CN103396170B - The preparation method of crucible pot coating for polysilicon casting ingot and crucible - Google Patents
The preparation method of crucible pot coating for polysilicon casting ingot and crucible Download PDFInfo
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- CN103396170B CN103396170B CN201310286498.8A CN201310286498A CN103396170B CN 103396170 B CN103396170 B CN 103396170B CN 201310286498 A CN201310286498 A CN 201310286498A CN 103396170 B CN103396170 B CN 103396170B
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Abstract
The invention provides a kind of preparation method of crucible pot coating for polysilicon casting ingot, comprise the following steps: the 1) preparatory stage: take a certain amount of silicon nitride powder; 2) pretreatment stage: described silicon nitride powder is toasted, then sieving is carried out to the silicon nitride powder after baking; 3) spraying stage: take out determined amounts and add in deionized water by it from the silicon nitride powder after sieving, obtains silicon nitride liquid after stirring, by described silicon nitride liquid spray on inner surface of crucible; 4) stage is sintered: the crucible after spraying is sintered, after sintering, namely forms crucible pot coating for polysilicon casting ingot at inner surface of crucible.
Description
Technical field
The present invention relates to a kind of preparation method and crucible of crucible pot coating for polysilicon casting ingot.
Background technology
At present, the absolute predominance on polycrystal silicon cell cost makes it progressively instead of monocrystalline silicon battery dominant position in the market.In silicon materials solar cell industry, polycrystalline silicon ingot casting has become main body ingot casting technology.In polycrystalline silicon ingot casting process, be separated for making the smooth demoulding of silicon ingot and prevent the crucible that liquid-state silicon and quartz-ceramics are made under high temperature from reacting, coating need be made on inner surface of crucible, and require that coating is high purity, stable in properties, and with inner surface of crucible, there is suitable bonding strength.
For a long time, the starting material of crucible pot coating for polysilicon casting ingot mainly adopt crystalline state Si
3n
4powder, normally it is directly added deionized water for stirring evenly after, then be sprayed on inner surface of crucible, then form silicon nitride coating through high temperature sintering.For reducing energy consumption cost, increase work efficiency, at present domestic there are some crucible sprayings after non-sintered coating production, mainly by increasing the material such as silicon sol, polyvinyl alcohol in silicon nitride suspending liquid, to play fast setting and to have the effect of effective adhesive.But the coating adopting these methods to make can the content of carbon oxygen metal impurities in corresponding increase silicon ingot.Such as, silicon sol comprises the silica dioxide granule of Nano grade, can react with silicon melt and generate silicon monoxide in ingot casting process; And organic substance at high temperature can occur to decompose or volatilization, all reduce coating compactness on the whole, easily contaminating impurity is to a certain degree caused to silicon ingot, thus affect the quality of silicon ingot.In addition, non-sintered after spraying, meaning that coating degree of crystallinity is low, is unstable relative to ingot casting heat-processed, then can impact the growth of crystal, particularly long brilliant initial stage nucleation stage.
In addition, although the numerous preparation method of photovoltaic enterprise to traditional coating improves and optimizes, but all unactual dispersiveness and the even particle size distribution considering silicon nitride powder, because the particle of silicon nitride powder is little, particle diameter is micron level, in packaging of dispatching from the factory, long-distance transport, unity can be extruded in long-term storage process even make moist, dispersed serious reduction, even if silicon nitride powder is slowly poured in deionized water, all easily produce the long-pending phenomenon of false particle and group in a liquid, thus cause and stir uneven and affect the phenomenon of coating result, and then have a strong impact on the quality of silicon ingot.Moreover because the particle diameter of silicon nitride powder fluctuates within the specific limits, distributing homogeneity is bad, and specific grain surface amasss little, and adsorptive power is weak, adheres to the silicon nitride coating of one deck white after easily causing the silicon ingot demoulding, cause the increase greatly of scrap stock cost recovery.
Summary of the invention
Technical problem to be solved by this invention is for above shortcomings in prior art, a kind of preparation method and crucible of crucible pot coating for polysilicon casting ingot are provided, the crucible coating layer good stability made by the method, the high-compactness that can ensure crucible coating layer and suitable bonding strength, thus the demoulding integrity of silicon ingot and the quality of silicon ingot can be guaranteed.
The technical scheme that solution the technology of the present invention problem adopts is this polysilicon ingot crucible coating production, comprises the following steps:
1) preparatory stage: take a certain amount of silicon nitride powder;
2) pretreatment stage: described silicon nitride powder is toasted, then sieving is carried out to the silicon nitride powder after baking;
3) spraying stage: take out determined amounts and add in deionized water by it from the silicon nitride powder after sieving, obtains silicon nitride liquid after stirring, by described silicon nitride liquid spray on inner surface of crucible;
4) stage is sintered: the crucible after spraying is sintered, after sintering, namely forms crucible pot coating for polysilicon casting ingot at inner surface of crucible.
