CN104183842A - Anode material and preparation method thereof - Google Patents

Anode material and preparation method thereof Download PDF

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Publication number
CN104183842A
CN104183842A CN201410401724.7A CN201410401724A CN104183842A CN 104183842 A CN104183842 A CN 104183842A CN 201410401724 A CN201410401724 A CN 201410401724A CN 104183842 A CN104183842 A CN 104183842A
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positive electrode
anode material
preparation
solution
fluorine
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CN104183842B (en
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阮丁山
郑春凤
谭欣欣
柳娜
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Ningde Amperex Technology Ltd
Dongguan Amperex Technology Ltd
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Ningde Amperex Technology Ltd
Dongguan Amperex Technology Ltd
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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
    • 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
    • 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
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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 invention discloses an anode material and a preparation method of the anode material. The preparation method of the anode material comprises the following steps: (1) dissolving fluorine-containing polymer in a solvent to form solution A, and dissolving metal salt in the same solvent to form a solution B; (2) mixing and stirring the solution A and the solution B uniformly, adding unmodified anode material powder in the obtained mixed solution, stirring, drying, and calcining at 300-750 DEG C to obtain a fluorine ion doped and metal fluoride clad anode material with treated polymer surface membrane. The cores of the anode material particles are doped with fluorine ions, and the surface of the anode material particle is modified by the metal fluoride layer and the polymer surface membrane. According to the preparation method of the anode material, fluorine ion doping, metal fluoride cladding and the polymer surface membrane treatment are carried out by one step and the synthetic efficiency is high, and the obtained anode material is suitable for use under high charge cut-off voltage and has high thermal stability.

Description

Positive electrode and preparation method thereof
Technical field
The invention belongs to lithium ion battery field, more particularly, the present invention relates to a kind of positive electrode and preparation method thereof.
Background technology
In anode material for lithium-ion batteries, lithium nickel cobalt manganese (NCM) ternary material because of possess higher capacity (can be up to 250mAh/g, for theoretical capacity 91%), the excellent advantage such as security performance and cheap price obtained researcher's extensive concern.But this material at high temperature poor cycle performance has but restricted its application and development.
Current research shows, the NCM ternary material at high temperature poor reason of cycle performance mainly contains the following aspects: 1) under high charge cut-ff voltage, Ni, the Co of a large amount of high valence states, the oxidation of Mn to electrolyte, cause the consumption of electrolyte and the enrichment of surperficial accessory substance, thereby accelerated the decay of circulation; 2), easily there is disproportionated reaction and cause the stripping of Mn ion in a small amount of trivalent Mn existing; 3) corrosion of HF acid to active material, causes deterioration and the digestion of metallic ion on active material surface; 4) polarization in cyclic process strengthens, and causes the fast-descending of capacity; 5) the mixing phenomenon that lithium and nickel produce in sintering process can further increase, so that reduce the coulomb efficiency of material, and further cause the capacity attenuation in cyclic process in cyclic process; 6) 104 of crystal oxygen loss also can cause electrolyte oxidation accelerating structure to destroy, and then cause circulation volume to decline.
At present, NCM ternary material being adulterated and be coated is the most common means that solves an above-mentioned difficult problem.
Doping is divided into cation doping and anion doped, is wherein mainly that employing is fluorine-ion-doped to the anion doped of NCM ternary material.Because fluorine possesses higher electronegativity, thus more stable metal level and the binder course of anion can be formed, thus reach the object of stable crystal structure.
Coated refer at materials such as the particle surface coated metal oxide of NCM material, metal fluoride, polymer, thereby stop the corrosion of HF to active material, reduce the polarization in cyclic process, the oxidation of partial rcsponse highly charged ions to electrolyte simultaneously, reaches and improves the circulation of ternary material and the object of high-temperature storage performance.
In order farthest to improve the chemical property of NCM ternary material, conventionally NCM ternary material is not only carried out doping vario-property but also is coated modification, but this needs multiple steps to realize conventionally.
In view of this, necessaryly provide a kind of novel method for preparing anode material that anion doped and surface coating modification can be combined and settle at one go.
Summary of the invention
The object of the invention is to: provide the coated and polymer surfaces film of a kind of fluorine-ion-doped, metal fluoride to process the method for preparing anode material that three settles at one go, and the positive electrode that provides the method to make.
