CN103396170A - Preparation method of crucible coating for polycrystalline silicon ingot and crucible - Google Patents
Preparation method of crucible coating for polycrystalline silicon ingot and crucible Download PDFInfo
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- CN103396170A CN103396170A CN2013102864988A CN201310286498A CN103396170A CN 103396170 A CN103396170 A CN 103396170A CN 2013102864988 A CN2013102864988 A CN 2013102864988A CN 201310286498 A CN201310286498 A CN 201310286498A CN 103396170 A CN103396170 A CN 103396170A
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Abstract
The invention provides a preparation method of a crucible coating for a polycrystalline silicon ingot. The preparation method comprises the following steps of: 1) preparation stage: weighing a certain quantity of silicon nitride powder; 2) pretreatment stage: baking the silicon nitride powder, and further performing screen filtration on the silicon nitride powder after baking; 3) spraying stage: taking out a determined quantity of the silicon nitride powder after screen filtration, adding into deionized water, uniformly stirring to obtain silicon nitride liquid, and spraying the silicon nitride liquid on the inner surface of a crucible; and 4) sintering stage: sintering the crucible after spraying, and forming the crucible coating for the polycrystalline silicon ingot on the inner surface of the crucible after the end of sintering.
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 the polycrystal silicon cell cost makes it progressively replace the dominant position of monocrystalline silicon battery in market.In silicon materials solar cell industry, polycrystalline silicon ingot casting has become the main body ingot casting technology.In the polycrystalline silicon ingot casting process, for the smooth demoulding of silicon ingot being separated and preventing that the crucible that under high temperature, liquid-state silicon and quartz-ceramics are made from reacting, need be made coating on inner surface of crucible, and to require coating be high purity, stable in properties, and with inner surface of crucible, have 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, after normally it directly being added deionized water for stirring evenly, then be sprayed on inner surface of crucible, then through high temperature sintering, forms silicon nitride coating.For reducing energy consumption cost, increase work efficiency, at present domesticly non-sintered coating production after some crucible sprayings having occurred, is mainly by increase the materials such as silicon sol, polyvinyl alcohol in silicon nitride suspending liquid, to play fast setting and the effect of effective adhesive is arranged.But the coating that adopts these methods making is understood the content of carbon oxygen metal impurities in corresponding increase silicon ingot.For example, silicon sol comprises the silica dioxide granule of Nano grade, can generate silicon monoxide with the silicon melt reaction in the ingot casting process; And organic substance at high temperature can occur to decompose or volatilization, has all reduced on the whole coating compactness, easily silicon ingot is caused to a certain degree contaminating impurity, thereby affects the quality of silicon ingot.In addition, spraying is non-sintered afterwards means that coating degree of crystallinity is low, with respect to ingot casting heat-processed, is unsettled, to the growth of crystal, can impact, particularly long brilliant initial stage nucleation stage.
in addition, although numerous photovoltaic enterprise improves and optimizes the preparation method of traditional coating, but equal actual dispersiveness and size distribution homogeneities of considering silicon nitride powder, because of the particle of silicon nitride powder little, particle diameter is micron level, in the packing of dispatching from the factory, long-distance transport, can extruding unite even to make moist in the long-term storage process, dispersed serious the reduction, even slowly pour into silicon nitride powder in deionized water, all easily produce the long-pending phenomenon of false particle and group in liquid, thereby cause and stir inhomogeneous 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 is long-pending little, a little less than adsorptive power, easily causes after the silicon ingot demoulding silicon nitride coating that adheres to one deck white, causes 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 of making by the method, the high-compactness of crucible coating layer and suitable bonding strength can be ensured, thereby 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 the silicon nitride powder after baking is carried out sieving;
3) the spraying stage: take out to determine amount the silicon nitride powder after sieving and it added in deionized water, obtaining silicon nitride liquid after stirring, with described silicon nitride liquid spray on inner surface of crucible;
4) the sintering stage: the crucible after spraying is carried out sintering, namely form crucible pot coating for polysilicon casting ingot at inner surface of crucible after sintering is complete.
Step 2) in, pretreatment stage comprises baking and two steps of sieving.For preventing that silicon nitride powder from causing the inhomogeneous coating result problem that affects of formed silicon nitride liquid agitation because of caking or make moist etc., taked baking processing to silicon nitride powder; Silicon nitride powder after baking is carried out sieving, can not only stop into the use of the silicon nitride powder of agllutination group, and improved the distributing homogeneity of silicon nitride particle diameter.
