CN110294479A - The preparation facilities of carbon-silicon composite material - Google Patents
The preparation facilities of carbon-silicon composite material Download PDFInfo
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- CN110294479A CN110294479A CN201910667630.7A CN201910667630A CN110294479A CN 110294479 A CN110294479 A CN 110294479A CN 201910667630 A CN201910667630 A CN 201910667630A CN 110294479 A CN110294479 A CN 110294479A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 64
- 239000002153 silicon-carbon composite material Substances 0.000 title claims abstract description 44
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 97
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 65
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 57
- 239000010439 graphite Substances 0.000 claims abstract description 57
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 40
- 238000002156 mixing Methods 0.000 claims abstract description 36
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 34
- 239000003960 organic solvent Substances 0.000 claims abstract description 32
- 230000007246 mechanism Effects 0.000 claims abstract description 28
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims abstract description 14
- 229920005591 polysilicon Polymers 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims description 46
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 34
- 238000012216 screening Methods 0.000 claims description 30
- 238000005406 washing Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 19
- 238000000227 grinding Methods 0.000 claims description 13
- 238000004140 cleaning Methods 0.000 claims description 10
- 239000007790 solid phase Substances 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 abstract description 29
- 239000010703 silicon Substances 0.000 abstract description 29
- 238000000034 method Methods 0.000 abstract description 28
- 230000008569 process Effects 0.000 abstract description 24
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 238000012546 transfer Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 21
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 11
- 239000007787 solid Substances 0.000 description 11
- 239000000843 powder Substances 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 230000036961 partial effect Effects 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 230000002401 inhibitory effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 229910021382 natural graphite Inorganic materials 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000004087 circulation Effects 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010981 drying operation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
- C01B32/963—Preparation from compounds containing silicon
- C01B32/984—Preparation from elemental silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
-
- 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
- C01P2006/40—Electric properties
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Silicon Compounds (AREA)
Abstract
The present invention provides a kind of preparation facilities of carbon-silicon composite material.The preparation facilities includes polysilicon preparing device, graphite feeding mechanism, mixing device and roasting unit, and polysilicon preparing device is provided with unformed silicon powder supply opening, for supplying unformed silicon powder；Graphite feeding mechanism is provided with graphite supply opening, for supplying graphite；Mixing device is provided with feed opening and mixing outlet, and feed opening is connected with unformed silicon powder supply opening and graphite supply opening respectively, while feed opening is also used for addition carbon source and organic solvent；Roasting unit is provided with mixing entrance, and mixing outlet is connected with mixing entrance by mixing transfer pipeline.There is lesser silicon source cubical expansivity and biggish battery capacity using carbon-silicon composite material made from above-mentioned preparation facilities.Furthermore the advantages that above-mentioned preparation facilities also has process short, and low energy consumption, environmentally friendly.
Description
Technical field
The present invention relates to field of polysilicon production, in particular to a kind of preparation facilities of carbon-silicon composite material.
Background technique
In recent years, with the improvement of people ' s living standards and the enhancing to environmental protection consciousness, reusable secondary
Battery using more and more extensive, the requirement to battery capacity is also higher and higher.On the other hand, as relevant laws and regulations are successive
Appearance and the reinforcement of national policy supporting dynamics also play good impetus to the application for promoting high-capacity battery.
Currently, limitation battery capacity improve principal element be the carbon negative pole material generally used capacity it is too low, can not
So that battery capacity is reached relevant regulations, only can just battery capacity be made to reach requirement using the higher novel anode material of capacity,
And in all negative electrode materials, Si-C composite material is most to be hopeful to replace carbon negative pole material.Therefore, research and development low cost,
The Si-C composite material of high capacity is at current heat subject.
Summary of the invention
The main purpose of the present invention is to provide a kind of preparation facilities of carbon-silicon composite material, to solve existing silicium cathode material
Material has that silicon materials volume expansion is larger.
To achieve the goals above, a kind of preparation facilities of carbon-silicon composite material is provided according to the present invention, preparation dress
It sets including polysilicon preparing device, graphite feeding mechanism, mixing device and roasting unit, polysilicon preparing device is provided with without fixed
Type silicon powder supply opening, for supplying unformed silicon powder；Graphite feeding mechanism is provided with graphite supply opening, for supplying graphite；It is mixed
Material device is provided with feed opening and mixing outlet, and feed opening is connected with unformed silicon powder supply opening and graphite supply opening respectively,
Feed opening is also used for addition carbon source and organic solvent simultaneously；Roasting unit is provided with mixing entrance, mixing outlet and mixing entrance
It is connected by mixing transfer pipeline.
