CN104651929B - A kind of method and apparatus that the deoxygenation of electron-beam smelting polysilicon is coupled with ingot casting - Google Patents

A kind of method and apparatus that the deoxygenation of electron-beam smelting polysilicon is coupled with ingot casting Download PDF

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CN104651929B
CN104651929B CN201310596052.5A CN201310596052A CN104651929B CN 104651929 B CN104651929 B CN 104651929B CN 201310596052 A CN201310596052 A CN 201310596052A CN 104651929 B CN104651929 B CN 104651929B
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ingot casting
electron
deoxygenation
polycrystalline silicon
smelting
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CN104651929A (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 NEW ENERGY SOLUTIONS Inc (NESI)
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Abstract

The invention belongs to metallurgical smelting fields, more particularly to a kind of method and apparatus that the deoxygenation of electron-beam smelting polysilicon is coupled with ingot casting, this method first vacuumizes furnace body and electron gun, starts melting and carries out electron-beam smelting to polycrystalline silicon material with electron gun, melting tentatively removes impurity oxygen;The further deoxygenation of liquid is kept in the case where radiation is acted on electron gun, it is led into ingot casting device finally by water cooling transmission belt, it is oriented long crystalline substance, obtain polycrystalline silicon ingot casting, the equipment includes electron-beam smelting component and ingot casting coupling assembly, ingot casting coupling assembly includes ingot casting device, ingot casting device is located at below water cooling transmission belt, and the flow-guiding mouth of water cooling transmission belt is located at the surface at the silica crucible center of ingot casting device, present invention firstly provides the process of electron-beam smelting deoxygenation and purposes, realize the effect of electron beam deoxygenation, it is coupled in combination with ingot casting, reduce the energy consumption needed for ingot casting heating raw material, substantially increase production efficiency.

Description

A kind of method and apparatus that the deoxygenation of electron-beam smelting polysilicon is coupled with ingot casting
Technical field
The invention belongs to metallurgical smelting field, more particularly to a kind of side that the removal of impurities of electron-beam smelting polysilicon is coupled with ingot casting Method additionally relates to its equipment.
Background technology
Currently, China has become world energy sources production and consumption big country, but per capita energy's level of consumption is also very low.With warp The continuous development of Ji and society, China's energy demand is by sustainable growth, and for current energy shortage situation, countries in the world all exist Deep thinking is carried out, and makes great efforts to improve efficiency of energy utilization, promotes the development and application of regenerative resource, reduces to import stone Energy security is reinforced in the dependence of oil.
The solar energy power generating of one of important development direction as regenerative resource develops rapidly in recent years, shared by Proportion is increasing.According to《Regenerative resource Long-and Medium-term Development is planned》, the year two thousand twenty is arrived, China strives that solar power generation is made to install Capacity reaches 1.8GW(Gigawatt), 600GW is up to the year two thousand fifty.Expect the year two thousand fifty, the electric power of Chinese regenerative resource Installation will account for the 25% of national electric power installation, and wherein photovoltaic generation installation will account for 5%.It is expected that before the year two thousand thirty, Chinese solar energy The compound growth rate of installed capacity will be up to 25% or more.
The development of solar photovoltaic industry is dependent on the purification to polycrystalline silicon raw material.The purifying technique of polycrystalline silicon raw material is current Rely primarily on following several techniques:Siemens Method, silane thermal decomposition process, gas fluidized bed process and metallurgy method.Metallurgy method prepares solar level The only way which must be passed of polycrystalline silicon technology as development low cost, environmental-friendly solar-grade polysilicon technology of preparing, at present Tremendous development is achieved, and realizes industrialized production.Metallurgy method purifying polycrystalline silicon refer to use Physical Metallurgy means, silicon not In the case that participation chemically reacts, the method for removing the various impurity elements (phosphorus, boron and metal) in silicon successively, it is not Single preparation method, but a kind of Integration Method, it is mainly former using saturated vapor pressure principle, segregation principle and oxidation sex differernce Reason, is respectively adopted different processes, to remove the impurity element in silicon, is wanted to obtain meeting solar energy polycrystalline silicon purity The silicon material asked.
