CN104651929A - Electron beam melting polysilicon deoxygenation and ingot casting coupling method and apparatus thereof - Google Patents

Electron beam melting polysilicon deoxygenation and ingot casting coupling method and apparatus thereof Download PDF

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Publication number
CN104651929A
CN104651929A CN201310596052.5A CN201310596052A CN104651929A CN 104651929 A CN104651929 A CN 104651929A CN 201310596052 A CN201310596052 A CN 201310596052A CN 104651929 A CN104651929 A CN 104651929A
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electron
ingot casting
melting
deoxygenation
polysilicon
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CN104651929B (en
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姜大川
王登科
安广野
郭校亮
谭毅
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QINGDAO NEW ENERGY SOLUTIONS INC. (NESI)
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Qingdao Longsheng Crystal Silicon Technology Co Ltd
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Abstract

The invention belongs to the field of metallurgic melting, and especially relates to an electron beam melting polysilicon deoxygenation and ingot casting coupling method and an apparatus thereof. The method comprises the following steps: carrying out vacuum pumping on a furnace body and electron guns, starting a melting electron gun to carry out electron beam melting on a polysilicon material, and melting to preliminarily remove impurity oxygen; maintaining a liquid state under the action of a radiation electron gun to further remove oxygen, guiding the obtained material to enter an ingot casting device through a water cooled conveyor belt, and carrying out oriented crystal growth to obtain polysilicon cast ingots. The apparatus comprises an electron beam melting assembly and an ingot casting coupling assemble, the ingot casting coupling assembly comprises the ingot casting device, the ingot casting device is positioned under the water cooled conveyor belt, and the flow guiding opening of the water cooled conveyor belt is positioned over the center of the quartz crucible of the ingot casting device. The electron beam melting deoxygenation method and a use thereof are provided for the first time, electron beam deoxygenation is realized, and ingot casting coupling is combined, so energy required by ingot casting heating of the raw material is reduced, and the production efficiency is greatly improved.

Description

The method and apparatus that the deoxygenation of a kind of electron beam melting polysilicon is coupled with ingot casting
Technical field
The invention belongs to metallurgical smelting field, particularly the method that is coupled with ingot casting of a kind of electron beam melting polysilicon removal of impurities, also relates to its equipment in addition.
Background technology
At present, China has become world energy sources production and consumption big country, but per capita energy's level of consumption is also very low.Along with development that is economic and society, 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 make great efforts to improve 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 the important development direction of renewable energy source is swift and violent, and its proportion is increasing.According to " planning of renewable energy source Long-and Medium-term Development ", to the year two thousand twenty, China strives making solar electrical energy generation installed capacity reach 1.8GW(gigawatt), will 600GW be reached 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 up to more than 25%.
The development of solar photovoltaic industry depends on the purification to polycrystalline silicon raw material.The purifying technique of polycrystalline silicon raw material mainly relies on following several technique at present: Siemens Method, silane thermal decomposition process, gas fluidized bed process and metallurgy method.Metallurgy method prepares solar-grade polysilicon technology the only way which must be passed as development low cost, eco-friendly solar-grade polysilicon technology of preparing, achieves tremendous development at present, and achieves suitability for industrialized production.Metallurgy method purifying polycrystalline silicon refers to and adopts physical metallurgy means, when silicon does not participate in chemical reaction occurs, remove the method for the various impurity elements (phosphorus, boron and metal) in silicon successively, it is not single preparation method, but a kind of Integration Method, mainly utilize saturated vapor pressure principle, segregation principle and oxidisability difference principle, adopt different processing methodes respectively, the impurity element of making a return journey in silica removal, thus the silicon material being met solar energy polycrystalline silicon purity requirement.
