CN110224137A - A method of orientation constructs manganese containing materials interface-modifying layer - Google Patents
A method of orientation constructs manganese containing materials interface-modifying layer Download PDFInfo
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- CN110224137A CN110224137A CN201910451573.9A CN201910451573A CN110224137A CN 110224137 A CN110224137 A CN 110224137A CN 201910451573 A CN201910451573 A CN 201910451573A CN 110224137 A CN110224137 A CN 110224137A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
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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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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
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Abstract
A method of orientation constructs manganese containing materials interface-modifying layer, comprising the following steps: (1) compound containing metallic element is dissolved into the solution containing dioxygen radical ion, obtains complex solution；(2) manganese containing materials, complex solution and precipitating reagent are mixed, carries out manganese containing materials surface modification, obtain the manganese containing materials of entire interface modification.The present invention can be realized the complete modification at manganese containing materials interface, and the property of oriented control interface-modifying layer, improve the performance of manganese containing materials to greatest extent.
Description
Technical field
The present invention relates to non-ferrous metal functional material interface modification fields, and in particular to a kind of orientation constructs manganese containing materials circle
The method of face decorative layer.
Background technique
In actual application, performance still has the defect in terms of certain to non-ferrous metal functional material.With lithium ion
For battery electrode material, common manganese containing materials have LiMn2O4 (LiMnO2) and nickel-cobalt-manganese ternary material (LiNi1-x- yCoxMnyO2(0≤x, y≤1, x+y≤1)), lithium-rich manganese base material (Li1-aNia-x-yCoxMnyO2(0≤x, y≤a, x+y≤
A)), manganese dioxide (MnO2), mangano-manganic oxide (Mn3O4), the LiMn2O4 (LiMn of spinel structure2O4) and polyanion class
Positive pole material phosphoric acid lithium metal (LiMPO4, M=Fe, Mn etc.) etc..Charge and discharge process of such manganese containing materials in lithium ion battery
It is middle that exclusive jahn-teller effect and the disproportionated reaction of Manganic ion etc. can occur, to seriously affect manganese element in electricity
The stability in liquid is solved, the chemical property of material is caused sharply to deteriorate.
Modifying interface is a kind of effective modified method, can improve the transmission performance of material electronics and lithium ion, isolation
Contact of the manganese containing materials with electrolyte improves stability (Xu M, Chen Z, Zhu H, et of the material in charge and discharge process
Al. J Mater Chem A, 2015,13933-13945.).
Coating decoration method in interface mainly has a sol-gal process at present, solvent evaporated method, spray drying process, hydro-thermal method, sinks
Shallow lake method etc..Although the above method can modify the interface of manganese containing materials, it cannot be guaranteed that manganese containing materials surface is realized
Complete modification.
Summary of the invention
The technical problem to be solved by the present invention is to overcome drawbacks described above of the existing technology, provide a kind of orientation structure
The method for building manganese containing materials interface-modifying layer, uses this method, it is ensured that realizes complete modification in manganese containing materials surface.
The technical solution adopted by the present invention to solve the technical problems is as follows: a kind of orientation constructs manganese containing materials modifying interface
The method of layer, comprising the following steps:
(1) compound containing metallic element is dissolved into hydrogen peroxide, obtains complex solution；
(2) by manganese containing materials, complex solution and precipitant mix, the reaction of manganese containing materials surface modification is carried out, modifying interface is obtained
Manganese containing materials and reaction solution mixed material；
(3) be separated by solid-liquid separation, obtained solid material washed, it is dry, then calcined in air atmosphere to get
The manganese containing materials completely modified to surface.
Substance containing metallic element is dissolved into containing in hydrogen peroxide by the present invention first, is formed using dioxygen root as ligand
Complex solution；Then mixed by manganese containing materials, complex solution and precipitating reagent, by manganese element to dioxygen root into
Row catalytic decomposition, so that metallic element be released, reacts with precipitating reagent, repairs to carry out interface to manganese containing materials
Decorations, until manganese containing materials surface fully achieves modification.
