CN107093725B - A kind of method of modifying of layered lithium manganate material - Google Patents

A kind of method of modifying of layered lithium manganate material Download PDF

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CN107093725B
CN107093725B CN201710298921.4A CN201710298921A CN107093725B CN 107093725 B CN107093725 B CN 107093725B CN 201710298921 A CN201710298921 A CN 201710298921A CN 107093725 B CN107093725 B CN 107093725B
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lithium
manganate
modifying
lithium manganate
layered lithium
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CN201710298921.4A
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CN107093725A (en
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刘兴亮
杨茂萍
李道聪
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合肥国轩高科动力能源有限公司
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    • H—ELECTRICITY
    • H01—BASIC 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—BASIC 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—BASIC 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—BASIC 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 present invention discloses a kind of method of modifying of layered lithium manganate material, comprising the following steps: prepares manganate precursor for lithium, burnt zirconic acid cerium (Ce using hydro-thermal method2Zr2O7) presoma, ball milling or ultrasonic mixing, Ce is made after calcining2Zr2O7The layered lithium manganate material of cladding；Ce made from this method2Zr2O7Material is evenly coated at LiMn2O4 surface, and clad is effectively reduced LiMn2O4 and contacts with the direct of electrolyte, reduces the dissolution of electrolyte erosion and manganese；Ce2Zr2O7Material surface clad chemical stability is good, in charge and discharge process repeatedly, can effectively keep the stable structure of LiMn2O4, promote the multiplying power and cycle performance of LiMn2O4；The preparation method of modified layered lithium manganate material, technical process is simple, is readily produced, and is with a wide range of applications in field of lithium ion battery.

Description

A kind of method of modifying of layered lithium manganate material

Technical field

The invention belongs to battery materials to prepare technical field of modification, and in particular to a kind of lithium manganate cell positive electrode material changes Property method.

Technical background

21 century, energy crisis and environmental degradation have become the big urgent problem to be solved in the world today two, and due to sky Between the fields such as technology, mobile communication, guided missile, aerospace, electric car fast development, to the pollution-free electrochmical power source of high-performance Demand sharp increase.Lithium ion battery belongs to clean energy resource field, with safety is good, cyclicity is good, the service life is long, nontoxic nothing The advantages that pollution, becomes the first choice of power battery.LiMn2O4 because its material source it is abundant, it is cheap, have a safety feature Etc. advantages, be constantly subjected to the concern learned both at home and abroad.The theoretical specific capacity of layered lithium manganate is 285mAh/g, is that one kind has very much The lithium ion anode material of application prospect.

From layered lithium manganate synthetic method, high temperature solid-state method, sol-gel method, hydro-thermal method are synthesis stratiform mangaic acids The main method of lithium, wherein high temperature solid-state method due to technical process it is simple, reaction condition is easily controllable, becomes current industrial production Main method；Sol-gel method is that the raw material that will be needed is distributed to the solution that low viscosity is formed in solvent respectively, can be very The uniformity of molecular level is obtained in the short time；When forming gel, reactant can be made to reach the mixing of molecular level, closed It is uniform at the product cut size gone out；Hydro-thermal method is usually to take water as a solvent, and is heated by reactor, is provided under high-temperature and high-pressure conditions The specific physical chemical environment that can not be provided under normal pressure makes predecessor react to obtain sufficiently, forms non-crystalline phase, formed after calcining Finished product manganate cathode material for lithium.

But due in lithium manganate material in charge and discharge process, LiMnO2Easily to the Li of spinel-like structural2Mn2O4Phase turns Become, lead to the rapid decaying of its capacity, in manganate cathode material for lithium the problems such as manganese dissolution in the electrolytic solution, limits manganese always The development of sour lithium.

Summary of the invention

In order to solve the above technical problems, the present invention provides a kind of modification sides of lithium ion anode layered lithium manganate material Method, the method for modifying make Ce2Zr2O7It is coated on LiMn2O4 surface, promotes the high rate performance and cycle performance of lithium manganate material.

