CN106025262B - A kind of preparation method of nanometer spinel type nickel ion doped - Google Patents
A kind of preparation method of nanometer spinel type nickel ion doped Download PDFInfo
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- CN106025262B CN106025262B CN201610573614.8A CN201610573614A CN106025262B CN 106025262 B CN106025262 B CN 106025262B CN 201610573614 A CN201610573614 A CN 201610573614A CN 106025262 B CN106025262 B CN 106025262B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention provides a kind of preparation method of nanometer spinel type nickel ion doped, include the following steps: uniformly to mix manganese salt, lithium salts, nickel salt, it is made into the mother liquor that total cation concentration is 0.1~1.0mol/L, a nanometer precursor is prepared by liquid-liquid coprecipitation reaction, and then sal volatile is added in 400~2200rpm in adults power reactor rotor speed；Under the action of super gravity field, mixed liquor is constantly recycled until the reaction is complete；By gained suspension by filtering, drying, precursor is obtained；Precursor is calcined in microwave Muffle furnace, obtains nanometer spinel type nickel ion doped.The present invention can prepare that crystallinity is high, crystal form is complete, particle is uniform, the spinel-type nickel ion doped of good dispersion, size tunable, and the average grain diameter of spinel-type nickel ion doped is up to 50~100nm；The preparation method simple process, low in cost, environmental-friendly, stability in batch production is good.
Description
Technical field
The present invention relates to lithium ion battery material preparation technical fields, and in particular to a kind of nanometer spinel type nickel ion doped
LiNi0.5Mn1.5O4Preparation method.
Background technique
In numerous anode material for lithium-ion batteries, the nickel ion doped material of spinel-type is because of its own height with 4.7V
The advantages that voltage, good cycle performance, can sufficiently meet the needs of green new kinetic energy, such as: the nickel ion doped of spinel-type
Material is compared to cobalt acid lithium material, and production cost is low, environmental pollution is small；The nickel ion doped material of spinel-type is compared to mangaic acid
Lithium material, the stability under high temperature circulation are preferable；The nickel ion doped material of spinel-type is closed compared to LiFePO 4 material
At simple process, stability in batch production is good, the single battery assembled when especially matching with lithium titanate anode, output voltage
Up to 3.2V, overall performance advantage is clearly.Nickel ion doped belongs to inorganic metal composite oxides, therefore, general inorganic
The synthetic method of material may be used to synthesize nickel ion doped.
Spinel-type nickel ion doped is as lithium ion anode material, and voltage platform is high, thermal cycling stability is good, charge and discharge
Speed is fast.During the charging process, the Ni in nickel ion doped material4+、Mn4+3d electron orbit and O2-In 2p electron orbit have
Effect ground hydridization, reaches mutual stable state, and then overcome the analysis oxygen problem of material.In addition, since nickel ion doped material is held back
The formation for making positive Manganic ion substantially eliminates capacity fade problem, therefore, fundamentally improves material in cycle charge-discharge
Stability.The method of prior art preparation spinel-type nickel ion doped has:
Patent of invention CN102569776A discloses a kind of using one solid phase two-step method of hydro-thermal preparation spherical high-voltage anode
The method of material spinelle type nickel ion doped, specifically: first by nickel source, manganese source and doping element compound solution and sodium/ammonium
Carbonate solution is uniformly mixed, then surfactant is added thereto, and spherical nickel manganese carbonic acid is prepared under hydrothermal conditions
Salt co-precipitation；Sintering obtains spherical nickel-manganese oxide after washing is dry；By oxide and lithium source through liquid phase ball milling mixing, dry,
Finally sintering obtains positive electrode active materials.The method complex process can only prepare spherical nickel ion doped.
Patent of invention CN103280570A discloses a kind of preparation method of micron-order single-crystal nickel lithium manganate anode material, tool
Body is: nickel-manganese composite hydroxide being made in solution, nickel manganese oxide complex hydroxide obtains complex chemical compound seed crystal；Yu Rong
It by nickel salt, manganese salt and alkali compounds hybrid reaction in liquid, and is aoxidized simultaneously, complex chemical compound seed crystal is made to grow up to partial size
It is 0.1~30 micron；Obtained crystal grain is directly mixed with lithiumation object in the solution, or will be after the processing of crystal grain acid
It is mixed with lithiumation object, oxidation reaction is then carried out in oxidative environment, it is dry after filtering, before roasting nickel ion doped compound
Drive body.The method preparation process is simple, available mono-crystalline structures, the nickel ion doped material of high-energy density, but its particle ruler
Very little is micron order, it is difficult to reach Nano grade.