Step 2) in, pretreatment stage comprises baking and sieving two steps.For preventing silicon nitride powder from affecting coating result problem because caking or make moist etc. causes formed silicon nitride liquid agitation uneven, baking processing is taken to silicon nitride powder; Sieving is carried out to the silicon nitride powder after baking, the use of the silicon nitride powder of agllutination group can not only be stopped into, and also improve the distributing homogeneity of silicon nitride particle diameter.
Preferably, step 2) in, toast silicon nitride powder and specifically silicon nitride powder is put into baking oven, toast at the temperature of 60 ~ 90 DEG C to it, baking time is 5 ~ 9hr.
Preferably, step 2) in, carry out sieving to the silicon nitride powder after baking and specifically adopt filter screen to carry out sieving to the silicon nitride powder after baking, the order number of filter screen is 80 ~ 200.
Preferably, sieving filter screen used is nylon material, thus not easily introduces metallic impurity.
For reducing β-Si
3n
4elongated grain shape on the impact of anchoring strength of coating, peeling off of the crucible coating layer avoiding silicon nitride to make, preferred steps 1) in silicon nitride powder adopt purity be more than 99.5% α-Si
3n
4powder.Due to α-Si
3n
4the grain shape of powder is needle-like, and the grain shape of this needle-like can the bonding strength of effective guarantee crucible coating layer.
Preferably, step 3) in, belong to ion with other ionic group on the impact of silicon nitride liquid suspension characteristic for reducing underwater gold, described deionized water employing resistivity is the deionized water of 10M more than Ω .cm.
Preferably, step 3) specifically comprise: from the silicon nitride powder after sieving, take out determined amounts and it is slowly poured in deionized water, then first high-speed stirring 10 ~ 20min at normal temperatures, stirring at low speed 10 ~ 20min again, be uniformly distributed in deionized water to make silicon nitride powder, namely obtain silicon nitride liquid after stirring, then by described silicon nitride liquid spray on inner surface of crucible, coating thickness is 80 ~ 200 μm.
Further preferably, in step 3) in, the velocity range of high agitation is 100 ~ 160rpm (rev/min), and the velocity range of stirring at low speed is 45 ~ 70rpm (rev/min).
Step 3) in, determined amounts is taken out and in the step being slowly poured in deionized water, the consumption of silicon nitride powder (unit: be g) 0.25 ~ 0.3g: 1ml with the numeric ratio of the consumption (unit: ml) of deionized water from the silicon nitride powder after sieving.
Preferably, step 3) in, when the silicon nitride liquid spray that will stir is on inner surface of crucible, the silicon nitride liquid sprayed is stirred with the speed of 45 ~ 100rpm, cause to prevent silicon nitride powder from precipitation occurring spraying problem of non-uniform, and in spraying process, the homo(io)thermism of maintenance crucible is the some definite values in 50 ~ 80 DEG C, produce to avoid Yin Wendu too low that bubble, be full of cracks or Yin Wendu are too high and to produce coating adhesion inadequate, and then affect coating quality.
Preferably, step 4) in, crucible after spraying is sintered and specifically the crucible after spraying is put into sintering oven and sintered, during sintering, by the temperature of described sintering oven with behind ramp to 800 ~ 1200 of 2.5 ~ 4 DEG C/min DEG C, be incubated 2 ~ 5hr again, to improve the stability of coating and to provide suitable bonding strength.
The present invention also provides a kind of crucible, and this crucible has the crucible coating layer made according to described method.
The invention has the beneficial effects as follows: the method is under the prerequisite not introducing impurity element as far as possible, coating can be made more even by carrying out pre-treatment to silicon nitride powder, effectively ensure the high compactness of crucible coating layer, make the crucible coating layer purity for preparing high, thus effectively inhibit the pollution of crucible impurity, improve Ingot quality; In addition, crucible coating layer good stability in the crucible after sintering and possess suitable bonding strength, has ensured silicon ingot demoulding integrity effectively, also reduces the processing cost of reclaimed materials while improving output.
The method also has the advantages such as technique is simple, convenient operation.
