CN106608629A - Method and device for preparing high-purity silicon monoxide by medium-frequency induction heating way - Google Patents
Method and device for preparing high-purity silicon monoxide by medium-frequency induction heating way Download PDFInfo
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- CN106608629A CN106608629A CN201611195184.7A CN201611195184A CN106608629A CN 106608629 A CN106608629 A CN 106608629A CN 201611195184 A CN201611195184 A CN 201611195184A CN 106608629 A CN106608629 A CN 106608629A
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- induction heating
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 59
- 230000006698 induction Effects 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 16
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 title abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000010703 silicon Substances 0.000 claims abstract description 32
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 30
- 239000002994 raw material Substances 0.000 claims abstract description 24
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 21
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 15
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 76
- 229910002804 graphite Inorganic materials 0.000 claims description 54
- 239000010439 graphite Substances 0.000 claims description 54
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 24
- 230000004888 barrier function Effects 0.000 claims description 22
- 229910052799 carbon Inorganic materials 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 22
- 238000009413 insulation Methods 0.000 claims description 8
- 238000009792 diffusion process Methods 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 238000009434 installation Methods 0.000 claims description 3
- 230000033228 biological regulation Effects 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims description 2
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 14
- 230000003647 oxidation Effects 0.000 description 13
- 238000007254 oxidation reaction Methods 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 10
- 238000005265 energy consumption Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 230000033001 locomotion Effects 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 239000005304 optical glass Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 230000003685 thermal hair damage Effects 0.000 description 2
- 238000002061 vacuum sublimation Methods 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 229910052571 earthenware Inorganic materials 0.000 description 1
- 210000003746 feather Anatomy 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000005092 sublimation method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000005439 thermosphere Substances 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- -1 vacuum furnace shell Chemical compound 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/03—Pressure vessels, or vacuum vessels, having closure members or seals specially adapted therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00132—Controlling the temperature using electric heating or cooling elements
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to the technical field of preparation of high-purity silicon monoxide, in particular, relates to a method and device for preparing high-purity silicon monoxide by a medium-frequency induction heating way, and is characterized in that the preparation method comprises the following steps: 1, preparing raw materials: mixing high-purity silicon with the content of more than 99.5 wt% and silicon dioxide with the content of more than 99.5 wt% according to the weight ratio of 1:1; 2, carrying out medium-frequency induction heating; and 3, cooling to obtain the finished product; when the medium-frequency induction heating temperature is 1200-1600 DEG C, the molar ratio of the raw materials of high-purity silicon and silicon dioxide is adjusted, and the value of x in the product SiOx is a fixed value; but when the medium-frequency induction heating temperature is more than or equal to 1600 DEG C, the value of the molar ratio of the raw materials of high-purity silicon and silicon dioxide is controlled to be 0.88-1.2, and the value of x in the product SiOx is adjustable in a range of 0.89-1.10. Compared with the prior art, the method and the device have the advantages of high heating efficiency and stable equipment; products with different silicon-oxygen ratios are obtained by adjustment of the heating temperature and the ratio of the raw materials.
Description
Technical field
The present invention relates to the preparing technical field of high pure zirconia Asia silicon, specifically Frequency Induction Heating mode prepares height
The method and apparatus of pure zirconia Asia silicon.
Background technology
The sub- silicon powder of oxidation is active because being rich in, can be used as the fine ceramics such as synthesis material such as silicon nitride, carborundum；True
Evaporated in the air, be coated on the metallic reflection minute surface of optical instrument, can be used as optical glass and semi-conducting material；Oxidation is sub-
Silicon can be additionally used in the excellent lithium ion battery negative material of processability.
The preparation principle of the sub- silicon of oxidation is Si+SiO2Silica flour and silicon dioxide are pressed 1: 1 mixed in molar ratio, true by → SiO
Product is obtained after heating under empty condition.This reaction is reversible reaction, if further reducing pressure, improves temperature, and balance is then
To the sub- silicon side shifting of oxidation.
