CN203559158U - Electronic beam smelting polycrystalline silicon deoxidizing and cast ingot coupling equipment - Google Patents
Electronic beam smelting polycrystalline silicon deoxidizing and cast ingot coupling equipment Download PDFInfo
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- CN203559158U CN203559158U CN201320745551.1U CN201320745551U CN203559158U CN 203559158 U CN203559158 U CN 203559158U CN 201320745551 U CN201320745551 U CN 201320745551U CN 203559158 U CN203559158 U CN 203559158U
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Abstract
The utility model belongs to the field of metallurgical smelting, and particularly relates to electronic beam smelting polycrystalline silicon deoxidizing and cast ingot coupling equipment. The equipment comprises an electronic beam smelting component and a cast ingot coupling component, wherein the electronic beam smelting component comprises a water-cooling conveyer belt at the upper part inside a furnace body; a charging device is arranged on the wall of the furnace body at one side of the water-cooling conveyer belt; a discharge hole of the charging device is arranged above the water-cooling conveyer belt; the other side of the water-cooling conveyer belt inclines downwards and is provided with a guide hole; an electronic gun for smelting and an electronic gun for radiation are fixedly arranged on the furnace body at the top of the water-cooling conveyer belt; the cast ingot coupling component comprises a cast ingot device; the cast ingot device is arranged below the water-cooling conveyer belt; the guide hole of the water-cooling conveyer belt is arranged just above the center of a quartz crucible of the cast ingot device. According to the utility model, the electronic beam smelting deoxidizing equipment is proposed for the first time, the electronic beam deoxidizing effect is achieved, and meanwhile, cast ingot coupling is combined, so that the energy consumption required for heating materials by a cast ingot is reduced, and the production efficiency is greatly improved.
Description
Technical field
The invention belongs to metallurgical smelting field, particularly the method for the removal of impurities of a kind of electron beam melting polysilicon and ingot casting coupling, also relates to its equipment in addition.
Background technology
At present, China has become world energy sources production and consumption big country, but 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 < < renewable energy source Long-and Medium-term Development planning > >, to the year two thousand twenty, China strives making solar electrical energy generation installed capacity to reach 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 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%.
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 dependence at present: Siemens Method, silane thermal decomposition process, gas fluidized bed method and metallurgy method.Metallurgy method is prepared solar-grade polysilicon technology the only way which must be passed as development low cost, eco-friendly solar-grade polysilicon technology of preparing, has obtained at present tremendous development, and has realized suitability for industrialized production.Metallurgy method purifying polycrystalline silicon refers to the physical metallurgy means that adopt, in the situation that silicon does not participate in chemical reaction occurs, remove successively the method for the various impurity elements (phosphorus, boron and metal) in silicon, it is not single preparation method, but a kind of Integration Method mainly utilizes saturated vapor pressure principle, segregation principle and oxidisability difference principle, adopts respectively different processing methodes, the impurity element of making a return journey in silica removal, thus be met the silicon material of solar energy polycrystalline silicon purity requirement.
In metallurgy method technique, the phosphorus of silicon material, boron, metal impurities all can be removed by effective process means, have reached comparatively ideal effect.But, in recent years, in to the research of polysilicon solar battery slice electricity conversion, find, the content of oxygen element produces material impact to the electricity conversion of cell piece, general oxygen is when interstitial site, conventionally aobvious electroactive, however in casting polycrystalline silicon oxygen concn conventionally 3 × 10
17～1.4 × 10
18cm
-3between, the interstitial oxygen concentration of high density, in device fabrication process subsequently, experiences the thermal treatment of all temps, and meeting segregation and precipitation in silicon crystal form oxygen and close the defects such as alms giver, oxygen precipitation.Simultaneously, in silicon crystal material growth, cooling process because the solubility with temperature of oxygen reduces and declines rapidly, oversaturated oxygen will form primary oxygen precipitation in casting polycrystalline silicon, also may form various complex bodys with other impurity, as N-O, C-O complex body.These oxygen precipitations and complex body thereof not only can reduce the effect of the outer gettering of phosphorus, even directly become the short-channel of battery.