Application for a patent for invention CN105047900A provides a kind of preparation method of nano-sheet nickel mangaic acid file material, specifically
Be: water-soluble salt of nickel and manganese is configured to solution, and precipitating reagent is added after reacting with complexing agent, and reaction obtains nickel manganese compound
Presoma roasts to obtain Ni, Mn oxide；Ni, Mn oxide and lithium compound mixing, high-temperature roasting prepare spinel-type nickel ion doped
Compound；By coating the metal oxide of one layer of uniform titanium and/or zirconium in particle surface, point prepared by surface modification is brilliant
Stone-type nickel ion doped compound.Though the spinel nickel mangaic acid file material prepared from method has nano-grade size, its microcosmic shape
Looks are sheet, and crystallinity is not high, it is difficult to be directly applied to the preparation of spinel-type nickel ion doped.
In conclusion urgent need, which develops one kind, can prepare nano-grade spinel type nickel ion doped to meet the needs of real.
Summary of the invention
It is an object of that present invention to provide a kind of preparation methods of nanometer spinel type nickel ion doped, comprising the following steps:
The first step prepares presoma, specifically:
The dissolution of lithium salts, nickel salt and manganese salt distilled water is configured to mixed solution；Mixed solution is passed through hypergravity reaction
In device；Precipitating reagent is added, the reaction was continued, and reaction is completed to obtain reaction solution；It is reacted with the pH value that ammonium hydroxide adjusts reaction solution
Slurry；Go water and drying to get presoma reaction slurry progress heating water bath；
Second step prepares nanometer spinel type LiNi0.5Mn1.5O4, specifically:
Presoma obtained by the first step is calcined under microwave heating to get nanometer spinel type
LiNi0.5Mn1.5O4Powder.
Preferred in above technical scheme, the supergravity reactor is rotating bed with helix channel or rotary packed bed,
The rotor speed of the supergravity reactor is 300-1500r/min, preferably 700-1200r/min.
Preferred in above technical scheme, the lithium salts, nickel salt, manganese salt press lithium ion: nickel ion: the molar ratio of manganese ion
Ingredient is carried out for the proportion of 1-1.1:0.5:1.5；The cationic total concentration of the mixed solution is 0.1-0.5mol/L.
Preferred in above technical scheme, the mixed solution is continuously passed through hypergravity with the rate of 200-500L/h and reacts
In device, 10-30min is recycled；Precipitating reagent is added dropwise with 100ml per minute, the reaction was continued after being added dropwise to complete, and 20-50min is reacted
Liquid；The pH value of the reaction slurry is 7.0-9.0.
Preferred in above technical scheme, the precipitating reagent is sal volatile, ammonium ion in the sal volatile
Concentration is the total cation concentration of mixed solution.
Preferred in above technical scheme, the heating water bath goes the water to be specifically: by being 60 DEG C -120 DEG C in temperature
Under the conditions of water-bath evaporation water, preferable temperature be 80 DEG C -120 DEG C；The drying is specifically: being 100 DEG C -180 DEG C in temperature
Under the conditions of dry 6-24h.
In above technical scheme preferably, calcining is specifically in the second step: with the rate of 5 DEG C/min-30 DEG C/min
780 DEG C -900 DEG C are warming up to, calcines 1.5-2.5h under the conditions of 780 DEG C -900 DEG C.
In above technical scheme preferably, calcining is specifically in the second step: being warming up to 850 with the rate of 10 DEG C/min
DEG C, 2h is calcined under the conditions of 850 DEG C.
Preferred in above technical scheme, the nickel salt is nickel nitrate, and the manganese salt is manganese nitrate, and the lithium salts is nitric acid
Lithium.
Using nanometer spinel type LiNi of the present invention0.5Mn1.5O4Preparation method, have the advantages that
(1) present invention provides a kind of method of novel preparation nano nickel lithium manganate, and can prepare average grain diameter is 50-
100nm, crystallinity are high, crystal form is complete, particle is uniform, the nanometer spinel type nickel ion doped of size tunable and good dispersion, gram
Taken prior art preparation nickel ion doped particle diameter distribution it is uneven, easy to reunite, crystal phase purity is low, crystallinity is not high the disadvantages of.
