CN105406040A - Coated and modified high-nickel ternary cathode material and preparation method thereof - Google Patents
Coated and modified high-nickel ternary cathode material and preparation method thereof Download PDFInfo
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- CN105406040A CN105406040A CN201510740732.9A CN201510740732A CN105406040A CN 105406040 A CN105406040 A CN 105406040A CN 201510740732 A CN201510740732 A CN 201510740732A CN 105406040 A CN105406040 A CN 105406040A
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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
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
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- 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
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- 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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- 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 coated and modified high-nickel ternary cathode material and a preparation method thereof. With a LiNi<x>Co<(1-x)/2>Mn<(1-x)/2>O<2> material as a matrix, wherein x is smaller than or equal to 0.9 and greater than or equal to 0.6; a coating layer coats the outside of the matrix; the coating layer contains a plurality of nano metal salts and/or nano metal oxides; and the total weight of cationic metal accounts for 0.01%-10% of weight of a ternary cathode material. The preparation method disclosed by the invention comprises the following steps: firstly, dissolving a soluble aluminum salt into deionized water to obtain an aluminum salt solution; adding the LiNi<x>Co<(1-x)/2>Mn<(1-x)/2>O<2> material to the aluminum salt solution for mixing evenly to obtain paste; adding an alkaline solution which is prepared from an alkaline metal compound to the paste until the pH value is greater than or equal to 7.0; and carrying out drying, sintering, natural cooling, crushing and sieving, and then obtaining the coated and modified high-nickel ternary cathode material. According to the coated and modified high-nickel ternary cathode material, the alkalinity of a high-nickel material is lowered; the coated and modified high-nickel ternary cathode material is high in processability and excellent in cycle performance and safety performance.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries technical field, especially relate to a kind of nickelic tertiary cathode material and preparation method thereof.
Background technology
In recent years, along with the develop rapidly of the emerging markets such as 3C consumer electronics field, power tool and electric automobile, people propose requirements at the higher level to lithium ion battery, require that battery has high power capacity, long flying power, and cell safety is reliable.Therefore, the lithium ion battery developing the more high-energy-density of stable performance is imperative.LiNi
xco
(1-x)/2mn
(1-x)/2o
2(0.6≤x≤0.9) nickelic ternary material has the specific discharge capacity higher than cobalt acid lithium material, and has the cost of raw material feature cheaper relative to the sour lithium of cobalt.Being applied in conventional batteries, under the condition not increasing battery plus-negative plate active material, can significantly improving battery capacity, is one of positive electrode of developing low-cost lithium ion battery with high energy density the best.But, due to LiNi
xco
(1-x)/2mn
(1-x)/2o
2the reactivity of (0.6≤x≤0.9) nickelic ternary material is lower, and synthesized material residues lithium is higher, thus causes the basicity of material higher, have impact on the pole piece processing characteristics of nickelic ternary material.In addition, the remaining lithium of nickelic ternary material and electrolyte generation side reaction, thus cause subsiding of positive electrode crystal structure, cause cycle performance of lithium ion battery poor, easily occurs bulging, blast, unsafe problem such as on fire even under the high temperature conditions.These problems significantly limit the practical application of nickelic ternary material in lithium ion battery.
In order to solve the problem, domestic and international researcher improves nickelic ternary material mainly through doping and coated method.As CN104638227A Chinese patent literature discloses a kind of method of modifying of anode material for lithium-ion batteries, the method is for alkali treatment agent with the aluminium salt of low melting point or zirconates, after alkali treatment agent is mixed with the anode material for lithium-ion batteries of high ph-values, adopt double sintering technique, obtain final products.The method effectively reduces remaining lithium and pH value, but owing to being physical mixed, being difficult to ensure the evenly coated of coating layer, and have passed through two-step sintering, also improve the cost of sintering.
