CN110438449A - A kind of cobalt acid lithium composite film electrode and preparation method thereof - Google Patents
A kind of cobalt acid lithium composite film electrode and preparation method thereof Download PDFInfo
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- CN110438449A CN110438449A CN201910792313.8A CN201910792313A CN110438449A CN 110438449 A CN110438449 A CN 110438449A CN 201910792313 A CN201910792313 A CN 201910792313A CN 110438449 A CN110438449 A CN 110438449A
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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
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- 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
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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
- C23C14/08—Oxides
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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
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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- 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
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
The invention discloses a kind of cobalt acid lithium composite film electrodes and preparation method thereof.Cobalt acid lithium target is sputtered simultaneously using More target sputtering together technology and aluminium target prepares the cobalt acid lithium composite film electrode of aluminium doping vario-property, regulate and control the ingredient and structure of laminated film by adjusting sputtering parameter and the target material composition of cobalt acid lithium target and aluminium target, to realize the preparation of high-performance cobalt acid lithium composite film electrode.The present invention has preparation process simply easily controllable, and metallic aluminium forms conductive network in the film, dramatically increases its electric conductivity, and part aluminium can enter cobalt acid lithium lattice during cosputtering, forms LiAlyCo1‑yO2On the one hand the presence of solid solution, the solid solution can promote transporting for lithium ion, on the other hand will improve the beneficial effect of electrode cycle stability.
Description
Technical field
The present invention relates to a kind of cobalt acid lithium electrode, especially a kind of cobalt acid lithium composite film electrode and preparation method thereof.
Background technique
Solid-State Thin Film Li-Ion Batteries due to it is high with energy density, have a safety feature, have extended cycle life, structure can be set
The advantages that meter property is good while compatible microelectronic technique, it is considered to be one of ideal source of microelectronic product.Membrane electrode is
Determine the key factor of solid-State Thin Film Li-Ion Batteries energy density and cycle performance.In numerous developed positive electrodes
In, LiCoO2Easily prepared film forming, and open-circuit voltage with higher and specific capacity can guarantee that the higher energy of membrane electrode is close
Degree, it is considered to be one of ideal film anode.But due in membrane electrode without conductive additive, when film increases to certain thickness
Its electronics and lithium ion conductive are limited to when spending, performance will decline.
Composite film electrode is prepared, can be solved to a certain extent using the compound raising electrodes conduct ability of conductive material
State problem.Such as existing research (J.S. Wook, S.M. Lee. LiCoO2/Ag multilayer film cathodes for
thin-film rechargeable lithium batteries[J]. J. Electrochem. Soc., 2007, 154
(1): A22-A25. LiCoO) is prepared for using magnetron sputtering method2/Ag/ LiCoO2/Ag/LiCoO2Multilayer films, due to
The presence of Ag improves thin film electronic electric conductivity, which is substantially better than LiCoO2Film.But it is parallel to electricity
The Ag layer of pole surface can hinder transporting for lithium ion to a certain extent, and Ag is that precious metal is unfavorable for electrode energy density
It is promoted.
Summary of the invention
The object of the present invention is to provide a kind of cobalt acid lithium composite film electrodes and preparation method thereof.The present invention has system
Standby process is simply easily controllable, and metallic aluminium forms conductive network in the film, dramatically increases its electric conductivity, in cosputtering process
Middle part aluminium can enter cobalt acid lithium lattice, form LiAlyCo1-yO2On the one hand the presence of solid solution, the solid solution can promote lithium
Ion transports, and on the other hand will improve the cyclical stability of electrode.
Technical solution of the present invention: a kind of cobalt acid lithium composite film electrode and preparation method thereof, using More target sputtering together skill
Art sputters cobalt acid lithium target simultaneously and aluminium target prepares the cobalt acid lithium composite film electrode of aluminium doping vario-property.
