CN105140482B - A kind of modification lithium-ion battery anode material and preparation method thereof - Google Patents

A kind of modification lithium-ion battery anode material and preparation method thereof Download PDF

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CN105140482B
CN105140482B CN201510480990.8A CN201510480990A CN105140482B CN 105140482 B CN105140482 B CN 105140482B CN 201510480990 A CN201510480990 A CN 201510480990A CN 105140482 B CN105140482 B CN 105140482B
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tungsten
lithium
molybdenum
preparation
positive electrode
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CN105140482A (en
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李新海
郑小波
王志兴
郭华军
黄振军
彭文杰
胡启阳
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Central South University
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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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • H01M4/50—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
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a kind of modification lithium-ion battery anode material is disclosed, including positive electrode ontology and the tungsten acid lithium layer for being coated on the positive electrode body surface, wherein the mass ratio of the tungsten acid lithium layer and positive electrode ontology is 0.5~5:100.The preparation method of the present invention, including step in detail below：1) lithium salts and tungsten source are added in into dissolving in solvent and forms solution；2) positive electrode ontology is added in the solution after step 1), constant temperature is dry after stirring evenly, and obtains presoma；3) presoma is warming up to 250~550 DEG C to roast, the modification lithium-ion battery anode material is obtained after cooling.The modification lithium-ion battery anode material of the present invention is coated with one layer of tungsten acid lithium layer on the surface of cell positive material, can preferably completely cut off CO in air2、H2O and electrolyte greatly improve the cyclical stability of the air storge quality of material, high-temperature electrolyte storge quality and material electrochemical.

Description

A kind of modification lithium-ion battery anode material and preparation method thereof
Technical field
The invention belongs to metallurgical electrode material field more particularly to a kind of modification lithium-ion battery anode material and its preparations Method.
Background technology
Since tungsten and molybdenum are all closely similar in atoms outermost electronics arrangement, ionic radius etc., tungsten, molybdenum compound are in water State in solution is also closely similar, and in alkaline solution, the common valence state of tungsten, molybdenum is+6 valencys, usually with WO4 2-And Mo4 2- In the presence of being then all readily formed isopolyacid and heteropoly acid, the behavior in the solution of tungsten compound in alkalescent and acid solution It is similar, for tungsten, molybdenum smelt in tungsten separation brings very big difficulty.Therefore in the smelting process of tungsten, tungsten detaches As a letter problem to be solved.
Lithium ion battery is as a new generation's environmental protection, high-energy battery, it has also become one of emphasis of battery industry development.It grinds at present Studying carefully more anode material for lithium-ion batteries mainly has LiNiO2、LiMPO4(M=Fe, Mn, V), LiCoO2、LiMn2O4、 LiNi1-x-yCoxMnyO2Deng, but there are the deficiency of itself and defects.LiNiO2It is difficult itself to there is synthesis, structural phase transition and heat The shortcomings of stability is poor and be difficult to functionization.Positive electrode LiMPO4, it is wide due to nontoxic, at low cost and good stability General research, but limit its large-scale use due to the shortcomings such as its poorly conductive, volume energy density be low.LiCoO2Middle cobalt money Source reserves are limited, expensive.The LiMn of spinel-type2O4Material construction is low, has good electro and ionic conductivity, But in charging process Mn3+Ion there are Jahn-Teller effects due to causing spinel-type to turn to tetrahedron manganese and oxygen compound The irreversible transition of change, causes capacitance loss；In addition, spinelle LiMn2O4Capacity it is relatively low, high-temperature behavior is poor.In addition these are being just Pole material also deposits the unstable grade common drawbacks of memory structure in storage characteristics difference in air and Charging state electrolyte.Therefore, it grinds Study carefully a kind of method being modified to anode material for lithium-ion batteries, effectively prevented just under the premise of not loss material specific capacity Pole material is reacted with electrolyte, improves the structural stability of positive electrode, is reduced positive electrode and is stored hygroscopicity in air, changes The security performance and cyclical stability of kind material, required by being current situation.
Invention content
The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, provide a kind of modification lithium-ion battery anode Material and preparation method thereof.
In order to solve the above technical problems, technical solution proposed by the present invention is：
A kind of modification lithium-ion battery anode material including positive electrode ontology and is coated on described this body surface of positive electrode The tungsten acid lithium layer in face, wherein the mass ratio of the tungsten acid lithium layer and positive electrode ontology is 0.5~5:100.Tungsten lithium molybdate Opposite positive electrode ontology quality it is too low when, clad does not have effect；The too high capacity that can lead to battery of relative mass Reduced performance even results in material other penalties.