The sub- silicon manufacturing apparatus of oxidation of early stage are made up of the aluminium oxide ceramics refractory tube of vacuum-pumping, will be mixed during work
SiO2It is placed in Si under one end of seal pipe, vacuum state and is heated to material gasification, is subsequently deposited upon the refractory tube other end.But
This device has low production efficiency, reaction tube and is easy to the shortcomings of rupturing.
Through improving, it is burner hearth that structure is changed to aluminium oxide inner tube to recent process units, is wound with muffle electric furnace silk, oxygen outside which
It is insulation jacket layer to change the outer tube outside of aluminum, and aluminium oxide inner tube, outer tube and the insulation jacket layer being set in together together is placed in
The seamless steel pipe inside the shell that axis horizontal is arranged, one end closing of aluminium oxide inner tube, the other end are fitted with the circle of one end closing
Catcher, the front end that the catcher of seamless steel pipe shell is located pass through end cap seal, and rear end is connected with the equipment of evacuation.
The utility model patent of Publication No. CN2451567Y, discloses a kind of new oxidation Asia silicon manufacturing apparatus, its
It is burner hearth by high-alumina inner tube, outside which, is wound with muffle electric furnace silk, the outer tube outside of high-alumina is insulation jacket layer, and pipe is outer logical
Circulating water, due to being still that resistance-type is heated, caliber is limited by thermograde, and the material yield and equipment energy consumption of preparation are not
Possesses economy.
Above-mentioned existing equipment improves yield to a certain extent, but as molybdenum filament is selected in heating, it is true through high temperature
Extremely brittle after empty-cooling, body of heater is easily damaged；In order to ensure being heated evenly property of the material in heating process and the safety of equipment
Property, per batch preparing feather weight, yield can not still meet needs of the market to such material to resistance-heated furnace；X values in SiOx
Difference directly determine the performance of material, this is huge for downstream application meaning, but existing equipment all effectively can not be adjusted
Control, therefore, current technology remains a need for further being lifted.
The content of the invention
The purpose of the present invention is to overcome the deficiencies in the prior art, production oxidation is heated using Frequency Induction Heating mode sub-
Silicon, to reduce equipment energy consumption and loss, and improves the purity for preparing the sub- silicon of oxidation；Can be set by improving Frequency Induction Heating in addition
It is standby improving the collection rate and yield of product.
Above-mentioned purpose is realized, a kind of method that Frequency Induction Heating mode prepares high pure zirconia Asia silicon is designed, its feature exists
In using following preparation method：
1st, raw material prepares：Content ＞ 99.5wt% HIGH-PURITY SILICONs, content ＞ 99.5wt% silicon dioxide are mixed by weight 1: 1
Close, be dehydrated Jing after tablet machine is pressed into pie；
2nd, Frequency Induction Heating：Pie mixed material is put in the graphite crucible of Intermediate Frequency Induction Heating Equipment, in vacuum
Under the conditions of be heated to 1200～2000 DEG C, 3～5h of constant temperature makes raw material be reacted and gradually be distilled；
3rd, cool down to obtain finished product：After constant temperature terminates 8～10h, material is cooled to room temperature, by the receipts in Intermediate Frequency Induction Heating Equipment
Storage is opened, and takes out high pure zirconia Asia silicon SiO of the absorption in inner collector wallxFinished product；
When intermediate frequency induction heating temperature is at 1200～1600 DEG C, the mol ratio of raw material HIGH-PURITY SILICON and silicon dioxide is adjusted
When, in product SiOx, x values are fixed value；
And when intermediate frequency induction heating temperature >=1600 DEG C, control the ratio of raw material HIGH-PURITY SILICON and the mol ratio of silicon dioxide
At 0.88～1.2, in product SiOx, the value of x is adjustable in the range of 0.89～1.10.
A kind of Intermediate Frequency Induction Heating Equipment for preparing high pure zirconia Asia silicon, including vacuum furnace shell, induction coil, thermal insulation separation
Thermosphere, graphite crucible, catcher, bell, water-cooling system, intermediate frequency power supply, intermediate frequency feeder equipment, pumped vacuum systems, temp measuring system,
It is characterized in that：The central axis of described vacuum furnace shell is 1～10 ° with the angle on the installation ground of vacuum furnace shell；Position
Carbon barrier is provided with least open end side of the graphite crucible of the central axis bottom of graphite crucible；In the opening of graphite crucible
It is covered with catcher on the end face at end, described catcher is in round platform tubular, and opens with the catcher of graphite crucible junction
The diameter of the tail end with diameter greater than catcher at mouth end.
