CN104835957B - Preparation method of high-nickel ternary material used for lithium ion battery - Google Patents
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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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- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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
- H01M4/62—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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- 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
A preparation method of a high-nickel ternary material used for a lithium ion battery. The ternary material is Li(Ni<0.6>Co<0.2>Mn<0.2>)O<2>, of which gram volume is not less than 180 mAh/g and service life retention rate after 2000 circulations is not less than 80%. The preparation method includes following steps: (1) preparation of a precursor solution; and (2) mix-calcination. During the preparation process, because an organic solution can reduce particle aggregation, a complexing agent can control the appearance and the compatibility between a titanium dioxide enhancing material and electrolyte, the ternary material is high in the gram volume (not less than 180 mAh/g) and is good in the service life retention rate after 2000 circulations (not less than 80%). The ternary material is easy to control in appearance, is simple in process and is suitable for industrialized production.
Description
Technical field
The present invention relates to lithium ion anode material preparation field, prepare the nickelic ternary of lithium ion battery particularly to one kind
The preparation method of positive electrode.
Background technology
Positive electrode is the crucial composition material of lithium ion battery, is cost accounting the best part in lithium ion battery.
The lithium electricity positive electrode obtaining commercial applications at present mainly has cobalt acid lithium, LiMn2O4, lithium nickelate, nickle cobalt lithium manganate, iron phosphate
Lithium etc..As one of most widely used positive electrode, the market share was once up to more than 70% to cobalt acid lithium, but cobalt is a kind of
Rare resource, because of factors such as raw material supply, cost prices, the application of cobalt acid lithium faces increasingly stern challenge, exploitation and
High performance substitution material is applied to become common recognition in the industry.Nickel cobalt manganese (1:1:1,5:2:3,4:3:3) acid lithium ternary material
With the advantage of its higher energy density, high security and lower cost, start a large amount of on some middle-end notebook computers
Application.For the requirement to power vehicle endurance, nickel cobalt manganese (1:1:1,5:2:3,4:3:3) acid lithium ternary material quilt
The electrokinetic cell giant such as Japan and Korea S introduces and adopts nickel cobalt as anode constituents to improve energy density, the such as Toyota Motor of Japan
Manganese ternary material, has taken into account cost and energy density advantage, has produced in batches on lithium ion battery used for electric vehicle.Cause
This, cobalt nickel lithium manganate ternary material is to think to have one of positive electrode of application prospect most, and nickelic low cobalt low manganese (6:2:2
Or 8:1:1) sour lithium, its energy density is higher, and bulk density is bigger, has more application prospect in some fields.Such as patent (cn
103872314 a) disclose a kind of method for pre-oxidizing with nickelic tertiary cathode active substance presoma for lithium ion battery, and it is first
First will filter through co-precipitation and process nickelic polynary hydroxide precursor, carry out anodic oxygen afterwards by the way of DC electrolysis
Change and obtain oxyhydroxide presoma nixm1-xOoh, with being vacuum dried under 70 DEG C of temperature conditionss after pure water, obtains
Ni to pre-oxidationxm1-xOoh presoma nixm1-x(oh)2, the ternary material li(ni that finally prepares0.6co0.2mn0.2) o2, its
Specific capacity be 172.2mah/g, 50 times circulation conservation rate be 94.1%, although its capacity is improved, cycle performance and its
Imbibition liquid-keeping property deviation, limits it and extensively applies.
Content of the invention
Ternary material li (ni at present0.6co0.2mn0.2)o2The gram volume existing is low, cycle life is poor and its liquid is protected in imbibition
The deficiency that ability exists, it is an object of the invention to provide a kind of preparation side of nickelic ternary material used by lithium ion battery
Method.
