CN104409717A - Nano rod-shaped nickel-lithium manganate cathode material and preparation method thereof - Google Patents
Nano rod-shaped nickel-lithium manganate cathode material and preparation method thereof Download PDFInfo
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- CN104409717A CN104409717A CN201410625032.0A CN201410625032A CN104409717A CN 104409717 A CN104409717 A CN 104409717A CN 201410625032 A CN201410625032 A CN 201410625032A CN 104409717 A CN104409717 A CN 104409717A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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 invention discloses a nano rod-shaped nickel-lithium manganate cathode material and a preparation method thereof, and belongs to the field of lithium battery cathode materials. The preparation method comprises the following steps: according to the ratio of amount of substance of the chemical formula (LiNi<0.5>Mn<1.5>O4), dissolving manganese salts and persulfide into distilled water, evenly stirring to obtain a mixed solution; sealing and heating the mixed solution to obtain MnO2 precipitate, washing and drying the MnO2 precipitate to obtain MnO2 nano rods; mixing the MnO2 nano rods and nickel salts in a polar solvent, carrying out supersonic dispersing, then dropwise adding an alkaline solution into the polar solvent to obtain nickel hydroxide and manganese hydroxide precipitate; washing and drying the precipitate, wherein during the dropwise addition process, the reaction system is sealed and heated; mixing the dried hydroxide precipitate with lithium salts, grinding the mixture, and then calcining the mixture so as to obtain the nano rod-shaped nickel-lithium manganate cathode material. The nickel-lithium manganate prepared by the provided method has a nano rod shape and has the advantages of stable structure and high cycle stability.
Description
Technical field
The present invention relates to field of lithium ion battery anode, particularly a kind of anode material for lithium-ion batteries and preparation method thereof.
Background technology
Nickel ion doped (LiNi
0.5mn
1.5o
4) be a kind of anode material for lithium-ion batteries of excellent electrochemical performance, the advantages such as reversible capacity is large, good cycle, operating voltage high (5V) that it has, are often used to the lithium ion battery preparing height ratio capacity and high-energy-density.So provide a kind of method preparing nickel lithium manganate cathode material very necessary.
For example, CN103579607A provides a kind of preparation method of spherical nickel-lithium manganate anode material, comprise the following steps: take Li source compound according to the ratio of mol ratio 2: 1: 1, nickel source compound and spherical mangano-manganic oxide, Li source compound and nickel source compound are dissolved in ethanol and are configured to the solution that metal cation total concentration is 0.1-0.3mol/L, spherical mangano-manganic oxide is added in above-mentioned solution, heating water bath is to forming paste mixture while stirring, grey black powder is obtained after 90-110 DEG C of oven dry, gained powder is at 750-950 DEG C of roasting 6-36h, 615-675 DEG C of annealing 2-6h, directly sieve after cooling and obtain nickel lithium manganate cathode material.
Inventor finds that prior art at least exists following problem:
In the charge and discharge process of the lithium ion battery prepared by nickel ion doped sphere material utilizing prior art to provide, improve cut-ff voltage, easily make the structure of nickel ion doped material change, cause the cyclical stability of lithium ion battery poor.
Summary of the invention
Embodiment of the present invention technical problem to be solved is, provides a kind of structural stability good, is beneficial to nano bar-shape nickel lithium manganate cathode material improving lithium ion battery cyclical stability and preparation method thereof.Described technical scheme is as follows:
On the one hand, provide a kind of nano bar-shape nickel lithium manganate cathode material preparation method, comprising:
Step a, according to chemical formula LiNi
0.5mn
1.5o
4in the amount of substance ratio of each element, the manganese salt of scheduled volume and persulfide are dissolved in distilled water, after stirring, obtain mixed solution;
Step b, airtight heat treated is carried out to described mixed solution, obtain MnO
2precipitation, and to described MnO
2precipitation carries out washing, drying and processing, obtains MnO
2nanometer rods;
Step c, by described MnO
2nanometer rods and nickel salt are blended in polar solvent, and carry out ultrasonic disperse, then in described polar solvent, alkaline solution is being dripped, obtain the precipitation of hydroxide of nickel manganese, and the precipitation of hydroxide of described nickel manganese is washed, drying and processing, wherein, described alkaline solution is being added drop-wise in the process of described polar solvent, is keeping reaction system to be in airtight heated condition;
Steps d, the precipitation of hydroxide of nickel manganese after drying to be mixed with lithium salts, after milled processed, carry out calcination processing, obtain nano bar-shape nickel lithium manganate cathode material.
