CN108878828A - Carbon-coated nickelic tertiary cathode material of one kind and preparation method thereof - Google Patents
Carbon-coated nickelic tertiary cathode material of one kind and preparation method thereof Download PDFInfo
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- CN108878828A CN108878828A CN201810670898.1A CN201810670898A CN108878828A CN 108878828 A CN108878828 A CN 108878828A CN 201810670898 A CN201810670898 A CN 201810670898A CN 108878828 A CN108878828 A CN 108878828A
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- 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
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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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- 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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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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 present invention provides a kind of carbon-coated nickelic tertiary cathode materials and preparation method thereof, belong to anode material of lithium battery technical field.It solves the problems such as existing positive electrode cyclical stability and not high high rate performance, a kind of carbon-coated nickelic tertiary cathode material, including nickelic tertiary cathode material and clad, the clad consist of carbon, and the molar ratio of nickel, cobalt, manganese element in the nickelic tertiary cathode material is 0.7:0.2:0.25.
Description
Technical field
The invention belongs to the technical field of anode material of lithium battery, be related to a kind of carbon-coated nickelic tertiary cathode material and
Preparation method.
Background technique
Currently, the positive electrode type of large-scale commercial production is limited, such as LiFePO4, ternary, cobalt acid lithium.
Among these, ternary lithium battery is due to higher energy density, relatively low production cost and the attention by enterprise.
But for many years, since tertiary cathode material mentality of designing is simple, so material category is very limited, currently popular extensive quotient
The material of industryization application has 523,622 and 811, since the reversible capacity of 523,622 tertiary cathode materials is not still able to satisfy electricity
The growing capacity requirement of electrical automobile power battery.811 since nickel content is very high, and the alkalinity of material is strong, hygroscopic, it is easier to
So that positive electrode binder PVDF is reunited, and then influences processing performance, or even cannot produce.Therefore, the development of ternary material is met
Bottleneck is arrived.
The covering material of some functionalization can further promote the cycle performance and high rate performance of material.Carbon coating is
The important means of material conductivity, lower cost are improved, advantages of environment protection makes carbon coating be increasingly becoming positive electrode
Modified Critical policies.Such as the various carbon coating means of LiFePO4, it has been widely used on the market at present.
The carbon coating of commonsense method is also extremely limited for the promotion and improvement of performance.Reason is common carbon coating
For means during carbonization, common carbon source will form CO or H with reproducibility2Equal reducibility gas, very maximum probability journey
It can have a certain impact to tertiary cathode material on degree.So that the valence state of its various metal generates variation, so that lattice structure declines
It moves back.
Summary of the invention
The first purpose of the invention is to provide a kind of carbon-coated nickelic tertiary cathode material, second mesh of the invention
The preparation method for being to provide a kind of carbon-coated nickelic tertiary cathode material.
The first purpose of this invention can be realized by the following technical scheme：A kind of carbon-coated nickelic tertiary cathode material
Material, which is characterized in that including nickelic tertiary cathode material and clad, the clad consist of carbon, and described nickelic three
The molar ratio of nickel, cobalt, manganese element in first positive electrode is 0.7:0.2:0.25.
Second object of the present invention can be realized by the following technical scheme：A kind of carbon-coated nickelic tertiary cathode material
The preparation method of material, which is characterized in that include the following steps：
(1) by nickel sulfate, cobaltous sulfate, manganese sulfate in molar ratio 0.7:0.2:0.25 ratio is dissolved in removal O2Go from
In sub- water；
(2) by step (1) metal salt solution and sodium hydroxide solution according to flow 1:1.15 ratio is transported to instead
It answers in kettle, while being passed through ammonium hydroxide；The pH for controlling entire reaction system is 11.5, and the stirring rate for controlling reaction kettle is 580r/
Min, the temperature of reaction paste are 65 DEG C；
(3) it by the slurries filtration after reaction in step (2), washs, 120 DEG C of dryings obtain nickelic ternary precursor；
(4) by the presoma and lithium carbonate mole 1 in step (3):0.53 ratio is uniformly mixed in batch mixer；
(5) material after mixing in step (4) is put into saggar and is pushed into kiln, 785 DEG C of reaction temperature, the reaction time 18
A hour, O2 is passed through in whole process, reaction terminates up to target product；
(6) presoma of target product obtained in step (5) and silica is added in solvent, is stirred evenly
Afterwards, 20 DEG C~80 DEG C 2~7h of reaction are heated to, then solvent evaporated, finally in 200 DEG C~700 DEG C 2~8h of calcining, obtain institute
State the nickelic tertiary cathode material of coated with silica；
(7) the nickelic tertiary cathode material and carbon source of coated with silica will be obtained in step (6), with mass ratio 1%-
10% mixing is distributed in solvent, is stirred to react, is obtained suspension, suspension washing filtering is formed filter cake, in sky after drying
100 DEG C of -1000 DEG C of calcining 1h-20h in gas or nitrogen or argon gas obtain silica and nickelic tertiary cathode that carbon double-contracting is covered
Material；
(8) by the step (7) silica and the nickelic tertiary cathode material that covers of carbon double-contracting to be immersed in alkalinity molten
In liquid, carbon-coated nickelic tertiary cathode material is obtained.
