CN107845799A - A kind of preparation method of titaniferous anode material for lithium-ion batteries - Google Patents
A kind of preparation method of titaniferous anode material for lithium-ion batteries Download PDFInfo
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- CN107845799A CN107845799A CN201711082905.8A CN201711082905A CN107845799A CN 107845799 A CN107845799 A CN 107845799A CN 201711082905 A CN201711082905 A CN 201711082905A CN 107845799 A CN107845799 A CN 107845799A
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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
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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
- H01M4/50—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
- H01M4/36—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
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- 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
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Abstract
A kind of preparation method of titaniferous anode material for lithium-ion batteries, the chemical general formula of positive electrode prepared by this method is LiNi1‑x‑y‑ zTixMnyMzO2, wherein the one or more in 0.01≤x≤0.20,0≤y≤0.5,0≤z≤0.05, M Zr, Co, Al, Mg, Zn element；The stoichiometric proportion of each metal ion is adjusted as needed, the 24h of ball milling 8, crushed after drying away solvent, mixture powder is made and loads quartzy alms bowl, it is put into stove under conditions of oxygen atmosphere or drum air, sintering temperature is 600~900 DEG C, and sintering time is 10~24h, room temperature is naturally cooled to, is gone after impurity removing through crushing, sieving prepares target material.The present invention has the advantage that：Cost is cheap, and not only manufacture craft is simple for it, and free from admixture, specific capacity are higher, cyclical stability is good, has longer service life, is adapted to industrialization large-scale production.
Description
Technical field
The present invention relates to technical field of lithium ion, a kind of preparation of titaniferous anode material for lithium-ion batteries of specific design
Method.
Background technology
Lithium ion battery has energy density height, quickly-chargeable, self discharge as excellent performance and the battery of environmental protection
It is small, can the advantages that long-time storage, cycle performance be superior, memory-less effect.Lithium ion battery has been widely used in various
On portable electric appts, also by as the preferred power supply of electric automobile in the future.
Anode material for lithium-ion batteries mainly has cobalt acid lithium, nickel-cobalt-manganese ternary material, nickel cobalt aluminium ternary material, mangaic acid at present
The lithium ion anode materials such as lithium, olivine-type LiFePO4.The positive electrode better performances such as cobalt acid lithium and ternary material, but use cobalt
Element is more, because the toxicity of cobalt is larger, scarcity of resources so that cost is higher；LiMn2O4, olivine-type LiFePO4 cost compared with
It is low, but also capacity is relatively low.
In summary, existing lithium ion battery manufacturing field is because the problem of using material, exist production cost it is high or
The relatively low deficiency of person's capacity.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the cheap titaniferous anode material for lithium-ion batteries of cost, it
Not only manufacture craft is simple, and free from admixture, specific capacity are higher, cyclical stability is good, has longer service life, is adapted to work
Industryization mass produces.
The purpose of the present invention realized by such technical scheme, a kind of system of titaniferous anode material for lithium-ion batteries
Preparation Method, the chemical general formula of positive electrode prepared by this method is LiNi1-x-y-zTixMnyMzO2, wherein 0.01≤x≤0.20,0
≤ y≤0.5,0≤z≤0.05, the one or more in M Zr, Co, Al, Mg, Zn element；Preparation method comprises the following steps：
S1, nickel source, titanium source, manganese source, lithium source and M compound are stoichiometrically weighed, form mixed powder A, and will
Mixed powder A is put into ball grinder；
S2, according to ball milling pearl：Mixed powder A：Ball-milling medium=9:1:1 mass ratio, ball milling pearl and ball milling are added into ball grinder
Medium is simultaneously fully pulverized and mixed on ball mill, 8~24h of ball milling, is dried and is removed solvent, then is crushed, and mixed powder is made；
S3, mixture powder is loaded into quartzy alms bowl, be put into stove the high temperature sintering under conditions of oxygen atmosphere or drum air, sintering
Temperature is 600~900 DEG C, and sintering time is 10~24h；
S4, room temperature is naturally cooled to stove, removes impurity removing, LiNi is prepared through crushing, sieving1-x-y-zTixMnyMzO2Positive electrode.
