CN107488873A - A kind of method of silicon ingot casting - Google Patents
A kind of method of silicon ingot casting Download PDFInfo
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- CN107488873A CN107488873A CN201710852270.9A CN201710852270A CN107488873A CN 107488873 A CN107488873 A CN 107488873A CN 201710852270 A CN201710852270 A CN 201710852270A CN 107488873 A CN107488873 A CN 107488873A
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- silicon
- silicon material
- silicon ingot
- ingot
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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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/02—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method without using solvents
-
- 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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- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a kind of method of silicon ingot casting, and the dopant of doped chemical is added in silicon material, and the silicon material is heated into molten state in the crucible of single crystal growing furnace, stop heating, cool down the silicon material so that silicon material solidifies in 2h, obtains the silicon ingot containing doped chemical.The silicon casting ingot method that the present invention uses, because silicon material solidifies in the short period of time, avoid fractional condensation of the doped chemical in silicon material, the uniformity of silicon ingot resistivity is ensure that, relative to prior art, without being drawn to the silicon material of molten state to obtain silicon ingot, operating process is simpler, and production cost is low, producing the silicon ingot of acquisition has uniform resistivity, and the solar cell prepared by the silicon ingot has preferable service behaviour.
Description
Technical field
The present invention relates to semiconductor preparation field, more particularly to a kind of method of silicon ingot casting.
Background technology
In photovoltaic industry, so-called foundry alloy is exactly the alloy of impurity element and silicon, and main is exactly that silicon material is doped,
For changing the concentration of donor impurity or acceptor impurity in silicon melt, its monocrystalline to grow out or polycrystalline resistor rate is set to reach both
Provisioning request.
The currently used method for preparing foundry alloy silicon ingot mainly draws silicon ingot once Cheng Jing using single crystal growing furnace.Using this
Preparation method manufactures silicon ingot, complex operation, realizes that difficulty is big, and production cost is high.
The content of the invention
It is an object of the invention to provide a kind of method of silicon ingot casting, solves the silicon ingot process containing doped chemical of preparation
In, the problem of operating procedure is complicated, and production cost is high.
In order to solve the above technical problems, the present invention provides a kind of method of silicon ingot casting, including:
The dopant of doped chemical is added in silicon material, and the silicon material is loaded in the crucible of single crystal growing furnace;By described
Single crystal growing furnace heats to the silicon material;After the silicon material is completely melt, stop heating, the silicon material of molten state is caused in 2h
Solidification, obtains the silicon ingot containing doped chemical.
Wherein, it is described heating is carried out to the silicon material by the single crystal growing furnace to include:
The silicon material is heated in the atmosphere of argon gas, in heating process, the flow of the argon gas is the
One flow value;
The cooling silicon material includes:
The flow of argon gas in single crystal growing furnace by first-class value is increased into second value.
Wherein, the first-class value is 25-35slm, and the second value is 45-55slm.
Wherein, it is described heating is carried out to the silicon material by the single crystal growing furnace to include:
The heating power of the heater of the single crystal growing furnace is set as 90-95KW, the silicon material is only added with a period of time
Heat so that the silicon material is completely melt as molten state.
Wherein, described after the silicon material is completely melt, stopping heating including:
The heating power of the single crystal growing furnace is down to 0KW by the segmentation of current heating power value;
Adjust the crucible position of crucible so that the silicon material of molten state is gradually solidified upwards by crucible bottom.
Wherein, after acquisition contains and mixes the silicon ingot of element, in addition to:
The silicon ingot after cooling is separated with crucible, the outer surface of the silicon ingot polished or sandblasting, then it is right
The silicon ingot is cleaned and dried.
Wherein, it is described cleaning is carried out to the silicon ingot to include:
Cleaned after the silicon ingot hydrofluoric acid dips, then with mixed acid, wherein the mixed acid is the mixed of HF and HNO3
Conjunction solution, HF and HNO3 concentration ratio are 1:(8~10).
Wherein, after the foundry alloy is cleaned and dried, in addition to:
The silicon ingot is divided into the silicon ingot block less than 30*30mm.
Wherein, it is described to include the dopant that doped chemical is added in silicon material:
The silicon raw material containing doped chemical is selected, wherein doped chemical concentration is not less than the default density in the silicon raw material
And no more than doped chemical concentration value in silicon ingot, and the summation of metallic element concentration is not higher than 1000ppmv in the silicon raw material;
The dopant of doped chemical is added into the silicon raw material according to target resistivity, obtains the silicon material doped with dopant.
Wherein, the doped chemical is boron element or P elements.
