CN107345304B - A kind of preparation method for the silicon electrolytic cell and its silicon preparing HIGH-PURITY SILICON - Google Patents

A kind of preparation method for the silicon electrolytic cell and its silicon preparing HIGH-PURITY SILICON Download PDF

Info

Publication number
CN107345304B
CN107345304B CN201610286747.7A CN201610286747A CN107345304B CN 107345304 B CN107345304 B CN 107345304B CN 201610286747 A CN201610286747 A CN 201610286747A CN 107345304 B CN107345304 B CN 107345304B
Authority
CN
China
Prior art keywords
cathode
silicon
anode
assembly
protective gas
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201610286747.7A
Other languages
Chinese (zh)
Other versions
CN107345304A (en
Inventor
周东方
白斌
刘伟
付松
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shenyang Aluminum and Magnesium Engineering and Research Institute Co Ltd
Original Assignee
Shenyang Aluminum and Magnesium Engineering and Research Institute Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shenyang Aluminum and Magnesium Engineering and Research Institute Co Ltd filed Critical Shenyang Aluminum and Magnesium Engineering and Research Institute Co Ltd
Priority to CN201610286747.7A priority Critical patent/CN107345304B/en
Publication of CN107345304A publication Critical patent/CN107345304A/en
Application granted granted Critical
Publication of CN107345304B publication Critical patent/CN107345304B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00Electrolytic production of inorganic compounds or non-metals
    • C25B1/01Products
    • C25B1/33Silicon
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/02Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B15/00Operating or servicing cells
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B9/00Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
    • C25B9/30Cells comprising movable electrodes, e.g. rotary electrodes; Assemblies of constructional parts thereof

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)

Abstract

The present invention relates to a kind of preparation methods of silicon electrolytic cell and its silicon for preparing HIGH-PURITY SILICON.Three cathode preheating chamber, intermediary operation room and crystalline silicon cooling chamber operating rooms including being located at same level are equipped with folding door between two adjacent operating rooms, and the cell reaction room communicated therewith is equipped with below intermediary operation room.It is equipped with fused electrolyte in electrolytic reaction chamber, anode assembly is equipped in fused electrolyte, anode assembly is used for fixed anode pole piece, and anode pole piece is connect by anode connection with DC power-supply system anode.Track is equipped in the cooling indoor top of cathode preheating chamber, intermediary operation room and crystalline silicon, track is equipped with mobile cathode moving device, cathode moving device is equipped with negative busbar, and negative busbar lower section connects cathode assembly by cathode collector bar, and cathode assembly is used for fixed negative pole pole piece.The present invention has many advantages, such as simple process, easy to operate, mechanization and high degree of automation, environmental protection and energy saving.

