CN110429274A - Lithium ion cell positive ternary material and preparation method thereof - Google Patents
Lithium ion cell positive ternary material and preparation method thereof Download PDFInfo
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- CN110429274A CN110429274A CN201910614088.9A CN201910614088A CN110429274A CN 110429274 A CN110429274 A CN 110429274A CN 201910614088 A CN201910614088 A CN 201910614088A CN 110429274 A CN110429274 A CN 110429274A
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- lithium ion
- film layer
- ion cell
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- 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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- 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 relates to a kind of lithium ion cell positive ternary materials and preparation method thereof, and preparation method includes: selection substrate, and is cleaned；It is designed according to film layer, selects lithium source, nickel source, cobalt source and manganese source target, be alternately coated with film layer in the substrate, obtain intermediate；The intermediate is subjected to the first heat treatment；The second heat treatment will be carried out by the intermediate of the first heat treatment, obtains lithium ion cell positive ternary material；Wherein, the film layer includes at least one unit film layer, and the unit film layer includes lithium layer, nickel layer, cobalt layers and manganese layer.The present invention requires the proportion of four kinds of metals different according to different use environments, only with four kinds of targets, the film layer that four kinds of presomas are alternately plated in substrate realizes that the stoichiometric ratio of three kinds of ingredients controls by the plated film time of every kind of element of control, so as to save experiment or production cost.
Description
Technical field
The present invention relates to field of lithium ion battery, more particularly to a kind of lithium ion cell positive ternary material and its preparation
Method.
Background technique
In terms of industrialization angle, film lithium ion battery has been applied to micro memory, wireless sensor, implantable medical
Equipment.Different application field proposes different requirements to the capacity of battery, high rate performance, stability safety.Nickel cobalt manganese systems
The chemical equation of lithium ion cell positive ternary material is LizNixCoyMn1-x-yO2.Mature technology is preparing film at present
During anode material for lithium-ion batteries film layer, the stoichiometric ratio of three kinds of metallic elements as needed is sintered into corresponding material first
The target of material, then by the method deposition plating of sputtering, if a certain or two kinds of constituent contents change in three kinds of elements
When, need to prepare the target being accordingly formulated again, the preparation of target needs to consume a large amount of cost, and target tends not to completely
It utilizes, forms waste.
Summary of the invention
It is a primary object of the present invention to provide a kind of novel lithium ion cell positive ternary material and its preparation side
Method, the technical problem to be solved is that making it save experiment or production cost, thus more suitable for practical.
The object of the invention to solve the technical problems adopts the following technical solutions to realize.It proposes according to the present invention
A kind of lithium ion cell positive ternary material preparation method comprising:
Substrate is selected, and is cleaned；
It is designed according to film layer, selects lithium source, nickel source, cobalt source and manganese source target, be alternately coated with film layer in the substrate,
Obtain intermediate；
The intermediate is subjected to the first heat treatment；
The second heat treatment will be carried out by the intermediate of the first heat treatment, obtains lithium ion cell positive ternary material；
Wherein, the film layer includes at least one unit film layer, and the unit film layer includes lithium layer, nickel layer, cobalt layers
With manganese layer.
The object of the invention to solve the technical problems also can be used following technical measures and further realize.
Preferably, the preparation method of lithium ion cell positive ternary material above-mentioned, wherein the substrate is in 500-
1000 DEG C have stability.
Preferably, the preparation method of lithium ion cell positive ternary material above-mentioned, wherein the substrate is graphite-based
Bottom, platinized platinum substrate or platinized substrate.
Preferably, the preparation method of lithium ion cell positive ternary material above-mentioned, wherein the lithium source be Li,
Li2CO3Or Li2O；
The nickel source is NiO, LiNiO2Or Ni2O3；
The cobalt source is CoO, LiCoO2Or Co2O3；
The manganese source is MnO, LiMnO2Or LiMn2O4。
Preferably, the preparation method of lithium ion cell positive ternary material above-mentioned, wherein the thickness of the unit film layer
Degree is less than 100nm.
Preferably, the preparation method of lithium ion cell positive ternary material above-mentioned, wherein first heat treatment
Temperature is 100-200 DEG C, and the time of the first heat treatment is greater than 100h, and the atmosphere of the first heat treatment is vacuum.