Particularly, as preferably, in described step a, the concentration of described mixed solution is 0.01-0.35mol/L.
Particularly, as preferably, in described step a, described persulfide is selected from least one in over cure ammonium, over cure potassium and sodium persulfide.
Particularly, as preferably, in described step b, the temperature of described airtight heat treated is 80-200 DEG C, and the time is 3-24 hour.
Particularly, as preferably, in described step c, described polar solvent is selected from water, methyl alcohol or ethanol.
Particularly, as preferably, in described step c, described alkaline solution is at least one in NaOH, potassium hydroxide, ammoniacal liquor, Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, triethylamine, diethylamide.
Particularly, as preferably, in described step c, described maintenance reaction system is in the process of airtight heated condition, and the temperature of described airtight heating is 100-200 DEG C, and the time is 1-4 hour.
Particularly, as preferably, in described steps d, described calcination processing comprises the first calcination processing and the second calcination processing;
The temperature of described first calcination processing is 400-600 DEG C, and the time is 2-12 hour;
The temperature of described second calcination processing is 800-950 DEG C, and the time is 10-24 hour.
On the other hand, provide a kind of nano bar-shape nickel lithium manganate cathode material utilizing above-mentioned method to prepare, the diameter of described nano bar-shape nickel lithium manganate cathode material is 70-100nm, and length is 5-12 μm.
As preferably, the diameter of described nano bar-shape nickel lithium manganate cathode material is 90nm, and length is 10 μm.
The beneficial effect that the technical scheme that the embodiment of the present invention provides is brought is:
The preparation method of the nano bar-shape nickel lithium manganate cathode material that the embodiment of the present invention provides, by obtaining MnO
2nanometer rods, and at MnO
2this architecture basics on further controllably form the precipitation of hydroxide of nickel manganese, then compound lithium salts, forms nano bar-shape nickel lithium manganate cathode material.Because prepared nickel ion doped is nano bar-shape structure, its structure is not only more stable, and there is relatively little specific area, reactivity point on it is relatively less, reduce the transmission of lithium ion active interface in this positive electrode, reduce the side reaction produced in charge and discharge process, improve the cyclical stability of prepared lithium ion battery.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme in the embodiment of the present invention, below the accompanying drawing used required in describing embodiment is briefly described, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the SEM Electronic Speculum figure of the nano bar-shape nickel lithium manganate cathode material that the embodiment of the present invention 1 provides.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly, below in conjunction with accompanying drawing, embodiment of the present invention is described further in detail.
On the one hand, embodiments provide a kind of nano bar-shape nickel lithium manganate cathode material preparation method, the method comprises:
Step 101, according to chemical formula LiNi
0.5mn
1.5o
4in the amount of substance ratio of each element, the manganese salt of scheduled volume and persulfide are dissolved in distilled water, after stirring, obtain mixed solution.
Step 102, airtight heat treated is carried out to the mixed solution obtained in step 101, obtain MnO
2precipitation, and to described MnO
2precipitation carries out washing, drying and processing, obtains MnO
2nanometer rods.
Step 103, the MnO will obtained in step 102
2nanometer rods and nickel salt are blended in polar solvent, and carry out ultrasonic disperse, then in this polar solvent, alkaline solution is being dripped, obtain the precipitation of hydroxide of nickel manganese, and the precipitation of hydroxide of this nickel manganese is washed, drying and processing, wherein, alkaline solution is being added drop-wise in the process of polar solvent, is keeping reaction system to be in airtight heated condition.