Description

A kind of preparation method for the silicon electrolytic cell and its silicon preparing HIGH-PURITY SILICON
Technical field
The present invention relates to a kind of electrolytic cell more particularly to the silicon electrolytic cells and its silicon of a kind of fused salt electrolysis process preparation HIGH-PURITY SILICON Preparation method.
Background technique
Silicon is the most abundant semiconductor element on the earth's crust, is the important source material for preparing semiconductor and advanced composite material (ACM).It is brilliant Body silicon light, in terms of have special physical property, make it in fields such as metallurgy, chemical industry, microelectronics, photovoltaic, solar energy It is widely used, yield and dosage also indicate a national electronics industry development level.Crystalline silicon can be divided by purity For metallurgical grade, solar level and electron level, wherein metallurgical grade silicon is the raw material for producing solar level and electronic-grade silicon, different purity Crystalline silicon have different purposes.Crystalline silicon material is the main material of photovoltaic, solar energy and microelectronic field, occupation rate of market It is 80%~90%, therefore reduces the price of silicon materials in raw material, for promotes the development of related fields that there is biggish promotion Effect.With the rapid development in the fields such as photovoltaic, solar energy and microelectronics, to the crystalline silicon demand of the above purity of solar level Also original bigger.
Currently, industrially the main method of the production above purity crystals silicon of solar level has improved Siemens and silane Method.Improved Siemens production crystalline silicon has many advantages, such as that technical maturity, product purity are high;However there are techniques to answer for this method Miscellaneous, the disadvantages of investment is big, energy consumption is high, seriously polluted, high production cost.Silane thermal decomposition process production crystalline silicon is low with reaction temperature, divides It solves fast speed, high conversion rate, corroded to equipment the advantages that small;However this method there are complex process, high production cost, it is inflammable easily Quick-fried, the disadvantages of safety is poor.All there is certain limitation and determine, constrain in the industrial production preparation method of above two crystalline silicon Crystalline silicon scale and enlargement production, to limit the extensive use of crystalline silicon.
In recent years, in new crystal silicon preparation method, has many advantages, such as simple process, low energy consumption, easy to operate molten Salt electrolysis method obtains the extensive concern of researcher and industry.It is by solid SiO that fused salt electrolysis process, which prepares crystalline silicon,2And metal Cathode is made, graphite does anode, in the molten salt system of chloride or fluoride, in the temperature lower than melting point metal and lower than molten Under conditions of salt decomposition voltage, by electrochemical reaction by SiO2It is reduced into crystalline silicon, and oxygen enters molten salt body in the form of an ion In system, move to the process that graphite anode discharges and generates gas, the crystalline silicon generated in order to prevent and other devices not by Oxidation, whole preparation process needs carry out under protective atmosphere.Currently, fused salt electrolysis process, which prepares crystalline silicon, has been achieved with the stage Journal of Sex Research achievement, but in scale, there are certain difficulty for enlarged popularization practical, be mainly reflected in fused salt atmosphere corrosion, yin There are problems that influencing continuous production in the processes such as the preheating of pole pole piece, crystalline silicon preparation, crystalline silicon cooling.
Summary of the invention
In order to solve the above-mentioned technical problem the present invention provides the standby side of a kind of silicon electrolytic cell for preparing HIGH-PURITY SILICON and its silicon processed Method, it is therefore an objective to realize the processes continuous production processes such as cathode sheet preheating, crystalline silicon preparation, the cooling of finished product crystalline silicon, simultaneously It can prevent corrosion of the fused salt atmosphere to electrolytic cell associated components.
