CN109628888A - Battery material coating control method and computer readable storage medium - Google Patents
Battery material coating control method and computer readable storage medium Download PDFInfo
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- CN109628888A CN109628888A CN201811620343.2A CN201811620343A CN109628888A CN 109628888 A CN109628888 A CN 109628888A CN 201811620343 A CN201811620343 A CN 201811620343A CN 109628888 A CN109628888 A CN 109628888A
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- baffle
- battery material
- target
- control method
- bombardment
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- 239000000463 material Substances 0.000 title claims abstract description 107
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000011248 coating agent Substances 0.000 title claims abstract description 25
- 238000000576 coating method Methods 0.000 title claims abstract description 25
- 238000003860 storage Methods 0.000 title claims abstract description 11
- 238000013519 translation Methods 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 238000006073 displacement reaction Methods 0.000 claims description 8
- 238000005566 electron beam evaporation Methods 0.000 claims description 5
- 238000007747 plating Methods 0.000 claims description 4
- 230000005611 electricity Effects 0.000 claims description 2
- 239000000523 sample Substances 0.000 claims 4
- 239000013068 control sample Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 5
- 239000010408 film Substances 0.000 description 59
- 239000000758 substrate Substances 0.000 description 20
- 238000012360 testing method Methods 0.000 description 10
- 238000000151 deposition Methods 0.000 description 8
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 7
- 230000008021 deposition Effects 0.000 description 7
- 229910052744 lithium Inorganic materials 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 239000007772 electrode material Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 230000033001 locomotion Effects 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910000420 cerium oxide Inorganic materials 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000001451 molecular beam epitaxy Methods 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical group [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000004549 pulsed laser deposition Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- 229910012925 LiCoO3 Inorganic materials 0.000 description 1
- 229910013292 LiNiO Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- 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
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
-
- 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
- C23C14/08—Oxides
-
- 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
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
-
- 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
-
- 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
- C23C14/54—Controlling or regulating the coating process
- C23C14/548—Controlling the composition
-
- 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
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
-
- 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)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention discloses a kind of battery material coating control method and a kind of computer readable storage medium, wherein the control method includes: a: opening the first battery material on the target bombardment device bombardment target placing device;B: during the baffle is moved to predeterminated position along first direction by initial position, the target bombardment device is closed;C: when the baffle is moved to the predeterminated position, the second battery material on the target bombardment device bombardment target placing device is opened;D: the baffle is controlled along first direction or second direction translation L1.Technical solution of the present invention can effectively be deposited together two kinds of battery materials, obtain the variation that heterogeneity matches from low to high of two kinds of materials, only need once to prepare the battery material intermediate, the preparation efficiency of optimal components ratio namely qualified battery material intermediate that two kinds of materials can be found from the battery material intermediate greatly promotes.
Description
Technical field
The present invention relates to battery technology fields, in particular to battery material coating control method and computer-readable storage medium
Matter.
Background technique
Currently used all solid-state thin-film lithium battery, battery material are all to use the deposition of film plating process in layer up
's.But the film prepared is exactly the uniform ingredient of material.Typically for the research and development of electrode film material itself, need
Different material mixing is attempted, the ingredient of material is different, the different combination of ratio.Such trial is according to existing method
It is very time-consuming with equipment, inefficiency.
For existing all solid-state thin-film lithium battery, the battery material of film is typically all cobalt acid lithium (LiCoO3), or now
Popular ternary material (LiMnNiCoOx).But if we will further research and develop new battery material, for example taste
Try the combination between different battery material ingredients, different ratios develops new material system with this, it is necessary to different
Material composition is tested according to different ratios.