(2) presoma of the present invention is prepared under Elevated Gravity (preferably with gas-liquid reaction or liquid-liquid reactions), surpasses
Gravity reaction is microcosmic to be uniformly mixed, greatly strengthens mass transfer, it is ensured that the granularity of presoma is controllable and is evenly distributed.
(3) presoma is made in the present invention under Elevated Gravity, then is calcined by microwave heating to presoma,
Calcination process temperature uniform, controllable and without temperature gradient, it is ensured that product particle size is uniform, crystallinity is high.
(4) the process step of the invention is simplified, and equipment is easy to get, with short production cycle, is suitble to industrialized production.
Other than objects, features and advantages described above, there are also other objects, features and advantages by the present invention.
Below with reference to figure, the present invention is described in further detail.
Detailed description of the invention
The attached drawing constituted part of this application is used to provide further understanding of the present invention, schematic reality of the invention
It applies example and its explanation is used to explain the present invention, do not constitute improper limitations of the present invention.In the accompanying drawings:
Fig. 1 is nanometer spinel type LiNi prepared by the preferred embodiment of the present invention 10.5Mn1.5O4XRD spectra；
Fig. 2 is nanometer spinel type LiNi prepared by the preferred embodiment of the present invention 10.5Mn1.5O4SEM spectrogram；
Fig. 3 is nanometer spinel type LiNi prepared by the preferred embodiment of the present invention 10.5Mn1.5O4TEM spectrogram；
Fig. 4 is the XRD spectra of the sample of embodiment 1- embodiment 3 (under reaction mass different conditions of mixture ratios)；
Fig. 5 is the XRD spectra of the sample of embodiment 1, embodiment 4 and embodiment 5 (reaction solutions of different pH value)；
Fig. 6 is the XRD spectra of the sample of embodiment 1 (supergravity reactor) and comparative example 1 (conventional reactor)；
Fig. 7 is the XRD spectra of the sample of embodiment 1 (microwave calcination) and comparative example 2 (Conventional calcination).
Specific embodiment
The embodiment of the present invention is described in detail below in conjunction with attached drawing, but the present invention can be limited according to claim
Fixed and covering multitude of different ways is implemented.
Embodiment 1:
A kind of nanometer spinel type nickel ion doped (LiNi0.5Mn1.5O4) preparation method, comprising the following steps:
The first step prepares presoma, specifically:
The dissolution of lithium salts, nickel salt and manganese salt distilled water is configured to the mixed solution that total cation concentration is 0.24mol/L；
Mixed solution is passed through in supergravity reactor (specifically: it is high-gravity rotating bed anti-that mixed solution first being poured into helical duct type
It answers in the reservoir of device, runs supergravity reactor, adjusting revolving bed rotor speed by frequency conversion instrument is 1000r/min, simultaneously
Centrifugal pump is opened, recycles mixed solution in super-gravity device, and controlling flow by spinner flowmeter is 400L/h, circulation
10min)；Sal volatile is added as precipitating reagent, and (concentration of ammonium ion is the total cation of mixed solution in sal volatile
Concentration, drop rate are 100ml per minute), the reaction was continued 30min, reaction is completed to obtain reaction solution；It is adjusted and is reacted with ammonium hydroxide
The pH value of liquid is 8.0, obtains reaction slurry；Go water and drying to get presoma, the water reaction slurry progress heating water bath
Bath heating goes the water to be specifically: by water-bath evaporation water under the conditions of at a temperature of 90 °C；The drying is specifically: being in temperature
Dry 12h under conditions of 120 DEG C.
Second step prepares nanometer spinel type LiNi0.5Mn1.5O4, specifically:
Presoma obtained by the first step is calcined under microwave heating to get nanometer spinel type
LiNi0.5Mn1.5O4Powder, calcining are specifically: being warming up to 850 DEG C with the rate of 10 DEG C/min, calcine 2h under the conditions of 850 DEG C.
The lithium salts, nickel salt, manganese salt are respectively lithium nitrate, nickel nitrate and manganese nitrate, the lithium nitrate, nickel nitrate and nitric acid
Manganese presses lithium ion: nickel ion: the proportion that the molar ratio of manganese ion is 1:0.5:1.5 carries out ingredient.