These oxygen defects have the impact of favourable and unfavorable two aspects on silicon materials and device, it can form intrinsic gettering in conjunction with device technology, absorb metallic impurity, all right pinning dislocation, the physical strength of raising silicon chip, but when oxygen precipitation is excessive, can induce again other lattice defect, introduce a large amount of secondary defects, also can attract the metallic elements such as iron, form iron oxygen precipitation complex body, there is very strong few sub-compound ability, can significantly reduce the conversion efficiency of solar cell of material.
In the techniques such as the directional freeze of metallurgy method, ingot casting, the oxygen element in crucible or the oxygen element passing in gas inevitably can enter into silicon material, are the major causes that oxygen impurities produces.In traditional test silicon, the common method of oxygen level is infrared spectra, respectively HIGH-PURITY SILICON material and batch mixing (scrap stock after casting casting mix with high-purity material) are detected with infrared spectra, in two kinds of material, the content of oxygen is more or less the same, and this has also caused the oxygen impurities of introducing in metallurgy method technique not come into one's own.
In fact, in silicon, oxygen element has two states: substitute position, oxo has been replaced the position of silicon; Gap digit, oxygen is in the gap of Siliciumatom.The oxygen level that in traditional test silicon, the infrared spectra of oxygen level can only detector gap position, can not truly reflect two kinds of oxygen levels in silicon material.Through applicant's experiment test, the oxygen that substitutes position can discharge electronics, similar to the effect that foreign matter of phosphor in silicon produces, and can affect polycrystalline silicon battery plate electricity conversion.Applicant is by sims repeated detection, and in above-mentioned two kinds of silicon material, oxygen element content differs greatly, and is mainly the difference that substitutes the oxygen element content of position.Therefore, for the impurity oxygen of introducing in the techniques such as ingot casting, can not ignore, must seek the content of impurity oxygen in effective means reduction silicon.
But, in prior art, not good to the removal effect of oxygen element.For the removal method of oxygen impurities, retrieve the method that mono-kind of patent of invention CN200810070925 reduces oxygen in Pure Silicon Metal, carbon content, this invention adopts and in silicon liquid, is blown into oxygen, hydrogen and water vapour, hydrogen and oxygen are reacted in silicon liquid and produce localized hyperthermia, oxygen, carbon in silicon liquid are removed with gaseous emission, but the method need to pass into oxygen and hydrogen under silicon molten state, operation easier is large, dangerous high, the removal effect of oxygen is not good.
, effectively reduce in polycrystalline silicon ingot casting raw material after oxygen level meanwhile, can obtain polycrystalline silicon ingot casting by directional long crystal technique, but before casting ingot method be all direct heating ingot casting raw material, can not realize ingot casting coupling, large with duration, energy consumption.
Summary of the invention
In order to overcome above the deficiencies in the prior art, the present invention proposes the equipment of the deoxygenation of a kind of electron beam melting polysilicon and ingot casting coupling, this equipment can be removed the impurity oxygen in polycrystalline silicon raw material by electron beam melting, obtain the polysilicon liquid of high-purity low-oxygen, direct this polysilicon liquid guiding is entered to ingot casting coupling device and complete directional long crystal casting ingot process, obtain the polycrystalline silicon ingot casting of high-purity low-oxygen, effectively reduce the oxygen level in silicon material, improved the efficiency of conversion of battery, reduced the operation of ingot casting heating raw materials, realize ingot casting coupling effect, reduce the process time, reduce the total energy consumption in production process, save cost.
