Z-direction, thus easily causes layering to open
Split；And carbon fiber felt acupuncture cover plate introduces carbon fiber in Z-direction, but simultaneously because the carbon fiber that acupuncture makes in-plane is damaged
Hinder and make overall performance decrease.It addition, currently used cover plate does not the most provide coat of silicon carbide.This technology aims to provide
The C/C composite cover plate technology of preparing of a kind of novel carbon fiber braiding structure, saves the seriality of carbon fiber completely, and leads to
Crossing linking of the upper and lower interlayer of carbon fiber, it is entirely avoided the defect of fiber fractionation, meanwhile, the introducing of coat of silicon carbide also makes to produce
Product are obviously improved service life.
Summary of the invention
1. the preparation method of the hard felt of C/C complex material heat preservation, it is characterised in that: the method comprises the following steps:
(1) 6K or 12K carbon fiber is selected, knitting forming in the way of 2.5D shallow friendship direct connection, form prefabricated carbon fiber body；
(2) select phenolic resin as impregnating agent, prefabricated carbon fiber body is put in liquid phenolic resin and carry out vacuum impregnation；
(3) hot-press solidifying, carbonization treatment will be carried out at goods；During hot-press solidifying, the thickness reduction of prefabricated carbon fiber body should be controlled
System is between 10～20%；
(4) will carry out CVD densification at goods, high temperature purification processes；
(5) it is processed into product；
(6) steaming process is used to prepare coat of silicon carbide at product surface.
2. according to the method described in right 1, it is characterised in that: described carbon fiber is the fine base carbon fibre of polypropylene, uses east beautiful
T700 series or ad eundem product.
3. according to the method described in right 1, it is characterised in that: the bulk density of described prefabricated carbon fiber body is, 0.40～0.60
g/cm3。
4. according to the method described in right 1, it is characterised in that: described phenolic resin is the thermosetting phenolic resin of liquid, Gu
Content is 55～65%, and resin carbon yield is 45～60%.
5. according to the method described in right 1, it is characterised in that: solidification temperature is 130～160 DEG C, hardening time 1～5h；Carbonization
Temperature 700～900 DEG C, carbonization time 1～5h, heating rate≤25 DEG C in carbonisation/h.
6. according to the method described in right 1, it is characterised in that: use chemical vapor deposition method to carry out during densification, adopt
With methane, ethylene or propane etc. as carbon-source gas, use Ar gas as carrier gas, depositing temperature 900～1100 DEG C；Need at least 2
Secondary above CVD, until density reaches more than 1.4g/cm3.Need turn-over up and down during CVD, to ensure even density every time.
7. according to the method described in right 1, it is characterised in that: high temperature purification treatment temperature is 1900～2400 DEG C, processes the time
3～5h, heating rate≤100 DEG C/h.
8. according to the method described in right 1, it is characterised in that: use steaming process to use when product surface prepares coat of silicon carbide
Silica flour and silicon dioxide powder, mass ratio is Si powder: SiO2 powder=1: 1.5～2, and powder granule degree requires as all can pass through 100 mesh
Sieve, is layered on the bottom of graphite crucible after powder body mix homogeneously, it is 10～20mm that powder body sprawls thickness, and cover plate stands up, and is suspended on powder
Above body, cover plate distance from bottom powder body about 50～200mm.Temperature during preparation coating is 1600 ± 50 DEG C, is incubated 1～3h.
Effect of the invention is that:
(1) present invention is by using 2.5D shallow friendship direct connection knitting forming mode weaving carbon fiber precast body, thoroughly solves carbon
The problem of fiber fractionation cracking.And it has been sufficiently reserved long stapled advantage；
(2) early stage molding of the present invention uses liquid phase mould pressing process, can control the flat of product thickness and apparent condition easily
Whole property；
(3) present invention later stage densification uses gas-phase deposition, is only passed through hydrocarbon gas and lazy in chemical vapor deposition processes
Property gas, does not introduce any impurity, it is ensured that product purity from source；
(4) present invention introduces coat of silicon carbide in C/C composite lid surface, and this coating has been effectively isolated use process
The further erosion to material of the middle silicon steam, can significantly extend the service life of cover plate；
(5) present invention employs special formula and technique prepares coat of silicon carbide, low cost, coating result is good.