In metallurgy method technique, the phosphorus of silicon material, boron, metal impurities are all removed by effective process means, reach comparatively ideal effect.But, in recent years, find in the research to polysilicon solar battery slice electricity conversion, the content of oxygen element produces material impact to the electricity conversion of cell piece, when general oxygen is in interstitial site, usually aobvious electroactive, however in casting polycrystalline silicon oxygen concn usually 3 × 10 17~ 1.4 × 10 18cm -3between, the interstitial oxygen concentration of high density is in device fabrication process subsequently, and the thermal treatment of experience all temps, meeting segregation and precipitation in silicon crystal, form oxygen and close the defect such as alms giver, oxygen precipitation.Simultaneously, decline rapidly because the solubility with temperature of oxygen reduces in the process of silicon crystal material growth, cooling, oversaturated oxygen will form grown-in oxygen precipitates in casting polycrystalline silicon, also may form various complex body 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 to silicon materials and device, it can form intrinsic gettering in conjunction with device technology, gettering metal impurity, all right pinning dislocation, improves the physical strength of silicon chip, but other lattice defect can be induced again when oxygen precipitation is excessive, 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, significantly can reduce the conversion efficiency of solar cell of material.
In the technique such as directional freeze, ingot casting of metallurgy method, the oxygen element in crucible or the oxygen element passed in gas inevitably 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 is detected with batch mixing (scrap stock after casting mix with high-purity material) with infrared spectra, in two kinds of material, the content of oxygen is more or less the same, and this result also in the oxygen impurities introduced in metallurgy method technique and does not come into one's own.
In fact, in silicon, oxygen element has two states: substitute position, namely oxygen instead of the position of silicon; Gap digit, namely oxygen is in the gap of Siliciumatom.In traditional test silicon, the infrared spectra of oxygen level can only the oxygen level of detector gap position, truly can not reflect the oxygen levels in two kinds of silicon material.Through the experiment test of applicant, the oxygen substituting 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 mainly substitutes the difference of the oxygen element content of position.Therefore, can not ignore for the impurity oxygen introduced in the techniques such as ingot casting, the content that effective means reduce impurity oxygen in silicon must be sought.
But, in prior art, not good to the removal effect of oxygen element.For the minimizing technology of oxygen impurities, retrieve the method that patent of invention CN200810070925 mono-kind reduces metal Oxygen in silicon, carbon content, this invention adopts and be blown into oxygen, hydrogen and water vapour in silicon liquid, hydrogen and oxygen are reacted in silicon liquid and produces localized hyperthermia, make the oxygen in silicon liquid, carbon removes with gaseous emission, but the method needs to pass into oxygen and hydrogen under silicon molten state, operation easier is large, dangerous high, the removal effect of oxygen is not good.
Meanwhile, effectively reduce in polycrystalline silicon ingot casting raw material after oxygen level, namely obtain polycrystalline silicon ingot casting by directional long crystal technique, but casting ingot method is before all direct heating ingot casting raw material, ingot casting coupling can not be realized, large by duration, energy consumption.
Summary of the invention
In order to overcome above the deficiencies in the prior art, the present invention proposes the method that the deoxygenation of a kind of electron beam melting polysilicon is coupled with ingot casting, the impurity oxygen in polycrystalline silicon raw material is removed by electron beam melting, obtain the polysilicon liquid of high-purity low-oxygen, this polysilicon liquid is directly guided and enters ingot casting coupling device and complete directional long crystal casting ingot process, obtain the polycrystalline silicon ingot casting of high-purity low-oxygen, the method effectively reduces the oxygen level in silicon material, improve the efficiency of conversion of battery, decrease 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 method that a kind of electron beam melting polysilicon of the present invention deoxygenation is coupled with ingot casting, first vacuumizes body of heater and electron beam gun, pre-thermionic electron guns; Then on electron beam melting furnace water-cooled transport tape, add polycrystalline silicon material by feeding device continuously, start melting electron beam gun and carry out electron beam melting to polycrystalline silicon material, melting tentatively removes impurity oxygen; Polysilicon liquid after preliminary deoxygenation flows downward along water-cooled transport tape and under the effect of radiation electron beam gun, keeps liquid deoxygenation further, obtains the polysilicon liquid after deoxygenation; Finally being guided by flow-guiding mouth by the polysilicon liquid after deoxygenation enters in ingot casting device, carries out directional long crystal casting ingot process, obtains polycrystalline silicon ingot casting.