Preferably, step 2) in, silicon nitride powder is toasted specifically silicon nitride powder is put into baking oven, at the temperature of 60～90 ℃, it is toasted, storing time is 5～9hr.
Preferably, step 2) in, the silicon nitride powder that the silicon nitride powder after baking is carried out after sieving specifically adopts filter screen to baking carries out sieving, and the order number of filter screen is 80～200.
Preferably, sieving filter screen used is nylon material, thereby is difficult for introducing metallic impurity.
For reducing β-Si
3N
4The impact of Elongated grain shape on anchoring strength of coating, avoid peeling off of crucible coating layer that silicon nitride makes, preferred steps 1) in silicon nitride powder to adopt purity be α-Si more than 99.5%
3N
4Powder.Due to α-Si
3N
4The grain shape of powder is needle-like, but the bonding strength of the grain shape effective guarantee crucible coating layer of this needle-like.
Preferably, step 3) in, belonging to ion and the impact of other ionic group on silicon nitride liquid suspension characteristic for reducing underwater gold, it is the above deionized water of 10M Ω .cm that described deionized water adopts resistivity.
Preferably, step 3) specifically comprise: take out the silicon nitride powder after sieving and determine measure and slowly be poured into it in deionized water, then first high-speed stirring 10～20min at normal temperatures, stirring at low speed 10～20min again, so that silicon nitride powder is uniformly distributed in deionized water, namely obtain silicon nitride liquid after stirring, then with described silicon nitride liquid spray on inner surface of crucible, coating thickness is 80～200 μ m.
Further preferably, in step 3) in, the velocity range that highly stirs be 100～160rpm (rev/min), the velocity range of stirring at low speed be 45～70rpm (rev/min).
Step 3) in, take out determining amount the silicon nitride powder after sieving and slowly be poured in step in deionized water, (unit: g) (unit: numeric ratio ml) is 0.25～0.3g: 1ml to the consumption of silicon nitride powder with the consumption of deionized water.
Preferably, step 3) in, when the silicon nitride liquid spray that will stir is on inner surface of crucible, the silicon nitride liquid that the sprays speed with 45～100rpm is stirred, cause spraying problem of non-uniform to prevent silicon nitride powder from precipitation occurring, and in spraying process, the homo(io)thermism that keeps crucible is the some definite values in 50～80 ℃, to avoid Yin Wendu too low and produce bubble, be full of cracks or to produce coating adhesion inadequate because of excess Temperature, and then affect coating quality.
Preferably, step 4) in, crucible after spraying is carried out crucible after sintering specifically will spray to be put into sintering oven and carries out sintering, during sintering, after the temperature of described sintering oven is warming up to 800～1200 ℃ with the speed of 2.5～4 ℃/min, be incubated again 2～5hr, with the stability that improves coating with suitable bonding strength is provided.
The present invention also provides a kind of crucible, and this crucible has the crucible coating layer of making according to described method.
The invention has the beneficial effects as follows: the method is not being introduced under the prerequisite of impurity element as far as possible, can make coating more even by silicon nitride powder being carried out pre-treatment, effectively ensured the high compactness of crucible coating layer, make the crucible coating layer purity for preparing high, thereby effectively suppressed the pollution of crucible impurity, improved the silicon ingot quality; In addition, crucible coating layer good stability and possess suitable bonding strength in the crucible after sintering, ensured silicon ingot demoulding integrity effectively, also reduced the processing cost of reclaimed materials when improving output.
The method also has the advantages such as technique is simple, convenient operation.
Description of drawings
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;
Fig. 2 is for adopting the shape appearance figure (or demoulding outside drawing) of the formed polycrystalline silicon ingot casting of crucible of the prior art;
Carry out the shape appearance figure of the formed polycrystalline silicon ingot casting of ingot casting in the crucible of Fig. 3 for the crucible coating layer of preparation in the embodiment of the present invention 2;
Carry out the shape appearance figure of the formed polycrystalline silicon ingot casting of ingot casting in the crucible of Fig. 4 for the crucible coating layer of preparation in the embodiment of the present invention 3.
In figure: the 1-silicon nitride layer
Embodiment
, for making those skilled in the art understand better technical scheme of the present invention, 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 the silicon nitride powder after baking is carried out sieving;
3) the spraying stage: take out to determine amount the silicon nitride powder after sieving and it added in deionized water, obtaining silicon nitride liquid after stirring, with described silicon nitride liquid spray on inner surface of crucible;
4) the sintering stage: the crucible after spraying is carried out sintering, namely form crucible pot coating for polysilicon casting ingot at inner surface of crucible after sintering is complete.
