CN105926037A - Method for removing hard-spot insoluble substances from polycrystalline silicon - Google Patents
Method for removing hard-spot insoluble substances from polycrystalline silicon Download PDFInfo
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- CN105926037A CN105926037A CN201610410891.7A CN201610410891A CN105926037A CN 105926037 A CN105926037 A CN 105926037A CN 201610410891 A CN201610410891 A CN 201610410891A CN 105926037 A CN105926037 A CN 105926037A
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- polysilicon
- hard
- hard inclusion
- quartz sand
- polycrystalline silicon
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
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- Crystallography & Structural Chemistry (AREA)
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- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to a method for removing hard-spot insoluble substances from polycrystalline silicon and belongs to the technical field of polycrystalline silicon. The method includes selecting polycrystalline silicon cast ingots/top and side claddings produced during purification as raw materials, heating the polycrystalline silicon cast ingots/top and side claddings by intermediate-frequency coil induction to be molten, controlling intermediate-frequency current, adding quartz sand to remove hard spots in silicon liquid, removing slag agents rich in the hard spots through a graphite ladle, and pouring the purified silicon liquid into cooling packages so as to obtain the polycrystalline silicon with the hard spots removed. The method for removing the hard-spot insoluble substances from the polycrystalline silicon solves the problems of poor removal effect, difficulty in separation, high-temperature insolubility and severe product wastage of a traditional method and is remarkable in hard spot removal effect and simple in required devices, thereby being promising in industrial application prospect.
Description
Technical field
The present invention relates to a kind of remove the method for Hard Inclusion insoluble matter in polysilicon, belong to field of polysilicon technology.
Background technology
In recent years, solaode market development is swift and violent, and the shortage of HIGH-PURITY SILICON material makes people produce the regeneration of HIGH-PURITY SILICON material
Keen interest and enthusiasm are given birth to.Select polycrystalline cast ingot top/edge skin material, and polycrystalline purifies ingot top/edge skin material as raw material, process
After Regeneration Treatment, carrying out efficient polycrystalline silicon ingot, the development to photovoltaic industry is most important.
Polycrystalline cast ingot top/edge skin material and polycrystalline purify in ingot top/side skin material rich in substantial amounts of impurity, Hard Inclusion granule, and
It is mingled with bubble.Traditional chemical method does not has obvious effect to the removal of the impurity in silicon material, Hard Inclusion and bubble.Common
The composition of Hard Inclusion granule be SiC and Si3N4.The producing cause of SiC is as follows: during high temperature ingot casting, graphite heating body
Doping to silicon melt causes silicon ingot surface to define one layer of SiC particulate；Si3N4Main source: silica crucible coating diffusion.
SiC and Si3N4All there is the fusing point of superelevation, and insoluble in acid, alkali, general method is difficult to be isolated.
The method that current industrialization process many employings acidleach is peeled off removes the Hard Inclusion granule of polysilicon surface, but is removing
During Hard Inclusion, a large amount of losses of silicon can be caused.Therefore, when in polysilicon rich in substantial amounts of Hard Inclusion SiC and Si3N4,
And when being mingled with substantial amounts of bubble, the method for traditional middle low-temperature bake, directional purification and acidleach is all unable to reach the effect of removal
Really.
Summary of the invention
It is an object of the invention to provide and a kind of remove the method for Hard Inclusion insoluble matter in polysilicon, solve present in traditional method
Poor removal effect, separate difficulty, high temperature indissoluble, problem that product wastage is big, have removal effect significantly, safety and environmental protection,
It is easy to the feature of industrial applications.
The method of Hard Inclusion insoluble matter in removal polysilicon of the present invention, comprises the following steps:
(1) the top skin that produced in ingot casting or purification process by polysilicon, edge skin material, as raw material, once purged are placed in intermediate frequency sense
In answering the crucible of stove；
(2) start heating, after raw material melts completely, add quartz sand, be then incubated after quartz sand is completely melt；
(3) claw upper strata slag agent with graphite spoon after agitated, obtain removing the polysilicon of Hard Inclusion after cooling.
Wherein:
In step (1), in raw material, the content of silicon is 90-99wt%, and its rich surface contains pore and Hard Inclusion.
When melting raw material in step (2), the heating power of intermediate frequency furnace is 40-150kW, and heat time heating time is 1-2h.