Further, roasting unit include: calciner and grinding screening plant, calciner be provided with mixing entrance and
Product of roasting outlet；And grinding screening plant is provided with product of roasting entrance, product of roasting entrance is connected with product of roasting outlet
It is logical.
Further, grinding screening plant is provided with screening materials carrying outlet, and above-mentioned preparation facilities further includes washing unit, is washed
Washing unit includes: hydrofluoric acid feeding mechanism, wash mill and filter device, and hydrofluoric acid feeding mechanism is provided with hydrofluoric acid supply
Mouthful；Wash mill is provided with cleaning solution entrance, screening materials carrying entrance and washing material outlet, screening materials carrying entrance and screening materials carrying
Outlet is connected, and cleaning solution entrance is connected with hydrofluoric acid supply opening；And filter device is provided with washing material entrance, washings
Material entrance is connected with washing material outlet.
Further, filter device is provided with solid-phase outlet, and above-mentioned washing unit further includes drying unit, and drying unit is set
It is equipped with material inlet to be dried, material inlet to be dried is connected with by solid-phase outlet, for drying through solid-phase outlet discharge
Material.
Further, above-mentioned roasting unit is additionally provided with temperature control equipment, and temperature control equipment is for controlling roasting dress
Temperature in setting.
Further, above-mentioned preparation facilities further includes charging metering device, and charging metering device is for controlling unformed silicon
The additional amount of powder, graphite, carbon source and organic solvent.
Further, above-mentioned preparation facilities further includes carbon source feeding mechanism and the first control valve, the setting of carbon source feeding mechanism
There is carbon source supply opening, carbon source supply opening is connected with feed opening by carbon source supply line, and the setting of the first control valve is supplied in carbon source
It answers on pipeline, and the first control valve is electrically connected with charging metering device.
Further, above-mentioned preparation facilities further includes organic solvent feeding mechanism and the second control valve, organic solvent supply
Device is provided with organic solvent supply opening, and organic solvent supply opening is connected with feed opening by organic solvent supply line, the
Two control valves are arranged on organic solvent supply line, and the second control valve is electrically connected with charging metering device.
Further, silicon powder supply opening is connected with feed opening by silicon powder supply line, and above-mentioned preparation facilities includes the
Three control valves, third control valve are arranged on silicon powder supply line, and third control valve is electrically connected with charging metering device.
Further, graphite supply opening is connected with feed opening by graphite supply line, and above-mentioned preparation facilities includes the
Four control valves, the 4th control valve are arranged on graphite supply line, and the 4th control valve is electrically connected with charging metering device.
It applies the technical scheme of the present invention, in the preparation facilities of above-mentioned carbon-silicon composite material, is supplied in polysilicon preparing device
The silicon powder answered is generated under gaseous environment, and partial size is very suitable to coat than the uniform particle sizes that ball milling obtains, this makes carbon silicon
The volume change of composite material silicon in application process is relatively small；The graphite that graphite device provides simultaneously is added to mixing device
When middle, since graphite is continuous conduction phase, graphite, which is added, can play the role of inhibiting silicon volume expansion.It is former at above-mentioned two aspect
Because under, using carbon-silicon composite material made from above-mentioned preparation facilities there is lesser silicon source cubical expansivity and biggish battery to hold
Amount.Furthermore the advantages that above-mentioned preparation facilities also has process short, and low energy consumption, environmentally friendly.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present invention, and of the invention shows
Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.In the accompanying drawings:
Fig. 1 shows the preparation facilities for the carbon-silicon composite material that a kind of typical embodiment according to the present invention provides
Structural schematic diagram；And
Fig. 2 shows a kind of preparation methods for the carbon-silicon composite material that typical embodiment provides according to the present invention
Process flow chart.
Wherein, the above drawings include the following reference numerals:
11, polysilicon preparing device；12, graphite feeding mechanism；13, carbon source feeding mechanism；14, organic solvent supply dress
It sets；
20, mixing device；
30, roasting unit；31, calciner；32, screening plant is ground；
40, washing unit；41, hydrofluoric acid feeding mechanism；42, wash mill；43, filter device；44, drying unit.