For example we want the material system that LiMn2O4 (LiMnOx) and lithium nickelate (LiNiOx) combination and exploitation is new.According to
Then existing conventional method (or first deposits together it is necessary to deposit the film of LiMnOx in deposition LiNiOx film combinations
LiNiOx film, the film of redeposited LiMnOx), after depositing this good mixed film (battery material test intermediate), then come
The performance of test material.But once such two kinds of films are deposited, their chemical component and ratio be it is fixed, can not
Variation.If attempting new proportion, that just needs to deposit such two kinds of film mixtures again, then to test its property
Energy.It is only in this way repeated as many times, does the preparation of multiple deposition and sample, be likely to find optimal ingredient ratio, it can be seen that,
Existing film plating process efficiency is extremely low.
Summary of the invention
The main object of the present invention is to provide a kind of battery material coating control method, it is intended to solve existing film plating process effect
The low problem of rate.
To achieve the above object, battery material coating control method proposed by the present invention, to control battery material plated film
Equipment plated film, the battery material filming equipment include shell, target bombardment device, target placing device, sample stage and setting
Baffle between the sample stage and the target placing device, the target placing device, sample stage and the baffle are set
It is placed in the shell, the control method includes the following steps:
A: the first battery material on the target bombardment device bombardment target placing device is opened;
B: it during the baffle is moved to predeterminated position along first direction by initial position, closes the target and bangs
Hit device;
C: when the baffle is moved to the predeterminated position, the target bombardment device bombardment target placing device is opened
On the second battery material;
D: the baffle is controlled along first direction or second direction translation L1;
Wherein, when closing the target bombardment device, the baffle is L along first direction displacement1, the baffle exists
Width on the first direction is L0, L1≤L0;The baffle is moved to the position when predeterminated position by the initial position
Shifting amount is S;
In step d, when the baffle translates L along first direction1When, S=L0;When the baffle translates in a second direction
L1When, S=L0+L1, the first direction is opposite with the second direction.
In one embodiment, in the step d, baffle translates in a second direction, and the step b includes:
B1: the baffle is controlled along first direction and translates L1After stop;
B2: in the preset time when the baffle stops or after stopping, the target bombardment device is closed;
B3: it after closing the target bombardment device, controls the baffle and continues to be moved to the predeterminated position.
In one embodiment, control the first battery material on target bombardment device bombardment target placing device it
Before further include step s1: control the sample stage and be heated to 450 DEG C~550 DEG C;It further include step between step s1 and step a
S2: it controls the sample stage and is heated to 600 DEG C~700 DEG C.
In one embodiment, the battery material filming equipment further includes vacuum source, between step s1 and step s2, also
Including step s3: controlling the vacuum source and vacuumized to the shell, so that vacuum degree reaches 10-8~10-10torr。
In one embodiment, the battery material filming equipment further includes source of oxygen, between step s2 and step s3 also
Including injecting oxygen in s4: Xiang Suoshu shell of step, so that oxygen pneumatic reaches 0.1~100mTorr in the shell.
In one embodiment, the baffle translates L along the first direction by initial position1Rate travel be V1, described
Baffle translates L by the predeterminated position in a second direction1Rate travel be V2, V1And V2It is uniform and equal.
In one embodiment, V1And V2It is 10-5M/s~10-4m/s。
In one embodiment, L0≥1.5L1。
In one embodiment, the target bombardment device is pulsed laser source, sputter gas source or electron beam evaporation rifle.
The present invention also provides a kind of computer readable storage medium, plated film is stored on the computer readable storage medium
Processing routine, the coating film treatment program realize following steps when being executed by processor:
A: the first battery material on the target bombardment device bombardment target placing device is opened;
B: it during the baffle is moved to predeterminated position along first direction by initial position, closes the target and bangs
Hit device;
C: when the baffle is moved to the predeterminated position, the target bombardment device bombardment target placing device is opened
On the second battery material;
D: the baffle is controlled along first direction or second direction translation L1;
Wherein, when closing the target bombardment device, the baffle is L along first direction displacement1, the baffle exists
Width on the first direction is L0, L1≤L0;The baffle is moved to the position when predeterminated position by the initial position
Shifting amount is S;
In step d, when the baffle translates L along first direction1When, S=L0;When the baffle translates in a second direction
L1When, S=L0+L1, the first direction is opposite with the second direction.
