CN106927802A - A kind of manufacture method for noting solidification forming fused silica crucible - Google Patents
A kind of manufacture method for noting solidification forming fused silica crucible Download PDFInfo
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- CN106927802A CN106927802A CN201710161949.3A CN201710161949A CN106927802A CN 106927802 A CN106927802 A CN 106927802A CN 201710161949 A CN201710161949 A CN 201710161949A CN 106927802 A CN106927802 A CN 106927802A
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- fused silica
- crucible
- microns
- manufacture method
- solidification forming
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 239000005350 fused silica glass Substances 0.000 title claims abstract description 30
- 238000007711 solidification Methods 0.000 title claims abstract description 27
- 230000008023 solidification Effects 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 239000004576 sand Substances 0.000 claims abstract description 48
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 27
- 239000010935 stainless steel Substances 0.000 claims abstract description 27
- 239000002002 slurry Substances 0.000 claims abstract description 22
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 6
- 238000004321 preservation Methods 0.000 claims abstract description 4
- 238000002347 injection Methods 0.000 claims description 16
- 239000007924 injection Substances 0.000 claims description 16
- 239000012298 atmosphere Substances 0.000 claims description 14
- 238000010304 firing Methods 0.000 claims description 13
- 238000005266 casting Methods 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000006255 coating slurry Substances 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 230000001590 oxidative effect Effects 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 230000003068 static effect Effects 0.000 claims description 7
- 230000032683 aging Effects 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 229920002635 polyurethane Polymers 0.000 claims description 6
- 239000004814 polyurethane Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000003638 chemical reducing agent Substances 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 2
- 238000007792 addition Methods 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 claims description 2
- 230000001070 adhesive effect Effects 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 2
- 229910017435 S2 In Inorganic materials 0.000 claims 1
- 229910052573 porcelain Inorganic materials 0.000 claims 1
- 239000000919 ceramic Substances 0.000 abstract description 13
- 238000005336 cracking Methods 0.000 abstract description 4
- 238000013467 fragmentation Methods 0.000 abstract description 4
- 238000006062 fragmentation reaction Methods 0.000 abstract description 4
- 238000001035 drying Methods 0.000 description 8
- 239000010410 layer Substances 0.000 description 7
- -1 na oxide Chemical compound 0.000 description 7
- 238000001514 detection method Methods 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 239000000395 magnesium oxide Substances 0.000 description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 5
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 5
- 229910001950 potassium oxide Inorganic materials 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 3
- 239000000292 calcium oxide Substances 0.000 description 3
- 238000007569 slipcasting Methods 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- ODLMAHJVESYWTB-UHFFFAOYSA-N propylbenzene Chemical compound CCCC1=CC=CC=C1 ODLMAHJVESYWTB-UHFFFAOYSA-N 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910052571 earthenware Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011505 plaster Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
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Abstract
The invention provides a kind of manufacture method for noting solidification forming fused silica crucible, comprise the following steps：Step S1, tekite sand, water, acrylamide and crosslinking agent are mixed and be sufficiently stirred for, obtain slurry；Step S2, tekite sand of the granularity within 30 microns is coated on the inner surface of stainless steel mould, then to pouring into a mould the slurry in the stainless steel mould；Step S3, the stainless steel mould after cast is placed in heat preservation solidification is carried out in baking oven, and the demoulding obtains crucible base substrate；Step S4, gained crucible base substrate is dried and burnt till successively, obtain noting solidification forming fused silica crucible.Coated tekite sand can sinter to form one layer of finer and close tekite sand ceramic layer, so as to improve the consistency and intensity of crucible outer surface, reduce crucible outer surface and be susceptible to cracking until the probability of fragmentation.
Description
Technical field
The present invention relates to the manufacturing technology field of fused silica crucible, and in particular to one kind note solidification forming fused silica crucible
Manufacture method.