CN103500827A Chinese patent literature discloses a kind of lithium ion battery and polynary positive pole material, preparation method, the method first synthesize a kind of body mutually in containing nickel, cobalt, manganese three kinds of elements polynary presoma, again through precursor liquid phase surface doped Ti and lithiumation process, finally carry out surperficial pyrogenic process doped with Mg and coated Al
2o
3process, has obtained composite modified polynary lithium ion anode material.This preparation method effectively can improve the high-temperature behavior of material, but the method have passed through twice liquid phase coating, three calcinings, sintering process relative complex.In addition, prior art also has other processes mainly to choose the coated ternary material of metal oxide, the stabilizing effect of this kind of method to reinforcing material is better, but owing to adopting high polymer polyacrylamide etc. as dispersant and having filter progress, add the difficulty of technical process control, cost is higher.
Therefore, be necessary that developing the new method that a kind of technique is simple, with low cost and covered effect is desirable carries out modification to nickelic tertiary cathode material, thus promote material property further.
Summary of the invention
Technical problem to be solved by this invention is, overcomes the deficiency and defect mentioned in above background technology, provides a kind of nickelic tertiary cathode material of coating modification reducing high-nickel material basicity, good processability, cycle performance and security performance excellence.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is the nickelic tertiary cathode material of a kind of coating modification, and described nickelic tertiary cathode material is with LiNi
xco
(1-x)/2mn
(1-x)/2o
2material is matrix, wherein 0.6≤x≤0.9; Described matrix is coated with a coating layer, containing multiple nano metal salt and/or nano-metal-oxide in described coating layer; Cationic metal gross mass in described multiple nano metal salt and/or nano-metal-oxide accounts for 0.01% ~ 10% of described nickelic tertiary cathode material quality.
In the nickelic tertiary cathode material of above-mentioned coating modification, preferably, containing at least one in nano metal aluminium salt, nano aluminium oxide in described multiple nano metal salt and/or nano-metal-oxide, and also containing at least one in alkaline nanometer slaine, alkaline nanometer metal oxide.Preferred, described nano metal aluminium salt is aluminum fluoride, and described alkaline nanometer slaine is at least one in nanometer potassium sulfate, nanometer strontium chloride, nano silver/silver chloride, and described alkaline nanometer metal oxide is nano calcium oxide.
As a total technical conceive, the present invention also provides the preparation method of the nickelic tertiary cathode material of a kind of above-mentioned coating modification, comprises the following steps:
Aluminum soluble salt being dissolved in deionized water according to adding metering, obtaining aluminum salt solution;
By described LiNi
xco
(1-x)/2mn
(1-x)/2o
2material joins in above-mentioned aluminum salt solution and fully mixes, and obtains slurry;
Alkaline metal cpds being dissolved in deionized water according to adding metering, obtaining alkaline solution;
The alkaline solution of gained is joined in above-mentioned slurry, makes pH value >=7.0 of slurry; Fully be uniformly mixed again, after drying obtained mixture; After slurry preparation completes, the pH value < 7.0 of gained slurry, then what need to reduce aluminum soluble salt adds metering, or improve alkaline metal cpds add metering, make pH value >=7.0 of gained slurry;
The mixture of gained is put into reacting furnace, sinters under air or oxygen atmosphere, naturally cool, products therefrom is through pulverizing and obtaining the nickelic tertiary cathode material of coating modification after sieving.
Above-mentioned preparation method, preferably, described aluminum soluble salt comprise in aluminium chloride, aluminum acetate, aluminum sulfate, aluminum nitrate one or more.
Above-mentioned preparation method, preferably, described alkaline metal cpds comprise in potassium hydroxide, NaOH, potassium fluoride, sodium fluoride, calcium hydroxide, strontium hydroxide, barium hydroxide and silver diamminohydroxide one or more.
Above-mentioned preparation method, preferably, described sintering refers to and is warmed up to constant temperature process 1 ~ 20h at 300 DEG C ~ 900 DEG C temperature.
Above-mentioned preparation method, preferably, the scope that metering accounts for 0.01 ~ 10% of nickelic tertiary cathode material quality according to the cationic metal gross mass of described aluminum soluble salt and alkaline metal cpds that adds of described aluminum soluble salt and alkaline metal cpds adds.