A kind of silicon electrolytic cell preparing HIGH-PURITY SILICON of the invention for the above-mentioned purpose, the cathode including being located at same level preheat Three operating rooms such as room, intermediary operation room and crystalline silicon cooling chamber are equipped with folding door, between two adjacent operating rooms Between the cell reaction room communicated therewith is equipped with below operating room.It is equipped with fused electrolyte in electrolytic reaction chamber, in fusion electrolysis Anode assembly is equipped in matter, anode assembly is used for fixed anode pole piece, and anode pole piece passes through anode connection and DC power-supply system Anode connection.It is equipped with liner in the outside of fused electrolyte, the outside of liner is pot shell.In cathode preheating chamber, intermediary operation room It is equipped with track with the cooling indoor top of crystalline silicon, track is equipped with mobile cathode moving device, sets on cathode moving device There is negative busbar, negative busbar lower section connects cathode assembly by cathode collector bar, and cathode assembly is used for fixed negative pole pole piece.It is intermediate It is equipped with cathode connection above operating room, when production, negative busbar is connected with cathode connection, and cathode connection is born with DC power-supply system Extremely it is connected.
Top seal cover is equipped on the outside of three operating rooms.
At the top of the top seal cover of three operating rooms or side is respectively equipped with connection and operates indoor protective gas exhaust dress It sets, temperature measuring equipment and atmosphere detection device, the lower part of the top seal cover of each operating room are equipped with connection and operate indoor protection Air inlet device.
Preheating device is equipped in the bottom of cathode preheating chamber.
Feeding gate is equipped in cathode preheating chamber side.
The side of crystalline silicon cooling chamber is equipped with discharge door.
The side of intermediary operation room is equipped with fused salt feed inlet and outlet.
Liner is built by graphite material, flame-proof thermal insulation material, heating element and impervious barrier, wherein being built by graphite material Build the slot thorax of cell reaction room;The flame-proof thermal insulation material for the heat preservation of slot thorax is built on the outside of graphite material, in fire resistant heat preserving material Installation heating element is inlayed in material;Below the graphite material of bottom and corner builds the impervious barrier of one layer of resistance to fused salt corrosion.
Pot shell is formed by fashioned iron or steel plate splicing.
Cathode assembly is fixed on negative busbar by cathode collector bar, and level is realized under the driving of cathode moving device It is mobile with vertical direction;Single cathode assembly can load >=1 group of cathode sheet, and cathode sheet is silica-base material.
Anode assembly is fixed on pot shell by the fixation bracket after insulation processing;Sole anode device can load >=1 Group anode pole piece, anode pole piece is graphite material.
A kind of preparation method of HIGH-PURITY SILICON, firstly, good one or more groups of silicon substrate cathodes pole will be loaded in cathode preheating chamber The cathode assembly of piece is installed on negative busbar by cathode collector bar, is then shut off feeding gate, will be negative by cathode moving device Pole device is moved to above preheating device, and starting preheating device preheats silicon substrate cathode sheet.It is reached in silicon substrate cathode sheet It to after preheating temperature, opens cathode and preheats indoor protective gas exhaust apparatus and protective gas inlet duct, in detection atmosphere After meeting the requirements, the folding door between intermediary operation room is opened, during cathode assembly enters under the driving of cathode moving device Between operating room;After cathode assembly is completely into intermediary operation room, close folding door and cathode preheat indoor protective gas into Device of air and protective gas exhaust apparatus.Cathode assembly is sunk in fused electrolyte by being accurately positioned, inserts cathode sheet Enter between two anode pole pieces, form anode-cathode-anode interlaced arrangement, closed two sides folding door, connects cathode Bus and cathode connection enter production status after energization.In process of production, the indoor protective gas exhaust apparatus of intermediary operation It is in the open state always with protective gas inlet duct, to silicon substrate cathode sheet end of reaction, disconnect negative busbar and cathode Wiring promotes cathode assembly by cathode moving device, is moved out fused electrolyte, stands a period of time;Open crystalline silicon The protective gas exhaust apparatus and protective gas inlet duct of cooling chamber, after atmosphere to be detected is met the requirements, open collapsible door will Cathode assembly is moved in crystalline silicon cooling chamber and is cooled down;After cathode assembly is completely into crystalline silicon cooling chamber, folding is closed Folded door.After reaching cooling requirement, cathode assembly is unloaded in crystalline silicon cooling chamber, takes out silicon substrate cathode sheet;Take out silicon substrate After cathode sheet, the protective gas inlet duct and protective gas exhaust apparatus of crystalline silicon cooling chamber are closed.One or more groups of When silicon substrate cathode sheet is cooling, another set or the preheated cathode assembly equipped with silicon substrate cathode sheet of multiple groups enter electrolysis instead Interior is answered to continue to produce.