The technical scheme is that and be accomplished by: nickelic ternary material used by a kind of lithium ion battery
Preparation method, described ternary material is li (ni0.6co0.2mn0.2)o2, gram volume >=180mah/g, 2000 times cycle life is protected
Holdup >=80%, comprises the following steps: 1) precursor solution preparation, 2) mixed calcining；It is characterized in that:
Prepared by presoma: by niso4·6h2o、coso4·7h2o、mncl2·4h2O joins for 6:2:2 ratio in molar ratio
Than, and add certain mass water-soluble carbochain organic solvent be configured in redistilled water 5% ~ 20% strength solution,
Ultrasonic disperse obtains mixed solution a；Simultaneously at a temperature of 30 ~ 80 DEG C, the naoh solution preparing 0.1mol/l is poured in four-necked bottle,
And add chelating agent, chelating agen and additive, wherein mol ratio: naoh: chelating agent: chelating agen: additive=(1 ~ 2): 1:1:(1
~ 2), obtain naoh mixed liquor b；Under uniform stirring, with constant flow pump, mixed solution a is added by naoh mixing with certain speed
In liquid b, Deca is further continued for uniform stirring 10 ~ 60 minutes after being fully completed, above procedure all completes under nitrogen protection, it
Afterwards the mother solution obtaining is carried out sucking filtration, washing, filter pressing, redrying, grinding are sieved, and finally prepare aspherical ni0.6co0.2mn0.2
(oh)2Presoma；
Described chelating agent is ammonium fluoride, sodium citrate, one of disodiumedetate (edta) or one kind with
On.
Described additive is nano-titanium oxide and activated carbon, and its molar ratio is 1:1.
Described chelating agen is nh3h2o.
Described organic solvent is one or more of soluble starch, Polyvinylpyrrolidone, Polyethylene Glycol.
2), baking mixed: by Lithium hydrate and ni0.6co0.2mn0.2(oh)2Example (1.01 ~ 1.10) in molar ratio: 1 mixing
Uniformly, mixture is put in alumina crucible, calcine in Muffle furnace: 1 ~ 10 DEG C/min of heating rate, two ranks of calcining point
Section, calcines (4 ~ 10) hour at 500 DEG C, spends calcining at constant temperature (12 ~ 24) hour at 800 DEG C, obtains ternary li
(ni0.6co0.2mn0.2)o2Material.
The present invention, 1) add a certain amount of carbochain organic additive during ultrasonic disperse, improve slurry viscosity, suppression
Raw material segregation in dry run, in high-temperature reaction process, organic additive burning liberated heat can directly feed reactant
Each position, make system each several part temperature Fast-Balance, prepare that pattern is homogeneous, the monocrystalline ternary material of rule, have simultaneously
In machine additive combustion process, volume expands, and suppresses intergranular reunion.2) and add chelating agent can improve material
Pattern and the tap density improving material, and improve the stability of precursor solution, the final chemical property improving material.
3) a certain proportion of nanometer titanium dioxide titanium additives are added, its cladding lithium battery material can suppress the oxidation activity on surface, reduces
Electrode and the interfacial reaction of electrolyte, thus improving the cyclical stability in lithium battery material charge and discharge process, improve battery material
Material chemical property, extends the life-span of lithium battery.Add a certain proportion of activated carbon additive simultaneously, material can be improved again
Imbibition liquid-keeping property.The ternary material of the present invention is li (ni0.6co0.2mn0.2)o2, gram volume >=180mah/g, 2000 circulations
Life-span conservation rate >=80%.Pattern is easily-controllable, process is simple the features such as, be suitable for industrialized production.
Brief description
Fig. 1 is the sem figure of the material that embodiment 1 is prepared.
Specific embodiment
Embodiment 1:
The preparation method of nickelic ternary material used by a kind of lithium ion battery, described ternary material is li
(ni0.6co0.2mn0.2)o2, gram volume >=180mah/g, 2000 cycle life conservation rate >=80%, comprise the following steps:
1st, precursor solution preparation: 15.78 grams of (0.06mol) niso will be weighed4·6h2O, 5.62 grams (0.02mol)
coso4·7h2O, 3.96 grams of (0.02mol) mncl2·4h2It is added to 5 grams of Polyvinylpyrrolidone and 70g bis- times after o powder
In distilled water, ultrasonic disperse obtains mixed solution a.Simultaneously at a temperature of 50 DEG C, bis- steamings of 8 grams of (0.2mol) naoh and 2000ml
Distilled water is configured to 0.1mol/lnaoh solution and pours in four-necked bottle, and add 25.6 grams of (0.1mol) sodium citrates, 3.5 grams
(0.1mol) ammonia, 4 grams of titanium oxides (0.05mol) and 0.6 gram of (0.05mol) activated carbon, are uniformly mixing to obtain naoh mixed liquor
b.Under uniform stirring, in the naoh mixed liquor b with the speed of 20ml/min, mixed solution a being added with constant flow pump, drip
It is further continued for uniform stirring after entirely terminating 20 minutes, above procedure all completes under nitrogen protection, the mother solution obtaining is carried out
Sucking filtration, washing, filter pressing, 80 DEG C of redryings, grindings are sieved, and finally prepare aspherical ni0.6co0.2mn0.2(oh)2Presoma.
