CN103482632A - Combined type crucible applied to directional solidification and purification of polycrystalline silicon - Google Patents
Combined type crucible applied to directional solidification and purification of polycrystalline silicon Download PDFInfo
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- CN103482632A CN103482632A CN201310421117.2A CN201310421117A CN103482632A CN 103482632 A CN103482632 A CN 103482632A CN 201310421117 A CN201310421117 A CN 201310421117A CN 103482632 A CN103482632 A CN 103482632A
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Abstract
The invention belongs to the field of polycrystalline silicon purification, in particular to a combined type crucible applied to directional solidification and purification of polycrystalline silicon. The combined type crucible comprises the quartz crucible wall and the graphite crucible bottom. The lower end of the quartz crucible wall and the graphite crucible bottom are mutually spliced. The quartz crucible wall is of a three-dimensional structure vertically communicated. The cross section shape of the graphite crucible bottom is the same as that of the quartz crucible wall. The combined type crucible has the advantages that as the crucible bottom is made of a graphite material, the advantage of a large heat conductivity coefficient of graphite is fully utilized, the directional solidification effect is improved, and the energy consumption is lowered greatly; as the quartz crucible wall and the graphite crucible bottom are connected in a splicing mode, convenience is brought to replacement when damage occurs, and the cost is reduced; the solid liquid interface is controlled stably and is less in fluctuation, impurities conveniently accumulate to the top ends of silicon ingots, and therefore the impurity removing effect is good.
Description
Technical field
The invention belongs to the polycrystalline silicon purifying field, be specifically related to a kind of combined type copple that polysilicon directional freezing is purified that is applied to.
Background technology
At present, China has become world energy sources production and consumption big country, but the energy expenditure level is also very low per capita.Along with economical and social development, China's energy demand is by sustainable growth, for current energy shortage situation, deep thinking is all being carried out in countries in the world, and effort improves efficiency of energy utilization, promote the development and application of renewable energy source, reduce the dependence to Imported oil, strengthen energy security.
Solar energy power generating development in recent years as one of important development direction of renewable energy source is swift and violent, and its proportion is increasing.According to " planning of renewable energy source Long-and Medium-term Development ", to the year two thousand twenty, China strives making the solar electrical energy generation installed capacity to reach the 1.8GW(gigawatt), will reach 600GW to the year two thousand fifty.Expect the year two thousand fifty, the electric power installation of Chinese renewable energy source will account for 25% of national electric power installation, and wherein the photovoltaic generation installation will account for 5%.Before estimating the year two thousand thirty, the compound growth rate of Chinese sun power installed capacity will be up to more than 25%.
Polysilicon is as the desirable feedstock of solar cell, impurity wherein mainly contains metallic impurity and the nonmetallic impuritys such as boron, phosphorus such as iron, aluminium, calcium, and these impurity elements can reduce the Compound Degree of silicon crystal grain interface photo-generated carrier, and the Compound Degree of photo-generated carrier has determined the photoelectric transformation efficiency of solar cell, so effectively remove these impurity, in the application facet of solar cell, vital effect is arranged.
The development of photovoltaic industry depends on the purification to the silicon raw material.The development of photovoltaic industry depends on the purification to polycrystalline silicon raw material.The purifying technique of polycrystalline silicon raw material is several technique below main the dependence at present: Siemens Method, silane thermal decomposition process, gas fluidized bed method or metallurgy method.Wherein, metallurgy method has that cost is low, technique is simple and free of contamination characteristics, more and more is applied to the purification of polysilicon.The main technique of metallurgy method is slag making melting, directional freeze, electron beam melting and ingot casting.In the process that the silicon raw material is purified, there are a key, requisite link, exactly the silicon raw material is carried out to the directional freeze purification, directional solidification technique used is widely used in field of metallurgy purification.Utilize the segregation coefficient between silicon and impurity in the silicon raw material to have these characteristics of larger difference, in process of setting, at first the silicon liquid of crucible bottom start to solidify, for reaching the fractional condensation balance, the impurity that segregation coefficient is little out is gathered in liquid state to the continuous separation by diffusion of liquid state from the silicon solidified, along with solidifying constantly, carry out, the concentration of impurity in liquid state is more and more higher, under finally solidifying on the top of ingot casting, be incubated for some time after having solidified under comparatively high temps, make each composition fully spread to reach the fractional condensation balance, finally by foreign matter content, a higher end is removed, obtain the polycrystalline silicon ingot casting of purifying.
In the directional freeze process, the crucible of carrying silicon material is quartz crucible, the thermal conductivity of self material quartz of quartz crucible is little, no matter be single crystal structure or ordinary construction, under normal temperature, thermal conductivity is all below 20W/ (mk), even if, along with temperature raises, the thermal conductivity ascensional range is also little.Because thermal conductivity is less, the silicon liquid that therefore fusing forms can carry out slowly in the process of outwards conducting heat, and causes directional freeze chronic, thereby has greatly increased energy consumption.