Advantages of the present invention effect:
Silicon electrolytic cell of the invention is suitable for solid SiO2As raw material, the crystalline substance of high-purity is prepared by fused salt electrolysis process Body silicon;The processes such as silicon electrolytic cell preheats cathode sheet, prepared by crystalline silicon, crystalline silicon is cooling are connected, and avoid cathode pole Piece has bad luck the secondary oxidation cooling with finished product crystalline silicon, improves the purity of crystalline silicon;The slot thorax of cell lining and heat preservation Material, heating element and impervious barrier isolation, avoid corrosion of the fused salt atmosphere to it, and greatly increase electrolytic cell uses the longevity Life;Cathode moving device guarantees continuity of the cathode sheet in preheating, reaction, cooling procedure, improves entire production procedure Automation and Mechanization Level;The not high anode pole piece of replacement frequency is fixed on pot shell by the bracket of anode assembly, Improve the continuity of production;It is filled with protective gas during cathode sheet reaction, cooling etc. simultaneously, can effectively prevent crystalline substance Body silicon secondary oxidation, and reaction gas is discharged by exhaust apparatus and carries out secondary treatment, is polluted small.It can be effective using the present invention Solution fused salt atmosphere corrosion, influence continuous production in the processes such as cathode sheet preheating, crystalline silicon preparation, finished product crystalline silicon be cooling The problem of, there is the application value being produced on a large scale;Also there is simple process, easy to operate, mechanization and automation simultaneously The advantages that degree height, environmental protection and energy saving.
Detailed description of the invention
Fig. 1 is main view of the present invention.
Fig. 2 is the side view of intermediary operation room and cell reaction room of the present invention.
In figure: 1, liner;2, pot shell;3, fused electrolyte;4, top seal cover;5, cathode assembly;6, anode assembly;7, Folding door;8, cathode moving device;9, anode connection;10, negative busbar;11, preheating device;12, fused salt feed inlet and outlet;13, Protective gas inlet duct;14, protective gas exhaust apparatus;15, temperature measuring equipment;16, atmosphere detection device;17, graphite material; 18, flame-proof thermal insulation material;19, heater element;20, impervious barrier;21, cathode sheet;22, anode pole piece;23, cathode preheating chamber; 24, intermediary operation room;25, cell reaction room;26, crystalline silicon cooling chamber;27, track;28, cathode connection;29, cathode collector bar; 30, fixed bracket.
Specific embodiment
Below with reference to embodiment, the invention will be described in further detail, but protection scope of the present invention is not by embodiment institute Limit.
A kind of silicon electrolytic cell for preparing HIGH-PURITY SILICON of the present invention as shown in the figure, the cathode preheating chamber including being located at same level 23,26 3 operating rooms in intermediary operation room 24 and crystalline silicon cooling chamber are equipped with folding door 7 between two adjacent operating rooms, The cell reaction room 25 communicated therewith is equipped with below intermediary operation room 24.Fused electrolyte 3 is equipped in cell reaction room 25, Anode assembly 6 is equipped in fused electrolyte 3, anode assembly 6 is used for fixed anode pole piece 22, and anode pole piece 22 is connect by anode Line 9 is connect with DC power-supply system anode.It is equipped with liner 1 in the outside of fused electrolyte 3, the outside of liner 1 is pot shell 2.? Top in cathode preheating chamber 23, intermediary operation room 24 and crystalline silicon cooling chamber 26 is equipped with track 27, and track 27 is equipped with movement Cathode moving device 8, cathode moving device 8 is equipped with negative busbar 10, and the lower section of negative busbar 10 passes through cathode collector bar 29 Cathode assembly 5 is connected, cathode assembly 5 is used for fixed negative pole pole piece 21.Cathode connection 28, production are equipped with above intermediary operation room 24 When, negative busbar 10 is connected with cathode connection 28, and cathode connection 28 is connected with DC power-supply system cathode.
