CN108123123A - A kind of preparation method of lithium ion battery trielement composite material - Google Patents
A kind of preparation method of lithium ion battery trielement composite material Download PDFInfo
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- CN108123123A CN108123123A CN201711377913.5A CN201711377913A CN108123123A CN 108123123 A CN108123123 A CN 108123123A CN 201711377913 A CN201711377913 A CN 201711377913A CN 108123123 A CN108123123 A CN 108123123A
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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
- 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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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
- 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
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of preparation method of lithium ion battery trielement composite material, including：(1) lithium oxalate, nickel hydroxide, cobalt carbonate, aluminium hydroxide and lanthana are weighed, adds in ball milling mixing after acetone, after vacuum drying, crushed material is added in chlorination zirconium solution, obtains the lithium nickel cobalt aluminum oxide of the rare earth doped elements La of zirconium cladded type；(2) lithium nickel cobalt aluminum oxide, cetyl trimethylammonium bromide, resorcinol and the acetaldehyde solution of the rare earth doped elements La of zirconium cladded type are added in water, add a small amount of saleratus, after reaction, drying, it is sintered in air atmosphere, obtains the lithium nickel cobalt aluminum oxide of the carbon modification rare earth doped elements La of zirconium cladded type.Lithium ion battery trielement composite material prepared by the present invention improves the high rate cyclic stability of material and high temperature circulation stability；When for lithium ion battery, there is higher electric conductivity and good cyclical stability.
Description
Technical field
The present invention relates to technical field of lithium-ion battery more particularly to a kind of lithium ion battery trielement composite materials
Preparation method.
Background technology
Lithium ion battery becomes the mainstream development direction of secondary cell with its outstanding performance, in new-energy automobile and big rule
Mould energy-storage system has huge growth potential, and positive electrode accounts for the 30%~40% of lithium ion manufacture cost, is to determine lithium
Ion battery safety, performance, cost and the critical material in service life
The positive electrode of the lithium rechargeable battery currently researched and developed mainly includes Layered Lithium cobalt there are many series
Oxide series, laminated Li-Ni oxide series, spinel lithium manganese oxide series and olivine-type LiFePO4 series.Institute
It states in positive electrode, LiCoO2Because with good chemical property, anode material is commercialized as lithium rechargeable battery
Material is widely used, but due to LiCoO2In Co belong to scarce resource, it is expensive, easily pollute the environment, and
LiCoO2It the shortcomings of unstable when voltage is higher than 4.3V, limits with LiCoO2Lithium rechargeable battery as positive electrode
Application on hybrid electrically and pure electric automobile；LiNiO2Stability it is poor, easily cause safety problem, easily occur cation
Mixing and generation non-stoichiometry structural compounds, and synthesis is more difficult；LiMn2O4Crystal form easily occurs during recycling
The dissolving of transformation, Jahn-Teller effects and manganese ion, causes with LiMn2O4Lithium rechargeable battery as positive electrode holds
Amount attenuation is very fast and high-temperature behavior is undesirable.The lithium-rich manganese-based trielement composite material Li-Mn-Ni-Co of stratiform have height ratio capacity, into
The advantages that this relatively low, good cycling stability and good security, and can effectively make up LiCoO2、LiNiO2And LiMn2O4Respectively
From deficiency.
Therefore layered lithium-rich manganese-based trielement composite material is developed into lithium ion secondary battery anode material field
The new ternary compound oxides nickel manganese cobalt acid lithium of research hotspot because cheap, the advantages that synthesis is easy, and energy density is high,
It is considered as most possible substitution commercialization at present LiCoO2Novel anode material and Study on Li-ion batteries now it is one big
Hot spot.But have a disadvantage in that it in high power charging-discharging, capacity attenuation is very fast, and high rate performance is bad, high temperature circulation
Poor performance.
The content of the invention
This present invention provides a kind of preparation method of lithium ion battery trielement composite material, is prepared just using this method
Pole material, under high power charging-discharging and high-temperature condition, still with good electrochemistry cycle performance.
