CN104878448A - Polycrystalline silicon zone melting equipment employing electron beam and method for removing impurities - Google Patents
Polycrystalline silicon zone melting equipment employing electron beam and method for removing impurities Download PDFInfo
- Publication number
- CN104878448A CN104878448A CN201510252743.2A CN201510252743A CN104878448A CN 104878448 A CN104878448 A CN 104878448A CN 201510252743 A CN201510252743 A CN 201510252743A CN 104878448 A CN104878448 A CN 104878448A
- Authority
- CN
- China
- Prior art keywords
- electron beam
- zone melting
- smelting furnace
- melting crucible
- smelting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Silicon Compounds (AREA)
Abstract
The invention discloses polycrystalline silicon zone melting equipment employing an electron beam. The equipment comprises a smelting furnace and a zone smelting crucible, wherein the zone smelting crucible is arranged in the smelting furnace; an observation window is formed in the upper part of the lateral wall of the smelting furnace; a cooling water inlet and a cooling water outlet are formed in the bottom end of the smelting furnace; the polycrystalline silicon zone melting equipment is characterized in that an electronic gun is arranged above the right side of the zone smelting crucible; and the electron beam of the electronic gun moves towards a region in the right side from the left side of the zone smelting crucible, and is used for heating a silicon block paved on the zone smelting crucible. The invention further discloses a method for removing impurities employing the equipment. Continuous smelting and solidification of the silicon block are realized; through controlling the movement speed of the electron beam, elements with large steam pressure are evaporated by irradiating zone smelting through the electron beam; meanwhile, the temperature gradually changes on the left side of an irradiation region due to the movement of the electron beam, so that directional solidification is realized by the silicon liquid on the left side; the single-furnace production time is shortened; the equipment is simple; the method is feasible; and energy consumption is reduced.
Description
Technical field
The invention belongs to the technical field of physical metallurgy technology purifying polycrystalline silicon, a kind of method of specifically electron beam zone melting polysilicon equipment and despumation.
Background technology
Solar polycrystalline silicon material is topmost photovoltaic material, it is applied to solar cell, can convert solar energy into electrical energy, in today that conventional energy resources is in short supply, sun power has huge using value, and in recent years, global solar photovoltaic industry increases rapidly, solar cell yield increases fast, the direct pull sharply expansion of polysilicon demand.But the preparation technology of the manufacturing cost that solar grade polycrystalline silicon material is high and complexity is the bottleneck of restriction photovoltaic industry great development, seriously hinders popularization and the use of China's solar cell.China can autonomous production the not enough demand of solar energy polycrystalline silicon 5%, overwhelming majority starting material need import, the solar energy polycrystalline silicon technology of preparing of the applicable China's national situation of exploitation meets the requirement of national energy strategy, is the only way of China's photovoltaic industry great development.
At present, in world wide, the polycrystalline silicon used for solar battery material of preparation forms large-scale production, prepares high purity polycrystalline silicon abroad and mainly uses Siemens Method, be specially silane decomposes method and chlorosilane gas phase reduction process, wherein SiHcl
3mainstream technology prepared by the current polysilicon of Fa Ji siemens Master.SiHcl
3the useful deposition rate of method is 1 × 10
-3, be SiH
4100 times.Siemens's sedimentation velocity can reach 8 ~ 10um/min.One-pass efficiency of conversion is 5% ~ 20%, and depositing temperature is 1100 DEG C, is only second to SiCl
4(1200 DEG C), current consumption is 120kwh/kg, and silicon rod diameter reaches about 100um.The drawback that Siemens Method exists is that it takes the thermal chemical vapor deposition comparatively fallen behind on the core link of flow process, and the link of technical process is too much, and a low conversion rate, causes flow time oversize, adds material consumption, energy consumption cost.