Accompanying drawing explanation
Fig. 1 is the schema of the preparation method of crucible pot coating for polysilicon casting ingot in the embodiment of the present invention 2;
The shape appearance figure (or demoulding outside drawing) of the polycrystalline silicon ingot casting that Fig. 2 is formed for employing crucible of the prior art;
Fig. 3 in the embodiment of the present invention 2 crucible coating layer of preparation crucible in carry out the shape appearance figure of the polycrystalline silicon ingot casting that ingot casting is formed;
Fig. 4 in the embodiment of the present invention 3 crucible coating layer of preparation crucible in carry out the shape appearance figure of the polycrystalline silicon ingot casting that ingot casting is formed.
In figure: 1-silicon nitride layer
Embodiment
For making those skilled in the art understand technical scheme of the present invention better, below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Embodiment 1:
In the present embodiment, the preparation method of invention crucible pot coating for polysilicon casting ingot, comprises the following steps:
1) preparatory stage: take a certain amount of silicon nitride powder;
2) pretreatment stage: described silicon nitride powder is toasted, then sieving is carried out to the silicon nitride powder after baking;
3) spraying stage: take out determined amounts and add in deionized water by it from the silicon nitride powder after sieving, obtains silicon nitride liquid after stirring, by described silicon nitride liquid spray on inner surface of crucible;
4) stage is sintered: the crucible after spraying is sintered, after sintering, namely forms crucible pot coating for polysilicon casting ingot at inner surface of crucible.
The present invention also provides a kind of crucible, and described crucible has the crucible coating layer adopting aforesaid method to make.
Embodiment 2:
As shown in Figure 1, in the present embodiment, the preparation method of crucible pot coating for polysilicon casting ingot of the present invention comprises the following steps:
S1) preparatory stage: take a certain amount of silicon nitride powder.
In the present embodiment, described silicon nitride powder adopts the α-Si of purity more than 99.5%
3n
4powder.
S2) pretreatment stage: described silicon nitride powder is toasted, then sieving is carried out to the silicon nitride powder after baking.
Particularly, by S1) in prepare silicon nitride powder put into baking oven, toast it at the temperature of 60 DEG C, baking time is 8hr; At once the screen cloth that the silicon nitride after baking adopts nylon to make is carried out sieving subsequently.In the present embodiment, the order number of screen cloth is 80 orders.
S3) spraying stage: take out determined amounts and add in deionized water by it from the silicon nitride powder after sieving, obtains single lily silicon nitride suspending liquid body, by described silicon nitride liquid spray on inner surface of crucible after stirring.
In the present embodiment, described deionized water employing resistivity is the deionized water of 10M more than Ω .cm.
Wherein, the crucible of required spraying is highly the ceramic crucible of 480mm.Take 480g silicon nitride powder, the numeric ratio according to the consumption of silicon nitride powder and the consumption of deionized water is 0.25 ~ 0.3g: 1ml, determines that the consumption of deionized water is 1800ml.
The concrete operations of this step are as follows: from the silicon nitride powder after sieving, take out 480g, it is slowly poured in the deionized water of 1800ml, and first stir 10 ~ 20min with the rotating speed of 120rpm at normal temperatures, 10 ~ 20min is stirred again with the rotating speed of 60rpm, namely silicon nitride liquid is obtained after stirring, subsequently, the silicon nitride liquid obtained is kept continue to stir with the rotating speed of 70rpm, simultaneously by described silicon nitride liquid spray on the internal surface of crucible, wherein coating thickness is 120 μm, and in spraying process, the homo(io)thermism keeping crucible is 55 DEG C.
S4) stage is sintered: the crucible after spraying is sintered, after sintering, namely forms crucible coating layer at inner surface of crucible.
The complete crucible of spraying is put into sintering oven sinter, in the present embodiment, during sintering, by the temperature of described sintering oven with the ramp to 800 DEG C of 4 DEG C/min, then be incubated 2 ~ 5hr, crucible coating layer can be formed on inner surface of crucible.
S5) examination phase: check the crucible coating layer formed, after passed examination, this crucible coating layer is described crucible pot coating for polysilicon casting ingot.
To step S4) in the crucible coating layer that obtains check, requiring coating uniform, coming off without peeling off, blistering and crackle, and the bad phenomenon such as surperficial bubble-free, be full of cracks, check without exception after namely obtain described crucible pot coating for polysilicon casting ingot.
The present invention also provides a kind of crucible, the internal surface of this crucible has the crucible coating layer made according to aforesaid method.