Above-mentioned modification lithium-ion battery anode material, it is preferred that the positive electrode ontology is LiNiO2、LiCoO2、 LiMn2O4、LiMPO4、xLi2MnO3·(1-x)LiMO2Or one or more of their derivative, wherein M for Fe, V, Ni, Co or Mn, 0≤x≤1.
The inventive concept total as one, the present invention also provides a kind of preparations of above-mentioned modification lithium-ion battery anode material Method includes the following steps：
1) lithium salts and tungsten source are added in into dissolving in solvent and forms solution；
2) positive electrode ontology is added in the solution after step 1), constant temperature is dry after stirring evenly, and obtains presoma；
3) presoma is warming up to 250~550 DEG C to roast, the modification lithium-ion battery is being obtained just after cooling Pole material.
Above-mentioned preparation method, it is preferred that in the step 1), the tungsten source is not except in molybdenum in tungsten metallurgical process Between product, molybdenum metallurgical process do not remove the intermediate products of tungsten or the mixture of tungsten source and molybdenum source.
Above-mentioned preparation method, it is preferred that the intermediate products in the tungsten, molybdenum metallurgical process are the ammonium salt containing tungsten, contain One or more of oxide and tungsten acid of tungsten.
Above-mentioned preparation method, it is preferred that in the step 1), tungsten source is in the oxide, wolframic acid and tungsten ammonium salt of tungsten It is one or more of；One or more of oxide, molybdic acid and the molybdenum ammonium salt of molybdenum source for molybdenum.
Above-mentioned preparation method, it is preferred that the oxide of the tungsten is tungstic acid；The tungsten ammonium salt for ammonium metatungstate and One or more of ammonium tungstate；The oxide of the molybdenum is molybdenum trioxide；The molybdenum ammonium salt for positive ammonium molybdate, ammonium paramolybdate, One or more of ammonium dimolybdate and ammonium tetramolybdate.
Above-mentioned preparation method, it is preferred that in the step 1), lithium salts is lithium carbonate, lithium acetate, lithium hydroxide and lemon One or more of sour lithium.
Above-mentioned preparation method, it is preferred that in the step 2), the temperature of constant temperature stirring is 25~80 DEG C；Dry temperature Spend is 120~200 DEG C.
Above-mentioned preparation method, it is preferred that in the step 3), the time of roasting is 2~8h；Heating rate is 3~10 ℃/min
Compared with prior art, the advantage of the invention is that：
1) modification lithium-ion battery anode material of the invention is coated with one layer of tungsten acid on the surface of cell positive material Lithium layer, due to tungsten acid lithium layer in air with preferable stability is respectively provided in electrolyte, can preferably completely cut off in air CO2、H2O and electrolyte greatly improve the air storge quality of material, high-temperature electrolyte storge quality and material electrochemical Cyclical stability.
2) preparation method of the invention has carried out tungsten lithium molybdate to lithium ion anode material using the method for liquid phase coating and has answered Close cladding, intermediate products of the raw material used for tungsten, in molybdenum metallurgical process, the raw material used need not move through tungsten compound by In property and its similar and lead to a great problem in field of metallurgy --- the process of tungsten separation, and then further save Cost of material is saved.
3) preparation method of the invention coats tungsten lithium molybdate using liquid phase method, and required equipment is very simple, only needs common Mixing plant, this greatly reduces the cost of production, and easily operated, is easy to implement industrialized production.
4) preparation method of the invention coats tungsten lithium molybdate using liquid phase method, and the surface of positive electrode ontology coats very Completely, dead angle, and then further CO in complete isolation air are not stayed2、H2O and electrolyte greatly improve the electrochemistry of material Energy.
Description of the drawings
Fig. 1 be the embodiment of the present invention 2 in it is unmodified before positive electrode SEM figure.
Fig. 2 is the SEM figures of anode material for lithium-ion batteries modified in the embodiment of the present invention 2.
Fig. 3 is the XRD diagram of modification lithium-ion battery anode material in the embodiment of the present invention 2.
Fig. 4 is the EDS figures of modification lithium-ion battery anode material in the embodiment of the present invention 2.
Fig. 5 is the cycle performance test chart that battery is made in modification lithium-ion battery anode material in the embodiment of the present invention 2.
Specific embodiment
For the ease of understanding the present invention, the present invention is made below in conjunction with Figure of description and preferred embodiment more complete Face meticulously describes, but the protection scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention Protection domain.
Except there is a special instruction, the various reagents used in the present invention, raw material be can be commercially commodity or Person can pass through product made from well known method.