Further, nickel source is nickel hydroxide, nickel protoxide, nickelous carbonate, nickel oxalate, at least one in nickel acetate in S1
Kind；Manganese source is at least one of manganese carbonate, electrolytic manganese dioxide, manganese acetate, manganese oxalate；Titanium source is titanium dioxide, metatitanic acid
At least one of.Lithium source is at least one of lithium carbonate, lithium hydroxide, lithium nitrate, lithium acetate.
Further, 200~400rpm of stir speed (S.S.) of slurry is formed in S2.
Further, the ball-milling medium in S2 is at least one of ethanol, sugar or resin.
Further, Ball-milling Time 16h.
Further, the speed that air is blasted in S4 is 0.1~10L/min.
Further, the speed that oxygen is blasted in S4 is 1.0L/min.
Further, 15h is sintered under the conditions of being 750 DEG C in sintering temperature in S4.
By adopting the above-described technical solution, the present invention has the advantage that：Cost is cheap, its not only manufacture craft letter
It is single, and free from admixture, specific capacity are higher, cyclical stability is good, have longer service life, are adapted to industrialization extensive raw
Production.
Brief description of the drawings
Fig. 1 is a kind of first 50 weeks schematic diagrames of circulation electric discharge of positive electrode prepared by the present invention.
Fig. 2 is a kind of the 20th week schematic diagram of charge-discharge test of positive electrode prepared by the present invention.
Fig. 3 is a kind of XRD diffraction schematic diagram of positive electrode prepared by the present invention.
Embodiment
Under the invention will be further described in conjunction with the accompanying drawings and embodiments.
Embodiment 1
S1, weigh 8.3083 grams of NiCO3, 0.9783 gram of TiO（OH）2With 2.2991 grams of MnCO3It is mixed to form mixture A；
S2, by 4.6156 grams of LiOHH under 200rpm speed stirring actions2O is slowly added to be mixed in A, forms mixing
Thing B；
S3, according to ball milling pearl：Mixture B：Ethanol=9:1:1 mass ratio is fully pulverized and mixed on ball mill, ball milling
8h, dry and remove solvent, then crush, mixture powder C is made；
S4, mixture powder C is loaded into quartzy alms bowl, is put into stove the high temperature sintering under conditions of oxygen atmosphere, sintering temperature is
900 DEG C, sintering time 10h；
S5, room temperature is naturally cooled to stove, removes impurity removing, LiNi is prepared through crushing, sieving0.75Ti0.1Mn0.15O2Positive electrode.
Embodiment 2
S1, weigh 9.0392 grams of Ni（OH）2With 0.1996 gram of TiO2It is mixed to form mixture A；
S2,4.6156 grams of LiOHH under 200rpm speed stirring actions2O is slowly added to be mixed in A, forms mixture
B；
S3, according to ball milling pearl：Mixture B：Ethanol=9:1:1 mass ratio is fully pulverized and mixed on ball mill, ball milling
24h, dry and remove solvent, then crush, mixture powder C is made；
S4, mixture powder C is loaded into quartzy alms bowl, be put into stove the high temperature under conditions of drum air speed is 0.1L/min and burn
Knot, sintering temperature are 600 DEG C, sintering time 24h；
S5, room temperature is naturally cooled to stove, removes impurity removing, LiNi is prepared through crushing, sieving0.975Ti0.025O2Positive electrode.