Technical scheme is as follows:

1, a kind of method of modifying of layered lithium manganate material, which comprises the following steps:

(1) preparation of layered lithium manganate presoma: being (2.5-5) by element Li:Mn molar ratio: 1 weighs lithium source, three oxidations Two manganese are placed in autoclave, and deionized water is added by the solid content of 20-50%, after mixing evenly, permanent at 140-220 DEG C Warm 10-40h, natural cooling after filtration washing 3-10 times, obtain dried feed A after dry in 100-150 DEG C；

(2) burnt zirconic acid cerium Ce2Zr2O7The preparation of presoma: being that weigh cerium source, zirconium source complete by 1:1 by Elements C e:Zr molar ratio Fully dissolved is made into mixed solution in deionized water, and ammonium hydroxide is added dropwise, and controls mixed solution pH value in 8-11, is stirred to react 1-3h, It is transferred in autoclave, the isothermal reaction 10-20h at 180-220 DEG C, natural cooling, after filtration washing 3-10 times, in Dried feed B is obtained after 100-130 DEG C of drying；

(3) it is 1:(0.01-0.1 by element Li:Ce molar ratio) weigh the dried feed A of step (1) and the drying of step (2) Expect B, ball milling is carried out as dispersing agent using dehydrated alcohol or ultrasonic mixing is handled, in 100-130 DEG C of dry obtained dried feed C；

(4) the dried feed C that step (3) obtains is placed under protective atmosphere, is obtained after being warming up to 600-800 DEG C of calcining 5-15h To burnt zirconic acid cerium Ce2Zr2O7The layered lithium manganate positive electrode of cladding.

2, further scheme, the lithium source in the step (1) are or mixtures thereof lithium nitrate, one kind of lithium hydroxide.

3, further scheme, the cerium source in the step (2) be cerous nitrate, ammonium ceric nitrate, cerous sulfate one kind or it is mixed Object is closed, the zirconium source in the step (2) is or mixtures thereof zirconium chloride, one kind of zirconium nitrate.

4, further scheme, the protective atmosphere in the step (4) are high pure nitrogen, high-purity argon gas, high-purity helium.

The method of modifying of layered lithium manganate of the present invention, its advantages are shown in:

(1) layered lithium manganate presoma is synthesized using hydro-thermal method, this method has formed LiMn2O4 phase, LiMn2O4 structure is made to become In stabilization；Burnt zirconic acid cerium Ce is synthesized using hydro-thermal method2Zr2O7Presoma, this method have formed Ce2Zr2O7Phase makes Ce2Zr2O7Material Material structure tends towards stability；

(2) by burnt zirconic acid cerium Ce2Zr2O7It is uniformly mixed with manganate precursor for lithium, then carries out calcining step, so that burnt zirconic acid Cerium Ce2Zr2O7It is more uniform that material coats LiMn2O4；

(3) burnt zirconic acid cerium Ce2Zr2O7Material is evenly coated at LiMn2O4 surface, and the formation of clad effectively reduces mangaic acid Lithium is directly contacted with electrolyte, reduces the dissolution of electrolyte erosion and manganese；

(4) modified layered lithium manganate material, burnt zirconic acid cerium Ce2Zr2O7Material surface clad chemical stability is good, In charge and discharge process repeatedly, the stable structure of LiMn2O4 can be effectively kept, promotes the multiplying power and cycle performance of LiMn2O4；

(5) preparation method of modified layered lithium manganate material, technical process is simple, is easy to test, in lithium-ion electric Pond field is with a wide range of applications.

Specific Contrast on effect example, it is seen that shown in attached drawing, the manganese of 1 technical solution of the present invention of attached drawing and comparative example preparation Sour lithium material different multiplying and cycle performance compare figure.Comparative example is prepared particular by following steps: (1) Layered Manganese The preparation of sour lithium presoma: being that 2.5:1 weighs lithium hydroxide, manganese sesquioxide managnic oxide is placed in reaction under high pressure by element Li:Mn molar ratio In kettle, deionized water, after mixing evenly, constant temperature 10h, natural cooling, filtration washing at 140 DEG C is added by 20% solid content After 3 times, dried feed A is obtained after dry in 100 DEG C；(2) the dried feed A that step (1) obtains is placed in high pure nitrogen protective atmosphere Under, Ce is obtained after being warming up to 600 DEG C of calcining 5h2Zr2O7The layered lithium manganate positive electrode of cladding.

