CN104868114A - Preparation method of nickel-rich concentration gradient nickel-cobalt-manganese anode material with low acidity or alkalinity and high processability - Google Patents
Preparation method of nickel-rich concentration gradient nickel-cobalt-manganese anode material with low acidity or alkalinity and high processability Download PDFInfo
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- CN104868114A CN104868114A CN201510157141.9A CN201510157141A CN104868114A CN 104868114 A CN104868114 A CN 104868114A CN 201510157141 A CN201510157141 A CN 201510157141A CN 104868114 A CN104868114 A CN 104868114A
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a preparation method of a nickel-rich concentration gradient nickel-cobalt-manganese anode material with low acidity or alkalinity and high processability. The preparation method comprises the following steps: firstly mixing a nickel-cobalt-manganese compound and a lithium compound in a proportion of Li to M being 1-1.1, performing first sintering under certain conditions of temperature, airflow and time, and then smashing and sieving a first sintering product to initially prepare and obtain a nickel-cobalt lithium manganate intermediate product; then uniformly mixing the intermediate product with an organic matter in a certain proportion, performing second sintering through a period of time under a certain temperature condition, and then smashing and sieving a second sintering product to obtain nickel-cobalt lithium manganate with low acidity or alkalinity and high processability. The material has the advantages of novel preparation technology and low acidity or alkalinity, and is high in processability.
Description
Technical field
The present invention relates to the preparation method that a kind of acid-base value is low, process excellent rich nickel concentration gradient nickel cobalt manganese cathode material.
Background technology
Lithium ion battery has the advantages such as energy is high, voltage is high, cycle performance is good, memory-less effect, environmentally friendly, is widely used in the every field such as each electronic product, electric tool and military affairs.
Along with the development of lithium ion battery technology, the kind of anode material for lithium ion battery increases gradually, to meet the demand of inhomogeneity product.Mainly comprise at present: the anode material for lithium-ion batteries such as cobalt acid lithium, nickle cobalt lithium manganate, LiFePO 4, LiMn2O4.Cobalt acid lithium, owing to having higher production cost, and to have a negative impact to environment, and the petering out of cobalt ore resource, and limits the development of its lithium ion battery and positive electrode application.The defect of LiFePO 4 in cryogenic property and in energy density also have impact on its development space.The advantages such as LiMn2O4 has aboundresources, cost is low, pollution-free, fail safe is good, good rate capability be desirable power battery anode material, but its poor cycle performance and electrochemical stability greatly limit its industrialization.
Along with the development of anode material for lithium-ion batteries, nickle cobalt lithium manganate is considered to the product of most probable substituting cobalt acid lithium gradually, and no matter it is in capacity, cycle performance, fail safe, or in electrokinetic cell field, all has good application prospect.Current nickle cobalt lithium manganate carries out solid-phase sintering after generally adopting nickel, cobalt and manganese oxide to mix with lithium salts and prepares gained, its acid-base value is higher, pH value more than 11.6, size mixing at lithium ion battery, in the processing such as coating application poor, be unfavorable for the extensive use of this material in lithium ion battery.
Summary of the invention
The invention provides the preparation method that a kind of acid-base value is low, process excellent rich nickel concentration gradient nickel cobalt manganese cathode material, it not only has novel preparation process, acid-base value is low, and processing characteristics is excellent.
Present invention employs following technical scheme: a kind of acid-base value is low, the preparation method that processes excellent rich nickel concentration gradient nickel cobalt manganese cathode material, it comprises the following steps: first nickel Co-Mn compound, lithium compound are mixed in 1 ~ 1.1 ratio according to Li:M, by carrying out first sintering under the conditions such as uniform temperature, air-flow, time, again sintered product is passed through broken, screening, the middle product of preliminary obtained nickle cobalt lithium manganate; Then, by these middle product and organic substance Homogeneous phase mixing according to a certain percentage, under uniform temperature condition, carry out second time sintering by certain hour, then sintered product is carried out fragmentation, screening obtains the nickle cobalt lithium manganate that acid-base value is low, processing characteristics is excellent.
Acid-base value of the present invention molecular formula that is low, that process excellent rich nickel concentration gradient nickel cobalt manganese cathode material is Li
m(Ni
xco
ymn
z) O
2wherein 1<m<1.1,0<x<1,0<y<1,0<z<1,0.90<x+y+z<1.
Nickel in nickel Co-Mn compound of the present invention: cobalt: manganese ratio adopts the one in 3:3:3,4:2:4,5:2:3,6:2:2,7:1.5:1.5,8:1:1.