Further, in step (1), the compound containing metallic element is cobalt chloride, cobaltous sulfate, copper chloride, sulfuric acid
One of copper, zinc sulfate, tetrabutyl titanate, methyl chloride zinc or trichloromethyl titanium or two or more mixtures.
Further, in step (1), compound and H containing metallic element2O2Molar ratio be (0.01~1).
Further, in step (2), the manganese containing materials, the ratio of complex solution and precipitating reagent is 1: (0.01~1000):
(0.01~1000).
In step (2), the manganese containing materials are LiMn2O4, nickle cobalt lithium manganate, lithium-rich manganese base material, manganese dioxide, three oxygen
Change one or more of two manganese, mangano-manganic oxide, lithium manganese phosphate, lithium ferric manganese phosphate, sodium manganate or nickel cobalt sodium manganate
Mixture.
Further, in step (2), the precipitating reagent is ammonium hydroxide, sodium hydroxide solution, sodium carbonate, lithium carbonate, bicarbonate
One of sodium, ammonium hydrogen carbonate, thioacetamide or two or more mixed solutions.
Further, in step (2), the mixing is by manganese containing materials, and any two kinds in complex solution and precipitating reagent are in advance
After mixing, then simultaneously or sequentially mixed with the third material.
Further, described to be mixed into mechanical stirring mixing or pipeline mixing in step (2)；The mechanical stirring mixes
Manganese containing materials, complex solution and precipitating reagent are simultaneously or sequentially added under conditions of mechanical stirring；Pipeline mixing be by
Manganese containing materials and complex solution are added in pipeline, are sufficiently mixed by pipe-line mixer.
It is further, described to be separated by solid-liquid separation as filtering or be centrifuged in step (3), it is washed with water, the temperature of the calcining
600-900 DEG C, the time of calcining is 2-6h.
The invention has the advantages that: the complete modification that can be realized manganese containing materials interface, and oriented control interface-modifying layer
Property improves the performance of manganese containing materials to greatest extent.
Specific embodiment
Below with reference to embodiment, the invention will be further described.
Chemical reagent used in the embodiment of the present invention is obtained by routine business approach unless otherwise specified.
Embodiment 1
The present embodiment is with lithium-rich manganese base material Li1.2Mn0.54Ni0.13Co0.13O2Implement orientation for modified object and constructs material containing manganese
Expect the method for interface-modifying layer, comprising the following steps:
(1) 30g tetrabutyl titanate is dissolved into the hydrogen peroxide solution that 150ml concentration is 20%, stands 120 min, is leaked with liquid separation
Bucket removes upper layer grease, obtains stable complex solution；
(2) using the ammonium hydroxide that concentration is 12% as precipitating reagent；Using 1 L reaction kettle as mixer；First by 5g lithium-rich manganese base material
The ammonium hydroxide for being 12% with 300ml concentration is added in reaction kettle, and after opening stirring, complex solution is at the uniform velocity added using peristaltic pump
In reaction kettle, the reaction of manganese containing materials surface modification is carried out, the manganese containing materials of modifying interface and the mixed material of reaction solution are obtained；
(3) it is separated by solid-liquid separation, is filtered, washed, dry, then 700 DEG C of calcining 5h in air atmosphere, obtain interface by TiO2
The lithium-rich manganese base material completely modified.
The interface that the present embodiment obtains is by TiO2The lithium-rich manganese base material completely modified carries out button cell test, specific to walk
It is rapid as follows:
According to active material: PVDF: acetylene black=8: 1: l (mass ratio) weighs smear, the circle that test electrode is diameter about 14mm
Piece；Various electrochemical property tests are carried out again after assembled battery standing 12h；Voltage is between 3.0-4.8V, in 12.5mA/
Under the charging or discharging current of g, first charge-discharge capacity is 304mAhg-1；Under the charging or discharging current of 250mA/g, first charge-discharge capacity is
230 mAhg-1, capacity retention is 86% after 500 circulations.