By nanometer spinel type LiNi obtained by the present embodiment0.5Mn1.5O4XRD and SEM detection is carried out, Fig. 1, figure are as a result detailed in
2 and Fig. 3.From Fig. 1, Fig. 2 and Fig. 3: spinelle LiNi manufactured in the present embodiment0.5Mn1.5O4Sample, high with crystallinity,
The features such as crystal form is complete, particle is uniform, size tunable, good dispersion, average grain diameter is up to 50~100nm.
Embodiment 2- embodiment 3
3 difference from Example 1 of embodiment 2- embodiment is the proportion of the lithium nitrate, nickel nitrate and manganese nitrate not
Together, specifically: lithium nitrate described in embodiment 2, nickel nitrate and manganese nitrate are by lithium ion: nickel ion: the molar ratio of manganese ion is
1.05:0.5:1.5 proportion carry out ingredient；Lithium nitrate described in embodiment 3, nickel nitrate and manganese nitrate press lithium ion: nickel ion:
The proportion that the molar ratio of manganese ion is 1.1:0.5:1.5 carries out ingredient.
3 gained nanometer spinel type LiNi of embodiment 2 and embodiment0.5Mn1.5O4XRD testing result be detailed in Fig. 4, by scheming
4 as can be seen that the proportion of lithium nitrate, nickel nitrate and manganese nitrate is important, according to the preparation of the proportion of embodiment 2 and embodiment 3
Spinelle LiNi0.5Mn1.5O4In have the impurity of a small amount of Ni, Mn oxide, it is therefore preferable that lithium nitrate, nickel nitrate and manganese nitrate
By lithium ion: nickel ion: the proportion that the molar ratio of manganese ion is 1.0:0.5:1.5 carries out ingredient.
Embodiment 4- embodiment 5
5 difference from Example 1 of embodiment 4- embodiment is that the pH value of the system is different, concrete example 4 be using
Ammonium hydroxide (NH3H2O the pH value for) adjusting reaction system is 7.5.In embodiment 5, ammonium hydroxide (NH is used3H2O the pH of reaction system) is adjusted
Value is 8.5.Other operating conditions are all the same.
5 gained nanometer spinel type LiNi of embodiment 4 and embodiment0.5Mn1.5O4XRD testing result be detailed in Fig. 5, from figure
5 it can be seen that the sample crystallinity prepared is high, and free from admixture generates when adjusting pH value to 8.
Comparative example 1
1 difference from Example 1 of comparative example is:
Mixed solution is placed in the three-necked flask with agitating paddle, stirring rate 1000r/min；
Sal volatile is added and is used as precipitating reagent, the reaction was continued 30min, reaction is completed to be to obtain reaction solution；
It is 8.0 with the pH value that ammonium hydroxide adjusts reaction solution, obtains reaction slurry；
Go water and drying to get presoma reaction slurry progress heating water bath.
1 gained nanometer spinel type LiNi of comparative example0.5Mn1.5O4XRD testing result be detailed in Fig. 6.
As shown in Figure 6: being prepared relative to conventional reactor (three-necked flask), supergravity reactor (RBHC)
LiNi0.5Mn1.5O4The crystallinity of powder is higher, and crystal form is complete.
Comparative example 2
Comparative example 2 difference from example 1 is that: presoma is calcined in conventional Muffle furnace, i.e.,
Obtain nanometer spinel type LiNi0.5Mn1.5O4Powder, calcining are specifically: warming naturally to 850 DEG C, calcine under the conditions of 850 DEG C
10h。
2 gained nanometer spinel type LiNi of comparative example0.5Mn1.5O4XRD testing result be detailed in Fig. 7, can from Fig. 7
Know: microwave calcination compares Conventional calcination, and microwave calcination can not only effectively promote the formation of crystal phase, and can greatly improve reaction
Effect, microwave calcination is more advantageous to obtain that crystallinity is high, the complete spinel powder material of crystal form.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of nanometer spinel type nickel ion doped LiNi0.5Mn1.5O4Preparation method, which comprises the following steps:
The first step prepares presoma, specifically:
The dissolution of lithium salts, nickel salt and manganese salt distilled water is configured to mixed solution；Mixed solution is passed through in supergravity reactor；
Precipitating reagent is added, the reaction was continued, and reaction is completed to obtain reaction solution；Reaction slurry is obtained with the pH value that ammonium hydroxide adjusts reaction solution；
Go water and drying to get presoma reaction slurry progress heating water bath；The lithium salts, nickel salt, manganese salt press lithium ion: nickel from
Son: the proportion that the molar ratio of manganese ion is 1-1.1:0.5:1.5 carries out ingredient；The cationic total concentration of the mixed solution is
0.1-0.5mol/L；The mixed solution is continuously passed through in supergravity reactor with the rate of 200-500L/h, recycles 10-
30min；Precipitating reagent is added dropwise with 10-120ml per minute, the reaction was continued after being added dropwise to complete, and 20-50min obtains reaction solution；
Second step prepares nanometer spinel type LiNi0.5Mn1.5O4, specifically:
Presoma obtained by the first step is calcined under microwave heating to get nanometer spinel type LiNi0.5Mn1.5O4Powder
End.
