CN105932327A - Preparation method for cubic-phase lithium lanthanum zirconium oxide solid-state electrolyte nano material - Google Patents
Preparation method for cubic-phase lithium lanthanum zirconium oxide solid-state electrolyte nano material Download PDFInfo
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- CN105932327A CN105932327A CN201610323476.8A CN201610323476A CN105932327A CN 105932327 A CN105932327 A CN 105932327A CN 201610323476 A CN201610323476 A CN 201610323476A CN 105932327 A CN105932327 A CN 105932327A
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- lithium lanthanum
- lanthanum zirconium
- zirconium oxygen
- solid electrolyte
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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
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid materials
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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
- H01M2300/00—Electrolytes
- H01M2300/0085—Immobilising or gelification of electrolyte
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention provides a preparation method for a cubic-phase lithium lanthanum zirconium oxide solid-state electrolyte nano material. A simple solution combustion synthesis technology is adopted, and a solid-state electrolyte material is obtained after heat treatment, and the solid-state electrolyte material has relatively high room temperature ionic conductivity and can be used as a solid-state electrolyte of a full solid-state battery. The preparation method of solution combustion synthesis is simple, and a prepared precursor is synthesized by one step, and element distribution is uniform. The layer thickness of a precursor particle is 100- 200 nano-meters, and the particle has a big specific surface area, so that element diffusion is facilitated at a high temperature, and a reaction is complete. Compared with other methods such as a sol-gel method and a solid phase method, the method has great technical advantages: low costs, high yield, simple operation and feasible industrial production.
Description
Technical field
The invention belongs to novel energy resource material technology field, be specifically related to lithium lanthanum zirconium oxygen solid electrolyte
The preparation method of nano material.
Background technology
The energy and environmental protection are two big key factors of current sustainable economic development.The most substantial amounts of
Combustion of fossil fuel, the most day by day consumes the non-renewable energy, and has had resulted in quite
Serious air pollution.The clean energy resourcies such as lithium ion battery are used to replace the fossil having pollution to fire
Expect extremely the most urgent, therefore on market, occur in that substantial amounts of lithium electricity equipment.Organic containing liquid
The conventional lithium ion battery of electrolyte, it may occur however that the danger that electrolyte leakage, burning are even exploded
Danger.The all-solid-state battery of conventional liquid organic electrolyte is replaced with safer solid electrolyte
Just attracting more and more to pay close attention to.Electric motor car (EV) and the large-sized battery of Locating Type electric power storage purposes
Application demand increase sharply, can expect safe becoming a candidate with long-life solid state battery
Product.In terms of pursuing the battery of new generation of high capacity, the weight of solid electrolyte figure
The property wanted also is improving day by day.
Traditional commercial Li-ion batteries, uses flammable organic electrolyte, there is electrolyte
Reveal, burn, the hidden danger such as blast.Lithium sulfur, lithium sky battery, and in order to improve energy density
Novel battery negative pole often use lithium metal, and the generation of Li dendrite can cause battery short circuit,
Impact safe handling.Use the all-solid-state battery of solid electrolyte, by its solid electrolyte not
Flammable, corrosion-free, do not reveal, and the growth of Li dendrite can be stoped, fundamentally solve
The short circuit problem of battery, improves safety, is also beneficial to the invention application of high energy density cells.
In the solid lithium ion electrolyte reported, there is the oxide lithium lanthanum of garnet structure
Zirconium oxygen (LLZO) has a comprehensive excellent properties: high lithium ion conductivity；Lithium ion mobility
Number is about 1；Electrochemical window width (> 7V vs.Li+/Li)；Stable to lithium metal；Right
Air stability is high；Easily operated, it is very good solid electrolyte material.