Summary of the invention
According to above the deficiencies in the prior art, the present invention proposes a kind of combined type copple that polysilicon directional freezing is purified, structure and material of carrying crucible by change of being applied to, improved the effect of directional freeze, improve radiating efficiency, shortened the directional freeze time, thereby reduced energy consumption.
A kind of combined type copple that polysilicon directional freezing is purified that is applied to of the present invention, at the bottom of comprising quartz crucible wall and plumbago crucible, splice at the bottom of the lower end of quartz crucible wall and plumbago crucible mutually; Wherein, the three-dimensional arrangement that the quartz crucible wall is up/down perforation, the shape of cross section at the bottom of plumbago crucible is consistent with the shape of cross section of quartz crucible wall.
Wherein, the quartz crucible wall is preferably rectangular parallelepiped or the right cylinder of up/down perforation.According in actual industrial production, polycrystalline silicon purifying is generally circular crucible or square crucible with crucible.
At the bottom of plumbago crucible, upper surface preferably is coated with silicon nitride coating or coat of silicon carbide.Because graphite self contains more impurity, prevent the secondary pollution of silicon liquid, spray anti-pollution coating before preferably using, silicon nitride coating and coat of silicon carbide are common coatings, other coating does not limit.
The present invention is spliced at the bottom of by quartz crucible wall and plumbago crucible, preferably following two kinds of modes:
Offer limited impression along opposite position place, quartz crucible wall lower edge at the bottom of plumbago crucible, quartz crucible wall lower end is positioned at limited impression; At the bottom of plumbago crucible, be inverted T shape, quartz crucible wall lower end is positioned at along inverted T shape gap position place.
In the present invention, at the bottom of selecting graphite material as crucible, fully take into account graphite and have high thermal conductivity coefficient, common graphite has 129W/ (mk) at normal temperatures, along with the temperature rising also can be higher.Because silicon liquid in the directional freeze process solidifies from bottom to top, the existence at the bottom of plumbago crucible makes silicon liquid to conduct heat fast downwards, constantly upwards solidify, thus the time of shortening directional freeze.In the present invention, still retaining sidewall of crucible is quartzy material, mainly contains the reason of two aspects, the one, if all adopt graphite material, therefore even if the coating of being coated with, also can cause larger secondary pollution to silicon liquid, partly adopting quartzy material with the large sidewall of crucible of silicon liquid contact area; The 2nd, the quartz crucible wall with respect to plumbago crucible at the bottom of thermal conductivity little a lot, the heat radiation of silicon liquid can be concentrated as downward heat loss through conduction, thus the long crystalline substance of silicon ingot is more even, solid-liquid interface trends towards level, is beneficial to impurity and assembles to the silicon ingot top.
The invention has the advantages that: (1) takes full advantage of the advantage that the graphite heat conducting coefficient is large at the bottom of adopting graphite material as crucible, has improved directional solidification effect, has shortened the directional freeze time, has greatly saved energy consumption; (2) at the bottom of quartz crucible wall and plumbago crucible, adopt the mode of splicing to be connected, the convenient appearance when damaged changed, and reduced cost; (3) solid-liquid interface is controlled and is stablized, and fluctuates little, facilitates impurity to assemble to the silicon ingot top, thus good impurity removing effect.
The accompanying drawing explanation
The structural representation that Fig. 1 is the embodiment of the present invention 1;
The structural representation that Fig. 2 is embodiment 2;
In figure: 1, at the bottom of quartz crucible wall 2, plumbago crucible.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described further.
Embodiment 1:
As shown in Figure 1, a kind ofly be applied to the combined type copple that polysilicon directional freezing is purified, comprise at the bottom of quartz crucible wall 1 and plumbago crucible 2, at the bottom of the lower end of quartz crucible wall 1 and plumbago crucible, 2 splice mutually.
Wherein, the rectangular parallelepiped that quartz crucible wall 1 is up/down perforation, at the bottom of plumbago crucible, 2 shape of cross section is consistent with the shape of cross section of quartz crucible wall 1.At the bottom of plumbago crucible, 2 is inverted T shape, and quartz crucible wall 1 lower end is positioned at along inverted T shape gap position place.
At the bottom of plumbago crucible, 2 upper surfaces are coated with silicon nitride coating.Contact with silicon melt due to graphite and can pollute silicon, prevent the secondary pollution of silicon liquid.
Embodiment 2:
As shown in Figure 1, a kind ofly be applied to the combined type copple that polysilicon directional freezing is purified, comprise at the bottom of quartz crucible wall 1 and plumbago crucible 2, at the bottom of the lower end of quartz crucible wall 1 and plumbago crucible, 2 splice mutually.
