CN108649208A - The low-temperature burning preparation method and positive electrode of spinel nickel LiMn2O4 - Google Patents
The low-temperature burning preparation method and positive electrode of spinel nickel LiMn2O4 Download PDFInfo
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- CN108649208A CN108649208A CN201810497096.5A CN201810497096A CN108649208A CN 108649208 A CN108649208 A CN 108649208A CN 201810497096 A CN201810497096 A CN 201810497096A CN 108649208 A CN108649208 A CN 108649208A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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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
- H01M4/50—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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- 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 low-temperature burning preparation method of spinel nickel LiMn2O4, and step includes:Lithium nitrate, nickel nitrate, manganese nitrate, organic-fuel and ammonium nitrate are made into uniform mixed liquor with deionized water, ammonium hydroxide is added, is adjusted to neutrality;The above-mentioned mixed liquor of heating evaporation, obtains sepia resinoid;Heating temperature is improved, makes above-mentioned resinoid that combustion reaction occur, the fluffy presoma of dark brown is obtained after completely burned;It is calcined in air atmosphere after above-mentioned presoma is crushed, cooling obtains spinel nickel manganate cathode material for lithium.The present invention also provides a kind of spinel nickel manganate cathode material for lithium prepared using the above method.
Description
Technical field
The invention belongs to electrochemical power source technical field of material more particularly to a kind of points of lithium rechargeable battery
The low-temperature burning preparation method of spar nickel lithium manganate cathode material and the positive electrode prepared using this method.
Background technology
Lithium rechargeable battery has been widely used for various portable battery products, in recent years electric vehicle and hybrid power
The demand of the energy storage device of vehicle puts forward higher requirements lithium rechargeable battery and its electrode material, and positive electrode is its key
Property component part, seek it is cheap, safe, environmental-friendly and with high potential, high-energy-density lithium ion secondary battery positive electrode material
Material becomes the research hotspot of field of lithium ion secondary.
Spinel nickel manganate cathode material for lithium has 4.7V discharge platforms and relatively high discharge capacity, charge and discharge process
Middle invertibity has good stability, and is the 5V positive electrodes with industrial development potentiality being expected.Currently, preparing spinel nickel
The method of LiMn2O4 mainly has solid-phase synthesis and coprecipitation method.Solid-phase synthesis is unable to reach molecule due to raw material mixing
Horizontal uniformity, and long-time calcining at constant temperature at relatively high temperatures is needed, generated time is long, and calcination temperature is high, production
Energy consumption is larger.In addition, being susceptible to the impurity such as NiO using the material that solid-phase synthesis is synthesized, exist in discharge process compared with
Big 4V discharge platforms.Although coprecipitation can realize the uniform mixing of raw material on a molecular scale, synthesis temperature is relatively low, product
Purity is higher, but complex process, cumbersome, and variable is difficult to control in the process, low output, it is difficult to mass produce.
For the deficiency of the above high temperature solid-state method and coprecipitation, low temperature combustion synthesis method is easy to operate, reaction temperature
Low, crystal growth is abundant, and product is mutually pure, is easy obtained nanometer grade powder, the existing application in other ceramic powder materials, but close
At the also rare report of spinel nickel LiMn2O4.
In the existing technology for preparing spinel nickel LiMn2O4, such as application No. is 200910166745.4 Chinese invention is special
The preparation method that profit is announced, deficiency are to use methanol, ethyl alcohol as dispersant, chelating certainly between carboxylate radical and metal ion
It acts on and insufficient, hardly results in gel state;And ethylene glycol improves system viscosity as dispersant, it is difficult to volatilize, need to overflow
Long heating process can just obtain gel state.
For another example application No. is the preparation sides that 201611042691.7,201710330440.7 Chinese invention patent is announced
Method, deficiency is that combustion reaction needs to cause (400 DEG C) at a higher temperature, in addition, the preparation method is just with raw material
Middle metal nitrate is in the very exothermic of flash-point, but shortage of heat causes combustion product yield so that gel rubber system fully burns
It is relatively low.
Invention content
The object of the present invention is to provide a kind of low-temperature burning preparation method of spinel nickel LiMn2O4 and utilize party's legal system
Standby positive electrode, this method are the compounding substances by lithium nitrate, nickel nitrate, manganese nitrate, organic-fuel and ammonium nitrate through too low
Temperature burning, spinel nickel manganate cathode material for lithium is obtained using calcining.