Specific embodiment
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.Below in conjunction with embodiment, the present invention will be described in detail.
As described in background technique, existing silicium cathode material has that silicon materials volume expansion is larger.For
Solution above-mentioned technical problem, this application provides a kind of preparation facilities of carbon-silicon composite material, as shown in Figure 1, the preparation fills
Set includes: polysilicon preparing device 11, graphite feeding mechanism 12, mixing device 20 and roasting unit 30.Polysilicon preparing device
11 are provided with unformed silicon powder supply opening, for supplying unformed silicon powder；Graphite feeding mechanism 12 is provided with graphite supply opening, uses
In supply graphite；Mixing device 20 be provided with feed opening and mixing outlet, feed opening respectively with unformed silicon powder supply opening and stone
Black supply opening is connected, while feed opening is also used for addition carbon source and organic solvent, and feed opening is also used for addition carbon source and organic
Solvent, roasting unit 30 are provided with mixing entrance, and mixing outlet is connected with mixing entrance by mixing transfer pipeline.
In the preparation facilities of above-mentioned carbon-silicon composite material, the silicon powder supplied in polysilicon preparing device 11 is in gaseous environment
Lower generation, partial size is usually 1~300nm than the uniform particle sizes that ball milling obtains, and is very suitable to coat, this makes carbon silicon composite wood
Expect that the volume change of silicon in application process is relatively small, and advantageously reduces preparation cost；Graphite device provides simultaneously
When graphite is added in mixing device 20, since graphite is continuous conduction phase, addition graphite, which can play, inhibits silicon source volume swollen
Swollen effect.Under above-mentioned two aspects reason, there is lesser silicon body using carbon-silicon composite material made from above-mentioned preparation facilities
Product expansion rate and biggish battery capacity.Furthermore above-mentioned preparation facilities also has process short, and low energy consumption, environmentally friendly etc. excellent
Point.
Silicon volume expansion rate is advantageously reduced using the preparation facilities of above-mentioned carbon-silicon composite material.In a kind of preferred implementation
In example, as shown in Figure 1, the roasting unit 30 includes calciner 31 and grinding screening plant 32, calciner 31 is provided with mixed
Expect entrance and product of roasting outlet；And grinding screening plant 32 is provided with product of roasting entrance, product of roasting entrance and roasting produce
Object outlet is connected.
The mixed material obtained after the mixing of mixing device 20, which is delivered in calciner 31, to be roasted, so that carbon silicon is multiple
Condensation material forms relatively stable porous structure, while making in the porous structure of graphite insertion aforementioned stable.Due to above-mentioned hole
Presence so that the expansion process of silicon volume the performance of the subsequent electrode containing carbon-silicon composite material is influenced it is smaller.Pass through simultaneously
Carbon-silicon composite material is ground into more tiny particle by grinding screening plant 32, to be conducive to further decrease silicon volume expansion
The performance of the subsequent electrode containing carbon-silicon composite material is influenced.
In a kind of preferred embodiment, as shown in Figure 1, grinding screening plant 32 is provided with screening materials carrying outlet, it is above-mentioned
Preparation facilities further includes washing unit 40, which further includes hydrofluoric acid feeding mechanism 41, wash mill 42 and filtering
Device 43, hydrofluoric acid feeding mechanism 41 are provided with hydrofluoric acid supply opening；Wash mill 42 is provided with cleaning solution entrance, screening materials carrying
Entrance and washing material outlet, screening materials carrying entrance are connected with screening materials carrying outlet, cleaning solution entrance and hydrofluoric acid supply opening
It is connected；And filter device 43 is provided with washing material entrance, washing material entrance is connected with washing material outlet.
The powders calcined filtered out is washed using the strong hydrofluoric acid of corrosivity, the gold in product of roasting can be removed
Category and other impurity, and then can be improved the purity of carbon-silicon composite material.
Surface of material after pickling would generally remain some cleaning solution hydrofluoric acid, in order to remove above-mentioned cleaning solution, such as Fig. 1
It is shown, it is preferable that above-mentioned filter device 43 is provided with solid-phase outlet, and washing unit 40 further includes drying unit 44, drying unit
44 are provided with material inlet to be dried, and material inlet to be dried is connected with by solid-phase outlet, for drying to through solid-phase outlet
The material of discharge.