In order to realize foregoing invention object, the invention provides a kind of preparation method of positive electrode, it comprises the following steps:
1) fluoropolymer is dissolved into and in solvent, forms A solution, and slaine is dissolved in and in identical solvent, forms B solution;
2) by A solution and B solution mixing and stirring, then add unmodified positive electrode powder, by stirring, dry and roasting at 300 DEG C～750 DEG C, obtain having fluorine-ion-doped, metal fluoride coated and the positive electrode of polymer surfaces film processing.
Compared with prior art, the preparation method of positive electrode disclosed by the invention is by selecting the suitable material modified and suitable solid phase reaction condition of control, positive electrode is carried out to fluorine-ion-doped modification, and make fluorine and source metal in polymer coated in conjunction with forming fluoride, polymer overmold is carried out to skin covering of the surface at positive electrode particle surface simultaneously and process modification, complete in the mode settling at one go that anion doped, the fluoride of positive electrode is coated, the processing of polymer surfaces film, have advantages of simple, controllability strong, easily realize.
Wherein, the structural formula of unmodified positive electrode is Li 1+xni yco zmn (1-y-z)m αo 2m in formula is selected from least one element in Zr, Mo, W, Al, Mg, Ca, Fe, 0≤x≤0.2,0.05 < y < 0.90,0.05 < z < 0.95,0≤α≤0.03.
One as the preparation method of positive electrode of the present invention is improved, and the solvent of described A solution and B solution is the one in dimethyl pyrrolidone, dimethylacetylamide, dimethyl formamide, triethyl phosphate, dimethyl suflfate.
One as the preparation method of positive electrode of the present invention is improved, described step 1) in fluoropolymer be one or both in polytetrafluoroethylene, Kynoar.
One as the preparation method of positive electrode of the present invention is improved, described step 1) in slaine be one or more the soluble-salt in Al, Ti, Zr, Mg.
In order to realize foregoing invention object, the present invention also provides a kind of positive electrode, and this positive electrode is that the method for preparing anode material described in the above-mentioned arbitrary paragraph of use makes.
One as positive electrode of the present invention is improved, and in described positive electrode, the content of fluorine accounts for the 0.01wt%～1wt% of whole positive electrode.
One as positive electrode of the present invention is improved, and in described positive electrode, the content of metal fluoride accounts for the 0.05wt%～1wt% of whole positive electrode.
Compared with prior art, the preparation method of positive electrode of the present invention anion doped, fluoride can be coated and polymer surfaces film processing three settles at one go, has greatly saved production stage, has improved production efficiency.In addition, positive electrode of the present invention at least possesses following advantage: 1) the anion doped adhesion that can increase metal ion and anion, stable crystal structure; 2) the coated coated maximum advantage of metal/metal oxide of comparing of fluoride is acid-alkali-corrosive-resisting, can reduce LiF enrichment simultaneously, reduces polarization; 3) skin covering of the surface processing can reduce contacting of electrolyte and active material to greatest extent, thereby alleviates oxidation and the corrosion of HF to active material of electrolyte.Therefore, it is adapted at using under high charge cut-ff voltage, and has higher thermal stability.
Embodiment
The positive electrode particle that the present invention makes is nucleocapsid structure, and wherein, kernel is fluorine-ion-doped Li 1+xni yco zmn (1-y-z)m αo 2m in formula is selected from least one element in Zr, Mo, W, Al, Mg, Ca, Fe, 0≤x≤0.2,0.05 < y < 0.90,0.05 < z < 0.95,0≤α≤0.03; Shell is metal fluoride layer and polymer surfaces film, and wherein metal fluoride layer is distributed in the surface of kernel, and polymer surfaces film wraps up the kernel that is distributed with metal fluoride layer completely from outermost.
In order to make goal of the invention of the present invention, technical scheme and useful technique effect more clear, below in conjunction with embodiment, the present invention is described in further detail, but, should be understood that, embodiments of the invention are only used to explain the present invention, be not intended to limit the present invention, and embodiments of the invention are not limited to the embodiment providing in specification.
Comparative example 1
By commercial hydroxide precursor Ni 0.5co 0.2mn 0.3(OH) 2with Li 2cO 3calculate, weigh according to mol ratio 1:1.02, join in ball grinder ball mill mixing 20h; In air atmosphere, according to 730 DEG C of sintering 10h, then 960 DEG C of sintering 12h, cool to room temperature with the furnace, obtain lithium nickel cobalt manganese oxygen (NCM) positive electrode; Then NCM is joined in the Al solution having dissolved, stir, filter, be dried, last 600 DEG C of sintering 4h, obtain desirable Al 2o 3coated blended positive pole material.