For this reason, countries in the world all have new process with short production cycle, to pollute little, that cost is low, technique is relatively simple, scale is controlled preparation HIGH-PURITY SILICON material at active development, and metallurgy method is owing to possessing above advantage, be considered to effectively to reduce one of technology of production of polysilicon cost, become the focus competitively researched and developed countries in the world at present.Electron beam melting technology is that metallurgy method prepares one of method important in solar energy polycrystalline silicon, it utilizes the electron beam of high-energy-density as the processing method of thermal source, general electron beam melting method is after forming molten bath by thawing silicon material, under the high temperature that electron beam produces, surface evaporation removes the higher impurity of saturated vapor pressure as phosphorus, aluminium etc., then silicon liquid is poured in solidification crucible, the directional freeze effect of recycling metallic impurity, make metal when solidifying, metals content impurity in liquid state is higher than solid-state, so, the region enrichment that metallic impurity in the end solidify, high purity silicon ingot can be obtained finally by the part removing metal content enrichment.But this process control is complicated, need to continue to heat solidification crucible with electron beam, and reduce electron beam line simultaneously and temperature is reduced gradually make ingot casting from Layer by layer solidification bottom solidification crucible.Single stove production time is long, and equipment is numerous and diverse.
Summary of the invention
According to the technical problem of above-mentioned proposition, and provide one to utilize electron beam melting polycrystalline silicon technology to remove foreign matter of phosphor in polysilicon, realize the method that directional freeze removes metallic impurity simultaneously, the invention still further relates to its equipment in addition.Solidification crucible and smelting pot mainly combine by the present invention, utilize zone melting principle, in process of cooling realize directional freeze while removing vapo(u)rability impurity in melting, metallic impurity enrichment are convenient to be removed.
The technique means that the present invention adopts is as follows:
A kind of electron beam zone melting polysilicon equipment, comprise smelting furnace and be arranged on the zone melting crucible in described smelting furnace, the side wall upper part of described smelting furnace is provided with viewing window, the bottom of described smelting furnace is provided with cooling water intake and cooling water outlet, it is characterized in that: above the right side of described zone melting crucible, be provided with electron beam gun, the electron beam of described electron beam gun moves in region to the right from the left side of described zone melting crucible, and to the silico briquette heating be laid on described zone melting crucible.
The invention also discloses the method for application above-mentioned electron beam zone melting polysilicon equipment despumation, it is characterized in that comprising the steps:
S1, preparatory stage: in zone melting crucible, evenly lay the silico briquette that a layer thickness is 5cm-10cm, diameter is less than 5cm;
S2, vacuumizing phase: vacuumize, make vacuum tightness in the furnace chamber of smelting furnace be less than 5 × 10
-2pa, electron beam gun rifle body vacuum tightness is less than 5 × 10
-3pa, passes into water coolant by cooling water intake that smelting furnace is arranged and cooling water outlet;
S3, electron beam gun preheating: by the preheating from 0kw of the beam power of electron beam gun, increase 30kw-50kw every 3min-8min, until be increased to 250kw, electron beam heats the silico briquette in described zone melting crucible;
S4, smelt stage: electron beam spot is concentrated on the left of described zone melting crucible, move from left to right with the speed of 1mm/s ~ 2mm/s, in the region of electron beam irradiation, silico briquette melts, when electron beam moves to the rightmost side, immediately bundle technique is fallen to electron beam, make beam power drop to 0kw immediately from 250kw;
S5, take out the silicon ingot after solidifying, by measured resistivity and minority carrier life time, remove the high part of right side foreign matter content, leave qualified silicon ingot.
As preferably, the width of described electron beam spot is identical with the width of described zone melting crucible.
Comparatively prior art is compared, equipment of the present invention achieves the serialization melting of silico briquette and solidifies, by controlling the translational speed of electron beam, electron beam irradiation zone melting is made to evaporate the large element of vapour pressure, progressively change due to the mobile formation temperature of electron beam in the left side of irradiated region simultaneously, make the silicon liquid in left side realize directional freeze, shorten single stove production time, equipment simple method is easy, saves energy consumption.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 is the structural representation of present device.
Fig. 2 is the vertical view of Fig. 1.
In figure: 1, cooling water intake 2, cooling water outlet 3, zone melting crucible 4, silico briquette 5, smelting furnace 6, electron beam gun 7, viewing window.
Embodiment
As Fig. 1, shown in Fig. 2, a kind of electron beam zone melting polysilicon equipment, the zone melting crucible 3 comprising smelting furnace 5 and be arranged in described smelting furnace 5, the side wall upper part of described smelting furnace 5 is provided with viewing window 7, the bottom of described smelting furnace 5 is provided with cooling water intake 1 and cooling water outlet 2, electron beam gun 6 is provided with above the right side of described zone melting crucible 3, the electron beam of described electron beam gun 6 moves in region to the right from the left side of described zone melting crucible 3, and heats the silico briquette 4 be laid on described zone melting crucible 3.