Step 104, the precipitation of hydroxide of nickel manganese after drying to be mixed with lithium salts, after milled processed, carry out calcination processing, obtain nano bar-shape nickel lithium manganate cathode material.
The preparation method of the nano bar-shape nickel lithium manganate cathode material that the embodiment of the present invention provides, by obtaining MnO
2nanometer rods, and at MnO
2this architecture basics on further controllably form the precipitation of hydroxide of nickel manganese, then compound lithium salts, forms nano bar-shape nickel lithium manganate cathode material.Because prepared nickel ion doped is nano bar-shape structure, its structure is not only more stable, and there is relatively little specific area, reactivity point on it is relatively less, reduce the transmission of lithium ion active interface in this positive electrode, reduce the side reaction produced in charge and discharge process, improve the cyclical stability of prepared lithium ion battery.
Further, in order to improve reaction rate, in step 101, the concentration of above-mentioned mixed solution is 0.01-0.35mol/L.
Particularly, in step 101, persulfide is selected from least one in over cure ammonium, over cure potassium and sodium persulfide.
As preferably, in step 102, generate MnO to improve
2the speed precipitated also makes to react completely, and the temperature of above-mentioned airtight heat treated is 80-200 DEG C, and the time is 3-24 hour.
Particularly, in step 103, polar solvent is selected from water, methyl alcohol or ethanol.Alkaline solution is at least one in NaOH, potassium hydroxide, ammoniacal liquor, Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, triethylamine, diethylamide.
Further, in step 103, be in the process of airtight heated condition in maintenance reaction system, in order to improve reaction rate and make to react completely thoroughly, the temperature controlling this airtight heating is 100-200 DEG C, and the time is 1-4 hour.
Particularly, in step 104, this calcination processing comprises the first calcination processing and the second calcination processing;
Wherein, the temperature of the first calcination processing is 400-600 DEG C, and the time is 2-12 hour;
The temperature of the second calcination processing is 800-950 DEG C, and the time is 10-24 hour.
The hydroxide in reactant and lithium salts can be made to decompose by above-mentioned first calcination processing, the precipitation of hydroxide and the lithium salts that are beneficial to nickel manganese react, generating nickel LiMn2O4.By carrying out the second calcination processing after the first calcination processing, being beneficial to generated nickel ion doped and better carrying out crystallization process, forming stable crystal orientation, thus the structural stability of nickel ion doped prepared by improving.
Be understandable that, manganese salt, nickel salt and lithium salts used in said method are the conventional material in this area, and such as they can be the chloride salt of corresponding metallic element, sulfate, nitrate or acetate.
On the other hand, provide a kind of nano bar-shape nickel lithium manganate cathode material utilizing above-mentioned method to prepare, the diameter of this nano bar-shape nickel lithium manganate cathode material is 70-100nm, and length is 5-12 μm.
The diameter of the nano bar-shape nickel lithium manganate cathode material that the embodiment of the present invention is prepared by said method is 70-100nm, length is 5-12 μm, there is structural stability good, good cycling stability, reversible capacity advantages of higher, its specific discharge capacity between 3.5-4.8V is greater than 130mAh/g, has excellent chemical property.
Further, become lithium ion battery for the ease of following process, the diameter of this nano bar-shape nickel lithium manganate cathode material is preferably 90nm, and length is preferably 10 μm.
Below further the present invention will be described by specific embodiment.
Embodiment 1
Present embodiments provide a kind of nano bar-shape nickel lithium manganate cathode material, its preparation method comprises the following steps:
According to chemical formula LiNi
0.5mn
1.5o
4in the amount of substance ratio of each element, 3.38g Manganous sulfate monohydrate and 4.76g sodium peroxydisulfate are dissolved in 100ml distilled water, magnetic agitation mixes, and obtaining concentration is 0.02mol/L mixed solution.