But the most at present, the production technology of lithium lanthanum zirconium oxygen solid electrolyte is the most always
Do not obtain important breakthrough, seriously constrain the application of all-solid-state battery.System in worldwide
The method making lithium lanthanum zirconium oxygen solid electrolyte mainly has two kinds: solid phase method and sol-gal process.Gu
Phase method complicated process of preparation, it is generally required to repeatedly ball milling and Technology for Heating Processing, relatively costly, property
Can be preferably；Sol-gal process preparation technology is relatively easy, but obtained electrolyte
Can be not enough, relative solid phase method, low 1-3 the order of magnitude of its conductivity at room temperature.Other are prepared
Technique many employings advanced instrument equipment, is unfavorable for reducing cost and scale application.The present invention adopts
By the simplest lithium lanthanum zirconium oxygen preparation technology of one, low cost, energy consumption
Few, yield is big, and prepared electrolyte superior performance solves large-scale industry metaplasia
Produce the technical barrier of solid electrolyte, and gained electrolyte granule is at nanosized, can
To prepare thin electrolyte films to reduce battery volume, the marketization application to all-solid-state battery has
High meaning, promotes the arrival in all-solid-state battery epoch.
Summary of the invention
The present invention mainly uses nitrate to be raw material, adds adulterant, solution combustion synthesis lithium
The presoma of lanthanum zirconium oxygen, through tabletting, calcining, it is provided that simply and on a large scale prepare lithium lanthanum zirconium oxygen
The method of solid electrolyte, the lithium lanthanum zirconium oxygen solid electrolyte prepared has excellent electrification
Learn performance, can be as the electrolyte of all-solid-state battery.And the method has low cost,
Yield is big, simple to operate, and purity is high, is suitable for the advantages such as production in enormous quantities, solves current lithium
The problem of lanthanum zirconium oxygen industrialized production difficulty.
For achieving the above object, technical scheme is as follows:
The preparation method of a kind of Emission in Cubic lithium lanthanum zirconium oxygen solid electrolyte nano material, including following
Step:
Comprise the following steps:
A) solution combustion synthetic method is used to prepare precursor powder；
B) presoma obtains lithium lanthanum zirconium oxygen solid electrolyte through pyroreaction；
C) solid electrolyte that pyroreaction obtains obtains lithium lanthanum zirconium oxygen nano material after ball milling.
Described step A) raw material includes: commercial lithium nitrate, Lanthanum (III) nitrate, zirconium nitrate, glycine
Deng, it is not necessary to any pretreatment, lithium nitrate, Lanthanum (III) nitrate, zirconium nitrate, glycine and adulterant are pressed
Mol ratio is dissolved in deionized water, is placed in heating by electric cooker, and solution occurs combustion reaction after being evaporated,
White precursor powder is obtained after several seconds.
Described precursor powder bulk multi-hole, it is internal is two-dimensional slice structure, lamellar spacing
100-300 nanometer, also has the hole of 30-200nm in lamella, composition mostly is zirconic acid lanthanum.
Wherein said step B) including: first precursor powder is ground in mortar, then will
Precursor powder depresses to diameter 10-15mm at 100-300MPa, the disk of thickness 1-3mm,
Then 700-1000 DEG C of roasting 2-8h under air atmosphere, finally gives lithium lanthanum zirconium oxygen solid state electrolysis
Matter；
The lithium lanthanum zirconium oxygen solid electrolyte potsherd obtained is white disk, and consistency is low, frangible,
Internal particle size 1-3um.
Wherein said step C) including: the Emission in Cubic lithium lanthanum zirconium oxygen solid-state electricity that will obtain after roasting
Solve matter potsherd to grind in mortar, then at planetary ball mill ball milling 6-10h, rotational speed of ball-mill
300-400r/min, the powder body obtained after ball milling i.e. Emission in Cubic lithium lanthanum zirconium oxygen nano material.
Lithium lanthanum zirconium oxygen nano-grain size 50-600nm obtained.
The most described adulterant includes aluminum source, tantalum source, niobium source, the one in tungsten source or many
Kind, wherein aluminum source includes that aluminum nitrate etc., tungsten source include ammonium metatungstate etc..
The invention have the benefit that
1, the abundant raw material source employed in the present invention, cheap, and whole technique is very
Simply, can produce by large-scale pipeline.A series of process for allied substances provide complete ginseng
Examine.
2, prepared lithium lanthanum zirconium oxygen solid electrolyte has high ionic conductivity, Ke Yizuo
For the electrolyte of all-solid-state battery, greatly improve safety and the capacity of battery.