Preferably, the presoma in the step (6) is silica dioxide granule, silicon tetrachloride, ethyl orthosilicate, diphenyl
One of dibromo (first) silane is a variety of.
Preferably, solvent is one of water, methanol, ethyl alcohol, isopropanol, ethylene glycol or a variety of in the step (6).
Preferably, in the step (6) in the nickelic tertiary cathode material of coated with silica silica quality hundred
Divide content in 0.5%~2wt%.
Preferably, the carbon source in the step (7) includes high-molecular organic material, glucide, dopamine.
Preferably, the solvent of the step (7) is one of water, ethyl alcohol, ethylene glycol, methylene chloride, methanol, isopropanol
Or it is a variety of.
Preferably, the alkaline solution in the step (8) is sodium hydroxide, potassium hydroxide, ammonium hydroxide, sodium bicarbonate, carbonic acid
One of sodium is a variety of.
Preferably, the concentration of the alkaline solution in the step (8) is 0.1mol/L-2mol/L.
Beneficial effects of the present invention：
1. traditional tertiary cathode material be designed with the molar ratio of nickel, cobalt, manganese adduction for 1 thought, and this
Nickelic positive electrode is then full with lithium in ternary material (+1 valence), nickel (+divalent), cobalt (+trivalent), manganese (+4 valence) each element mol ratio
The principle of sufficient substance electroneutral prepares a kind of novel nickelic tertiary cathode material LiNi0.7Co0.2Mn0.25O2, due in material
The content of nickel is higher, so improve the reversible capacity of material, while this material is because meet the principle of substance electroneutral,
Structure is stablized than traditional positive electrode during charge and discharge, and cycle performance is more excellent.
2. the method that the embodiment of the present invention prepares the nickelic tertiary cathode material of carbon coating, using silica as centre
Protective layer prevents carbon source from discharging reducibility gas reduction material of main part during high temperature cabonization, and the carbon coating layer of formation can be with
The more obvious electric conductivity for showing that conductive carbon is excellent, improves the high current charge-discharge ability of battery, to improve forthright again
Energy.
3. the high rate performance that the nickelic tertiary cathode material of carbon coating has good material circulation stability and material.
4. the method preparation flow of the embodiment of the present invention is simple, low in cost, it is suitable for industrialized production.
Detailed description of the invention
Fig. 1 is uncoated nickelic tertiary cathode material scanning electron microscope (SEM) photograph.
Specific embodiment
The present invention will be further described below with reference to examples.Following embodiment is only intended to clearly illustrate this
The performance of invention, and the following examples cannot be limited only to.
The preparation of the nickelic tertiary cathode material of embodiment 1
By nickel sulfate, cobaltous sulfate, manganese sulfate in molar ratio 0.7:0.2:0.25 ratio is dissolved in removal O2Deionization
In water；By metal salt solution and sodium hydroxide solution according to flow 1:1.15 ratio is transported in reaction kettle, while being passed through ammonia
Water；The pH for controlling entire reaction system is 11.5, and the stirring rate for controlling reaction kettle is 580r/min, and the temperature of reaction paste is
65℃.；Slurries filtration after reaction, washing, 120 DEG C of dryings obtain nickelic ternary precursor；By nickelic ternary precursor and carbon
Sour lithium mole 1:0.53 ratio is uniformly mixed in batch mixer；Material after mixing, which is put into saggar, is pushed into kiln, reaction temperature
785 DEG C of degree, O2 is passed through in whole process at 18 hours of reaction time, and reaction terminates up to target product.