2nd, weigh ni in 24.24 grams of (1.01mol) Lithium hydrates and above-mentioned steps0.6co0.2mn0.2(oh)29.2 gram
(1.0mol) mix homogeneously, puts into mixture in alumina crucible, calcines (5 DEG C/min of heating rate), forge in Muffle furnace
Burn in two stages, calcine 6 hours at 500 DEG C, spend calcining at constant temperature 16h at 800 DEG C, finally obtain ternary
lini0.6co0.2mn0.2o2Sample.
Embodiment 2:
The preparation method of nickelic ternary material used by a kind of lithium ion battery, comprises the following steps:
1st, precursor solution preparation: 15.78 grams of (0.06mol) niso will be weighed4·6h2O, 5.62 grams (0.02mol)
coso4·7h2O, 3.96 grams of (0.02mol) mncl2·4h2It is added to 2.5 grams of Polyethylene Glycol and bis- steamings of 240g after o powder
In distilled water, ultrasonic disperse obtains mixed solution a.Simultaneously at a temperature of 30 DEG C, 4 grams of (0.1mol) naoh and 1000ml second distillation
Water is configured to 0.1mol/lnaoh solution and pours in four-necked bottle, and add 3.7 grams of (0.1mol) ammonium fluorides, 3.5 grams
(0.1mol) ammonia, 8 grams of titanium oxides (0.1mol) and 1.2 grams of (0.1mol) activated carbons, are uniformly mixing to obtain naoh mixed liquor b.
Under uniform stirring, in the naoh mixed liquor b being added mixed solution a with the speed of 20ml/min with constant flow pump, Deca is complete
It is further continued for uniform stirring after end 20 minutes, above procedure all completes under nitrogen protection, the mother solution obtaining is taken out
Filter, washing, filter pressing, 80 DEG C of redryings, grindings are sieved, and finally prepare aspherical ni0.6co0.2mn0.2(oh)2Presoma.
2nd, weigh ni in 25.2 grams of (1.05mol) Lithium hydrates and above-mentioned steps0.6co0.2mn0.2(oh)29.2 gram
(1.0mol) mix homogeneously, puts into mixture in alumina crucible, calcines (1 DEG C/min of heating rate), forge in Muffle furnace
Burn in two stages, calcine 4 hours at 500 DEG C, spend calcining at constant temperature 10h at 800 DEG C, finally obtain ternary
lini0.6co0.2mn0.2o2Sample.
Embodiment 3:
1st, precursor solution preparation: 15.78 grams of (0.06mol) niso will be weighed4·6h2O, 5.62 grams (0.02mol)
coso4·7h2O, 3.96 grams of (0.02mol) mncl2·4h2It is added to 12 grams of soluble starches and bis- steamings of 37g after o powder
In distilled water, ultrasonic disperse obtains mixed solution a.Simultaneously at a temperature of 30 DEG C, 4 grams of (0.1mol) naoh and 1000ml second distillation
Water is configured to 0.1mol/lnaoh solution and pours in four-necked bottle, and add 3.7 grams of (0.1mol) ammonium fluorides, 3.5 grams
(0.1mol) ammonia, 8 grams of titanium oxides (0.1mol) and 1.2 grams of (0.1mol) activated carbons, are uniformly mixing to obtain naoh mixed liquor b.
Under uniform stirring, in the naoh mixed liquor b being added mixed solution a with the speed of 20ml/min with constant flow pump, Deca is complete
It is further continued for uniform stirring after end 20 minutes, above procedure all completes under nitrogen protection, the mother solution obtaining is taken out
Filter, washing, filter pressing, 80 DEG C of redryings, grindings are sieved, and finally prepare aspherical ni0.6co0.2mn0.2(oh)2Presoma.