Background technology
Fused quartz ceramic crucible is the easily-consumed products during polycrystalline silicon ingot casting, and every polycrystalline furnace needs ceramics side's earthenware every year
Crucible about 120.Domestic crucible demand~120,000 are annual within 07 year, and such as nearest 2 years of this year is in again explosive growth.Existing market
The mainstream technology injection forming (slipcasting) of upper fused silica crucible.Injection forming is traditional moulding process, its feature
It is product density (1.89-2.0g/cm high3), intensity is higher.But slip-casting shaping process has the shortcomings that cannot be overcome：1, note
The plaster mold quality of slurry is unstable, when have fluctuation so that influence crucible quality；2, the green strength of injection forming is low, and production is big
Size crucible difficulty is very big；3, injection forming structure is uneven, or even has interlayer, and intensity is relatively low；4 mould access times are limited,
Die cost is very high；5, burning till rear crucible bottom needs polishing, and cost is increased substantially；6, the requirement of forming temperature humidity etc. is very
It is high.Current 880 crucible is the market mainstream, but the even more big crucible of 1024 crucibles is the direction developed in the future.Injection forming into
It is very big that type does so large-scale crucible difficulty, highlights the limitation of slip casting method.
Note solidification forming (gelcasting) is new ceramic preparation technology, and the technique has that green strength is high, production week
Phase is short, can the remarkable advantage such as one-shot forming, producing large-scale fused silica crucible has unrivaled advantage.Domestic seldom factory
Family expenses note solidification forming prepares quartz ceramic crucible, and compared with the crucible of injection forming production, notes the crucible density of solidification forming
Relatively low (about 1.80g/cm3), too low density has a strong impact on to the performance of crucible.Particularly in use, outside crucible
Surface is because of contact high temperature action so that crucible outer surface is susceptible to cracking, until fragmentation.
The content of the invention
Therefore, the technical problem to be solved in the present invention is to overcome crucible outer surface to be in the prior art susceptible to cracking directly
To the defect of fragmentation.
Therefore, the invention provides a kind of manufacture method for noting solidification forming fused silica crucible, comprising the following steps：Step
S1, tekite sand, water, acrylamide and crosslinking agent are mixed and be sufficiently stirred for, obtain slurry；Step S2, in stainless steel mold
Coat tekite sand of the granularity within 30 microns on the inner surface of tool, then to pouring into a mould the slurry in the stainless steel mould
Material；Step S3, the stainless steel mould after cast is placed in heat preservation solidification is carried out in baking oven, and the demoulding obtains crucible base substrate；Step
S4, gained crucible base substrate is dried and burnt till successively, obtain noting solidification forming fused silica crucible.
Preferably, step S1 includes：By the grinding, granularity control of being added water in 40-50 parts of block tekite sand input grinder
System is within 30 microns；After above-mentioned slurry is aged 10 days, then to material by middle 50~100 microns of granularity of 20-25 parts of addition, 25-35
Part granularity is 250~350 microns of tekite sand, is subsequently adding acrylamide, crosslinking agent and is sufficiently stirred for until slurry temperature
Reach 30~45 degrees Celsius.
Preferably, in step S2, froth in vacuum, then pressure injection stainless steel mould are first carried out to slurry, while being aided with shake
Dynamic, vibration frequency is 20~40 beats/min, amplitude~3 millimeter, static 15~30 minutes after casting complete.
Preferably, in step S3, in the baking oven the stainless steel mould after cast as 40~100 degree, insulation 1~5 is small
When.
Preferably, in step S4, first dried 1~12 hour in the environment of humidity is more than 80% after the demoulding, then 100
Dried 20~30 hours in~200 degree of baking oven；Dried green compact are put into kiln to burn till, 6 are first protected in oxidizing atmosphere
~10 hours, then in reducing atmosphere protect 5~50 hours, 1000~1300 degree of firing temperature, firing time be 15~56
Hour, gained crucible is fused quartz ceramic crucible.
Preferably, granularity is coated on the inner surface of stainless steel mould to be wrapped the step of the tekite sand within 30 microns
Include：Tekite sand and organic coat solvent by granularity within 30 microns are well mixed, and obtain coating slurry；By coating materials
On material coating to the inner surface of stainless steel mould.