In metallurgy method technique, the phosphorus of silicon material, boron, metal impurities can be removed by effective process means, be reached Comparatively ideal effect.But in recent years, it is found in the research to polysilicon solar battery slice electricity conversion, oxygen The content of element has an important influence on the electricity conversion of cell piece, when general oxygen is in interstitial site, usually not aobvious electricity Activity, however oxygen concentration is usually 3 × 10 in casting polysilicon17~1.4 × 1018cm-3Between, the interstitial oxygen concentration of high concentration with During device fabrication afterwards, the heat treatment of various temperature is undergone, can be applied in segregation and precipitation, formation oxygen pass in silicon crystal The defects of master, oxygen precipitation.Meanwhile silicon crystal material growth, it is cooling during since the solubility with temperature of oxygen reduces and Rapid to decline, oversaturated oxygen will form grown-in oxygen precipitates in casting polysilicon, it is also possible to be formed with other impurity various each The complex of sample, such as N-O, C-O complex.These oxygen precipitations and its complex can not only reduce the effect of the outer gettering of phosphorus, even It is directly becoming the short-channel of battery.
These oxygen defects there is advantageous and unfavorable both sides to influence silicon materials and device, it can combine device technology Intrinsic gettering is formed, gettering metal impurity can improve the mechanical strength of silicon chip, but again when oxygen precipitation excess with pinning dislocation Other crystal defects can be induced, a large amount of secondary defect is introduced, can also attract the metallic elements such as iron, it is compound to form iron oxygen precipitation Body has very strong few sub- compound ability, can significantly reduce the conversion efficiency of solar cell of material.
In the techniques such as directional solidification, the ingot casting of metallurgy method, oxygen element in crucible or the oxygen element that is passed through in gas are not Avoidable ground can enter in silicon material, be the main reason for oxygen impurities generate.The common method of oxygen content in traditional test silicon For infrared spectrum, with infrared spectrum respectively to high-purity silicon material and batch mixing(Leftover pieces after casting casting are mixed with high pure material)It is examined It surveys, the content of oxygen is not much different in two kinds of material, this also results in the oxygen impurities introduced in metallurgy method technique and is not affected by attention.
In fact, in silicon, there are two types of states for oxygen element:Substitute position, i.e., oxygen instead of silicon position;Gap digit, i.e. oxygen In the gap of silicon atom.In traditional test silicon the infrared spectrum of oxygen content can only detector gap position oxygen content, Bu Nengzhen Oxygen levels in two kinds of silicon materials of real reflection.Experiment test through applicant, substitute position oxygen can discharge it is miscellaneous in electronics, with silicon The effect that matter phosphorus generates is similar, can influence polycrystalline silicon battery plate electricity conversion.Applicant passes through ion microprobe Repeated detection, in above two silicon material, oxygen element content differs greatly, and mainly substitutes the difference of the oxygen element content of position. Therefore, the impurity oxygen introduced in the techniques such as ingot casting cannot be ignored, it is necessary to which seeking effective means reduces impurity oxygen in silicon Content.
But in the prior art, bad to the removal effect of oxygen element.For the minimizing technology of oxygen impurities, hair is retrieved Bright patent CN200810070925 is a kind of reduce metal Oxygen in silicon, carbon content method, the invention in silicon liquid using being blown into oxygen Gas, hydrogen and vapor make hydrogen and oxygen be reacted in silicon liquid and generate localized hyperthermia, makes oxygen in silicon liquid, carbon with gas Body is discharged and is removed, but this method needs are passed through oxygen and hydrogen under silicon molten condition, and operation difficulty is big, dangerous high, The removal effect of oxygen is bad.
Meanwhile effectively reducing in polycrystalline silicon ingot casting raw material after oxygen content, you can polycrystalline is obtained by directional long crystal technique Silicon ingot casting, but casting ingot method before is all to directly heat ingot casting raw material, can not achieve ingot casting coupling, it is big with duration, energy consumption.
Invention content
In order to overcome the above the deficiencies in the prior art, the present invention proposes a kind of electron-beam smelting polysilicon deoxygenation and ingot casting The method of coupling removes the impurity oxygen in polycrystalline silicon raw material by electron-beam smelting, the polycrystalline silicon liquid of high-purity low-oxygen is obtained, by this Polycrystalline silicon liquid is guided directly into ingot casting coupling device and completes directional long crystal casting ingot process, obtains the polysilicon casting of high-purity low-oxygen Ingot, this method effectively reduce the oxygen content in silicon material, improve the transfer efficiency of battery, reduce the work of ingot casting raw material heating Sequence realizes ingot casting coupling effect, reduces the process time, reduces the total energy consumption in production process, saves cost.