Embodiment 1：
A kind of modification lithium-ion battery anode material of the present invention, including positive electrode ontology LiNi0.5Co0.2Mn0.3O2With It is coated on LiNi0.5Co0.2Mn0.3O2The tungsten acid lithium layer on surface, wherein tungsten acid lithium layer and LiNi0.5Co0.2Mn0.3O2Quality Than being 3:100.
The preparation method of the modification lithium-ion battery anode material of the present embodiment, includes the following steps：
1) lithium acetate and tungsten metallurgical process are not had by forming solution except the intermediate products APT of molybdenum is added to the water dissolving.
2) by LiNi0.5Co0.2Mn0.3O2(its addition is with tungsten lithium molybdate and LiNi0.5Co0.2Mn0.3O2Mass ratio is 3:100 Amount calculate) add in step 1) after solution in, after 50 DEG C of constant temperature stir evenly, be placed in 150 DEG C of air dry oven and done It is dry, obtain presoma.
3) presoma is warming up to 350 DEG C with the heating rate of 5 DEG C/min and carries out roasting 5h, modified lithium is obtained after cooling Ion battery positive electrode.
By the present embodiment it is unmodified before positive electrode LiNi0.5Co0.2Mn0.3O2After battery is made, 1C cycles are carried out Performance test, the capacity retention ratio of battery is 75% after 100 loop tests.The modification lithium-ion electricity that this implementation is obtained Battery is made in pond positive electrode, carries out 1C cycle performance tests, and the capacity retention ratio of battery improves after 100 loop tests To 87%.
Embodiment 2：
A kind of modification lithium-ion battery anode material of the present invention, including positive electrode ontology LiNi0.8Co0.1Mn0.1O2With It is coated on LiNi0.8Co0.1Mn0.1O2The tungsten acid lithium layer on surface, wherein tungsten acid lithium layer and LiNi0.8Co0.1Mn0.1O2Quality Than being 0.5:100.
The preparation method of the modification lithium-ion battery anode material of the present embodiment, includes the following steps：
1) by LiOH, H2WO4And H2MoO4It adds in dissolving in the mixed liquor of water and alcohol and forms solution.
2) by LiNi0.8Co0.1Mn0.1O2(its addition is with tungsten lithium molybdate and LiNi0.8Co0.1Mn0.1O2Mass ratio is 0.5: 100 amount calculates) it adds in the solution after step 1), after 50 DEG C of constant temperature stir evenly, it is placed in 120 DEG C of air dry oven and carries out It is dry, obtain presoma.
3) presoma is warming up to 350 DEG C with the heating rate of 5 DEG C/min and carries out roasting 5h, modified lithium is obtained after cooling Ion battery positive electrode.
The SEM figures point of lithium ion anode material and modified anode material for lithium-ion batteries before the present embodiment is unmodified Not as depicted in figs. 1 and 2, by it was found that, modified anode material for lithium-ion batteries is for Fig. 1 in Fig. 2, material Surface blur, and there is cotton-shaped substance to generate, boundary line is unintelligible between primary particle, this is because anode material for lithium-ion batteries table Bread covers the reason of one layer of tungsten acid lithium layer.
The XRD diagram for the modification lithium-ion battery anode material that the present embodiment obtains is as shown in figure 3,20-40 ° of appearance in figure H2WO4And H2MoO4Characteristic peak, it was demonstrated that there are tungsten lithium molybdate complex chemical compound in material.
The EDS figures for the modification lithium-ion battery anode material that the present embodiment obtains are as shown in figure 4, in addition to this in positive electrode There are Ni, Co, Mn for body, have also appeared W, Mo peak, it was demonstrated that have the presence of tungsten, molybdenum.
Following for battery is made in positive electrode of the present embodiment before unmodified and modified anode material for lithium-ion batteries Ring performance test figure as shown in figure 5, after battery is made in the positive electrode before unmodified, carries out 2C cycle performance tests, passes through The capacity retention ratio of battery is 71% after 100 loop tests, and modification lithium-ion battery anode material is made battery progress 1C and follows Ring performance test, the capacity retention ratio of battery is increased to 86% after 100 loop tests.
Embodiment 3：
A kind of modification lithium-ion battery anode material of the present invention, including positive electrode ontology Li1.2Mn0.54Co0.13Ni0.13O2Be coated on Li1.2Mn0.54Co0.13Ni0.13O2The tungsten acid lithium layer on surface, wherein tungsten lithium molybdate Layer and Li1.2Mn0.54Co0.13Ni0.13O2Mass ratio is 2:100.
The preparation method of the modification lithium-ion battery anode material of the present embodiment, includes the following steps：
1) by lithium acetate, (NH4)10W12O41·nH2O and (NH4)2MoO4It adds in dissolving in ammonium hydroxide and forms solution.