In cobalt acid lithium composite film electrode above-mentioned and preparation method thereof, comprising the following steps:
(1) cobalt acid lithium target and aluminium target are installed on magnetron sputtering cavity, persistently vacuumized, placed the substrate in substrate and press from both sides and add
Heat, rotation；
(2) after being evacuated to back end vacuum, be passed through working gas, using More target sputtering together technology simultaneously sputter cobalt acid lithium target and
Aluminium target prepares the cobalt acid lithium composite film electrode of aluminium doping vario-property, passes through control cobalt acid lithium target and the sputtering parameter and target of aluminium target
Material ingredient regulates and controls the ingredient and structure of laminated film；
(3) natural cooling after the completion of sputtering, obtains cobalt acid lithium composite film electrode.
In cobalt acid lithium composite film electrode above-mentioned and preparation method thereof, in the step (1), cobalt acid lithium target material composition is
LixCoO2, wherein 1≤x≤1.2, aluminium target material composition is Al.
In cobalt acid lithium composite film electrode above-mentioned and preparation method thereof, in the step (1), substrate is the stainless of cleaning
One of steel substrate, glass substrate or silicon chip.
In cobalt acid lithium composite film electrode above-mentioned and preparation method thereof, in the step (1), the substrate heats temperature
Degree is 300-600 DEG C and keeps, and substrate revolving speed is 5-20rpm.
In cobalt acid lithium composite film electrode above-mentioned and preparation method thereof, in the step (2), back end vacuum is 1 × 10-4-1×10-3Pa, sputtering working gas is argon gas or argon oxygen gas mixture, makes sputtering pressure 0.2- after being passed through working gas
5.0Pa。
In cobalt acid lithium composite film electrode above-mentioned and preparation method thereof, the volume fraction of oxygen in the argon oxygen gas mixture
For 5-50%.
In cobalt acid lithium composite film electrode above-mentioned and preparation method thereof, in the step (2), More target sputtering together cobalt acid lithium
Target as sputter parameter are as follows: target-substrate distance 3-10cm, sputtering power 50-250W.
In cobalt acid lithium composite film electrode above-mentioned and preparation method thereof, in the step (2), More target sputtering together aluminium target
Sputtering parameter are as follows: target-substrate distance 3-10cm, sputtering power 10-100W.
In cobalt acid lithium composite film electrode above-mentioned and preparation method thereof, in the step (2), cobalt acid lithium laminated film electricity
Pole is with a thickness of 300-2000nm.
Compared with prior art, the invention has the following advantages:
1, the present invention sputters cobalt acid lithium target and aluminium target simultaneously using More target sputtering together technology, and the cobalt acid lithium for preparing aluminium doping is multiple
Film is closed, preparation process is simply easily controllable, and metallic aluminium forms conductive network in the film, dramatically increases its conductive capability.
2, part aluminium can enter cobalt acid lithium lattice during cosputtering, form LiAlyCo1-yO2Solid solution, the solid solution
On the one hand the presence of body can promote transporting for lithium ion, on the other hand will improve the cyclical stability of electrode.
Experiments have shown that:
Applicant carries out following experiment for case study on implementation 1-3:
Embodiment 1: Fig. 1 is the surface SEM figure of cobalt acid lithium composite film electrode prepared by the present embodiment 1, it can be seen that can be seen
The cobalt acid lithium laminated film surfacing obtained out, crystalline particle is obvious, illustrates that this programme can be preferable with preparation structure pattern
Membrane electrode.
Charge-discharge test: using laminated film made above as anode, using metal Li as to electrode, diaphragm is used
2400 model single-layer polypropylene of Celgard company is used with EC:DEC:DMC=1:1:1(volume ratio) it is what organic solvent was prepared
Concentration is the lithium hexafluoro phosphate (LiPF of 1 mol/L6) solution (Huarong company, Zhangjiagang Cathay) be electrolyte be assembled into half-cell
Carry out charge-discharge test.Meanwhile as control, cobalt acid lithium target is sputtered to only independent in step 2 as above in the same way,
Pure cobalt acid lithium membrane electrode is prepared, half-cell is assembled into and carries out charge-discharge test.Fig. 2 is two kinds of membrane electrodes by above-mentioned preparation
In the cycle performance curve graph of the section 3-4.2V test, wherein curve a is the cobalt prepared by 1 the method cosputtering of embodiment
Preceding 50 weeks cycle performance curves of the half-cell of sour lithium composite meas dress；Curve b is the pure cobalt of no cosputtering preparation
Preceding 50 weeks cycle performance curves of the half-cell of sour lithium membrane electrode assembling.It can be seen that utilize by correlation curve a, b and splash altogether
The cobalt acid lithium composite film electrode for penetrating technology preparation has higher specific discharge capacity and better discharge capacitance (circulation
Capacity retention ratio after 50 weeks relative to first week is 99.21%), to effectively increase the capacity and cyclical stability of battery.