Accompanying drawing explanation
Fig. 1 is 2.5D shallow friendship direct connection knitting forming mode schematic diagram；
Detailed description of the invention
Below in conjunction with specific embodiment prepared by a kind of polycrystalline ingot furnace carbon/carbon (C/C) composite cover plate of the present invention
Method is further described in detail.
Embodiment 1
(1) the eastern beautiful fine base carbon fibre of T700-12K polypropylene is selected, knitting forming in the way of 2.5D shallow friendship direct connection, formed
Prefabricated carbon fiber body；Precast body density is 0.50g/cm3；Precast body a size of 1000 × 1000 × 10mm；
(2) select the thermosetting phenolic resin of solid content about 60% as impregnating agent, prefabricated carbon fiber body is put into Vaccum Permeating
In stain tank, suck phenolic resin after evacuation 30min, do not had precast body to resin completely；
(3) the prefabricated carbon fiber body impregnating resin is placed on flat-bed press carries out hot-press solidifying, solidification temperature 150
DEG C, hardening time 3h；Adjust daylight opening before solidification, precast body thickness is depressed into 8.5mm；
(4) solidification is completed in goods put into carbide furnace, carry out carbonization treatment, with the intensification of 20 DEG C/h speed during process
Rate is warming up to 800 DEG C, is then incubated 3h, and whole process is passed through Ar gas and protects；
(5) loading in CVD stove at goods of carbonization being completed carries out CVD densification, use methane as carbon-source gas,
Use Ar gas as carrier gas, depositing temperature 1100 DEG C, each sedimentation time 72h；More than at least 2 times CVD,
Processed test density, until density reaches 1.4g/cm every time3Above.Need to turn over up and down during CVD every time
Face, to ensure even density；
(6) being put into by the sample that densification completes and carry out high temperature purification process in high temperature graphitization stove, treatment temperature is 2000
DEG C, process time 4h, 80 DEG C/h of heating rate.Vacuum state in omnidistance holding furnace；
(7) sheet material after coming out of the stove is processed into product according to drawing；
(8) according to Si powder: SiO2 powder=1: the proportional arrangement mixed powder of 1.5, the cover plate loading after purifying prepares in advance
Good graphite crucible top, stands up；Being layered on the bottom of graphite crucible after powder body mix homogeneously, powder body sprawls thickness
For 10mm, cover plate stands up, and is suspended on above powder body, cover plate distance from bottom powder body 100mm.By charged earthenware
Crucible entirety is put into and is carried out coating in vacuum sintering furnace and prepare, and preparation temperature is 1600 DEG C, is incubated 2h, omnidistance logical
Enter Ar protection, in stove, keep normal pressure.
Embodiment 2
(1) the eastern beautiful fine base carbon fibre of T700-6K polypropylene is selected, knitting forming in the way of 2.5D shallow friendship direct connection, formed
Prefabricated carbon fiber body；Precast body density is 0.60g/cm3；Precast body a size of 1000 × 1000 × 10mm；
(2) select the thermosetting phenolic resin of solid content about 55% as impregnating agent, prefabricated carbon fiber body is put into Vaccum Permeating
In stain tank, suck phenolic resin after evacuation 30min, do not had precast body to resin completely；
(3) the prefabricated carbon fiber body impregnating resin is placed on flat-bed press carries out hot-press solidifying, solidification temperature 130
DEG C, hardening time 5h；Adjust daylight opening before solidification, precast body thickness is depressed into 9mm；
(4) solidification is completed in goods put into carbide furnace, carry out carbonization treatment, with the intensification of 25 DEG C/h speed during process
Rate is warming up to 900 DEG C, is then incubated 1h, and whole process is passed through Ar gas and protects；
(5) loading in CVD stove at goods of carbonization being completed carries out CVD densification, use ethylene as carbon-source gas,
Use Ar gas as carrier gas, depositing temperature 1000 DEG C, each sedimentation time 72h；More than at least 2 times CVD,
Processed test density, until density reaches 1.4g/cm every time3Above.Need to turn over up and down during CVD every time
Face, to ensure even density；
(6) being put into by the sample that densification completes and carry out high temperature purification process in high temperature graphitization stove, treatment temperature is 2400
DEG C, process time 3h, 100 DEG C/h of heating rate.Vacuum state in omnidistance holding furnace；
(7) sheet material after coming out of the stove is processed into product according to drawing；
(8) according to Si powder: SiO2 powder=1: the proportional arrangement mixed powder of 2, the cover plate loading after purifying is ready in advance
Graphite crucible top, stand up；Being layered on the bottom of graphite crucible after powder body mix homogeneously, powder body is sprawled thickness and is
20mm, cover plate stands up, and is suspended on above powder body, cover plate distance from bottom powder body 200mm.By charged crucible
Entirety is put into and is carried out coating in vacuum sintering furnace and prepare, and preparation temperature is 1650 DEG C, is incubated 1h, and whole process is passed through
Ar protects, and keeps normal pressure in stove.
