CN103757695B - A kind of sidewall heat compensation device of polysilicon directional freezing equipment - Google Patents

A kind of sidewall heat compensation device of polysilicon directional freezing equipment Download PDF

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CN103757695B
CN103757695B CN201310726451.9A CN201310726451A CN103757695B CN 103757695 B CN103757695 B CN 103757695B CN 201310726451 A CN201310726451 A CN 201310726451A CN 103757695 B CN103757695 B CN 103757695B
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crucible
cavity
heating unit
polysilicon
housing
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CN103757695A (en
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朱徐立
洪永强
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Xiamen University
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Xiamen University
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Abstract

A sidewall heat compensation device for polysilicon directional freezing equipment, relates to polysilicon.There is provided can significantly reduce energy consumption and cost, equipment simple and reliable, can keep that polysilicon solidified front level rises, the sidewall heat compensation device of superior in quality a kind of polysilicon directional freezing equipment of purifying.Be provided with top cover, heating unit, housing, thermal insulation layer, crucible, heating panel; Described top cover is located at the top of housing, and heating unit and crucible are located in the cavity of housing, and heating unit is located at above crucible, and the edge of heating unit extends to cavity top; Described thermal insulation layer is wrapped in outside in cavity and bottom, holds silicon liquid in crucible, and heating panel to be placed in immediately below crucible and to fit tightly with crucible.