3, the lithium lanthanum zirconium oxygen of Emission in Cubic is than high 2 orders of magnitude of electrical conductivity of Tetragonal lithium lanthanum zirconium oxygen,
And granule is owing to having higher specific surface area, it is possible to reduce element segregation and raising agglutinating property,
Improve border electrical conductivity, thus improve the electrical conductivity of LLZO pottery.
4, gained electrolyte is at nanosized, can prepare thin electrolyte films to reduce electricity
Pond volume and weight.
5, the LLZO of nano-particle can also be combined with the polymer such as PEO, prepares thickness ten
Flexible solid electrolyte within several microns, it is simple to market is applied.
Accompanying drawing explanation
Fig. 1 present invention prepares the stereoscan photograph of lithium lanthanum zirconium oxygen nano-powder；
The room temperature ac impedance spectroscopy of lithium lanthanum zirconium oxygen potsherd prepared by Fig. 2 present invention；
The Arrhenius curve of lithium lanthanum zirconium oxygen potsherd prepared by Fig. 3 present invention.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with
Drawings and Examples, are explained in further detail the present invention.Should be appreciated that this place is retouched
The specific embodiment stated is only used for explaining the present invention, is not intended to limit the present invention.
On the contrary, the present invention contains any spirit and scope in the present invention being defined by the claims
On replacement, amendment, equivalent method and the scheme made.Further, in order to make the public to this
Bright having a better understanding, during the details to the present invention describes below, detailed to describe some special
Fixed detail section.
The invention provides the preparation method of a kind of lithium lanthanum zirconium oxygen solid electrolyte material, by molten
Liquid conbustion synthesis prepares presoma, and doping element obtains Emission in Cubic lithium lanthanum zirconium through high-temperature heat treatment
Oxygen；Described lithium lanthanum zirconium oxygen electrolyte granular is tens to hundreds of nanometer, and granule profile is not advised
Then, the mol ratio containing element Li, Al, La, Zr, O is (5.5-7.7): (0.1-0.5):
3:2:(10-12).
The commercial nitrate of example 1 and glycine are raw material, it is not necessary to any pretreatment.First weigh
15.4mmol lithium nitrate, 6mmol Lanthanum (III) nitrate, 4mmol zirconium nitrate, 0.48mmol aluminum nitrate and
12.94mmol glycine dissolves in deionized water, is placed on electric furnace, heating, until being evaporated
There is combustion synthesis reaction later, obtain the powder body material of white puff.Powder body material is existed
Being cold-pressed into the disk of diameter 15mm under 300MPa, in Muffle furnace, 900 DEG C of 4h heat subsequently
To Emission in Cubic lithium lanthanum zirconium oxygen.By the Emission in Cubic lithium lanthanum zirconium oxygen that obtains through ball milling 10h, rotational speed of ball-mill
300r/min, the powder body after ball milling is cold-pressed into the disk of diameter 15mm, warp again at 300MPa
1200 DEG C of 5h heat treatments are fired into potsherd, 1 DEG C/min of heating rate.
Lithium lanthanum zirconium oxygen potsherd upper and lower surface metal spraying, test cabinet on electrochemical workstation will be obtained
Temperature AC impedance, arranging parameter is 0.1-1MHz, and calculating its electrical conductivity is 3.54 × 10-4S/cm,
At a temperature of 25-80 DEG C, test its electrical conductivity obtain Arrhenius curve and calculate its activation energy
For 0.34eV.
The commercial nitrate of example 2 and carbamide are raw material, it is not necessary to any pretreatment.First weigh
15.4mmol lithium nitrate, 6mmol Lanthanum (III) nitrate, 4mmol zirconium nitrate, 0.48mmol aluminum nitrate and
15mmol carbamide dissolves in deionized water, is placed on electric furnace, heating, until after being evaporated
There is combustion synthesis reaction, obtain the powder body material of white puff.By powder body material at 200MPa
Under be cold-pressed into the disk of diameter 15mm, in Muffle furnace, 700 DEG C of 4h heating obtain cube subsequently
Phase lithium lanthanum zirconium oxygen.By the Emission in Cubic lithium lanthanum zirconium oxygen that obtains through ball milling 15h, rotational speed of ball-mill
300r/min, the powder body after ball milling is cold-pressed into the disk of diameter 15mm, warp again at 200MPa