One of the preparation of the carbon-coated nickelic tertiary cathode material of embodiment 2
1. the nickelic tertiary cathode material and ethyl orthosilicate (being converted to silica) in mass ratio 1 that will be prepared:
0.01 is blended in ethyl alcohol phase, 60 DEG C of stirring 3h, a certain amount of deionized water is being added dropwise according to stoichiometric ratio, 800r/min is anti-
It answers and is warming up to 100 DEG C after 3h and distributes all solvents, scrape powder and be placed in 500 DEG C of air and be sintered 5h, then cooled down,
Therefrom obtain the nickelic tertiary cathode material of coated with silica.
2. the nickelic tertiary cathode material of coated with silica is added to heating stirring in 5% glucose solution,
It is evaporated to dryness, is then placed in tube furnace and is sintered 3h under the atmosphere of nitrogen for 800 DEG C, the double-contracting of silica and carbon is covered nickelic
Tertiary cathode material.
It is soaked 3. the nickelic tertiary cathode material that the double-contracting of silica and carbon is covered is put into the NaOH solution of 0.5mol/L
Bubble 1h is etched away, and is obtained simple carbon encapsulated material, then filtering drying, is completed the preparation of carbon-coated positive electrode.
The two of the preparation of the carbon-coated nickelic tertiary cathode material of embodiment 3
1. the nickelic tertiary cathode material and silicon tetrachloride (being converted to silica) in mass ratio 1 that will be prepared:0.005
It is blended in ethyl alcohol phase, 20 DEG C are stirred, 7h, a certain amount of deionized water are being added dropwise according to stoichiometric ratio, 800r/min reacts 3h
After be warming up to 100 DEG C and distribute all solvents, scrape powder juxtaposition, 8h be sintered in 200 DEG C of air, is then cooled down, therefrom
Obtain the nickelic tertiary cathode material of coated with silica.
2. the nickelic tertiary cathode material of coated with silica is added to heating stirring in 1% glucose solution,
It is evaporated to dryness, is then placed in tube furnace and is sintered 20h, the height that the double-contracting of silica and carbon is covered under the atmosphere of nitrogen for 100 DEG C
Nickel tertiary cathode material.
3. the material in nickelic tertiary cathode material that the double-contracting of silica and carbon is covered to be put into the ammonium hydroxide of 0.1mol/L
1h is impregnated in solution to etch away, and is obtained simple carbon encapsulated material, then filtering drying, is completed the system of carbon-coated positive electrode
It is standby.
The three of the preparation of the carbon-coated nickelic tertiary cathode material of embodiment 4
1. the nickelic tertiary cathode material and silica dioxide granule in mass ratio 1 that will be prepared:0.02 is blended in methanol phase
In, 80 DEG C of stirring 2h are being added dropwise a certain amount of deionized water according to stoichiometric ratio, are being warming up to 100 after 800r/min reaction 3h
DEG C all solvents are distributed, scrape powder and be placed in 700 DEG C of air and be sintered 2h, is then cooled down, therefrom obtain titanium dioxide
The nickelic tertiary cathode material of silicon cladding.
2. the nickelic tertiary cathode material of coated with silica is added to heating stirring in 10% glucose solution,
It is evaporated to dryness, is then placed in tube furnace and is sintered 1h under the atmosphere of nitrogen for 1000 DEG C, the double-contracting of silica and carbon is covered nickelic
Tertiary cathode material.
3. the double-contracting of silica and carbon is covered nickelic tertiary cathode material and is put into the KOH solution of 2mol/L and impregnates 1h quarter
Eating away obtains simple carbon encapsulated material, then filtering drying, completes the preparation of carbon-coated positive electrode.
Comparative example 1
A kind of nickelic tertiary cathode material prepared is added to heating stirring in 10% glucose solution, is evaporated to
It is dry.It is then placed in tube furnace and is sintered 3h under the atmosphere of nitrogen for 800 DEG C.Obtain carbon-coated nickelic tertiary cathode material.
Comparative example 2
By common nickel-cobalt-manganternary ternary anode material (Li (Ni5Co2Mn3)O2) be added in 10% glucose solution
Heating stirring is evaporated to dryness.It is then placed in tube furnace and is sintered 3h under the atmosphere of nitrogen for 800 DEG C.Obtain carbon-coated nickel cobalt
Manganese tertiary cathode material.