Carry out airtight heat treated to mixed solution obtained above, heating time is 15h, and heating-up temperature is 180 DEG C, after question response is complete, obtains MnO
2precipitation, after this precipitation of filtration washing, in atmosphere at 100 DEG C to its heat drying 6h, obtain MnO
2nanometer rods.
By 0.87g MnO
2nanometer rods and 7.89g six hydration nickel sulfate ultrasonic disperse are in 200ml ethanolic solution, then in this ethanolic solution, the sodium hydroxide solution that 100ml concentration is 0.3mol/L is being dripped, obtain the precipitation of hydroxide of nickel manganese, and the precipitation of hydroxide of this nickel manganese is washed, drying and processing, wherein, NaOH is being added drop-wise in the process of ethanolic solution, is keeping reaction system to be in airtight heated condition, heating time is 1 hour, and heating-up temperature is 120 DEG C.
Step 104, the precipitation of hydroxide of nickel manganese after drying is mixed (wherein by amount of substance ratio with lithium salts, lithium salts excessive 5%), after grinding distribution is even, obtain powder, 500 DEG C are heated to the programming rate of 5 DEG C/min after this powder is carried out drying, and calcine 12h, carry out the first calcination processing; And then rise to 950 DEG C with the programming rate of 10 DEG C/min, and calcine 12h, carry out the second calcination processing.Naturally cool to room temperature, namely obtain nano bar-shape nickel lithium manganate cathode material.
The structure of ESEM to prepared nano bar-shape nickel lithium manganate cathode material is utilized to observe, the SEM structure chart of the nano bar-shape nickel lithium manganate cathode material that accompanying drawing 1 provides for the present embodiment.As shown in Figure 1, the nano bar-shape nickel lithium manganate cathode material that the present embodiment provides presents uniform nano bar-shape structure.Record this nano bar-shape nickel lithium manganate cathode material diameter be 75nm, length is 8 μm.
Embodiment 2
Present embodiments provide a kind of nano bar-shape nickel lithium manganate cathode material, its preparation method comprises the following steps:
According to chemical formula LiNi
0.5mn
1.5o
4in the amount of substance ratio of each element, 3.78g manganese chloride and 8.11g potassium peroxydisulfate are dissolved in 300ml distilled water, magnetic agitation mixes, and obtaining concentration is 0.01mol/L mixed solution.
Carry out airtight heat treated to mixed solution obtained above, heating time is 8h, and heating-up temperature is 130 DEG C, after question response is complete, obtains MnO
2precipitation, after this precipitation of filtration washing, in atmosphere at 80 DEG C to its heat drying 12h, obtain MnO
2nanometer rods.
By 0.87g MnO
2nanometer rods and 3.91g nickel chloride ultrasonic disperse are in the 200ml aqueous solution, then in this aqueous solution, the potassium hydroxide solution that 120ml concentration is 0.25mol/L is being dripped, obtain the precipitation of hydroxide of nickel manganese, and the precipitation of hydroxide of this nickel manganese is washed, drying and processing, wherein, potassium hydroxide is being added drop-wise in the process of the aqueous solution, is keeping reaction system to be in airtight heated condition, heating time is 4 hours, and heating-up temperature is 200 DEG C.
Step 104, the precipitation of hydroxide of nickel manganese after drying is mixed (wherein by amount of substance ratio with lithium salts, lithium salts excessive 3%), after grinding distribution is even, obtain powder, 480 DEG C are heated to the programming rate of 10 DEG C/min after this powder is carried out drying, and calcine 8h, carry out the first calcination processing; And then rise to 900 DEG C with the programming rate of 8 DEG C/min, and calcine 12h, carry out the second calcination processing.Naturally cool to room temperature, namely obtain nano bar-shape nickel lithium manganate cathode material.Record this nano bar-shape nickel lithium manganate cathode material diameter be 90nm, length is 10 μm.