Preferably, the thickness that coating forms vitreous silica layer of sand on the inner surface of stainless steel mould is 5-30mm.
Preferably, tekite sand and organic coat solvent of the granularity within 30 microns are according to volume ratio 1:5-1：15 mix
Close.
Preferably, the organic coat solvent is polyurethane-coated agent or acrylate adhesive.
Preferably, in the step of obtaining coating slurry, the tekite sand, organic coat by granularity within 30 microns are molten
Agent and organic water reducer are according to volume ratio 1:5-15：0.1-0.5 is well mixed.
Technical solution of the present invention, has the following advantages that：
The manufacture method of the note solidification forming fused silica crucible that the present invention is provided, coats on the inner surface of stainless steel mould
Tekite sand of the granularity within 30 microns, then to pouring into a mould slurry in the stainless steel mould, slurry reclaimed water, acrylamide and
Crosslinking agent can spread and disperse to coated tekite sand, then after follow-up cast, heat preservation solidification, drying and burning till, institute
Coating tekite sand can sinter to form one layer of finer and close tekite sand ceramic layer, so as to improve crucible outer surface
Consistency and intensity, reduce crucible outer surface and are susceptible to cracking until the probability of fragmentation.
This technique has been captured note solidification forming and has prepared the relatively low problem of quartz ceramic crucible density, the density of products obtained therefrom
1.88-1.99g/cm3, the consistent in density with injection forming gained crucible.Technique has following features in terms of comprehensive：1st, green compact are strong
Degree is high, and qualification rate is high；2nd, the density of crucible is high, with injection forming gained crucible consistent in density；3rd, convenient, molding cycle is poured into a mould
It is short；4th, one-shot forming, without crossing multi-processing, therefore cost is far below injection forming；5th, even structure, intensity are high；6th, produce large-scale
Crucible (1024mm and dimensions above) has unrivaled advantage；7th, less investment, instant effect, risk are low, with injection forming phase
Than either place or equipment are all few a lot.
Specific embodiment
Technical scheme will be clearly and completely described below, it is clear that described embodiment is this hair
Bright a part of embodiment, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not having
There is the every other embodiment made and being obtained under the premise of creative work, belong to the scope of protection of the invention.
Case 1
Tekite sand and polyurethane-coated agent by granularity within 25 microns is according to volume ratio 1:5 mixing, will coat
Slurry is coated to the inner surface of stainless steel mould, and the thickness for forming vitreous silica layer of sand is 30mm.
By 50 parts of block glass sands, (mass percent of its component is：Silica ＞ 99.75%, iron oxide ＜
38ppm, aluminum oxide ＜ 950ppm, other are inevitable impurity, such as potassium oxide, na oxide, magnesium oxide or calcium oxygen
Compound etc.) input ball mill in carry out wet ball grinding, size controlling within 10 microns, ageing 8 days after add 60 microns,
Each 25 parts of 220 microns of high-purity tekite sand, is subsequently adding acrylamide monomer, cumyl peroxide crosslinking agent abundant
Stirring, is sufficiently stirred for reaching 35 degrees Celsius, after physical and chemical index detection is qualified up to slurry temperature, and pressure injection is applied after froth in vacuum
Being covered with tekite sand of the granularity within 25 microns has stainless steel mould, while being aided with slight vibrations, 30 beats/min of vibration frequency
Clock, 3 millimeters of amplitude.Static 20 minutes after casting complete.After 50 degrees Celsius of drying rooms are placed 5 hours, the demoulding is taken out, green compact exist
Humidity is dried 10 hours in the environment of being more than 80%, is then dried 25 hours in the environment of 200 degrees Celsius.By dried life
Base is put into kiln and burns till, and first protects 8 hours, then protection of reducing atmosphere 45 hours in oxidizing atmosphere.1100 degree of firing temperature, burns
It it is 55 hours into the time, gained crucible is fused quartz ceramic crucible sample 1.