In technical solution of the present invention material 0.1,0.2,0.5,1C multiplying power first discharge specific capacity be respectively 180.12, 172.40,164.54,159.61mAh/g, the capacity retention ratio that 50 times are recycled under 1C multiplying power is 95.60%；And comparative example The material of preparation 0.1,0.2,0.5,1C multiplying power first discharge specific capacity be respectively 167.26,156.78,149.12, The capacity retention ratio that 50 times are recycled under 141.05mAh/g, 1C multiplying power is 92.7%.Ce prepared by the present embodiment 12Zr2O7Cladding It is real that the layered lithium manganate positive electrode either cycle performance of the specific capacity of phase same multiplying or 1C multiplying power is substantially better than comparison Apply example.

Detailed description of the invention:

Attached drawing 1 is mode of the present invention compared with lithium manganate material different multiplying and cycle performance prepared by comparative example Figure.

Specific embodiment

Embodiment 1

(1) preparation of layered lithium manganate presoma: being that 2.5:1 weighs lithium hydroxide, three oxidations by element Li:Mn molar ratio Two manganese are placed in autoclave, and deionized water is added by 20% solid content, after mixing evenly, the constant temperature 10h at 140 DEG C, Natural cooling after filtration washing 3 times, obtains dried feed A after dry in 100 DEG C；

(2)Ce2Zr2O7The preparation of presoma: being that weigh cerous nitrate, zirconium chloride complete by 1:1 by Elements C e:Zr molar ratio Dissolution is made into mixed solution in deionized water, and ammonium hydroxide is added dropwise, and control mixed solution pH value is stirred to react 1h 8, shifts supreme It presses in reaction kettle, the isothermal reaction 10h at 180 DEG C, natural cooling, after filtration washing 3 times, obtains drying after dry in 100 DEG C Expect B；

It (3) is that 1:0.01 weighs the dried feed A of step (1) and the dried feed B of step (2) by element Li:Ce molar ratio, with Dehydrated alcohol is that dispersing agent carries out ball milling mixing processing, in 100 DEG C of dry obtained dried feed C；

(4) the dried feed C that step (3) obtains is placed under high pure nitrogen protective atmosphere, is obtained after being warming up to 600 DEG C of calcining 5h To Ce2Zr2O7The layered lithium manganate positive electrode of cladding.

Embodiment 2

(1) preparation of layered lithium manganate presoma: being that 3:1 weighs lithium nitrate, manganese sesquioxide managnic oxide by element Li:Mn molar ratio It is placed in autoclave, deionized water is added by 25% solid content, after mixing evenly, the constant temperature 15h at 160 DEG C is natural It is cooling, after filtration washing 5 times, dried feed A is obtained after dry in 110 DEG C；

(2)Ce2Zr2O7The preparation of presoma: being that weigh ammonium ceric nitrate, zirconium nitrate complete by 1:1 by Elements C e:Zr molar ratio Dissolution is made into mixed solution in deionized water, and ammonium hydroxide is added dropwise, and controls mixed solution pH value 9, is stirred to react 1.5h, is transferred to In autoclave, the isothermal reaction 12h at 190 DEG C, natural cooling after filtration washing 4 times, is done after dry in 105 DEG C Dry material B；

It (3) is that 1:0.03 weighs the dried feed A of step (1) and the dried feed B of step (2) by element Li:Ce molar ratio, with Dehydrated alcohol is that dispersing agent carries out ball milling mixing processing, in 100 DEG C of dry obtained dried feed C；

(4) the dried feed C that step (3) obtains is placed under high-purity argon gas protective atmosphere, is obtained after being warming up to 650 DEG C of calcining 7h To Ce2Zr2O7The layered lithium manganate positive electrode of cladding.

0.1C multiplying power first discharge specific capacity is 182.46mAh/g in the present embodiment, and 0.2C, 0.5C, 1C multiplying power are put for the first time Electric specific capacity is respectively 174.68,166.82,162.21mAh/g, and the capacity retention ratio for recycling 50 times under 1C multiplying power is 96.47%.

