CN102976331A - Silane-decomposition-method polysilicon preparation device - Google Patents
Silane-decomposition-method polysilicon preparation device Download PDFInfo
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- CN102976331A CN102976331A CN2011102615702A CN201110261570A CN102976331A CN 102976331 A CN102976331 A CN 102976331A CN 2011102615702 A CN2011102615702 A CN 2011102615702A CN 201110261570 A CN201110261570 A CN 201110261570A CN 102976331 A CN102976331 A CN 102976331A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
Abstract
The invention relates to a polysilicon preparation device, and specifically relates to a device for preparing polysilicon through a silane thermal decomposition reaction. Aiming at overcoming defects of silane-method polysilicon preparation, the invention provides a silane-decomposition-method polysilicon preparation device with high safety coefficient and production capacity. The device provided by the invention comprises a main reaction chamber, a gas source unit, a controlling unit, a power supply unit, a suppressing unit, and a vacuum unit. The gas source unit, the controlling unit, the power supply unit, the suppressing unit, and the vacuum unit are connected with the main reaction chamber. The gas source unit is connected with a storage tank. With the structure, a dangerous chemical reaction of silane decomposition can be carried out stably, a controlling effect is good, and safety and high efficiency of the entire production process are improved. Through a Kingview interface, operators are provided with a detailed understanding of the operation condition of the thermal decomposition furnace. Therefore, accident rate is reduced, and purposes of high safety, high efficiency, energy saving, and consumption reducing of the system are achieved.
Description
Technical field
The present invention relates to a kind of equipment for preparing polycrystalline silicon, specifically, relate to a kind of pyrolysis of silane that utilizes and produce equipment for preparing polycrystalline silicon.
Background technology
Polysilicon is the starting material of preparation silicon single crystal and solar cell, is the foundation stone of global electronic industry and photovoltaic industry.Along with the fast development of photovoltaic industry, solar cell increases rapidly the demand of polysilicon.
Existing production of polysilicon Technology mainly contains: improved Siemens, metallurgy method, silane thermal decomposition process.
Improved Siemens: most domestic producer adopts improved Siemens to produce the industry that polysilicon (being the trichlorosilane method) belongs to high energy consumption.In trichlorosilane method production process, can discharge the tail gas such as silicon tetrachloride, hydrogenchloride.Silicon tetrachloride particularly, if do not process, will serious environment pollution.The insider introduces, and domestic most producer whenever produces 1 ton of polysilicon now, will produce 12 tons of silicon tetrachlorides.Wherein power cost accounts for about 70% of total cost, has simultaneously the shortcomings such as technical process is long, investment is large, the technological operation difficulty is large.
Metallurgy method: the main technique of metallurgy method is: (1) select purity preferably industrial silicon carry out the horizontal zone melting unidirectional solidification and become silicon ingot; (2) remove part and the outer matrix section that metallic impurity are assembled in the silicon ingot; (3) carry out coarse reduction and cleaning; (4) melt at plasma body and remove boron impurity in the stove, carry out again horizontal zone melting second time unidirectional solidification and become silicon ingot, (5) remove metallic impurity are assembled in the zone melting and refining silicon ingot for the second time part and outer matrix section (6) through coarse reduction with clean after, melt in the stove except dephosphorization and carbon impurity at electron beam, directly generate solar-grade polysilicon.To existing at least 25 years of metallurgy method research, still can't really provide up-to-standard silicon materials for photovoltaic industry so far abroad.Therefore, it is not accessible in the recent period attempting to produce the polysilicon that satisfies the solar cell specification of quality with metallurgical method of refining.
Silane thermal decomposition process: namely utilize the pyrolysis high purity silicon of silane (SiH4), new silane thermal decomposition process developed comparatively fast in recent years, and the incomparable advantage of many improved Siemens is arranged really.
Mainly utilize at present silane (SiH4) pyrolysis high-purity silicon, high-risk explosive in silane (SiH4) the thermolysis polysilicon production process processed, the equipment for preparing polycrystalline silicon by using silane decomposition method safety coefficient is required high, but at present equipment for preparing polycrystalline silicon by using silane decomposition method ubiquity poor stability, problem that production capacity is low.
Summary of the invention
The present invention overcomes silane thermal decomposition process to prepare the defective that polysilicon exists, and the equipment for preparing polycrystalline silicon by using silane decomposition method that a kind of safety coefficient is high, production capacity is high is provided.