2nd, weigh ni in 26.4 grams of (1.1mol) Lithium hydrates and above-mentioned steps0.6co0.2mn0.2(oh)29.2 gram
(1.0mol) mix homogeneously, puts into mixture in alumina crucible, calcines (1 DEG C/min of heating rate), forge in Muffle furnace
Burn in two stages, calcine 10 hours at 500 DEG C, spend calcining at constant temperature 24h at 800 DEG C, finally obtain ternary
lini0.6co0.2mn0.2o2Sample.
(1) surface sweeping Electronic Speculum test: as seen from Figure 1, the ternary material that embodiment 1 is prepared assumes spherical, surface light
Sliding, granule is homogeneous.
(2) detain electrical testing
In mass ratio 0.9: 0.05: 0.05 weighs the positive active material that 2.0000g embodiment 1 ~ 3 prepares respectively
lini0.6co0.2mn0.2o2Powder, 0.1111g conductive black, 0.1111gpvdf, mixing, add addition 2.5g organic molten
Agent nmp (n- methyl pyrrolidone), is sufficiently mixed uniformly.The thin film that thickness is 140 microns, 120 DEG C of vacuum are painted on aluminium foil
Dry 2h, break into the disk of 5mm using card punch, using tablet machine in 10mpa lower sheeting, 120 DEG C of vacuum heat-preserving 12h, weigh
Positive pole sheet weight.It is assembled into button cell in the glove box of argon protection, with metal lithium sheet as negative pole, electrolyte is volume ratio
1: 1 ec(ethylene carbonate), dmc(1,2- dimethyl carbonate) solvent, electrolyte lipf6, barrier film is
Celgard2400 microporous polyethylene film.The battery installing is tested on blue electric tester electrical property.In 3v-4.25v voltage
In the range of, with 0.2c constant current charge/discharge, test specific capacity, as shown in table 1, specific discharge capacity respectively reaches 184.1mah/
G, 183.6mah/g, 182.9mah/g.
Comparative example be the ternary material not being modified purchased with market as positive electrode, other same as described above.
Button electrical test results are as shown in Figure 1.
Table 1 embodiment and comparative example buckle electrical test results contrast
| The electric battery of button | a1 | a2 | a3 | Comparative example |
| Positive electrode | Embodiment 1 | Embodiment 2 | Embodiment 3 | Ternary material |
| Discharge capacity (mah/g) first | 184.1 | 183.6 | 182.9 | 165 |
| Efficiency (%) first | 91.5 | 90.9 | 90.2 | 88.2 |
As it can be seen from table 1 the button electricity battery being obtained using embodiment 1～3 gained tertiary cathode material, its discharge capacity
And efficiency is all apparently higher than comparative example.Test result indicate that, the positive electrode of the present invention can make battery have good electric discharge appearance
Amount and first efficiency.
(3) soft-package battery test
Respectively with embodiment 1, embodiment 2, the ternary material that embodiment 3 is prepared as positive electrode, with Delanium
For negative material, using lipf6/ ec+dec(volume ratio 1: 1) it is electrolyte, celgard 2400 film is barrier film, prepares 5ah
Soft-package battery c1, c2, c3, and test the cycle performance of its soft-package battery；
Battery as a comparison: unmodified ternary material is purchased using on market as positive electrode, Delanium is negative pole
Material, using lipf6/ ec+dec(volume ratio 1: 1) it is electrolyte, celgard 2400 film is barrier film, prepares 5ah Soft Roll electricity
Pond d；And with multiplying power as 0.5c/0.5c, under conditions of voltage is 2.7 ~ 4.2v, test the cycle performance of its battery.Refer to table 2.
The cycle performance comparison sheet of table 2, embodiment and comparative example
| Embodiment | Initial capacity (ah) | Capacity (ah) after 500 times | Capacity (ah) after 1000 times | Capacity (ah) after 1500 times | Capacity (ah) after 2000 times |
| Embodiment 1 | 5.24 | 4.95 | 4.85 | 4.78 | 4.75 |
| Embodiment 2 | 5.27 | 4.99 | 4.88 | 4.79 | 4.70 |
| Embodiment 3 | 5.26 | 4.92 | 4.85 | 4.77 | 4.70 |
| Comparative example | 5.21 | 4.71 | 4.64 | 4.52 | 4.38 |
| Embodiment | Initial capacity conservation rate (%) | 500 conservation rates (%) of circulation | Conservation rate (%) after circulating 1000 times | Conservation rate (%) after circulating 1500 times | 2000 conservation rates (%) of circulation |
| Embodiment 1 | 100 | 94.62 | 92.58 | 91.40 | 90.69 |
| Embodiment 2 | 100 | 94.78 | 92.71 | 91.02 | 89.26 |
| Embodiment 3 | 100 | 93.39 | 92.29 | 90.63 | 89.46 |
| Comparative example | 100 | 91.55 | 89.14 | 86.82 | 84.42 |
As can be seen from Table 2, the cycle performance of the nickelic ternary material prepared using the present invention is better than comparative example, and it is former
Because being likely due to add a small amount of nanometer titanium dioxide titanium additives, cladding lithium battery material surface can suppress the oxidation on surface to live
Property, reduce the interfacial reaction of electrode and electrolyte, thus improving the cyclical stability in lithium battery material charge and discharge process.