Embodiment 3

(1) preparation of layered lithium manganate presoma: being that 3.5:1 weighs lithium hydroxide, three oxidations by element Li:Mn molar ratio Two manganese are placed in autoclave, and deionized water is added by 30% solid content, after mixing evenly, the constant temperature 20h at 170 DEG C, Natural cooling after filtration washing 7 times, obtains dried feed A after dry in 120 DEG C；

(2)Ce2Zr2O7The preparation of presoma: being that weigh cerous sulfate, zirconium chloride complete by 1:1 by Elements C e:Zr molar ratio Dissolution is made into mixed solution in deionized water, and ammonium hydroxide is added dropwise, and control mixed solution pH value is stirred to react 2h 9, shifts supreme It presses in reaction kettle, the isothermal reaction 15h at 200 DEG C, natural cooling, after filtration washing 6 times, obtains drying after dry in 115 DEG C Expect B；

It (3) is that 1:0.05 weighs the dried feed A of step (1) and the dried feed B of step (2) by element Li:Ce molar ratio, with Dehydrated alcohol is that dispersing agent carries out ultrasonic mixing processing, in 120 DEG C of dry obtained dried feed C；

(4) the dried feed C that step (3) obtains is placed under high-purity argon gas protective atmosphere, after being warming up to 700 DEG C of calcining 10h Obtain Ce2Zr2O7The layered lithium manganate positive electrode of cladding.

0.1C multiplying power first discharge specific capacity is 183.45mAh/g in the present embodiment, 0.2,0.5,1C multiplying power discharges for the first time Specific capacity is respectively 175.12,167.21,152.68mAh/g, and the capacity retention ratio that 50 times are recycled under 1C multiplying power is 96.72%.

Embodiment 4

(1) preparation of layered lithium manganate presoma: being that 4:1 weighs lithium nitrate, manganese sesquioxide managnic oxide by element Li:Mn molar ratio It is placed in autoclave, deionized water is added by 40% solid content, after mixing evenly, the constant temperature 30h at 200 DEG C is natural It is cooling, after filtration washing 8 times, dried feed A is obtained after dry in 130 DEG C；

(2)Ce2Zr2O7The preparation of presoma: being that weigh cerous nitrate, zirconium nitrate completely molten by 1:1 by Elements C e:Zr molar ratio Solution is made into mixed solution in deionized water, and ammonium hydroxide is added dropwise, and controls mixed solution pH value 10, is stirred to react 2.5h, is transferred to In autoclave, the isothermal reaction 15h at 200 DEG C, natural cooling after filtration washing 7 times, is done after dry in 120 DEG C Dry material B；

It (3) is that 1:0.07 weighs the dried feed A of step (1) and the dried feed B of step (2) by element Li:Ce molar ratio, with Dehydrated alcohol is that dispersing agent carries out ultrasonic mixing processing, in 120 DEG C of dry obtained dried feed C；

(4) the dried feed C that step (3) obtains is placed under high-purity helium protective atmosphere, is warming up to 750 DEG C of calcining 5-15h After obtain Ce2Zr2O7The layered lithium manganate positive electrode of cladding.

0.1C multiplying power first discharge specific capacity is 178.95mAh/g in the present embodiment, 0.2,0.5,1C multiplying power discharges for the first time Specific capacity is respectively 171.02,158.42,150.48mAh/g, and the capacity retention ratio that 50 times are recycled under 1C multiplying power is 96.12%.

Embodiment 5

(1) preparation of layered lithium manganate presoma: being that 5:1 weighs lithium hydroxide, three oxidations two by element Li:Mn molar ratio Manganese is placed in autoclave, and deionized water is added by 50% solid content, after mixing evenly, the constant temperature 40h at 220 DEG C, from It is so cooling, after filtration washing 10 times, dried feed A is obtained after dry in 150 DEG C；

(2)Ce2Zr2O7The preparation of presoma: being that weigh cerous nitrate, zirconium nitrate completely molten by 1:1 by Elements C e:Zr molar ratio Solution is made into mixed solution in deionized water, and ammonium hydroxide is added dropwise, and control mixed solution pH value is stirred to react 3h 11, shifts supreme It presses in reaction kettle, the isothermal reaction 20h at 220 DEG C, natural cooling, after filtration washing 10 times, obtains drying after dry in 130 DEG C Expect B；

It (3) is that 1:0.1 weighs the dried feed A of step (1) and the dried feed B of step (2) by element Li:Ce molar ratio, with Dehydrated alcohol is that dispersing agent carries out ball milling mixing processing, in 130 DEG C of dry obtained dried feed C；

(4) the dried feed C that step (3) obtains is placed under high-purity helium protective atmosphere, after being warming up to 800 DEG C of calcining 15h Obtain Ce2Zr2O7The layered lithium manganate positive electrode of cladding.

