CN104803610A - Manufacturing method of highly pure spray-free fused quartz crucible for polysilicon ingot casting - Google Patents
Manufacturing method of highly pure spray-free fused quartz crucible for polysilicon ingot casting Download PDFInfo
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- CN104803610A CN104803610A CN201410038257.6A CN201410038257A CN104803610A CN 104803610 A CN104803610 A CN 104803610A CN 201410038257 A CN201410038257 A CN 201410038257A CN 104803610 A CN104803610 A CN 104803610A
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Abstract
The invention discloses a manufacturing method of a highly pure spray-free fused quartz crucible for polysilicon ingot casting. The method comprises the following steps: carrying out ball milling on highly pure fused quartz raw materials to realize wet granulation, fully stirring a slip, adding the above obtained powdery highly pure fused quartz raw materials, uniformly mixing, injecting the above obtained mixture into a gypsum mould, and carrying out full dehydration molding, and demolding; drying the above obtained demolded green body at a temperature of below 180DEG C to obtain a blank; carrying out polishing and cleaning pretreatment on the blank; spraying the inner wall of the blank with 150-300 mesh quartz sand; spraying the internal surface of the blank with a silicon nitride coating layer with the thickness of 0.2-0.7mm; and sintering the blank sprayed with the silicon nitride coating layer in a shuttle kiln at 1000-1300DEG C for 14-24h. Compared with the prior art, the method disclosed in the invention has the advantages of production cycle shortening, production technology simplification, great reduction of the energy consumption, and increase of the production efficiency, the yield, the photoelectric conversion efficiency and the enterprise's economic benefit.
Description
Technical field
The invention belongs to quartz crucible and manufacture field, be specifically related to a kind of high-purity manufacture method exempting from spraying molten quartz crucible for polycrystalline silicon ingot casting.
Background technology
The fast development of solar energy polycrystalline silicon, accelerates the researchdevelopment of the fused silica crucible that polysilicon melting ingot casting uses greatly.Due to the problem of crucible yield rate in industry, the quartz crucible produced at present does not spray mostly, user is must provide spraying equipment for oneself with during this crucible, spray one deck silicon nitride coating in finished product crucible inside, then more than 1000 DEG C, sintering could start to load pure silicon material for more than 24 hours and uses.Market also has and exempts from sputtered quartz crucible on a small quantity, but this just continues spray and sinter after crucible is produced, technique does not change, and this explained hereafter cycle is long, consumes energy huge.Polishing operation in existing crucible production is carried out after crucible sintering, because the crucible hardness after sintering is very high, causes the requirement of equipment and grinding tool also high, and need in bruting process to cool with a large amount of water.In addition with the common silicon ingot of exempting from spraying molten quartz crucible and being difficult to produce high conversion efficiency.
Summary of the invention
The object of the invention is to solve the problem, a kind of high-purity manufacture method exempting from spraying molten quartz crucible for polycrystalline silicon ingot casting is provided, this method can make the production cycle of quartz crucible shorten, simplify the technique that client uses crucible, greatly reduce energy consumption, improve crucible yield rate, improve the efficiency of conversion of silicon ingot simultaneously.
Object of the present invention can be reached by following measures:
A kind of high-purity manufacture method exempting from spraying molten quartz crucible for polycrystalline silicon ingot casting: to exempt from spraying molten quartz crucible blank polishing, after cleaning pretreatment, after first spraying 150 ~ 300 object high-purity ground quartzs on this blank internal surface, again at the silicon nitride coating of the internal surface spraying 0.2 ~ 0.7mm of blank, finally this blank is sintered 14 ~ 24 hours in shuttle kiln at 1000 ~ 1300 DEG C, to obtain final product.
Must spray high purity quartz bisque in silicon nitride coating in present method, the particle diameter of the high-purity ground quartz adopted is preferably 150 ~ 300 orders, most preferably 200 orders.The thickness of this high purity quartz bisque is 1-3mm.