Top seal cover 4 is equipped on the outside of three operating rooms, 4 top of top seal cover of three operating rooms or side are set respectively There is connection to operate indoor protective gas exhaust apparatus 14, temperature measuring equipment 15 and atmosphere detection device 16, each operating room it is upper The lower part of portion's seal closure 4 is equipped with connection and operates indoor protective gas inlet duct 13.
It is equipped with preheating device 11 in the bottom of cathode preheating chamber 23, is equipped with feeding gate in 23 side of cathode preheating chamber.
The side of crystalline silicon cooling chamber 26 is equipped with discharge door.
The side of intermediary operation room 24 is equipped with fused salt feed inlet and outlet 12.
Liner 1 is built by graphite material 17, flame-proof thermal insulation material 18, heating element 19 and impervious barrier 20, wherein by The slot thorax of the masonry of graphite material 17 cell reaction room 25;The fire resistant heat preserving material for the heat preservation of slot thorax is built on the outside of graphite material 17 Material 18 inlays installation heating element 19 in flame-proof thermal insulation material 18;Below bottom graphite material 17 and corner builds one layer The impervious barrier 20 of resistance to fused salt corrosion.
Pot shell 2 is formed by fashioned iron or steel plate splicing.
Cathode assembly 5 is fixed on negative busbar 10 by cathode collector bar 29, and real under the driving of cathode moving device 8 Now both horizontally and vertically move;Single cathode assembly 5 can load >=1 group of cathode sheet 21, and cathode sheet 21 is silicon substrate Material.
Anode assembly 6 is fixed on pot shell 2 by the fixation bracket 30 after insulation processing;Sole anode device 6 can fill >=1 group of anode pole piece 22 is carried, anode pole piece 22 is graphite material.
A kind of preparation method of HIGH-PURITY SILICON, firstly, good one or more groups of silicon substrate cathodes will be loaded in cathode preheating chamber 23 The cathode assembly 5 of pole piece 21 is installed on negative busbar 10 by cathode collector bar 29, is then shut off feeding gate, is passed through movable cathode Cathode assembly 5 is moved to 11 top of preheating device by device 8, and starting preheating device 11 preheats silicon substrate cathode sheet 21. After silicon substrate cathode sheet 21 reaches preheating temperature, the protective gas exhaust apparatus 14 and protection gas in cathode preheating chamber 23 are opened Body inlet duct 13 opens the folding door 7 between intermediary operation room 24 after detection atmosphere is met the requirements, and cathode assembly 5 exists Enter intermediary operation room 24 under the driving of cathode moving device 8;After cathode assembly 5 is completely into intermediary operation room 24, close Folding door 7 and cathode preheat indoor protective gas inlet duct 13 and protective gas exhaust apparatus 14.It will by being accurately positioned Cathode assembly 5 is sunk in fused electrolyte 3, is inserted into cathode sheet 21 between two anode pole pieces 22, forms anode-yin Pole-anode interlaced arrangement has closed two sides folding door 7, connection negative busbar 10 and cathode connection 28, life is entered after energization Occurrence state.Protective gas exhaust apparatus 14 and protective gas inlet duct 13 during production, in intermediary operation room 24 Always in the open state, to 21 end of reaction of silicon substrate cathode sheet, negative busbar 10 and cathode connection 28 are disconnected, cathode is passed through Mobile device 8 promotes cathode assembly 5, is moved out fused electrolyte 3, stands a period of time;Open crystalline silicon cooling chamber 26 Protective gas exhaust apparatus 14 and protective gas inlet duct 13, after atmosphere to be detected is met the requirements, open collapsible door 7 will be negative Pole device 5 is moved in crystalline silicon cooling chamber 26 and is cooled down;After cathode assembly 5 is completely into crystalline silicon cooling chamber 26, close Close folding door 7.After reaching cooling requirement, cathode assembly 5 is unloaded in crystalline silicon cooling chamber 26, takes out silicon substrate cathode sheet 21;After taking out silicon substrate cathode sheet 21, protective gas inlet duct 13 and the protective gas exhaust of crystalline silicon cooling chamber 26 are closed Device 14.When one or more groups of silicon substrate cathode sheets are cooling, another set or multiple groups it is preheated silicon substrate cathode sheet is housed Cathode assembly enter electrolytic reaction chamber and continue to produce.