The present invention also provides a kind of crucible, and described crucible has the crucible coating layer that adopts 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 the silicon nitride powder after baking is carried out sieving.
Particularly, with S1) in the silicon nitride powder prepared put into baking oven, at the temperature of 60 ℃, it is toasted, storing time is 8hr; At once the screen cloth that the silicon nitride after toasting subsequently adopts nylon to make carries out sieving.In the present embodiment, the order number of screen cloth is 80 orders.
S3) the spraying stage: take out to determine amount the silicon nitride powder after sieving and it added in deionized water, obtaining single lily silicon nitride suspending liquid body after stirring, with described silicon nitride liquid spray on inner surface of crucible.
In the present embodiment, it is the above deionized water of 10M Ω .cm that described deionized water adopts resistivity.
Wherein, the crucible of required spraying is highly to be the ceramic crucible of 480mm.Taking the 480g silicon nitride powder, is 0.25～0.3g: 1ml according to the numeric ratio of the consumption of the consumption of silicon nitride powder and deionized water, and the consumption of determining deionized water is 1800ml.
The concrete operations of this step are as follows: take out 480g the silicon nitride powder after sieving, it slowly is poured in the deionized water of 1800ml, and first rotating speed with 120rpm stirs 10～20min at normal temperatures, rotating speed with 60rpm stirs 10～20min again, namely obtain silicon nitride liquid after stirring, subsequently, the silicon nitride liquid that obtains is kept continuing to stir with the rotating speed of 70rpm, simultaneously with described silicon nitride liquid spray on the internal surface of crucible, wherein coating thickness is 120 μ m, and in spraying process, keeping the homo(io)thermism of crucible is 55 ℃.
S4) the sintering stage: the crucible after spraying is carried out sintering, namely form crucible coating layer at inner surface of crucible after sintering is complete.
The complete crucible of spraying is put into sintering oven and carried out sintering, in the present embodiment, during sintering, the temperature of described sintering oven is warming up to 800 ℃ with the speed of 4 ℃/min, then is incubated 2～5hr, can form crucible coating layer on inner surface of crucible.
S5) examination phase: the crucible coating layer that forms is checked, 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, require coating even, come off without peeling off, blistering and crackle, and surface checks after abnormal and namely obtains described crucible pot coating for polysilicon casting ingot without bad phenomenon such as bubble, be full of cracks.
The present invention also provides a kind of crucible, has the crucible coating layer of making according to aforesaid method on the internal surface of this crucible.
Figure 3 shows that the shape appearance figure that carries out formed polycrystalline silicon ingot casting after polycrystalline silicon ingot casting in the crucible of the present embodiment.As can be seen from Figure 3, the demolding performace of this polycrystalline silicon ingot casting is good, the silicon ingot outside surface is light totally, particularly few to the adhesion of the white silicon nitride layer that applies on crucible, and then greatly reduce sticking silicon and split the probability that ingot produces, thereby indirectly promoted output, also reduced 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 that forms in existing common crucible to the polycrystalline silicon ingot casting that forms in Fig. 3.As shown in Figure 2, be stained with the silicon nitride layer 1 of a large amount of whites on the outside surface of the polycrystalline silicon ingot casting that forms in existing common crucible, show that this crucible coating layer and inner surface of crucible bonding strength are inadequate, have 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 the silicon nitride powder after baking is carried out sieving.
Particularly, with S1) in the silicon nitride powder prepared put into baking oven, at the temperature of 60 ℃, it is toasted, storing time is 8hr; At once the screen cloth that the silicon nitride after toasting subsequently adopts nylon to make carries out sieving.In the present embodiment, the order number of screen cloth is 80 orders.
S3) the spraying stage: take out to determine amount the silicon nitride powder after sieving and it added in deionized water, obtaining single pure white silicon nitride suspending liquid body after stirring, with described silicon nitride liquid spray on inner surface of crucible.
In the present embodiment, it is the above deionized water of 10M Ω .cm that described deionized water adopts resistivity.
Wherein, the crucible of required spraying is highly to be the ceramic crucible of 540mm.Taking the 540g silicon nitride powder, is 0.25～0.3g: 1ml according to the numeric ratio of the consumption of the consumption of silicon nitride powder and deionized water, and the consumption of determining deionized water is 2000ml.