It is highly preferred that as shown in Figure 1, above-mentioned drying unit 44 is negative pressure calciner 31.It will be under the negative pressure of roasting process
The efficiency for being conducive to improve drying is carried out, and then shortens manufacturing cycle.
In order to precisely control the maturing temperature in roasting unit 30, as illustrated in fig. 1, it is preferred that roasting unit 30 is also
It is provided with temperature control equipment, temperature control equipment is used to control the temperature in calciner 31.
In order to preferably control silicon powder, graphite, carbon source and the amount of being included in of organic solvent, it is preferable that above-mentioned preparation facilities is also
Including the metering device that feeds, charging metering device is used to control the additional amount of unformed silicon powder, graphite, carbon source and organic solvent.
In order to further increase the degree of automation of above-mentioned carbon-silicon composite material preparation facilities, Automatic-feeding dress can be set
It sets.As long as automatic feeder can be realized above-mentioned function, structure is not specifically limited.
In a kind of preferred embodiment, as shown in Figure 1, above-mentioned preparation facilities further includes carbon source feeding mechanism 13 and first
Control valve, carbon source feeding mechanism 13 are provided with carbon source supply opening, and carbon source supply opening is connected with feed opening by carbon source supply line
Logical, the first control valve is arranged on carbon source supply line, and third control valve is electrically connected with charging metering device.
In a kind of preferred embodiment, as shown in Figure 1, above-mentioned preparation facilities further includes 14 He of organic solvent feeding mechanism
Second control valve, organic solvent feeding mechanism 14 are provided with organic solvent supply opening, and organic solvent supply opening passes through with feed opening
Organic solvent supply line is connected, and the second control valve is arranged on organic solvent supply line, and the second control valve and charging
Metering device electrical connection.
Specifically, as shown in Figure 1, in a kind of preferred embodiment, above-mentioned preparation facilities includes third control valve, silicon powder
Supply opening is connected with feed opening by silicon powder supply line, and third control valve is arranged on silicon powder supply line, and third control
Valve processed is electrically connected with charging metering device.
In a kind of preferred embodiment, above-mentioned preparation facilities includes the 4th control valve, and graphite supply opening and feed opening are logical
It crosses graphite supply line to be connected, the 4th control valve is arranged on graphite supply line, and the 4th control valve and charging metering dress
Set electrical connection.
The another aspect of the application additionally provides a kind of preparation method of carbon-silicon composite material, as shown in Fig. 2, the preparation side
Method includes: to mix silicon source, carbon source, graphite and organic solvent, obtains mixture, wherein the system of above-mentioned carbon-silicon composite material
During standby, silicon source is the grade amorphous silicon powder of nanometer generated in polysilicon production process；And under protective atmosphere, make mixture
It is roasted, obtains carbon-silicon composite material.
The present invention using the unformed silicon powder of silicon source is generated under gaseous environment, and partial size is more equal than the partial size that ball milling obtains
It is even, it is very suitable to coat, this makes the volume change of carbon-silicon composite material in application process relatively small；Graphite is to connect simultaneously
Continuous conductive phase, graphite is added during the preparation process can play the role of inhibiting silicon source volume expansion.In above-mentioned two aspects reason
Under, above-mentioned carbon-silicon composite material has lesser silicon volume expansion rate and biggish battery capacity.Furthermore above-mentioned technique also has
The advantages that process is simple, and low energy consumption, environmentally friendly.
There is lower silicon volume expansion rate and higher battery using carbon-silicon composite material made from above-mentioned preparation method
Capacity.In a preferred embodiment, the weight ratio of silicon source, carbon source and graphite is (1~30): (20~69): (30~
50).The weight ratio of silicon source, carbon source and graphite includes but is not limited to above range, and is limited and be conducive within the above range
The cubical expansivity of silicon is further suppressed, and improves battery capacity.
The carbon source used during above-mentioned preparation of silicon carbon composite materials can use carbon source commonly used in the art.Preferably,
Carbon source include but is not limited to charcoal, polyvinyl chloride and glucose group after pitch, coke, thermal decomposition at one of group or more
Kind, or the solution comprising above-mentioned carbon source.Above-mentioned carbon source have many advantages, such as it is cheap be easy to get, select above-mentioned carbon source to be conducive to drop
The cost of low Si-C composite material.