The method of a kind of silicon ingot casting provided by the present invention, by the way that the dopant containing doped chemical is added into silicon material
In, and by after silicon material heating and melting, stop heating, make silicon material cooled and solidified in 2h, because the freezing point temperature of silicon material is higher,
Stop after heating by heat transfer, silicon material can quick cooled and solidified within a short period of time, so as to cause the doping member in silicon material
Element has not occurred fractional condensation, and just whole cooled and solidifieds have been solid to silicon material, so as to obtain the silicon of doped chemical general uniform distribution
Ingot, because doped chemical has preferable uniformity in silicon ingot, therefore the resistivity for obtaining silicon ingot is also just comparatively uniform.
Preparation method provided by the invention, not only the simple production cost of operating procedure is low, and the resistivity of the silicon ingot prepared
Also it is comparatively uniform so that the solar cell prepared by the silicon ingot has preferable service behaviour, is advantageous to the sun
The popularization of energy battery applications.
Brief description of the drawings
, below will be to embodiment or existing for the clearer explanation embodiment of the present invention or the technical scheme of prior art
The required accompanying drawing used is briefly described in technology description, it should be apparent that, drawings in the following description are only this hair
Some bright embodiments, for those of ordinary skill in the art, on the premise of not paying creative work, can be with root
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is a kind of flow chart of silicon casting ingot method provided in an embodiment of the present invention;
Fig. 2 is the cross-sectional view of crucible and heater relative position in the embodiment of the present invention;
Fig. 3 is to the test point distribution schematic diagram of fixed resistance rate detection in the embodiment of the present invention;
In accompanying drawing, 1 it is heater, 2 is crucible, 3 is silicon material, 4 is liquid level, 5 is silicon ingot, 6 is test point.
Embodiment
The core of the present invention is to provide a kind of method of silicon ingot casting, and whole preparation process is simple to operate, and production cost is low, and
The resistivity evenness for obtaining silicon ingot is good.
In order that those skilled in the art more fully understand the present invention program, with reference to the accompanying drawings and detailed description
The present invention is described in further detail.Obviously, described embodiment is only part of the embodiment of the present invention, rather than
Whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not making creative work premise
Lower obtained every other embodiment, belongs to the scope of protection of the invention.
Fig. 1 is refer to, Fig. 1 is a kind of flow chart of silicon casting ingot method provided in an embodiment of the present invention, and this method can wrap
Include:
Step S101:The dopant of doped chemical is added in silicon material, and the silicon material is loaded in the crucible of single crystal growing furnace.
Step S102:The silicon material is heated by the single crystal growing furnace.
Step S103:After the silicon material is completely melt, stop heating, the silicon material solidification of molten state is caused in 2h, is obtained
Obtain the silicon ingot containing doped chemical.
It is current conventional prepare silicon ingot during, usually by after silicon material heating and melting, monocrystalline is drawn into silicon material
Rod is so as to obtain silicon ingot, in whole pulling process, it is necessary to silicon material continuous heating, avoid pulling monocrystal rod duration compared with
Long, remaining silicon material solidifies, in addition, during pulling monocrystal rod, there is also very strict technological requirement, otherwise very
Easily cause monocrystal rod nonconforming, can be segregated in silicon material additionally, due to doped chemical, the head of the monocrystal rod of production
Concentration with afterbody doped chemical is also what is differed.
In the present invention, after silicon material is heated into molten condition, stop heating, it is quick to cool down, and by silicon material in 2h
Solidification obtain silicon ingot, due to silicon material by molten state to solidify state process duration it is relatively short, the doped chemical in silicon material
Fractional condensation is had not occurred, silicon material i.e. solidification completely, therefore, in the silicon ingot of acquisition comparatively the concentration of doped chemical is also that comparison is equal
Even, and the present invention is in terms of existing technologies, without carrying out the drawing of monocrystal rod, this considerably simplifies whole
The operating process of silicon ingot casting, while also largely reduce production cost.
In addition, it is necessary to explanation, because the freezing point temperature of silicon material is higher, probably in 1400 degrees centigrades, silicon material
By heat transfer can in 2h within be frozen into silicon ingot, after silicon material solidification, temperature in single crystal growing furnace is still significantly larger than room
Temperature makes the temperature in single crystal growing furnace be cooled to close to normal temperature state, it is necessary to persistently cool down 2-3h again, can tear stove open, obtains silicon ingot.