The end face of the tail end of described catcher is provided with hole, and the radius in hole is 2～5cm；Detachable connection one on hole
The blind patch of covering openings.
The end face of the opening of described catcher is provided with the flange being connected with graphite crucible.
Described carbon barrier is located at the nearly opening of the lower half inwall of graphite crucible；Or described carbon barrier
It is located in X axis at the nearly opening of the lower half inwall for being respectively provided at graphite crucible and on the lower half inwall of graphite crucible
At portion.
The height of the carbon barrier at the opening of described graphite crucible for graphite crucible internal diameter 1/2 or 1/3 or 1/
4；Height on the lower half inwall of graphite crucible positioned at the carbon barrier of the center of X axis is the 1/5 of graphite crucible internal diameter.
Described bell is flexibly connected a bell go-cart；
Described bell go-cart includes that a bottom is provided with the flat board of pulley, and one end of flat board is rotatably connected the bottom of a primary push rod
End, the top of primary push rod are provided with mounting hole along the length direction of primary push rod, and one end of a pin is slidably connected in mounting hole, pin
The other end of post be rotatably connected bell lateral wall middle and upper part；The other end of flat board is rotatably connected the bottom of a driven push rod,
Another mounting hole is set along the length direction of driven push rod on the top of dynamic push rod, one end of another pin is slidably connected at another waist
In shape hole, the other end of another pin be rotatably connected bell lateral wall the nearly vacuum furnace shell side in bottom；
The bottom of described bell go-cart is provided with track.
Described pumped vacuum systems be sequentially connected using pipeline mechanical pump, lobe pump, diffusion pump；Described diffusion pump
Entrance point connect vacuum furnace shell air vent.
The power-supply controller of electric of described intermediate frequency power supply is controlled using uncontrollable rectifier circuit, described power-supply controller of electric output
Constant current and invariable power, the power work frequency for controlling of described power-supply controller of electric is 2000～2800Hz；Described power supply
Controller is by telecommunication come the parameter in read-write controller and control running status.
Described temp measuring system connects PID temp controlled meters respectively using two outfans of thermometric galvanic couple and is constituted, thermometric electricity
Two even side warm spots are respectively provided at middle part and the opening of graphite crucible；Described thermometric galvanic couple adopts W-Re thermocouple.
The present invention compared with prior art, prepares the sub- silicon of oxidation using Frequency Induction Heating mode, makes equipment continuous-stable：
Induction heating avoid using power it is high, energy consumption is big, easy cause thermal damage electric furnace heating wire, generated heat by the eddy current effect of graphite crucible,
The efficiency of heating surface is high, and equipment is stable, and maintenance cost is low；
Sensing heating sublimed method is pollution-free in addition：Vacuum sublimation is a physically separate method, does not carry out chemical reaction, whole
During individual separating-purifying, no waste mine, waste gas are produced, environmentally safe；
The oxidation Asia silicon purity prepared simultaneously is high, can reach more than 99.9%；
In addition, shape design of the Intermediate Frequency Induction Heating Equipment using the body of heater, increase carbon barrier, catcher being in tilted layout
The yield height of product is made, compared with traditional resistor stove, yield is greatly increased, and energy consumption of unit product is low；
In addition, product specification controllable can be made：Heating-up temperature and the adjustment of the proportioning raw materials different silica of acquisition can be passed through
Compare product.
Description of the drawings
Fig. 1 is the SiOx sample XRD spectrums that gained is prepared using the inventive method.
Fig. 2 is the structural representation of Intermediate Frequency Induction Heating Equipment in the present invention.
Fig. 3 is the enlarged drawing at graphite crucible in Fig. 2.
Structural representations of the Fig. 4 for cylindrical collection device.
Structural representations of the Fig. 5 for slot ampuliform catcher.
