CN107482160A - The method that lithium battery C Si negative pole coatings are prepared using vacuum magnetron sputtering coating film technology - Google Patents
The method that lithium battery C Si negative pole coatings are prepared using vacuum magnetron sputtering coating film technology Download PDFInfo
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- CN107482160A CN107482160A CN201710656804.0A CN201710656804A CN107482160A CN 107482160 A CN107482160 A CN 107482160A CN 201710656804 A CN201710656804 A CN 201710656804A CN 107482160 A CN107482160 A CN 107482160A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- 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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0421—Methods of deposition of the material involving vapour deposition
- H01M4/0423—Physical vapour deposition
- H01M4/0426—Sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0605—Carbon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
Abstract
The present invention discloses a kind of method that lithium battery C Si negative pole coatings are prepared using vacuum magnetron sputtering coating film technology, and this method comprises the following steps：Shiny copper foil is chosen, is cut by used vacuum magnetron sputtering coating film equipment stowing dimensions；The Si cathode targets of vacuum magnetron sputtering coating film equipment and the installation site of C cathode targets are set, the Si plasmas that Si cathode targets sputter and the C plasma doping sputters that C cathode targets sputter is realized that 1/2 volume is overlapping；Vacuum magnetic control sputtering process condition is set；In vacuum environment, vacuum direct magnetic control sputter mixes plating C Si films, makes Si plasmas and C plasma dopings and reaches 200 500nm thickness；Vacuum bag is sealed up for safekeeping after copper foil after plated film is dried in vacuum drying chamber；The present invention deposits one layer of C Si composite negative pole film by magnetic control sputtering vacuum coating technology on cathode of lithium battery copper foil, to improve negative electrode electrical property.
Description
Technical field
The present invention relates to lithium battery device and lithium battery material manufacturing technology field, and in particular to one kind utilizes vacuum magnetic control
The method that sputter coating technology prepares lithium battery C-Si negative pole coatings.
Background technology
Lithium ion battery is mainly made up of positive pole, negative pole, barrier film and electrolyte.The potential that battery the two poles of the earth are added in during charging is compeled
The lithium intercalation compound of positive pole is set to discharge lithium ion, by the graphite cathode of embedded six square piece Rotating fields after barrier film；During electric discharge
Lithium ion then separates out from the graphite of lamellar structure, and the lithium intercalation compound with positive pole combines again, and the movement of lithium ion generates
Electric current.
In the negative pole of lithium ion battery, in lithium ion battery negative material, native graphite and Delanium in occupation of
More than the 90% negative material market share, graphitized intermediate-phase carbosphere (MCMB), amorphous carbon, silicon or tin class occupy small portion
Divide the market share.
Silicon is as the material (4199mAh/g) with known highest lithium ion storage volume, in embedded or abjection lithium
A maximum of about of 300% great Volume Changes can occur.Due to the Volume Changes, active material and overall electrode structure is caused to have
There is big mechanical stress, if carrying out electrochemical milling, the loss of electrical contact can be caused and thus in the case of capacitance loss
Cause electrode damage.In addition, the surface of silicium cathode material and being reacted into branch for electrolyte, so as to be continuously formed passivation
Protective layer (solid electrolyte interface SEI), this causes irreversible lithium to lose.
One kind, which possible solution, to be, not in pure form, but uses silicon-based active as the compound with carbon
Material.Carbonaceous amount is small, is characterised by that the Volume Changes during charge/discharge are small, carbon based negative electrodes have extraordinary electrochemistry
Stability, by the way that the advantages of both elements to be combined together to (Si has big capacity, and C has high stability), C/Si
Base electrode active material also has the cycle characteristics more more stable than pure silicon in the case of the capacity that can be improved.
Magnetron sputtering method has been successfully applied to the system of different films as a kind of method of common physical vapour deposition (PVD)
Standby technique, particularly in thin film semiconductor manufactures, widely use different material mixes sputter manufacture various functions device.
Existing lithium battery manufacturing process, it is that wet coating is on copper foil after being stirred using graphite with silicon materials mechanical mixture
Face makes cathode of lithium battery, and the high power capacity performance of Si materials is used without getting a desired effect.
The content of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide one kind utilizes vacuum magnetron sputtering coating film
The method that technology prepares lithium battery C-Si negative pole coatings, it is by magnetic control sputtering vacuum coating technology on cathode of lithium battery copper foil
One layer of C-Si composite negative pole film is deposited, to improve negative electrode electrical property.