Embodiment 1
The first step, batching: the Li of configuration 1mol/L 2cO 3solution, stand-by; By commercial hydroxide precursor Ni 0.5co 0.2mn 0.3(OH) 2calculate, weigh according to mol ratio 1:1.02 with the LiOH solution of 1mol/L, join in ball grinder ball mill mixing 20h;
Second step, NCM is synthetic: the mixed powder that the first step is obtained is poured in alumina crucible, is warming up to sintering 10h at 700～800 DEG C with the speed of 10 DEG C/min, continues identical speed and is warming up to 900～1000 DEG C of sintering 12h, obtains the evenly LiNi of diffusion of lithium 0.5co 0.2mn 0.3o 2material; Above sintering process need to complete under elevated oxygen level atmosphere;
The 3rd step, the preparation of covering liquid: first polytetrafluoroethylene is dissolved in dimethyl pyrrolidone, forms A covering liquid; By Al (NO 3) 3be dissolved in dimethyl pyrrolidone, form B solution; Then by A and B solution mix and blend 10～60min, form AB covering liquid, stand-by;
The 4th step, coated: NCM to be joined in AB covering liquid, stir 2h; Then place it in 105 DEG C of oil baths, heating 24h then heats 4h in 350～750 DEG C, obtain anion doped, aluminum fluoride coated and the NCM material of skin covering of the surface processing.
Embodiment 2
The first step, batching: the Li of configuration 1mol/L 2cO 3solution, stand-by; By commercial hydroxide precursor Ni 0.5co 0.2mn 0.3(OH) 2calculate, weigh according to mol ratio 1:1.02 with the LiOH solution of 1mol/L, join in ball grinder ball mill mixing 20h;
Second step, NCM is synthetic: the mixed powder that the first step is obtained is poured in alumina crucible, is warming up to sintering 10h at 700～800 DEG C with the speed of 10 DEG C/min, continues identical speed and is warming up to 900～1000 DEG C of sintering 12h, obtains the evenly LiNi of diffusion of lithium 0.5co 0.2mn 0.3o 2material; Above sintering process need to complete under elevated oxygen level atmosphere;
The 3rd step, the preparation of covering liquid: first Kynoar is dissolved in dimethyl pyrrolidone, forms A covering liquid; By Zr (NO 3) 4be dissolved in dimethyl pyrrolidone, form B solution; Then by A and B solution mix and blend 10～60min, form AB covering liquid, stand-by;
The 4th step, coated: NCM to be joined in AB covering liquid, stir 2h; Then place it in 105 DEG C of oil baths, heating 24h then heats 4h in 350～750 DEG C, obtain fluorine-ion-doped, zirconium fluoride coated and the NCM material of skin covering of the surface processing.
Embodiment 3
The first step, batching: the Li of configuration 1mol/L 2cO 3solution, stand-by; By commercial hydroxide precursor Ni 0.5co 0.2mn 0.3(OH) 2calculate, weigh according to mol ratio 1:1.02 with the LiOH solution of 1mol/L, join in ball grinder ball mill mixing 20h;
Second step, NCM is synthetic: the mixed powder that the first step is obtained is poured in alumina crucible, is warming up to sintering 10h at 700～800 DEG C with the speed of 10 DEG C/min, continues identical speed and is warming up to 900～1000 DEG C of sintering 12h, obtains the evenly LiNi of diffusion of lithium 0.5co 0.2mn 0.3o 2material; Above sintering process need to complete under elevated oxygen level atmosphere;
The 3rd step, the preparation of covering liquid: first polytetrafluoroethylene is dissolved in dimethyl pyrrolidone, forms A covering liquid; By Mg (NO 3) 2be dissolved in dimethyl pyrrolidone, form B solution; Then by A and B solution mix and blend 10～60min, form AB covering liquid, stand-by;
The 4th step, coated: NCM to be joined in AB covering liquid, stir 2h; Then place it in 105 DEG C of oil baths, heating 24h then heats 4h in 350～750 DEG C, obtain fluorine-ion-doped, magnesium fluoride coated and the NCM material of skin covering of the surface processing.