Fig. 6 is the structural representation of round platform shaped collector in the embodiment of the present invention.
Fig. 7 be the embodiment of the present invention in be provided with flange round platform shaped collector structural representation.
Fig. 8 is the structural representation of the round platform shaped collector that connection end is slot.
Specific embodiment
The present invention is further described in conjunction with accompanying drawing.
Embodiment 1
A kind of method that Frequency Induction Heating mode prepares high pure zirconia Asia silicon, it is characterised in that using following preparation side
Method：
1st, raw material prepares：Content ＞ 99.5wt% HIGH-PURITY SILICONs, content ＞ 99.5wt% silicon dioxide are mixed by weight 1: 1
Close, be dehydrated Jing after tablet machine is pressed into pie；
2nd, Frequency Induction Heating：Pie mixed material is put in the graphite crucible of Intermediate Frequency Induction Heating Equipment, in vacuum
Under the conditions of be heated to 1200～2000 DEG C, 3～5h of constant temperature makes raw material be reacted and gradually be distilled；Wherein Frequency Induction Heating
Catcher in equipment is introduced into sublimation gases in the cavity of catcher；
3rd, cool down to obtain finished product：After constant temperature terminates 8～10h, material is cooled to room temperature, by the receipts in Intermediate Frequency Induction Heating Equipment
Storage is opened, and takes out high pure zirconia Asia silicon SiO of the absorption in inner collector wallxFinished product.Its principle is, when gas settling, cold
But the composite construction SiO of nano Si is uniformly distributed in gradually forming Si-O structures afterwardsx, wherein after the sub- silicon of oxidation is sublimed into steam
Contact with 12 inwall of catcher, temperature drop is condensed into solid, and the impurity in its raw material, such as boron, due to not possessing distillation
Characteristic can not become steam and remain in graphite crucible 10, both natural separation.Referring to Fig. 1, it can be seen that sample is in nothing
Stabilized condition.
The SiO prepared in the present inventionxIn, when intermediate frequency induction heating temperature is at 1200～1600 DEG C, raw material HIGH-PURITY SILICON with
During the mol ratio of silicon dioxide, in product SiOx, x values are fixed value, i.e., non-adjustable；
And when intermediate frequency induction heating temperature >=1600 DEG C, control the ratio of raw material HIGH-PURITY SILICON and the mol ratio of silicon dioxide
At 0.88～1.2, in product SiOx, the value of x is adjustable in the range of 0.89～1.10.
In this example, the sub- silicon of oxidation is prepared using Frequency Induction Heating mode, equipment continuous-stable is made：Induction heating is avoided
Using power it is high, energy consumption is big, easy cause thermal damage electric furnace heating wire, is generated heat by the eddy current effect of graphite crucible, the efficiency of heating surface is high, equipment
Stable, maintenance cost is low；
Sensing heating sublimed method is pollution-free in addition：Vacuum sublimation is a physically separate method, does not carry out chemical reaction, whole
During individual separating-purifying, no waste mine, waste gas are produced, environmentally safe；
The oxidation Asia silicon purity prepared simultaneously is high, can reach more than 99.9%, many by what is prepared using the inventive method
Sample obtained by individual batch carries out the result of icp analysis, impurity content summation<0.05%, referring to table 1：
The purity analysis result of 1 gained sample of table
The high pure zirconia Asia silicon prepared in the present invention can be applicable to lithium ion battery negative, optical glass and high-quality and apply
Material.
Embodiment 2
Referring to Fig. 2 and Fig. 3, this example is the Intermediate Frequency Induction Heating Equipment supporting with preparation method in embodiment 1, including true
Empty furnace shell 6, induction coil 8, heat insulation layer 9, graphite crucible 10, catcher, bell 15, water-cooling system 14, intermediate frequency power supply
4th, intermediate frequency feeder equipment 5, pumped vacuum systems, temp measuring system, it is characterised in that the central axis of described vacuum furnace shell 6 with
The angle on the installation ground of vacuum furnace shell 6 is 1～10 °；Positioned at the graphite crucible 10 of the central axis bottom of graphite crucible 10
At least open end side be provided with carbon barrier 11；Catcher 12 is covered with the end face of the opening of graphite crucible 10, it is described
Catcher 12 be in round platform tubular, and with the opening of the catcher 12 of 10 junction of graphite crucible with diameter greater than catcher
The diameter of tail end.