Based on above-described embodiment, in order to accelerate the process of setting of silicon material, can be wrapped in another specific embodiment of the invention
Include:
In the silicon material heating in single crystal growing furnace, the silicon material is heated in the atmosphere of argon gas, heated
During, the flow of the argon gas is first-class value;
When cooling down the silicon material, the flow of argon gas in single crystal growing furnace is increased into second value by first-class value.
In order to accelerate the speed of silicon material cooled and solidified, it can increase the flow value for being passed through argon gas when cooling down silicon material, pass through
Heat transfer between argon gas and silicon material absorbs the heat of silicon material, accelerates the cooling of silicon material, the argon flow amount value being passed through can be by
First-class value originally directly increases to second value or is gradually increased to second flow by first-class value
Value, but first way is more preferable to the effect of the quick cooled and solidified of silicon material.
In actual mechanical process, because argon gas is passed through from top to bottom from single crystal growing furnace, so in crucible, argon gas
The heat of silicon material upper surface in crucible can be more absorbed, it is a large amount of to absorb silicon material upper table if the flow velocity that argon gas is passed through is too fast
The heat in face, it may result in silicon material a part of above in crucible and solidified, and the silicon material positioned at crucible bottom is not coagulated
Gu so as to cause the heat of crucible bottom silicon material can not be gone out by silicon material quick heat radiating a part of above, once crucible bottom
Portion's silicon material solidification, extremely easily bursts crucible bottom, causes crucible to burst, so as to cause serious accident, therefore cold
But during silicon material, the flow for the argon gas being passed through just needs in right amount.Therefore, can further be improved in the present invention, including:
The first-class value is 25-35slm, and the second value is 45-55slm.
Specific first-class value can be 25slm, 27slm, 30slm, 33slm, 35slm etc., and second value can be with
For 45slm, 47slm, 50slm, 53slm, 55slm etc..
Based on above-described embodiment, in another specific embodiment of the invention, can include:
The heating power of the heater of the single crystal growing furnace is set as 90-95KW, the silicon material is only added with a period of time
Heat so that the silicon material is completely melt as molten state.
After melting silicon materials are molten condition, in order to ensure that silicon material can solidify within the time as short as possible, avoid
Doped chemical segregates in silicon material, so the heating power of the heater in single crystal growing furnace is unsuitable excessive, avoid be silicon material temperature
It is too high, cause the overlong time of silicon material cooled and solidified.But if heating power is too low, it is possible to cause silicon material heating inadequate,
Fusing time is lasting long, reduces operating efficiency.Therefore whether heating power setting is properly to influence whole silicon ingot casting mistake
One of an important factor for journey.Heating power in the present invention can be any including endpoint value between 90-95KW
Performance number, can be specifically 90KW, 91KW, 92KW, 93KW, 94KW, 95KW etc..
After silicon material is heated into complete molten condition, the temperature in single crystal growing furnace is of a relatively high, if now stopping heating, makes
Heater heating power is 0KW, then the temperature of crucible outer surface may drastically change, this be to crucible it is very unfavorable,
Serious can even burst, and produce serious accident, be that can also further be improved in this present embodiment, including:
The heating power of the single crystal growing furnace is down to 0KW by the segmentation of current heating power value, specifically, for example, heater
Heating power is 90KW, then can reduce heating power successively according to 75KW, 50KW, 35KW, 20KW, 0KW order, heat
The speed of device power drop can be set according to actual conditions.
As described in above-mentioned embodiment, in cooled and solidified silicon material, in order to prevent crucible from explosion occurs, it is necessary to which silicon material is had into earthenware
The gradual upward cooled and solidified in crucible bottom, therefore, in the present embodiment, can adjust crucible crucible position so that the silicon material of molten state
Gradually solidified upwards by crucible bottom, specifically, refer to Fig. 2, Fig. 2 is crucible in the embodiment of the present invention and heater with respect to position
Highest temperature position is heated in the cross-sectional view put, the position in Fig. 2 between dotted line for heater 1, can be according to actual earthenware
The amount of silicon material 3 in crucible 2 adjusts crucible position up and down, if liquid level 4 of the silicon material 2 of molten condition in crucible is located exactly at heater
1 temperature highest horizontal plane, then need not adjust crucible 2, if liquid level 4 is not in the temperature highest horizontal plane of heater 1, that
The crucible position of adjustment crucible 2 up and down, the liquid level 4 of silicon material is set to pass through heater exactly with the temperature highest horizontal plane of heater 1
1 residual temperature suitably slows down the cooled and solidified process of a part above silicon material 3 in crucible 2.