Performance test
Assembled battery method：By in embodiment 1-4 and comparative example 1 positive electrode powder and conductive black super P and
Binder Kynoar (PVDF) is according to mass ratio 85：10：5 hand lappings are uniform.A certain amount of 1- methyl -2- pyrroles is added
Alkanone (NMP) is stirred evenly with refiner.Then it is scratched with plate coating machine, blade coating thickness is set as 0.02mm (drying
Before).It is put into 80 DEG C to dry five hours, places into 100 DEG C of vacuum oven overnights.It is cut to the electrode slice that diameter is 11.7mm, it
After be put into argon air box assembled battery in order.It is tested after standing one day after being completed.
Test method：Battery is tested on blue electricity 5V-5mA or 5V-10mA battery test system, and test method is with electric current
Density is to carry out charge-discharge test in the electrochemical window of 2.8-4.3V subject to 1C=180mA/g；And with 0.2C, 0.5C, 1C,
The circulation of charge and discharge is completed under 2C, 5C different multiplying powers.
Experimental result
By battery composed by embodiment 1-4 and comparative example 1 in 4.3V voltage range, under 0.5C multiplying power, discharge
Test (the unit of capacity：MAh/g), test result is as shown in table 1：
The discharge capacity test result of 1 battery of table
| Group | Capacity for the first time | Capacity after circulation 50 times | Capacity retention ratio |
| Embodiment 1 | 180.4 | 162.5 | 90.1% |
| Embodiment 2 | 197.9 | 195.5 | 98.8% |
| Embodiment 3 | 193.2 | 182.6 | 94.5% |
| Embodiment 4 | 190.1 | 183.3 | 96.4% |
| Comparative example 1 | 186.5 | 172.1 | 92.3% |
| Comparative example 2 | 176.0 | 143.0 | 81.3% |
By battery composed by embodiment 1-4 and comparative example 1 respectively under the multiplying power of 0.2C, 0.5C, 1C, 2C, 5C, test
Discharge capacity (unit：MAh/g), its discharge capacity of loop test at 0.2C again after circulation, discharge specific volume
The results are shown in Table 2 for amount：
Test result of 2 battery of table in different multiplying discharge capacity
| Group | 0.2C | 0.5C | 1C | 2C | 5C | 0.2C (after circulation) |
| Embodiment 1 | 183.4 | 179.8 | 168.7 | 151.9 | 140.6 | 180.0 |
| Embodiment 2 | 199.3 | 197.0 | 188.2 | 179.5 | 160.4 | 198.2 |
| Embodiment 3 | 197.6 | 192.3 | 187.8 | 176.3 | 158.3 | 195.0 |
| Embodiment 4 | 193.5 | 186.2 | 178.1 | 162.6 | 149.9 | 190.1 |
| Comparative example 1 | 189.7 | 181.3 | 170.1 | 157.4 | 145.0 | 186.2 |
| Comparative example 2 | 178.0 | 153.0 | 143.0 | 132.0 | 108.0 | 168.0 |
Specific embodiment described herein is only an example for the spirit of the invention.The neck of technology belonging to the present invention
The technical staff in domain can make various modifications or additions to the described embodiments or replace by a similar method
In generation, however, it does not deviate from the spirit of the invention or beyond the scope of the appended claims.
Claims (9)
1. a kind of carbon-coated nickelic tertiary cathode material, which is characterized in that including nickelic tertiary cathode material and clad, institute
The clad stated consist of carbon, and the molar ratio of nickel, cobalt, manganese element in the nickelic tertiary cathode material is 0.7:0.2:
0.25。
2. a kind of preparation method of carbon-coated nickelic tertiary cathode material, which is characterized in that include the following steps：
(1) by nickel sulfate, cobaltous sulfate, manganese sulfate in molar ratio 0.7:0.2:0.25 ratio is dissolved in removal O2Deionized water
In；
(2) by step (1) metal salt solution and sodium hydroxide solution according to flow 1:1.15 ratio is transported to reaction kettle
In, while being passed through ammonium hydroxide；The pH for controlling entire reaction system is 11.5, and the stirring rate for controlling reaction kettle is 580r/min, instead
The temperature for answering slurry is 65 DEG C；
(3) it by the slurries filtration after reaction in step (2), washs, 120 DEG C of dryings obtain nickelic ternary precursor；
(4) by the presoma and lithium carbonate mole 1 in step (3):0.53 ratio is uniformly mixed in batch mixer；
(5) material after mixing in step (4) is put into saggar and is pushed into kiln, it is 785 DEG C of reaction temperature, the reaction time 18 small
When, O2 is passed through in whole process, reaction terminates up to target product；
(6) presoma of target product obtained in step (5) and silica is added in solvent, after mixing evenly, is added
Heat is to 20 DEG C~80 DEG C 2~7h of reaction, and then solvent evaporated obtains the dioxy finally in 200 DEG C~700 DEG C 2~8h of calcining
The nickelic tertiary cathode material of SiClx cladding；
(7) the nickelic tertiary cathode material and carbon source of coated with silica will be obtained in step (6), it is mixed with mass ratio 1%-10%
Conjunction is distributed in solvent, is stirred to react, and suspension is obtained, and suspension washing filtering is formed filter cake, in air or nitrogen after drying
100 DEG C of -1000 DEG C of calcining 1h-20h in gas or argon gas obtain silica and nickelic tertiary cathode material that carbon double-contracting is covered；
(8) by the step (7) silica and the nickelic tertiary cathode material that covers of carbon double-contracting be immersed in alkaline solution,
Obtain carbon-coated nickelic tertiary cathode material.