To achieve the above object, the present invention uses following technical scheme：
The first aspect of the invention is to provide a kind of preparation method of lithium ion battery trielement composite material, including such as
Lower step：
(1) the lithium nickel cobalt aluminum oxide of the rare earth doped elements La of zirconium cladded type is prepared
Lithium oxalate, nickel hydroxide, cobalt carbonate, aluminium hydroxide and lanthana are weighed, is added in after mixing and accounts for mixture gross mass
The acetone of 5-10%, when ball milling mixing 2-3 is small, rotational speed of ball-mill 200-300r/min, then after 100-110 DEG C of vacuum drying
900-950 DEG C is warming up to the heating rate of 15-20 DEG C/min, 10-12h is kept the temperature, is crushed after cooling；
Zirconium chloride is soluble in water, it is 0.05-0.1 by the mass ratio of zirconium chloride and above-mentioned crushed material:1, by crushed material plus
Enter in chlorination zirconium solution, when 40-50 DEG C of stirring 2-3 is small, filters, wash, dry, then 500-600 DEG C of heat preservation 5-8h, obtains zirconium
The lithium nickel cobalt aluminum oxide of the rare earth doped elements La of cladded type；
(2) the lithium nickel cobalt aluminum oxide of the carbon modification rare earth doped elements La of zirconium cladded type
With molar ratio 1：10-15：2-4：3-5 adds in the lithium nickel cobalt alumina of the rare earth doped elements La of zirconium cladded type in water
Object, cetyl trimethylammonium bromide, resorcinol and acetaldehyde solution add a small amount of saleratus；
It is being stirred under the conditions of 90-95 DEG C and react 1-2h, it obtains to surface and is coated with the zirconium cladded type doping of phenolic resin
The lithium nickel cobalt aluminum oxide of rare-earth elements of lanthanum, through filtering, wash and dry be coated with phenolic resin zirconium cladded type doping it is dilute
The lithium nickel cobalt aluminum oxide of earth elements lanthanum；
It finally in tube furnace inert atmosphere, is sintered, is warming up to 5-10 DEG C/min heating rates in air atmosphere
When heat preservation 2-3 is small after 600-700 DEG C, 900-1000 DEG C then is warming up to the heating rate of 10-15 DEG C/min, keeps the temperature 4-5h,
400-600 DEG C of annealing 5-10h is finally down to the cooling rate of 15-20 DEG C/min, carbonized phenolic resin obtains carbon modification zirconium cladding
The lithium nickel cobalt aluminum oxide of the rare earth doped elements La of type.
Further, the preparation method of the lithium ion battery trielement composite material the step of in (1), the grass
Lithium in sour lithium, nickel hydroxide, cobalt carbonate, aluminium hydroxide and lanthana, nickel, cobalt, the molar ratio of aluminium and lanthanum are 1.05:0.5：0.4:
(0.05-0.1)：(0.005-0.01).
Further, the preparation method of the lithium ion battery trielement composite material the step of in (1), the powder
The drying temperature to mince after adding in the chlorination zirconium solution is 850-900 DEG C, then keeps the temperature 6h in 540-560 DEG C.
Further, the preparation method of the lithium ion battery trielement composite material the step of in (2), the carbon
The addition of potassium hydrogen phthalate is the 5-10% of the lithium nickel cobalt aluminum oxide dosage of the rare earth doped elements La of zirconium cladded type.
Further, the preparation method of the lithium ion battery trielement composite material the step of in (2), the burning
Knot technique is：When heat preservation 2-3 is small after being warming up to 600-700 DEG C with 5-10 DEG C/min heating rates, then with 10-15 DEG C/min's
Heating rate is warming up to 900-1000 DEG C, keeps the temperature 4-5h, is finally down to 400-600 DEG C with the cooling rate of 15-20 DEG C/min and moves back
Fiery 5-10h.
The second aspect of the present invention is to provide lithium ion battery trielement composite material prepared by a kind of the method.