Nickel Co-Mn compound of the present invention adopts nickel, cobalt and manganese oxide, nickel cobalt manganese hydroxide, the mixture of one or more in the hopcalite of nickel, cobalt, manganese.
Lithium compound of the present invention adopts the mixture of one or more in lithium carbonate, lithium hydroxide, lithium acetate, lithium phosphate.
First sintering temperature of the present invention is: 750-950 DEG C, and air-flow is 1-5m
3/ h, the time is 8-20h; Second time sintering temperature is 200-600 DEG C, and air-flow is 1-5 m
3/ h, the time is 1-10h.
Organic substance of the present invention adopts the mixture of one or more in oxalic acid, citric acid, sucrose, acetic acid, graphite.
Middle product of the present invention and organic ratio according to mass ratio between 0%----1%.
The present invention has following beneficial effect: after have employed following technical scheme, the acid-base value that the present invention adopts is low, the preparation method that processes excellent rich nickel concentration gradient nickel cobalt manganese cathode material, there is novel preparation technology, employing organic substance adds, under the prerequisite reducing energy consumption, prepare acid-base value low, the nickle cobalt lithium manganate that processing characteristics is excellent.Preparation method provided by the invention is adopted to synthesize the nickle cobalt lithium manganate acid-base value of gained low, pH value controls below 11.2, and material fluidity is better, lithium ion battery processing and fabricating has excellent performance, between 2.75-4.25V charging/discharging voltage, the gram volume of electric discharge first of 0.2C charging and discharging currents reaches more than 170mAh/g.General solid-phase synthesis and preparation method's Performance comparision of the present invention, in table 1.
The general solid-phase synthesis of table 1 and preparation method's Performance comparision of the present invention
Accompanying drawing explanation
Fig. 1 is the first charge-discharge curve chart of nickle cobalt lithium manganate of the present invention.
Fig. 2 is the electronic scanning video picture figure of nickle cobalt lithium manganate of the present invention when 2.00KX and 10 μm of state.
Fig. 3 is the electronic scanning video picture figure of nickle cobalt lithium manganate of the present invention when 10.00KX and 1 μm of state.
Embodiment
Embodiment 1: by nickel cobalt manganese hydroxide (nickel: cobalt: manganese=5:2:3) and lithium carbonate according to Li:M=1.05 Homogeneous phase mixing, with the heating rate of 5 DEG C/min, at 850 DEG C of insulation 16h, gas flow optimized is at 3 m
3/ h, carries out first sintering, and cooling, ball milling, obtains Li after sieving
1.05(Ni
0.5co
0.2mn
0.3) O
2positive electrode.Then carry out first charge-discharge test, the curve chart of first charge-discharge is shown in Fig. 1, and nickle cobalt lithium manganate electronic scanning video picture figure is shown in Fig. 2 and Fig. 3.
Embodiment 2: by nickel cobalt manganese hydroxide (nickel: cobalt: manganese=5:2:3) and lithium carbonate according to Li:M=1.05 Homogeneous phase mixing, with the heating rate of 5 DEG C/min, at 850 DEG C of insulation 16h, gas flow optimized is at 3 m
3/ h, carries out first sintering, and cooling, ball milling, obtains Li after sieving
1.05(Ni
0.5co
0.2mn
0.3) O
2middle product.Then mixed according to 1:0.2% ratio uniform with oxalic acid by these middle product, with the heating rate of 3 DEG C/min, at 300 DEG C of insulation 6h, gas flow optimized is at 5 m
3/ h, carry out second time sintering, cooling, ball milling, obtains Li after sieving
1.05(Ni
0.5co
0.2mn
0.3) O
2positive electrode.Then carry out first charge-discharge test, the curve chart of first charge-discharge is shown in Fig. 1, and nickle cobalt lithium manganate electronic scanning video picture figure is shown in Fig. 2 and Fig. 3.
Embodiment 3: by nickel cobalt manganese hydroxide (nickel: cobalt: manganese=5:2:3) and lithium carbonate according to Li:M=1.05 Homogeneous phase mixing, with the heating rate of 5 DEG C/min, at 850 DEG C of insulation 16h, gas flow optimized is at 3 m
3/ h, carries out first sintering, and cooling, ball milling, obtains Li after sieving
1.05(Ni
0.5co
0.2mn
0.3) O
2middle product.Then mixed according to 1:0.6% ratio uniform with oxalic acid by these middle product, with the heating rate of 3 DEG C/min, at 300 DEG C of insulation 6h, gas flow optimized is at 5 m
3/ h, carry out second time sintering, cooling, ball milling, obtains Li after sieving
1.05(Ni
0.5co
0.2mn
0.3) O
2positive electrode.Then carry out first charge-discharge test, the curve chart of first charge-discharge is shown in Fig. 1, and nickle cobalt lithium manganate electronic scanning video picture figure is shown in Fig. 2 and Fig. 3.
