CN103730653A - Method for preparing rare earth element-doped nickel cobalt lithium manganate positive electrode material - Google Patents
Method for preparing rare earth element-doped nickel cobalt lithium manganate positive electrode material Download PDFInfo
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- CN103730653A CN103730653A CN201410007088.XA CN201410007088A CN103730653A CN 103730653 A CN103730653 A CN 103730653A CN 201410007088 A CN201410007088 A CN 201410007088A CN 103730653 A CN103730653 A CN 103730653A
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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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- 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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- 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 method for preparing a rare earth element-doped nickel cobalt lithium manganate positive electrode material. The method comprises the following steps: dissolving nickel cobalt manganese salts in water to prepare a solution, adding a rare earth soluble salt, preparing ammonia water by taking ammonia water serving as a complexing agent according to a salt ammonia ratio, and preparing into a solution with NaOH as a precipitator; respectively adding the ammonia water and sodium hydroxide in a nitrogen atmosphere under the condition of water bath temperature of 70 DEG C, and stirring during the reaction process so that the reaction can be uniform; stirring and ageing for 10-15 hours, filtering the obtained reaction solution to obtain a precursor of nickel cobalt lithium manganate, performing microwave drying, and drying in a vacuum drying oven for 5 hours; mixing the precursor with a lithium salt, and mechanically performing ball milling and mixing through a wet method; sintering the material at the treatment temperature of 700-850 DEG C, and introducing oxygen in the sintering process; and grinding the material subjected to complete sintering, and allowing the material to pass through a 325-mesh sieve, thus obtaining the final product.
Description
Technical field
The present invention relates to a kind of method of doped with rare-earth elements modification lithium-ion secondary cell nickel-cobalt lithium manganate cathode material of passing through, relate in particular to a kind of preparation method of nickel-cobalt lithium manganate cathode material of doped with rare-earth elements.
Background technology
In recent years, for reply auto industry fast development bring such as negative effects such as environmental pollution petroleum resources sharply consume, each state is all actively developing the employing electric automobile EV of clean energy resource and the research of hybrid-power electric vehicle HEV, and using it as the inevitable direction of automobile industry development from now on, wherein as the electrokinetic cell of vehicle-mounted power, directly affect the performance of electric motor car, and the Main Bottleneck lithium-ion-power cell that becomes EV and HEV development is as the topmost candidate's electrical source of power of following electric automobile, the feature with excellent performance with low cost, become the main target of research.
Business-like lithium ion battery mainly adopts LiCoO
2as positive electrode, because cobalt resource is deficient, cause lithium ion battery high expensive, limited the expansion of its application, particularly the application in electrokinetic cell.The LiNi of nickel-cobalt-manganese ternary compound transition metal oxide Ni-Co-Mn element cooperative effect
0.5co
0.2mn
0.3o
2combine the advantage of other materials, as LiCoO
2good cycle performance LiNiO
2height ratio capacity and LiMn
2o
4high security and the feature such as low-cost, be considered to have most the novel anode material of application prospect, be also considered to the ideal chose for pure electrical source of power (EV) and mixed type electrical source of power (HEV).
Summary of the invention
The object of this invention is to provide a kind of preparation technology simple, the low and synthetic product that requires of equipment is had to the preparation method of nickel-cobalt lithium manganate cathode material of a kind of doped with rare-earth elements of high specific capacity and excellent cycle performance.
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of nickel-cobalt lithium manganate cathode material of doped with rare-earth elements, is characterized in that: comprise the following steps:
(1) salt of nickel cobalt manganese is water-soluble, be mixed with solution, then add rare earth soluble-salt, with ammoniacal liquor, as complexing agent, with salt ammonia, than preparation ammoniacal liquor, use NaOH as precipitation reagent, and be mixed with solution;
(2) under the condition of 70 ℃ of nitrogen atmosphere and water-baths, add respectively ammoniacal liquor and NaOH, in course of reaction, need to stir, make the reaction can be evenly;
(3) stir ageing 10-15 hour;
(4) step (3) gained reacting liquid filtering is obtained to the presoma of nickle cobalt lithium manganate, after microwave drying, then in vacuum drying oven, be dried 5 hours;
(5) presoma in step (4) is mixed in proportion with lithium salts, and by wet method machinery ball mill mixing;
(6) by the sintering under the treatment temperature of 700～850 ℃ of the material in step (5), sintering process passes into oxygen;
(7) material after sintering was ground to 325 mesh sieves, obtained final products.