Figure 3 shows that the shape appearance figure of the polycrystalline silicon ingot casting formed carry out polycrystalline silicon ingot casting in the crucible of the present embodiment after.As can be seen from Figure 3, the demolding performace of this polycrystalline silicon ingot casting is good, silicon ingot outside surface is totally bright, particularly few to the adhesion of the white silicon nitride layer that crucible applies, and then greatly reduce the probability that sticky silicon splits ingot generation, thus indirectly improve output, also reduce the processing cost of reclaimed materials.As a complete unit, its performance is much better than the stripping result of the polycrystalline silicon ingot casting formed in existing common crucible to the polycrystalline silicon ingot casting formed in Fig. 3.As shown in Figure 2, the outside surface of the polycrystalline silicon ingot casting formed in existing common crucible is stained with the silicon nitride layer 1 of a large amount of white, shows this crucible coating layer and inner surface of crucible bonding strength not, there is serious peeling phenomenon.
Embodiment 3:
As shown in Figure 1, in the present embodiment, the preparation method of crucible pot coating for polysilicon casting ingot of the present invention comprises the following steps:
S1) preparatory stage: take a certain amount of silicon nitride powder.
In the present embodiment, described silicon nitride powder adopts the α-Si of purity more than 99.5%
3n
4powder.
S2) pretreatment stage: described silicon nitride powder is toasted, then sieving is carried out to the silicon nitride powder after baking.
Particularly, by S1) in prepare silicon nitride powder put into baking oven, toast it at the temperature of 60 DEG C, baking time is 8hr; At once the screen cloth that the silicon nitride after baking adopts nylon to make is carried out sieving subsequently.In the present embodiment, the order number of screen cloth is 80 orders.
S3) spraying stage: take out determined amounts and add in deionized water by it from the silicon nitride powder after sieving, obtains single pure white silicon nitride suspending liquid body, by described silicon nitride liquid spray on inner surface of crucible after stirring.
In the present embodiment, described deionized water employing resistivity is the deionized water of 10M more than Ω .cm.
Wherein, the crucible of required spraying is highly the ceramic crucible of 540mm.Take 540g silicon nitride powder, the numeric ratio according to the consumption of silicon nitride powder and the consumption of deionized water is 0.25 ~ 0.3g: 1ml, determines that the consumption of deionized water is 2000ml.
The concrete operations of this step are as follows: from the silicon nitride powder after sieving, take out 540g, it is slowly poured in the deionized water of 2000ml, and first stir 10 ~ 20min with the rotating speed of 130rpm at normal temperatures, 10 ~ 20min is stirred again with the rotating speed of 65rpm, namely silicon nitride liquid is obtained after stirring, subsequently, the silicon nitride liquid obtained is kept continue to stir with the rotating speed of 80rpm, simultaneously by described silicon nitride liquid spray on the internal surface of crucible, wherein coating thickness is 100 μm, and in spraying process, the homo(io)thermism keeping crucible is 55 DEG C.
S4) stage is sintered: the crucible after spraying is sintered, after sintering, namely forms crucible coating layer at inner surface of crucible.
The complete crucible of spraying is put into sintering oven sinter, in the present embodiment, during sintering, by the temperature of described sintering oven with the ramp to 800 DEG C of 4 DEG C/min, then be incubated 2 ~ 5hr, crucible coating layer can be formed on inner surface of crucible.
S5) examination phase: check the crucible coating layer formed, after passed examination, this crucible coating layer is described crucible pot coating for polysilicon casting ingot.
To step S4) in the crucible coating layer that obtains check, check without exception after namely obtain described crucible pot coating for polysilicon casting ingot.
The present invention also provides a kind of crucible, the internal surface of this crucible has the crucible coating layer made according to aforesaid method.
Figure 4 shows that the shape appearance figure of the polycrystalline silicon ingot casting formed carry out polycrystalline silicon ingot casting in the present embodiment crucible after.As can be seen from Figure 4, the demolding performace of this polycrystalline silicon ingot casting is good, ingot phenomenon is split without sticky crucible, and only have the silicon nitride layer of minute quantity white to stick on silicon ingot outside surface, and then greatly reduce the probability that sticky silicon splits ingot generation, thus indirectly improve output, also reduce the processing cost of reclaimed materials.
Be understandable that, the illustrative embodiments that above embodiment is only used to principle of the present invention is described and adopts, but the present invention is not limited thereto.For those skilled in the art, without departing from the spirit and substance in the present invention, can make various modification and improvement, these modification and improvement are also considered as protection scope of the present invention.