Wherein, the right cylinder that quartz crucible wall 1 is up/down perforation, at the bottom of plumbago crucible, 2 shape of cross section is consistent with the shape of cross section of quartz crucible wall 1.At the bottom of plumbago crucible, 2 offer limited impression along quartz crucible wall 1 opposite position place, lower edge, and quartz crucible wall 1 lower end is positioned at limited impression.
At the bottom of plumbago crucible, 2 upper surfaces are coated with coat of silicon carbide.Contact with silicon melt due to graphite and can pollute silicon, prevent the secondary pollution of silicon liquid.
Claims (5)
1. one kind is applied to the combined type copple that polysilicon directional freezing is purified, and at the bottom of it is characterized in that comprising quartz crucible wall and plumbago crucible, at the bottom of the lower end of quartz crucible wall and plumbago crucible, mutually splices; Wherein, the three-dimensional arrangement that the quartz crucible wall is up/down perforation, the shape of cross section at the bottom of plumbago crucible is consistent with the shape of cross section of quartz crucible wall.
2. the combined type copple that is applied to the polysilicon directional freezing purification according to claim 1, is characterized in that rectangular parallelepiped or right cylinder that the quartz crucible wall is up/down perforation.
3. according to claim 1ly be applied to the combined type copple that polysilicon directional freezing is purified, it is characterized in that plumbago crucible at the bottom of upper surface be coated with silicon nitride coating or coat of silicon carbide.
4. according to claim 1, the 2 or 3 described combined type copples that are applied to the polysilicon directional freezing purification, it is characterized in that offering limited impression along opposite position place, quartz crucible wall lower edge at the bottom of plumbago crucible, quartz crucible wall lower end is positioned at limited impression.
5. according to claim 1, the 2 or 3 described combined type copples that are applied to the polysilicon directional freezing purification, it is characterized in that at the bottom of plumbago crucible be inverted T shape, quartz crucible wall lower end is positioned at along inverted T shape gap position place.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310421117.2A CN103482632A (en) | 2013-09-16 | 2013-09-16 | Combined type crucible applied to directional solidification and purification of polycrystalline silicon |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104048505A (en) * | 2014-05-24 | 2014-09-17 | 长沙湘愿节能科技有限公司 | Large pressure-bearing wedged sealed combination graphite crucible and fabrication method thereof |
| CN106133207A (en) * | 2014-03-06 | 2016-11-16 | Ald 真空技术股份有限公司 | Mixing crucible for material crystalline |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101479410A (en) * | 2006-06-23 | 2009-07-08 | Rec斯坎沃佛股份有限公司 | Method and crucible for direct solidification of semiconductor grade multi-crystalline silicon ingots |
| CN101928980A (en) * | 2010-09-17 | 2010-12-29 | 浙江碧晶科技有限公司 | Seeding guidance die for growing silicon crystal by directional solidification method |
| CN201713324U (en) * | 2009-04-01 | 2011-01-19 | 北京京运通科技股份有限公司 | Technological crucible device for polysilicon growth |
| CN203486914U (en) * | 2013-09-16 | 2014-03-19 | 青岛隆盛晶硅科技有限公司 | Combined crucible applied to polycrystalline silicon directional solidification and purification |
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2013
- 2013-09-16 CN CN201310421117.2A patent/CN103482632A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101479410A (en) * | 2006-06-23 | 2009-07-08 | Rec斯坎沃佛股份有限公司 | Method and crucible for direct solidification of semiconductor grade multi-crystalline silicon ingots |
| CN201713324U (en) * | 2009-04-01 | 2011-01-19 | 北京京运通科技股份有限公司 | Technological crucible device for polysilicon growth |
| CN101928980A (en) * | 2010-09-17 | 2010-12-29 | 浙江碧晶科技有限公司 | Seeding guidance die for growing silicon crystal by directional solidification method |
| CN203486914U (en) * | 2013-09-16 | 2014-03-19 | 青岛隆盛晶硅科技有限公司 | Combined crucible applied to polycrystalline silicon directional solidification and purification |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106133207A (en) * | 2014-03-06 | 2016-11-16 | Ald 真空技术股份有限公司 | Mixing crucible for material crystalline |
| EP3114259A1 (en) * | 2014-03-06 | 2017-01-11 | Ald Vacuum Technologies GmbH | Hybrid crucible for crystallizing materials |
| EP3114259B1 (en) * | 2014-03-06 | 2023-07-12 | ALD Vacuum Technologies GmbH | Hybrid crucible for crystallizing materials |
| CN104048505A (en) * | 2014-05-24 | 2014-09-17 | 长沙湘愿节能科技有限公司 | Large pressure-bearing wedged sealed combination graphite crucible and fabrication method thereof |
| CN104048505B (en) * | 2014-05-24 | 2016-09-21 | 青岛百顿坩埚有限公司 | Large-scale pressure-bearing wedge-type seal combination type graphite crucible and preparation method thereof |
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Application publication date: 20140101 |