Technical solution of the present invention can effectively be deposited together two kinds of battery materials, obtain two kinds of materials from as low as
The variation of high heterogeneity proportion can be quickly found out the optimum proportioning of two kinds of battery materials, also when carrying out electrode test
It is only to need once to prepare the battery material intermediate, preferably matching for two kinds of materials can be found from the battery material intermediate
Than namely the preparation efficiency of qualified battery material intermediate greatly promote.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
The structure shown according to these attached drawings obtains other attached drawings.
Fig. 1 is the structural schematic diagram for implementing the electrode material filming equipment of control method of the present invention;
Fig. 2 has plated state diagram when first electrode layer for electrode material filming equipment in Fig. 1;
Fig. 3 is moved to state diagram when predeterminated position for baffle in Fig. 2;
Fig. 4 is state diagram when electrode material filming equipment has plated the second electrode lay;
Fig. 5 is the flow chart of one embodiment of electrode material coating control method of the present invention;
Fig. 6 is the flow chart of another embodiment of electrode material coating control method of the present invention;
Fig. 7 is the flow chart of the another embodiment of electrode material coating control method of the present invention;
Fig. 8 is the structural schematic diagram that battery material tests intermediate;
Fig. 9 is the position corresponding diagram of per distribution ratio and two electrode points shared by the second electrode lay in two electrode layers in Fig. 8.
Drawing reference numeral explanation:
The embodiments will be further described with reference to the accompanying drawings for the realization, the function and the advantages of the object of the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiment is only a part of the embodiments of the present invention, instead of all the embodiments.Base
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts it is all its
His embodiment, shall fall within the protection scope of the present invention.
It is to be appreciated that the directional instruction (such as up, down, left, right, before and after ...) of institute is only used in the embodiment of the present invention
In explaining in relative positional relationship, the motion conditions etc. under a certain particular pose (as shown in the picture) between each component, if should
When particular pose changes, then directionality instruction also correspondingly changes correspondingly.
In addition, the description for being related to " first ", " second " etc. in the present invention is used for description purposes only, and should not be understood as referring to
Show or imply its relative importance or implicitly indicates the quantity of indicated technical characteristic." first ", " are defined as a result,
Two " feature can explicitly or implicitly include at least one of the features.In addition, the technical solution between each embodiment can
It to be combined with each other, but must be based on can be realized by those of ordinary skill in the art, when the combination of technical solution occurs
Conflicting or cannot achieve when, will be understood that the combination of this technical solution is not present, also not the present invention claims protection model
Within enclosing.
The present invention proposes a kind of battery material coating control method and computer readable storage medium in fact, and following the description will
It is described in detail with specific embodiment combination Figure of description.
Referring to figs. 1 to Fig. 4, the present invention proposes a kind of battery material coating control method, to control battery material plated film
20 plated film of equipment, the battery material filming equipment 20 include shell, target bombardment device, target placing device 23, sample stage
29 and the baffle 24 that is set between the sample stage 29 and the target placing device 23, the target placing device 23, sample
Sample platform 29 and the baffle 24 are set in the shell.
Specifically, target placing device 23 is for putting battery material in shell 21, it usually needs place two
Kind of battery material, for all solid-state thin-film lithium battery system, the battery material of film can be lithium nickelate and LiMn2O4
Combination.For solid oxide fuel battery system, electrolyte is zirconium oxide and cerium oxide.Here, target is set
A kind of battery material can individually be put by putting device 23, when needing to use another battery material plated film, can be replaced manually
Another battery material.Certainly, target placing device 23 can be with two or more target putting positions, and two targets are set
It puts on position while putting two kinds of battery materials;It is also possible to there are two target placing devices 23, on two target placing devices 23
It can respectively correspond and put two kinds of battery materials, which kind of battery material needed to use, sputter process can be carried out to which kind of material.