The method of the present invention's application aforesaid device despumation, comprises the steps:
S1, preparatory stage: in zone melting crucible 3 (described zone melting crucible 3 adopts water jacketed copper crucible), evenly lay the silico briquette that a layer thickness is 5cm-10cm, diameter is less than 5cm;
S2, vacuumizing phase: vacuumize, make vacuum tightness in the furnace chamber of smelting furnace 5 be less than 5 × 10
-2pa, electron beam gun 6 rifle body vacuum tightness is less than 5 × 10
-3pa, by smelting furnace 5 arrange cooling water intake 1 and cooling water outlet 2 pass into water coolant;
S3, electron beam gun preheating: by the preheating from 0kw of the beam power of electron beam gun 6, increase 30kw-50kw every 3min-8min, until be increased to 250kw, electron beam heats the silico briquette 4 in described zone melting crucible 3;
S4, smelt stage: electron beam spot is concentrated on the left of described zone melting crucible 3, move from left to right with the speed of 1mm/s ~ 2mm/s, the width of described electron beam spot is identical with the width of described zone melting crucible, guarantees that electron beam spot can cover whole zone melting crucible 3 in moving process.In the region of electron beam irradiation, silico briquette melts, element such as the phosphorus that vapour pressure is large is evaporated, simultaneously, silicon liquid after thawing progressively solidifies from left to right because temperature gradually changes, due to the dephlegmation of element, metallic element concentrates on the region of silicon liquid final set, namely concentrate on the rightmost side and (guarantee described zone melting crucible 3 sufficiently long, to such an extent as to can with the movement of electron beam, left side silicon liquid solidifies gradually, right side silicon liquid is still melting state), when electron beam moves to the rightmost side, immediately bundle technique is fallen to electron beam, beam power is made to drop to 0kw immediately from 250kw,
S5, take out the silicon ingot after solidifying, by the means such as measured resistivity and minority carrier life time, remove the high part of right side foreign matter content, leave qualified silicon ingot.
The present invention is by controlling the translational speed of electron beam, electron beam irradiation zone melting crucible 3 is made to evaporate the large element of vapour pressure, progressively change due to the mobile formation temperature of electron beam in the left side of irradiated region simultaneously, the silicon liquid in left side is made to realize directional freeze, shorten single stove production time, equipment simple method is easy, saves energy consumption.
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (3)
1. an electron beam zone melting polysilicon equipment, comprise smelting furnace and be arranged on the zone melting crucible in described smelting furnace, the side wall upper part of described smelting furnace is provided with viewing window, the bottom of described smelting furnace is provided with cooling water intake and cooling water outlet, it is characterized in that: above the right side of described zone melting crucible, be provided with electron beam gun, the electron beam of described electron beam gun moves in region to the right from the left side of described zone melting crucible, and to the silico briquette heating be laid on described zone melting crucible.
2. application rights requires a method for the electron beam zone melting polysilicon equipment despumation described in 1, it is characterized in that comprising the steps:
S1, preparatory stage: in zone melting crucible, evenly lay the silico briquette that a layer thickness is 5cm-10cm, diameter is less than 5cm;
S2, vacuumizing phase: vacuumize, make vacuum tightness in the furnace chamber of smelting furnace be less than 5 × 10
-2pa, electron beam gun rifle body vacuum tightness is less than 5 × 10
-3pa, passes into water coolant by cooling water intake that smelting furnace is arranged and cooling water outlet;
S3, electron beam gun preheating: by the preheating from 0kw of the beam power of electron beam gun, increase 30kw-50kw every 3min-8min, until be increased to 250kw, electron beam heats the silico briquette in described zone melting crucible;
S4, smelt stage: electron beam spot is concentrated on the left of described zone melting crucible, move from left to right with the speed of 1mm/s ~ 2mm/s, in the region of electron beam irradiation, silico briquette melts, when electron beam moves to the rightmost side, immediately bundle technique is fallen to electron beam, make beam power drop to 0kw immediately from 250kw;
S5, take out the silicon ingot after solidifying, by measured resistivity and minority carrier life time, remove the high part of right side foreign matter content, leave qualified silicon ingot.