Embodiment 2
Tekite sand and polyurethane-coated agent by granularity within 25 microns is according to volume ratio 1：15 mixing, will coat
Slurry is coated to the inner surface of stainless steel mould, and the thickness for forming vitreous silica layer of sand is 5mm.
By 45 parts of block glass sands, (mass percent of its component is：Silica ＞ 99.8%, iron oxide ＜
25ppm, aluminum oxide ＜ 400ppm, other are inevitable impurity, such as potassium oxide, na oxide, magnesium oxide or calcium oxygen
Compound etc.) input ball mill in carry out wet ball grinding, size controlling within 20 microns, ageing 10 days after add 20 parts 80 microns
High-purity tekite sand, 35 parts 300 microns of high-purity tekite sand, be subsequently adding acrylamide monomer, peroxidating two different
Propyl benzene crosslinking agent is sufficiently stirred for, and is sufficiently stirred for reaching 40 degrees Celsius up to slurry temperature, and after physical and chemical index detection is qualified, vacuum is removed
Pressure injection is coated with tekite sand of the granularity within 25 microns after bubble stainless steel mould, while it is aided with slight vibrations,
38 beats/min of vibration frequency, 5 millimeters of amplitude.Static 25 minutes after casting complete.Then it is small in 80 degrees Celsius of drying room placement 3
Shi Hou, takes out the demoulding, and green compact are dried 6 hours in the environment of humidity is more than 80%, then done in the environment of 180 degrees Celsius
Dry 21 hours.Dried green compact are put into kiln to burn till, first 10 hours, then protection of reducing atmosphere 30 is protected in oxidizing atmosphere
Hour.1200 degree of firing temperature, firing time is 30 hours, and gained crucible is fused quartz ceramic crucible sample 2.
Case 3
Tekite sand, polyurethane-coated agent, polypropylene phthalein amine water reducer by granularity within 25 microns is according to volume
Than 1:10：0.1 mixing, coating slurry is coated to the inner surface of stainless steel mould, forms the thickness of vitreous silica layer of sand
It is 20mm.
By 40 parts of block glass sands, (mass percent of its component is：Silica ＞ 99.95%, aluminum oxide ＜
10ppm, other are inevitable impurity, such as potassium oxide, na oxide, magnesium oxide or calcium oxide) input ball milling
Wet ball grinding is carried out in machine, within 25 microns, ageing adds 25 parts 90 microns of high-purity vitreous silica to size controlling after 12 days
Sand, 35 parts 330 microns of high-purity tekite sand, are subsequently adding acrylamide monomer, cumyl peroxide crosslinking agent abundant
Stirring, is sufficiently stirred for reaching 45 degrees Celsius, after physical and chemical index detection is qualified up to slurry temperature, and pressure injection is applied after froth in vacuum
Being covered with tekite sand of the granularity within 25 microns has stainless steel mould, while being aided with slight vibrations, 25 beats/min of vibration frequency
Clock, 2 millimeters of amplitude.Static 15 minutes after casting complete.Then after 100 degrees Celsius of drying room is placed 2 hours, the demoulding is taken out,
Green compact are dried 3 hours in the environment of humidity is more than 80%, are then dried 28 hours in the environment of 120 degrees Celsius.By drying
Green compact afterwards are put into kiln and burn till, and first protect 6 hours, then protection of reducing atmosphere 10 hours in oxidizing atmosphere.Firing temperature
1200 degree, firing time is 30 hours, and gained crucible is fused quartz ceramic crucible sample 3.
Case 4
Tekite sand, polyurethane-coated agent, polypropylene phthalein amine water reducer by granularity within 25 microns is according to volume
Than 1:10：0.5 mixing, coating slurry is coated to the inner surface of stainless steel mould, forms the thickness of vitreous silica layer of sand
It is 20mm.