The present invention compared with prior art, is had the following technical effect that using above-mentioned technical proposal：
Lithium ion battery trielement composite material prepared by the method for the present invention employs solid-phase sintering process, prepares doping
The lithium nickel cobalt alumina material of lanthanum, and in its surface clad zirconium, followed with improving the high rate cyclic stability of material and high temperature
Then ring stability modifies its surface using carbon again, improve its conductivity, therefore the composite material is for lithium ion battery
When, there is higher electric conductivity and good cyclical stability so that lithium ion battery has high specific capacity and longer
Service life.
Specific embodiment
The present invention is described in more detail below by specific embodiment, for a better understanding of the present invention,
But following embodiments are not intended to limit the scope of the invention.
The preparation of 1 lithium ion battery trielement composite material of embodiment
(1) by the molar ratio 1.05 of lithium, nickel, cobalt, aluminium and lanthanum:0.5：0.4:0.05：0.005 weighs lithium oxalate, hydroxide
Nickel, cobalt carbonate, aluminium hydroxide and lanthana add in the acetone for accounting for mixture gross mass 5%, when ball milling mixing 3 is small, ball after mixing
Mill rotating speed is 200r/min, is then warming up to 900 DEG C after 100 DEG C of vacuum drying with the heating rate of 15 DEG C/min, heat preservation
12h is crushed after cooling；
Zirconium chloride is soluble in water, it is 0.05 by the mass ratio of zirconium chloride and above-mentioned crushed material:1, crushed material is added in into chlorine
Change in zirconium solution, when 40 DEG C of stirrings 3 are small, filter, wash, dry, then 500 DEG C of heat preservation 8h, it is rare earth doped to obtain zirconium cladded type
The lithium nickel cobalt aluminum oxide of elements La；
(2) with molar ratio 1：10：2：3 in water add in the rare earth doped elements La of zirconium cladded type lithium nickel cobalt aluminum oxide,
Cetyl trimethylammonium bromide, resorcinol and acetaldehyde solution add a small amount of saleratus.
It is being stirred under the conditions of 90 DEG C and react 2h, it obtains to surface and is coated with the rare earth doped member of zirconium cladded type of phenolic resin
The lithium nickel cobalt aluminum oxide of plain lanthanum is coated with the rare earth doped element of zirconium cladded type of phenolic resin by filtering, washing and dry
The lithium nickel cobalt aluminum oxide of lanthanum.
It finally in tube furnace inert atmosphere, is sintered in air atmosphere, 600 DEG C is warming up to 5 DEG C/min heating rates
When heat preservation 3 is small afterwards, 900 DEG C then are warming up to the heating rate of 10 DEG C/min, keeps the temperature 5h, finally with the cooling speed of 15 DEG C/min
Degree is down to 600 DEG C of annealing 10h, and carbonized phenolic resin obtains the lithium nickel cobalt alumina that carbon modifies the rare earth doped elements La of zirconium cladded type
Object.
The preparation of 2 lithium ion battery trielement composite material of embodiment
(1) by the molar ratio 1.05 of lithium, nickel, cobalt, aluminium and lanthanum:0.5：0.4:0.1)：0.01 weighs lithium oxalate, hydroxide
Nickel, cobalt carbonate, aluminium hydroxide and lanthana add in the acetone for accounting for mixture gross mass 10% after mixing, when ball milling mixing 2 is small,
Rotational speed of ball-mill is 300r/min, is then warming up to 950 DEG C after 110 DEG C of vacuum drying with the heating rate of 20 DEG C/min, heat preservation
10h is crushed after cooling.
Zirconium chloride is soluble in water, it is 0.1 by the mass ratio of zirconium chloride and above-mentioned crushed material:1, crushed material is added in into chlorination
It in zirconium solution, when 50 DEG C of stirrings 2 are small, filters, washs, dry, then 5600 DEG C of heat preservation 5h, obtain the rare earth doped member of zirconium cladded type
The lithium nickel cobalt aluminum oxide of plain lanthanum.
(2) with molar ratio 1：15：4：5 in water add in the rare earth doped elements La of zirconium cladded type lithium nickel cobalt aluminum oxide,
Cetyl trimethylammonium bromide, resorcinol and acetaldehyde solution add a small amount of saleratus.