2. nanometer spinel type nickel ion doped LiNi according to claim 10.5Mn1.5O4Preparation method, feature exists
In the supergravity reactor is rotating bed with helix channel or rotary packed bed, the rotor speed of the supergravity reactor
For 300-1500r/min.
3. nanometer spinel type nickel ion doped LiNi according to claim 20.5Mn1.5O4Preparation method, feature exists
In the rotor speed of the supergravity reactor is 700-1200r/min.
4. nanometer spinel type nickel ion doped LiNi according to claim 10.5Mn1.5O4Preparation method, feature exists
In the pH value of the reaction slurry is 7.0-9.0.
5. nanometer spinel type nickel ion doped LiNi according to claim 40.5Mn1.5O4Preparation method, feature exists
In the precipitating reagent is sal volatile, and the concentration of ammonium ion is that the total cation of mixed solution is dense in the sal volatile
Degree.
6. nanometer spinel type nickel ion doped LiNi according to claim 10.5Mn1.5O4Preparation method, feature exists
The water is gone to be specifically in, the heating water bath: by water-bath evaporation water under conditions of temperature is 60 DEG C -120 DEG C；The drying
Specifically: dry 6-24h under conditions of temperature is 100 DEG C -180 DEG C.
7. nanometer spinel type nickel ion doped LiNi according to claim 60.5Mn1.5O4Preparation method, feature exists
In, pass through temperature be 80 DEG C -120 DEG C under conditions of water-bath evaporation water.
8. nanometer spinel type nickel ion doped LiNi according to claim 10.5Mn1.5O4Preparation method, feature exists
In, in the second step calcining be specifically: be warming up to 780 DEG C -900 DEG C with the rate of 5 DEG C/min-30 DEG C/min, 780 DEG C -
1.5-2.5 h is calcined under the conditions of 900 DEG C.
9. nanometer spinel type nickel ion doped LiNi according to claim 80.5Mn1.5O4Preparation method, feature exists
In, in the second step calcining be specifically: be warming up to 850 DEG C with the rate of 10 DEG C/min, calcine 2h under the conditions of 850 DEG C.
10. nanometer spinel type nickel ion doped LiNi according to claim 10.5Mn1.5O4Preparation method, feature exists
In the nickel salt is nickel nitrate, and the manganese salt is manganese nitrate, and the lithium salts is lithium nitrate.
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| CN106564967B (en) * | 2016-10-31 | 2018-06-05 | 安泰科技股份有限公司 | Lithium-rich manganese-based anode material presoma, positive electrode and preparation method thereof |
| CN107739057B (en) * | 2017-11-03 | 2019-10-29 | 云南民族大学 | A kind of preparation method of lithium manganate having spinel structure |
| CN109935798A (en) * | 2017-12-19 | 2019-06-25 | 宁波高新区锦众信息科技有限公司 | A kind of preparation method of lithium ion battery nickel manganese lithium composite material |
| CN109292826B (en) * | 2018-07-26 | 2020-12-22 | 华南理工大学 | Porous lithium manganate material with high charge-discharge capacity, and preparation method and application thereof |
| CN109678219B (en) * | 2018-12-28 | 2022-05-13 | 湘潭大学 | Preparation method of nano layered lithium nickel cobalt manganese oxide |
| CN110282665B (en) * | 2019-07-04 | 2022-01-25 | 成都尤尼瑞克科技有限公司 | Lithium battery positive electrode material precursor with mesoscopic structure and preparation method thereof |
| CN113120963A (en) * | 2021-03-20 | 2021-07-16 | 安徽博石高科新材料股份有限公司 | Preparation of lithium manganate by microwave heating and sintering |
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| CN103066270A (en) * | 2012-12-28 | 2013-04-24 | 湘潭大学 | Preparation method of nano-spinel type LiMn2O4 |
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