Embodiment 3
S1, weigh 8.7147 grams of Ni（OH）2, 0.2395 gram of TiO2With 0.2608 gram of MnO2It is mixed to form mixture A；
S2, by 4.0607 grams of Li under 200rpm rate actions2CO3It is slowly added to be mixed in A, forms mixture B；
S3, according to ball milling pearl：Mixture B：Ethanol=9:1:1 mass ratio is fully pulverized and mixed on ball mill, ball milling
16h, dry and remove solvent, then crush, mixture powder C is made；
S4, mixture powder C is loaded into quartzy alms bowl, be put into stove the high temperature under conditions of drum air speed is 1.0L/min and burn
Knot, sintering temperature are 750 DEG C, sintering time 15h；
S5, room temperature is naturally cooled to stove, removes impurity removing, LiNi is prepared through crushing, sieving0.94Ti0.03Mn0.03O2Positive electrode.
Embodiment 4
S1, weigh 14.9316 grams of Ni（CH3COO）2·4H2O, 1.5966 grams of TiO2, 4.9018 grams of Mn（CH3COO）2·4H2O is mixed
Conjunction forms mixture A；
S2, by 4.6156 grams of LiOHH of lithium carbonate under 200rpm speed stirring actions2O is slowly added to be mixed in A, shape
Resulting mixture B；
S3, according to ball milling pearl：Mixture B：Ethanol=9:1:1 mass ratio is fully pulverized and mixed on ball mill, ball milling
16h, dry and remove solvent, then crush, mixture powder C is made；
S4, mixture powder C is loaded into quartzy alms bowl, be put into stove the high temperature under conditions of drum air speed is 1.5L/min and burn
Knot, sintering temperature are 800 DEG C, sintering time 12h；
S5, room temperature is naturally cooled to stove, removes impurity removing, LiNi is prepared through crushing, sieving0.94Ti0.03Mn0.03O2Positive electrode.
Embodiment 5
S1, weigh 7.4168 grams of Ni（OH）2, 0.7983 gram of TiO2With 0.7825 gram of MnO2It is mixed to form mixture A；
S2, under stirring by 0.1682 gram of Nd2O3With 4.6156 grams of LiOH H2O is slowly added to be mixed in A, is formed mixed
Compound B；
S3, according to ball milling pearl：Mixture B：Ethanol=9:1:1 mass ratio is fully pulverized and mixed on ball mill, ball milling
12h, dry and remove solvent, then crush, mixture powder C is made；
S4, mixture powder C is loaded into quartzy alms bowl, is put into stove the high temperature sintering under conditions of drum air speed is 10L/min,
Sintering temperature is 850 DEG C, sintering time 10h；
S5, room temperature is naturally cooled to stove, removes impurity removing, LiNi0.8Ti is prepared through crushing, sieving0.1Mn0.09Nd0.01O2Positive pole
Material.
Battery performance test
LiFePO will be obtained in embodiment4/ C composite respectively with conductive agent acetylene black, binding agent PVDF, according to mass ratio 8:
1:1 mixing, is modulated into slurry by this mixture with 1-METHYLPYRROLIDONE, is coated uniformly on aluminium foil, dries, obtain at 100 DEG C
To working electrode.Electrode slice is cut into sheet-punching machine, then electrode slice is dried 8 in vacuum drying chamber at 110~120 DEG C
~24 hours, and be placed in argon gas atmosphere glove box.Making negative pole with lithium piece, 1mol/L LiPF6/EC+DMC makees electrolyte,
Using Cegard-2000 barrier films, be assembled into button cell, then in battery detecting instrument system, in the range of 2.5~4.3V with
0.5C charge-discharge tests, it is as follows to obtain result：
Specific discharge capacity is 150mAh/g in embodiment 1；
Specific discharge capacity is 134mAh/g in embodiment 2；
Specific discharge capacity is 142mAh/g in embodiment 3；
Specific discharge capacity is 129mAh/g in embodiment 4；
Specific discharge capacity is 138mAh/g in embodiment 5.
As shown in figure 1, be the present invention in method prepare a kind of cell positive material in the range of 2.5~4.3V,
Cycle-index and specific discharge capacity figure under 0.5C multiplying powers；It can be seen that the sample highest being prepared in the present invention is put
Electric specific capacity 152mAh/g, capability retention is 95% after 50 circulations.Thus, the sample that the present invention is prepared is shown well
Cyclical stability and higher specific discharge capacity.