Embodiment 4: by nickel cobalt manganese hydroxide (nickel: cobalt: manganese=5:2:3) and lithium carbonate according to Li:M=1.05 Homogeneous phase mixing, with the heating rate of 5 DEG C/min, at 850 DEG C of insulation 16h, gas flow optimized is at 3 m
3/ h, carries out first sintering, and cooling, ball milling, obtains Li after sieving
1.05(Ni
0.5co
0.2mn
0.3) O
2middle product.Then mixed according to 1:1% ratio uniform with oxalic acid by these middle product, with the heating rate of 3 DEG C/min, at 300 DEG C of insulation 6h, gas flow optimized is at 5 m
3/ h, carry out second time sintering, cooling, ball milling, obtains Li after sieving
1.05(Ni
0.5co
0.2mn
0.3) O
2positive electrode.Then carry out first charge-discharge test, the curve chart of first charge-discharge is shown in Fig. 1, and nickle cobalt lithium manganate electronic scanning video picture figure is shown in Fig. 2 and Fig. 3.
Embodiment 5: by nickel cobalt manganese hydroxide (nickel: cobalt: manganese=8:1:1) and lithium carbonate according to Li:M=1.05 Homogeneous phase mixing, with the heating rate of 5 DEG C/min, at 850 DEG C of insulation 16h, gas flow optimized is at 3 m
3/ h, carries out first sintering, and cooling, ball milling, obtains Li after sieving
1.05(Ni
0.5co
0.2mn
0.3) O
2positive electrode.Then carry out first charge-discharge test, the curve chart of first charge-discharge is shown in Fig. 1, and nickle cobalt lithium manganate electronic scanning video picture figure is shown in Fig. 2 and Fig. 3.
Embodiment 6: by nickel cobalt manganese hydroxide (nickel: cobalt: manganese=8:1:1) and lithium carbonate according to Li:M=1.05 Homogeneous phase mixing, with the heating rate of 5 DEG C/min, at 850 DEG C of insulation 16h, gas flow optimized is at 3 m
3/ h, carries out first sintering, and cooling, ball milling, obtains Li after sieving
1.05(Ni
0.5co
0.2mn
0.3) O
2middle product.Then mixed according to 1:0.6% ratio uniform with oxalic acid by these middle product, with the heating rate of 3 DEG C/min, at 300 DEG C of insulation 6h, gas flow optimized is at 5 m
3/ h, carry out second time sintering, cooling, ball milling, obtains Li after sieving
1.05(Ni
0.5co
0.2mn
0.3) O
2positive electrode.Then carry out first charge-discharge test, the curve chart of first charge-discharge is shown in Fig. 1, and nickle cobalt lithium manganate electronic scanning video picture figure is shown in Fig. 2 and Fig. 3.
Claims (8)
1. low, the preparation method that processes excellent rich nickel concentration gradient nickel cobalt manganese cathode material of an acid-base value, it is characterized in that it comprises the following steps: first nickel Co-Mn compound, lithium compound are mixed in 1 ~ 1.1 ratio according to Li:M, by carrying out first sintering under the conditions such as uniform temperature, air-flow, time, again sintered product is passed through broken, screening, the middle product of preliminary obtained nickle cobalt lithium manganate; Then, by these middle product and organic substance Homogeneous phase mixing according to a certain percentage, under uniform temperature condition, carry out second time sintering by certain hour, then sintered product is carried out fragmentation, screening obtains the nickle cobalt lithium manganate that acid-base value is low, processing characteristics is excellent.
2. low, the preparation method that processes excellent rich nickel concentration gradient nickel cobalt manganese cathode material of acid-base value according to claim 1, it is characterized in that described acid-base value is low, process the molecular formula of excellent rich nickel concentration gradient nickel cobalt manganese cathode material is Li
m(Ni
xco
ymn
z) O
2wherein 1<m<1.1,0<x<1,0<y<1,0<z<1,0.90<x+y+z<1.
3. low, the preparation method that processes excellent rich nickel concentration gradient nickel cobalt manganese cathode material of acid-base value according to claim 1, is characterized in that nickel in described nickel Co-Mn compound: cobalt: manganese ratio adopts 3:3:3,4:2:4,5:2:3, one in 6:2:2,7:1.5:1.5,8:1:1.