To achieve the above object, the technical solution adopted by the present invention is：Utilize plasma vacuum magnetic-controlled sputtering coating equipment
Sputtering prepares C-Si laminated films on the copper foil of lithium battery colelctor electrode.
Preferably, this method it comprise the following steps：
A, shiny copper foil is chosen, is cut by used vacuum magnetron sputtering coating film equipment stowing dimensions；
B, the Si cathode targets of vacuum magnetron sputtering coating film equipment are set to splash Si cathode targets with the installation site of C cathode targets
The C plasma doping sputters for Si plasmas and C the cathode targets sputtering penetrated realize that 1/2 volume is overlapping；
Vacuum magnetic control sputtering process condition is set c,；
D, in vacuum environment, vacuum direct magnetic control sputter mixes plating C-Si films, makes Si plasmas and C plasma dopings simultaneously
Reach 200-500nm thickness；
E, vacuum bag is sealed up for safekeeping after the copper foil after plated film is dried in vacuum drying chamber；
Preferably, vacuum splashing and plating process conditions are in the step c：Background vacuum 5x10 is set-3Pa, it is filled with high-purity argon
Gas is until sputter working vacuum degree reaches 3x10-1Pa。
Preferably, it is 6kw-9kw that C cathode targets power bracket is set in the step d, sets Si negative electrode target power outputs 1kw-
4kw, the component ratio of C plasmas and Si plasmas is controlled 1:3.
Preferably, the spacing in the step b between Si cathode targets and C cathode targets is arranged to 10mm.
Preferably, step e includes：Vacuum bag seals after copper foil after plated film dries 2h in 40-60 DEG C of vacuum drying chamber
Deposit.
Preferably, carry out to comprise the following steps before step a：The copper foil of lithium battery colelctor electrode is passed through into NaOH
Or HCl etc. acid or alkaline substance solution infiltration and stop the regular hour, reuse clear water by its remained on surface acid or
Person is that alkali cleans up, finally by drying.
Preferably, the plasma vacuum magnetic-controlled sputtering coating equipment is that Taiwan production MS-700/In-Line vacuum magnetic controls splash
Penetrate system.
Preferably, the thickness for choosing shiny copper foil is 8-12um, selects shiny copper foil to cut into by described
600mmX250mm magnitude units are loaded into MS-700/In-Line vacuum magnetic-control sputtering systems.
Preferably, high annealing can also be carried out to the copper foil of plated film in vacuum environment after the step d.
After the above method, the preferred embodiment of the invention has the beneficial effect that：
1st, using existing vacuum magnetron sputtering coating film experimental facilities, realize that doping sputtering prepares C-Si laminated films.
2nd, using the control to cathodic sputtering power, realize doping ratio and flexibly can adjust.
3rd, vacuum environment high temperature is annealed, and improves the crystallinity of material.
4th, so that the negative plate of the material lithium battery such as LiFePO4, lithium titanate caking property of film surface and paper tinsel in manufacturing process
Big embankment is high.Solves the problem that current LiFePO 4 and lithium titanate run into dry linting in actual production.
Figure of description
The present invention is further illustrated below in conjunction with the accompanying drawings.
Fig. 1 is vacuum magnetic control sputter C-Si film layer schematic diagrams；
Fig. 2 is that MS-700/In-Line vacuum magnetron sputtering coating film systems mix sputter C-Si film schematic diagrames；
Fig. 3 is the top layer condition diagram of copper foil before plasma surface pre-treatment；
Fig. 4 is the top layer condition diagram of copper foil after plasma surface pre-treatment.
Embodiment
Below in conjunction with embodiment of the present invention, the technology in embodiment of the present invention is clearly and completely described,
Obviously, described embodiment only a part of scheme of the present invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment party that those of ordinary skill in the art are obtained under the premise of creative work is not made
Case, belong to the scope of protection of the invention.
In the description of the invention, it is to be understood that term " " center ", " longitudinal direction ", " transverse direction ", " length ", " width ",
" thickness ", " on ", " under ", "front", "rear", "left", "right", " vertical ", " level ", " top ", " bottom " " interior ", " outer ", " up time
The orientation or position relationship of the instruction such as pin ", " counterclockwise " are based on orientation shown in the drawings or position relationship, are for only for ease of
Description is of the invention to be described with simplified, rather than the device or element of instruction or hint meaning must be with specific orientation, Yi Te
Fixed azimuth configuration and operation, therefore be not considered as limiting the invention.