A kind of as shown in Fig. 2 cell positive material that as in the present invention prepared by method 0.5C in the range of 2.5~4.3V
20th week charging and discharging curve figure under multiplying power；It can be seen that the material that is prepared of the present invention filling in second circulation
Discharge curve, 152mAh/g is reached, has shown that this material has higher charging and discharging capacity.
As shown in figure 3, it is a kind of a kind of XRD diffraction schematic diagram of cell positive material prepared by method in the present invention；From
It can be seen from the figure that, each diffraction maximum is all present and each peak is sharp, and free from admixture peak is present.
Thus, the present invention has the advantage that：Cost is cheap, and not only manufacture craft is simple for it, and free from admixture, specific capacity
It is higher, cyclical stability is good, there is longer service life, be adapted to industrialization large-scale production.
Claims (9)
1. a kind of preparation method of titaniferous anode material for lithium-ion batteries, it is characterised in that positive electrode prepared by this method
Chemical general formula is LiNi1-x-y-zTixMnyMzO2, wherein 0.01≤x≤0.20,0≤y≤0.5,0≤z≤0.05, M Zr, Co,
One or more in Al, Mg, Zn element；Preparation method comprises the following steps：
S1, nickel source, titanium source, manganese source, lithium source and M compound are stoichiometrically weighed, form mixed powder A, and will
Mixed powder A is put into ball grinder；
S2, according to ball milling pearl：Mixed powder A：Ball-milling medium=9:1:1 mass ratio, ball milling pearl and ball milling are added into ball grinder
Medium is simultaneously fully pulverized and mixed on ball mill, 8~24h of ball milling, is dried and is removed solvent, then is crushed, and mixed powder is made；
S3, mixture powder is loaded into quartzy alms bowl, be put into stove the high temperature sintering under conditions of oxygen atmosphere or drum air, sintering
Temperature is 600~900 DEG C, and sintering time is 10~24h；
S4, room temperature is naturally cooled to stove, removes impurity removing, LiNi is prepared through crushing, sieving1-x-y-zTixMnyMzO2Positive electrode.
2. the preparation method of titaniferous anode material for lithium-ion batteries according to claim 1, it is characterised in that nickel source in S1
For at least one of nickel hydroxide, nickel protoxide, nickelous carbonate, nickel oxalate, nickel acetate；Manganese source is manganese carbonate, electrolysis titanium dioxide
At least one of manganese, manganese acetate, manganese oxalate；Titanium source is at least one of titanium dioxide, metatitanic acid.
3. the preparation method of titaniferous anode material for lithium-ion batteries according to claim 1, it is characterised in that lithium source in S1
For at least one of lithium carbonate, lithium hydroxide, lithium nitrate, lithium acetate.
4. the preparation method of titaniferous anode material for lithium-ion batteries according to claim 1, it is characterised in that formed in S2
200~400rpm of stir speed (S.S.) of slurry.
5. the preparation method of titaniferous anode material for lithium-ion batteries according to claim 1, it is characterised in that the ball in S2
Grinding media is at least one of ethanol, sugar or resin.
6. the preparation method of titaniferous anode material for lithium-ion batteries according to claim 1, it is characterised in that Ball-milling Time
For 16h.
7. the preparation method of titaniferous anode material for lithium-ion batteries according to claim 1, it is characterised in that blasted in S3
The speed of air is 0.1~10L/min.
8. the preparation method for the titaniferous anode material for lithium-ion batteries stated according to claim 8, it is characterised in that oxygen is blasted in S3
The speed of gas is 1.0L/min.
9. the preparation method of titaniferous anode material for lithium-ion batteries according to claim 1, it is characterised in that burnt in S3
Junction temperature sinters 15h under the conditions of being 750 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109686965A (en) * | 2018-12-12 | 2019-04-26 | 无锡晶石新型能源股份有限公司 | A kind of wet process technique of manganese titanate lithium |
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Application publication date: 20180327 |