Since when carrying out plated film, battery material is sputtered downwards, the battery material powder sputtered downwards be easy by
Interference in air flow here, shell 21 mainly provides a stable environment to the formation of internal membrane, such as avoids outer gas stream
It influences.
Sample stage 29 is mainly used for putting substrate 22, and the spacing between sample stage 29 and target placing device 23 exists
Between 50mm~100mm.For different films, the better substrate of more matching degree can be replaced according to the type of film
22.Such as all solid-state thin-film lithium battery system, SrTiOxThe crystal structure and LiNiO of oxidex、LiMnOxLattice
Structure is similar, and lattice structure is similar, and well, Lattice Matching is good, and film is not easy to fall off, and subsequent deposition comes out for the linking between film
Battery material film quality it is high.So can preferably guarantee to be mutually matched between the film lattice deposited in this way, substrate 22
Optimal selection be SrTiOx.But one side SrTiOxPrice costly, so, even with SrTiOxMake substrate 22,
Thickness is also required to be strictly controlled.On the other hand, SrTiOxIntensity be not so good as SiOx.The substrate 22 can be by SiOxWith
SrTiOxCombination, SrTiOxIt is plated on SiOxOn, substrate 22 is collectively formed.Again for example for solid oxide fuel battery system and
Speech, Al2O3Crystal structure it is similar with cerium oxide lattice structure with zirconium oxide, so can preferably guarantee in this way deposition film
It is mutually matched between lattice, the optimal selection of substrate 22 is Al2O3。
Spacing between sample stage 29 and baffle 24 needs to control between 0.1mm~10mm, this is because substrate 22 compared with
Thin, film is also relatively thin, usually Nano grade, if the spacing between sample stage 29 and baffle 24 is less than normal, during fabrication, needs
Want the spacing between strict control baffle 24 and sample stage 29.Because baffle 24 in moving process, may touch substrate
22 or sample stage 29, so it is difficult to form film.If the spacing between sample stage 29 and baffle 24 is bigger than normal, in plated film
When, the line of demarcation fuzzy of film, film forming effect is also bad, may finally will affect test result.Based on this, in this reality
Apply in example, the spacing between sample stage 29 and baffle 24 can be 0.3mm, 0.5mm, 0.8mm, 1mm, 1.2mm, 1.5mm,
1.6mm、1.8mm、2.0mm、2.2mm、2.4mm、2.5mm、2.8mm、3.0mm、3.2mm、3.5mm、3.6mm、3.8mm、
4.0mm, 4.2mm, 4.5mm, 4.8mm, 5.0mm, 6mm, 7mm, 8mm, 9mm etc. are possible.
Following the description will describe control method in detail, please refer to Fig. 5:
A: the first battery material on the target bombardment device bombardment target placing device 23 is opened, is to pass through target herein
Material bombards device and bombards target, sputters target downwards.
B: during the baffle 24 is moved to predeterminated position along first direction by initial position, the target is closed
Bombard device.Baffle 24 is displaced in a first direction, and target bombardment device is interrupted during displacement to the first battery material
Bombardment, so that target is not re-directed towards the sputtering of substrate 22, the first battery material deposits on substrate 22 and forms first electrode layer at this time
11。
C: it when the baffle 24 is moved to the predeterminated position, opens the target bombardment device bombardment target and puts dress
Set the second battery material on 23.When closing target bombardment device the first battery material of bombardment, baffle 24 can be off pre-
If the time, because there is also a small amount of in the space of 24 top of baffle when closing target bombardment device the first battery material of bombardment
The target powder that will be deposited, control baffle 24 is out of service at this time, and 11 boundary of first electrode layer plated can be made clearly more demarcated,
To reduce the later period to the evaluated error of resistance.