In this example, the shaft of vacuum furnace shell 6 adopts water-cooled double-walled staving shape, the bell 15 of vacuum furnace shell 6 and vacuum drying oven
The furnace bottom of housing 6 is respectively adopted water-cooled double-walled arch form, is provided with sealing gasket between the port of vacuum furnace shell 6 and bell 15, therefore
When vacuum furnace shell 6 is evacuated, bell 15 can be sealed by external atmospheric pressure.Wherein intermediate frequency feeder equipment 5 with
Intermediate frequency power supply 4 be connected, for melting induction coil 8 be located at vacuum furnace shell 6 in centre, induction coil 8 it is upper and lower
Portion sets rustless steel controlling the water circulation cooling system 14 respectively, its objective is to make furnace lining material, namely 9 material of heat insulation layer axial direction heated equal
It is even, extend the service life of furnace lining.
Carbon barrier 11 is adopted in this example, both can guarantee that, realization prepares every batch more than 50kG's
Sub- silicon is aoxidized, and carbon barrier 11 can also generate heat in the course of the work, it is ensured that raw material of the graphite crucible in open end side
Temperature, reduce the thermograde of raw material reaction.
In addition, the catcher 12 that round platform tubular is adopted in this example is the result through various testing and verifications：It is specific as follows：
No. 2 catchers, referring to Fig. 4, existing catcher typically adopts columnar structured catcher, finds its collection rate not
It is very high；
No. 1 catcher, slot ampuliform as shown in Figure 5；
No. 3 catchers, as shown in fig. 6, which adopts round platform tubular, and the opening with the catcher of graphite crucible connecting side
For wide opening, nested structure can be adopted when being connected with graphite crucible；Or in order to easy to connect, also can be in the opening of catcher
If a circle flange is for being connected with graphite crucible, referring to Fig. 7；
No. 4 catchers, shown in Figure 8, which also uses round platform tubular, simply the catcher with graphite crucible connecting side
Opening be in slot.
Finally found that the catcher effect of round platform tubular shown in Fig. 6 or Fig. 7 preferably, which improves than cylindrical collection device and receives
Collection amount is about 7%.
Alternatively, it is also possible to the apertured on the end face of the tail end of described catcher 12, the radius in hole is 2～5cm；Kong Shangke
It is detachably connected with the blind patch of a covering openings.When Intermediate Frequency Induction Heating Equipment works, after the hole is opened, collection rate is found
Improve 2% again, this should be due to catcher inside aerodynamic factor cause steam be easier to flow and deposit and
It is difficult the reason lost.2 are shown in Table using the yield situation of above-mentioned shape catcher：
Table 2
| Catcher is numbered | 1 | 2 | 3-a | 3-b | 4 |
| Yield | 63% | 82% | 89% | 91% | 76% |
In upper table, 3-a is by the bore closure of catcher tail end；3-b for catcher tail end hole in opened condition.
In the present invention, the material of catcher installs tungsten carbide coating additional using 304 rustless steels or in 304 stainless outer surfaces
Or install the unlike materials such as ceramic coating additional, it is ensured that effective taking-up of material and avoid introducing impurity, shape and material are not only limited
In one kind.
In this example, described catcher 12 is may also be employed along catcher central axis in symmetrical two panels split assembling
Into.
In addition, the central axis of vacuum furnace shell 6 and the angle design for installing ground in the present invention, one is to consider that product exists
It is usually toward rising, so smoothly entering catcher, raising yield, by vacuum furnace shell 6 for the ease of finished product in sublimation process
It is designed to high skewed in port；Also demonstrate in actual production process, can also while yield is improved using the design
Improve collection rate.Wherein, when tilting furnace angle is respectively 1 °, 7 °, the yield of product will be 5 ° less than tilting furnace angle
When yield, it is seen that the central axis of vacuum furnace shell 6 is with to install the preferable angle on ground be 5 °.