3. the method for despumation according to claim 2, is characterized in that: the width of described electron beam spot is identical with the width of described zone melting crucible.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510252743.2A CN104878448A (en) | 2015-05-15 | 2015-05-15 | Polycrystalline silicon zone melting equipment employing electron beam and method for removing impurities |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510252743.2A CN104878448A (en) | 2015-05-15 | 2015-05-15 | Polycrystalline silicon zone melting equipment employing electron beam and method for removing impurities |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104878448A true CN104878448A (en) | 2015-09-02 |
Family
ID=53946116
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510252743.2A Pending CN104878448A (en) | 2015-05-15 | 2015-05-15 | Polycrystalline silicon zone melting equipment employing electron beam and method for removing impurities |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104878448A (en) |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11335196A (en) * | 1998-05-22 | 1999-12-07 | Hitachi Ltd | Growth of group iii nitride single crystal, and horizontal type boat crystal-growth apparatus |
| CN101318655A (en) * | 2008-06-19 | 2008-12-10 | 大连理工大学 | Method and device for removing foreign matter of phosphor in polysilicon |
| CN101445957A (en) * | 2008-12-16 | 2009-06-03 | 桂林实创真空数控设备有限公司 | Vacuum electron beam melting furnace for polysilicon purification |
| CN101787563A (en) * | 2010-03-19 | 2010-07-28 | 大连隆田科技有限公司 | Method and device for removing impurities of phosphorus and boron by induction and electronic beam melting |
| CN102112394A (en) * | 2008-08-12 | 2011-06-29 | 株式会社爱发科 | Silicon purification method |
| CN102392294A (en) * | 2011-11-15 | 2012-03-28 | 中国科学院上海技术物理研究所 | Horizontal vacuum zone-melting preparation method of high-purity semiconductor material |
| KR20120058330A (en) * | 2010-11-29 | 2012-06-07 | 한국에너지기술연구원 | Apparatus for manufacturing polysilicon based electron-beam melting using dummy bar and method of manufacturing polysilicon using the same |
| CN102602933A (en) * | 2011-01-20 | 2012-07-25 | 江西开昂新能源科技有限公司 | Polycrystalline silicon purifying device and method |
| CN103420380A (en) * | 2013-08-28 | 2013-12-04 | 青岛隆盛晶硅科技有限公司 | Method and device for manufacturing polycrystalline silicon by coupling electron beam smelting technology and directional solidification technology |
| CN103420375A (en) * | 2012-05-21 | 2013-12-04 | 韩国能量技术研究院 | Polysilicon manufacturing device based on electron beam melting by utilizing dummy bar and method thereof |
| CN103420379A (en) * | 2013-08-28 | 2013-12-04 | 青岛隆盛晶硅科技有限公司 | Method and device for manufacturing solar grade polycrystalline silicon by continuously smelting electron beams |
| CN103882509A (en) * | 2012-12-19 | 2014-06-25 | 北京有色金属研究总院 | Electron beam zone melting furnace and method for carrying out float zone purification on material |
| CN104388697A (en) * | 2014-10-31 | 2015-03-04 | 峨嵋半导体材料研究所 | Method for preparing 6N high-purity aluminum |
-
2015
- 2015-05-15 CN CN201510252743.2A patent/CN104878448A/en active Pending
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11335196A (en) * | 1998-05-22 | 1999-12-07 | Hitachi Ltd | Growth of group iii nitride single crystal, and horizontal type boat crystal-growth apparatus |
| CN101318655A (en) * | 2008-06-19 | 2008-12-10 | 大连理工大学 | Method and device for removing foreign matter of phosphor in polysilicon |
| CN102112394A (en) * | 2008-08-12 | 2011-06-29 | 株式会社爱发科 | Silicon purification method |
| CN101445957A (en) * | 2008-12-16 | 2009-06-03 | 桂林实创真空数控设备有限公司 | Vacuum electron beam melting furnace for polysilicon purification |
| CN101787563A (en) * | 2010-03-19 | 2010-07-28 | 大连隆田科技有限公司 | Method and device for removing impurities of phosphorus and boron by induction and electronic beam melting |
| KR20120058330A (en) * | 2010-11-29 | 2012-06-07 | 한국에너지기술연구원 | Apparatus for manufacturing polysilicon based electron-beam melting using dummy bar and method of manufacturing polysilicon using the same |
| CN102602933A (en) * | 2011-01-20 | 2012-07-25 | 江西开昂新能源科技有限公司 | Polycrystalline silicon purifying device and method |