It is being stirred under the conditions of 95 DEG C and react 1h, it obtains to surface and is coated with the rare earth doped member of zirconium cladded type of phenolic resin
The lithium nickel cobalt aluminum oxide of plain lanthanum is coated with the rare earth doped element of zirconium cladded type of phenolic resin by filtering, washing and dry
The lithium nickel cobalt aluminum oxide of lanthanum.
It finally in tube furnace inert atmosphere, is sintered in air atmosphere, 700 DEG C is warming up to 10 DEG C/min heating rates
When heat preservation 2 is small afterwards, 1000 DEG C then are warming up to the heating rate of 15 DEG C/min, 4h is kept the temperature, finally with the cooling of 20 DEG C/min
Speed is down to 4000 DEG C of annealing 5h, and carbonized phenolic resin obtains the lithium nickel cobalt alumina that carbon modifies the rare earth doped elements La of zirconium cladded type
Compound.
Comparative example
The manganese acetate of the nickel acetate of 0.005mol, the cobalt acetate of 0.005mol and 0.02mol is dissolved in 100ml deionized waters
In, magnetic agitation 4h forms it into homogeneous mixed solution, wherein Ni at 30 DEG C2+:Co2+:Mn2+Substance amount ratio be 1:1:
4.Lithium hydroxide is dissolved in stirring and dissolving in deionized water and obtains the clear lithium hydroxide solutions of 60ml, wherein lithium hydroxide is dense
It spends for 1.25mol/L；Mixed solution is added dropwise to the speed of 3ml/min in lithium hydroxide solution and is mixed to get reaction solution, is used
The pH value that ammonium hydroxide adjusts reaction solution is 11.0, and places reaction liquid into 50 DEG C of water-baths and be stirred to react 3h with the speed of 120rmp,
4h is aged again, and suction filtration obtains sediment, cleaned 3 times with distilled water, the sediment after being cleaned；Sediment after cleaning is put
Enter in cold-trap, -90 DEG C are cooled to together with cold-trap, rate of temperature fall is 2 DEG C/min, after freezing 3h, by the sediment of freezing true
It is dried in vacuo under reciprocal of duty cycle≤10.0Pa for 24 hours, obtains precursor.Precursor is mixed with lithium hydroxide, wherein, Li:Ni:
Co:The amount ratio of the substance of Mn is 9:1:1:4, it is uniformly mixed with mortar grinder, obtains mixture, mixture is first with Muffle furnace
In 480 DEG C of pre-burning 8h, room temperature tabletting is cooled to, then 3h is sintered in 900 DEG C, it is lithium-rich manganese-based to obtain one kind of the present invention
Ternary composite cathode material.
Above-described embodiment 1, embodiment 2 and comparative example products therefrom and conductive agent acetylene black, binding agent PVDF is (poly- inclined
Vinyl fluoride) according to mass ratio 8:1:1 is uniformly mixed, this mixture is modulated into slurry with NMP (1-Methyl-2-Pyrrolidone),
It being evenly applied on aluminium foil, is put into baking oven, 80-120 DEG C of drying 1h, taking-up is washed into pole piece, when 85 DEG C of vacuum drying 12 are small, into
Row tabletting, when 85 DEG C of vacuum drying 12 are small, obtained experimental cell pole piece.
Using lithium piece as to electrode, electrolyte is EC (ethyl carbonate ester)+DMC (dimethyl carbonic acid of 1.5mol/L LiPF6
Ester) (volume ratio 1: 1) solution, membrane is celgard2400 films, and CR2025 types are assembled into the glove box full of argon gas atmosphere
Button cell, charge and discharge are 3.6V by voltage.Electric performance test is carried out in the case where test temperature is 45 DEG C, after tested the embodiment
For one and two material compared with the product of comparative example, specific capacity improves 37-42%, and service life improves 1.6-2 times.
Specific embodiments of the present invention are described in detail above, but it is intended only as example, it is of the invention and unlimited
It is formed on particular embodiments described above.To those skilled in the art, it is any to the equivalent modifications that carry out of the present invention and
It substitutes also all among scope of the invention.Therefore, the impartial conversion made without departing from the spirit and scope of the invention and
Modification, all should be contained within the scope of the invention.