Description

A kind of sidewall heat compensation device of polysilicon directional freezing equipment
Technical field
The present invention relates to polysilicon, especially relate to a kind of sidewall heat compensation device of polysilicon directional freezing equipment.
Background technology
In the today of advocating low-carbon emission reduction, sun power has become the green energy resource received much concern.Polysilicon is current most widely used solar cell material.General in the process of metallurgy method purifying solar energy level polysilicon (6N level), directional freeze is an important step of removal of impurities, and at present, conventional directional solidification process has two kinds: heat-exchanging method (HEM) and Bridgman method (Bridgman).In the world, numerous production of polysilicon business as Japanese capital make pottery, the company such as Bayer Bitterfeld GmbH, French Ford Wa Ke have employed heat-exchanging method, in directional freeze process, the solidified front of silicon can keep level to rise, and refining effect is excellent.But the equipment complex and expensive of heat-exchanging method, in process of setting, the induction coil heating apparatus of top and sidewall needs a direct-open, and relies on bottom forced heat radiation to form the vertical temperature gradient of directional freeze, which results in the huge loss of electric energy.And the Bridgman method that GTSolar provides, crucible and heating unit need relative movement, and this adds the complicacy of equipment undoubtedly, also require higher reliability and wearing quality.
The domestic Dai Xin etc. being engaged in the research of metallurgy method purifying polycrystalline silicon (wears prosperous, Du Haiwen, Zhang Junyan, Wang Feng. the impact of graphite heater in polysilicon directional freezing technique. electronics manufacturing engineering, 2012, the well heater that 2:106-109) comparative studies heater top, side well heater and top-side well heater three kinds is different, thinks that the top-side well heater adopted at present can obtain good efficiency and solidified front (solid-liquid phase interface) in polysilicon melting and crystal growing process.This and heat-exchanging method are very similar, all adopt Multi-surface heating to build the thermograde of vertical direction, ensure directional freeze purification quality, but also bring the problem of equipment complexity, high energy consumption simultaneously.And general conventional apparatus for directional solidification only accommodates thermal source at top, in process of setting, sidewall leaks heat, causes solidified front to present spill, has a strong impact on the purification quality of polysilicon.
Collateral security purification quality, and reduce costs the angle with energy consumption, make full use of the latent heat of solidification of top firing device and silicon to maintain directional freeze thermal field, keeping the horizontal configuration of solidified front, is the developing direction of metallurgy method purifying polycrystalline silicon.
Summary of the invention
The shortcomings such as the heating arrangement that the object of the invention is to exist for existing solar-grade polysilicon apparatus for directional solidification is complicated, energy consumption is huge, solidified front not easily maintenance level, provide can significantly reduce energy consumption and cost, equipment simple and reliable, can keep that polysilicon solidified front level rises, the sidewall heat compensation device of superior in quality a kind of polysilicon directional freezing equipment of purifying.
The present invention is provided with top cover, heating unit, housing, thermal insulation layer, crucible, heating panel; Described top cover is located at the top of housing, and heating unit and crucible are located in the cavity of housing, and heating unit is located at above crucible, and the edge of heating unit extends to cavity top; Described thermal insulation layer is wrapped in outside in cavity and bottom, holds silicon liquid in crucible, and heating panel to be placed in immediately below crucible and to fit tightly with crucible.
The edge of described heating unit preferably extends to cavity top and higher than cavity hatch 3 ~ 10mm.
The thickness of described thermal insulation layer can be 100 ~ 350mm.
Described cavity can be axially symmetric structure, cavity is centered around the outer side of crucible and close contact, the section of cavity is up-narrow and down-wide gradual change type triangular structure of right angle, the inclined-plane of described triangular structure of right angle can be the curved surface of indent a little after plane, the vertical surface of triangular structure of right angle and plane perpendicular, the angle on bottom surface and inclined-plane can be 73 ° ~ 78 °.
The present invention is according to the principle of heat in the internal reflection of class right-angle triangle cavity, refraction, coupling, by the thermal coupling that equipment top firing device, silicon liquid upper surface and crucible wall distribute, to in silicon process of setting, crucible wall dispersed heat compensates, the heat flow density flowed out from sidewall is made to be reduced to the order of magnitude close to 0, be equal to desirable adiabatic, form vertical orientation temperature of solidification gradient, ensure that the level of solidified front rises.
The present invention takes full advantage of the heat that top heater and silicon liquid solidify the heat compensation sidewall loss of distributing, to reach the effect of sidewall thermal insulation.Both can omit the side heaters of heat-exchanging method (HEM), and again without the need to the running gear of Bridgman method (Bridgman), and excellent refining effect can have been reached, not only simplified construction, and can saves energy consumption greatly.The present invention makes polysilicon in directional freeze process, and solidified front (solid-liquid phase interface) can keep level to rise always, suitable with the refining effect of heat-exchanging method and Bridgman method, but structure simplifies greatly, and energy consumption also significantly reduces.Therefore the present invention is used can to obtain larger economic benefit and social benefit.
Accompanying drawing explanation
Fig. 1 is the schematic perspective view of the embodiment of the present invention.
Fig. 2 is the schematic top plan view of the embodiment of the present invention.
Fig. 3 is the diagrammatic cross-section of the embodiment of the present invention.
Fig. 4 is the perspective diagram of the embodiment of the present invention.
Embodiment
As illustrated in fig. 1 and 2, the embodiment of the present invention is provided with top cover 1, heating unit 2, housing 3, thermal insulation layer 4, crucible 8, heating panel 11.Described top cover 1 is located at the top of housing 3, and heating unit 2 and crucible 8 are located in the cavity 5 of housing 3, and heating unit 2 is located at above crucible 8, and the edge of heating unit 2 extends to cavity 5 top; Described thermal insulation layer 4 is wrapped in outside in cavity 5 and bottom, holds silicon liquid 9 in crucible 8, and heating panel 11 to be placed in immediately below crucible 8 and to fit tightly with crucible 8.
The edge of described heating unit 2 extends to cavity 5 top and higher than cavity 5 opening 3 ~ 10mm.
The thickness of described thermal insulation layer 4 is 100 ~ 350mm.