The graphite used during above-mentioned preparation of silicon carbon composite materials can be natural graphite, be also possible to artificial graphite.
The organic solvent used during above-mentioned preparation of silicon carbon composite materials can use organic solvent commonly used in the art.
Preferably, organic solvent includes but is not limited to one of group of tetrahydrofuran, glucose, toluene and n-hexane composition or more
Kind.
Roasting process makes even closer in combination between carbon source, silicon source and graphite, and can remove silicon carbon material surface
Labile functional groups, and then be conducive to improve battery capacity.In a preferred embodiment, above-mentioned roasting process -0.2~
It is carried out under the pressure of 0.2bar.There is gas generation in above-mentioned roasting process, above-mentioned roasting process is conducive under negative pressure
The expulsion efficiency for improving gaseous product, improves the progress of roasting process, to be conducive to improve battery capacity and first charge-discharge
Efficiency.
Above-mentioned protective atmosphere is non-oxidized gas, it is preferable that protective atmosphere is argon gas and/or hydrogen.
In a preferred embodiment, the temperature of roasting process is 600~1300 DEG C.Since the application prepares carbon silicon
During composite material, the grade amorphous silicon powder of specific nanometer joined as silicon source, while being also added into graphite, due to original
Maturing temperature is limited the extent of reaction for being conducive to improve roasting process within the above range, and then is conducive to by the particularity of material
Reduce silicon source cubical expansivity and battery capacity in carbon-silicon composite material.It is highly preferred that the temperature of roasting process is 850~1200
℃。
In order to further increase the comprehensive performance of carbon-silicon composite material, in a preferred embodiment, above-mentioned preparation
Method further includes the steps that successively being ground the product system of calcination, sieves and pickling and drying.
Preferably, the granularity of the solid particle obtained after screened process is 100~500 μm.By the granularity of solid particle
It limits within the above range, relative to the total volume of silicon source, the expansion variation of silicon source volume is lower in use process, and then its is right
The influence of battery capacity is smaller.It is highly preferred that the granularity of the solid particle obtained after screened process is 100~300 μm.
In a preferred embodiment, acid used in acid cleaning process is hydrofluoric acid.Using the strong hydrogen fluorine of corrosivity
Acid washs the powders calcined filtered out, can remove metal and other impurity in product of roasting, and then can be improved
The purity of carbon-silicon composite material.
In a preferred embodiment, baking step carries out under conditions of -0.1~0bar and 100~250 DEG C.
Above-mentioned drying course is carried out to the time for being conducive to shorten drying course under the above conditions, and then is conducive to shorten preparation week
Phase.
The another aspect of the application additionally provides a kind of carbon silicon combination electrode, and the carbon silicon combination electrode is multiple comprising above-mentioned silicon-carbon
Condensation material.
The present invention using the unformed silicon powder of silicon source is generated under gaseous environment, and partial size is more equal than the partial size that ball milling obtains
It is even, it is very suitable to coat, this makes the volume change of carbon-silicon composite material in application process relatively small；Graphite is to connect simultaneously
Continuous conductive phase, graphite is added during the preparation process can play the role of inhibiting silicon source volume expansion.Thus above-mentioned carbon silicon is compound
Material has lesser silicon volume expansion rate and biggish battery capacity.On this basis, containing the electrode of carbon-silicon composite material
With relatively stable battery capacity and energy density.
The another aspect of the application additionally provides a kind of battery, which includes carbon silicon combination electrode provided by the present application.
Since the electrode provided by the present application containing carbon-silicon composite material has relatively stable battery capacity and energy close
Degree, the battery containing above-mentioned carbon silicon combination electrode have relatively stable battery capacity and first charge-discharge efficiency.
The application is described in further detail below in conjunction with specific embodiment, these embodiments should not be understood as limitation originally
Apply for range claimed.
Carbon-silicon composite material is prepared using preparation facilities shown in FIG. 1 in the embodiment of the present application.
Embodiment 1
Polysilicon preparing device 11 is for supplying unformed silicon powder；Graphite feeding mechanism 12 is for supplying graphite.