3. the preparation method of the carbon-coated nickelic tertiary cathode material of one kind according to claim 2, which is characterized in that institute
The presoma in step (6) is stated as in silica dioxide granule, silicon tetrachloride, ethyl orthosilicate, diphenyl dibromo (first) silane
It is one or more.
4. the preparation method of the carbon-coated nickelic tertiary cathode material of one kind according to claim 2, which is characterized in that institute
Stating solvent in step (6) is one of water, methanol, ethyl alcohol, isopropanol, ethylene glycol or a variety of.
5. the preparation method of the carbon-coated nickelic tertiary cathode material of one kind according to claim 2, which is characterized in that institute
State the mass percentage of silica in the nickelic tertiary cathode material of coated with silica in step (6) 0.5%~
2wt%.
6. a kind of preparation method of the nickelic tertiary cathode material of dioxygen compound cladding according to claim 2, special
Sign is that the carbon source in the step (7) includes high-molecular organic material, glucide, dopamine.
7. a kind of preparation method of the nickelic tertiary cathode material of dioxygen compound cladding according to claim 2, special
Sign is that the solvent of the step (7) is one of water, ethyl alcohol, ethylene glycol, methylene chloride, methanol, isopropanol or a variety of.
8. a kind of preparation method of the nickelic tertiary cathode material of dioxygen compound cladding according to claim 2, special
Sign is, the alkaline solution in the step (8) is sodium hydroxide, potassium hydroxide, ammonium hydroxide, sodium bicarbonate, one in sodium carbonate
Kind is a variety of.
9. a kind of preparation method of the nickelic tertiary cathode material of dioxygen compound cladding according to claim 2, special
Sign is that the concentration of the alkaline solution in the step (8) is 0.1mol/L-2mol/L.
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| CN109728279A (en) * | 2018-12-29 | 2019-05-07 | 桂林电器科学研究院有限公司 | The surface treatment method and product and battery of a kind of nickelic tertiary cathode material |
| CN109994725A (en) * | 2018-12-12 | 2019-07-09 | 彩虹集团新能源股份有限公司 | A kind of manufacturing method of the nickelic tertiary cathode material of hydrophobic type |
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| CN111217408A (en) * | 2020-01-16 | 2020-06-02 | 东莞东阳光科研发有限公司 | High-nickel anode material and preparation method and application thereof |
| CN112151781A (en) * | 2020-09-24 | 2020-12-29 | 贵州梅岭电源有限公司 | Rapid composite coating modification method for lithium battery positive electrode material |
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| CN111217408B (en) * | 2020-01-16 | 2022-08-12 | 东莞东阳光科研发有限公司 | High-nickel anode material and preparation method and application thereof |
| CN113140713A (en) * | 2020-01-20 | 2021-07-20 | 中国科学院金属研究所 | LiFePO4/C-coated ternary cathode material and preparation method and application thereof |
| CN113889624A (en) * | 2020-07-02 | 2022-01-04 | 中国石油化工股份有限公司 | Carbon-coated ternary cathode material and preparation method and application thereof |
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| CN114005970A (en) * | 2021-10-12 | 2022-02-01 | 合肥国轩高科动力能源有限公司 | Carbon/conductive polymer coated ternary positive electrode material and preparation method thereof |
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