Invention further provides more specifically for high-purity manufacture method exempting from spraying molten quartz crucible of polycrystalline silicon ingot casting, it comprises the steps:
(1) bulk and granular high-purity fused quartz raw material are carried out wet granulation by ball milling together, the slip particle diameter after grinding is 10 μm ~ 50 μm;
(2) after slip fully being stirred, then add the high-purity fused quartz raw material of powdery and mix, then inject gypsum mold and carry out sufficient dehydration forming, the demoulding;
(3) base substrate after the demoulding carries out drying below 180 DEG C, obtained blank;
(4) blank is polished, cleaning pretreatment;
(5) at blank inner-wall spraying 150 ~ 300 object high-purity ground quartz;
(6) at the silicon nitride coating of blank internal surface spraying 0.2 ~ 0.7mm;
(7) blank being sprayed with silicon nitride coating is sintered 14 ~ 24 hours in shuttle kiln at 1000 ~ 1300 DEG C.
High-purity fused quartz raw material of the present invention, its purity is generally more than 99.9%.Present method can obtain high-purityly exempting from spraying molten quartz crucible.
In step (1), the mass ratio of block high-purity fused quartz raw material and granular high-purity fused quartz raw material is 25 ~ 30:70 ~ 75, the particle diameter of the high-purity fused quartz raw material of described bulk is 20 ~ 60nm, and the particle diameter of described granular high-purity fused quartz raw material is 5 ~ 20nm.
The water of two kinds of high-purity fused quartz raw materials quality 20 ~ 30% is added in wet granulation processes in step (1).
Described in the high-purity fused quartz raw material of powdery and step (1), the mass ratio of slip is 30 ~ 40:70 ~ 60, and the high-purity fused quartz raw material particle size of described powdery is 50 ~ 200 orders.
In step (2), slip fully stirs more than 72 hours before adding the high-purity fused quartz raw material of powdery, is preferably 72 ~ 200 hours, more preferably 100 ~ 170 hours.The dehydration forming time in this step is generally 5 ~ 20 hours, is preferably 10 ~ 15 hours.
In step (3), drying temperature is preferably 100 ~ 180 DEG C.
Pre-treatment in step (4) comprises polishes and cleaning to base substrate, and bruting process particularly adopts bottom grinder buffing blank, and this bruting process generally only needs 5 ~ 25 minutes; Cleaning course is clean blank internal surface particularly.
Described in step (5), quartz sand particle size is 150 ~ 300 orders, and the size of this silica powder particle is preferably 200 orders.
Described in step (6), silicon nitride coating is the Si3N4 aqueous solution of 20 ~ 25wt%, and the thickness of this silicon nitride coating is preferably 0.5mm.
The quartz crucible that ultrasonic flaw detection or X-ray examination can be adopted to sinter after step (7) terminates, detects yield rate and other performances of crucible.
Polishing step, on the basis of existing technique, is carried to blank pre-treatment from finished product aftertreatment, is not only greatly reduced intractability by present method, and decreases treatment facility and materials consumption.This law overcomes the restriction will be coated with after silicon nitride because yield rate is low, blank sintering and silicon nitride coating preparation are united two into one, under the cooperation of other steps, not only simplify technical process, more considerably reduce energy consumption and equipment investment, also improve the preparation yield rate of crucible, make yield rate be increased to 70 ~ 75% from about 60%.Turn improve the efficiency of conversion of prepared silicon ingot simultaneously, make efficiency of conversion be increased to 17.5% from about 17%.
Compared with method of the present invention sprays crucible with nothing, because the sintering of the sintering in being produced by crucible and silicon nitride coating unites two into one, shorten the production cycle, comparatively, shorten 30%; Simplify the production technique of client, improve the production efficiency of client; Improve the economic benefit of yield rate, finished product photoelectric transformation efficiency and enterprise.
Present method is exempted to spray compared with crucible with existing, greatly reduces energy consumption, than front saving more than 40%.
Present method is exempted to spray compared with crucible with existing, substantially increases the photoelectric transformation efficiency of prepared silicon ingot.
This technique, compared with existing technique, is carried out bottom grinding pre-treatment in advance and has been stopped the waste of water resources, reduce intractability, also improve the utilization ratio of raw material.
Embodiment
Embodiment 1
Granular high-purity fused quartz raw material of to be bulk high-purity fused quartz raw material of 50 ~ 60mm and 750kg particle diameter by 250kg particle diameter be 10 ~ 20mm (mass component of block and granular high-purity fused quartz raw material: silicon-dioxide >99.9%, aluminum oxide <2000ppm, ferric oxide <50ppm, sodium oxide <50ppm, other component is inevitable impurity in raw material; Lower same), drop into the water adding 250kg in ball mill and carry out wet grinding, the slip size controlling after grinding is at 10 μm ~ 30 μm.