The equipment of electron beam melting polysilicon of the present invention deoxygenation and ingot casting coupling, comprises body of heater, it is characterized in that: in body of heater, be provided with electron beam melting assembly and ingot casting coupling assembly, wherein:
Electron beam melting assembly comprises the water-cooled transport tape that is installed on body of heater internal upper part, on the furnace body wall of this water-cooled transport tape one side, be provided with feeding device, the discharge port of this feeding device is positioned at water-cooled transport tape top, this water-cooled transport tape opposite side is downward-sloping and be provided with flow-guiding mouth, is installed with melting electron beam gun and radiation electron beam gun on this water-cooled transport tape top body of heater;
Ingot casting coupling assembly comprises ingot casting device, and ingot casting device is positioned at water-cooled transport tape below, and the flow-guiding mouth of water-cooled transport tape be positioned at ingot casting device quartz crucible center directly over.
Described water-cooled transport tape is downward-sloping, and the angle of inclination between itself and horizontal plane is 5 °～15 °.
Described ingot casting device comprises the magnetism servo-electric motor water-cooling that is fixedly installed in body of heater inner bottom part, and this magnetism servo-electric motor water-cooling is provided with quartz crucible, is provided with from inside to outside well heater and insulation sleeve on quartz crucible outer wall.
Described magnetism servo-electric motor water-cooling adopts water-cooled ingot pulling mechanism, the graphite heater that described well heater is integrated.
Described magnetism servo-electric motor water-cooling is fixing magnetism servo-electric motor water-cooling, and the graphite heater that described well heater is split comprises three of upper, middle and lower graphite heating sheet.
In the present invention, the equipment of electron beam melting deoxygenation has been proposed first, utilize electron beam melting high temperature evaporation to go deimpurity characteristic, by melting, use electron beam gun to melt on water-cooled transport tape and the preliminary deoxygenation of melting, further efficient deoxygenation under the effect of electron beam gun of radiation use on large surface area on water-cooled transport tape, and maintain liquid state and enter in ingot casting device, for casting ingot process provides the liquid high-purity polycrystalline silicon raw material of hypoxemia, and carry out directional long crystal casting ingot process, realized the effect of ingot casting coupling, the present invention has realized the effect of electron beam deoxygenation, in conjunction with ingot casting, be coupled simultaneously, reduced the time of electron beam melting after coagulation and ingot casting heating raw, reduced the required energy consumption of ingot casting heating raw, greatly improved production efficiency.
The invention has the advantages that:
(1) proposed the equipment of electron beam deoxygenation, solved the difficult problem that in polysilicon, impurity oxygen is removed, oxygen level can be reduced to 0.0571ppmw, meets the requirement of solar cell to polycrystalline silicon ingot casting oxygen level.
(2) this equipment has been realized when the preliminary deoxygenation of melting and polysilicon are liquid to flow by the further deoxygenation of radiating electron bundle, shortens the deoxygenation time more than 20%.
(3) electron beam melting deoxygenation technology and ingot casting technology coupling, realize serialization and produce, and can enhance productivity more than 40%, and energy efficient is more than 25%.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
In figure: 1, body of heater 2, water-cooled transport tape 3, electron beam gun 4 for melting, electron beam gun 5, feeding device 6, quartz crucible 7, magnetism servo-electric motor water-cooling 8, well heater 9, insulation sleeve 10, flow-guiding mouth for radiation
Embodiment
Below in conjunction with specific embodiments and the drawings, describe the present invention in detail, but the present invention is not limited to specific embodiment.
Embodiment 1:
As shown in Figure 1, the equipment of the deoxygenation of electron beam melting polysilicon and ingot casting coupling, comprises body of heater, is provided with electron beam melting assembly and ingot casting coupling assembly in body of heater 1, wherein:
Electron beam melting assembly comprises the water-cooled transport tape 2 that is installed on body of heater internal upper part, on the furnace body wall of this water-cooled transport tape one side, be provided with feeding device 5, the discharge port of this feeding device is positioned at water-cooled transport tape top, this water-cooled transport tape opposite side is downward-sloping and be provided with flow-guiding mouth, on water-cooled transport tape, have Baltimore groove, for the polysilicon liquid guiding of the preliminary deoxygenation of melting is flowed to the direction of ingot casting device, and enter in ingot casting device by the flow-guiding mouth on water-cooled transport tape, on this water-cooled transport tape top body of heater, be installed with melting electron beam gun 3 and electron beam gun 4 for radiation,
Water-cooled transport tape is made by copper product, wherein pass into recirculated cooling water, to avoid fusing and to damage, water-cooled transport tape is downward-sloping, angle of inclination between itself and horizontal plane is 5 °, so that silicon liquid flows downward smoothly along Baltimore groove on water-cooled transport tape, and enters in the quartz crucible 6 in ingot casting device by flow-guiding mouth 10.