D: the baffle 24 is controlled along first direction or second direction translation L1.Here, the moving direction of baffle 24 is can
With selection.Define first direction be from left to right, the predeterminated position of baffle 24 can there are two, one is when a left side for baffle 24
The position of baffle 24 when end and the flush left of film;The other is the baffle when the flush right of the left end of baffle 24 and film
24 position.It should be noted that the left side of film is the left side for referring to the wedge-like portion (left low and right high) of film, the right side of film
While being the right for referring to the wedge-like portion of film.
It is illustrated respectively below for two kinds of situations.
When the baffle 24 translates L along first direction1When, with the proviso that the left end of baffle 24 is concordant with the left side of film.
Namely when closing the target bombardment device, the baffle 24 is L along first direction displacement1, the baffle 24 is in institute
Stating the width on first direction is L0, L1≤L0;The baffle 24 is moved to the position when predeterminated position by the initial position
Shifting amount is S, S=L0。
When the baffle 24 translates L in a second direction1When, with the proviso that the left end of baffle 24 is concordant with the right of film.
Namely when closing the target bombardment device, the baffle 24 is L along first direction displacement1, the baffle 24 is in institute
Stating the width on first direction is L0, L1≤L0;The baffle 24 is moved to the position when predeterminated position by the initial position
Shifting amount is S, S=L0+L1, the first direction is opposite with the second direction.
Fig. 8 and Fig. 9 are please referred to, after having plated to first electrode layer 11 and the second electrode lay 12, battery material test is intermediate
Body 10 is formed, and battery material can be tested intermediate 10 and sealed in circuit.One electrode N1Connect first electrode layer 11
Lower surface, another electrode M1Connect the second electrode lay 12 upper surface (two electrodes be located at perpendicular to substrate 22 it is same always
On line), then repeatedly adjust the position (M of two electrodes2And N2、M3And N3、M4And N4、M5And N5、M6And N6), so as to obtain
Multiple groups resistance Value Data, by the proportion of available two battery material of multiple groups resistance Value Data and the relationship of resistance value, in turn
Optimum proportioning can therefrom be selected.
Referring to Fig. 9, M1And N1Corresponding the second electrode lay 12 occupies 100%, M of entire electrode layer specific gravity2And N2It is corresponding
The second electrode lay 12 occupy 95%, M of entire electrode layer specific gravity3And N3Corresponding the second electrode lay 12 occupies entire electrode layer
Specific gravity 85%, M4And N4Corresponding the second electrode lay 12 occupies 60%, M of entire electrode layer specific gravity5And N5Corresponding second electricity
Pole layer 12 occupies 40%, M of entire electrode layer specific gravity6And N6Corresponding the second electrode lay 12 occupies entire electrode layer specific gravity
0%.
Technical solution of the present invention can effectively be deposited together two kinds of battery materials, obtain two kinds of materials from as low as
The variation of high heterogeneity proportion can be quickly found out the optimum proportioning of two kinds of battery materials, also when carrying out electrode test
It is only to need once to prepare the battery material intermediate, preferably matching for two kinds of materials can be found from the battery material intermediate
Than namely the preparation efficiency of qualified battery material intermediate greatly promote.
Referring to Fig. 6, on the basis of a upper embodiment, in order to keep the boundary of film clearly more demarcated, in the present embodiment, institute
It states in step d, baffle 24 translates in a second direction, and the step b includes:
B1: the baffle 24 is controlled along first direction and translates L1After stop.
B2: in the preset time when the baffle 24 stops or after stopping, the target bombardment device is closed.
B3: it after closing the target bombardment device, controls the baffle 24 and continues to be moved to the predeterminated position.