In the method, the salt of described nickel cobalt manganese is soluble-salt, and solution is 1.5moL/L; The concentration of described NaOH solution is 4 moL/L; Described lithium salts is a kind of or its mixture in lithium carbonate, lithium hydroxide, lithium nitrate; Described rare earth soluble-salt is a kind of in lanthanum nitrate, ceric sulfate soluble rare-earth salt or multiple mixture wherein.
In the method, the salt of nickel cobalt manganese described in step (1) and the mol ratio of ammoniacal liquor are 0.2～1.0; The integral molar quantity of nickel cobalt manganese of take is total amount, and rare earth soluble-salt accounts for 0.02～0.10%; Presoma is 1.0～1.2 with the ratio of lithium salts.
In the method, contain one or more rare earth elements in synthetic nickel-cobalt lithium manganate material, described rare earth element is one or more in La, Ce, Pr, Nd, Sm, Dy, Ho.
Advantageous effect of the present invention is: owing to having used preparation method of the present invention, so the product of preparation has the following advantages: 1) synthetic product granularity is even, and tap density is large; 2) capacity of product is high, and cycle performance is good; 3) raw material using at a low price; 4) technique is simple, and suitability for industrialized is produced.
Accompanying drawing explanation
Fig. 1 is LiNi
0.5co
0.2mn
0.3o
2surface topography SEM figure after rare earth doped salt;
Fig. 2 is the LiNi of rare earth doped salt
0.5co
0.2mn
0.3o
2cycle graph.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described:
The present invention as shown in Figure 1, 2,
embodiment 1
Choose nickelous sulfate, cobaltous sulfate and manganese sulfate as raw material, be configured to the solution of 2moL/L, add four-hole boiling flask, rare-earth salts ceric sulfate accounts for 2% of nickelous sulfate, cobaltous sulfate and manganese sulfate gross mass.Then ceric sulfate is added in solution and dissolved.The ammoniacal liquor of configuration 15% and the NaOH of 4moL/L.In ammoniacal liquor and nickelous sulfate, cobaltous sulfate and manganese sulfate solution, the ratio of the integral molar quantity of nickel, cobalt, manganese is 0.2:1.
The ammoniacal liquor configuring is splashed in solution to complexing 50min by constant pressure funnel.Then drip NaOH, the pH value of controlling solution is 12 left and right.Ageing 10 hours, the precursor then filtering, vacuum drying 5 hours.
The precursor of oven dry and lithium carbonate are prepared burden according to a certain ratio, and wet method machinery ball milling mixes.Dry, calcining, sintering temperature is 750 ℃, 10 hours.After sintering, ground 325 mesh sieves.
By synthetic nickle cobalt lithium manganate, acetylene black, binding agent polyvinylidene fluoride (PVDF) in mass ratio 85:10:5 mix, twin rollers press mold, dries, stamp film, puts into glove box.Take lithium metal as negative pole assembling button cell, carry out electro-chemical test.
First and second time of charge-discharge magnification is 0.1C, is for 3,4 times 0.5C, and the 5th is 1.0C later, and voltage range is 2.7～4.3, and reversible specific capacity is 158mAh/g first, repeatedly after circulation, occurs decay, and after 500 circulations, Capacitance reserve is more than 80%.
embodiment 2
Choose nickelous sulfate, cobaltous sulfate and manganese sulfate as raw material, be configured to the solution of 2moL/L, add four-hole boiling flask, rare-earth salts lanthanum nitrate accounts for 2% of nickelous sulfate, cobaltous sulfate and manganese sulfate gross mass.Then lanthanum nitrate is added in solution and dissolved.The ammoniacal liquor of configuration 15% and the NaOH of 4moL/L.In ammoniacal liquor and nickelous sulfate, cobaltous sulfate and manganese sulfate solution, the ratio of the integral molar quantity of nickel, cobalt, manganese is 0.5:1.
The ammoniacal liquor configuring is splashed in solution to complexing 50min by constant pressure funnel.Then drip NaOH, the pH value of controlling solution is 12 left and right.Ageing 10 hours, the precursor then filtering, vacuum drying 5 hours.