Embodiment 2
The present embodiment is with spinel lithium manganate LiMn2O4Implement orientation for modified object and constructs manganese containing materials interface-modifying layer
Method, comprising the following steps:
(1) 1g zinc sulfate is dissolved into the hydrogen peroxide solution that 150ml concentration is 20%, obtains stable complex solution；
(2) using concentration be 12% ammonium hydroxide and concentration be 20% liquid alkaline according to after mass ratio 1:1 mixing as precipitating reagent；With 1 L
Reaction kettle is as mixer；The precipitating reagent that 300ml is prepared first is added in reaction kettle, after opening stirring, uses feeder
Lithium manganate material and complex solution are at the uniform velocity added in reaction kettle with peristaltic pump；
(3) material obtained after filtration washing obtains interface in 800 DEG C of calcining 2h and is completely repaired by ZnO under conditions of air
The lithium manganate material of decorations.
The present embodiment obtains the lithium manganate material that interface is completely modified by ZnO and carries out button cell test, and specific steps are such as
Under:
According to active material: PVDF: acetylene black=8: 1: l (mass ratio) weighs smear, the circle that test electrode is diameter about 14mm
Piece.Various electrochemical property tests are carried out again after assembled battery standing 12h.Voltage is between 3.0-4.4V, in 12mA/g
Charging or discharging current under, first charge-discharge capacity be 120mAhg-1.Under the charging or discharging current of 120mA/g, first charge-discharge capacity is
112 mAhg-1, capacity retention is 90% after 500 circulations.
Embodiment 3
The present embodiment is with ternary material LiNi0.5Co0.2Mn0.3O2Manganese containing materials interface is constructed for modified object implementation orientation to repair
The method for adoring layer, comprising the following steps:
(1) 30g tetrabutyl titanate is dissolved into the hydrogen peroxide solution that 150ml concentration is 20%, stands 300 min, is leaked with liquid separation
Bucket removes upper layer grease, obtains stable complex solution；
(2) using the ammonium hydroxide that concentration is 12% as precipitating reagent；Using 1 L reaction kettle as mixer；First by 5g ternary material with
The ammonium hydroxide that 300ml concentration is 12% is added in reaction kettle, and after opening stirring, complex solution is at the uniform velocity added instead using peristaltic pump
It answers in kettle, the material obtained after filtration washing, under conditions of air, obtains interface by TiO in 600 DEG C of calcining 6h2Completely
The ternary material of modification.
The interface that the present embodiment obtains is by TiO2The ternary material completely modified carries out button cell test, and specific steps are such as
Under:
According to active material: PVDF: acetylene black=8: 1: l (mass ratio) weighs smear, the circle that test electrode is diameter about 14mm
Piece.Various electrochemical property tests are carried out again after assembled battery standing 12h.Voltage is between 3.0-4.3V, in 15mA/g
Charging or discharging current under, first charge-discharge capacity be 175 mAhg-1.Under the charging or discharging current of 150mA/g, first charge-discharge capacity is
160 mAhg-1, capacity retention is 88% after 500 circulations.
Embodiment 4
The present embodiment is with nickelic ternary material LiNi0.80Co0.1Mn0.1O2Implement orientation for modified object and constructs manganese containing materials circle
The method of face decorative layer, comprising the following steps:
(1) 50g tetrabutyl titanate is dissolved into the hydrogen peroxide solution that 300ml concentration is 20%, stands 500 min, is leaked with liquid separation
Bucket removes upper layer grease, obtains stable complex solution；
(2) using the liquid alkaline that concentration is 32% as precipitating reagent；Using 1 L reaction kettle as mixer；First by the nickelic ternary material of 5g
The pure water of material, the liquid alkaline that 30ml concentration is 32% and 300ml is added in reaction kettle, after opening stirring, will be complexed using peristaltic pump
Object solution is at the uniform velocity added in reaction kettle, the material obtained after filtration washing, under conditions of air, obtains in 900 DEG C of calcining 3h
To interface by TiO2The nickelic ternary material completely modified.