Before plated film, there may be impurity on substrate 22, impurity has an impact to the molding of film, it is also possible to can direct shadow
The electric conductivity of film is rung, such as there are moisture content, organic matters etc. on substrate 22.In consideration of it, in the present embodiment, step a it
Before further include step s1: control the sample stage 29 and be heated to 450 DEG C~550 DEG C.Heating device 28 is provided in sample stage 29,
Substrate 22 is heated by heating device 28, so as to remove the impurity on substrate 22, and removes having for impurity on substrate 22
Effect temperature is usually required at 500 DEG C or so.In addition, film is formed in order to make battery material be easier to deposit, at this in plated film
Further include step s2 between step s1 and step a in embodiment: controlling the sample stage 29 and be heated to 600 DEG C~700 DEG C.
28 heating temperature of heating device is relatively low to be unfavorable for battery material (oxidation film) deposition.
Referring to Fig. 7, the gas flowing in shell 21 will affect the deposition position of battery material, to influence when plated film
The final shape of film.In consideration of it, in the present embodiment, the battery material filming equipment 20 further includes vacuum source 27, in step
Between rapid s1 and step s2, further includes step s3: controlling the vacuum source 27 and the shell is vacuumized, so that vacuum degree reaches
10-8~10-10torr.Here, in order to make in shell to there is preferable vacuum degree to need to make shell when vacuumizing object
Intracorporal vacuum degree is higher than 10-8Torr, such as 10-8torr、5×10-9torr、2×10-9torr、10-9torr。
For sull, need to keep certain oxygen pneumatic in shell.In the present embodiment, the battery material
Filming equipment 20 further includes source of oxygen 26, further includes that oxygen is injected in s3: Xiang Suoshu shell of step between step s2 and step a
Gas, so that oxygen pneumatic reaches 0.1~100mTorr in the shell, while vacuum degree will also reach 10-4~10-6torr。
Referring to Fig. 8, baffle 24 is V along the rate that first direction translates by initial position in plated film1, the baffle
24 translate L by the predeterminated position in a second direction1Rate travel be V2, the mobile rate of baffle 24 can always at the uniform velocity,
It is exactly V1And V2Can be always uniformly, the contact surface between the first electrode layer 11 being thusly-formed and the second electrode lay 12 is
Straight inclined-plane.Certainly, V1It can be and be gradually reduced from left to right, V2Right-to-left is gradually increased, final first electrode layer 11 with
Contact surface between the second electrode lay 12 is upward convex cambered surface.It can also be V1It is gradually increased from left to right, V2Right-to-left by
Decrescence small, the contact surface between final first electrode layer 11 and the second electrode lay 12 is to recessed cambered surface.It can also be baffle
24 move along first direction intermittence, same baffle 24 be also in a second direction it is intermittent mobile, in this way, first electrode layer 11 with
Contact surface between the second electrode lay 12 is step-like.
The baffle 24 translates L along the first direction by initial position1Rate travel be V1, the baffle 24 is by institute
It states predeterminated position and translates L in a second direction1Rate travel be V2, V1And V2It is uniform and equal.In this way, final first electrode layer
Straight inclined-plane can be formed between 11 and the second electrode lay 12,0% to 100% all changes can be covered by obtaining two kinds of materials
Change, it is only necessary to once prepare the battery material intermediate, the best of two kinds of materials can be found from the battery material intermediate
Proportion.