1200 DEG C of 4h heat treatments are fired into potsherd, 1 DEG C/min of heating rate.
Lithium lanthanum zirconium oxygen potsherd upper and lower surface metal spraying, test cabinet on electrochemical workstation will be obtained
Temperature AC impedance, arranging parameter is 0.1-1MHz, and calculating its electrical conductivity is 2.9 × 10-4S/cm,
At a temperature of 25-80 DEG C, test its electrical conductivity obtain Arrhenius curve and calculate its activation energy
For 0.38eV.
The commercial nitrate of example 3 and glycine are raw material, it is not necessary to any pretreatment.First weigh
15.4mmol lithium nitrate, 6mmol Lanthanum (III) nitrate, 4mmol zirconyl nitrate, 0.48mmol aluminum nitrate
Dissolving in deionized water with 10mmol glycine, be placed on electric furnace, heating, until being evaporated
There is combustion synthesis reaction later, obtain the powder body material of white puff.Powder body material is existed
Being cold-pressed into the disk of diameter 10mm under 200MPa, in Muffle furnace, 800 DEG C of 4h heat subsequently
To Emission in Cubic lithium lanthanum zirconium oxygen.By the Emission in Cubic lithium lanthanum zirconium oxygen that obtains through ball milling 10h, rotational speed of ball-mill
300r/min, the powder body after ball milling is cold-pressed into the disk of diameter 15mm, warp again at 200MPa
1200 DEG C of 5h heat treatments are fired into potsherd, 1 DEG C/min of heating rate.
Lithium lanthanum zirconium oxygen potsherd upper and lower surface metal spraying, test cabinet on electrochemical workstation will be obtained
Temperature AC impedance, arranging parameter is 0.1-1MHz, and calculating its electrical conductivity is 3.4 × 10-4S/cm,
At a temperature of 25-80 DEG C, test its electrical conductivity obtain Arrhenius curve and calculate its activation energy
For 0.37eV.
The commercial nitrate of example 4 and carbamide are raw material, it is not necessary to any pretreatment.First weigh
15.4mmol lithium nitrate, 6mmol Lanthanum (III) nitrate, 4mmol zirconyl nitrate, 0.48mmol aluminum nitrate
Dissolve in deionized water with 15mmol carbamide, be placed on electric furnace, stir and heat,
Until there is combustion synthesis reaction after being evaporated, obtain the powder body material of white puff.By powder body
Material is cold-pressed into the disk of diameter 10mm, subsequently 700 DEG C of 4h in Muffle furnace under 200MPa
Heating obtains Emission in Cubic lithium lanthanum zirconium oxygen.By the Emission in Cubic lithium lanthanum zirconium oxygen that obtains through ball milling 15h, ball
Mill rotating speed 300r/min, the powder body after ball milling is cold-pressed into diameter 15mm's at 200MPa again
Disk, is fired into potsherd, 1 DEG C/min of heating rate through 1200 DEG C of 5h heat treatments.
Lithium lanthanum zirconium oxygen potsherd upper and lower surface metal spraying, test cabinet on electrochemical workstation will be obtained
Temperature AC impedance, arranging parameter is 0.1-1MHz, and calculating its electrical conductivity is 2.9 × 10-4S/cm,
At a temperature of 25-80 DEG C, test its electrical conductivity obtain Arrhenius curve and calculate its activation energy
For 0.41eV.
Claims (4)
1. a preparation method for Emission in Cubic lithium lanthanum zirconium oxygen solid electrolyte nano material, it is special
Levy and be, comprise the following steps:
A) solution combustion synthetic method is used to prepare precursor powder；
B) presoma obtains lithium lanthanum zirconium oxygen solid electrolyte through pyroreaction；
C) solid electrolyte that pyroreaction obtains obtains lithium lanthanum zirconium oxygen nano material after ball milling.