The method that a kind of electron-beam smelting polysilicon deoxygenation of the present invention is coupled with ingot casting, first by furnace body and electronics Rifle vacuumizes, pre- thermionic electron guns;Then polysilicon is continuously added to in electron beam furnace water cooling transmission belt by feeding device Material starts melting and carries out electron-beam smelting to polycrystalline silicon material with electron gun, and melting tentatively removes impurity oxygen;It is more after preliminary deoxygenation Crystal silicon liquid flows downward along water cooling transmission belt and keeps the further deoxygenation of liquid in the case where radiation is acted on electron gun, after obtaining deoxygenation Polycrystalline silicon liquid;Finally the polycrystalline silicon liquid after deoxygenation is led by flow-guiding mouth in ingot casting device, is oriented long brilliant casting Ingot technique, obtains polycrystalline silicon ingot casting.
It is preferred that following the steps below:
(1)Charging vacuumizes:By granular size to be put into feeding device after the polycrystalline silicon material cleaning, drying of 10-30mm, It is laid with the polycrystalline silicon ingot casting bottom material of 6N in the silica crucible bottom of ingot casting device, and furnace body and electron gun are vacuumized, pre- thermoelectricity Sub- rifle 10-15min;
(2)Preliminary deoxygenation:By feeding device step is continuously added to in electron beam furnace water cooling transmission belt(1)In Polycrystalline silicon material starts melting electron gun, sets the electron beam line of melting electron gun as 200-1200mA fusings and melting Polycrystalline silicon material tentatively removes impurity oxygen therein;
(3)Further deoxygenation:Polycrystalline silicon liquid after preliminary deoxygenation flows downward along water cooling transmission belt and in radiation electronics Rifle effect is lower to keep the further deoxygenation of liquid, obtains the polycrystalline silicon liquid after deoxygenation, the electricity of radiation electron gun is set during this Beamlet line is 200-800mA;
(4)Polycrystalline silicon casting ingot process:The 6N polycrystalline silicon ingot castings bottom that the silica crucible bottom of heating fusing ingot casting device is laid with Material makes it be liquid, and the polycrystalline silicon liquid after deoxygenation is led by flow-guiding mouth in the silica crucible of ingot casting device, control casting It is liquid that the heater power of ingot device, which maintains polysilicon, and the polycrystalline silicon liquid is continuously added into the silica crucible of ingot casting device, To the 80%-85% for reaching silica crucible volume, it is oriented long brilliant casting ingot process, obtains the polysilicon casting of electron beam deoxygenation Ingot.
The vacuum degree of the furnace body is less than 5 × 10-2The vacuum degree of Pa, the electron gun are less than 5 × 10-3Pa。
The polycrystalline silicon material purity is 99.996%-99.998%, oxygen content 4-20ppmw.
The step(2)The smelting time that middle melting polysilicon material removes impurity oxygen therein is 5-20min.
The equipment that electron-beam smelting polysilicon deoxygenation of the present invention is coupled with ingot casting, including furnace body, it is characterised in that: Electron-beam smelting component and ingot casting coupling assembly are provided in furnace body, wherein:
Electron-beam smelting component includes the water cooling transmission belt for being installed on furnace body internal upper part, the furnace body of the water cooling transmission belt side Feeding device is provided on wall, the discharge port of the feeding device is located above water cooling transmission belt, and the water cooling transmission belt is another lateral Lower inclination is simultaneously equipped with flow-guiding mouth, and melting electron gun and radiation electronics are installed on furnace body at the top of the water cooling transmission belt Rifle;
Ingot casting coupling assembly includes ingot casting device, ingot casting device is located at below water cooling transmission belt, and water cooling transmission belt is led Head piece is located at the surface at the silica crucible center of ingot casting device.
The water cooling transmission belt tilts down, and the angle of inclination between horizontal plane is 5 °~15 °.
The ingot casting device includes the magnetism servo-electric motor water-cooling for being fixedly installed in bottom in furnace body, which is equipped with quartzy earthenware Crucible is equipped with heater and heat preservation sleeve on silica crucible outer wall from inside to outside.