Claims (10)

1. a kind of silicon electrolytic cell for preparing HIGH-PURITY SILICON, it is characterised in that be located at cathode preheating chamber, the intermediary operation room of same level With three operating rooms of crystalline silicon cooling chamber, it is equipped with folding door between two adjacent operating rooms, is set below intermediary operation room There is the cell reaction room communicated therewith, is equipped with fused electrolyte in electrolytic reaction chamber, anode is equipped in fused electrolyte and is filled It sets, anode assembly is used for fixed anode pole piece, and anode pole piece is connect with DC power-supply system anode by anode connection, melted The outside of electrolyte is equipped with liner, and the outside of liner is pot shell;In cathode preheating chamber, intermediary operation room and crystalline silicon cooling chamber Top be equipped with track, track is equipped with mobile cathode moving device, and cathode moving device is equipped with negative busbar, and cathode is female Cathode assembly is connected by cathode collector bar below line, cathode assembly is used for fixed negative pole pole piece;Yin is equipped with above intermediary operation room Pole wiring, when production, negative busbar is connected with cathode connection, and cathode connection is connected with DC power-supply system cathode;Three operations Outside is equipped with top seal cover;At the top of the top seal cover of three operating rooms or side is respectively equipped with connection and operates indoor guarantor Gas releaser, temperature measuring equipment and atmosphere detection device are protected, the lower part of the top seal cover of each operating room is equipped with connection behaviour Make indoor protective gas inlet duct.
2. a kind of silicon electrolytic cell for preparing HIGH-PURITY SILICON according to claim 1, it is characterised in that at the bottom of cathode preheating chamber Portion is equipped with preheating device.
3. a kind of silicon electrolytic cell for preparing HIGH-PURITY SILICON according to claim 2, it is characterised in that in cathode preheating chamber side Equipped with feeding gate.
4. a kind of silicon electrolytic cell for preparing HIGH-PURITY SILICON according to claim 1, it is characterised in that the side of crystalline silicon cooling chamber Face is equipped with discharge door.
5. a kind of silicon electrolytic cell for preparing HIGH-PURITY SILICON according to claim 1, it is characterised in that the side of intermediary operation room Equipped with fused salt feed inlet and outlet.
6. a kind of silicon electrolytic cell for preparing HIGH-PURITY SILICON according to claim 1, it is characterised in that liner is by graphite material, resistance to Fiery thermal insulation material, heating element and impervious barrier are built, wherein building the slot thorax of cell reaction room by graphite material;In graphite Outer material side builds the flame-proof thermal insulation material for the heat preservation of slot thorax, and installation heating element is inlayed in flame-proof thermal insulation material;The bottom of at Below portion's graphite material and corner builds the impervious barrier of one layer of resistance to fused salt corrosion.
7. a kind of silicon electrolytic cell for preparing HIGH-PURITY SILICON according to claim 1, it is characterised in that pot shell is by fashioned iron or steel plate It is spliced.
8. a kind of silicon electrolytic cell for preparing HIGH-PURITY SILICON according to claim 1, it is characterised in that cathode assembly passes through cathode Guide rod is fixed on negative busbar, and is realized under the driving of cathode moving device and both horizontally and vertically moved;Single cathode Device loads >=1 group of cathode sheet, and cathode sheet is silica-base material.
9. a kind of silicon electrolytic cell for preparing HIGH-PURITY SILICON according to claim 1, it is characterised in that anode assembly passes through insulation Treated, and fixed bracket is fixed on pot shell;Sole anode device loads >=1 group of anode pole piece, and anode pole piece is graphite material Material.
10. a kind of preparation method of HIGH-PURITY SILICON, it is characterised in that: firstly, will be loaded in cathode preheating chamber good one or more groups of The cathode assembly of silicon substrate cathode sheet is installed on negative busbar by cathode collector bar, is then shut off feeding gate, is moved by cathode Cathode assembly is moved to above preheating device by dynamic device, and starting preheating device preheats silicon substrate cathode sheet;In silicon substrate After cathode sheet reaches preheating temperature, opens cathode and preheats indoor protective gas exhaust apparatus and protective gas inlet duct, After detection atmosphere is met the requirements, the folding door between intermediary operation room, drive of the cathode assembly in cathode moving device are opened It is dynamic lower into intermediary operation room;After cathode assembly is completely into intermediary operation room, closes folding door and cathode preheating is indoor Protective gas inlet duct and protective gas exhaust apparatus;Cathode assembly is sunk in fused electrolyte by being accurately positioned, is made Cathode sheet is inserted between two anode pole pieces, forms anode-cathode-anode interlaced arrangement, has closed two sides folding Door connects negative busbar and cathode connection, and production status is entered after energization;In process of production, the indoor protection of intermediary operation Gas releaser and protective gas inlet duct are in the open state always, to silicon substrate cathode sheet end of reaction, disconnect yin Pole bus and cathode connection promote cathode assembly by cathode moving device, remove fused electrolyte, stand a period of time;It beats The protective gas exhaust apparatus and protective gas inlet duct for opening crystalline silicon cooling chamber after atmosphere to be detected is met the requirements, are opened Cathode assembly is moved in crystalline silicon cooling chamber and cools down by folding door;To cathode assembly completely into crystalline silicon cooling chamber Afterwards, folding door is closed;After reaching cooling requirement, cathode assembly is unloaded in crystalline silicon cooling chamber, takes out silicon substrate cathode sheet; After taking out silicon substrate cathode sheet, the protective gas inlet duct and protective gas exhaust apparatus of crystalline silicon cooling chamber are closed;One When group or multiple groups silicon substrate cathode sheet are cooling, another set or the preheated cathode assembly equipped with silicon substrate cathode sheet of multiple groups into Enter electrolytic reaction chamber to continue to produce.
CN201610286747.7A 2016-05-04 2016-05-04 A kind of preparation method for the silicon electrolytic cell and its silicon preparing HIGH-PURITY SILICON Active CN107345304B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610286747.7A CN107345304B (en) 2016-05-04 2016-05-04 A kind of preparation method for the silicon electrolytic cell and its silicon preparing HIGH-PURITY SILICON