Embodiment 2: Fig. 3 is the surface SEM figure of cobalt acid lithium composite film electrode prepared by the present embodiment 2, it can be seen that
The cobalt acid lithium laminated film surfacing arrived is fine and close, has certain crystallinity, and crystalline particle is in rice-shaped, illustrates that this programme can
With the preferable membrane electrode of preparation structure pattern.
Embodiment 3: ac impedance measurement: using laminated film made above as anode, using metal Li as to electrode,
Diaphragm uses 2400 model single-layer polypropylene of Celgard company, and use is with EC:DEC:DMC=1:1:1(volume ratio) it is organic molten
The concentration that agent is prepared is the lithium hexafluoro phosphate (LiPF of 1 mol/L6) solution (Huarong company, Zhangjiagang Cathay) be electrolyte assembling
Ac impedance measurement is carried out at half-cell.Meanwhile as control, in the same way to only individually sputtering in step 2 as above
Cobalt acid lithium target prepares pure cobalt acid lithium membrane electrode, is assembled into half-cell and carries out charge-discharge test.Fig. 4 is the preparation of the present embodiment 3
The ac impedance spectroscopy tested in 3.0V of two kinds of membrane electrodes, wherein curve c is by 3 the method cosputtering system of embodiment
The ac impedance spectroscopy of the half-cell of standby cobalt acid lithium composite meas dress；Curve d is the pure cobalt of no cosputtering preparation
The ac impedance spectroscopy of the half-cell of sour lithium membrane electrode assembling.It can be seen that by correlation curve c, d and utilize co-sputtering technology
The cobalt acid lithium composite film electrode of preparation has smaller impedance, illustrates that this programme More target sputtering together improves composite film electrode
Conductive capability.
In conclusion the present invention has preparation process simply easily controllable, metallic aluminium forms conductive network in the film, makes
Its electric conductivity dramatically increases, and part aluminium can enter cobalt acid lithium lattice during cosputtering, forms LiAlyCo1-yO2Solid solution,
On the one hand the presence of the solid solution can promote transporting for lithium ion, on the other hand will improve the beneficial effect of electrode cycle stability
Fruit.
Detailed description of the invention
Fig. 1 is the surface SEM figure of the cobalt acid lithium composite film electrode prepared in case study on implementation 1；
Fig. 2 is the cycle performance curve graph that the two kinds of membrane electrodes prepared in case study on implementation 1 are tested in the section 3-4.2V；
Fig. 3 is the surface SEM figure of the cobalt acid lithium composite film electrode prepared in case study on implementation 2；
Fig. 4 is the ac impedance spectroscopy that the two kinds of membrane electrodes prepared in case study on implementation 3 are tested in 3.0V.
Specific embodiment
The present invention is further illustrated with reference to the accompanying drawings and examples, but be not intended as to the present invention limit according to
According to.
A kind of embodiment 1: cobalt acid lithium composite film electrode and preparation method thereof, comprising the following steps:
(1) by LiCoO2Target and Al target are installed on magnetron sputtering cavity, persistently vacuumize, and clean stainless steel substrate is set
In substrate press from both sides and be heated to 550 DEG C and keep, substrate revolving speed be 10rpm；
(2) it is evacuated to back end vacuum 6 × 10-4After Pa, after being passed through Ar gas, make sputtering pressure 2.5Pa, build-up of luminance cosputtering
LiCoO2Target and Al target, wherein LiCoO2Target parameter are as follows: target-substrate distance 5cm, sputtering power 160W, Al target parameter are as follows: target
Cardinal distance 6.5cm, sputtering power 20W；
(3) natural cooling after the completion of sputtering, obtains cobalt acid lithium composite film electrode.