The present invention adopts liquid phase method, make to be evenly dispersed in solution containing two kinds of aluminium and the element of above slaine or the coated material of metal oxide, with the well-mixed process of positive electrode, metallic aluminium is precipitated by original position generation alkaline environment or exogenously added alkali, simultaneously in the process of drying, go out uniform nano metal salt or metal oxide nano coating layer at the surface crystallization of positive electrode, achieve containing two kinds of aluminium and above nano metal salt or metal oxide coated uniformly to positive pole material surface.
Compared with prior art, the invention has the advantages that: the aluminum soluble salt that the present invention adds can integrate the remaining lithium in nickelic positive electrode effectively, the coated material formed has intercepted the side reaction that nickelic ternary material and electrolyte occur effectively, the effect of stable crystal structure is served when discharge and recharge, thus improve the processing characteristics of nickelic ternary material, greatly improve cycle performance and the security performance of nickelic ternary material.
Tertiary cathode material of the present invention is having more low alkalinity by modified, thus improve processing characteristics greatly, cycle performance and security performance are also significantly improved, being the positive electrode being applied in lithium ion battery with high energy density middle ideal, is also the positive electrode being applied in 3C electronics, electric tool and electric automobile middle ideal; Synthetic method is simple, is easy to industrialization.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is 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 electron scanning micrograph of the nickelic tertiary cathode material of embodiment 1 coating modification.
Fig. 2 is the X ray diffracting spectrum of the nickelic tertiary cathode material of embodiment 1 coating modification;
Fig. 3 is the cycle performance figure of the nickelic tertiary cathode material of embodiment 1 coating modification, and its charge-discharge magnification is 1C/1C, and voltage range is 3.0 ~ 4.2V, tests at normal temperature 25 DEG C.
Embodiment
For the ease of understanding the present invention, hereafter will do to describe more comprehensively, meticulously to the present invention in conjunction with Figure of description and preferred embodiment, but protection scope of the present invention is not limited to following specific embodiment.
Unless otherwise defined, hereinafter used all technical terms are identical with the implication that those skilled in the art understand usually.The object of technical term used herein just in order to describe specific embodiment is not be intended to limit the scope of the invention.
Unless otherwise specified, the various raw material, reagent, instrument and equipment etc. used in the present invention are all bought by market and are obtained or prepare by existing method.
Embodiment 1:
The nickelic tertiary cathode material of a kind of coating modification of the present invention is with LiNi
0.6co
0.2mn
0.2o
2material is matrix; Matrix is coated with nano aluminium oxide and nano calcium oxide; Cationic metal gross mass in nano aluminium oxide and nano calcium oxide accounts for 0.17% of nickelic tertiary cathode material quality.
The preparation method of the nickelic tertiary cathode material of coating modification that the present embodiment is above-mentioned, specifically comprises the following steps:
1) 6.5g aluminum nitrate being dissolved in 500ml deionized water according to adding metering, obtaining aluminum nitrate solution;
2) 1000gLiNi will prepared
0.6co
0.2mn
0.2o
2basis material joins in above-mentioned aluminum nitrate solution and fully mixes, and obtains slurry;
3) get excess calcium hydroxide to be dissolved in the deionized water of 30 DEG C, obtain the clarification limewash that 1500ml is saturated; At 30 DEG C, the solubility of calcium hydroxide is 0.153g, has both added the quality > 2.30g of calcium hydroxide;
4) 1500ml of gained is clarified limewash to join in above-mentioned slurry, make the pH value of slurry be about 11.5; Fully be uniformly mixed 2h again, after drying obtained mixture;
5) mixture of gained is put into Muffle furnace, sinter in air atmosphere, constant temperature process 10h at being warming up to 550 DEG C, naturally cool, material is direct after coming out of the stove crosses manual sieve, the obtained coating modification LiNi being coated with nano aluminium oxide and calcium oxide
0.6co
0.2mn
0.2o
2tertiary cathode material.
The coating modification LiNi that the present embodiment obtains
0.6co
0.2mn
0.2o
2as shown in Figure 1, adopt the surface topography of the S-4800 cold field emission electron microscope observation sample of HIT, multiplication factor is 10000 times to the electron scanning micrograph of tertiary cathode material.As can be seen from Figure 1 LiNi
0.6co
0.2mn
0.2o
2particle surface has the equally distributed coating layer of one deck.