After the unformed silicon powder of collection is sieved in grinding screening plant 32, and by itself and organic solvent, grinding
Graphite well, charcoal are mixed in mixing device 20, obtain mixture；Said mixture is put into calciner 31 (high temperature furnace)
In, and roasted under the conditions of protective atmosphere, obtain product of roasting.It takes out, and carries out after product of roasting is gradually cooling to room temperature
Obtained solid, is put into drying box after being filtered dry and dries by cleaning.By after drying by solid abrasive to meeting the requirements, most afterwards through sieving
Get qualified Si-C composite material.
The actual conditions of the present embodiment are as follows:
(1) unformed silicon powder is sieved using the sieve of 300 mesh, the qualified powder of screening is continued to employ.
(2) natural graphite after grinding is sieved using the sieve of 300 mesh, the qualified powder of screening is continued to employ.
(3) in mixing device 20, ingredient is carried out by weight 25:45:30 by silicon powder, graphite and pitch, it then will drip
Amorphous silica powder and graphite green, after screening are dissolved completely in organic solvent (tetrahydrofuran), after mixing evenly, are filtered insoluble
Object obtains filtrate.
(4) in calciner 31, using above-mentioned filtrate 850 DEG C, -0.05bar~-0.1bar, use argon gas as protection gas
In the environment of roast, volatilize until by whole solvents, obtain product of roasting solid, then continue above-mentioned product of roasting solid
It is cooled to room temperature under an argon.
(5) product of roasting is delivered in grinding screening plant 32, and under an argon, above-mentioned product of roasting solid is ground
200 μm are milled to, screening product is left；Above-mentioned screening product is washed with hydrofluoric acid in wash mill 42, with remove by
Metal and the removal of other impurity in qualified powder are sieved, solid powder finally is obtained by filtration through filter device 43.
(6) by the solid filtered in step (5) under conditions of -0.1bar, 150 DEG C, argon atmosphere in drying unit 44
Middle carry out drying operation, the solid powder after Drying and cooling is Si-C composite material finished product.
(7) the button cell tester of Ke Jing company is made button cell to silicon-carbon cathode dusty material and carries out performance survey
Examination, battery capacity is still greater than 1000mAh/g after 1000 circulations.
It can be seen from the above description that the above embodiments of the present invention realized the following chievements: using above-mentioned
Carbon-silicon composite material made from preparation facilities has lesser silicon source cubical expansivity and biggish battery capacity.Furthermore above-mentioned system
The advantages that standby device also has process short, and low energy consumption, environmentally friendly.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation facilities of carbon-silicon composite material, which is characterized in that the preparation facilities includes:
Polysilicon preparing device (11), the polysilicon preparing device (11) is provided with unformed silicon powder supply opening, for supplying
Unformed silicon powder；
Graphite feeding mechanism (12), the graphite feeding mechanism (12) is provided with graphite supply opening, for supplying graphite；
Mixing device (20), the mixing device (20) be provided with feed opening and mixing outlet, the feed opening respectively with it is described
Unformed silicon powder supply opening is connected with the graphite supply opening, while the feed opening is also used for addition carbon source and organic molten
Agent；
Roasting unit (30), the roasting unit (30) are provided with mixing entrance, and the mixing outlet and the mixing entrance are logical
Overmulling material conveying tube road is connected.
2. preparation facilities according to claim 1, which is characterized in that the roasting unit (30) includes:
Calciner (31), the calciner (31) are provided with the mixing entrance and product of roasting outlet；And
It grinds screening plant (32), the grinding screening plant (32) is provided with product of roasting entrance, the product of roasting entrance
It is connected with product of roasting outlet.
3. preparation facilities according to claim 2, which is characterized in that the grinding screening plant (32) is provided with screening object
Material outlet, the preparation facilities further includes washing unit (40), and the washing unit (40) includes:
Hydrofluoric acid feeding mechanism (41), the hydrofluoric acid feeding mechanism (41) are provided with hydrofluoric acid supply opening；
Wash mill (42), the wash mill (42) are provided with cleaning solution entrance, screening materials carrying entrance and washing material outlet,
The screening materials carrying entrance is connected with screening materials carrying outlet, and the cleaning solution entrance is connected with the hydrofluoric acid supply opening
It is logical；And
Filter device (43), the filter device (43) are provided with washing material entrance, and the washing material entrance is washed with described
Material outlet is washed to be connected.