The technical scheme of equipment for preparing polycrystalline silicon by using silane decomposition method of the present invention is such: it comprises main reaction chamber, gas source unit, control unit, power subsystem, suppresses unit, vacuum unit, gas source unit, control unit, power subsystem, suppress the unit, vacuum unit all is connected with main reaction chamber, gas source unit is connected with hold-up vessel.
The layering of described each unit arranges, and is divided into two-layerly, and main reaction chamber is arranged on the second layer, vacuum unit, gas source unit, suppresses unit, power subsystem the first layer all is set.
Described main reaction chamber comprises the furnace wall, and burner hearth is set in the furnace wall, and inlet pipe, electrode, silicon core, internal cooling pipe are set in the burner hearth, inlet pipe is arranged on the central authorities of burner hearth, electrode, internal cooling pipe and silicon core are around the inlet pipe setting, and the furnace wall is provided with interlayer, and cooling duct is set in the interlayer.
Described main reaction chamber arranges bell, and overflow device is set on the bell.
Described main reaction chamber arranges hoisting appliance outward.
Described gas source unit comprises silane storage tank, housing, the polycarbosilane hydroxide air separation, pressurizing device after the silane Hydrogen Separation, hydrogen storage tank, the polycarbosilane hydroxide device of air is connected with main reaction chamber, the polycarbosilane hydroxide air separation connects two shunt, pressurizing device after the one route silane Hydrogen Separation, the hydrogen storage tank forms, pressurizing device after the silane Hydrogen Separation, be connected with hydrogen gas recovering device with the source of the gas cabinet respectively after the series connection of hydrogen storage tank, pressurizing device after another route silane Hydrogen Separation, the silane storage tank, pressurizing device after the silane Hydrogen Separation, be connected with housing after the series connection of silane storage tank.
Described control unit is set to the central controlled PLC control unit by CPU.
The present invention has guaranteed that silane decomposes this hazardous chemical stable reaction operation owing to adopt said structure, controls respond wellly, has improved security and the high efficiency of whole Production Flow Chart.Operator are by the KingView interface, and careful understanding thermal decomposition furnace running situation reduces accident rate, has finally realized efficient, the energy-saving and cost-reducing target of security of system.
Description of drawings
Fig. 1 is schematic diagram of the present invention.
Fig. 2 is layout drawing of the present invention.
Fig. 3 is the structural representation of main reaction chamber of the present invention.
Fig. 4 is the structural representation of viewing window of the present invention.
The 1-main reaction chamber, the 2-gas source unit, the 3-control unit, the 4-power subsystem, 5-suppresses the unit, the 6-vacuum unit, 7-boosting unit, the 9-transformer, 10-high pressure connector element, the 11-furnace wall, the 12-burner hearth, the 13-tracheae, the 14-electrode, 15-silicon core, 16-internal cooling pipe, 17-furnace wall cooling tube, the 18-base plate, the double-deck viewing window of 19-, the 20-pipe that blows side, the 21-expansion joint, the 22-silane storage tank, 23-polycarbosilane hydroxide air separation, pressurizing device after the 24-silane Hydrogen Separation, 25-hydrogen storage tank, the 26-hydrogen gas recovering device.
Embodiment
As shown in Figure 1, equipment for preparing polycrystalline silicon by using silane decomposition method of the present invention mainly by CVD main reaction chamber 1, gas source unit, control unit 3, power subsystem 4, suppress unit 5, vacuum unit 6, boosting unit 7 and form, gas source unit 2, control unit 3, power subsystem 4, suppress unit 5, vacuum unit 6, boosting unit 7 and all is connected connection with the CVD main reaction chamber, gas source unit 2 is connected with hold-up vessel.As shown in Figure 2, the present invention divides two-layer setting, CVD main reaction chamber 1 is arranged on the second layer, gas source unit 2, power subsystem 4, suppress unit 5, vacuum unit 6, transformer 9, high pressure connector element 10 and all be arranged on the first layer, wherein power subsystem 4 gives the CVD main reaction chamber 1 power supply by high pressure connector element 10 after transformer 9 voltages of transformation.