Embodiment 3
(1) the eastern beautiful fine base carbon fibre of T700-12K polypropylene is selected, knitting forming in the way of 2.5D shallow friendship direct connection, formed
Prefabricated carbon fiber body；Precast body density is 0.40g/cm3；Precast body a size of 1000 × 1000 × 10mm；
(2) select the thermosetting phenolic resin of solid content about 65% as impregnating agent, prefabricated carbon fiber body is put into Vaccum Permeating
In stain tank, suck phenolic resin after evacuation 30min, do not had precast body to resin completely；
(3) the prefabricated carbon fiber body impregnating resin is placed on flat-bed press carries out hot-press solidifying, solidification temperature 160
DEG C, hardening time 1h；Adjust daylight opening before solidification, precast body thickness is depressed into 8mm；
(4) solidification is completed in goods put into carbide furnace, carry out carbonization treatment, with the intensification of 15 DEG C/h speed during process
Rate is warming up to 700 DEG C, is then incubated 5h, and whole process is passed through Ar gas and protects；
(5) loading in CVD stove at goods of carbonization being completed carries out CVD densification, use propane as carbon-source gas,
Use Ar gas as carrier gas, depositing temperature 900 DEG C, each sedimentation time 72h；More than at least 2 times CVD,
Processed test density, until density reaches 1.4g/cm every time3Above.Need to turn over up and down during CVD every time
Face, to ensure even density；
(6) being put into by the sample that densification completes and carry out high temperature purification process in high temperature graphitization stove, treatment temperature is 1900
DEG C, process time 5h, 60 DEG C/h of heating rate.Vacuum state in omnidistance holding furnace；
(7) sheet material after coming out of the stove is processed into product according to drawing；
(8) according to Si powder: SiO2 powder=1: the proportional arrangement mixed powder of 1.5, the cover plate loading after purifying prepares in advance
Good graphite crucible top, stands up；Being layered on the bottom of graphite crucible after powder body mix homogeneously, powder body sprawls thickness
For 10mm, cover plate stands up, and is suspended on above powder body, cover plate distance from bottom powder body 100mm.By charged earthenware
Crucible entirety is put into and is carried out coating in vacuum sintering furnace and prepare, and preparation temperature is 1550 DEG C, is incubated 3h, omnidistance logical
Enter Ar protection, in stove, keep normal pressure.
Claims (9)
1. the present invention provides the preparation method of a kind of polycrystalline ingot furnace thermal field cover plate, and the method comprises the following steps: (1) chooses carbon fiber, knitting forming, forms prefabricated carbon fiber body；(2) prefabricated carbon fiber body is put in resin impregnation liquid and impregnate；(3) hot-press solidifying, carbonization treatment will be carried out at goods；(4) will carry out densification at goods, high temperature purification processes；(5) coat of silicon carbide is being prepared at product surface；(6) it is processed into product.The present invention is easy and simple to handle, good integrity, and during use, product is not stratified, does not ftractures, and service life is long.
2. the preparation method of the hard felt of C/C complex material heat preservation, it is characterised in that: the method comprises the following steps:
(1) 6K or 12K carbon fiber is selected, knitting forming in the way of 2.5D shallow friendship direct connection, form prefabricated carbon fiber body；
(2) select phenolic resin as impregnating agent, prefabricated carbon fiber body is put in liquid phenolic resin and carry out vacuum impregnation；
(3) hot-press solidifying, carbonization treatment will be carried out at goods；During hot-press solidifying, the thickness reduction of prefabricated carbon fiber body should control between 10～20%.
(4) will carry out CVD densification at goods, high temperature purification processes；
(5) it is processed into product；
(6) steaming process is used to prepare coat of silicon carbide at product surface.
3. according to the method described in right 1, it is characterised in that: described carbon fiber is the fine base carbon fibre of polypropylene, uses eastern beautiful T700 series or ad eundem product.