Claims (1)
1. the preparation method of nickelic ternary material used by a kind of lithium ion battery, comprises the following steps: 1) precursor solution preparation,
2) mixed calcining；It is characterized in that:
1), presoma preparation: by niso4·6h2o、coso4·7h2o、mncl2·4h2O joins for 6:2:2 ratio in molar ratio
Than, and add certain mass water-soluble carbochain organic solvent be configured in redistilled water 5% ~ 20% strength solution,
Ultrasonic disperse obtains mixed solution a；Simultaneously at a temperature of 30 ~ 80 DEG C, the naoh solution preparing 0.1mol/l is poured in four-necked bottle,
And add chelating agent, chelating agen and additive, wherein mol ratio: naoh: chelating agent: chelating agen: additive=1 ~ 2:1:1:1 ~ 2,
Obtain naoh mixed liquor b；Under uniform stirring, with constant flow pump, mixed solution a is added by naoh mixed liquor b with certain speed
In, Deca is further continued for uniform stirring 10 ~ 60 minutes after being fully completed, above procedure all completes under nitrogen protection, afterwards
The mother solution obtaining is carried out sucking filtration, washing, filter pressing, redrying, grinding are sieved, and finally prepare aspherical ni0.6co0.2mn0.2
(oh)2Presoma；
Described chelating agent be one of ammonium fluoride, sodium citrate, disodiumedetate (edta) or more than one；
Described additive is nano-titanium oxide and activated carbon, and its molar ratio is 1:1；Described chelating agent is ammonium fluoride, citric acid
One of sodium, disodiumedetate (edta) or more than one；Described chelating agen is nh3h2o；Described is organic molten
Agent is one or more of soluble starch, Polyvinylpyrrolidone, Polyethylene Glycol；
2), mixed calcining: by Lithium hydrate and ni0.6co0.2mn0.2(oh)2Example 1.01 ~ 1.10:1 mix homogeneously in molar ratio,
Mixture is put in alumina crucible, in Muffle furnace calcine: 1 ~ 10 DEG C/min of heating rate, calcining in two stages,
Calcine 4 ~ 10 hours for 500 DEG C, spend calcining at constant temperature 12 ~ 24 hours at 800 DEG C, obtain ternary li (ni0.6co0.2mn0.2)o2Material.
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| CN106058238A (en) * | 2016-07-25 | 2016-10-26 | 四川省有色冶金研究院有限公司 | Modified spherical nickel cobalt lithium manganate NCM622 anode material and preparation method thereof |
| CN106532006A (en) * | 2016-12-16 | 2017-03-22 | 无锡晶石新型能源有限公司 | Preparation method of cobaltous oxide coated ternary anode material |
| CN107978751B (en) * | 2017-11-30 | 2020-07-03 | 宁波容百新能源科技股份有限公司 | Ternary positive electrode material with high electrochemical activity and preparation method thereof |
| CN109461925B (en) * | 2018-06-29 | 2022-01-25 | 北京当升材料科技股份有限公司 | Single crystal nickel cobalt lithium manganate positive electrode material, precursor and preparation method thereof |
| CN109841827A (en) * | 2019-01-22 | 2019-06-04 | 上海应用技术大学 | A kind of tertiary cathode material and preparation method thereof that lithium ion battery vanadium replaces |
| CN113998744A (en) * | 2021-10-29 | 2022-02-01 | 西南交通大学 | High-capacity and high-multiplying-power LiNi0.6Co0.2Mn0.2O2Positive electrode material, preparation method and application |
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