The magnetism servo-electric motor water-cooling uses water cooling ingot pulling mechanism, the graphite heater that the heater is integrated.
The magnetism servo-electric motor water-cooling is fixed magnetism servo-electric motor water-cooling, and the heater is seperated graphite heater, including it is upper, in, Lower three graphite heating pieces.
In the present invention, it has been put forward for the first time the process and purposes of electron-beam smelting deoxygenation, has utilized electron-beam smelting height The characteristic of warm evaporative removal impurity melts the simultaneously preliminary deoxygenation of melting by melting electron gun, in water cooling in water cooling transmission belt Further efficient deoxygenation under the action of radiation electron gun on large surface area in transmission belt, and liquid is maintained to enter casting In ingot device, the liquid high-purity polycrystalline silicon raw material of hypoxemia is provided for casting ingot process, and carries out directional long crystal casting ingot process, is realized The effect of ingot casting coupling, the present invention realize the effect of electron beam deoxygenation, are coupled in combination with ingot casting, reduce electron-beam smelting The time of solidification and ingot casting heating raw material afterwards reduces the energy consumption needed for ingot casting heating raw material, substantially increases production efficiency.
The advantage of the invention is that:
(1)The process and purposes for proposing electron beam deoxygenation solve the problems, such as that impurity oxygen removes in polysilicon, oxygen Content can be reduced to 0.0571ppmw, meet requirement of the solar cell to polycrystalline silicon ingot casting oxygen content.
(2)By the further deoxygenation of radiation electric beamlet when realizing the preliminary deoxygenation of melting and the flowing of polysilicon liquid, shorten 20% or more deoxygenation time.
(3)Electron-beam smelting deoxygenation technology is coupled with ingot casting technology, realizes continuous production, production efficiency 40% can be improved More than, save 25% or more energy consumption.
Description of the drawings
Fig. 1 is the structural diagram of the present invention;
In figure:1, furnace body 2, water cooling transmission belt 3, melting electron gun 4, radiation electron gun 5, feeding device 6, silica crucible 7, magnetism servo-electric motor water-cooling 8, heater 9, heat preservation sleeve 10, flow-guiding mouth
Specific implementation mode
With reference to specific embodiments and the drawings, the present invention will be described in detail, but the invention is not limited in specific embodiments.
Embodiment 1:
As shown in Figure 1, the equipment that the deoxygenation of electron-beam smelting polysilicon is coupled with ingot casting, including furnace body, it is provided in furnace body 1 Electron-beam smelting component and ingot casting coupling assembly, wherein:
Electron-beam smelting component includes the water cooling transmission belt 2 for being installed on furnace body internal upper part, the stove of the water cooling transmission belt side Feeding device 5 is provided on body wall, the discharge port of the feeding device is located above water cooling transmission belt, the water cooling transmission belt other side Flow-guiding mouth is tilted down and be equipped with, baltimore groove is provided in water cooling transmission belt, for guiding the polycrystalline silicon liquid of the preliminary deoxygenation of melting It flows, and is entered in ingot casting device by the flow-guiding mouth in water cooling transmission belt, the water cooling transmission belt top to the direction of ingot casting device Melting electron gun 3 and radiation electron gun 4 are installed on portion's furnace body;
Water cooling transmission belt is made of copper product, wherein it is passed through recirculated cooling water, to avoid melting and damaging, water cooling transmission belt It tilts down, the angle of inclination between horizontal plane is 5 °, so that silicon liquid is smoothly downward along baltimore groove in water cooling transmission belt Flowing, and entered in the silica crucible 6 in ingot casting device by flow-guiding mouth 10.
Ingot casting coupling assembly includes ingot casting device, ingot casting device is located at below water cooling transmission belt, and water cooling transmission belt is led Head piece is located at the surface at the silica crucible center of ingot casting device, to ensure that ingot casting dress is smoothly added in the silicon liquid flowed out from flow-guiding mouth In the silica crucible set.
Ingot casting device includes the magnetism servo-electric motor water-cooling 7 for being fixedly installed in bottom in furnace body, which is equipped with silica crucible, Heater 8 and heat preservation sleeve 9 are equipped on silica crucible outer wall from inside to outside.