The concrete operations of this step are as follows: take out 540g the silicon nitride powder after sieving, it slowly is poured in the deionized water of 2000ml, and first rotating speed with 130rpm stirs 10～20min at normal temperatures, rotating speed with 65rpm stirs 10～20min again, namely obtain silicon nitride liquid after stirring, subsequently, the silicon nitride liquid that obtains is kept continuing to stir with the rotating speed of 80rpm, simultaneously with described silicon nitride liquid spray on the internal surface of crucible, wherein coating thickness is 100 μ m, and in spraying process, keeping the homo(io)thermism of crucible is 55 ℃.
S4) the sintering stage: the crucible after spraying is carried out sintering, namely form crucible coating layer at inner surface of crucible after sintering is complete.
The complete crucible of spraying is put into sintering oven and carried out sintering, in the present embodiment, during sintering, the temperature of described sintering oven is warming up to 800 ℃ with the speed of 4 ℃/min, then is incubated 2～5hr, can form crucible coating layer on inner surface of crucible.
S5) examination phase: the crucible coating layer that forms is checked, 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 after abnormal and namely obtain described crucible pot coating for polysilicon casting ingot.
The present invention also provides a kind of crucible, has the crucible coating layer of making according to aforesaid method on the internal surface of this crucible.
Figure 4 shows that the shape appearance figure that carries out formed polycrystalline silicon ingot casting after polycrystalline silicon ingot casting in the present embodiment crucible.As can be seen from Figure 4, the demolding performace of this polycrystalline silicon ingot casting is good, split the ingot phenomenon without sticking crucible, and the silicon nitride layer that only has minute quantity white sticks on the silicon ingot outside surface, and then greatly reduce sticking silicon and split the probability that ingot produces, thereby indirectly promoted output, also reduced the processing cost of reclaimed materials.
Be understandable that, above embodiment is only the illustrative embodiments that adopts for principle of the present invention is described, yet 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 also are considered as protection scope of the present invention.
Claims (10)
1. the preparation method of a 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 the silicon nitride powder after baking is carried out sieving;
3) the spraying stage: take out to determine amount the silicon nitride powder after sieving and it added in deionized water, obtaining silicon nitride liquid after stirring, with described silicon nitride liquid spray on inner surface of crucible;
4) the sintering stage: the crucible after spraying is carried out sintering, namely form crucible pot coating for polysilicon casting ingot at inner surface of crucible after sintering is complete.
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, it is the above deionized water of 10M Ω .cm that described deionized water adopts resistivity.
3. method according to claim 1, is characterized in that step 2) in, silicon nitride powder is toasted specifically silicon nitride powder is put into baking oven, at the temperature of 60～90 ℃, it is toasted, storing time is 5～9hr.
4. method according to claim 1, is characterized in that step 2) in, the silicon nitride powder that the silicon nitride powder after baking is carried out after sieving specifically adopts filter screen to baking carries out sieving, and the order number of filter screen is 80～200.
5. method according to claim 1, it is characterized in that, step 3) specifically comprise: take out the silicon nitride powder after sieving and determine measure and slowly be poured into it 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 with described silicon nitride liquid spray on inner surface of crucible, coating thickness is 80～200 μ m.
6. method according to claim 5, is characterized in that step 3) in, the velocity range that highly stirs is 100～160rpm, the velocity range of stirring at low speed is 45～70rpm.
7. method according to claim 5, it is characterized in that, step 3) in, take out the silicon nitride powder after sieving and determine to measure in the step that also slowly is poured 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.
8. method according to claim 5, 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 that the sprays speed with 45～100rpm is stirred, and in spraying process, the homo(io)thermism that keeps crucible is the some definite values in 50～80 ℃.
9. one of according to claim 1-8 described methods, it is characterized in that, step 4) in, crucible after spraying is carried out crucible after sintering specifically will spray to be put into sintering oven and carries out sintering, during sintering, after the temperature of described sintering oven is warming up to 800～1200 ℃ with the speed of 2.5～4 ℃/min, then be incubated 2～5hr.
10. a crucible, is characterized in that, described crucible has the crucible coating layer that one of according to claim 1-9 described methods are made.
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| CN110049946A (en) * | 2016-12-12 | 2019-07-23 | 宇部兴产株式会社 | The manufacturing method of alpha-silicon nitride powders, polycrystalline silicon ingot casting release agent and polycrystalline silicon ingot casting |
| 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 |
| CN111349967A (en) * | 2018-12-20 | 2020-06-30 | 比亚迪股份有限公司 | Efficient crucible and preparation method thereof |
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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 |
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