In addition, term " first ", " second " are only used for describing purpose, and it is not intended that instruction or hint relative importance
Or the implicit quantity for indicating indicated technical characteristic.Thus, define " first ", the feature of " second " can be expressed or
Implicitly include one or more this feature.In the description of the invention, " multiple " are meant that two or more,
Unless otherwise specifically defined.
In the present invention, unless otherwise clearly defined and limited, term " installation ", " connected ", " connection ", " fixation " etc.
Term should be interpreted broadly, for example, it may be being fixedly connected or being detachably connected, or be integrally connected；It can be machine
Tool connects or electrical connection；Can be joined directly together, can also be indirectly connected by intermediary, can be two members
Connection inside part.For the ordinary skill in the art, above-mentioned term can be understood in this hair as the case may be
Concrete meaning in bright.
In the present invention, unless otherwise clearly defined and limited, fisrt feature second feature it " on " or it " under "
Can directly it be contacted including the first and second features, it is not directly to contact but pass through it that can also include the first and second features
Between other characterisation contact.Moreover, fisrt feature second feature " on ", " top " and " above " to include first special
Sign is directly over second feature and oblique upper, or is merely representative of fisrt feature level height and is higher than second feature.Fisrt feature exists
Second feature " under ", " lower section " and " following " fisrt feature that includes are immediately below second feature and obliquely downward, or be merely representative of
Fisrt feature level height is less than second feature.
The present invention needs the sputter C-Si composite membranes on cathode of lithium battery copper foil of affluxion body.
In order to realize above-mentioned purpose, the present invention is using Taiwan production MS-700/In-Line vacuum magnetic-control sputtering systems.
As the preferred embodiment of the present invention, the sputter C-Si composite membranes on cathode of lithium battery copper foil of affluxion body the step of
It is as follows：
A, shiny copper foil is chosen, is cut by used vacuum magnetron sputtering coating film equipment stowing dimensions, specifically,
The thickness for choosing shiny copper foil is 8-12um, selects shiny copper foil to cut into 600mmX250mm magnitude units loading by described
In in MS-700/In-Line vacuum magnetic-control sputtering systems；
B, the Si cathode targets of vacuum magnetron sputtering coating film equipment are set to splash Si cathode targets with the installation site of C cathode targets
The C plasma doping sputters for Si plasmas and C the cathode targets sputtering penetrated realize that 1/2 volume is overlapping, specifically, are specifically designed peace
Dress MS-700/In-Line vacuum magnetic controls splash adjacent 2 magnetron sputtering cathode target position of system, make C cathode targets and Si cathode targets
Body is close to greatest extent, until 2 target plasma volume laps reach 1/2, Si cathode targets and C negative electrodes in the present embodiment
Spacing between target is arranged to 10mm, respectively by C cathode targets and Si cathode targets on C cathode targets and Si cathode targets；
Vacuum magnetic control sputtering process condition is set, and specifically, operation MS-700/In-Line vacuum magnetic controls splash system, take out c,
Vacuum to system background vacuum is taken to reach 5x10-3Gas mass flow gauge is opened after Pa and is filled with high-purity argon gas, until system is true
Reciprocal of duty cycle reaches 3x10-1Pa；
D, in above-mentioned vacuum environment, vacuum direct magnetic control sputter mixes plating C-Si films, makes Si plasmas and C plasmas
Sputter is adulterated, specifically, operation MS-700/In-Line vacuum magnetic controls splash the C cathode targets of system respectively and Si cathode target direct currents splash
Radio source, set C negative electrodes target power output to be adjusted in 6kw-9kw, setting Si negative electrodes target power output in 1kw-4kw, repetition experiment, control C-
The component ratio of C and Si in Si plated films are 1：3, make C-Si film deposition thickness 200-500nm；
E, vacuum bag is sealed up for safekeeping after the copper foil after plated film is dried in vacuum drying chamber, and specifically, the copper foil after plated film is in 40-
Vacuum bag is sealed up for safekeeping after drying 2h in 60 DEG C of vacuum drying chamber.