Preferably, the preparation method of lithium ion cell positive ternary material above-mentioned, wherein second heat treatment
Temperature is 500-1000 DEG C, and the time 2-24h of the second heat treatment, the atmosphere of the second heat treatment is atmospheric atmosphere or oxygen atmosphere.
Also the following technical solution is employed for the object of the invention to solve the technical problems to realize.It proposes according to the present invention
A kind of lithium ion cell positive ternary material, be prepared by method above-mentioned comprising:
Substrate；
Lithium ion cell positive film layer is attached in the substrate.
The object of the invention to solve the technical problems also can be used following technical measures and further realize.
Preferably, lithium ion cell positive ternary material above-mentioned, wherein the lithium ion cell positive film layer is
LizNixCoyMn1-x-yO2, wherein 0 < x < 1,0 < y < 1.
By above-mentioned technical proposal, lithium ion cell positive ternary material of the present invention and preparation method thereof at least has following
Advantage:
Li is required according to different use environmentszNixCoyMn1-x-yO2In four kinds of metals proportion it is different, only with four kinds of targets
Material alternately plates the film layer of four kinds of presomas in substrate, and the change of three kinds of ingredients is realized by the plated film time of every kind of element of control
Metering is learned than control, after the overall thickness for reaching requirement, first carries out being diffused between the multilayer film of Low Temperature Heat Treatment intermediate, shape
At the equal phase structure that amorphous state is spread, then high-temperature heat treatment crystallization is carried out, is sufficiently mixed and reacts between realization film layer, prepare
Satisfactory ternary material, so as to save experiment or production cost.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, the following is a detailed description of the preferred embodiments of the present invention and the accompanying drawings.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of intermediate；
Fig. 2 is the structural schematic diagram of lithium ion cell positive ternary material；
Fig. 3 is the Ni-Co-Mn component distributing figure of the film layer depth direction of 1 lithium ion cell positive ternary material of embodiment；
Fig. 4 is the Ni-Co-Mn component distributing figure of the film layer depth direction of comparative example lithium ion cell positive ternary material.
Specific embodiment
It is of the invention to reach the technical means and efficacy that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Attached drawing and preferred embodiment, to lithium ion cell positive ternary material proposed according to the present invention and preparation method thereof, it is specific real
Mode, structure, feature and its effect are applied, detailed description is as follows.In the following description, different " embodiment " or " embodiment "
What is referred to is not necessarily the same embodiment.In addition, the special characteristic, structure or feature in one or more embodiments can be by any conjunction
Conformal formula combination.
A kind of preparation method for lithium ion cell positive ternary material that one embodiment of the present of invention proposes comprising:
Substrate is selected, and is cleaned；
According to film layer LizNixCoyMn1-x-yO2Composition selects lithium source, nickel source, cobalt source and manganese source target, according to experiment or life
It produces and requires, calculate overall thickness requirement and component requirements；Extrapolate presoma proportion, single layer film thickness and multilayer film periodicity；It adopts
It alternately is coated with film layer in the substrate with magnetically controlled sputter method or ion beam sputtering method, obtains intermediate；
The intermediate is subjected to the first heat treatment；
The second heat treatment will be carried out by the intermediate of the first heat treatment, obtains lithium ion cell positive ternary material；
Wherein, the structure of intermediate is as shown in Figure 1, intermediate includes substrate 1 and film layer 2, and the film, 2 include at least
One unit film layer 3, the unit film layer 3 include lithium layer, nickel layer, cobalt layers and manganese layer.
Preferably, substrate has stability at 500-1000 DEG C, and substrate is graphite base, platinized platinum substrate or platinized substrate.
Preferably, cleaning includes: to carry out first pass cleaning using deionized water ultrasound, is carried out second time using acetone ultrasound
Cleaning, gas drying, using cleaning plasma processing substrate surface.
Preferably, lithium source Li, Li2CO3Or Li2O；Nickel source is NiO, LiNiO2Or Ni2O3；Cobalt source is CoO, LiCoO2Or
Co2O3；Manganese source is MnO, LiMnO2Or LiMn2O4。
Preferably, the thickness of unit film layer is less than 100nm.The plated film sequence of unit film layer are as follows: nickel-cobalt-manganese-lithium, nickel-
Manganese-cobalt-lithium, cobalt-nickel-manganese-lithium, cobalt-manganese-nickel-lithium, manganese-nickel-cobalt-lithium or manganese-cobalt-nickel-lithium.Co element, Ni element and Mn member
The molar ratio of element is any, and Li element is stoichiometrically.