Preferably carry out according to following steps:
(1) charging vacuumizes: be put into feeding device after the polycrystalline silicon material cleaning, drying of 10-30mm by granular size, the polycrystalline silicon ingot casting bed material of 6N is laid bottom the quartz crucible of ingot casting device, and body of heater and electron beam gun are vacuumized, pre-thermionic electron guns 10-15min;
(2) preliminary deoxygenation: added the polycrystalline silicon material in step (1) by feeding device on electron beam melting furnace water-cooled transport tape continuously, start melting electron beam gun, the electron beam line of setting melting electron beam gun is 200-1200mA fusing and impurity oxygen wherein tentatively removed by melting polysilicon material;
(3) deoxygenation further: the polysilicon liquid after preliminary deoxygenation flows downward along water-cooled transport tape and keep liquid deoxygenation further under the effect of radiation electron beam gun, obtain the polysilicon liquid after deoxygenation, the electron beam line setting radiation electron beam gun in this process is 200-800mA;
(4) polycrystalline silicon casting ingot process: the 6N polycrystalline silicon ingot casting bed material laid bottom the quartz crucible of heat fused ingot casting device is liquid, being guided by flow-guiding mouth by polysilicon liquid after deoxygenation enters in the quartz crucible of ingot casting device, the heater power maintenance polysilicon controlling ingot casting device is liquid, this polysilicon liquid is added continuously in the quartz crucible of ingot casting device, to the 80%-85% reaching quartz crucible volume, carry out directional long crystal casting ingot process, obtain the polycrystalline silicon ingot casting of electron beam deoxygenation.
The low vacuum of described body of heater is in 5 × 10 -2pa, the low vacuum of described electron beam gun is in 5 × 10 -3pa.
Described polycrystalline silicon material purity is 99.996%-99.998%, and oxygen level is 4-20ppmw.
In described step (2), the smelting time of the impurity oxygen that melting polysilicon material is removed wherein is 5-20min.
The equipment that electron beam melting polysilicon of the present invention deoxygenation is coupled with ingot casting, comprises body of heater, it is characterized in that: be provided with electron beam melting assembly and ingot casting coupling assembly in body of heater, wherein:
Electron beam melting assembly comprises the water-cooled transport tape being installed on body of heater internal upper part, the furnace body wall of this water-cooled transport tape side is provided with feeding device, the discharge port of this feeding device is positioned at above water-cooled transport tape, this water-cooled transport tape opposite side is downward-sloping and be provided with flow-guiding mouth, and this water-cooled transport tape top body of heater is installed with melting electron beam gun and radiation electron beam gun;
Ingot casting coupling assembly comprises ingot casting device, and ingot casting device is positioned at below water-cooled transport tape, and the flow-guiding mouth of water-cooled transport tape is positioned at directly over the quartz crucible center of ingot casting device.
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 being fixedly installed in body of heater inner bottom part, and this magnetism servo-electric motor water-cooling is provided with quartz crucible, quartz crucible outer wall is provided with from inside to outside well heater and insulation sleeve.
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 described well heater is the graphite heater of split, comprises three, upper, middle and lower graphite heating sheet.
In the present invention, propose processing method and the purposes of electron beam melting deoxygenation first, electron beam melting high temperature evaporation is utilized to go deimpurity characteristic, melted on water-cooled transport tape and the preliminary deoxygenation of melting by melting electron beam gun, efficient deoxygenation further under the effect of radiation electron beam gun 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, achieve the effect of ingot casting coupling, present invention achieves the effect of electron beam deoxygenation, be coupled in conjunction with ingot casting simultaneously, decrease the time of electron beam melting after coagulation and ingot casting heating raw, reduce the energy consumption needed for ingot casting heating raw, substantially increase production efficiency.
The invention has the advantages that:
(1) propose processing method and the purposes of electron beam deoxygenation, solve 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) achieve the preliminary deoxygenation of melting and polysilicon liquid state flowing time by the further deoxygenation of radiating electron bundle, shorten the deoxygenation time more than 20%.
(3) electron beam melting deoxygenation technology is coupled with ingot casting technology, realizes continuous prodution, can enhance productivity more than 40%, energy efficient 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, melting electron beam gun 4, radiation 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
Embodiment
Describe the present invention in detail below in conjunction with specific embodiments and the drawings, but the present invention is not limited to specific embodiment.