The precursor of oven dry and lithium hydroxide are prepared burden according to a certain ratio, and wet method machinery ball milling mixes.Dry, calcining, sintering temperature is 750 ℃, 10 hours.After sintering, ground 325 mesh sieves.
Chemical property detects with embodiment 1.
embodiment 3
Choose nickelous sulfate, cobaltous sulfate and manganese sulfate as raw material, be configured to the solution of 2moL/L, add four-hole boiling flask, rare-earth salts ceric sulfate and lanthanum nitrate account for 2% of nickelous sulfate, cobaltous sulfate and manganese sulfate gross mass.Then ceric sulfate and lanthanum nitrate are added in solution and dissolved.The ammoniacal liquor of configuration 15% and the NaOH of 4moL/L.In ammoniacal liquor and nickelous sulfate, cobaltous sulfate and manganese sulfate solution, the ratio of the integral molar quantity of nickel, cobalt, manganese is 1.0:1.
The ammoniacal liquor configuring is splashed in solution to complexing 50min by constant pressure funnel.Then drip NaOH, the pH value of controlling solution is 12 left and right.Ageing 10 hours, the precursor then filtering, vacuum drying 5 hours.
The precursor of oven dry and lithium hydroxide are prepared burden according to a certain ratio, and wet method machinery ball milling mixes.Dry, calcining, sintering temperature is 750 ℃, 10 hours.After sintering, ground 325 mesh sieves.
Chemical property detects with embodiment 1.
A kind ofly by doped with rare-earth elements, prepare lithium ion secondary battery anode material LiNi
0.5co
0.2mn
0.3o
2method, the preparation method of the lithium ion secondary battery anode material class spherical nickel-cobalt LiMn2O4 of a kind of synthesizing blender rare earth element La and Ce, Pr, Nd, Sm, Dy, Ho etc., take nickel, cobalt, manganese, rare earth soluble-salt is raw material, adopts coprecipitation synthesizing lithium ion precursor of nickel-cobalt-lithium-manganese-oxide; Then press certain proportion ingredient with lithium salts, adopt the method for wet method machinery ball milling to carry out batch mixing; Last sintering, crosses 325 mesh sieves, makes simulated battery, and capacity is more than 170mAh/g first, and first effect is greater than 92%, and after cycle performance button electricity half-cell can reach 500 circulations, Capacitance reserve is 90%; And with low cost, technique is simple, be applicable to the production of large-scale industrialization, synthetic stable performance, cycle performance excellence, high conformity, be with a wide range of applications.
Claims (7)
1. a preparation method for the nickel-cobalt lithium manganate cathode material of doped with rare-earth elements, is characterized in that: comprise the following steps:
(1) salt of nickel cobalt manganese is water-soluble, be mixed with solution, then add rare earth soluble-salt, with ammoniacal liquor, as complexing agent, with salt ammonia, than preparation ammoniacal liquor, use NaOH as precipitation reagent, and be mixed with solution;
(2) under the condition of 70 ℃ of nitrogen atmosphere and water-baths, add respectively ammoniacal liquor and NaOH, in course of reaction, need to stir, make the reaction can be evenly;
(3) stir ageing 10-15 hour;
(4) step (3) gained reacting liquid filtering is obtained to the presoma of nickle cobalt lithium manganate, after microwave drying, then in vacuum drying oven, be dried 5 hours;
(5) presoma in step (4) is mixed in proportion with lithium salts, and by wet method machinery ball mill mixing;
(6) by the sintering under the treatment temperature of 700～850 ℃ of the material in step (5), sintering process passes into oxygen;
(7) material after sintering was ground to 325 mesh sieves, obtained final products.
2. the preparation method of the nickel-cobalt lithium manganate cathode material of a kind of doped with rare-earth elements according to claim 1, is characterized in that: the salt of described nickel cobalt manganese is soluble-salt, and solution is 1.5moL/L; The concentration of described NaOH solution is 4 moL/L; Described lithium salts is a kind of or its mixture in lithium carbonate, lithium hydroxide, lithium nitrate; Described rare earth soluble-salt is a kind of in lanthanum nitrate, ceric sulfate soluble rare-earth salt or multiple mixture wherein.