0.1C multiplying power first discharge specific capacity is 178.21mAh/g in the present embodiment, 0.2,0.5,1C multiplying power discharges for the first time Specific capacity be respectively recycled under 169.89,161.92mAh/g, 150.46,1C multiplying power 50 times capacity retention ratio be 94.96%.

Above content is only to structure example of the invention and explanation, affiliated those skilled in the art It makes various modifications or additions to the described embodiments or is substituted in a similar manner, without departing from this hair Bright structure or beyond the scope defined by this claim, is within the scope of protection of the invention.

Claims (7)

1. a kind of method of modifying of layered lithium manganate material, including hydro-thermal method prepare manganate precursor for lithium, it is characterised in that including Following steps:
(1) burnt zirconic acid cerium Ce is prepared using hydro-thermal method2Zr2O7Presoma；
(2) it is 1:(0.01-0.1 by element Li:Ce molar ratio) manganate precursor for lithium and burnt zirconic acid cerium precursor are weighed, with anhydrous Ethyl alcohol is that dispersing agent carries out ball milling or ultrasonic mixing processing, in 100-130 DEG C of dry obtained dried feed；
(3) dried feed that step (2) obtains is placed under protective atmosphere, is obtained after being warming up to 600-800 DEG C of calcining 5-15h Ce2Zr2O7The layered lithium manganate positive electrode of cladding.
2. a kind of method of modifying of layered lithium manganate material according to claim 1, it is characterised in that hydro-thermal method prepares manganese The step of sour lithium presoma are as follows: by element Li:Mn molar ratio be (2.5-5): 1 weighs that lithium source, that manganese sesquioxide managnic oxide is placed in high pressure is anti- It answers in kettle, deionized water is added by the solid content of 20-50%, after mixing evenly, the constant temperature 10-40h at 140-220 DEG C is natural It is cooling, after filtration washing 3-10 times, manganate precursor for lithium is obtained after dry in 100-150 DEG C.
3. a kind of method of modifying of layered lithium manganate material according to claim 1, it is characterised in that step (1) hydro-thermal method The step of preparing burnt zirconic acid cerium precursor are as follows: by Elements C e:Zr molar ratio be 1:1 weigh cerium source, zirconium source be dissolved completely in from It is made into mixed solution in sub- water, ammonium hydroxide is added dropwise, controls mixed solution pH value in 8-11, is stirred to react 1-3h, it is anti-to be transferred to high pressure It answers in kettle, the isothermal reaction 10-20h at 180-220 DEG C, natural cooling, after filtration washing 3-10 times, in 100-130 DEG C of drying After obtain burnt zirconic acid cerium precursor.
4. a kind of method of modifying of layered lithium manganate material according to claim 2, it is characterised in that: described to prepare mangaic acid Lithium source in lithium presoma is or mixtures thereof lithium nitrate, one kind of lithium hydroxide.
5. a kind of method of modifying of layered lithium manganate material according to claim 3, it is characterised in that: the step (1) In cerium source be or mixtures thereof cerous nitrate, ammonium ceric nitrate, one kind of cerous sulfate.
6. a kind of method of modifying of layered lithium manganate material according to claim 3, it is characterised in that: the step (1) In zirconium source be or mixtures thereof zirconium chloride, one kind of zirconium nitrate.
7. a kind of method of modifying of layered lithium manganate material according to claim 1, it is characterised in that: the step (3) In protective atmosphere be high pure nitrogen or high-purity argon gas or high-purity helium.
CN201710298921.4A 2017-04-29 2017-04-29 A kind of method of modifying of layered lithium manganate material CN107093725B (en)

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KR20150003552A (en) * 2013-07-01 2015-01-09 한국과학기술연구원 Cathode active material coated with metallic mixed metal oxide, preparation method for the same and rechargeable lithium batteries including the same
CN106058241A (en) * 2016-07-21 2016-10-26 天津巴莫科技股份有限公司 Ce1-xZrxO2 nano solid solution homogenate modified lithium ion battery anode material and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20150003552A (en) * 2013-07-01 2015-01-09 한국과학기술연구원 Cathode active material coated with metallic mixed metal oxide, preparation method for the same and rechargeable lithium batteries including the same
CN106058241A (en) * 2016-07-21 2016-10-26 天津巴莫科技股份有限公司 Ce1-xZrxO2 nano solid solution homogenate modified lithium ion battery anode material and preparation method thereof

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