Preferably, first heat treatment temperature be 100-200 DEG C, first heat treatment time be greater than 100h, first heat at
The atmosphere of reason is vacuum.
Preferably, the temperature of the second heat treatment is 1500-1000 DEG C, the time 2-24h of the second heat treatment, the second heat treatment
Atmosphere be atmospheric atmosphere or oxygen atmosphere.
As shown in Fig. 2, another embodiment of the present invention proposes a kind of lithium ion cell positive ternary material, by side above-mentioned
Method is prepared comprising:
Substrate 4；
Lithium ion cell positive film layer 5 is attached in the substrate 3.
Preferably, lithium ion cell positive film layer is LizNixCoyMn1-x-yO2, wherein 0 < x < 1,0 < y < 1.
Embodiment 1
A kind of preparation method for lithium ion cell positive ternary material that one embodiment of the present of invention proposes comprising:
It chooses having a size of 25 × 25 × 2mm platinum plating quartz glass as substrate, platinum film is as conductive current collector；Spend from
Sub- water ultrasound 10min carries out first pass cleaning, carries out second time cleaning, gas drying, using cleaning using acetone ultrasound 10min
With plasma processing substrate surface 5min；
According to film layer LiNi0.3Co0.3Mn0.3O2Stoichiometric ratio, overall thickness 300nm, molar ratio Li:Ni:Co:Mn
=1:0.3:0.3:0.3；The source Li uses Li2CO3Target, metal simple-substance target is respectively adopted in the source Ni, Co and Mn, in sputtering process
By adjusting Ar/O2Than according to NiO-CoO-MnO-Li in substrate2CO3Sequence, which is repeated 3 times, is coated with film layer, obtains intermediate；
Wherein film layer includes three unit film layers, and each unit thicknesses of layers is 100nm.
By intermediate in vacuum degree 8 × 10-7The first heat treatment is carried out under Torr environment, and 200 DEG C of heat are warming up to 5 DEG C/min
Handle 100h；
The second heat treatment will be carried out in atmospheric conditions by the intermediate of the first heat treatment, is warming up to 10 DEG C/min
600 DEG C of heat treatment 5h, obtain lithium ion cell positive ternary material.
Another embodiment of the present invention proposes a kind of lithium ion cell positive ternary material, is prepared by the method for embodiment 1
And it obtains comprising:
Substrate；
Lithium ion cell positive film layer is LiNi0.3Co0.3Mn0.3O2, it is attached in the substrate.
Embodiment 2
A kind of preparation method for lithium ion cell positive ternary material that one embodiment of the present of invention proposes comprising:
It chooses having a size of 25 × 25 × 2mm platinum plating quartz glass as substrate, platinum film is as conductive current collector；Spend from
Sub- water ultrasound 10min carries out first pass cleaning, carries out second time cleaning, gas drying, using cleaning using acetone ultrasound 10min
With plasma processing substrate surface 5min；
According to film layer LiNi0.8Co0.1Mn0.1O2Stoichiometric ratio, overall thickness 100nm, molar ratio Li:Ni:Co:Mn
=1:0.8:0.1:0.1；The source Li uses Li2CO3NiO, CoO, MnO target is respectively adopted in target, the source Ni, Co and Mn, is sputtering
By adjusting Ar/O in journey2Than according to NiO-CoO-MnO-Li in substrate2CO3Sequence is coated with film layer, obtains intermediate；Wherein
Film layer includes a unit film layer.
By intermediate in vacuum degree 8 × 10-7The first heat treatment is carried out under Torr environment, and 200 DEG C of heat are warming up to 5 DEG C/min
Handle 200h；
The second heat treatment will be carried out under Oxygen Condition by the intermediate of the first heat treatment, be warming up to 10 DEG C/min
700 DEG C of heat treatment 10h, obtain lithium ion cell positive ternary material.
Another embodiment of the present invention proposes a kind of lithium ion cell positive ternary material, is prepared by the method for embodiment 1
And it obtains comprising:
Substrate；
Lithium ion cell positive film layer is LiNi0.8Co0.1Mn0.1O2, it is attached in the substrate.