A kind of embodiment 2: cobalt acid lithium composite film electrode and preparation method thereof, comprising the following steps:
(1) by LiCoO2Target and Al target are installed on magnetron sputtering cavity, persistently vacuumize, and clean stainless steel substrate is set
In substrate press from both sides and be heated to 550 DEG C and keep, substrate revolving speed be 10rpm；
(2) it is evacuated to back end vacuum 6 × 10-4After Pa, it is passed through argon oxygen gas mixture, wherein argon oxygen volume ratio is 4:1, makes to adjust
Sputtering pressure is 2.5Pa, build-up of luminance cosputtering LiCoO2Target and Al target, wherein LiCoO2Target parameter are as follows: target-substrate distance 5cm splashes
Penetrate power 160W, Al target parameter are as follows: target-substrate distance 6.5cm, sputtering power 20W；
(3) natural cooling after the completion of sputtering, obtains cobalt acid lithium composite film electrode.
A kind of embodiment 3: cobalt acid lithium composite film electrode and preparation method thereof, comprising the following steps:
(1) by LiCoO2Target and Al target are installed on magnetron sputtering cavity, persistently vacuumize, and clean stainless steel substrate is set
In substrate press from both sides and be heated to 500 DEG C and keep, substrate revolving speed be 10rpm；
(2) it is evacuated to back end vacuum 7 × 10-4After Pa, after being passed through Ar gas, make sputtering pressure 2.5Pa, build-up of luminance cosputtering
LiCoO2Target and Al target, wherein LiCoO2Target parameter are as follows: target-substrate distance 6cm, sputtering power 200W, Al target parameter are as follows: target
Cardinal distance 7cm, sputtering power 30W；
(3) natural cooling after the completion of sputtering, obtains cobalt acid lithium composite film electrode.
A kind of embodiment 4: cobalt acid lithium composite film electrode and preparation method thereof, comprising the following steps:
(1) by LiCoO2Target and Al target are installed on magnetron sputtering cavity, persistently vacuumize, and clean glass substrate is placed in
Substrate press from both sides and be heated to 300 DEG C and keep, substrate revolving speed be 5rpm；
(2) it is evacuated to back end vacuum 1 × 10-3After Pa, after being passed through Ar gas, make sputtering pressure 5.0Pa, build-up of luminance cosputtering
LiCoO2Target and Al target, wherein LiCoO2Target parameter are as follows: target-substrate distance 3cm, sputtering power 50W, Al target parameter are as follows: target
Cardinal distance 3cm, sputtering power 10W；
(3) natural cooling after the completion of sputtering, obtains cobalt acid lithium composite film electrode.
A kind of embodiment 5: cobalt acid lithium composite film electrode and preparation method thereof, comprising the following steps:
(1) by Li1.1CoO2Target and Al target are installed on magnetron sputtering cavity, persistently vacuumize, and clean silicon chip is placed in
Substrate press from both sides and be heated to 500 DEG C and keep, substrate revolving speed be 15rpm；
(2) it is evacuated to back end vacuum 8 × 10-4After Pa, after being passed through argon oxygen gas mixture, make sputtering pressure 0.2Pa, build-up of luminance is total
Sputter Li1.1CoO2Target and Al target, wherein Li1.1CoO2Target parameter are as follows: target-substrate distance 7cm, sputtering power 150W, Al target
Parameter are as follows: target-substrate distance 9cm, sputtering power 70W；The volume fraction of oxygen is 50% in the argon oxygen gas mixture；
(3) natural cooling after the completion of sputtering, obtains cobalt acid lithium composite film electrode.
A kind of embodiment 6: cobalt acid lithium composite film electrode and preparation method thereof, comprising the following steps:
(1) by Li1.2CoO2Target and Al target are installed on magnetron sputtering cavity, persistently vacuumize, by clean stainless steel substrate
Be placed in substrate press from both sides and be heated to 600 DEG C and keep, substrate revolving speed be 20rpm；
(2) it is evacuated to back end vacuum 1 × 10-4After Pa, after being passed through Ar gas, make sputtering pressure 3.0Pa, build-up of luminance cosputtering
Li1.2CoO2Target and Al target, wherein Li1.2CoO2Target parameter are as follows: target-substrate distance 10cm, sputtering power 250W, Al target parameter
Are as follows: target-substrate distance 10cm, sputtering power 100W；
(3) natural cooling after the completion of sputtering, obtains cobalt acid lithium composite film electrode.