Shown in Figure 3, CVD main reaction chamber 1 mainly contains furnace wall 11, is arranged on burner hearth 12, inlet pipe 13, electrode 14, silicon core 15, internal cooling pipe 16, furnace wall cooling tube 17, base plate 18 compositions in the furnace wall, described inlet pipe 13, electrode 14, silicon core 15, internal cooling pipe 16 are arranged in the burner hearth 12, inlet pipe 13 is arranged on the central authorities of burner hearth 12, electrode 14, internal cooling pipe 16 and silicon core 15 arrange around inlet pipe 13, and furnace wall 11, inlet pipe 13, internal cooling pipeline 16 and electrode 14 all are fixedly connected on the base plate 18.Electrode 14 links to each other with silicon core 15, and the electric current of electrode 14 flows through the effect that silicon core 15 plays heating, and electrode 14 adopts the mode of direct insertion electrode, and is easy to operate reliable and stable.In a reaction chamber, 12 pairs of silicon plugs can be set, be used for the growth of polysilicon, the feed rate that control unit 3 meetings are regulated silane and hydrogen automatically according to production of polysilicon speed.Furnace wall cooling tube 17 is fixedly mounted on the top of furnace wall 11.Furnace wall 11 is bilayer structure, and internal layer is the 316L stainless steel, and joint flange is the 316L stainless steel, and the body of heater shell is structural carbon steel, and spray treatment is carried out on the surface, and upper of furnace body is standard butterfly end socket.Described CVD main reaction chamber 1 adopts the mode of oil cooling, can flow according to fixing direction for making oil, between the internal layer of furnace wall 11, skin cooling duct 16 is set, and guarantees cooling performance.Cause industrial accident for preventing that the oil cooling system from breaking down, be provided with the oil spill device at the bell of CVD main reaction chamber.
As shown in Figure 4, at the body of heater of CVD main reaction chamber double-deck viewing window 19 is set, its adopting quartz glass is made, and is used for polycrystalline silicon growth situation in the observation stove.Adopt double-deck viewing window 19 can prevent that the glass breakage silane of inner layer glass window from overflowing, and blasts.Described inner layer glass window is connected (such as Fig. 4) with side-blown pipe 20, and hydrogen purges the inner layer glass window glass by side-blown pipe 20, and it is on glass to prevent that silica flour is bonded at.For preventing that slight crack from appearring in the cooling of frequently being heated of double-deck viewing window 19 and body of heater weld, at the forms of double-deck viewing window 19 expansion joint 21 is set.
The described CVD main reaction chamber 1 outer hoisting appliance that arranges arranges the hoisting appliance main purpose and is the cleaning for feeding and reaction chamber.After polycrystalline silicon growth is finished, after namely a technological process finishes, take the polycrystalline silicon rod that generates away, in order to carry out the technical process of next round.Be provided with pressure assembly in the CVD main reaction chamber 1, be automated closed-loop control, control accuracy is high, and speed of response is fast.
Gas source unit as shown in Figure 1 comprises silane storage tank 22, source of the gas cabinet 2, polycarbosilane hydroxide air separation 23, pressurizing device 24 after the silane Hydrogen Separation, hydrogen storage tank 25, polycarbosilane hydroxide air separation 23 is connected connection with the CVD main reaction chamber, polycarbosilane hydroxide air separation 23 connects two shunt, pressurizing device 24 after the one route silane Hydrogen Separation, hydrogen storage tank 25 forms, pressurizing device 24 after the silane Hydrogen Separation, are connected with the source of the gas cabinet respectively after hydrogen storage tank 25 series connection and are connected connection with hydrogen gas recovering device, pressurizing device 24 after another route silane Hydrogen Separation, silane storage tank 22, pressurizing device 24 after the silane Hydrogen Separation, are connected connection after silane storage tank 22 series connection with the source of the gas cabinet.
Boosting unit 7 as shown in Figure 1 is comprised of heating system for oil, oil circulating system.Its main purpose makes the silicon core in the main reaction chamber reach the high temperature that punctures, and requires simultaneously oil groove to have refrigerating function, avoids temperature to raise always, causes the polycrystalline furnace sealing-ring aging, causes gas leakage, causes danger.
As shown in Figure 1, the design consideration U/I curve of power subsystem 4 power-supply systems designs, and minute a plurality of transformer transformation points can heat the polycrystalline silicon rod of different rugosity, heat reliable and stable.Suppress the high pressure that needs when unit 5 mainly provides silicon core 15 to puncture, high voltage intensity reaches 10kV.It is comprised of vacuum unit 6 import dry type lobe pump unit and related valve, is filled with nitrogen again in stove after vacuumizing, and vacuumizes again, carries out technique.The air that act as remnants in the dilution chamber of inflated with nitrogen, the purity of the polysilicon that assurance is produced, this step can according to circumstances be carried out the setting of number of times.