Described cavity 5 is axially symmetric structure, cavity 5 is centered around the outer side of crucible 8 and close contact, the section of cavity 5 is up-narrow and down-wide gradual change type triangular structure of right angle, the inclined-plane 6 of described triangular structure of right angle can be the curved surface of indent a little after plane, the vertical surface 7 of triangular structure of right angle is vertical with bottom surface 10, and bottom surface 10 can be 73 ° ~ 78 ° with the angle on inclined-plane 6.
Because top cover 1 is placed in body top, housing 3 is wrapped in outside, because herein is provided support structure and protection.
As shown in Figures 3 and 4, heating unit 2 is installed on directly over crucible 8, and edge extends to heat compensation cavity 5 top, higher than cavity 5 opening 3 ~ 10mm, for keeping surface temperature and the heating cavity 5 of silicon liquid 9; Thermal insulation layer 4 is wrapped in outside and the bottom of heat compensation cavity 5, thick 100 ~ 350mm; Heat compensation cavity 5 is axially symmetric structure, be centered around the outer side of crucible 8 and close contact, cavity 5 section is upper narrow opening (width 20 ~ 50mm), the gradual change class triangular structure of right angle of bottom wider (width 200 ~ 300mm), inside has three, is respectively inclined-plane 6, vertical surface 7, bottom surface 10, wherein, internal surface 6 can be plane, also can be the curved surface of indent a little, and face 6 is 73 ° ~ 78 ° with the angle in face 10; Silicon liquid 9 is contained among crucible 8; Heating panel 11 is placed in immediately below crucible 8, fits tightly with crucible 8.
The present invention can according to the specific requirement of output, the size of bi-directional scaling device.
Below provide some examples of sidewall heat compensation device.
Embodiment 1
Heating unit (graphite heater) is installed higher than 4 ~ 6mm place, crucible top, and the cavity cross-section upper opening of heat compensation device is 30mm, and bottom lengths is 200mm, and inclined-plane and bottom surface angle are 78 °.In cavity inner surface, inclined-plane adopts high compactness, resistant to elevated temperatures black fiber sheet material, and surfaceness is between Ra6.3 ~ Ra12.5; The vertical surface contacted with crucible adopts the graphite cake of high strength to make, and surfaceness is Ra3.2; Cavity bottom surface adopts stupalith, surface finish process, surface roughness Ra 0.1.
Embodiment 2
Heating unit (graphite heater) is installed higher than 8mm place, crucible top, and the cavity cross-section upper opening of heat compensation device is 20mm, and bottom lengths is 250mm, and inclined-plane and bottom surface angle are 73 °.In cavity inner surface, inclined-plane and vertical surface all adopt the graphite sheet of high strength to make, and surfaceness is respectively Ra6.3 and Ra3.2; Cavity bottom surface adopts stupalith, surface finish process, surface roughness Ra 0.2.
Embodiment 3
Heating unit (graphite heater) is installed higher than 5mm place, crucible top, and the cavity cross-section upper opening of heat compensation device is 40mm, and bottom lengths is 220mm, and the slight indent in inclined-plane is 75 ° with bottom surface angle.In cavity inner surface, inclined-plane adopts high compactness, resistant to elevated temperatures black fiber sheet material, and surfaceness is Ra12.5; The vertical surface contacted with crucible adopts the graphite cake of high strength to make, and surfaceness is Ra1.6; Cavity bottom surface adopts stupalith, surface finish process, surface roughness Ra 0.05.
Ultimate principle of the present invention is as follows:
Get a certain section of sidewall heat compensation device, if inside cavity inclined-plane is face I, vertical surface is face II, and bottom surface is face III, and top firing device surface is face IV.Because cavity is by heater heats, temperature can reach more than 1000K, and inner air is very thin, can think and be similar to vacuum in cavity, meets the law that to conduct heat between grey surface: wherein, for the heat flow density by each surface in cavity, ε ifor each surface heat radiant emittance, σ is Stefan-Boltzmann constant, J ifor each surface launching heat density, T ifor each internal surface temperature, for the angle factor of mutual relationship between surface.
That is:
In cavity, angle, the cavity size relation of inclined-plane I and bottom surface III determine angle factor value, and the material kind of internal surface, surfaceness determine thermal radiation emissivity ε ivalue.Therefore, the inner lining material that properly design cavity geometry is suitable with selection, can make the heat flow density by vertical surface in cavity II value is 0, because vertical surface II and crucible wall fit tightly mutually, therefore, is also 0 by the heat of crucible outer side wall, by this system of equations, can obtains one group of theoretical value:
F ‾ 11 = 0 , F ‾ 12 = 1 2 , F ‾ 13 = 1 3 , F ‾ 14 = 1 6 F ‾ 21 = 1 2 , F ‾ 22 = 0 , F ‾ 23 = 3 10 , F ‾ 24 = 2 10 F ‾ 31 = 5 9 , F ‾ 32 = 1 3 , F ‾ 33 = 0 , F ‾ 34 = 1 9 F ‾ 41 = 5 11 , F ‾ 42 = 4 11 , F ‾ 43 = 2 11 , F ‾ 44 = 0 With ϵ I = 0.92 ϵ II = 0.8 ϵ III = 0.23 ϵ IV = 0.9
Binding isotherm value and engineering reality, inclined-plane I gets 73 ° ~ 78 °, the thermal radiation emissivity ε of inclined-plane I, vertical surface II, bottom surface III correspondence with the angle of bottom surface III iget respectively: 0.9 ~ 0.95,0.75 ~ 0.85,0.2 ~ 0.25.Therefore, crucible wall is just equal to desirable adiabatic condition, and polysilicon defines the thermograde of vertical direction at process of setting, and solidified front can keep level to rise well.
The pyramid structure of the present invention's entirety in flat-top, top cover is made up of the refractory fibrous material of densification; Base material using graphite sheet as heat compensation cavity, its section is upper narrow opening, the gradual change cavity configuration that bottom is wider, cavity configuration is totally in class right-angle triangle, wherein, the inclined-plane of inside cavity can be plane, also can be the curved surface of indent a little.The material of the different thermal radiation emittance of heat compensation cavity liner, as required, can select fiberboard, graphite cake, refractory brick, the differing materials such as pottery; Cavity outer side covers has thermal insulation layer and device case, and thermal insulation layer can adopt refractory brick, refractory fibre or resistant to elevated temperatures porous material, and device case adopts 4 ~ 10mm Plate Steel.Top is provided with heating unit, and heating unit can adopt graphite heating plate, is placed in directly over crucible, and extends to cavity top, higher than cavity open top 3 ~ 10mm, carries out heating and thermal insulation, power adjustable by thermal radiation to silicon liquid surface and inside cavity.Heat compensation inside cavity buries thermopair underground, collecting temperature signal, transfers to temperature controlling system process; Temperature controlling system comprises thermopair, signal collection and analysis equipment, microcomputer, thermosistor etc., can be controlled the output rating of cavity top firing device voluntarily, also can carry out manual intervention control by temperature controlling system.
The present invention is around being arranged on outside directional freeze crucible, and both fit tightly by contact surface; Can installation and removal be facilitated, be conducive to the repacking of conventional apparatus for directional solidification; Silicon liquid slowly pour directional freeze crucible into after can being melted by other equipment, and carries out forced-ventilation heat radiation by the heating panel of crucible bottom, and silicon directional freeze from bottom to top gradually in container, obtains highly purified polysilicon after cooling.