4. low, the preparation method that processes excellent rich nickel concentration gradient nickel cobalt manganese cathode material of acid-base value according to claim 1, it is characterized in that described nickel Co-Mn compound adopts nickel, cobalt and manganese oxide, nickel cobalt manganese hydroxide, the mixture of one or more in the hopcalite of nickel, cobalt, manganese.
5. low, the preparation method that processes excellent rich nickel concentration gradient nickel cobalt manganese cathode material of acid-base value according to claim 1, is characterized in that described lithium compound adopts the mixture of one or more in lithium carbonate, lithium hydroxide, lithium acetate, lithium phosphate.
6. low, the preparation method that processes excellent rich nickel concentration gradient nickel cobalt manganese cathode material of acid-base value according to claim 1, it is characterized in that described first sintering temperature is: 750-950 DEG C, air-flow is 1-5m
3/ h, the time is 8-20h; Second time sintering temperature is 200-600 DEG C, and air-flow is 1-5 m
3/ h, the time is 1-10h.
7. low, the preparation method that processes excellent rich nickel concentration gradient nickel cobalt manganese cathode material of acid-base value according to claim 1, is characterized in that described organic substance adopts the mixture of one or more in oxalic acid, citric acid, sucrose, acetic acid, graphite.
8. low, the preparation method that processes excellent rich nickel concentration gradient nickel cobalt manganese cathode material of acid-base value according to claim 1, is characterized in that described middle product and organic ratio according to mass ratio between 0%----1%.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108417828A (en) * | 2018-03-09 | 2018-08-17 | 无锡晶石新型能源股份有限公司 | A kind of preparation method of vapour phase coating modification nickel-cobalt lithium manganate cathode material |
CN108767255A (en) * | 2018-05-28 | 2018-11-06 | 格林美(无锡)能源材料有限公司 | A kind of high voltage high capacity type lithium cobaltate cathode material and preparation method thereof |
CN109950530A (en) * | 2017-12-21 | 2019-06-28 | 天津国安盟固利新材料科技股份有限公司 | With the nickelic tertiary cathode material and preparation method thereof for improving electrical property |
WO2020083068A1 (en) * | 2018-10-23 | 2020-04-30 | 宁德时代新能源科技股份有限公司 | Positive electrode sheet, manufacturing method therefor, lithium ion secondary battery, battery module, battery pack, and device |
CN111834629A (en) * | 2019-04-17 | 2020-10-27 | 北京新能源汽车股份有限公司 | Cathode material, preparation method thereof and lithium ion battery |
CN114242998A (en) * | 2021-11-27 | 2022-03-25 | 桂林理工大学 | Method for improving electrochemical performance of lithium-rich manganese-based oxide positive electrode material |
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CN103367705A (en) * | 2012-04-11 | 2013-10-23 | 河南科隆集团有限公司 | Double-layer cladded composite lithium ion positive material and preparation method thereof |
CN104201326A (en) * | 2014-07-29 | 2014-12-10 | 江西世纪长河新电源有限公司 | Pole piece of lithium ion secondary battery |
CN104393278A (en) * | 2014-10-29 | 2015-03-04 | 新乡市天力能源材料有限公司 | Preparation method of nickel cobalt lithium manganate ternary material |
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CN1838453A (en) * | 2005-03-23 | 2006-09-27 | 中南大学 | Lithium-nickel-cobalt-manganese-oxygen material for lithium ion battery positive electrode and preparation method thereof |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109950530A (en) * | 2017-12-21 | 2019-06-28 | 天津国安盟固利新材料科技股份有限公司 | With the nickelic tertiary cathode material and preparation method thereof for improving electrical property |
CN108417828A (en) * | 2018-03-09 | 2018-08-17 | 无锡晶石新型能源股份有限公司 | A kind of preparation method of vapour phase coating modification nickel-cobalt lithium manganate cathode material |
CN108767255A (en) * | 2018-05-28 | 2018-11-06 | 格林美(无锡)能源材料有限公司 | A kind of high voltage high capacity type lithium cobaltate cathode material and preparation method thereof |
WO2020083068A1 (en) * | 2018-10-23 | 2020-04-30 | 宁德时代新能源科技股份有限公司 | Positive electrode sheet, manufacturing method therefor, lithium ion secondary battery, battery module, battery pack, and device |
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CN111834629A (en) * | 2019-04-17 | 2020-10-27 | 北京新能源汽车股份有限公司 | Cathode material, preparation method thereof and lithium ion battery |
CN114242998A (en) * | 2021-11-27 | 2022-03-25 | 桂林理工大学 | Method for improving electrochemical performance of lithium-rich manganese-based oxide positive electrode material |
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