Embodiment 4
The first step, batching: the Li of configuration 1mol/L 2cO 3solution, stand-by; By commercial hydroxide precursor Ni 0.5co 0.2mn 0.3(OH) 2calculate, weigh according to mol ratio 1:1.02 with the LiOH solution of 1mol/L, join in ball grinder ball mill mixing 20h;
Second step, NCM is synthetic: the mixed powder that the first step is obtained is poured in alumina crucible, is warming up to sintering 10h at 700～800 DEG C with the speed of 10 DEG C/min, continues identical speed and is warming up to 900～1000 DEG C of sintering 12h, obtains the evenly LiNi of diffusion of lithium 0.5co 0.2mn 0.3o 2material; Above sintering process need to complete under elevated oxygen level atmosphere;
The 3rd step, the preparation of covering liquid: first Kynoar is dissolved in dimethylacetylamide, forms A covering liquid; By Al (NO 3) 3be dissolved in dimethylacetylamide, form B solution; Then by A and B solution mix and blend 10～60min, form AB covering liquid, stand-by;
The 4th step, coated: NCM to be joined in AB covering liquid, stir 2h; Then place it in 105 DEG C of oil baths, heating 24h then heats 4h in 350～750 DEG C, obtain fluorine-ion-doped, magnesium fluoride coated and the NCM material of skin covering of the surface processing.
Embodiment 5
The first step, batching: the Li of configuration 1mol/L 2cO 3solution, stand-by; By commercial hydroxide precursor Ni 0.5co 0.2mn 0.3(OH) 2calculate, weigh according to mol ratio 1:1.02 with the LiOH solution of 1mol/L, join in ball grinder ball mill mixing 20h;
Second step, NCM is synthetic: the mixed powder that the first step is obtained is poured in alumina crucible, is warming up to sintering 10h at 700～800 DEG C with the speed of 10 DEG C/min, continues identical speed and is warming up to 900～1000 DEG C of sintering 12h, obtains the evenly LiNi of diffusion of lithium 0.5co 0.2mn 0.3o 2material; Above sintering process need to complete under elevated oxygen level atmosphere;
The 3rd step, the preparation of covering liquid: first polytetrafluoroethylene is dissolved in dimethylacetylamide, forms A covering liquid; By Al (NO 3) 3be dissolved in dimethylacetylamide, form B solution; Then by A and B solution mix and blend 10～60min, form AB covering liquid, stand-by;
The 4th step, coated: NCM to be joined in AB covering liquid, stir 2h; Then place it in 105 DEG C of oil baths, heating 24h then heats 4h in 350～750 DEG C, obtain fluorine-ion-doped, magnesium fluoride coated and the NCM material of skin covering of the surface processing.
Preparation experiment battery
The positive electrode that embodiment 1-5 and comparative example 1 are made is mixed into anode sizing agent with bonding agent, conductive agent respectively, and this anode sizing agent is coated on plus plate current-collecting body, then through colding pressing, dry and the operation such as cut and make positive plate; Positive plate is assembled into lithium ion battery with negative plate, electrolyte and barrier film respectively; To utilize embodiment 1-5 and the prepared battery number consecutively of comparative example 1 positive electrode is S1-S5 and D1.
Battery performance test
The lithium ion battery that is numbered S1-S5 and D1 is evaluated as follows, be the results are shown in table 1.
Cycle performance test: at 60 DEG C, with the rate of charge of 0.7C by constant-current charging of battery to 4.4V, then with the rate of charge constant voltage charge of 0.05C to 4.4V, be then discharged to 3.0V with the discharge-rate of 1C; Repeatedly carry out this charge and discharge cycles 400 times, measure the discharge capacity of circulation time and the discharge capacity of the 400th circulation time for the first time, obtain the capability retention after circulation, formula is: capability retention=(discharge capacity of the 400th circulation time)/(discharge capacity of circulation time for the first time) × 100% after circulation.
Security performance test: at 25 DEG C, with the rate of charge of 0.5C by constant-current charging of battery to 4.45V, then with the rate of charge constant voltage charge of 0.05C to 4.45V; Leave standstill after 1h, battery is put into convection oven, oven temperature is set as to 30min and is warming up to 150 DEG C, and continue baking 6 hours at 150 DEG C; Whether burn as the index of weighing battery safety quality using battery in bake process.