Further, described carbon barrier 11 is located at the nearly opening of the lower half inwall of graphite crucible 10；Or
Described carbon barrier 11 be respectively provided at the nearly opening of the lower half inwall of graphite crucible 10 and graphite crucible 10 lower half
The center of X axis is located on portion's inwall, makes the raw material of various pieces increase heating surface, it is ensured that to be heated evenly.
Further, the height of the carbon barrier 11 at the opening of described graphite crucible 10 is 10 internal diameter of graphite crucible
1/2 or 1/3 or 1/4；The height of carbon barrier 11 of the center on the lower half inwall of graphite crucible 10 positioned at X axis is
The 1/5 of 10 internal diameter of graphite crucible.
Therefore, height and position, quantity and the tilting furnace angle and raw material that adjustment carbon barrier 11 is found in the present invention is matched somebody with somebody
Comparing product structure and product yield has different impacts, referring to table 3：
Table 3
In table 3, x values are obtained by LECO ONH836 oxygen nitrogen hydrogen analyzer measurements.
In from table 3, as a example by when reaction temperature is 1400 DEG C, it is earthenware to compare 11 height of carbon barrier at opening
Crucible internal diameter 1/4,1/3,1/2 when impact.The carbon barrier 11 of 1/3 crucible internal diameter height is used at the same terms lower open end
When product collection efficiency be up to 93wt%, and increase the carbon barrier of one 1/5 crucible internal diameter height in crucible center, produce
Thing yield further increases as 94wt%.
When other conditions are identical, raw material Si: SiO2Weight ratio be 34: 66, when reaction temperature be 1400 DEG C when, product
In SiOx, x values are 0.97, improve reaction temperature to 1800 DEG C, and x values are reduced to 0.94.This should be under a high vacuum, it is higher
Temperature is entered in the material collected after causing part material direct gasification, changes the silica ratio of product.
Further, the power-supply controller of electric of described intermediate frequency power supply 4 is controlled using uncontrollable rectifier circuit, whole using not controlling
Current circuit technology is compared other full-controlled rectifier technologies and has power factor (PF) tall and big in 0.95, the advantages of electric network pollution is little；
Described power-supply controller of electric output constant current and invariable power, can remain that power-supply controller of electric is in most effective power
Output mode, makes input power be fully utilized, it is adaptable to need frequent starting or long playing workplace, power supply
The power work frequency for controlling of controller is 2000～2800Hz；
And described power-supply controller of electric by telecommunication come the parameter and running status in read-write controller.Which adopts people
Machine controlling interface, with communication function, using ModBus rtu protocols, RS-485 connected modes, can be read and write by telecommunication
Power-supply controller of electric intrinsic parameter and running status.
Further, described bell 15 is flexibly connected a bell go-cart 13；Described bell go-cart 13 includes a bottom
It is provided with the flat board 13-1 of pulley, one end of flat board 13-1 is rotatably connected the bottom of a primary push rod 13-2, the top of primary push rod 13-2
Mounting hole is provided with along the length direction of primary push rod, one end of a pin is slidably connected in mounting hole, the other end rotation of pin
The middle and upper part of the lateral wall of connection bell 15；The other end of flat board 13-1 is rotatably connected the bottom of a driven push rod 13-3, dynamic
The top of push rod 13-3 sets another mounting hole along the length direction of driven push rod 13-3, and one end of another pin is slidably connected at separately
In one mounting hole, the other end of another pin be rotatably connected bell 15 lateral wall nearly 6 side of vacuum furnace shell in bottom, so lead to
Cross promotion bell go-cart 13 and just can easily open bell.
In order to be able to make bell go-cart 13 along the stable movement of straight line, track can be set in the bottom of bell go-cart 13, facilitate stove
13 orbiting of lid go-cart, can not also set track certainly.
Further, described pumped vacuum systems be sequentially connected using pipeline mechanical pump 1, lobe pump 2, diffusion pump 3；
The air vent of the entrance point connection vacuum furnace shell 6 of described diffusion pump 3.