In order to achieve the above objectives, the present invention adopts the following technical scheme that:
A kind of low-temperature burning preparation method of spinel nickel LiMn2O4, as shown in Figure 1, step includes:
Lithium nitrate, nickel nitrate, manganese nitrate, organic-fuel and ammonium nitrate are made into uniform mixed liquor with deionized water, added
Enter ammonium hydroxide, is adjusted to neutrality;
The above-mentioned mixed liquor of heating evaporation, obtains sepia resinoid;
Heating temperature is improved, makes above-mentioned resinoid that combustion reaction occur, it is fluffy that dark brown is obtained after completely burned
Presoma;
It is calcined in air atmosphere after above-mentioned presoma is crushed, cooling obtains spinel nickel lithium manganate cathode material
Material.
Further, the lithium nitrate, nickel nitrate, manganese nitrate, organic-fuel and ammonium nitrate press 1:0.5:1.5:(3~6):
The molecule molar ratio of (7~42) mixes.
Further, the organic-fuel includes citric acid, acrylic acid, glycine, sucrose etc..
Further, evaporating temperature is 90~100 DEG C.
Further, heating temperature is improved to about 200 DEG C.
Further, calcining device includes Muffle furnace, crucible.
Further, calcination temperature is 700~900 DEG C, and calcination time is 4~12h.
A kind of spinel nickel manganate cathode material for lithium prepared using the above method.
Compared with the existing method for preparing spinel nickel LiMn2O4, the method for the present invention is easy to operate, and ignition temperature is low, forges
The burning time is short, and yield is high, and crystal growth is abundant, and product is mutually pure, is easy obtained nanometer grade powder, can prepare high-performance point crystalline substance
Stone nickel lithium manganate cathode material.
Description of the drawings
Fig. 1 is a kind of low-temperature burning preparation method flow chart of spinel nickel LiMn2O4.
Fig. 2 is the X-ray diffraction analysis spectrogram of product.
Fig. 3 is battery performance comparison diagram.
Specific implementation mode
Features described above and advantage to enable the present invention are clearer and more comprehensible, special embodiment below, and institute's attached drawing is coordinated to make
Detailed description are as follows.
Embodiment 1
The present embodiment provides a kind of low-temperature burning preparation method of spinel nickel LiMn2O4, step includes:
(1) lithium nitrate, nickel nitrate, manganese nitrate, citric acid and ammonium nitrate are pressed 1:0.5:1.5:3:7 molecule molar ratio is molten
It is uniformly mixed in 100ml deionized waters, it is 7 that ammonium hydroxide, which adjusts solution ph,;
(2) 90 DEG C of heating evaporation dehydrations are warming up to, it is gradually sticky, obtain resinoid;
(3) 200 DEG C or so are warming up to, ignition obtains fluffy frangible presoma;
(4) be fitted into Muffle furnace after grinding product, air atmosphere it is lower 800 DEG C calcining 6h after furnace cooling obtain spinelle
Nickel lithium manganate cathode material.
As Fig. 2 X-ray diffractogram in shown in S1, analysis result shows that powder is spinel-type nickel ion doped, is free of
NiO and LixNi1-xThe diffraction maximum of O.
Embodiment 2
The present embodiment provides a kind of low-temperature burning preparation method of spinel nickel LiMn2O4, step includes:
(1) lithium nitrate, nickel nitrate, manganese nitrate, acrylic acid and ammonium nitrate are pressed 1:0.5:1.5:4.5:28 molecule mole
It is uniformly mixed than being dissolved in 100ml deionized waters, it is 7 that ammonium hydroxide, which adjusts solution ph,;
(2) 95 DEG C of heating evaporation dehydrations are warming up to, it is gradually sticky, obtain resinoid;
(3) 200 DEG C or so are warming up to, ignition obtains fluffy frangible presoma;
(4) be fitted into crucible after grinding product, air atmosphere it is lower 700 DEG C calcining 12h after furnace cooling obtain spinelle
Nickel lithium manganate cathode material.
As Fig. 2 X-ray diffractogram in shown in S2, analysis result shows that powder is spinel-type nickel ion doped, is free of
NiO and LixNi1-xThe diffraction maximum of O.