Described step A) raw material includes: commercial lithium nitrate, Lanthanum (III) nitrate, zirconium nitrate, glycine,
Without any pretreatment, lithium nitrate, Lanthanum (III) nitrate, zirconium nitrate, glycine and adulterant by mole
Ratio is dissolved in deionized water, is placed in heating by electric cooker, and solution occurs combustion reaction after being evaporated, several
White precursor powder is obtained after second；
Described precursor powder bulk multi-hole, it is internal is two-dimensional slice structure, lamellar spacing
100-300 nanometer, also has the hole of 30-200nm in lamella, composition mostly is zirconic acid lanthanum.
A kind of Emission in Cubic lithium lanthanum zirconium oxygen solid electrolyte nanometer the most according to claim 1
The preparation method of material, it is characterised in that described step B) including: first by precursor
End is ground in mortar, then at 100-300MPa, precursor powder is depressed to diameter 10-15mm,
The disk of thickness 1-3mm, then 700-1000 DEG C of roasting 2-8h under air atmosphere, final
To lithium lanthanum zirconium oxygen solid electrolyte；
The lithium lanthanum zirconium oxygen solid electrolyte potsherd obtained is white disk, and consistency is low, frangible,
Internal particle size 1-3um.
A kind of Emission in Cubic lithium lanthanum zirconium oxygen solid electrolyte nanometer the most according to claim 1
The preparation method of material, it is characterised in that described step C) including: by obtain after roasting
Emission in Cubic lithium lanthanum zirconium oxygen solid electrolyte potsherd grinds, then at planetary ball mill in mortar
Ball milling 6-10h, rotational speed of ball-mill 300-400r/min, the powder body obtained after ball milling i.e. Emission in Cubic lithium
Lanthanum zirconium oxygen nano material；The lithium lanthanum zirconium oxygen nano-grain size obtained is at 50-600nm.
A kind of Emission in Cubic lithium lanthanum zirconium oxygen solid electrolyte nanometer the most according to claim 1
The preparation method of material, it is characterised in that described adulterant include aluminum source, tantalum source, niobium source,
One or more of tungsten source, wherein aluminum source is aluminum nitrate, and tungsten source is ammonium metatungstate.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107162049A (en) * | 2017-06-05 | 2017-09-15 | 清华大学 | Lithium lanthanum zirconium epoxide oxide-based nanomaterial and preparation method thereof |
| CN109052473A (en) * | 2018-08-10 | 2018-12-21 | 淮安新能源材料技术研究院 | A kind of industrialized process for preparing of the zirconic acid lanthanum lithium solid electrolyte of tantalum aluminium codope |
| CN109319837A (en) * | 2018-11-29 | 2019-02-12 | 江苏海基新能源股份有限公司 | A kind of garnet of cubic phase containing aluminium Li7La3Zr2O12Preparation method |
| CN109378522A (en) * | 2018-10-22 | 2019-02-22 | 北京科技大学 | A kind of sodium zirconium silicon phosphorus method for preparing composite solid electrolyte |
| CN111732433A (en) * | 2020-07-02 | 2020-10-02 | 西安瑞智材料科技有限公司 | Preparation method of garnet type solid electrolyte with controllable particle size |
| CN112429770A (en) * | 2020-12-01 | 2021-03-02 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of lithium lanthanum zirconium oxide particles, product and application thereof |
| CN113912120A (en) * | 2021-10-11 | 2022-01-11 | 福州大学 | Method for improving lithium lanthanum zirconium oxygen cubic phase stability |
| CN114349045A (en) * | 2021-12-28 | 2022-04-15 | 广东马车动力科技有限公司 | Preparation method of high-yield pure-phase lithium lanthanum zirconium oxide solid electrolyte material |
| CN114605152A (en) * | 2022-04-27 | 2022-06-10 | 佛山(华南)新材料研究院 | Cubic-phase lithium lanthanum zirconium oxide and preparation method thereof |