3. the preparation method of the nickel-cobalt lithium manganate cathode material of a kind of doped with rare-earth elements according to claim 2, is characterized in that: the salt of nickel cobalt manganese described in step (1) and the mol ratio of ammoniacal liquor are 0.2～1.0; The integral molar quantity of nickel cobalt manganese of take is total amount, and rare earth soluble-salt accounts for 0.02～0.10%; Presoma is 1.0～1.2 with the ratio of lithium salts.
4. the preparation method of the nickel-cobalt lithium manganate cathode material of a kind of doped with rare-earth elements according to claim 3, it is characterized in that: in synthetic nickel-cobalt lithium manganate material, contain one or more rare earth elements, described rare earth element is one or more in La, Ce, Pr, Nd, Sm, Dy, Ho.
5. the preparation method of the nickel-cobalt lithium manganate cathode material of a kind of doped with rare-earth elements according to claim 1, it is characterized in that: choose nickelous sulfate, cobaltous sulfate and manganese sulfate as raw material, be configured to the solution of 2moL/L, add four-hole boiling flask, rare-earth salts ceric sulfate accounts for 2% of nickelous sulfate, cobaltous sulfate and manganese sulfate gross mass, then ceric sulfate is added in solution and dissolved, configuration 15% ammoniacal liquor and the NaOH of 4moL/L, in ammoniacal liquor and nickelous sulfate, cobaltous sulfate and manganese sulfate solution, the ratio of the integral molar quantity of nickel, cobalt, manganese is 0.2:1; The ammoniacal liquor configuring is splashed in solution by constant pressure funnel, and complexing 50min, then drips NaOH, and the pH value of controlling solution is 12 left and right, ageing 10 hours, the precursor then filtering, vacuum drying 5 hours; The precursor of oven dry and lithium carbonate are prepared burden in proportion, and wet method machinery ball milling mixes, dry, calcining, and sintering temperature is 750 ℃, 10 hours, after sintering, ground 325 mesh sieves, obtain final products.
6. the preparation method of the nickel-cobalt lithium manganate cathode material of a kind of doped with rare-earth elements according to claim 1, it is characterized in that: choose nickelous sulfate, cobaltous sulfate and manganese sulfate as raw material, be configured to the solution of 2moL/L, add four-hole boiling flask, rare-earth salts lanthanum nitrate accounts for 2% of nickelous sulfate, cobaltous sulfate and manganese sulfate gross mass; Then lanthanum nitrate is added in solution and dissolved, configuration 15% ammoniacal liquor and the NaOH of 4moL/L, in ammoniacal liquor and nickelous sulfate, cobaltous sulfate and manganese sulfate solution, the ratio of the integral molar quantity of nickel, cobalt, manganese is 0.5:1; The ammoniacal liquor configuring is splashed in solution by constant pressure funnel, and complexing 50min, then drips NaOH, and the pH value of controlling solution is 12 left and right, ageing 10 hours, the precursor then filtering, vacuum drying 5 hours; The precursor of oven dry and lithium hydroxide are prepared burden in proportion, and wet method machinery ball milling mixes, dry, calcining, and sintering temperature is 750 ℃, 10 hours; After sintering, grind 325 mesh sieves, obtained final products.
7. the preparation method of the nickel-cobalt lithium manganate cathode material of a kind of doped with rare-earth elements according to claim 1, it is characterized in that: choose nickelous sulfate, cobaltous sulfate and manganese sulfate as raw material, be configured to the solution of 2moL/L, add four-hole boiling flask, rare-earth salts ceric sulfate and lanthanum nitrate account for 2% of nickelous sulfate, cobaltous sulfate and manganese sulfate gross mass, then ceric sulfate and lanthanum nitrate are added in solution and dissolved, configuration 15% ammoniacal liquor and the NaOH of 4moL/L, in ammoniacal liquor and nickelous sulfate, cobaltous sulfate and manganese sulfate solution, the ratio of the integral molar quantity of nickel, cobalt, manganese is 1.0:1; The ammoniacal liquor configuring is splashed in solution by constant pressure funnel, and complexing 50min, then drips NaOH, and the pH value of controlling solution is 12 left and right, ageing 10 hours, the precursor then filtering, vacuum drying 5 hours; The precursor of oven dry and lithium hydroxide are prepared burden in proportion, and wet method machinery ball milling mixes, dry, calcining, and sintering temperature is 750 ℃, 10 hours, after sintering, ground 325 mesh sieves, obtain final products.
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