Embodiment 3
The present embodiment provides a kind of low-temperature burning preparation method of spinel nickel LiMn2O4, step includes:
(1) lithium nitrate, nickel nitrate, manganese nitrate, glycine and ammonium nitrate are pressed 1:0.5:1.5:6:42 molecule molar ratio
It is dissolved in 100ml deionized waters and being uniformly mixed, it is 7 that ammonium hydroxide, which adjusts solution ph,;
(2) 100 DEG C of heating evaporation dehydrations are warming up to, it is gradually sticky, obtain resinoid;
(3) 200 DEG C or so are warming up to, ignition obtains fluffy frangible presoma;
(4) be fitted into crucible after grinding product, air atmosphere it is lower 900 DEG C calcining 4h after furnace cooling obtain spinel nickel
Manganate cathode material for lithium.
As Fig. 2 X-ray diffractogram in shown in S3, analysis result shows that powder is spinel-type nickel ion doped, is free of
NiO and LixNi1-xThe diffraction maximum of O.
To absolutely prove the superiority of the method for the present invention, following three comparative examples are enumerated for embodiment 1:
Comparative example 1
This comparative example is used application No. is the preparation method of 200910166745.4 publication, specific as follows:
Using lithium nitrate, nickel nitrate, manganese acetate as raw material, using ethyl alcohol as dispersant, three kinds of raw materials are first pressed into Li:Ni:Mn's
Molar ratio 1:0.5:1.5 mixing, and ethyl alcohol mixed grinding is added, heating evaporation is until form gel;Then improve heating temperature
It is allowed to that self-propagating combustion occurs, obtains primary stage solids powder;This primary stage solids powder is burnt in air atmosphere at a temperature of 700 DEG C
Knot 12h obtains the positive electrode LiNi of final product spinel structure0.5Mn1.5O4。
Comparative example 2
This comparative example is used application No. is the preparation method of 201611042691.7 publication, specific as follows:
Acetic acid reason 1.6909g, nickel acetate 0.2062g and manganese acetate 7.9212g are weighed, is respectively placed in 300mL in order
In crucible;Then crucible is put into heat in preheating 400 DEG C of Muffle furnaces of constant temperature and combustion reaction occurs, after combustion reaction 1h, taken out
It is cooled to room temperature to obtain combustion product;It after grinding, is put into the earthenware misfortune of 300mL, then is carried out in the Muffle furnace of 600 DEG C of constant temperature of preheating
Roasting heat preservation 3h, takes out cooling, obtains final products.
Comparative example 3
This comparative example is used application No. is the preparation method of 201710330440.7 publication, specific as follows:
Lithium nitrate 1.1427g, manganese acetate 7.9215g and nickel acetate 0.2062g are weighed, l0mL distilled water is added, at 50 DEG C
Under the conditions of heated at constant temperature stir to form uniform mixed solution, the salpeter solution of 6mol/L is added dropwise under the stirring of this constant temperature
5mL forms the mixed solution of light red, keeps the temperature 10min;Solution is set to evaporate overall solution volume in 100 DEG C of heated at constant temperature stirrings
Then mixed solution is transferred in porcelain mandarin orange whirlpool by the moisture of 1/5th volumes;Porcelain crucible is moved to 150 DEG C of temperature programming case
In formula resistance furnace, Heat preservation 5min in air atmosphere;Again 400 DEG C are warming up to the rate of 20 DEG C/min in air atmosphere
Heat combustion reaction 30min;500 DEG C of heat preservation 1h are finally warming up to the rate of 20 DEG C/min, takes out and is cooled to room temperature after heat preservation,
And product grind into powder;Powder after grinding is roasted under 700 DEG C of air atmospheres and kept the temperature 6h, regrinds to obtain nanoscale
Final product.
Interpretation of result:
Positive electrode LiNi is prepared using comparative example 10.5Mn1.5O4When, make since organic matter not being added in reaction system
For complexing agent, heating is evaporated rear system and does not form gel completely, hence it is evident that there is the metal salt particle for having neither part nor lot in complexing, to lead
Cause complexing of metal ion uneven, combustion reaction also fails to fully carry out.
Positive electrode LiNi is prepared using comparative example 2,30.5Mn1.5O4When, the two is required to heating evaporation after being complexed and obtains
To gel be placed in 400 DEG C of resistance furnace, combustion reaction could occur.In addition, combustion reaction and being not thorough, only occur zero
Spark star, burn incompletely generate volume of smoke, cause products collection efficiency very low.
Wherein, the final product yield obtained using comparative example 2 is about 42%, the final product obtained using comparative example 3
Yield is about 50%, and the two is far below the yield 85% of embodiment 1.