2) by Li1.2Mn0.54Co0.13Ni0.13O2(its addition is with tungsten lithium molybdate and Li1.2Mn0.54Co0.13Ni0.13O2Quality Than being 2:100 amount calculates) it adds in the solution after step 1), after 80 DEG C of constant temperature stir evenly, it is placed in 120 DEG C of forced air drying Case is dried, and obtains presoma.
3) presoma is warming up to 500 DEG C with the heating rate of 5 DEG C/min and carries out roasting 6h, modified lithium is obtained after cooling Ion battery positive electrode.
By the present embodiment it is unmodified before positive electrode Li1.2Mn0.54Co0.13Ni0.13O2After battery is made, carry out Charge and discharge are carried out under 4.6V, 1C multiplying power, the capacity retention ratio of battery is 78.6% after 100 loop tests.This is implemented Battery is made in obtained modification lithium-ion battery anode material, carries out 1C cycle performance tests, electric after 100 loop tests The capacity retention ratio in pond is increased to 84.6%.

Claims (8)

1. a kind of preparation method of modification lithium-ion battery anode material, which is characterized in that including positive electrode ontology and cladding In the tungsten acid lithium layer of the positive electrode body surface, wherein the tungsten acid lithium layer and the mass ratio of positive electrode ontology are 0.5~5:100；The preparation method includes the following steps：
1）Lithium salts and tungsten source are added in into dissolving in solvent and form solution；The tungsten source is not except in molybdenum in tungsten metallurgical process Between product, molybdenum metallurgical process do not remove the intermediate products of tungsten or the mixture of tungsten source and molybdenum source；
2）Positive electrode ontology is added in into step 1）In solution afterwards, constant temperature is dry after stirring evenly, and obtains presoma；
3）Presoma is warming up to 250~550 DEG C to roast, the modification lithium-ion battery anode material is obtained after cooling Material.
2. preparation method as described in claim 1, which is characterized in that the positive electrode ontology is LiNiO2、LiCoO2、 LiMn2O4 、LiMPO4、xLi2MnO3·(1-x)LiMO2Or one or more of their derivative, wherein M for Fe, V, One or more of Ni, Co and Mn, 0≤x≤1.
3. preparation method as described in claim 1, which is characterized in that intermediate products in the tungsten, molybdenum metallurgical process be containing One or more of the ammonium salt of tungsten, the oxide containing tungsten and tungsten acid.
4. preparation method as described in claim 1, which is characterized in that the step 1）In, tungsten source is oxide, the wolframic acid of tungsten One or more of with tungsten ammonium salt；One or more of oxide, molybdic acid and the molybdenum ammonium salt of molybdenum source for molybdenum.
5. preparation method as claimed in claim 4, which is characterized in that the oxide of the tungsten is tungstic acid；The tungsten ammonium Salt is one or more of ammonium metatungstate and ammonium tungstate；The oxide of the molybdenum is molybdenum trioxide；The molybdenum ammonium salt is positive molybdenum One or more of sour ammonium, ammonium paramolybdate, ammonium dimolybdate and ammonium tetramolybdate.
6. such as Claims 1 to 4 any one of them preparation method, which is characterized in that the step 1）In, lithium salts is carbonic acid One or more of lithium, lithium acetate, lithium hydroxide and lithium citrate.
7. such as Claims 1 to 4 any one of them preparation method, which is characterized in that the step 2）In, the temperature of constant temperature stirring Spend is 25~80 DEG C；Dry temperature is 120~200 DEG C.
8. such as Claims 1 to 4 any one of them preparation method, which is characterized in that the step 3）In, the time of roasting is 2~8h；Heating rate is 3~10 DEG C/min.
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CN108649193B (en) * 2018-04-24 2021-07-23 芜湖浙鑫新能源有限公司 Modified lithium ion battery anode material and preparation method thereof
CN108493429A (en) * 2018-05-03 2018-09-04 中南大学 The preparation method of anode composite material of lithium ion battery
CN110137464B (en) * 2019-05-13 2022-11-01 湖北锂诺新能源科技有限公司 Lithium-rich nickel cobalt manganese oxide positive electrode material coated by vanadium lithium molybdate, positive electrode piece and preparation method thereof, and lithium battery
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CN113054168B (en) * 2019-12-28 2022-06-03 巴斯夫杉杉电池材料有限公司 Tungsten-molybdenum composite coated ternary cathode material and preparation method thereof
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CN113078316B (en) * 2021-03-23 2022-04-12 电子科技大学 Lithium molybdate-coated lithium-rich manganese-based positive electrode material and preparation method and application thereof
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