As shown in Figure 2, as can be seen from Figure 2, because covering amount is less, the crystal structure of coated rear material is still pure phase structure to the material X ray diffracting spectrum that the present embodiment obtains, and does not occur oxide impurity peak.
The electrochemical property test of the nickelic tertiary cathode material of the present embodiment coating modification adopts 523450 type aluminum-shell batteries, and negative electrode active material is Bei Terui 818; Adopt new prestige battery test system to test under normal temperature (25 DEG C), test voltage scope is 3.0 ~ 4.2V; Carry out discharge and recharge with 1C multiplying power, circulate 250 weeks, investigate capability retention.As shown in Figure 3, as seen from Figure 3, the nickelic tertiary cathode material of coating modification of the present embodiment is 164mAh/g at 1C specific discharge capacity to the cycle performance figure of this material, illustrate coated after LiNi
0.6co
0.2mn
0.2o
2still maintain higher specific discharge capacity, the 1C charge and discharge 250 weeks capability retentions that circulate are 89.0%, illustrate that this material has good cycle performance under high voltages.
Embodiment 2:
The nickelic tertiary cathode material of a kind of coating modification of the present invention is with LiNi
0.8co
0.1mn
0.1o
2material is matrix; Matrix is coated with nanometer aluminum fluoride and nanometer potassium sulfate; Cationic metal gross mass in nanometer aluminum fluoride and nanometer potassium sulfate accounts for 9.4% of nickelic tertiary cathode material quality.
The preparation method of the nickelic tertiary cathode material of coating modification that the present embodiment is above-mentioned, specifically comprises the following steps:
1) 296.5g aluminum sulfate being dissolved in 1000ml deionized water according to adding metering, obtaining aluminum sulfate solution;
2) 2000gLiNi will prepared
0.8co
0.1mn
0.1o
2basis material joins in above-mentioned aluminum sulfate solution and fully mixes, and obtains slurry;
3) get 200.2g potassium fluoride to be dissolved in 1000ml deionized water, obtain potassium fluoride solution;
4) potassium fluoride solution of gained is joined in above-mentioned slurry, make the pH value of slurry be about 9.0; Fully be uniformly mixed 1h again, after drying obtained mixture;
5) mixture of gained is put into Muffle furnace, sinter in air atmosphere, constant temperature process 18h at being warming up to 350 DEG C, naturally cool, material is direct after coming out of the stove crosses manual sieve, the obtained nickelic tertiary cathode material of coating modification.
Embodiment 3:
The nickelic tertiary cathode material of a kind of coating modification of the present invention is with LiNi
0.7mn
0.15co
0.15o
2material is matrix; Matrix is coated with nano aluminium oxide, nanometer strontium chloride and nano silver/silver chloride; Cationic metal gross mass in nano aluminium oxide, nanometer strontium chloride and nano silver/silver chloride accounts for 3.5% of nickelic tertiary cathode material quality.
The preparation method of the nickelic tertiary cathode material of coating modification that the present embodiment is above-mentioned, specifically comprises the following steps:
1) 10.49g aluminium chloride being dissolved in 120ml deionized water according to adding metering, obtaining liquor alumini chloridi;
2) 500gLiNi will prepared
0.7mn
0.15co
0.15o
2basis material joins in above-mentioned liquor alumini chloridi and fully mixes, and obtains slurry;
3) get 8.71g strontium hydroxide to be dissolved in 500ml deionized water, obtain strontium hydroxide solution; Get 14.73g silver diamminohydroxide to be dissolved in 500ml deionized water.
4) strontium hydroxide solution of gained and silver diamminohydroxide solution are joined in above-mentioned slurry, make the pH value of slurry be about 7.5; Fully be uniformly mixed 3h again, after drying obtained mixture;
5) mixture of gained is put into Muffle furnace, sinter under oxygen atmosphere, constant temperature process 2h at being warming up to 850 DEG C, naturally cool, material is direct after coming out of the stove crosses manual sieve, the obtained nickelic tertiary cathode material of coating modification.