By 40 parts of block glass sands, (mass percent of its component is：Silica ＞ 99.95%, aluminum oxide ＜
10ppm, other are inevitable impurity, such as potassium oxide, na oxide, magnesium oxide or calcium oxide) input ball milling
Wet ball grinding is carried out in machine, within 25 microns, ageing adds 25 parts 90 microns of high-purity vitreous silica to size controlling after 12 days
Sand, 35 parts 330 microns of high-purity tekite sand, are subsequently adding acrylamide monomer, cumyl peroxide crosslinking agent abundant
Stirring, is sufficiently stirred for reaching 45 degrees Celsius, after physical and chemical index detection is qualified up to slurry temperature, and pressure injection is applied after froth in vacuum
Being covered with tekite sand of the granularity within 25 microns has stainless steel mould, while being aided with slight vibrations, 25 beats/min of vibration frequency
Clock, 2 millimeters of amplitude.Static 15 minutes after casting complete.Then after 100 degrees Celsius of drying room is placed 2 hours, the demoulding is taken out,
Green compact are dried 3 hours in the environment of humidity is more than 80%, are then dried 28 hours in the environment of 120 degrees Celsius.By drying
Green compact afterwards are put into kiln and burn till, and first protect 6 hours, then protection of reducing atmosphere 10 hours in oxidizing atmosphere.Firing temperature
1200 degree, firing time is 30 hours, and gained crucible is fused quartz ceramic crucible sample 4.
Comparative example
By 40 parts of block glass sands, (mass percent of its component is：Silica ＞ 99.95%, aluminum oxide ＜
10ppm, other are inevitable impurity, such as potassium oxide, na oxide, magnesium oxide or calcium oxide) input ball milling
Wet ball grinding is carried out in machine, within 25 microns, ageing adds 25 parts 90 microns of high-purity vitreous silica to size controlling after 12 days
Sand, 35 parts 330 microns of high-purity tekite sand, are subsequently adding acrylamide monomer, cumyl peroxide crosslinking agent abundant
Stirring, is sufficiently stirred for reaching 45 degrees Celsius, after physical and chemical index detection is qualified up to slurry temperature, and pressure injects not after froth in vacuum
Rust steel mold (being not coated with tekite sand of the granularity within 25 microns), while be aided with slight vibrations, vibration frequency 25 times/
Minute, 2 millimeters of amplitude.Static 15 minutes after casting complete.Then after 100 degrees Celsius of drying room is placed 2 hours, take out de-
Mould, green compact are dried 3 hours in the environment of humidity is more than 80%, are then dried 28 hours in the environment of 120 degrees Celsius.Will be dry
Green compact after dry are put into kiln and burn till, and first protect 6 hours, then protection of reducing atmosphere 10 hours in oxidizing atmosphere.Firing temperature
1200 degree, firing time is 30 hours, and gained crucible is fused quartz ceramic crucible sample 5.
Performance detection is carried out to above-mentioned silica crucible product, its main performance index is shown in Table 1.
Table 1
Obviously, above-described embodiment is only intended to clearly illustrate example, and not to the restriction of implementation method.It is right
For those of ordinary skill in the art, can also make on the basis of the above description other multi-forms change or
Change.There is no need and unable to be exhaustive to all of implementation method.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (10)
1. it is a kind of note solidification forming fused silica crucible manufacture method, it is characterised in that comprise the following steps：
Step S1, tekite sand, water, acrylamide and crosslinking agent are mixed and be sufficiently stirred for, obtain slurry；
Step S2, tekite sand of the granularity within 30 microns is coated on the inner surface of stainless steel mould, then to it is described not
The cast slurry in rust steel mold；
Step S3, the stainless steel mould after cast is placed in heat preservation solidification is carried out in baking oven, and the demoulding obtains crucible base substrate；
Step S4, gained crucible base substrate is dried and burnt till successively, obtain noting solidification forming fused silica crucible.
2. it is according to claim 1 it is a kind of note solidification forming fused silica crucible manufacture method, it is characterised in that step S1
Including：
By the grinding that added water in 40-50 parts of block tekite sand input grinder, Task-size Controlling is within 30 microns；Above-mentioned slurry
After ageing 10 days, then middle 50~100 microns of granularity of 20-25 parts of additions, 25-35 parts of granularity are 250~350 microns to material melt
Fused silica sand, is subsequently adding acrylamide, crosslinking agent and is sufficiently stirred for until slurry temperature reaches 30~45 degrees Celsius.