Based on above-mentioned any embodiment, also include in another specific embodiment of the invention:
Obtaining containing after mixing the silicon ingot of element, the silicon ingot after cooling is being separated with crucible, to the silicon ingot
Outer surface polished or sandblasting, then the silicon ingot is cleaned and dried.
In order to which the silicon ingot obtained to production cleans, the waste material on silicon ingot surface is removed, after the cooling period, can be by single crystal growing furnace
Tear stove open, isolate the silicon ingot in crucible, silicon ingot is polished or sandblasting, the thickness of polishing or sandblasting can be 2-5mm.
In addition, after cleaning to silicon ingot can specifically use hydrofluoric acid dips, then cleaned with mixed acid, mixed acid be HF and
HNO3 mixed solution, HF and HNO3 concentration ratio are 1:(8~10), quickly the waste material on silicon material surface can be disposed.
Based on above-described embodiment because for whole silicon ingot, the concentration of doped chemical be it is substantial uniform, in order to
The silicon ingot being more uniformly distributed is obtained, the present invention can further be improved, can specifically included:
The silicon ingot is divided into the silicon ingot block less than 30*30mm, 30*30mm size to for whole big silicon ingot and
Speech, size are very small, therefore, for the less silicon ingot block of size, can consider doped chemical in whole silicon ingot block substantially
It is equally distributed, even if also saying that resistivity is uneven in silicon ingot block error is small to can ignore completely.
During in order to prevent that certain part doped chemical spreads in silicon material in silicon ingot, skewness, silicon ingot is obtained in production
Afterwards, Resistivity testing can be first carried out to whole silicon ingot, specifically usable KDY-1 resistivity testers, reading requirement is accurate
To 0.0001 Ω cm, four probe directions must be parallel with cutting lines during test, first carries out an inspection, is detected again after point inspection is qualified
The resistivity of silicon ingot.The distribution of tested measuring point specifically refers to Fig. 3, and Fig. 3 is that fixed resistance rate is detected in the embodiment of the present invention
Test point distribution schematic diagram, test point 6 is substantially evenly distributed on the surface of silicon ingot 5 in Fig. 3, but this is not uniquely to detect
The distribution mode of point 6, each section test point 6 of silicon ingot 5 are no less than 20 points, each test point 6 are detected one by one, until reading
Number stablizes constant rear record reading.
Based on above-described embodiment, it is contemplated that if adding doping into silicon raw material as silicon raw material using the silicon of high-purity
Agent, the silicon raw material of high-purity can undoubtedly increase production cost, are in this another specific embodiment provided by the invention, can wrap
Include:
The silicon raw material containing doped chemical is selected, wherein doped chemical concentration is not less than the default density in the silicon raw material
And no more than doped chemical concentration value in silicon ingot.Specifically, doping concentration may be selected close to the silicon raw material of target doping concentration, mesh
Mark doping concentration is finally to need the doping concentration of doped chemical in the silicon ingot that obtains;And currently used raw material be 6N levels with
On HIGH-PURITY SILICON and high-purity dopant, the cost of both raw materials is higher, and former using the silicon containing dopant in the present invention
Material prepares silicon ingot, not only reduces the cost of silicon raw material, also reduces the dosage of dopant, therefore the solution of the present invention can be
Largely reduce the production cost of silicon ingot.
In addition, the summation of metallic element concentration is not higher than 1000ppmv in silicon raw material, in order to avoid the too high shadow of metallic element concentration
Ring the quality of silicon ingot;
The dopant of doped chemical is added into the silicon raw material according to target resistivity, obtains the institute doped with dopant
Silicon material is stated, target resistivity and target doping concentration are mutually corresponding, and target doping concentration and target resistivity meet:Wherein N is target doping concentration, and ρ is target resistivity.
Based on above-described embodiment, in another specific embodiment of the invention, doped chemical can be specifically that boron element also may be used
To be P elements, other doped chemicals are can also be.
For boron element, it is 0.8, very close 1 in the middle fractional condensation system of solid and liquid, quickly cools down molten state
During silicon material, boron also has little time to segregate, and silicon has just been cooled to solid-state, that is to say, that instantaneous cooling, in solid-state and liquid state diffusion
Speed approach, even silicon material cooled and solidified relative time is long, and the distribution of the roc element in silicon ingot can also ensure greatly
Uniform when on body, segregation coefficient is 0.3 for P elements, the speed for just needing to accelerate silicon material cooled and solidified as far as possible for this
Degree.
It should be noted that each embodiment is described by the way of progressive in this specification, each embodiment emphasis is said
Bright is all the difference with other embodiment, between each embodiment identical similar portion mutually referring to.