Ingot casting coupling assembly comprises ingot casting device, ingot casting device is positioned at water-cooled transport tape below, and the flow-guiding mouth of water-cooled transport tape be positioned at ingot casting device quartz crucible center directly over, with guarantee from flow-guiding mouth flow out silicon liquid add smoothly the quartz crucible of ingot casting device.
Ingot casting device comprises the magnetism servo-electric motor water-cooling 7 that is fixedly installed in body of heater inner bottom part, and this magnetism servo-electric motor water-cooling is provided with quartz crucible, is provided with from inside to outside well heater 8 and insulation sleeve 9 on quartz crucible outer wall.
Magnetism servo-electric motor water-cooling can adopt water-cooled ingot pulling mechanism, now adopts the graphite heater of one, by heating, is kept liquid and is drawn ingot to realize directional long crystal technique; Also can adopt fixing magnetism servo-electric motor water-cooling, now adopt the graphite heater of split, this graphite heater is divided into three of upper, middle and lower graphite heating sheet, be arranged at respectively the upper, middle and lower portion of quartz crucible, by the heating power of graphite heating sheet that regulates upper, middle and lower, carry out directional long crystal technique, this ingot casting device can be realized all processes of directional long crystal casting ingot process.
Embodiment 2:
Device described in employing embodiment 1, carries out the deoxygenation of electron beam melting polysilicon and ingot casting coupling technique, and concrete steps are as follows:
(1) charging vacuumizes: by granular size, be to put into feeding device after the polycrystalline silicon material cleaning, drying that 10-12mm, purity are 99.996%, oxygen level is 20ppmw, the polycrystalline silicon ingot casting bed material of 6N is laid in quartz crucible bottom at ingot casting device, and the vacuum tightness of body of heater is evacuated to 3 × 10
-2pa, the vacuum tightness of electron beam gun is evacuated to 4 × 10
-3pa, pre-thermionic electron guns 15min;
(2) preliminary deoxygenation: add continuously the polycrystalline silicon material in step (1) by feeding device on electron beam melting furnace water-cooled transport tape, start melting electron beam gun, setting the melting electron beam line of electron beam gun is 1200mA fusing the preliminary impurity oxygen of removing wherein of melting 15min polycrystalline silicon material;
(3) further deoxygenation: the polysilicon liquid after preliminary deoxygenation flows downward and keep liquid further deoxygenation under the effect of radiation electron beam gun along water-cooled transport tape, obtain the polysilicon liquid after deoxygenation, the electron beam line of setting radiation electron beam gun in this process is 800mA;
(4) polycrystalline silicon casting ingot process: the 6N(massfraction that lay the quartz crucible bottom of heat fused ingot casting device is 99.9999%) polycrystalline silicon ingot casting bed material, polysilicon liquid after deoxygenation is guided by flow-guiding mouth in the quartz crucible that enters ingot casting device, the heater power of controlling ingot casting device maintains this polysilicon liquid for liquid, in the quartz crucible of ingot casting device, add this polysilicon liquid continuously, to reach quartz crucible volume 80% after, carry out directional long crystal casting ingot process, in this process, control directional long crystal speed and be 1.2cm-1.3cm/h (centimetre per hour), obtain the polycrystalline silicon ingot casting of electron beam deoxygenation, this polycrystalline silicon ingot casting detects through second ion mass spectroscopy (SIMS), its oxygen level is lower than second ion mass spectroscopy limit of detection, lower than 0.0571ppmw.