Further, in the present invention, described temp measuring system connects PID respectively using two outfans of thermometric galvanic couple 7
Temp controlled meter is constituted, and two side warm spots of thermometric galvanic couple 7 are respectively provided at middle part and the opening of graphite crucible；Described thermometric
Galvanic couple 7 adopts W-Re thermocouple.The main body of wherein thermometric galvanic couple 7 is located at outside vacuum furnace shell 6, and the hot junction of thermometric galvanic couple 7 is fixed
In the center of 10 housing of graphite crucible, the cold end of thermometric galvanic couple 7 is fixed in the heat insulation layer 9 at proximal port.Setting PID
Regulation program can make heating-up temperature according to the curvilinear motion of setting, and can control raw material reaction gradient less than 1 DEG C.
Claims (10)
1. a kind of method that Frequency Induction Heating mode prepares high pure zirconia Asia silicon, it is characterised in that using following preparation method：
(1), raw material prepares：Content ＞ 99.5wt% HIGH-PURITY SILICONs, content ＞ 99.5wt% silicon dioxide mix by weight 1: 1,
It is dehydrated Jing after tablet machine is pressed into pie；
(2), Frequency Induction Heating：Pie mixed material is put in the graphite crucible of Intermediate Frequency Induction Heating Equipment, in vacuum bar
1200～2000 DEG C are heated under part, 3～5h of constant temperature makes raw material be reacted and gradually be distilled；
(3), cool down to obtain finished product：After constant temperature terminates 8～10h, material is cooled to room temperature, by the collection in Intermediate Frequency Induction Heating Equipment
Device is opened, and takes out high pure zirconia Asia silicon SiO of the absorption in inner collector wallxFinished product；
When intermediate frequency induction heating temperature is at 1200～1600 DEG C, during the mol ratio of regulation raw material HIGH-PURITY SILICON and silicon dioxide, produce
In thing SiOx, x values are fixed value；
And when intermediate frequency induction heating temperature >=1600 DEG C, the ratio for controlling raw material HIGH-PURITY SILICON with the mol ratio of silicon dioxide exists
When 0.88～1.2, in product SiOx, the value of x is adjustable in the range of 0.89～1.10.
2. a kind of Frequency Induction Heating mode as claimed in claim 1 prepares the Frequency Induction Heating of high pure zirconia Asia silicon and sets
It is standby, including vacuum furnace shell (6), induction coil (8), heat insulation layer (9), graphite crucible (10), catcher, bell (15),
Water-cooling system (14), intermediate frequency power supply (4), intermediate frequency feeder equipment (5), pumped vacuum systems, temp measuring system, it is characterised in that described
The angle on installation ground of central axis and vacuum furnace shell (6) of vacuum furnace shell (6) be 1～10 °；Positioned at graphite crucible
(10) at least open end side of the graphite crucible (10) of central axis bottom is provided with carbon barrier (11)；In graphite crucible (10)
Opening end face on be covered with catcher (12), described catcher (12) in round platform tubular, and with graphite crucible (10)
The diameter of the tail end with diameter greater than catcher of the opening of the catcher (12) of junction.
3. Intermediate Frequency Induction Heating Equipment as claimed in claim 2, it is characterised in that the end of the tail end of described catcher (12)
Face is provided with hole, and the radius in hole is 2～5cm；The blind patch of one covering openings of detachable connection on hole.
4. Intermediate Frequency Induction Heating Equipment as claimed in claim 2 or claim 3, it is characterised in that the opening of described catcher (12)
The end face at end is provided with the flange being connected with graphite crucible (10).
5. Intermediate Frequency Induction Heating Equipment as claimed in claim 2, it is characterised in that described carbon barrier (11) is located at graphite
At the nearly opening of the lower half inwall of crucible (10)；Or described carbon barrier (11) is respectively provided at graphite crucible (10)
Center at the nearly opening of lower half inwall and on the lower half inwall of graphite crucible (10) positioned at X axis.