The present embodiment obtains interface by TiO2The nickelic ternary material completely modified carries out button cell test, specific steps
It is as follows:
According to active material: PVDF: acetylene black=8: 1: l (mass ratio) weighs smear, the circle that test electrode is diameter about 14mm
Piece.Various electrochemical property tests are carried out again after assembled battery standing 12h.Voltage is between 3.0-4.3V, in 20mA/g
Charging or discharging current under, first charge-discharge capacity be 205 mAhg-1.Under the charging or discharging current of 200mA/g, first charge-discharge capacity is
190 mAhg-1, capacity retention is 87% after 500 circulations.
Claims (10)
1. a kind of orient the method for constructing manganese containing materials interface-modifying layer, which comprises the following steps:
(1) compound containing metallic element is dissolved into hydrogen peroxide, obtains complex solution；
(2) by manganese containing materials, complex solution and precipitant mix, the reaction of manganese containing materials surface modification is carried out, modifying interface is obtained
Manganese containing materials and reaction solution mixed material；
(3) be separated by solid-liquid separation, obtained solid material washed, it is dry, then calcined in air atmosphere to get
The manganese containing materials completely modified to surface.
2. orienting the method for constructing manganese containing materials interface-modifying layer according to claim 1, which is characterized in that in step (1),
The compound containing metallic element is cobalt chloride, cobaltous sulfate, copper chloride, copper sulphate, zinc sulfate, tetrabutyl titanate, chlorination
One of methyl zinc or trichloromethyl titanium or two or more mixtures.
3. according to claim 1 or claim 2 orient the method for constructing manganese containing materials interface-modifying layer, which is characterized in that step (1)
In, compound and H containing metallic element2O2Molar ratio be 0.01~1.
4. the method for constructing manganese containing materials interface-modifying layer is oriented described in one of -3 according to claim 1, which is characterized in that step
(2) in, the manganese containing materials, the mass ratio of complex solution and precipitating reagent is 1: (0.01~1000): (0.01~1000).
5. the method for constructing manganese containing materials interface-modifying layer is oriented described in one of -4 according to claim 1, which is characterized in that step
(2) in, the manganese containing materials are LiMn2O4, nickle cobalt lithium manganate, lithium-rich manganese base material, manganese dioxide, manganese sesquioxide managnic oxide, four oxidations
The mixture of one or more of three manganese, lithium manganese phosphate, lithium ferric manganese phosphate, sodium manganate or nickel cobalt sodium manganate.
6. the method for constructing manganese containing materials interface-modifying layer is oriented described in one of -5 according to claim 1, which is characterized in that step
(2) in, the precipitating reagent is ammonium hydroxide, sodium hydroxide solution, sodium carbonate, lithium carbonate, sodium bicarbonate, ammonium hydrogen carbonate, thioacetyl
One of amine or two or more mixed solutions.
7. the method for constructing manganese containing materials interface-modifying layer is oriented described in one of -6 according to claim 1, which is characterized in that step
(2) in, the mixing is by manganese containing materials, after any two kinds in complex solution and precipitating reagent are pre-mixed, then with the third object
Material is simultaneously or sequentially mixed.
8. the method for constructing manganese containing materials interface-modifying layer is oriented described in one of -7 according to claim 1, which is characterized in that step
(2) described to be mixed into mechanical stirring mixing or pipeline mixing in；The mechanical stirring mixing is same under conditions of mechanical stirring
When or sequentially add manganese containing materials, complex solution and precipitating reagent；The pipeline mixing is to add manganese containing materials and complex solution
Enter in pipeline, is sufficiently mixed by pipe-line mixer.
9. the method for constructing manganese containing materials interface-modifying layer is oriented described in one of -8 according to claim 1, which is characterized in that step
(3) described to be separated by solid-liquid separation as filtering or centrifugation in.
10. the method for constructing manganese containing materials interface-modifying layer is oriented described in one of -9 according to claim 1, which is characterized in that step
Suddenly in (3), 600-900 DEG C of the temperature of the calcining, the time of calcining is 2-6h.
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Cited By (1)
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| CN114678522A (en) * | 2022-04-25 | 2022-06-28 | 西安理工大学 | Modification method of lithium-rich manganese-based positive electrode material by regulating manganese vacancy and application of material |
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