Water cooling ingot pulling mechanism may be used in magnetism servo-electric motor water-cooling, uses the graphite heater of one at this time, and liquid is kept by heating State realizes directional long crystal technique with ingot is drawn;Fixed magnetism servo-electric motor water-cooling can also be used, uses seperated graphite heater at this time, The graphite heater is divided into the graphite heating piece of upper, middle and lower three, is respectively arranged at the upper, middle and lower portion of silica crucible, passes through tune The heating power of the graphite heating piece of upper, middle and lower is saved to be oriented crystal growing technology, which can realize that directional long crystal is cast The all processes of ingot technique.
Embodiment 2:
Using device described in embodiment 1, the deoxygenation of electron-beam smelting polysilicon and ingot casting coupling technique, specific steps are carried out It is as follows:
(1)Charging vacuumizes:By the polycrystalline that granular size is 10-12mm, purity 99.996%, oxygen content are 20ppmw It is put into feeding device after silicon material cleaning, drying, the polycrystalline silicon ingot casting bottom material of 6N is laid in the silica crucible bottom of ingot casting device, And the vacuum degree of furnace body is evacuated to 3 × 10-2The vacuum degree of Pa, electron gun are evacuated to 4 × 10-3Pa, pre- thermionic electron guns 15min;
(2)Preliminary deoxygenation:By feeding device step is continuously added to in electron beam furnace water cooling transmission belt(1)In Polycrystalline silicon material starts melting electron gun, sets the electron beam line of melting electron gun as 1200mA fusings and melting 15min Polycrystalline silicon material tentatively removes impurity oxygen therein;
(3)Further deoxygenation:Polycrystalline silicon liquid after preliminary deoxygenation flows downward along water cooling transmission belt and in radiation electronics Rifle effect is lower to keep the further deoxygenation of liquid, obtains the polycrystalline silicon liquid after deoxygenation, the electricity of radiation electron gun is set during this Beamlet line is 800mA;
(4)Polycrystalline silicon casting ingot process:The 6N that the silica crucible bottom of heating fusing ingot casting device is laid with(Mass fraction is 99.9999%)Polycrystalline silicon liquid after deoxygenation is led into the quartzy earthenware of ingot casting device by polycrystalline silicon ingot casting bottom material by flow-guiding mouth In crucible, the heater power for controlling ingot casting device maintains the polycrystalline silicon liquid for liquid, continuously into the silica crucible of ingot casting device The polycrystalline silicon liquid is added, until reach silica crucible volume 80% after, be oriented long brilliant casting ingot process, it is fixed to control during this It is 1.2cm-1.3cm/h (centimetre per hour) to long brilliant speed, obtains the polycrystalline silicon ingot casting of electron beam deoxygenation, the polycrystalline silicon ingot casting Through Secondary Ion Mass Spectrometry(SIMS)Detection, oxygen content are less than Secondary Ion Mass Spectrometry detectable limit, that is, are less than 0.0571ppmw.
Embodiment 3:
Using device described in embodiment 1, the deoxygenation of electron-beam smelting polysilicon and ingot casting coupling technique, specific steps are carried out It is as follows:
(1)Charging vacuumizes:By the polycrystalline that granular size is 24-30mm, purity 99.997%, oxygen content are 11ppmw It is put into feeding device after silicon material cleaning, drying, the polycrystalline silicon ingot casting bottom material of 6N is laid in the silica crucible bottom of ingot casting device, And the vacuum degree of furnace body is evacuated to 4 × 10-2The vacuum degree of Pa, electron gun are evacuated to 4.5 × 10-3Pa, pre- thermionic electron guns 13min;
(2)Preliminary deoxygenation:By feeding device step is continuously added to in electron beam furnace water cooling transmission belt(1)In Polycrystalline silicon material starts melting electron gun, and the electron beam line for setting melting electron gun is melted as 800mA and melting 5min is more Crystal silicon material tentatively removes impurity oxygen therein;
(3)Further deoxygenation:Polycrystalline silicon liquid after preliminary deoxygenation flows downward along water cooling transmission belt and in radiation electronics Rifle effect is lower to keep the further deoxygenation of liquid, obtains the polycrystalline silicon liquid after deoxygenation, the electricity of radiation electron gun is set during this Beamlet line is 500mA;
(4)Polycrystalline silicon casting ingot process:The 6N polycrystalline silicon ingot castings bottom that the silica crucible bottom of heating fusing ingot casting device is laid with Material, the polycrystalline silicon liquid after deoxygenation are led by flow-guiding mouth in the silica crucible of ingot casting device, and the heating of ingot casting device is controlled It is liquid that device power, which maintains the polycrystalline silicon liquid, the polycrystalline silicon liquid is continuously added into the silica crucible of ingot casting device, until reaching stone Directional long crystal casting ingot process is carried out after the 82% of English crucible volume, control directional long crystal speed is 1.2cm-1.3cm/h during this (centimetre per hour), obtains the polycrystalline silicon ingot casting of electron beam deoxygenation, the polycrystalline silicon ingot casting is through Secondary Ion Mass Spectrometry(SIMS)Detection, Its oxygen content is less than Secondary Ion Mass Spectrometry detectable limit, that is, is less than 0.0571ppmw.