Claims (5)
1. an equipment for the deoxygenation of electron beam melting polysilicon and ingot casting coupling, comprises body of heater, it is characterized in that: in body of heater, be provided with electron beam melting assembly and ingot casting coupling assembly, wherein:
Electron beam melting assembly comprises the water-cooled transport tape that is installed on body of heater internal upper part, on the furnace body wall of this water-cooled transport tape one side, be provided with feeding device, the discharge port of this feeding device is positioned at water-cooled transport tape top, this water-cooled transport tape opposite side is downward-sloping and be provided with flow-guiding mouth, is installed with melting electron beam gun and radiation electron beam gun on this water-cooled transport tape top body of heater;
Ingot casting coupling assembly comprises ingot casting device, and ingot casting device is positioned at water-cooled transport tape below, and the flow-guiding mouth of water-cooled transport tape be positioned at ingot casting device quartz crucible center directly over.
2. the equipment of a kind of electron beam melting polysilicon according to claim 1 deoxygenation and ingot casting coupling, is characterized in that: described water-cooled transport tape is downward-sloping, and the angle of inclination between itself and horizontal plane is 5 °～15 °.
3. the equipment of a kind of electron beam melting polysilicon according to claim 1 deoxygenation and ingot casting coupling, it is characterized in that: described ingot casting device comprises the magnetism servo-electric motor water-cooling that is fixedly installed in body of heater inner bottom part, this magnetism servo-electric motor water-cooling is provided with quartz crucible, is provided with from inside to outside well heater and insulation sleeve on quartz crucible outer wall.
4. the equipment of a kind of electron beam melting polysilicon according to claim 3 deoxygenation and ingot casting coupling, is characterized in that: described magnetism servo-electric motor water-cooling adopts water-cooled ingot pulling mechanism, the graphite heater that described well heater is integrated.
5. the equipment of a kind of electron beam melting polysilicon according to claim 3 deoxygenation and ingot casting coupling, it is characterized in that: described magnetism servo-electric motor water-cooling is fixing magnetism servo-electric motor water-cooling, described well heater is the graphite heater of split, comprises three of upper, middle and lower graphite heating sheet.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320745551.1U CN203559158U (en) | 2013-11-22 | 2013-11-22 | Electronic beam smelting polycrystalline silicon deoxidizing and cast ingot coupling equipment |
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|---|---|---|---|
| CN201320745551.1U CN203559158U (en) | 2013-11-22 | 2013-11-22 | Electronic beam smelting polycrystalline silicon deoxidizing and cast ingot coupling equipment |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104372407A (en) * | 2014-11-19 | 2015-02-25 | 李剑 | Equipment and method for directional solidification growth of crystalline silicon |
| CN104532340A (en) * | 2014-12-24 | 2015-04-22 | 大连理工大学 | Device and method for electron beam melting and single-crystal lifting coupling |
| CN104651929A (en) * | 2013-11-22 | 2015-05-27 | 青岛隆盛晶硅科技有限公司 | Electron beam melting polysilicon deoxygenation and ingot casting coupling method and apparatus thereof |
-
2013
- 2013-11-22 CN CN201320745551.1U patent/CN203559158U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104651929A (en) * | 2013-11-22 | 2015-05-27 | 青岛隆盛晶硅科技有限公司 | Electron beam melting polysilicon deoxygenation and ingot casting coupling method and apparatus thereof |
| CN104651929B (en) * | 2013-11-22 | 2018-08-21 | 青岛昌盛日电太阳能科技股份有限公司 | A kind of method and apparatus that the deoxygenation of electron-beam smelting polysilicon is coupled with ingot casting |
| CN104372407A (en) * | 2014-11-19 | 2015-02-25 | 李剑 | Equipment and method for directional solidification growth of crystalline silicon |
| CN104532340A (en) * | 2014-12-24 | 2015-04-22 | 大连理工大学 | Device and method for electron beam melting and single-crystal lifting coupling |
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