Comparative example
A kind of preparation method for lithium ion cell positive ternary material that a comparative example of the invention proposes comprising:
It chooses having a size of 25 × 25 × 2mm platinum plating quartz glass as substrate, platinum film is as conductive current collector；Spend from
Sub- water ultrasound 10min carries out first pass cleaning, carries out second time cleaning, gas drying, using cleaning using acetone ultrasound 10min
With plasma processing substrate surface 5min；
According to film layer LiNi0.3Co0.3Mn0.3O2Stoichiometric ratio, overall thickness 300nm, molar ratio Li:Ni:Co:Mn
=1:0.3:0.3:0.3；The source Li uses Li2CO3Target, metal simple-substance target is respectively adopted in the source Ni, Co and Mn, in sputtering process
By adjusting Ar/O2Than according to NiO-CoO-MnO-Li in substrate2CO3Sequence, which is repeated 3 times, is coated with film layer, obtains intermediate；
Wherein film layer includes three unit film layers, and each unit thicknesses of layers is 100nm.
Intermediate is heat-treated in atmospheric conditions, 600 DEG C of heat treatment 5h are warming up to 10 DEG C/min, obtain lithium from
Sub- anode ternary material.
Another comparative example of the invention proposes a kind of lithium ion cell positive ternary material, by the method preparation of comparative example
Comprising:
Substrate；
Lithium ion cell positive film layer is attached in the substrate.
The lithium ion cell positive ternary material of embodiment 1 and comparative example is subjected to SIMS test, embodiment 1 and comparative example
Lithium ion cell positive ternary material film layer depth direction Ni-Co-Mn component distributing figure difference it is as shown in Figure 3 and Figure 4.It says
Bright to be heat-treated by increasing by first, Ni, Co, Mn are more uniform in the distribution of film layer depth direction.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, according to
According to technical spirit any simple modification, equivalent change and modification to the above embodiments of the invention, this hair is still fallen within
In the range of bright technical solution.
Claims (9)
1. a kind of preparation method of lithium ion cell positive ternary material, characterized in that it comprises:
Substrate is selected, and is cleaned；
It is designed according to film layer, selects lithium source, nickel source, cobalt source and manganese source target, be alternately coated with film layer in the substrate, obtain
Intermediate；
The intermediate is subjected to the first heat treatment；
The second heat treatment will be carried out by the intermediate of the first heat treatment, obtains lithium ion cell positive ternary material；
Wherein, the film layer includes at least one unit film layer, and the unit film layer includes lithium layer, nickel layer, cobalt layers and manganese
Layer.
2. the preparation method of lithium ion cell positive ternary material according to claim 1, which is characterized in that the base
Bottom has stability at 500-1000 DEG C.
3. the preparation method of lithium ion cell positive ternary material according to claim 1, which is characterized in that the base
Bottom is graphite base, platinized platinum substrate or platinized substrate.
4. the preparation method of lithium ion cell positive ternary material according to claim 1, which is characterized in that the lithium
Source is Li, Li2CO3Or Li2O；
The nickel source is NiO, LiNiO2Or Ni2O3；
The cobalt source is CoO, LiCoO2Or Co2O3；
The manganese source is MnO, LiMnO2Or LiMn2O4。
5. the preparation method of lithium ion cell positive ternary material according to claim 1, which is characterized in that the list
The thickness of first film layer is less than 100nm.
6. the preparation method of lithium ion cell positive ternary material according to claim 1, which is characterized in that described
The temperature of one heat treatment is 100-200 DEG C, and the time of the first heat treatment is greater than 100h, and the atmosphere of the first heat treatment is vacuum atmosphere
It encloses.
7. the preparation method of lithium ion cell positive ternary material according to claim 1, which is characterized in that described
The temperature of two heat treatments is 1500-1000 DEG C, and the time 2-24h of the second heat treatment, the atmosphere of the second heat treatment is atmospheric atmosphere
Or oxygen atmosphere.
8. a kind of lithium ion cell positive ternary material, which is characterized in that prepared by the described in any item methods of claim 1-7
And it obtains comprising:
Substrate；
Lithium ion cell positive film layer is attached in the substrate.
9. lithium ion cell positive ternary material according to claim 8, which is characterized in that the lithium ion battery is just
Pole film layer is LizNixCoyMn1-x-yO2, wherein 0 < x < 1,0 < y < 1.
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