| CN115340378A (en) * | 2022-10-20 | 2022-11-15 | 江苏蓝固新能源科技有限公司 | Oxide solid electrolyte, preparation method thereof and lithium ion battery |
| CN115724463A (en) * | 2021-12-13 | 2023-03-03 | 湖州南木纳米科技有限公司 | Precursor material for preparing lithium lanthanum zirconium oxide |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102367383A (en) * | 2011-10-29 | 2012-03-07 | 南昌大学 | Preparation method of yttrium aluminum garnet yellow fluorescent powder for white light LED |
| CN103524128A (en) * | 2013-10-12 | 2014-01-22 | 南昌大学 | Preparation method of yttria-stabilized zirconia tetragonal nano powder with high specific surface area |
| CN104124467A (en) * | 2014-07-22 | 2014-10-29 | 武汉理工大学 | Method for preparing solid electrolyte by using lithium lanthanum zirconium oxide precursor coated powder |
| WO2015002410A1 (en) * | 2013-07-04 | 2015-01-08 | 한국생산기술연구원 | Solid electrolyte for all solid-state lithium-ion battery and manufacturing method therefor |
| CN105406118A (en) * | 2015-12-30 | 2016-03-16 | 哈尔滨工业大学 | Ceramic solid electrolyte and preparation method thereof |
-
2016
- 2016-05-16 CN CN201610323476.8A patent/CN105932327B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102367383A (en) * | 2011-10-29 | 2012-03-07 | 南昌大学 | Preparation method of yttrium aluminum garnet yellow fluorescent powder for white light LED |
| WO2015002410A1 (en) * | 2013-07-04 | 2015-01-08 | 한국생산기술연구원 | Solid electrolyte for all solid-state lithium-ion battery and manufacturing method therefor |
| CN103524128A (en) * | 2013-10-12 | 2014-01-22 | 南昌大学 | Preparation method of yttria-stabilized zirconia tetragonal nano powder with high specific surface area |
| CN104124467A (en) * | 2014-07-22 | 2014-10-29 | 武汉理工大学 | Method for preparing solid electrolyte by using lithium lanthanum zirconium oxide precursor coated powder |
| CN105406118A (en) * | 2015-12-30 | 2016-03-16 | 哈尔滨工业大学 | Ceramic solid electrolyte and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| N.JANANI ETAL.: ""Synthesis of cubic Li7La3Zr2O12 by modified sol-gel process"", 《IONICS》 * |
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| CN112429770A (en) * | 2020-12-01 | 2021-03-02 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of lithium lanthanum zirconium oxide particles, product and application thereof |
| CN113912120A (en) * | 2021-10-11 | 2022-01-11 | 福州大学 | Method for improving lithium lanthanum zirconium oxygen cubic phase stability |
| CN113912120B (en) * | 2021-10-11 | 2023-05-12 | 福州大学 | Method for improving stability of lithium lanthanum zirconium oxygen cubic phase |
| CN115724463A (en) * | 2021-12-13 | 2023-03-03 | 湖州南木纳米科技有限公司 | Precursor material for preparing lithium lanthanum zirconium oxide |
| CN114349045A (en) * | 2021-12-28 | 2022-04-15 | 广东马车动力科技有限公司 | Preparation method of high-yield pure-phase lithium lanthanum zirconium oxide solid electrolyte material |
| CN114349045B (en) * | 2021-12-28 | 2022-09-27 | 广东马车动力科技有限公司 | Preparation method of high-yield pure-phase lithium lanthanum zirconium oxide solid electrolyte material |
| CN114605152B (en) * | 2022-04-27 | 2022-11-29 | 佛山(华南)新材料研究院 | Cubic-phase lithium lanthanum zirconium oxide and preparation method thereof |
| CN114605152A (en) * | 2022-04-27 | 2022-06-10 | 佛山(华南)新材料研究院 | Cubic-phase lithium lanthanum zirconium oxide and preparation method thereof |
| CN115340378A (en) * | 2022-10-20 | 2022-11-15 | 江苏蓝固新能源科技有限公司 | Oxide solid electrolyte, preparation method thereof and lithium ion battery |
| CN115340378B (en) * | 2022-10-20 | 2023-02-03 | 江苏蓝固新能源科技有限公司 | Oxide solid electrolyte, preparation method thereof and lithium ion battery |
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