Claims (6)
1. a kind of preparation method of lithium ion battery trielement composite material, which is characterized in that include the following steps：
(1) the lithium nickel cobalt aluminum oxide of the rare earth doped elements La of zirconium cladded type is prepared
Lithium oxalate, nickel hydroxide, cobalt carbonate, aluminium hydroxide and lanthana are weighed, is added in after mixing and accounts for mixture gross mass 5-
10% acetone, when ball milling mixing 2-3 is small, rotational speed of ball-mill 200-300r/min, then 100-110 DEG C vacuum drying after with
The heating rate of 15-20 DEG C/min is warming up to 900-950 DEG C, keeps the temperature 10-12h, is crushed after cooling；
Zirconium chloride is soluble in water, it is 0.05-0.1 by the mass ratio of zirconium chloride and above-mentioned crushed material:1, crushed material is added in into chlorine
Change in zirconium solution, when 40-50 DEG C of stirring 2-3 is small, filters, wash, dry, then 500-600 DEG C of heat preservation 5-8h, obtains zirconium cladding
The lithium nickel cobalt aluminum oxide of the rare earth doped elements La of type；
(2) the lithium nickel cobalt aluminum oxide of the carbon modification rare earth doped elements La of zirconium cladded type
With molar ratio 1：10-15：2-4：3-5 add in water the rare earth doped elements La of zirconium cladded type lithium nickel cobalt aluminum oxide,
Cetyl trimethylammonium bromide, resorcinol and acetaldehyde solution add a small amount of saleratus；
It is being stirred under the conditions of 90-95 DEG C and react 1-2h, obtain to surface be coated with phenolic resin zirconium cladded type it is rare earth doped
The lithium nickel cobalt aluminum oxide of elements La is coated with the rare earth doped member of zirconium cladded type of phenolic resin by filtering, washing and dry
The lithium nickel cobalt aluminum oxide of plain lanthanum；
It finally in tube furnace inert atmosphere, is sintered in air atmosphere, 600-700 is warming up to 5-10 DEG C/min heating rates
Kept the temperature after DEG C 2-3 it is small when, be then warming up to 900-1000 DEG C with the heating rate of 10-15 DEG C/min, keep the temperature 4-5h, finally with
The cooling rate of 15-20 DEG C/min is down to 400-600 DEG C of annealing 5-10h, and carbonized phenolic resin obtains carbon modification zirconium cladded type doping
The lithium nickel cobalt aluminum oxide of rare-earth elements of lanthanum.
2. the preparation method of lithium ion battery trielement composite material according to claim 1, which is characterized in that step
(1) in, lithium in the lithium oxalate, nickel hydroxide, cobalt carbonate, aluminium hydroxide and lanthana, nickel, cobalt, the molar ratio of aluminium and lanthanum are
1.05:0.5：0.4:(0.05-0.1)：(0.005-0.01).
3. the preparation method of lithium ion battery trielement composite material according to claim 1, which is characterized in that step
(1) in, the drying temperature after the crushed material addition chlorination zirconium solution is 850-900 DEG C, then in 540-560 DEG C of heat preservation
6h。
4. the preparation method of lithium ion battery trielement composite material according to claim 1, which is characterized in that step
(2) in, the addition of the saleratus is the 5- of the lithium nickel cobalt aluminum oxide dosage of the rare earth doped elements La of zirconium cladded type
10%.
5. the preparation method of lithium ion battery trielement composite material according to claim 1, which is characterized in that step
(2) in, the sintering process is：After being warming up to 600-700 DEG C with 5-10 DEG C/min heating rates keep the temperature 2-3 it is small when, then with
The heating rate of 10-15 DEG C/min is warming up to 900-1000 DEG C, keeps the temperature 4-5h, is finally dropped with the cooling rate of 15-20 DEG C/min
To 400-600 DEG C of annealing 5-10h.
6. a kind of lithium ion battery trielement composite material prepared by method as described in claim 1.
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