Embodiment 1:
As shown in Figure 1, the equipment that the deoxygenation of electron beam melting polysilicon is coupled with ingot casting, 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 being installed on body of heater internal upper part, the furnace body wall of this water-cooled transport tape side is provided with feeding device 5, the discharge port of this feeding device is positioned at above water-cooled transport tape, this water-cooled transport tape opposite side is downward-sloping and be provided with flow-guiding mouth, water-cooled transport tape has Baltimore groove, flow to the direction of ingot casting device for the polysilicon liquid of preliminary for melting deoxygenation is guided, and enter in ingot casting device by the flow-guiding mouth on water-cooled transport tape, this water-cooled transport tape top body of heater is installed with melting electron beam gun 3 and radiation electron beam gun 4,
Water-cooled transport tape is made up of 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 entered by flow-guiding mouth 10 in the quartz crucible 6 in ingot casting device.
Ingot casting coupling assembly comprises ingot casting device, ingot casting device is positioned at below water-cooled transport tape, and the flow-guiding mouth of water-cooled transport tape is positioned at directly over the quartz crucible center of ingot casting device, to ensure that the silicon liquid flowed out from flow-guiding mouth adds the quartz crucible of ingot casting device smoothly.
Ingot casting device comprises the magnetism servo-electric motor water-cooling 7 being fixedly installed in body of heater inner bottom part, and this magnetism servo-electric motor water-cooling is provided with quartz crucible, quartz crucible outer wall is provided with from inside to outside well heater 8 and insulation sleeve 9.
Magnetism servo-electric motor water-cooling can adopt water-cooled ingot pulling mechanism, now adopts the graphite heater of one, keeps liquid and draw ingot to realize directional long crystal technique by heating; Also fixing magnetism servo-electric motor water-cooling can be adopted, now adopt the graphite heater of split, this graphite heater is divided into three, upper, middle and lower graphite heating sheet, be arranged at the upper, middle and lower portion of quartz crucible respectively, carry out directional long crystal technique by the heating power of the graphite heating sheet regulating upper, middle and lower, this ingot casting device can realize all processes of directional long crystal casting ingot process.
Embodiment 2:
Adopt the device described in embodiment 1, carry out the deoxygenation of electron beam melting polysilicon and ingot casting coupling technique, concrete steps are as follows:
(1) charging vacuumizes: be 10-12mm by granular size, purity is 99.996%, oxygen level is put into feeding device after the polycrystalline silicon material cleaning, drying of 20ppmw, bottom the quartz crucible of ingot casting device, lay the polycrystalline silicon ingot casting bed material of 6N, 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: added the polycrystalline silicon material in step (1) by feeding device on electron beam melting furnace water-cooled transport tape continuously, start melting electron beam gun, the electron beam line of setting melting electron beam gun is 1200mA fusing and melting 15min polycrystalline silicon material tentatively removes impurity oxygen wherein;
(3) deoxygenation further: the polysilicon liquid after preliminary deoxygenation flows downward along water-cooled transport tape and keep liquid deoxygenation further under the effect of radiation electron beam gun, obtain the polysilicon liquid after deoxygenation, the electron beam line setting radiation electron beam gun in this process is 800mA;
(4) polycrystalline silicon casting ingot process: the 6N(massfraction laid bottom the quartz crucible of heat fused ingot casting device is 99.9999%) polycrystalline silicon ingot casting bed material, being guided by flow-guiding mouth by polysilicon liquid after deoxygenation enters in the quartz crucible of ingot casting device, the heater power controlling ingot casting device maintains this polysilicon liquid for liquid, this polysilicon liquid is added continuously in the quartz crucible of ingot casting device, to reach quartz crucible volume 80% after, carry out directional long crystal casting ingot process, controlling directional long crystal speed in this process is 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, namely lower than 0.0571ppmw.