Claims (1)

1. a sidewall heat compensation device for polysilicon directional freezing equipment, is characterized in that being provided with top cover, heating unit, housing, thermal insulation layer, cavity, crucible, heating panel; Described top cover is located at the top of housing, heating unit, cavity and crucible are located in housing, described cavity is axially symmetric structure, cavity be centered around crucible outer side and with crucible close contact, the section of cavity is up-narrow and down-wide gradual change type triangular structure of right angle, the inclined-plane of right-angle triangle is inner sunken face, and the angle on bottom surface and inclined-plane is 73 ° ~ 78 °; Heating unit is located at above crucible, and the edge of heating unit extends to cavity top and higher than cavity hatch 3 ~ 10mm; Described thermal insulation layer be wrapped in outside cavity with bottom, hold silicon liquid in crucible, heating panel to be placed in immediately below crucible and to fit tightly with crucible; The thickness of described thermal insulation layer is 100 ~ 350mm.
CN201310726451.9A 2013-12-25 2013-12-25 A kind of sidewall heat compensation device of polysilicon directional freezing equipment Expired - Fee Related CN103757695B (en)

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CN106378439B (en) * 2016-09-18 2018-11-06 辽宁科技大学 A kind of two-way horizontal directional freeze method and device
CN111850683B (en) * 2020-07-31 2021-12-24 扬州晶樱光电科技有限公司 Heat balance's high-efficient type ingot furnace

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201506708U (en) * 2009-09-29 2010-06-16 常州天合光能有限公司 Thermal field structure for polycrystalline ingot production furnace
CN202030862U (en) * 2011-03-10 2011-11-09 无锡开日能源科技股份有限公司 Three-section type thermal field for polysilicon ingot furnace
CN202390560U (en) * 2011-12-26 2012-08-22 石金精密科技(深圳)有限公司 Large-capacity polysilicon ingot furnace thermal field structure
CN202595325U (en) * 2012-05-09 2012-12-12 熊红兵 Gas guide device used for crystalline silicon ingot furnace

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201506708U (en) * 2009-09-29 2010-06-16 常州天合光能有限公司 Thermal field structure for polycrystalline ingot production furnace
CN202030862U (en) * 2011-03-10 2011-11-09 无锡开日能源科技股份有限公司 Three-section type thermal field for polysilicon ingot furnace
CN202390560U (en) * 2011-12-26 2012-08-22 石金精密科技(深圳)有限公司 Large-capacity polysilicon ingot furnace thermal field structure
CN202595325U (en) * 2012-05-09 2012-12-12 熊红兵 Gas guide device used for crystalline silicon ingot furnace

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