As other embodiments of the present invention, can also comprise the following steps before step a：By lithium battery current collection
The copper foil of pole passes through the infiltration of the acid such as NaOH or HCl or alkaline substance solution and stopped the regular hour, reuses clear water
The acid either alkali of its remained on surface is cleaned up, finally by drying.With reference to shown in figure 3 and Fig. 4, the step for process,
Can be that copper foil surface reaches preferable sputtering conditions.
, can also be in vacuum environment to the copper foil of plated film after the step d as other embodiments of the present invention
High annealing is carried out, improves the crystallinity of material.
In order to ensure to will not fall off coated in the negative material on electrolytic copper foil, suitable bonding can be also added in the preparation
Agent, binding agent PVDF, PTFE, SBR, LA133 etc., its adhesion strength depend not only on the physical chemistry of adhesive in itself
Can, and have much relations with the surface characteristic of copper foil.When the adhesion strength of coating is sufficiently high, charge and discharge cycles process can be prevented
The powder of detached of middle negative pole, or substrate is peeled off because of excessive dilation, reduce circulation volume conservation rate.Conversely, when bond
Intensity does not reach requirement, then with the increase of cycle-index, makes the anti-constantly increase of the internal resistance of cell because coating stripping degree aggravates,
Circulation volume declines aggravation.
In the description of this specification, reference term " embodiment ", " some embodiments ", " an implementation
The description of example ", " some embodiments ", " example ", " specific example " or " some examples " etc. means to combine the embodiment or example
Specific features, structure, material or the feature of description are contained at least one embodiment or example of the present invention.In this explanation
In book, identical embodiment or example are not necessarily referring to the schematic representation of above-mentioned term.Moreover, the specific spy of description
Sign, structure, material or feature can combine in an appropriate manner in any one or more embodiments or example.
Above content is to combine specific embodiment further description made for the present invention, it is impossible to assert this hair
Bright specific implementation is confined to these explanations.For general technical staff of the technical field of the invention, do not taking off
On the premise of from present inventive concept, some simple deduction or replace can also be made.
Claims (10)
1. the method for lithium battery C-Si negative pole coatings is prepared using vacuum magnetron sputtering coating film technology, it is characterised in that utilize etc. from
Sub- vacuum magnetron sputtering coating film equipment sputters on the copper foil of lithium battery colelctor electrode prepares C-Si laminated films.
2. the side according to claim 1 that lithium battery C-Si negative pole coatings are prepared using vacuum magnetron sputtering coating film technology
Method, it is characterised in that it comprises the following steps：
A, shiny copper foil is chosen, is cut by used vacuum magnetron sputtering coating film equipment stowing dimensions；
B, the Si cathode targets of vacuum magnetron sputtering coating film equipment are set to make what Si cathode targets sputtered with the installation site of C cathode targets
Si plasmas and the C plasma doping sputters of C cathode targets sputtering realize that 1/2 volume is overlapping；
Vacuum magnetic control sputtering process condition is set c,；
D, in vacuum environment, vacuum direct magnetic control sputter mixes plating C-Si films, makes Si plasmas and C plasma dopings and reaches
200-500nm thickness；
E, vacuum bag is sealed up for safekeeping after the copper foil after plated film is dried in vacuum drying chamber.
3. the side according to claim 2 that lithium battery C-Si negative pole coatings are prepared using vacuum magnetron sputtering coating film technology
Method, it is characterised in that vacuum splashing and plating process conditions are in the step c：Background vacuum 5x10 is set-3Pa, it is filled with high-purity argon gas
Until sputter working vacuum degree reaches 3x10-1Pa。
4. the side according to claim 2 that lithium battery C-Si negative pole coatings are prepared using vacuum magnetron sputtering coating film technology
Method, it is characterised in that it is 6kw-9kw that C cathode targets power bracket is set in the step d, sets Si negative electrode target power outputs 1kw-
4kw, the component ratio of C plasmas and Si plasmas is controlled 1:3.
5. the side according to claim 2 that lithium battery C-Si negative pole coatings are prepared using vacuum magnetron sputtering coating film technology
Method, it is characterised in that the spacing in the step b between Si cathode targets and C cathode targets is arranged to 10mm.
6. the side according to claim 2 that lithium battery C-Si negative pole coatings are prepared using vacuum magnetron sputtering coating film technology
Method, it is characterised in that step e includes：Vacuum bag is sealed up for safekeeping after copper foil after plated film dries 2h in 40-60 DEG C of vacuum drying chamber.