Carry out stirring 120 hours after slip being derived ball mill, check physics and the chemical property of slip; The dry powder (the high-purity fused quartz raw material of 100 order powdery) adding 673kg more fully stirs; Proceed to pouring can after stirring and inject gypsum mold, leave standstill in a mold and carry out the demoulding after 10 hours.
Crucible blank after the demoulding carries out drying, and drying temperature controls at 140 DEG C.
Carry out bottom polishing to dried blank, the polishing time is 15 minutes.
Inner surface of crucible after clean polishing.
Crucible internal walls after the cleaning sprays one deck 150 order, and thickness is the high-purity ground quartz of 2mm.
Silicon nitride coating (the Si of 21wt% of one deck 0.3mm thickness is sprayed at inner surface of crucible
3n
4the aqueous solution).
Crucible blank after spraying is good is put into shuttle kiln and is sintered, and the temperature of sintering controls at 1200 DEG C, and sintering time is 20 hours.
With the quartz crucible that ultrasonic flaw detection or X-ray examination sinter, removing substandard products, obtain and of the present inventionly high-purityly exempt from spraying molten quartz crucible.
Learn through Performance Detection: what the present embodiment obtained high-purityly exempts from spraying molten quartz crucible, and yield rate is 70% ~ 75%, silicon ingot efficiency of conversion 17.5%, and its room temperature flexural intensity is at more than 17MPa, and volume density is 1.85 ~ 1.98g/cm
3, true density is 2.16 ~ 2.23g/cm
3, coefficient of linear expansion is 0.6 × 10
-6/ DEG C, void content is 11% ~ 14%.
Embodiment 2
Granular high-purity fused quartz raw material of to be bulk high-purity fused quartz raw material of 40 ~ 50mm and 700kg particle diameter by 300kg particle diameter be 10 ~ 15mm, drop into the water adding 250kg in ball mill and carry out wet grinding, the slip size controlling after grinding is at 10 μm ~ 50 μm.
Carry out stirring 168 hours after slip being derived ball mill, check physics and the chemical property of slip; The dry powder (the high-purity fused quartz raw material of 100 order powdery) adding 680kg more fully stirs; Proceed to pouring can after stirring and inject gypsum mold, leave standstill in a mold and carry out the demoulding after 15 hours.
Crucible blank after the demoulding carries out drying, and drying temperature controls at 100 DEG C.
Carry out bottom polishing to dried blank, the polishing time is 15 minutes.
Inner surface of crucible after clean polishing.
Crucible internal walls after the cleaning sprays one deck 200 order, and thickness is the high-purity ground quartz of 2mm.
Silicon nitride coating (the Si of 22wt% of one deck 0.5mm thickness is sprayed at inner surface of crucible
3n
4the aqueous solution).
Crucible blank after spraying is good is put into shuttle kiln and is sintered, and the temperature of sintering controls at 1300 DEG C, and sintering time is 24 hours.
With the quartz crucible that ultrasonic flaw detection or X-ray examination sinter, obtain and of the present inventionly high-purityly exempt from spraying molten quartz crucible.
Learn through Performance Detection: high-purity fused silica crucible that the present embodiment obtains, yield rate is 71% ~ 75%, silicon ingot efficiency of conversion 17.5%, and its room temperature flexural intensity is at more than 17MPa, and volume density is 1.85 ~ 1.98g/cm
3, true density is 2.16 ~ 2.23g/cm
3, coefficient of linear expansion is 0.6 × 10
-6/ DEG C, void content is 11% ~ 14%.
Efficiency of conversion is tested
Except not spraying except high-purity ground quartz in silicon nitride coating, other all prepare quartz crucible by the method for embodiment 1 and 2, obtain quartz crucible 1 and quartz crucible 2 respectively.