4. preparation facilities according to claim 3, which is characterized in that the filter device (43) is provided with solid-phase outlet,
The washing unit (40) further includes drying unit (44), and the drying unit (44) is provided with material inlet to be dried, described
Material inlet to be dried is connected with by the solid-phase outlet, for drying the material being discharged through the solid-phase outlet.
5. preparation facilities according to claim 2, which is characterized in that the roasting unit (30) is additionally provided with temperature control
Device, the temperature control equipment are used to control the temperature in the calciner (31).
6. preparation facilities according to any one of claim 1 to 5, which is characterized in that the preparation facilities further includes adding
Expect that metering device, the charging metering device are used to control the unformed silicon powder, the graphite, the carbon source and described organic
The additional amount of solvent.
7. preparation facilities according to claim 6, which is characterized in that the preparation facilities further includes carbon source feeding mechanism
(13) and the first control valve, the carbon source feeding mechanism (13) are provided with carbon source supply opening, and the carbon source supply opening adds with described
Material mouth is connected by carbon source supply line, and first control valve is arranged on the carbon source supply line, and described first
Control valve is electrically connected with the charging metering device.
8. preparation facilities according to claim 6, which is characterized in that the preparation facilities further includes organic solvent supply dress
(14) and the second control valve are set, the organic solvent feeding mechanism (14) is provided with organic solvent supply opening, the organic solvent
Supply opening is connected with the feed opening by organic solvent supply line, and second control valve is arranged in the organic solvent
On supply line, and second control valve is electrically connected with the charging metering device.
9. preparation facilities according to claim 6, which is characterized in that the silicon powder supply opening and the feed opening pass through silicon
Powder supply line is connected, and the preparation facilities includes third control valve, and the third control valve setting is supplied in the silicon powder
On pipeline, and the third control valve is electrically connected with the charging metering device.
10. preparation facilities according to claim 6, which is characterized in that the graphite supply opening passes through with the feed opening
Graphite supply line is connected, and the preparation facilities includes the 4th control valve, and the 4th control valve setting is supplied in the graphite
It answers on pipeline, and the 4th control valve is electrically connected with the charging metering device.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001345100A (en) * | 2000-05-31 | 2001-12-14 | Hitachi Chem Co Ltd | Carbonaceous particles for negative electrode of lithium secondary cell, preparation process thereof, negative electrode for lithium secondary cell and lithium secondary cell |
| CN103833034A (en) * | 2014-02-12 | 2014-06-04 | 浙江天乐新材料科技有限公司 | Method for preparation of silicon carbide slurry with nano-carbontube and graphene as carbon sources |
| CN103904307A (en) * | 2012-12-24 | 2014-07-02 | 宁波杉杉新材料科技有限公司 | Silicon-carbon composite material, preparation method and application thereof |
| CN106744919A (en) * | 2017-01-17 | 2017-05-31 | 韩俊培 | A kind of production technology of polycrystalline silicon base plate special graphite |
| CN210595289U (en) * | 2019-07-23 | 2020-05-22 | 中国恩菲工程技术有限公司 | Preparation device of carbon-silicon composite material |
-
2019
- 2019-07-23 CN CN201910667630.7A patent/CN110294479B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001345100A (en) * | 2000-05-31 | 2001-12-14 | Hitachi Chem Co Ltd | Carbonaceous particles for negative electrode of lithium secondary cell, preparation process thereof, negative electrode for lithium secondary cell and lithium secondary cell |
| CN103904307A (en) * | 2012-12-24 | 2014-07-02 | 宁波杉杉新材料科技有限公司 | Silicon-carbon composite material, preparation method and application thereof |
| CN103833034A (en) * | 2014-02-12 | 2014-06-04 | 浙江天乐新材料科技有限公司 | Method for preparation of silicon carbide slurry with nano-carbontube and graphene as carbon sources |
| CN106744919A (en) * | 2017-01-17 | 2017-05-31 | 韩俊培 | A kind of production technology of polycrystalline silicon base plate special graphite |
| CN210595289U (en) * | 2019-07-23 | 2020-05-22 | 中国恩菲工程技术有限公司 | Preparation device of carbon-silicon composite material |
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