Embodiment 3:
Adopt the device described in embodiment 1, carry out the deoxygenation of electron beam melting polysilicon and ingot casting coupling technique, concrete steps are as follows:
(1) charging vacuumizes: be 24-30mm by granular size, purity is 99.997%, oxygen level is put into feeding device after the polycrystalline silicon material cleaning, drying of 11ppmw, bottom the quartz crucible of ingot casting device, lay the polycrystalline silicon ingot casting bed material of 6N, and the vacuum tightness of body of heater is evacuated to 4 × 10 -2pa, the vacuum tightness of electron beam gun is evacuated to 4.5 × 10 -3pa, pre-thermionic electron guns 13min;
(2) preliminary deoxygenation: added the polycrystalline silicon material in step (1) by feeding device on electron beam melting furnace water-cooled transport tape continuously, start melting electron beam gun, the electron beam line of setting melting electron beam gun is 800mA fusing and melting 5min polycrystalline silicon material tentatively removes impurity oxygen wherein;
(3) deoxygenation further: the polysilicon liquid after preliminary deoxygenation flows downward along water-cooled transport tape and keep liquid deoxygenation further under the effect of radiation electron beam gun, obtain the polysilicon liquid after deoxygenation, the electron beam line setting radiation electron beam gun in this process is 500mA;
(4) polycrystalline silicon casting ingot process: the 6N polycrystalline silicon ingot casting bed material laid bottom the quartz crucible of heat fused ingot casting device, polysilicon liquid after deoxygenation is guided by flow-guiding mouth and enters in the quartz crucible of ingot casting device, the heater power controlling ingot casting device maintains this polysilicon liquid for liquid, this polysilicon liquid is added continuously in the quartz crucible of ingot casting device, to reach quartz crucible volume 82% after carry out directional long crystal casting ingot process, controlling directional long crystal speed in this process is 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, namely lower than 0.0571ppmw.
Embodiment 4
Adopt the device described in embodiment 1, carry out the deoxygenation of electron beam melting polysilicon and ingot casting coupling technique, concrete steps are as follows:
(1) charging vacuumizes: be 15-20mm by granular size, purity is 99.998%, oxygen level is put into feeding device after the polycrystalline silicon material cleaning, drying of 4ppmw, bottom the quartz crucible of ingot casting device, lay the polycrystalline silicon ingot casting bed material of 6N, and the vacuum tightness of body of heater is evacuated to 4.5 × 10 -2pa, the vacuum tightness of electron beam gun is evacuated to 4.7 × 10 -3pa, pre-thermionic electron guns 10min;
(2) preliminary deoxygenation: added the polycrystalline silicon material in step (1) by feeding device on electron beam melting furnace water-cooled transport tape continuously, start melting electron beam gun, the electron beam line of setting melting electron beam gun is 200mA fusing and melting 20min polycrystalline silicon material tentatively removes impurity oxygen wherein;
(3) deoxygenation further: the polysilicon liquid after preliminary deoxygenation flows downward along water-cooled transport tape and keep liquid deoxygenation further under the effect of radiation electron beam gun, obtain the polysilicon liquid after deoxygenation, the electron beam line setting radiation electron beam gun in this process is 200mA;
(4) polycrystalline silicon casting ingot process: the 6N polycrystalline silicon ingot casting bed material laid bottom the quartz crucible of heat fused ingot casting device, polysilicon liquid after deoxygenation is guided by flow-guiding mouth and enters in the quartz crucible of ingot casting device, the heater power controlling ingot casting device maintains this polysilicon liquid for liquid, this polysilicon liquid is added continuously in the quartz crucible of ingot casting device, to reach quartz crucible volume 85% after carry out directional freeze casting ingot process, controlling directional long crystal speed in this process is 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, namely lower than 0.0571ppmw.

Claims (10)

1. the method that is coupled with ingot casting of electron beam melting polysilicon deoxygenation, is characterized in that: first body of heater and electron beam gun are vacuumized, pre-thermionic electron guns; Then on electron beam melting furnace water-cooled transport tape, add polycrystalline silicon material by feeding device continuously, start melting electron beam gun and carry out electron beam melting to polycrystalline silicon material, melting tentatively removes impurity oxygen; Polysilicon liquid after preliminary deoxygenation flows downward along water-cooled transport tape and under the effect of radiation electron beam gun, keeps liquid deoxygenation further, obtains the polysilicon liquid after deoxygenation; Finally being guided by flow-guiding mouth by the polysilicon liquid after deoxygenation enters in ingot casting device, carries out directional long crystal casting ingot process, obtains polycrystalline silicon ingot casting.