| CN102392294A (en) * | 2011-11-15 | 2012-03-28 | 中国科学院上海技术物理研究所 | Horizontal vacuum zone-melting preparation method of high-purity semiconductor material |
| CN103420375A (en) * | 2012-05-21 | 2013-12-04 | 韩国能量技术研究院 | Polysilicon manufacturing device based on electron beam melting by utilizing dummy bar and method thereof |
| CN103882509A (en) * | 2012-12-19 | 2014-06-25 | 北京有色金属研究总院 | Electron beam zone melting furnace and method for carrying out float zone purification on material |
| CN103420380A (en) * | 2013-08-28 | 2013-12-04 | 青岛隆盛晶硅科技有限公司 | Method and device for manufacturing polycrystalline silicon by coupling electron beam smelting technology and directional solidification technology |
| CN103420379A (en) * | 2013-08-28 | 2013-12-04 | 青岛隆盛晶硅科技有限公司 | Method and device for manufacturing solar grade polycrystalline silicon by continuously smelting electron beams |
| CN104388697A (en) * | 2014-10-31 | 2015-03-04 | 峨嵋半导体材料研究所 | Method for preparing 6N high-purity aluminum |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103420380B (en) | Method and device for manufacturing polycrystalline silicon by coupling electron beam smelting technology and directional solidification technology | |
| CN102145894B (en) | Method and device for smelting and purifying polysilicon by using electron beams and adopting slag filtering | |
| CN105129804B (en) | The production technology of polysilicon | |
| CN1873062A (en) | Method for preparing polysilicon in high purity in use for solar cell | |
| CN102120579B (en) | Method and device for efficiently and continuously smelting and purifying polysilicon with electron beams | |
| US20120216572A1 (en) | Method and apparatus for removing phosphorus and boron from polysilicon by continuously smelting | |
| CN101787563A (en) | Method and device for removing impurities of phosphorus and boron by induction and electronic beam melting | |
| CN101698481B (en) | Solar-grade polysilicon purifying device and solar-grade polysilicon purifying method | |
| CN101798705A (en) | Method and device for continuous crystal-pulling purification of polysilicon from low-temperature melt | |
| CN102120578B (en) | Method and device for coupling and purifying polysilicon and removing phosphorus and metal with electron beams | |
| CN103387236A (en) | Refining device and method of high purity silicon | |
| CN102602933A (en) | Polycrystalline silicon purifying device and method | |
| CN101850975A (en) | Method for purifying silicon by removing phosphorus and metal impurities | |
| CN101824650A (en) | Purifying system of high purity polysilicon and purifying method | |
| CN201981012U (en) | Equipment for effectively purifying polycrystalline silicon powder body by electron beam | |
| CN203440097U (en) | Device for preparing polycrystalline silicon through coupling of electron-beam smelting technology and directional solidification technology | |
| CN103420379B (en) | Method and the device thereof of solar-grade polysilicon are prepared in electron beam serialization melting | |
| CN202063730U (en) | Electron beam and slag filter smelting polycrystalline silicon purifying equipment | |
| CN103539125B (en) | Medium melting is connected the method for purifying polycrystalline silicon with preliminary directional freeze | |
| CN102408112A (en) | Method and equipment for purification of polysilicon by using electron beam melting under action of high purity silicon substrate | |
| CN104878448A (en) | Polycrystalline silicon zone melting equipment employing electron beam and method for removing impurities | |
| CN101905886B (en) | Method for purifying polycrystalline silicon by electron beam gradient smelting | |
| CN103738965B (en) | Method for removal of oxygen from liquid silicon by electron beam melting and device thereof | |
| CN203558861U (en) | Water-cooled copper crucible applied to smelting polysilicon with electron beam | |
| CN203440095U (en) | Device for preparing solar-grade polycrystalline silicon through electron-beam continuous smelting |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150902 |
|
| RJ01 | Rejection of invention patent application after publication |