Embodiment 4
Using device described in embodiment 1, the deoxygenation of electron-beam smelting polysilicon and ingot casting coupling technique, specific steps are carried out It is as follows:
(1)Charging vacuumizes:By the polysilicon that granular size is 15-20mm, purity 99.998%, oxygen content are 4ppmw It is put into feeding device after material cleaning, drying, it is laid with the polycrystalline silicon ingot casting bottom material of 6N in the silica crucible bottom of ingot casting device, and The vacuum degree of furnace body is evacuated to 4.5 × 10-2The vacuum degree of Pa, electron gun are evacuated to 4.7 × 10-3Pa, pre- thermionic electron guns 10min;
(2)Preliminary deoxygenation:By feeding device step is continuously added to in electron beam furnace water cooling transmission belt(1)In Polycrystalline silicon material starts melting electron gun, sets the electron beam line of melting electron gun as 200mA fusings and melting 20min Polycrystalline silicon material tentatively removes impurity oxygen therein;
(3)Further deoxygenation:Polycrystalline silicon liquid after preliminary deoxygenation flows downward along water cooling transmission belt and in radiation electronics Rifle effect is lower to keep the further deoxygenation of liquid, obtains the polycrystalline silicon liquid after deoxygenation, the electricity of radiation electron gun is set during this Beamlet line is 200mA;
(4)Polycrystalline silicon casting ingot process:The 6N polycrystalline silicon ingot castings bottom that the silica crucible bottom of heating fusing ingot casting device is laid with Material, the polycrystalline silicon liquid after deoxygenation are led by flow-guiding mouth in the silica crucible of ingot casting device, and the heating of ingot casting device is controlled It is liquid that device power, which maintains the polycrystalline silicon liquid, the polycrystalline silicon liquid is continuously added into the silica crucible of ingot casting device, until reaching stone Directional solidification casting ingot process is carried out after the 85% of English crucible volume, control directional long crystal speed is 1.2cm-1.3cm/h during this (centimetre per hour), obtains the polycrystalline silicon ingot casting of electron beam deoxygenation, the polycrystalline silicon ingot casting is through Secondary Ion Mass Spectrometry(SIMS)Detection, Its oxygen content is less than Secondary Ion Mass Spectrometry detectable limit, that is, is less than 0.0571ppmw.

Claims (8)

1. a kind of method that the deoxygenation of electron-beam smelting polysilicon is coupled with ingot casting, it is characterised in that:First by furnace body and electron gun It vacuumizes, pre- thermionic electron guns;Then polycrystalline silicon material is continuously added to in electron beam furnace water cooling transmission belt by feeding device, Start melting and electron-beam smelting is carried out to polycrystalline silicon material with electron gun, melting tentatively removes impurity oxygen;Polycrystalline after preliminary deoxygenation Silicon liquid flows downward along water cooling transmission belt and keeps the further deoxygenation of liquid in the case where radiation is acted on electron gun, after obtaining deoxygenation Polycrystalline silicon liquid;Finally the polycrystalline silicon liquid after deoxygenation is led by flow-guiding mouth in ingot casting device, is oriented long brilliant casting Ingot technique, obtains polycrystalline silicon ingot casting.