4. according to the method described in right 1, it is characterised in that: the bulk density of described prefabricated carbon fiber body is, 0.40～0.60g/cm3。
5. according to the method described in right 1, it is characterised in that: described phenolic resin is the thermosetting phenolic resin of liquid, and solid content is 55～65%, and resin carbon yield is 45～60%.
6. according to the method described in right 1, it is characterised in that: solidification temperature is 130～160 DEG C, hardening time 1～5h；Carburizing temperature 700～900 DEG C, carbonization time 1～5h, heating rate≤25 DEG C in carbonisation/h.
7. according to the method described in right 1, it is characterised in that: use chemical vapor deposition method to carry out during densification, use methane, ethylene or propane etc. as carbon-source gas, use Ar gas as carrier gas, depositing temperature 900～1100 DEG C；Need more than at least 2 times CVD, until density reaches more than 1.4g/cm3.Need turn-over up and down during CVD, to ensure even density every time.
8. according to the method described in right 1, it is characterised in that: high temperature purification treatment temperature is 1900～2400 DEG C, processes time 3～5h, heating rate≤100 DEG C/h.
9. according to the method described in right 1, it is characterized in that: use steaming process to use silica flour and silicon dioxide powder when product surface prepares coat of silicon carbide, mass ratio is Si powder: SiO2 powder=1: 1.5～2, powder granule degree requires as all can pass through 100 mesh sieves, being layered on the bottom of graphite crucible after powder body mix homogeneously, it is 10～20mm that powder body sprawls thickness, and cover plate stands up, it is suspended on above powder body, cover plate distance from bottom powder body about 50～200mm.Temperature during preparation coating is 1600 ± 50 DEG C, is incubated 1～3h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107504325A (en) * | 2017-07-29 | 2017-12-22 | 南京航空航天大学 | A kind of preparation method of high temperature VIP composites |
| CN108409351A (en) * | 2018-03-26 | 2018-08-17 | 甘肃新西北碳素科技有限公司 | The carbon of high temperature-resistant acid-resistant liquid/carbon template quick molding method |
| CN109161961A (en) * | 2018-11-27 | 2019-01-08 | 晶科能源有限公司 | A kind of polycrystalline cast ingot crucible cover plate and preparation method thereof |
| CN111377754A (en) * | 2018-12-29 | 2020-07-07 | 洛阳阿特斯光伏科技有限公司 | Composite carbon cover plate for ingot furnace, and preparation method and application thereof |
| CN111996813A (en) * | 2020-08-27 | 2020-11-27 | 佛山市石金科技有限公司 | Coating of hard felt and preparation method thereof |
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| CN101905977A (en) * | 2010-08-04 | 2010-12-08 | 蒋建纯 | Method for manufacturing integral heater for carbon/carbon polycrystalline silicon ingot furnace |
| CN103193497A (en) * | 2013-04-07 | 2013-07-10 | 山东国晶新材料有限公司 | Sticky product with silicon erosion resistance of carbon/carbon composite material and preparation method thereof |
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| CN101905977A (en) * | 2010-08-04 | 2010-12-08 | 蒋建纯 | Method for manufacturing integral heater for carbon/carbon polycrystalline silicon ingot furnace |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107504325A (en) * | 2017-07-29 | 2017-12-22 | 南京航空航天大学 | A kind of preparation method of high temperature VIP composites |
| CN108409351A (en) * | 2018-03-26 | 2018-08-17 | 甘肃新西北碳素科技有限公司 | The carbon of high temperature-resistant acid-resistant liquid/carbon template quick molding method |
| CN109161961A (en) * | 2018-11-27 | 2019-01-08 | 晶科能源有限公司 | A kind of polycrystalline cast ingot crucible cover plate and preparation method thereof |
| CN111377754A (en) * | 2018-12-29 | 2020-07-07 | 洛阳阿特斯光伏科技有限公司 | Composite carbon cover plate for ingot furnace, and preparation method and application thereof |
| CN111377754B (en) * | 2018-12-29 | 2022-05-03 | 洛阳阿特斯光伏科技有限公司 | Composite carbon cover plate for ingot furnace, and preparation method and application thereof |
| CN111996813A (en) * | 2020-08-27 | 2020-11-27 | 佛山市石金科技有限公司 | Coating of hard felt and preparation method thereof |
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