Embodiment 3
Present embodiments provide a kind of nano bar-shape nickel lithium manganate cathode material, its preparation method comprises the following steps:
According to chemical formula LiNi
0.5mn
1.5o
4in the amount of substance ratio of each element, 49.1g manganese acetate and 45.6g ammonium persulfate are dissolved in 200ml distilled water, magnetic agitation mixes, and obtaining concentration is 0.35mol/L mixed solution.
Carry out airtight heat treated to mixed solution obtained above, heating time is 24h, and heating-up temperature is 165 DEG C, after question response is complete, obtains MnO
2precipitation, after this precipitation of filtration washing, in atmosphere at 180 DEG C to its heat drying 12h, obtain MnO
2nanometer rods.
By 0.87g MnO
2nanometer rods and 24.9g nickel acetate ultrasonic disperse are in 1000ml methanol solution, then in this methanol solution, the ammoniacal liquor that 500ml concentration is 0.7mol/L is being dripped, obtain the precipitation of hydroxide of nickel manganese, and the precipitation of hydroxide of this nickel manganese is washed, drying and processing, wherein, ammoniacal liquor is being added drop-wise in the process of methanol solution, is keeping reaction system to be in airtight heated condition, heating time is 3 hours, and heating-up temperature is 100 DEG C.
Step 104, the precipitation of hydroxide of nickel manganese after drying is mixed (wherein by amount of substance ratio with lithium salts, lithium salts excessive 3%), after grinding distribution is even, obtain powder, 600 DEG C are heated to the programming rate of 4 DEG C/min after this powder is carried out drying, and calcine 2h, carry out the first calcination processing; And then rise to 800 DEG C with the programming rate of 6 DEG C/min, and calcine 10h, carry out the second calcination processing.Naturally cool to room temperature, namely obtain nano bar-shape nickel lithium manganate cathode material.Record this nano bar-shape nickel lithium manganate cathode material diameter be 90nm, length is 9 μm.
Embodiment 4
The nano bar-shape nickel lithium manganate cathode material that the present embodiment utilizes embodiment 1-3 to provide prepares lithium ion battery, and tests the cyclical stability of this lithium ion battery.Wherein, the preparation process of this lithium ion battery is as follows:
Nickel lithium manganate cathode material is mixed according to mass ratio 8:1:1 with conductive agent acetylene black, binding agent PVDF (Kynoar), with NMP (1-Methyl-2-Pyrrolidone), this mixture is modulated into slurry, evenly be coated on aluminium foil, put into baking oven, dry 3h for 110 DEG C, take out and be washed into pole piece, 85 DEG C of vacuumize 12 hours, carry out compressing tablet, 85 DEG C of vacuumize 12 hours, obtained experimental cell pole piece.Be to electrode with lithium sheet, electrolyte is 1.0mol/L LiPF
6eC (ethyl carbonate ester)+DMC (dimethyl carbonate) (volume ratio 3:7) solution, barrier film is celgard2325 film, is assembled into CR2025 type button cell in the glove box being full of argon gas atmosphere.
Carry out charge and discharge cycles test to above-mentioned button cell: wherein, charging/discharging voltage scope is 3.5 ~ 4.9V, be the condition of 0.5C at charging and discharging currents under (1C=130mA/g).Test result shows, the voltage platform of the positive electrode that embodiment 1-3 provides all has stable 5V platform.Concrete test data is as shown in table 1:
The stable circulation performance data test table of table 1 lithium ion battery
As shown in Table 1, the first discharge specific capacity of the lithium ion battery prepared by the method utilizing the embodiment of the present invention to provide is high, good cycling stability, has excellent cyclical stability.Visible, the nickel lithium manganate cathode material that the embodiment of the present invention provides, based on its stable club shaped structure, has good structural stability, and its voltage platform high (5V), the cyclical stability improving lithium ion battery is had great importance.