2. the method that a kind of electron-beam smelting polysilicon deoxygenation according to claim 1 is coupled with ingot casting, it is characterised in that It is as follows:(1)Charging vacuumizes:Granular size is filled to be put into charging after the polycrystalline silicon material cleaning, drying of 10-30mm In setting, it is laid with the polycrystalline silicon ingot casting bottom material of 6N in the silica crucible bottom of ingot casting device, and furnace body and electron gun are vacuumized, Pre- thermionic electron guns 10-15min;(2)Preliminary deoxygenation:It is continuously added to in electron beam furnace water cooling transmission belt by feeding device Step(1)In polycrystalline silicon material, start melting electron gun, set the electron beam line of melting electron gun as 200-1200mA It melts and melting polysilicon material tentatively removes impurity oxygen therein;(3)Further deoxygenation:Polycrystalline silicon liquid after preliminary deoxygenation is along water Cold transmission belt flows downward and keeps the further deoxygenation of liquid in the case where radiation is acted on electron gun, obtains the polysilicon after deoxygenation Liquid, this sets the electron beam line of radiation electron gun as 200-800mA in the process;(4)Polycrystalline silicon casting ingot process:Heating is molten Change the 6N polycrystalline silicon ingot casting bottom materials that the silica crucible bottom of ingot casting device is laid with, the polycrystalline silicon liquid after deoxygenation is passed through into flow-guiding mouth Lead into the silica crucible of ingot casting device, control ingot casting device heater power maintain polysilicon be liquid, continuously to The polycrystalline silicon liquid is added in the silica crucible of ingot casting device, until after reaching the 80%-85% of silica crucible volume, is oriented long crystalline substance Casting ingot process obtains the polycrystalline silicon ingot casting of electron beam deoxygenation.
3. special according to the method that a kind of any electron-beam smelting polysilicon deoxygenation of claims 1 or 2 is coupled with ingot casting Sign is:The vacuum degree of the furnace body is less than 5 × 10-2Pa, and the vacuum degree of the electron gun is less than 5 × 10-3Pa.
4. according to the method that a kind of any electron-beam smelting polysilicon deoxygenation of claims 1 or 2 is coupled with ingot casting, It is characterized in that:The polycrystalline silicon material purity is 99.996%-99.998%, oxygen content 4-20ppmw.
5. the method that a kind of electron-beam smelting polysilicon deoxygenation according to claim 2 is coupled with ingot casting, feature exist In:The step(2)The smelting time that middle melting polysilicon material removes impurity oxygen therein is 5-20min.
6. a kind of equipment that the deoxygenation of electron-beam smelting polysilicon is coupled with ingot casting, including furnace body, it is characterised in that:It is arranged in furnace body There are electron-beam smelting component and ingot casting coupling assembly, wherein:Electron-beam smelting component includes the water cooling for being installed on furnace body internal upper part Transmission belt is provided with feeding device on the furnace body wall of the water cooling transmission belt side, and the discharge port of the feeding device is located at water cooling biography Above defeated band, the water cooling transmission belt is another to be sloped downwardly and is equipped with flow-guiding mouth, fixed peace on furnace body at the top of the water cooling transmission belt Equipped with melting electron gun and radiation electron gun;Ingot casting coupling assembly includes ingot casting device, and ingot casting device is located at water cooling transmission Band lower section, and the flow-guiding mouth of water cooling transmission belt is located at the surface at the silica crucible center of ingot casting device;The water cooling transmission belt It tilts down, the angle of inclination between horizontal plane is 5 °~15 °;The ingot casting device includes being fixedly installed in furnace body The magnetism servo-electric motor water-cooling of bottom, the magnetism servo-electric motor water-cooling are equipped with silica crucible, heater and guarantor are equipped with from inside to outside on silica crucible outer wall Warm sleeve.
7. the equipment that a kind of electron-beam smelting polysilicon deoxygenation according to claim 6 is coupled with ingot casting, feature exist In:The magnetism servo-electric motor water-cooling uses water cooling ingot pulling mechanism, the graphite heater that the heater is integrated.
8. the equipment that a kind of electron-beam smelting polysilicon deoxygenation according to claim 6 is coupled with ingot casting, it is characterised in that: The magnetism servo-electric motor water-cooling is fixed magnetism servo-electric motor water-cooling, and the heater is the graphite heater of fission, including the stone of upper, middle and lower three Black heating plate.
CN201310596052.5A 2013-11-22 2013-11-22 A kind of method and apparatus that the deoxygenation of electron-beam smelting polysilicon is coupled with ingot casting Expired - Fee Related CN104651929B (en)

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