Since the thickness of film is nanoscale, so the movement speed control to baffle 24 is stringenter.Baffle 24 cannot
Movement is fast, and the movement speed of baffle 24 necessarily is in an extremely low state.In the present embodiment, V1And V2It is 10-5M/s~
10-4m/s。
Above content has addressed L0≥L1, in order to guarantee coating quality, L0It can not get too close to L1, this is because plated film
When there are diffraction phenomenas, if L0Close to L1, then when having plated first electrode layer 11, the left end boundary of first electrode layer 11
Fuzzy, when having plated the second electrode lay 12, when the second electrode lay 12, the right margin fuzzy of the second electrode lay 12, finally
Two endpoints that will lead to battery material test intermediate 10 are difficult to confirm, to be easy test inaccuracy.In the present embodiment,
L0≥1.5L1.Certainly, optimal, L0Also not than L1Big too many (being related to controlling precision problem), here, 1.5L1≤L0≤
3L0。
Target bombard device can there are many, target bombardment device is pulsed laser source, uses laser pulse heavy
The mode of product (Pulsed Laser Deposition, PLD), the pulsed laser source is installed on the shell 21, to bombard
Target.21 inside of shell is mounted in this pulsed laser source or outside is ok, and is placed on outside, low cost, because in this way
Vacuum chamber is with regard to small;Laser source itself is smaller, and so as to be placed on inside, however vacuum chamber must just be done greatly, and vacuum chamber one is big,
Cost will be higher.The target bombardment device is also possible to sputter gas source, and the sputter gas source is installed on the shell
It (because sputter gas source is the plasma gas for leading to argon gas toward vacuum chamber, can only be carried out in vacuum chamber) in 21, the sputtering
Gas source bombards target by plasma gas, that is, in such a way that Sputter is deposited.The target bombardment device may be used also
To be electron beam evaporation rifle, the electron beam evaporation rifle is installed in the shell 21, to bombard target, that is, use point
The mode of beamlet epitaxial growth (Molecular Beam Epitaxy, MBE).
For laser source, the wavelength of laser light source is 250nm~270nm, and laser energy is that each pulse is 1J/
cm2~3J/cm2, laser pulse frequency is about 5Hz~10Hz.After its unlatching, laser-impact target, fallen target starts
It is deposited on substrate 22, forms film.For sputter gas source, mainly pass through Ar+Impact target, fallen target
Material starts to deposit on substrate 22, forms film.For mainly being impacted by high-speed electron flow for electron beam evaporation rifle
Target, fallen target start to deposit on substrate 22, form film.
The present invention also provides a kind of computer readable storage medium, plated film is stored on the computer readable storage medium
Processing routine, the coating film treatment program realize following steps when being executed by processor:
A: the first battery material on the target bombardment device bombardment target placing device is opened;
B: it during the baffle is moved to predeterminated position along first direction by initial position, closes the target and bangs
Hit device;
C: when the baffle is moved to the predeterminated position, the target bombardment device bombardment target placing device is opened
On the second battery material;
D: the baffle is controlled along first direction or second direction translation L1;
Wherein, when closing the target bombardment device, the baffle is L along first direction displacement1, the baffle exists
Width on the first direction is L0, L1≤L0;The baffle is moved to the position when predeterminated position by the initial position
Shifting amount is S;
In step d, when the baffle translates L along first direction1When, S=L0;When the baffle translates in a second direction
L1When, S=L0+L1, the first direction is opposite with the second direction.
The above description is only a preferred embodiment of the present invention, is not intended to limit the scope of the invention, all at this
Under the inventive concept of invention, using equivalent structure transformation made by description of the invention and accompanying drawing content, or directly/use indirectly
It is included in other related technical areas in scope of patent protection of the invention.
Claims (10)
1. a kind of battery material coating control method, to control battery material filming equipment plated film, which is characterized in that the electricity
Pond material film plating equipment includes shell, target bombardment device, target placing device, sample stage and is set to the sample stage and institute
State the baffle between target placing device, the target placing device, sample stage and the baffle plate setting are in the shell, institute
Control method is stated to include the following steps:
A: the first battery material on the target bombardment device bombardment target placing device is opened;
B: during the baffle is moved to predeterminated position along first direction by initial position, the target bombardment dress is closed
It sets;
C: it when the baffle is moved to the predeterminated position, opens on the target bombardment device bombardment target placing device
Second battery material;
D: the baffle is controlled along first direction or second direction translation L1;
Wherein, when closing the target bombardment device, the baffle is L along first direction displacement1, the baffle is described
Width on first direction is L0, L1≤L0;The baffle is moved to the displacement when predeterminated position by the initial position
For S;
In step d, when the baffle translates L along first direction1When, S=L0;When the baffle translates L in a second direction1When,
S=L0+L1, the first direction is opposite with the second direction.