Respectively by embodiment 1 and 2, and quartz crucible 1 and quartz crucible 2, by the G5 explained hereafter silicon ingot of U.S. GT ingot furnace, adopt PL technological method to measure its average light photoelectric transformation efficiency to obtained silicon ingot, result is as follows:
| Crucible | Embodiment 1 | Embodiment 2 | Quartz crucible 1 | Quartz crucible 2 |
| Photoelectric transformation efficiency | 17.5% | 17.5% | 17% | 17% |
Claims (10)
1. the high-purity manufacture method exempting from spraying molten quartz crucible for polycrystalline silicon ingot casting, it is characterized in that: to exempt from spraying molten quartz crucible blank polishing, after cleaning pretreatment, after first spraying 150 ~ 300 object high-purity ground quartzs on this blank internal surface, again at the silicon nitride coating of the internal surface spraying 0.2 ~ 0.7mm of blank, finally this blank is sintered 14 ~ 24 hours in shuttle kiln at 1000 ~ 1300 DEG C, to obtain final product.
2. method according to claim 1, the particle diameter that it is characterized in that stating high-purity ground quartz is 150 ~ 300 orders, and the thickness of the high purity quartz bisque obtained after spraying high-purity ground quartz is 1-3mm.
3. method according to claim 1, is characterized in that described the method comprises the steps:
(1) bulk and granular high-purity fused quartz raw material are carried out wet granulation by ball milling together, the slip particle diameter after grinding is 10 μm ~ 50 μm;
(2) after slip fully being stirred, then add the high-purity fused quartz raw material of powdery and mix, then inject gypsum mold and carry out sufficient dehydration forming, the demoulding;
(3) base substrate after the demoulding carries out drying below 180 DEG C, obtained blank;
(4) described blank is polished, cleaning pretreatment;
(5) 150 ~ 300 object high-purity ground quartzs are sprayed at described blank inwall;
(6) at the silicon nitride coating of blank internal surface spraying 0.2 ~ 0.7mm;
(7) blank being sprayed with silicon nitride coating is sintered 14 ~ 24 hours in shuttle kiln at 1000 ~ 1300 DEG C.
4. method according to claim 1, is characterized in that described silicon nitride coating is the Si3N4 aqueous solution of 20 ~ 25wt%.
5. method according to claim 1, is characterized in that: in step (4), bruting process is for adopting bottom grinder buffing blank, and cleaning course is clean blank internal surface.
6. method according to claim 1, it is characterized in that: the mass ratio of described bulk high-purity fused quartz raw material and granular high-purity fused quartz raw material is 25 ~ 30:70 ~ 75, the particle diameter of the high-purity fused quartz raw material of described bulk is 20 ~ 60nm, and the particle diameter of described granular high-purity fused quartz raw material is 5 ~ 20nm.
7. method according to claim 1, is characterized in that: the water adding high-purity fused quartz raw materials quality 20 ~ 30% in step (1) in wet granulation processes.
8. method according to claim 1, is characterized in that: described in the high-purity fused quartz raw material of described powdery and step (1), the mass ratio of slip is 30 ~ 40:70 ~ 60, and the high-purity fused quartz raw material particle size of described powdery is 50 ~ 200 orders.
9. method according to claim 1, is characterized in that: in step (2), slip fully stirs more than 72 hours before adding the high-purity fused quartz raw material of powdery.
10. method according to claim 1, is characterized in that: in step (2), the time of dehydration forming is 5 ~ 20 hours; In step (3), drying temperature is 100 ~ 180 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410038257.6A CN104803610A (en) | 2014-01-26 | 2014-01-26 | Manufacturing method of highly pure spray-free fused quartz crucible for polysilicon ingot casting |
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| CN201410038257.6A CN104803610A (en) | 2014-01-26 | 2014-01-26 | Manufacturing method of highly pure spray-free fused quartz crucible for polysilicon ingot casting |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105645782A (en) * | 2016-02-03 | 2016-06-08 | 季勇升 | Manufacturing method for efficient spraying-free fused quartz crucible for polycrystalline silicon ingot casting |