Principle of work: the used principle of this equipment is silane decomposition, namely utilizes the pyrolysis high purity silicon of silicomethane (SiH4), and chemical reaction is as follows:
This reaction is carried out in CVD main reaction chamber 1 as shown in Figure 3, and silane at high temperature decomposes, and the polysilicon of generation constantly is deposited on the silicon wicking surface, and the silicon core is with gradually chap.By polycrystalline silicon growth situation in the double-deck viewing window 19 observation stoves on the body of heater, when polycrystalline silicon growth is finished, in time take the polysilicon of generation away by being arranged on CVD main reaction chamber 1 outer upgrading mechanism, getting rid of tail gas by tail gas treating unit after to polycrystalline silicon growth processes, mainly be to generating the recovery of H2, and to the decomposition of remaining SiH4.The vacuum unit 6 of equipment provides high-purity gas reaction environment for reaction, power subsystem 4, boosting unit 7, suppresses unit 5, gas source unit 2 and control unit 3 and is used for decomposing temperature and the sufficient source of the gas amount provide suitable for silane.
Equipment for preparing polycrystalline silicon by using silane decomposition method of the present invention has guaranteed that silane decomposes the operation of this hazardous chemical stable reaction, controls respond wellly, has improved security and the high efficiency of whole Production Flow Chart.Operator are by the touch-screen-enabled interface, and careful understanding thermal decomposition furnace running situation reduces accident rate, has finally realized efficient, the energy-saving and cost-reducing target of security of system.
Claims (7)
1. equipment for preparing polycrystalline silicon by using silane decomposition method, it is characterized in that, it comprises main reaction chamber, gas source unit, control unit, power subsystem, suppresses unit, vacuum unit, gas source unit, control unit, power subsystem, suppress the unit, vacuum unit all is connected with main reaction chamber, gas source unit is connected with hold-up vessel.
2. equipment for preparing polycrystalline silicon by using silane decomposition method according to claim 1, it is characterized in that, main reaction chamber comprises the furnace wall, burner hearth is set in the furnace wall, inlet pipe, electrode, silicon core, internal cooling pipe are set in the burner hearth, and inlet pipe is arranged on the central authorities of burner hearth, and electrode, internal cooling pipe and silicon core are around the inlet pipe setting, the furnace wall is provided with interlayer, and cooling duct is set in the interlayer.
3. equipment for preparing polycrystalline silicon by using silane decomposition method according to claim 2 is characterized in that, main reaction chamber arranges bell, and overflow device is set on the bell.
4. equipment for preparing polycrystalline silicon by using silane decomposition method according to claim 1, it is characterized in that, gas source unit comprises silane storage tank, housing, the polycarbosilane hydroxide air separation, pressurizing device after the silane Hydrogen Separation, hydrogen storage tank, the polycarbosilane hydroxide device of air is connected with main reaction chamber, the polycarbosilane hydroxide air separation connects two shunt, pressurizing device after the one route silane Hydrogen Separation, the hydrogen storage tank forms, pressurizing device after the silane Hydrogen Separation, be connected with hydrogen gas recovering device with housing respectively after the series connection of hydrogen storage tank, pressurizing device after another route silane Hydrogen Separation, the silane storage tank, pressurizing device after the silane Hydrogen Separation, be connected with housing after the series connection of silane storage tank.
5. equipment for preparing polycrystalline silicon by using silane decomposition method according to claim 1 is characterized in that, control unit is set to the central controlled PLC control unit by CPU.
6. equipment for preparing polycrystalline silicon by using silane decomposition method according to claim 1 is characterized in that, main reaction chamber arranges hoisting appliance outward.
7. equipment for preparing polycrystalline silicon by using silane decomposition method according to claim 1, it is characterized in that each unit layering of this setting arranges, and is divided into two-layer, main reaction chamber is arranged on the second layer, vacuum unit, gas source unit, suppresses unit, power subsystem the first layer all is set.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011102615702A CN102976331A (en) | 2011-09-06 | 2011-09-06 | Silane-decomposition-method polysilicon preparation device |
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| CN2011102615702A CN102976331A (en) | 2011-09-06 | 2011-09-06 | Silane-decomposition-method polysilicon preparation device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112575372A (en) * | 2020-12-05 | 2021-03-30 | 王力群 | Laminated external expanding type silicon rod forming equipment |
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| CN101959794A (en) * | 2008-03-04 | 2011-01-26 | 乔治洛德方法研究和开发液化空气有限公司 | Method for recycling silane (SiH4) |
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| CN112575372A (en) * | 2020-12-05 | 2021-03-30 | 王力群 | Laminated external expanding type silicon rod forming equipment |
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Application publication date: 20130320 |