In step (2), quartz sand is 1:50-200 with the mass ratio of raw material.
When adding quartz sand in step (2), the heating power of intermediate frequency furnace is 40-80kW, and the joining day controls
10-30min,；When quartz sand is completely melt, the heating power of intermediate frequency furnace is 80-120kW, and fusing time controls
10-30min；During insulation, the heating power of intermediate frequency furnace is 120-150kW, and temperature retention time controls at 10-30min.
In step (2), holding temperature is maintained at 1650-1850 DEG C.
In step (2), the granularity of quartz sand is 0.1-2mm, and purity is 99.99%.
In step (3), mixing time is 5-30min.
Beneficial effects of the present invention is as follows:
The present invention selects the polycrystalline silicon ingot casting/top skin of purification process generation, edge skin material as raw material, is realized by fusing, slagging-off
The removal of Hard Inclusion, required equipment is simple, and the effect removing Hard Inclusion is notable, and industrial applications has a extensive future.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
Remove the method for Hard Inclusion insoluble matter in polysilicon, comprise the following steps:
(1) the top skin that produced during ingot casting by 100kg polysilicon, edge skin material, as raw material, once purged are placed in intermediate frequency sense
In answering the crucible of stove；Wherein, in raw material, the content of silicon is 91wt%；
(2) starting heating, the heating power of intermediate frequency furnace is 50kW, and heat time heating time is 0.5h, and heating-up temperature is 1700 DEG C,
After raw material melts completely add 1kg granularity be 0.1-2mm, purity be the quartz sand of 99.99%, then treat that quartz sand is the most molten
It is incubated after change；Wherein, when adding quartz sand, the heating power of intermediate frequency furnace is 80kW, and the joining day is 10min；
When quartz sand is completely melt, the heating power of intermediate frequency furnace is 100kW, and fusing time is 10min；Medium frequency induction during insulation
The heating power of stove is 120kW, and temperature retention time is 10min；
(3) claw upper strata slag agent with graphite spoon after stirring 10min, obtain removing the polysilicon of Hard Inclusion after cooling.After testing,
The clearance of Hard Inclusion is 99%.
Embodiment 2
Remove the method for Hard Inclusion insoluble matter in polysilicon, comprise the following steps:
(1) the top skin that produced during ingot casting by 50kg polysilicon, edge skin material, as raw material, once purged are placed in intermediate frequency sense
In answering the crucible of stove；Wherein, in raw material, the content of silicon is 94wt%；
(2) starting heating, the heating power of intermediate frequency furnace is 40kW, and heat time heating time is 1h, and heating-up temperature is 1650 DEG C,
After raw material melts completely add 1kg granularity be 0.1-2mm, purity be the quartz sand of 99.99%, then treat that quartz sand is the most molten
It is incubated after change；Wherein, when adding quartz sand, the heating power of intermediate frequency furnace is 50kW, and the joining day is 20min；
When quartz sand is completely melt, the heating power of intermediate frequency furnace is 80kW, and fusing time is 20min；Intermediate frequency furnace during insulation
Heating power be 130kW, temperature retention time is 20min；
(3) claw upper strata slag agent with graphite spoon after stirring 5min, obtain removing the polysilicon of Hard Inclusion after cooling.After testing,
The clearance of Hard Inclusion is more than 99.5%.
Embodiment 3
Remove the method for Hard Inclusion insoluble matter in polysilicon, comprise the following steps:
(1) the top skin that produced during ingot casting by 200kg polysilicon, edge skin material, as raw material, once purged are placed in intermediate frequency sense
In answering the crucible of stove；Wherein, in raw material, the content of silicon is 97wt%；
(2) starting heating, the heating power of intermediate frequency furnace is 150kW, and heat time heating time is 2h, and heating-up temperature is 1850 DEG C,
After raw material melts completely add 1kg granularity be 0.1-2mm, purity be the quartz sand of 99.99%, then treat that quartz sand is the most molten
It is incubated after change；Wherein, when adding quartz sand, the heating power of intermediate frequency furnace is 40kW, and the joining day is 30min；
When quartz sand is completely melt, the heating power of intermediate frequency furnace is 120kW, and fusing time is 30min；Medium frequency induction during insulation
The heating power of stove is 150kW, and temperature retention time is 30min；
(3) claw upper strata slag agent with graphite spoon after stirring 30min, obtain removing the polysilicon of Hard Inclusion after cooling.After testing,
The clearance of Hard Inclusion is 99.9%.