Claims (8)
1. a preparation method for crucible pot coating for polysilicon casting ingot, comprises the following steps:
1) preparatory stage: take a certain amount of silicon nitride powder;
2) pretreatment stage: described silicon nitride powder is toasted, then sieving is carried out to the silicon nitride powder after baking;
Wherein, toast specifically silicon nitride powder is put into baking oven to silicon nitride powder, toast at the temperature of 60 ~ 90 DEG C to it, baking time is 5 ~ 9hr;
Carrying out sieving to the silicon nitride powder after baking specifically adopts filter screen to carry out sieving to the silicon nitride powder after baking, and the order number of filter screen is 80 ~ 200;
3) spraying stage: take out determined amounts and add in deionized water by it from the silicon nitride powder after sieving, obtains silicon nitride liquid after stirring, by described silicon nitride liquid spray on inner surface of crucible;
4) stage is sintered: the crucible after spraying is sintered, after sintering, namely forms crucible pot coating for polysilicon casting ingot at inner surface of crucible.
2. method according to claim 1, is characterized in that, step 1) in, described silicon nitride powder adopts the α-Si of purity more than 99.5%
3n
4powder; Step 3) in, described deionized water employing resistivity is the deionized water of 10M more than Ω .cm.
3. method according to claim 1, it is characterized in that, step 3) specifically comprise: from the silicon nitride powder after sieving, take out determined amounts and it is slowly poured in deionized water, then first high-speed stirring 10 ~ 20min at normal temperatures, stirring at low speed 10 ~ 20min again, namely obtain silicon nitride liquid after stirring, then by described silicon nitride liquid spray on inner surface of crucible, coating thickness is 80 ~ 200 μm.
4. method according to claim 3, is characterized in that, step 3) in, the velocity range of high agitation is 100 ~ 160rpm, and the velocity range of stirring at low speed is 45 ~ 70rpm.
5. method according to claim 3, it is characterized in that, step 3) in, from the silicon nitride powder after sieving, take out determined amounts and be slowly poured in the step in deionized water, the numeric ratio of the consumption of silicon nitride powder and the consumption of deionized water is 0.25 ~ 0.3g:1ml.
6. method according to claim 3, it is characterized in that, step 3) in, when the silicon nitride liquid spray that will stir is on inner surface of crucible, the silicon nitride liquid sprayed is stirred with the speed of 45 ~ 100rpm, and in spraying process, the homo(io)thermism of maintenance crucible is the some definite values in 50 ~ 80 DEG C.
7. according to the method one of claim 1-6 Suo Shu, it is characterized in that, step 4) in, crucible after spraying is sintered and specifically the crucible after spraying is put into sintering oven and sintered, during sintering, by the temperature of described sintering oven with behind ramp to 800 ~ 1200 of 2.5 ~ 4 DEG C/min DEG C, then be incubated 2 ~ 5hr.
8. a crucible, is characterized in that, described crucible has the crucible coating layer made according to the method one of claim 1-7 Suo Shu.
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| TWI657042B (en) * | 2016-12-12 | 2019-04-21 | 日商宇部興產股份有限公司 | Silicon nitride powder, release agent for polycrystalline silicon ingot and method for manufacturing polycrystalline silicon ingot |
| CN111349967B (en) * | 2018-12-20 | 2022-03-18 | 比亚迪股份有限公司 | Efficient crucible and preparation method thereof |
| CN110408985A (en) * | 2019-08-19 | 2019-11-05 | 大同新成新材料股份有限公司 | A method of reducing the thermal field crucible service failure of single-item silicon |
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| CN101428273A (en) * | 2008-12-05 | 2009-05-13 | 江阴海润太阳能电力有限公司 | Silicon nitride spray finishing method for quartz crucible for polysilicon solar battery casting ingot |
| CN101508590A (en) * | 2009-03-20 | 2009-08-19 | 江西赛维Ldk太阳能高科技有限公司 | Crucible pot coating for polysilicon casting ingot and preparation method |
| CN201305659Y (en) * | 2008-12-05 | 2009-09-09 | 江阴海润太阳能电力有限公司 | Silicon nitride spraying device of quartz crucible for multi-crystal silicon solar battery ingot casting |
| CN101844935A (en) * | 2010-05-31 | 2010-09-29 | 江西赛维Ldk太阳能高科技有限公司 | Crucible coating layer for polycrystal silicon or single crystal silicon and preparation method thereof |
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Patent Citations (4)
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|---|---|---|---|---|
| CN101428273A (en) * | 2008-12-05 | 2009-05-13 | 江阴海润太阳能电力有限公司 | Silicon nitride spray finishing method for quartz crucible for polysilicon solar battery casting ingot |
| CN201305659Y (en) * | 2008-12-05 | 2009-09-09 | 江阴海润太阳能电力有限公司 | Silicon nitride spraying device of quartz crucible for multi-crystal silicon solar battery ingot casting |
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| CN101844935A (en) * | 2010-05-31 | 2010-09-29 | 江西赛维Ldk太阳能高科技有限公司 | Crucible coating layer for polycrystal silicon or single crystal silicon and preparation method thereof |
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