A kind of embodiment 7: cobalt acid lithium composite film electrode and preparation method thereof, comprising the following steps:
(1) by LiCoO2Target and Al target are installed on magnetron sputtering cavity, persistently vacuumize, and clean stainless steel substrate is set
In substrate press from both sides and be heated to 500 DEG C and keep, substrate revolving speed be 5rpm；
(2) it is evacuated to back end vacuum 3 × 10-4Afterwards, after being passed through argon oxygen gas mixture, make sputtering pressure 3.0Pa, build-up of luminance splashes altogether
Penetrate LiCoO2Target and Al target, wherein LiCoO2Target parameter are as follows: target-substrate distance 5cm, sputtering power 200W, Al target parameter are as follows:
Target-substrate distance 7cm, sputtering power 50W；The volume fraction of oxygen is 5% in the argon oxygen gas mixture.
(3) natural cooling after the completion of sputtering, obtains cobalt acid lithium composite film electrode.
Claims (9)
1. a kind of cobalt acid lithium composite film electrode and preparation method thereof, it is characterised in that: splashed simultaneously using More target sputtering together technology
It penetrates cobalt acid lithium target and aluminium target prepares the cobalt acid lithium composite film electrode of aluminium doping vario-property.
2. cobalt acid lithium composite film electrode according to claim 1 and preparation method thereof, it is characterised in that: including following step
It is rapid:
(1) cobalt acid lithium target and aluminium target are installed on magnetron sputtering cavity, persistently vacuumized, placed the substrate in substrate and press from both sides and add
Heat, rotation；
(2) after being evacuated to back end vacuum, be passed through working gas, using More target sputtering together technology simultaneously sputter cobalt acid lithium target and
Aluminium target prepares the cobalt acid lithium composite film electrode of aluminium doping vario-property, passes through control cobalt acid lithium target and the sputtering parameter and target of aluminium target
Material ingredient regulates and controls the ingredient and structure of laminated film；
(3) natural cooling after the completion of sputtering, obtains cobalt acid lithium composite film electrode.
3. cobalt acid lithium composite film electrode according to claim 2 and preparation method thereof, it is characterised in that: the step
(1) in, cobalt acid lithium target material composition is LixCoO2, wherein 1≤x≤1.2, aluminium target material composition is Al.
4. cobalt acid lithium composite film electrode according to claim 2 and preparation method thereof, it is characterised in that: the step
(1) in, the substrate heating temperature is 300-600 DEG C and keeps, and substrate revolving speed is 5-20rpm.
5. cobalt acid lithium composite film electrode according to claim 2 and preparation method thereof, it is characterised in that: the step
(2) in, back end vacuum is 1 × 10-4-1×10-3Pa, sputtering working gas is argon gas or argon oxygen gas mixture, is passed through working gas
After make sputtering pressure 0.2-5.0Pa.
6. cobalt acid lithium composite film electrode according to claim 5 and preparation method thereof, it is characterised in that: the argon oxygen is mixed
The volume fraction for closing oxygen in gas is 5-50%.
7. cobalt acid lithium composite film electrode according to claim 2 and preparation method thereof, it is characterised in that: the step
(2) in, More target sputtering together cobalt acid lithium target as sputter parameter are as follows: target-substrate distance 3-10cm, sputtering power 50-250W.
8. cobalt acid lithium composite film electrode according to claim 2 and preparation method thereof, it is characterised in that: the step
(2) in, More target sputtering together aluminium target as sputter parameter are as follows: target-substrate distance 3-10cm, sputtering power 10-100W.
9. cobalt acid lithium composite film electrode according to claim 2 and preparation method thereof, it is characterised in that: the step
(2) in, cobalt acid lithium composite film electrode is with a thickness of 300-2000nm.
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Application publication date: 20191112 |