Claims (7)
1. remove the method for Hard Inclusion insoluble matter in polysilicon for one kind, it is characterised in that: comprise the following steps:
(1) the top skin that produced in ingot casting or purification process by polysilicon, edge skin material, as raw material, once purged are placed in intermediate frequency sense
In answering the crucible of stove；Wherein, in described raw material, the content of silicon is 90-99wt%, and its rich surface contains pore and Hard Inclusion；
(2) start heating, after raw material melts completely, add quartz sand, be then incubated after quartz sand is completely melt；
(3) claw upper strata slag agent with graphite spoon after agitated, obtain removing the polysilicon of Hard Inclusion after cooling.
The method of Hard Inclusion insoluble matter in removal polysilicon the most according to claim 1, it is characterised in that: step (2)
During middle thawing raw material, the heating power of intermediate frequency furnace is 40-150kW, and heat time heating time is 0.5-2h.
The method of Hard Inclusion insoluble matter in removal polysilicon the most according to claim 1, it is characterised in that: step (2)
Middle quartz sand is 1:50-200 with the mass ratio of raw material.
The method of Hard Inclusion insoluble matter in removal polysilicon the most according to claim 1, it is characterised in that: step (2)
During middle addition quartz sand, the heating power of intermediate frequency furnace is 40-80kW；When quartz sand is completely melt, adding of intermediate frequency furnace
Thermal power is 80-120kW；During insulation, the heating power of intermediate frequency furnace is 120-150kW.
The method of Hard Inclusion insoluble matter in removal polysilicon the most according to claim 1, it is characterised in that: step (2)
Middle holding temperature is 1650-1850 DEG C.
The method of Hard Inclusion insoluble matter in removal polysilicon the most according to claim 1, it is characterised in that: step (2)
The granularity of middle quartz sand is 0.1-2mm, and purity is 99.99%.
The method of Hard Inclusion insoluble matter in removal polysilicon the most according to claim 1, it is characterised in that: step (3)
Middle mixing time is 5-30min.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101218176A (en) * | 2005-07-04 | 2008-07-09 | 夏普株式会社 | Recycling method for silicon, silicon and silicon ingot prepared by the method |
| CN101837348A (en) * | 2010-04-28 | 2010-09-22 | 江西赛维Ldk太阳能高科技有限公司 | Method for separating silicon from impurities |
| CN102134075A (en) * | 2011-01-24 | 2011-07-27 | 云南乾元光能产业有限公司 | Novel method for producing solar-grade polysilicon |
| CN102491338A (en) * | 2011-11-22 | 2012-06-13 | 虞海盈 | Method for producing polysilicon |
| CN103342363A (en) * | 2013-06-19 | 2013-10-09 | 青岛隆盛晶硅科技有限公司 | Slag-forming agent convenient for silicon slag separation in medium smelting of polycrystalline silicon, and application method thereof |
| CN104499049A (en) * | 2014-12-29 | 2015-04-08 | 江西赛维Ldk太阳能高科技有限公司 | Method for removing polysilicon hard inclusion in ingot casting process |
-
2016
- 2016-06-08 CN CN201610410891.7A patent/CN105926037B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101218176A (en) * | 2005-07-04 | 2008-07-09 | 夏普株式会社 | Recycling method for silicon, silicon and silicon ingot prepared by the method |
| CN101837348A (en) * | 2010-04-28 | 2010-09-22 | 江西赛维Ldk太阳能高科技有限公司 | Method for separating silicon from impurities |
| CN102134075A (en) * | 2011-01-24 | 2011-07-27 | 云南乾元光能产业有限公司 | Novel method for producing solar-grade polysilicon |
| CN102491338A (en) * | 2011-11-22 | 2012-06-13 | 虞海盈 | Method for producing polysilicon |
| CN103342363A (en) * | 2013-06-19 | 2013-10-09 | 青岛隆盛晶硅科技有限公司 | Slag-forming agent convenient for silicon slag separation in medium smelting of polycrystalline silicon, and application method thereof |
| CN104499049A (en) * | 2014-12-29 | 2015-04-08 | 江西赛维Ldk太阳能高科技有限公司 | Method for removing polysilicon hard inclusion in ingot casting process |
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