2. the method that is coupled with ingot casting of a kind of electron beam melting polysilicon according to claim 1 deoxygenation, is characterized in that concrete steps are as follows:
(1) charging vacuumizes: be put into feeding device after the polycrystalline silicon material cleaning, drying of 10-30mm by granular size, the polycrystalline silicon ingot casting bed material of 6N is laid bottom the quartz crucible of ingot casting device, and body of heater and electron beam gun are vacuumized, pre-thermionic electron guns 10-15min;
(2) preliminary deoxygenation: added the polycrystalline silicon material in step (1) by feeding device on electron beam melting furnace water-cooled transport tape continuously, start melting electron beam gun, the electron beam line of setting melting electron beam gun is 200-1200mA fusing and impurity oxygen wherein tentatively removed by melting polysilicon material;
(3) deoxygenation further: the polysilicon liquid after preliminary deoxygenation flows downward along water-cooled transport tape and keep liquid deoxygenation further under the effect of radiation electron beam gun, obtain the polysilicon liquid after deoxygenation, the electron beam line setting radiation electron beam gun in this process is 200-800mA;
(4) polycrystalline silicon casting ingot process: the 6N polycrystalline silicon ingot casting bed material laid bottom the quartz crucible of heat fused ingot casting device, being guided by flow-guiding mouth by polysilicon liquid after deoxygenation enters in the quartz crucible of ingot casting device, the heater power maintenance polysilicon controlling ingot casting device is liquid, this polysilicon liquid is added continuously in the quartz crucible of ingot casting device, to the 80%-85% reaching quartz crucible volume, carry out directional long crystal casting ingot process, obtain the polycrystalline silicon ingot casting of electron beam deoxygenation.
3., according to the method that the arbitrary described a kind of electron beam melting polysilicon deoxygenation of claim 1 or 2 is coupled with ingot casting, it is characterized in that: the low vacuum of described body of heater is in 5 × 10 -2pa, the low vacuum of described electron beam gun is in 5 × 10 -3pa.
4., according to the method that the arbitrary described a kind of electron beam melting polysilicon deoxygenation of claim 1 or 2 is coupled with ingot casting, it is characterized in that: described polycrystalline silicon material purity is 99.996%-99.998%, oxygen level is 4-20ppmw.
5. the method that is coupled with ingot casting of a kind of electron beam melting polysilicon according to claim 2 deoxygenation, is characterized in that: in described step (2), the smelting time of the impurity oxygen that melting polysilicon material is removed wherein is 5-20min.
6. the equipment that is coupled with ingot casting of electron beam melting polysilicon according to claim 1 deoxygenation, comprises body of heater, it is characterized in that: be provided with electron beam melting assembly and ingot casting coupling assembly in body of heater, wherein:
Electron beam melting assembly comprises the water-cooled transport tape being installed on body of heater internal upper part, the furnace body wall of this water-cooled transport tape side is provided with feeding device, the discharge port of this feeding device is positioned at above water-cooled transport tape, this water-cooled transport tape opposite side is downward-sloping and be provided with flow-guiding mouth, and this water-cooled transport tape top body of heater is installed with melting electron beam gun and radiation electron beam gun;
Ingot casting coupling assembly comprises ingot casting device, and ingot casting device is positioned at below water-cooled transport tape, and the flow-guiding mouth of water-cooled transport tape is positioned at directly over the quartz crucible center of ingot casting device.
7. the equipment that is coupled with ingot casting of a kind of electron beam melting polysilicon according to claim 6 deoxygenation, it is characterized in that: described water-cooled transport tape is downward-sloping, the angle of inclination between itself and horizontal plane is 5 ° ~ 15 °.
8. the equipment that is coupled with ingot casting of a kind of electron beam melting polysilicon according to claim 6 deoxygenation, it is characterized in that: described ingot casting device comprises the magnetism servo-electric motor water-cooling being fixedly installed in body of heater inner bottom part, this magnetism servo-electric motor water-cooling is provided with quartz crucible, quartz crucible outer wall is provided with from inside to outside well heater and insulation sleeve.
9. the equipment that is coupled with ingot casting of a kind of electron beam melting polysilicon according to claim 8 deoxygenation, 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.
10. the equipment that is coupled with ingot casting of a kind of electron beam melting polysilicon according to claim 8 deoxygenation, 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, upper, middle and lower graphite heating sheet.
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TWI553127B (en) * 2015-11-13 2016-10-11 Nat Inst Chung Shan Science & Technology An electron beam vacuum refining furnace
CN106555224A (en) * 2015-09-30 2017-04-05 枣庄市天工新能源器材有限公司 A kind of production method and production equipment of monocrystal silicon
CN109023521A (en) * 2018-08-29 2018-12-18 孟静 The preparation method of solar cell module polysilicon chip

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