Embodiment recited above is only be described embodiments of the present invention; under the prerequisite not departing from design concept of the present invention; the various modification that the R&D personnel in this area is made technical scheme of the present invention and improvement, all should fall into protection scope of the present invention.
Claims (8)
1. the nickelic tertiary cathode material of coating modification, is characterized in that, described nickelic tertiary cathode material is with LiNi
xco
(1-x)/2mn
(1-x)/2o
2material is matrix, wherein 0.6≤x≤0.9; Described matrix is coated with a coating layer, containing multiple nano metal salt and/or nano-metal-oxide in described coating layer; Cationic metal gross mass in described multiple nano metal salt and/or nano-metal-oxide accounts for 0.01% ~ 10% of described nickelic tertiary cathode material quality.
2. the nickelic tertiary cathode material of coating modification according to claim 1, it is characterized in that, containing at least one in nano metal aluminium salt, nano aluminium oxide in described multiple nano metal salt and/or nano-metal-oxide, and also containing at least one in alkaline nanometer slaine, alkaline nanometer metal oxide.
3. the nickelic tertiary cathode material of coating modification according to claim 2, it is characterized in that, described nano metal aluminium salt is aluminum fluoride, described alkaline nanometer slaine is at least one in nanometer potassium sulfate, nanometer strontium chloride, nano silver/silver chloride, and described alkaline nanometer metal oxide is nano calcium oxide.
4. a preparation method for the nickelic tertiary cathode material of the coating modification according to any one of claim 1-3, comprises the following steps:
Aluminum soluble salt being dissolved in deionized water according to adding metering, obtaining aluminum salt solution;
By described LiNi
xco
(1-x)/2mn
(1-x)/2o
2material joins in above-mentioned aluminum salt solution and fully mixes, and obtains slurry;
Alkaline metal cpds being dissolved in deionized water according to adding metering, obtaining alkaline solution;
The alkaline solution of gained is joined in above-mentioned slurry, makes pH value >=7.0 of slurry; Fully be uniformly mixed again, after drying obtained mixture;
The mixture of gained is put into reacting furnace, sinters under air or oxygen atmosphere, naturally cool, products therefrom is through pulverizing and obtaining the nickelic tertiary cathode material of coating modification after sieving.
5. preparation method according to claim 4, is characterized in that, described aluminum soluble salt comprise in aluminium chloride, aluminum acetate, aluminum sulfate, aluminum nitrate one or more.
6. preparation method according to claim 4, is characterized in that, described alkaline metal cpds comprise in potassium hydroxide, NaOH, potassium fluoride, sodium fluoride, calcium hydroxide, strontium hydroxide, barium hydroxide and silver diamminohydroxide one or more.
7. the preparation method according to claim 4,5 or 6, is characterized in that, described sintering refers to and is warmed up to constant temperature process 1 ~ 20h at 300 DEG C ~ 900 DEG C temperature.
8. the preparation method according to claim 4,5 or 6, it is characterized in that, the scope that metering accounts for 0.01 ~ 10% of nickelic tertiary cathode material quality according to the cationic metal gross mass of described aluminum soluble salt and alkaline metal cpds that adds of described aluminum soluble salt and alkaline metal cpds adds.
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|---|---|---|---|---|
| CN105932259A (en) * | 2016-06-30 | 2016-09-07 | 复旦大学 | Surface treatment method of nickel-cobalt lithium manganate positive electrode material |
| CN106299320A (en) * | 2016-11-07 | 2017-01-04 | 珠海格力电器股份有限公司 | A kind of cobalt nickel lithium manganate ternary material of modification and preparation method thereof |
| CN107591532A (en) * | 2017-08-22 | 2018-01-16 | 中航锂电（洛阳）有限公司 | A kind of aluminum fluoride/silver-colored double-coating nickel-cobalt lithium manganate cathode material and preparation method thereof |
| CN108130074A (en) * | 2018-01-15 | 2018-06-08 | 东南大学 | A kind of method for preparing high crystalline nano silicon nitride matter fluorescent powder |
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| CN108682822A (en) * | 2018-05-30 | 2018-10-19 | 陕西煤业化工技术研究院有限责任公司 | A kind of nickelic ternary material of long circulation life and preparation method thereof |
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