The foregoing description of the disclosed embodiments, professional and technical personnel in the field are enable to realize or using the present invention.
A variety of modifications to these embodiments will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention
The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one
The most wide scope caused.
Claims (10)
- A kind of 1. method of silicon ingot casting, it is characterised in that including:The dopant of doped chemical is added in silicon material, and the silicon material is loaded in the crucible of single crystal growing furnace;The silicon material is heated by the single crystal growing furnace;After the silicon material is completely melt, stop heating, the silicon material solidification of molten state is caused in 2h, acquisition contains doped chemical Silicon ingot.
- 2. according to the method for claim 1, it is characterised in that described that the silicon material is heated by the single crystal growing furnace Including:The silicon material is heated in the atmosphere of argon gas, in heating process, the flow of the argon gas is first-class Value;The cooling silicon material includes:The flow of argon gas in single crystal growing furnace by first-class value is increased into second value.
- 3. according to the method for claim 2, it is characterised in that the first-class value is 25-35slm, the second Value is 45-55slm.
- 4. according to the method for claim 3, it is characterised in that described that the silicon material is heated by the single crystal growing furnace Including:The heating power of the heater of the single crystal growing furnace is set as 90-95KW, to the silicon material only with the heating of a period of time, is made The silicon material is obtained to be completely melt as molten state.
- 5. according to the method for claim 4, it is characterised in that it is described after the silicon material is completely melt, stop heating bag Include:The heating power of the single crystal growing furnace is down to 0KW by the segmentation of current heating power value;Adjust the crucible position of crucible so that the silicon material of molten state is gradually solidified upwards by crucible bottom.
- 6. according to the method for claim 1, it is characterised in that also include after obtaining containing the silicon ingot for mixing element:The silicon ingot after cooling is separated with crucible, the outer surface of the silicon ingot polished or sandblasting, then to described Silicon ingot is cleaned and dried.
- 7. according to the method for claim 6, it is characterised in that described cleaning is carried out to the silicon ingot to include:Cleaned after the silicon ingot hydrofluoric acid dips, then with mixed acid, wherein the mixed acid is HF and HNO3Mixing it is molten Liquid, HF and HNO3Concentration ratio be 1:(8~10).
- 8. according to the method for claim 7, it is characterised in that after the foundry alloy is cleaned and dried, also Including:The silicon ingot is divided into the silicon ingot block less than 30*30mm.
- 9. according to the method described in any one of claim 1 to 8, it is characterised in that described doped chemical to be added in silicon material Dopant includes:The silicon raw material containing doped chemical is selected, wherein doped chemical concentration is not less than the default density and not in the silicon raw material More than doped chemical concentration value in silicon ingot, and the summation of metallic element concentration is not higher than 1000ppmv in the silicon raw material;The dopant of doped chemical is added into the silicon raw material according to target resistivity, obtains the silicon doped with dopant Material.
- 10. according to the method for claim 9, it is characterised in that the doped chemical is boron element or P elements.
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Cited By (2)
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CN109056063A (en) * | 2018-08-29 | 2018-12-21 | 孟静 | The preparation method of polycrystalline silicon used for solar battery piece |
CN114059152A (en) * | 2021-11-19 | 2022-02-18 | 包头美科硅能源有限公司 | Gallium element doping method for producing silicon single crystal rod by Czochralski method |
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CN102817075A (en) * | 2012-08-18 | 2012-12-12 | 安阳市凤凰光伏科技有限公司 | Master alloy production method by using polycrystalline foundry furnace |
CN104195638A (en) * | 2014-09-01 | 2014-12-10 | 大连理工大学 | Method for preparing boron master alloy by using metallurgy method |
CN105780114A (en) * | 2016-05-20 | 2016-07-20 | 江苏协鑫硅材料科技发展有限公司 | Silicon ingot and preparation method thereof |
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CN102817075A (en) * | 2012-08-18 | 2012-12-12 | 安阳市凤凰光伏科技有限公司 | Master alloy production method by using polycrystalline foundry furnace |
CN104195638A (en) * | 2014-09-01 | 2014-12-10 | 大连理工大学 | Method for preparing boron master alloy by using metallurgy method |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN109056063A (en) * | 2018-08-29 | 2018-12-21 | 孟静 | The preparation method of polycrystalline silicon used for solar battery piece |
CN114059152A (en) * | 2021-11-19 | 2022-02-18 | 包头美科硅能源有限公司 | Gallium element doping method for producing silicon single crystal rod by Czochralski method |
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Application publication date: 20171219 |