The foregoing is only preferred embodiment of the present invention, not in order to limit the scope of the invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a nano bar-shape nickel lithium manganate cathode material preparation method, comprising:
Step a, according to chemical formula LiNi
0.5mn
1.5o
4in the amount of substance ratio of each element, the manganese salt of scheduled volume and persulfide are dissolved in distilled water, after stirring, obtain mixed solution;
Step b, airtight heat treated is carried out to described mixed solution, obtain MnO
2precipitation, and to described MnO
2precipitation carries out washing, drying and processing, obtains MnO
2nanometer rods;
Step c, by described MnO
2nanometer rods and nickel salt are blended in polar solvent, and carry out ultrasonic disperse, then in described polar solvent, alkaline solution is being dripped, obtain the precipitation of hydroxide of nickel manganese, and the precipitation of hydroxide of described nickel manganese is washed, drying and processing, wherein, described alkaline solution is being added drop-wise in the process of described polar solvent, is keeping reaction system to be in airtight heated condition;
Steps d, the precipitation of hydroxide of nickel manganese after drying to be mixed with lithium salts, after milled processed, carry out calcination processing, obtain nano bar-shape nickel lithium manganate cathode material.
2. method according to claim 1, is characterized in that, in described step a, the concentration of described mixed solution is 0.01-0.35mol/L.
3. method according to claim 2, is characterized in that, in described step a, described persulfide is selected from least one in over cure ammonium, over cure potassium and sodium persulfide.
4. method according to claim 1, is characterized in that, in described step b, the temperature of described airtight heat treated is 80-200 DEG C, and the time is 3-24 hour.
5. method according to claim 1, is characterized in that, in described step c, described polar solvent is selected from water, methyl alcohol or ethanol.
6. method according to claim 5, is characterized in that, in described step c, described alkaline solution is at least one in NaOH, potassium hydroxide, ammoniacal liquor, Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, triethylamine, diethylamide.
7. method according to claim 6, is characterized in that, in described step c, described maintenance reaction system is in the process of airtight heated condition, and the temperature of described airtight heating is 100-200 DEG C, and the time is 1-4 hour.
8. method according to claim 1, is characterized in that, in described steps d, described calcination processing comprises the first calcination processing and the second calcination processing;
The temperature of described first calcination processing is 400-600 DEG C, and the time is 2-12 hour;
The temperature of described second calcination processing is 800-950 DEG C, and the time is 10-24 hour.
9. utilize nano bar-shape nickel lithium manganate cathode material prepared by the method described in any one of claim 1-8, the diameter of described nano bar-shape nickel lithium manganate cathode material is 70-100nm, and length is 5-12 μm.
10. positive electrode according to claim 9, is characterized in that, the diameter of described nano bar-shape nickel lithium manganate cathode material is 90nm, and length is 10 μm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108417830A (en) * | 2018-03-21 | 2018-08-17 | 湖北大学 | A kind of nickel lithium manganate cathode material and preparation method thereof |
| CN111354942A (en) * | 2019-11-26 | 2020-06-30 | 焦作伴侣纳米材料工程有限公司 | Micron-sized rod-shaped lithium manganate and preparation method and application thereof |
| CN117543008A (en) * | 2024-01-10 | 2024-02-09 | 南开大学 | Nano rod-shaped lithium nickel manganese oxide positive electrode material, preparation method and battery |
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| CN108417830A (en) * | 2018-03-21 | 2018-08-17 | 湖北大学 | A kind of nickel lithium manganate cathode material and preparation method thereof |
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| CN117543008A (en) * | 2024-01-10 | 2024-02-09 | 南开大学 | Nano rod-shaped lithium nickel manganese oxide positive electrode material, preparation method and battery |
| CN117543008B (en) * | 2024-01-10 | 2024-03-26 | 南开大学 | Nano rod-shaped lithium nickel manganese oxide positive electrode material, preparation method and battery |
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