Table 1, respectively organize the performance test results of lithium ion battery
Battery numbering Capability retention after 400 circulations Whether burn
S1 89％ No
S2 92％ No
S3 86％ No
S4 88％ No
S5 86％ No
D1 75％ Be
As can be seen from Table 1: lithium ion battery prepared by the positive electrode that adopts the present invention to make, it experiences 400 Capacitance reserves after circulation and still remains on more than 85% under high voltage hot conditions, higher than the battery capacity conservation rate that is numbered D1, this shows that the prepared positive electrode of the present invention can improve the cycle performance of battery under high pressure-temperature condition far away.In addition, can not there is not like that combustion phenomena to the battery of comparative example 1 in lithium ion battery prepared by the positive electrode that adopts the present invention to make, illustrate that it has higher security performance under identical test condition.
The announcement of book and instruction according to the above description, those skilled in the art in the invention can also carry out suitable change and amendment to above-mentioned execution mode.Therefore, the present invention is not limited to embodiment disclosed and described above, also should fall in the protection range of claim of the present invention modifications and changes more of the present invention.In addition,, although used some specific terms in this specification, these terms just for convenience of description, do not form any restriction to the present invention.

Claims (8)

1. a preparation method for positive electrode, is characterized in that comprising the following steps:
1) fluoropolymer is dissolved into and in solvent, forms A solution, and slaine is dissolved in and in identical solvent, forms B solution;
2) by A solution and B solution mixing and stirring, then add unmodified positive electrode powder, by stirring, dry and roasting at 300 DEG C～750 DEG C, obtain having fluorine-ion-doped, metal fluoride coated and the positive electrode of polymer surfaces film processing.
2. the preparation method of positive electrode according to claim 1, the structural formula of described unmodified positive electrode is Li 1+xni yco zmn (1-y-z)m αo 2wherein M is selected from least one element in Zr, Mo, W, Al, Mg, Ca, Fe, 0≤x≤0.2,0.05 < y < 0.90,0.05 < z < 0.95,0≤α≤0.03.
3. the preparation method of positive electrode according to claim 1, is characterized in that: described solvent is the one in dimethyl pyrrolidone, dimethylacetylamide, dimethyl formamide, triethyl phosphate, dimethyl suflfate.
4. the preparation method of positive electrode according to claim 1, is characterized in that: described step 1) in fluoropolymer be one or both in polytetrafluoroethylene, Kynoar.
5. the preparation method of positive electrode according to claim 1, is characterized in that: described step 1) in slaine be one or more the soluble-salt in Al, Ti, Zr, Mg.
6. a positive electrode, is characterized in that: described positive electrode makes via the preparation method of any one positive electrode in claim 1 to 5.
7. positive electrode according to claim 6, is characterized in that: in described positive electrode, the content of fluorine accounts for the 0.01wt%～1wt% of whole positive electrode.
8. positive electrode according to claim 6, is characterized in that: in described positive electrode, the content of metal fluoride accounts for the 0.05wt%～1wt% of whole positive electrode.
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CN105990577A (en) * 2016-06-15 2016-10-05 电子科技大学 LiNi0.6-xCo0.2Mn0.2AlxO2-yFy positive electrode material for lithium ion cell and preparation method thereof
CN106848260A (en) * 2017-03-25 2017-06-13 宁波吉电鑫新材料科技有限公司 A kind of non-acid system liquid phase synthesis C/Cu, Zr/ZrF4Compound zirconium fluoride anode material for lithium-ion batteries and preparation method thereof
CN106848259A (en) * 2017-03-25 2017-06-13 宁波吉电鑫新材料科技有限公司 A kind of continuous conduction original position C/Ag, Zr/ZrF4Compound zirconium fluoride anode material for lithium-ion batteries and preparation method thereof
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CN106953081A (en) * 2017-03-25 2017-07-14 宁波吉电鑫新材料科技有限公司 A kind of non-acid system liquid phase synthesis C/Ag, Zr/ZrF4Compound zirconium fluoride anode material for lithium-ion batteries and preparation method thereof
CN106953084A (en) * 2017-03-25 2017-07-14 宁波吉电鑫新材料科技有限公司 A kind of continuous conduction original position C/Ag, metal solid solution/Cr3+Adulterate ZrF4Positive pole and preparation method
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CN107215903A (en) * 2017-06-07 2017-09-29 四川科能锂电有限公司 The preparation method of high voltage tertiary cathode material
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