6. Intermediate Frequency Induction Heating Equipment as claimed in claim 5, it is characterised in that the opening of described graphite crucible (10)
The height of the carbon barrier (11) at place for graphite crucible (10) internal diameter 1/2 or 1/3 or 1/4；The lower half of graphite crucible (10)
Height on inwall positioned at the carbon barrier (11) of the center of X axis is the 1/5 of graphite crucible (10) internal diameter.
7. Intermediate Frequency Induction Heating Equipment as claimed in claim 2, it is characterised in that
Described bell (15) is flexibly connected a bell go-cart (13)；
Described bell go-cart (13) is provided with the flat board (13-1) of pulley including a bottom, and one end of flat board (13-1) is rotatably connected
The bottom of one primary push rod (13-2), the top of primary push rod (13-2) are provided with mounting hole along the length direction of primary push rod, a pin
One end is slidably connected in mounting hole, the other end of pin be rotatably connected bell (15) lateral wall middle and upper part；Flat board (13-
1) the other end is rotatably connected the bottom of a driven push rod (13-3), on the top of dynamic push rod (13-3) along driven push rod (13-3)
Length direction set another mounting hole, one end of another pin is slidably connected in another mounting hole, the other end of another pin
Be rotatably connected bell (15) lateral wall nearly vacuum furnace shell (6) side in bottom；
The bottom of described bell go-cart (13) is provided with track.
8. Intermediate Frequency Induction Heating Equipment as claimed in claim 2, it is characterised in that described pumped vacuum systems is to adopt pipeline
The mechanical pump (1) that is sequentially connected, lobe pump (2), diffusion pump (3)；The entrance point connection vacuum furnace shell of described diffusion pump (3)
(6) air vent.
9. Intermediate Frequency Induction Heating Equipment as claimed in claim 2, it is characterised in that the power supply control of described intermediate frequency power supply (4)
Device processed is controlled using uncontrollable rectifier circuit, and described power-supply controller of electric exports constant current and invariable power, described power supply
The power work frequency for controlling of device is 2000～2800Hz；Described power-supply controller of electric is by telecommunication come read-write controller
Interior parameter and control running status.
10. Intermediate Frequency Induction Heating Equipment as claimed in claim 2, it is characterised in that described temp measuring system is using thermometric electricity
Two outfans of even (7) connect PID temp controlled meters respectively and are constituted, and two side warm spots of thermometric galvanic couple (7) are respectively provided at graphite
At the middle part of crucible and opening；Described thermometric galvanic couple (7) is using W-Re thermocouple.
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| CN107176609A (en) * | 2017-07-04 | 2017-09-19 | 山西科德技术陶瓷有限公司 | A kind of evaporation deposition equipment of the sub- silicon of big yield low cost production oxidation |
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| CN110657668A (en) * | 2018-12-12 | 2020-01-07 | 株洲诺天电热科技有限公司 | Horizontal side collecting method for solid purified substances of electric heating equipment |
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| CN110655085A (en) * | 2018-12-12 | 2020-01-07 | 株洲诺天电热科技有限公司 | Single-side collecting method for solid purified object horizontal electric heating equipment |
| CN110671933A (en) * | 2018-12-12 | 2020-01-10 | 株洲诺天电热科技有限公司 | Method for collecting solid-state purified matter on two lateral sides of horizontal electric heating equipment |
| CN110668448A (en) * | 2018-12-12 | 2020-01-10 | 株洲诺天电热科技有限公司 | Single-side lateral horizontal collecting device of solid pure object electric heating equipment |
| CN110657669A (en) * | 2018-12-12 | 2020-01-07 | 株洲诺天电热科技有限公司 | Horizontal collecting device for two-side surfaces of solid pure object electric heating equipment |
| CN109650858A (en) * | 2018-12-18 | 2019-04-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of silicon oxygen negative electrode material and products thereof and application |
| CN113937259A (en) * | 2021-09-07 | 2022-01-14 | 惠州市贝特瑞新材料科技有限公司 | Preparation method and device of silicon monoxide for lithium ion battery and lithium ion battery |
| CN114394599A (en) * | 2022-01-18 | 2022-04-26 | 郑州炬煌新材料科技有限公司 | Preparation method of silicon monoxide and preparation device for realizing method |
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