3. it is according to claim 2 it is a kind of note solidification forming fused silica crucible manufacture method, it is characterised in that step S2
In, first carry out froth in vacuum to slurry, then pressure injection stainless steel mould, while be aided with vibrations, vibration frequency for 20~40 times/
Minute, amplitude~3 millimeter, static 15~30 minutes after casting complete.
4. it is according to claim 3 it is a kind of note solidification forming fused silica crucible manufacture method, it is characterised in that step S3
In, in the baking oven the stainless steel mould after cast as 40~100 degree, it is incubated 1~5 hour.
5. it is according to claim 4 it is a kind of note solidification forming fused silica crucible manufacture method, it is characterised in that step S4
In, first dried 1~12 hour in the environment of humidity is more than 80% after the demoulding, 20 are then dried in 100~200 degree of baking oven
~30 hours；
Dried green compact are put into kiln to burn till, 6~10 hours, the then guarantor in reducing atmosphere are first protected in oxidizing atmosphere
Shield 5~50 hours, 1000~1300 degree of firing temperature, firing time is 15~56 hours, and gained crucible is vitreous silica pottery
Porcelain crucible.
6. it is according to any one of claim 1 to 5 it is a kind of note solidification forming fused silica crucible manufacture method, its feature
It is that granularity is coated on the inner surface of stainless steel mould to be included the step of the tekite sand within 30 microns：
Tekite sand and organic coat solvent by granularity within 30 microns are well mixed, and obtain coating slurry；
Coating slurry is coated to the inner surface of stainless steel mould.
7. it is according to claim 6 it is a kind of note solidification forming fused silica crucible manufacture method, it is characterised in that stainless
The thickness that coating forms vitreous silica layer of sand on the inner surface of steel mold is 5-30mm.
8. it is according to claim 6 it is a kind of note solidification forming fused silica crucible manufacture method, it is characterised in that granularity exists
Tekite sand and organic coat solvent within 30 microns is according to volume ratio 1:5-1：15 mixing.
9. it is according to claim 6 it is a kind of note solidification forming fused silica crucible manufacture method, it is characterised in that it is described to have
Machine coating solvent is polyurethane-coated agent or acrylate adhesive.
10. it is according to claim 6 it is a kind of note solidification forming fused silica crucible manufacture method, it is characterised in that obtain
In the step of coating slurry, tekite sand, organic coat solvent and organic water reducer by granularity within 30 microns according to
Volume ratio 1:5-15：0.1-0.5 is well mixed.
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| CN109020523B (en) * | 2018-07-27 | 2022-01-21 | 东海县太阳光新能源有限公司 | Preparation method of low-iron ultra-white fused quartz ceramic crucible |
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| CN115108841A (en) * | 2021-03-23 | 2022-09-27 | 新沂市中鑫光电科技有限公司 | Heat treatment method for high-strength quartz crucible |
| CN113321405A (en) * | 2021-05-12 | 2021-08-31 | 陈富伦 | High-purity opaque quartz glass, manufacturing method and application thereof |
| CN114014641A (en) * | 2021-11-26 | 2022-02-08 | 徐州康纳高新材料科技有限公司 | Method for forming fused quartz ceramic by low-toxicity gel system gel injection |
| CN114133256A (en) * | 2021-12-30 | 2022-03-04 | 辽宁省轻工科学研究院有限公司 | Ceramic crucible matched with intermediate frequency furnace and preparation method thereof |
| CN115231910A (en) * | 2022-07-20 | 2022-10-25 | 徐州协鑫太阳能材料有限公司 | Method for manufacturing special-shaped high-purity silica brick |
| CN116813318A (en) * | 2023-04-24 | 2023-09-29 | 江苏锡沂高新材料产业技术研究院有限公司 | Preparation method of dynamic gel injection molding fused quartz ceramic biscuit |
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