The positive electrode LiNi that embodiment 1 is prepared with comparative example 1-30.5Mn1.5O4It is assembled at battery testing, 3.5V~
It is tested under the conditions of 0.5C (75mA/g) between 4.9V, specific capacity comparison is as shown in Figure 3.As seen from the figure, the anode that prepared by embodiment 1
The battery testing of material learns that first discharge specific capacity 132mAh/g, the capacity after recycling 50 times is 129mAh/g, conservation rate
It is 97.7%, significantly larger than comparative example 1-3, it is seen that the method for the present invention can prepare more high performance spinel nickel LiMn2O4
Positive electrode.
The above embodiments are merely illustrative of the technical solutions of the present invention rather than is limited, the ordinary skill of this field
Personnel can be modified or replaced equivalently technical scheme of the present invention, without departing from the spirit and scope of the present invention, this
The protection domain of invention should be subject to described in claims.
Claims (8)
1. a kind of low-temperature burning preparation method of spinel nickel LiMn2O4, step include:
Lithium nitrate, nickel nitrate, manganese nitrate, organic-fuel and ammonium nitrate are made into uniform mixed liquor with deionized water, ammonia is added
Water is adjusted to neutrality;
The above-mentioned mixed liquor of heating evaporation, obtains sepia resinoid;
Heating temperature is improved, makes above-mentioned resinoid that combustion reaction occur, the fluffy forerunner of dark brown is obtained after completely burned
Body;
It is calcined in air atmosphere after above-mentioned presoma is crushed, cooling obtains spinel nickel manganate cathode material for lithium.
2. according to the method described in claim 1, it is characterized in that, the lithium nitrate, nickel nitrate, manganese nitrate, organic-fuel and
Ammonium nitrate presses 1:0.5:1.5:(3~6):The molecule molar ratio of (7~42) mixes.
3. according to the method described in claim 1, it is characterized in that, the organic-fuel includes citric acid, acrylic acid, sweet ammonia
Acid, sucrose.
4. according to the method described in claim 1, it is characterized in that, evaporating temperature is 90~100 DEG C.
5. according to the method described in claim 1, it is characterized in that, improving heating temperature to 200 DEG C.
6. according to the method described in claim 1, it is characterized in that, calcining device includes Muffle furnace, crucible.
7. according to the method described in claim 1, it is characterized in that, calcination temperature be 700~900 DEG C, calcination time be 4~
12h。
8. a kind of spinel nickel manganate cathode material for lithium prepared using any the methods of the claims 1-7.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109437334A (en) * | 2018-10-31 | 2019-03-08 | 云南民族大学 | A kind of preparation method of high magnification nickel cobalt codope lithium manganate having spinel structure material |
CN109686974A (en) * | 2018-12-25 | 2019-04-26 | 安徽理工大学 | A method of burning or even detonation synthesize NCA battery material |
CN114014380A (en) * | 2021-10-28 | 2022-02-08 | 蜂巢能源科技有限公司 | Lithium nickel manganese oxide, preparation method and application thereof |
WO2023184995A1 (en) * | 2022-03-29 | 2023-10-05 | 广东邦普循环科技有限公司 | Ternary positive electrode material having core-shell structure and preparation method therefor and use thereof |
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2018
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Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN104787805A (en) * | 2015-04-20 | 2015-07-22 | 齐鲁工业大学 | Cobalt lithium monoxide and simple synthesis method thereof |
Non-Patent Citations (1)
Title |
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赵玉超等: ""溶胶-凝胶-自蔓延燃烧法合成 LiNi0.5Mn1.5O4 的性能研"", 《化工新型材料》 * |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109437334A (en) * | 2018-10-31 | 2019-03-08 | 云南民族大学 | A kind of preparation method of high magnification nickel cobalt codope lithium manganate having spinel structure material |
CN109686974A (en) * | 2018-12-25 | 2019-04-26 | 安徽理工大学 | A method of burning or even detonation synthesize NCA battery material |
CN109686974B (en) * | 2018-12-25 | 2021-11-30 | 安徽理工大学 | Method for synthesizing NCA battery material by combustion and even deflagration |
CN114014380A (en) * | 2021-10-28 | 2022-02-08 | 蜂巢能源科技有限公司 | Lithium nickel manganese oxide, preparation method and application thereof |
WO2023184995A1 (en) * | 2022-03-29 | 2023-10-05 | 广东邦普循环科技有限公司 | Ternary positive electrode material having core-shell structure and preparation method therefor and use thereof |
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