2. battery material coating control method as described in claim 1, which is characterized in that in the step d, baffle is along second
Direction translation, the step b include:
B1: the baffle is controlled along first direction and translates L1After stop;
B2: in the preset time when the baffle stops or after stopping, the target bombardment device is closed;
B3: it after closing the target bombardment device, controls the baffle and continues to be moved to the predeterminated position.
3. battery material coating control method as claimed in claim 2, which is characterized in that before step a further include step
S1: it controls the sample stage and is heated to 450 DEG C~550 DEG C;It further include step s2 between step s1 and step a: described in control
Sample stage is heated to 600 DEG C~700 DEG C.
4. battery material coating control method as claimed in claim 3, the battery material filming equipment further includes vacuum source,
It is characterized in that, further including step s3 between step s1 and step s2: it controls the vacuum source and the shell is vacuumized,
So that vacuum degree reaches 10-8~10-10torr。
5. battery material coating control method as claimed in claim 4, the battery material filming equipment further includes source of oxygen,
It is characterized in that, further including injecting oxygen in s4: Xiang Suoshu shell of step between step s2 and step s3, so that the shell
Interior oxygen pneumatic reaches 0.1~100mTorr.
6. the battery material coating control method as described in claim 1 to 5 any one, which is characterized in that the baffle by
Initial position translates L along the first direction1Rate travel be V1, the baffle put down in a second direction by the predeterminated position
Move L1Rate travel be V2, V1And V2It is uniform and equal.
7. battery material coating control method as claimed in claim 6, which is characterized in that V1And V2It is 10-5M/s~10-4m/
s。
8. battery material coating control method as claimed in any one of claims 1 to 7, which is characterized in that L0≥1.5L1。
9. the battery material coating control method as described in claim 1 to 5 any one, which is characterized in that the target bangs
Hitting device is pulsed laser source, sputter gas source or electron beam evaporation rifle.
10. a kind of computer readable storage medium, which is characterized in that be stored at plated film on the computer readable storage medium
Program is managed, the battery material as described in any one of claims 1 to 5 is realized when the coating film treatment program is executed by processor
The step of coating control method.
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JPS5970774A (en) * | 1982-10-18 | 1984-04-21 | Matsushita Electric Ind Co Ltd | Vapor deposition device |
JPH0317267A (en) * | 1989-06-14 | 1991-01-25 | Sanyo Electric Co Ltd | Production of gradient functional material |
CN1869281A (en) * | 2005-05-24 | 2006-11-29 | 鸿富锦精密工业(深圳)有限公司 | Film coating equipment and its film coating method |
CN101487113A (en) * | 2009-02-16 | 2009-07-22 | 大连理工大学 | Preparation of mask locating continuous component spreading thin film warehouse |
CN102191469A (en) * | 2011-04-25 | 2011-09-21 | 东莞市康达机电工程有限公司 | Auxiliary coating device for film product development and coating method thereof |
CN207596952U (en) * | 2017-12-19 | 2018-07-10 | 成都亦道科技合伙企业(有限合伙) | A kind of polynary magnetic control sputtering device and the equipment for preparing electrode |
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JPS5970774A (en) * | 1982-10-18 | 1984-04-21 | Matsushita Electric Ind Co Ltd | Vapor deposition device |
JPH0317267A (en) * | 1989-06-14 | 1991-01-25 | Sanyo Electric Co Ltd | Production of gradient functional material |
CN1869281A (en) * | 2005-05-24 | 2006-11-29 | 鸿富锦精密工业(深圳)有限公司 | Film coating equipment and its film coating method |
CN101487113A (en) * | 2009-02-16 | 2009-07-22 | 大连理工大学 | Preparation of mask locating continuous component spreading thin film warehouse |
CN102191469A (en) * | 2011-04-25 | 2011-09-21 | 东莞市康达机电工程有限公司 | Auxiliary coating device for film product development and coating method thereof |
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