7. the side according to claim 2 that lithium battery C-Si negative pole coatings are prepared using vacuum magnetron sputtering coating film technology
Method, it is characterised in that can also be comprised the following steps before step a：By the copper foil of lithium battery colelctor electrode by NaOH or
HCl etc. acid or alkaline substance solution infiltration simultaneously stop the regular hour, reuse clear water by its remained on surface acid or
It is that alkali cleans up, finally by drying.
8. prepare the painting of lithium battery C-Si negative poles using vacuum magnetron sputtering coating film technology according to claim any one of 1-7
The method of layer, it is characterised in that the plasma vacuum magnetic-controlled sputtering coating equipment is that MS-700/In-Line Vacuum Magnetics are produced in Taiwan
Control sputtering system.
9. the side according to claim 8 that lithium battery C-Si negative pole coatings are prepared using vacuum magnetron sputtering coating film technology
Method, it is characterised in that the thickness for choosing shiny copper foil is 8-12um, selects shiny copper foil to cut into 600mmX250mm by described
Magnitude unit is loaded into MS-700/In-Line vacuum magnetic-control sputtering systems.
10. the side according to claim 2 that lithium battery C-Si negative pole coatings are prepared using vacuum magnetron sputtering coating film technology
Method, it is characterised in that high annealing can also be carried out to the copper foil of plated film in vacuum environment after the step d.
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| CN2016106309268 | 2016-08-04 | ||
| CN201610630926.8A CN106119795A (en) | 2016-08-04 | 2016-08-04 | Utilize the method that vacuum magnetron sputtering coating film technology prepares lithium battery C Si negative pole coating |
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| CN201710656804.0A Pending CN107482160A (en) | 2016-08-04 | 2017-08-03 | The method that lithium battery C Si negative pole coatings are prepared using vacuum magnetron sputtering coating film technology |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108390017A (en) * | 2018-01-31 | 2018-08-10 | 电子科技大学 | A kind of lithium metal composite negative pole preparation facilities based on principle of magnetron-sputtering |
| CN108565394A (en) * | 2018-04-12 | 2018-09-21 | 太原科技大学 | The method for preparing lithium-sulphur cell positive electrode piece using magnetron sputtering technique |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113410445A (en) * | 2021-06-18 | 2021-09-17 | 电子科技大学 | Silicon-carbon composite negative electrode material for secondary battery and preparation method thereof |
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| CN101640261A (en) * | 2008-08-01 | 2010-02-03 | 中信国安盟固利新能源科技有限公司 | Cathode of lithium-ion secondary battery, preparation method and lithium-ion secondary battery |
| CN102709531A (en) * | 2012-01-09 | 2012-10-03 | 宁德新能源科技有限公司 | Lithium ion battery and cathode thereof |
| CN103222091A (en) * | 2010-11-26 | 2013-07-24 | 日产自动车株式会社 | Si alloy-containing negative electrode active material for electrical devices |
| CN103474632A (en) * | 2012-06-07 | 2013-12-25 | 中国科学院物理研究所 | Negative electrode material used for lithium battery and preparation method and application thereof |
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2016
- 2016-08-04 CN CN201610630926.8A patent/CN106119795A/en active Pending
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2017
- 2017-08-03 CN CN201710656804.0A patent/CN107482160A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101640261A (en) * | 2008-08-01 | 2010-02-03 | 中信国安盟固利新能源科技有限公司 | Cathode of lithium-ion secondary battery, preparation method and lithium-ion secondary battery |
| CN103222091A (en) * | 2010-11-26 | 2013-07-24 | 日产自动车株式会社 | Si alloy-containing negative electrode active material for electrical devices |
| CN102709531A (en) * | 2012-01-09 | 2012-10-03 | 宁德新能源科技有限公司 | Lithium ion battery and cathode thereof |
| CN103474632A (en) * | 2012-06-07 | 2013-12-25 | 中国科学院物理研究所 | Negative electrode material used for lithium battery and preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108390017A (en) * | 2018-01-31 | 2018-08-10 | 电子科技大学 | A kind of lithium metal composite negative pole preparation facilities based on principle of magnetron-sputtering |
| CN108565394A (en) * | 2018-04-12 | 2018-09-21 | 太原科技大学 | The method for preparing lithium-sulphur cell positive electrode piece using magnetron sputtering technique |
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