| CN107986769A (en) * | 2017-12-13 | 2018-05-04 | 苏州浩焱精密模具有限公司 | A kind of preparation method of quartz pincers pot mould |
| CN113443903A (en) * | 2021-07-20 | 2021-09-28 | 烟台核晶陶瓷新材料有限公司 | Preparation method of oversized cuboid fused quartz crucible and method for producing hollow square silicon core by using same |
| CN116903260A (en) * | 2023-09-14 | 2023-10-20 | 烟台核晶陶瓷新材料有限公司 | Manufacturing process of high-purity coating of crucible for polycrystalline silicon ingot casting |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101956231A (en) * | 2010-10-28 | 2011-01-26 | 杭州先进石英材料有限公司 | Quartz glass crucible and preparation method thereof |
| CN102219360A (en) * | 2011-05-08 | 2011-10-19 | 江苏润弛太阳能材料科技有限公司 | Method for manufacturing polycrystalline silicon ingot casting fused quartz crucible without spraying |
| CN102225837A (en) * | 2011-05-08 | 2011-10-26 | 江苏润弛太阳能材料科技有限公司 | Manufacture method of spray-free fused quartz crucible used for polycrystalline silicon cast ingots |
| CN102249523A (en) * | 2011-05-08 | 2011-11-23 | 江苏润弛太阳能材料科技有限公司 | Method for manufacturing spray-free fused quartz crucible for polycrystalline silicon cast ingot |
| CN102776561A (en) * | 2012-04-01 | 2012-11-14 | 江西赛维Ldk太阳能高科技有限公司 | Polycrystalline silicon ingot, preparation method of polycrystalline silicon ingot, polycrystalline silicon slice and crucible for polycrystalline silicon ingot casting |
| CN103361722A (en) * | 2013-07-23 | 2013-10-23 | 江西赛维Ldk太阳能高科技有限公司 | Polycrystalline silicon ingots and preparation method thereof, polycrystalline silicon chips and polycrystalline silicon ingot casting crucible |
-
2014
- 2014-01-26 CN CN201410038257.6A patent/CN104803610A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101956231A (en) * | 2010-10-28 | 2011-01-26 | 杭州先进石英材料有限公司 | Quartz glass crucible and preparation method thereof |
| CN102219360A (en) * | 2011-05-08 | 2011-10-19 | 江苏润弛太阳能材料科技有限公司 | Method for manufacturing polycrystalline silicon ingot casting fused quartz crucible without spraying |
| CN102225837A (en) * | 2011-05-08 | 2011-10-26 | 江苏润弛太阳能材料科技有限公司 | Manufacture method of spray-free fused quartz crucible used for polycrystalline silicon cast ingots |
| CN102249523A (en) * | 2011-05-08 | 2011-11-23 | 江苏润弛太阳能材料科技有限公司 | Method for manufacturing spray-free fused quartz crucible for polycrystalline silicon cast ingot |
| CN102776561A (en) * | 2012-04-01 | 2012-11-14 | 江西赛维Ldk太阳能高科技有限公司 | Polycrystalline silicon ingot, preparation method of polycrystalline silicon ingot, polycrystalline silicon slice and crucible for polycrystalline silicon ingot casting |
| CN103361722A (en) * | 2013-07-23 | 2013-10-23 | 江西赛维Ldk太阳能高科技有限公司 | Polycrystalline silicon ingots and preparation method thereof, polycrystalline silicon chips and polycrystalline silicon ingot casting crucible |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105645782A (en) * | 2016-02-03 | 2016-06-08 | 季勇升 | Manufacturing method for efficient spraying-free fused quartz crucible for polycrystalline silicon ingot casting |
| CN105645782B (en) * | 2016-02-03 | 2018-10-30 | 季勇升 | The manufacturing method for efficiently exempting from spraying molten silica crucible for polycrystalline silicon ingot casting |
| CN107986769A (en) * | 2017-12-13 | 2018-05-04 | 苏州浩焱精密模具有限公司 | A kind of preparation method of quartz pincers pot mould |
| CN107986769B (en) * | 2017-12-13 | 2021-06-15 | 苏州浩焱精密模具有限公司 | Preparation method of quartz crucible mold |
| CN113443903A (en) * | 2021-07-20 | 2021-09-28 | 烟台核晶陶瓷新材料有限公司 | Preparation method of oversized cuboid fused quartz crucible and method for producing hollow square silicon core by using same |
| CN116903260A (en) * | 2023-09-14 | 2023-10-20 | 烟台核晶陶瓷新材料有限公司 | Manufacturing process of high-purity coating of crucible for polycrystalline silicon ingot casting |
| CN116903260B (en) * | 2023-09-14 | 2023-11-21 | 烟台核晶陶瓷新材料有限公司 | Manufacturing process of high-purity coating of crucible for polycrystalline silicon ingot casting |
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Application publication date: 20150729 |