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610286747.7A CN107345304B (en) 2016-05-04 2016-05-04 A kind of preparation method for the silicon electrolytic cell and its silicon preparing HIGH-PURITY SILICON

Publications (2)

Publication Number Publication Date
CN107345304A CN107345304A (en) 2017-11-14
CN107345304B true CN107345304B (en) 2019-07-23

Family

ID=60252933

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610286747.7A Active CN107345304B (en) 2016-05-04 2016-05-04 A kind of preparation method for the silicon electrolytic cell and its silicon preparing HIGH-PURITY SILICON

Country Status (1)

Country Link
CN (1) CN107345304B (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201809445U (en) * 2010-08-06 2011-04-27 昆明理工大学 Molten salt electrolysis device for reducing SiO2 to Si
CN103459675A (en) * 2011-02-04 2013-12-18 金属电解有限公司 Electrolysis method, apparatus and product
CN104733702A (en) * 2013-12-18 2015-06-24 北京有色金属研究总院 Apparatus for preparing nanometer silicon-carbon composite negative material through fused salt electrolysis, and method thereof
CN205099767U (en) * 2015-04-23 2016-03-23 四川航都钛业科技有限公司 Electrolytic cell assembly with extensive rare refractory metal of continuous production

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8388914B2 (en) * 2010-12-23 2013-03-05 Memc Electronic Materials, Inc. Systems for producing silane

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201809445U (en) * 2010-08-06 2011-04-27 昆明理工大学 Molten salt electrolysis device for reducing SiO2 to Si
CN103459675A (en) * 2011-02-04 2013-12-18 金属电解有限公司 Electrolysis method, apparatus and product
CN104733702A (en) * 2013-12-18 2015-06-24 北京有色金属研究总院 Apparatus for preparing nanometer silicon-carbon composite negative material through fused salt electrolysis, and method thereof
CN205099767U (en) * 2015-04-23 2016-03-23 四川航都钛业科技有限公司 Electrolytic cell assembly with extensive rare refractory metal of continuous production

Also Published As

Publication number Publication date
CN107345304A (en) 2017-11-14

Similar Documents

Publication Publication Date Title
CN103334126B (en) A kind of method adopting fused salt electrolysis process to prepare titanium sponge in resistance furnace
CN102534663B (en) The device of generating metal magnesium by electrolyzing magnesium chloride
CN101760759B (en) Method for preparing metal lithium by electrolyzing molten salt
CN104947152A (en) Method for preparing high-purity titanium by fused-salt electrolytic refining
CN105088274B (en) A kind of device for processing and reclaiming aluminium electroloysis solid waste
US6287448B1 (en) Electrochemical production of lithium using a lithium amalgam anode
WO2017031798A1 (en) Apparatus for treating and recycling aluminum electrolysis solid waste
CN104711638B (en) Method for extracting indium and tin from waste ITO targets through reduction and electrolysis
JP7428411B2 (en) Systems and methods for molten oxide electrolysis
CN103014775A (en) Method and device for producing titanium by fused salt electrolysis process
CN103484898B (en) A kind of vacuum high-temperature continuous electrolysis furnace system and electrolysis process
CN104313643A (en) High-purity antimony producing method by two-section fused salt electrolysis method
CN114908380A (en) One-key type automatic continuous quantitative discharging system
CN104711426B (en) A kind of useless methods of the target through reducing electroextraction indium tin of ITO
CN106894052B (en) A kind of conjuncted-multilevel aluminum electrolysis unit and its application method preparing rafifinal
CN107345304B (en) A kind of preparation method for the silicon electrolytic cell and its silicon preparing HIGH-PURITY SILICON
CN206580891U (en) A kind of fused salt electrolysis apparatus
CN104711637B (en) Method for recovering metal lead from solid lead oxide
CN207362344U (en) A kind of electrolytic cell with anode covering and heat insulating device
CN202450165U (en) Device for producing metal magnesium through electrolytic magnesium chloride
CN103728054B (en) Method for calculating heat loss of large direct-current closed electric furnace for smelting high-titanium slag
CN101962786B (en) Control method for blowing-free heat dissipating window after starting large aluminum electrolysis cell
CN207362343U (en) New refined aluminum process units
CN108048872B (en) Electrolytic purification system for preparing high-purity metallic sodium
CN206109553U (en) A temperature control electrolysis trough for in chemical industry field

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant