CN105036182A - Preparation method and application of high-purity lithium titanate negative pole material - Google Patents
Preparation method and application of high-purity lithium titanate negative pole material Download PDFInfo
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- CN105036182A CN105036182A CN201510328775.6A CN201510328775A CN105036182A CN 105036182 A CN105036182 A CN 105036182A CN 201510328775 A CN201510328775 A CN 201510328775A CN 105036182 A CN105036182 A CN 105036182A
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- lithium
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- lithium titanate
- titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
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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
- H01M6/00—Primary cells; Manufacture thereof
- H01M6/14—Cells with non-aqueous electrolyte
Abstract
The invention belongs to the field of lithium ion batteries, and particularly discloses a preparation method and application of a high-purity lithium titanate negative pole material. The preparation method uses titanium dioxide as the raw material and is characterized by comprising the following steps: uniformly mixing titanium dioxide, an adhesive and a conducting agent, and pressing into a sheet; assembling a battery by using the pressed sheet as a positive pole and a lithium piece as a negative pole, calculating the electric quantity required by lithium embedment according to the mass of the titanium dioxide and the lithium/titanium ratio, and discharging on a discharging apparatus; and after finishing discharging, taking out the lithium-embedded titanium dioxide, and carrying out high-temperature annealing treatment to obtain the lithium titanate product. The lithium titanate material is prepared by electrochemical treatment and high-temperature treatment, and has high purity. The assembled battery has the advantages of high specific capacity and excellent cycle performance.
Description
(1) technical field
The invention belongs to field of lithium ion battery, particularly a kind of preparation method of high purity lithium titanate anode material and application thereof.
(2) background technology
Lithium titanate attracts wide attention as lithium ion battery negative material, lithium titanate belongs to spinel structure, its structure can provide three-dimensional passage for the diffusion of lithium ion, lithium ion embedding and deviate from process, the unit cell parameters of lithium titanate and volume change are very little, are called as " zero strain " material.Extremely low volume change and sufficient lithium ion duct, make lithium titanate have extremely excellent cycle performance and high rate charge-discharge performance.
The common preparation method of current lithium titanate mainly contains solid reaction process, sol-gel method and hydro-thermal reaction method etc.Solid phase method technique is simple, but is often difficult to ensure that batch mixing is even, and long-time high-temperature calcination causes energy consumption higher, and lithium salts at high temperature volatilizees and causes product purity lower; Sol-gel method product purity is high, and granular size is controlled well, but uses the titanic acid ester of high cost to cause cost very high for raw material, is mainly used in laboratory study; Hydrothermal method product purity is high, and cost is low, but uses the system of High Temperature High Pressure, and equipment requirements is high, drops into larger.
Electrochemical method is simple, and clean energy, cost is low, is a kind of desirable synthetic method.Chinese patent CN103290426A discloses " a kind of preparation method of lithium titanate ", and employing titanium dioxide is negative electrode, and graphite is anode, and the alkali metal halide of melting is ionogen, and electrolysis under high temperature, obtains lithium titanate after annealing.This method can obtain purer lithium titanate, but production process needs high temperature fused state, and titanium lithium ratio is difficult to accurate control and hinders its industrial application.
(3) summary of the invention
The present invention in order to make up the deficiencies in the prior art, provide a kind ofly to be produced on a large scale, the preparation method of high purity lithium titanate anode material that battery performance is good and application thereof.
The present invention is achieved through the following technical solutions:
A preparation method for high purity lithium titanate anode material, take titanium dioxide as raw material, comprises the steps:
(1) after titanium dioxide, binding agent, conductive agent being mixed, tabletted;
(2) with the sheet of compacting in step (1) for positive pole, lithium sheet is that negative pole is assembled into battery, calculates the electricity that embedding lithium needs, electric discharge instrument discharges according to the quality of titanium dioxide and the ratio of lithium titanium;
(3), after discharge off, take out the titanium dioxide of embedding lithium, the high temperature anneal obtains lithium titanate product.
More excellent technical scheme of the present invention is:
Described titanium dioxide is nano particle, and granular size is 25nm; Macrobead adds the difficulty of Lithium-ion embeding, and embedding lithium may be caused uneven, and reduce purity, short grained cost is higher, operational difficulty, and the titanium dioxide granule of 25nm is commercial materials ripe at present, is the size of over-all properties optimum.
Described binding agent is polyvinylidene difluoride (PVDF) or tetrafluoroethylene, and conductive agent is one or more in acetylene black, SuperP, Ketjen black, KS-6, carbon nanotube and Graphene.Binding agent ensure that the intensity of compressing tablet, but can affect the electroconductibility of compressing tablet too much and increase cost, does not have cohesive action very little, and massfraction is 5 ~ 20% is optimum proportion.Conductive agent ensure that the electroconductibility of compressing tablet in discharge process, but can affect the difficulty of film-making too much and increase cost, acts on not obvious very little, and massfraction is 5 ~ 20% is optimum proportion; The quality proportioning of described titanium dioxide, binding agent, conductive agent is 60-90:5-20:5-20, and the blending means of three is ball milled or polishing.
In step (2), the mol ratio of lithium titanium is 4:5, then the electricity calculation formula required for certain mass titanium dioxide embedding corresponding amount lithium is:
mAh, wherein m is the grams of titanium dioxide, and M is the molecular weight of titanium dioxide, and the lithium-inserting amount discharging into now titanium dioxide is 0.8 just; Electric discharge instrument is the cell tester as far as possible selecting low range under cell tester or electrochemical operation stand in the condition of meet volume journey, and discharging current controls at below 0.1C, ensures that lithium ion can be embedded in titanium dioxide equably.
In step (3), described annealing temperature is 400-1000 DEG C, preferably 400-700 DEG C, further preferably 550 DEG C; Annealing time is 5-24h, and object is the oxygen utilized in air, and the restructuring of lithium titanyl forms lithium titanate.
Utilize the method for the invention to prepare preparation that products obtained therefrom is applied to CR2032 type button cell, it is characterized in that: lithium titanate is mixed by the mass ratio of 80:10:10 with acetylene black, polyvinylidene difluoride (PVDF), add 1-Methyl-2-Pyrrolidone and mixture is modulated into slurry, evenly be coated on aluminium foil, drying 6 hours at 80 DEG C, at 120 DEG C, vacuum-drying 12 hours obtained pole pieces, transfer to pole piece in glove box, with metallic lithium for be assembled into CR2032 type button cell to pole.
The present invention has prepared lithium titanate material by electrochemistry and pyroprocessing, and the lithium titanate purity of preparation is high, and the battery specific storage of assembling is high, and cycle performance is excellent.
The present invention accurately can control lithium titanium ratio, raw material is cheap, only need to use business-like nanometer titanic oxide material, just lithium titanate can be obtained by electrochemistry and pyroprocessing two steps, according to the quality of titanium dioxide, controlled discharge amount accurately can control the amount embedding lithium, ensure that the purity of lithium titanate.By battery prepared by the present invention, first discharge specific capacity reaches 160mAh/g, and under larger multiplying power, circulation volume is unattenuated.
(4) accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is further illustrated.
Fig. 1 is the XRD figure of lithium titanate material prepared by the embodiment of the present invention 1;
Fig. 2 is the high rate performance test pattern of the lithium ion battery that the lithium titanate material of the embodiment of the present invention 2 preparation is made;
Fig. 3 is the charge-discharge performance test pattern of the lithium ion battery that the lithium titanate material of the embodiment of the present invention 1 preparation is made;
Fig. 4 is the charge-discharge performance test pattern of the lithium ion battery that the lithium titanate material of the embodiment of the present invention 4 preparation is made.
(5) embodiment
Below by specific embodiments, the present invention is described in further detail, but these embodiments are only to illustrate, do not limit scope of the present invention.
Embodiment 1:
Take 1.6g titanium dioxide, 0.2gPVDF and 0.2g acetylene black, grind in mortar and fully mix half an hour, get 0.2g mixture and put into mould, suppress 1 minute under 20MPa pressure in flakes.Compressing tablet is done positive pole, selects CR2032 button cell shell, according to the der group packed battery of negative electrode casing, spring piece, pad, lithium sheet, barrier film, positive pole, anode cover, drip 5 lithium-ion battery electrolytes, prepare button cell with sealing machine sealing.Be put on cell tester by the button cell of preparation, 0.05C constant-current discharge is to the capacity of 42.88mAh.Take out the titanium dioxide after embedding lithium, in retort furnace, 550 DEG C of insulations obtain lithium titanate in 15 hours.
By the lithium titanate of gained and conductive agent acetylene black, binding agent PVDF in mass ratio 80:10:10 mix, add NMP(1-methyl-2 pyrrolidone) mixture is modulated into slurry, evenly be coated on aluminium foil, 80 DEG C of dryings 6 hours, 120 DEG C of vacuum-drying, 12 hours obtained pole pieces, pole piece is transferred in glove box, with metallic lithium for be assembled into CR2032 type button cell to pole.
By the battery of this case making, 0.2C multiplying power first discharge specific capacity reaches 175.4mAh/g, still has 155.5mAh/g after 2 times after 300 circulations of 1C multiplying power.
Embodiment 2:
Take 12g titanium dioxide, 4gPVDF, 2g acetylene black and 2gSuperP, put into 100ml ball grinder, ratio of grinding media to material is 3:1, grinds and fully mixes for 2 hours, get 0.2g mixture and put into mould, suppresses 1 minute in flakes under 20MPa pressure.Compressing tablet is done positive pole, selects CR2032 button cell shell, according to the der group packed battery of negative electrode casing, spring piece, pad, lithium sheet, barrier film, positive pole, anode cover, drip 5 lithium-ion battery electrolytes, prepare button cell with sealing machine sealing.Be put on cell tester by the button cell of preparation, 0.05C constant-current discharge is to the capacity of 32.16mAh.Take out the titanium dioxide after embedding lithium, in retort furnace, 750 DEG C of insulations obtain lithium titanate in 5 hours.
By the lithium titanate of gained and conductive agent acetylene black, binding agent PVDF in mass ratio 80:10:10 mix, add NMP and mixture is modulated into slurry, evenly be coated on aluminium foil, 80 DEG C of dryings 6 hours, 120 DEG C of vacuum-drying, 12 hours obtained pole pieces, pole piece is transferred in glove box, with metallic lithium for be assembled into CR2032 type button cell to pole.
By the battery of this case making, 0.2C multiplying power first discharge specific capacity reaches 178.7mAh/g, and after 2 times, 1C multiplying power, 3C multiplying power and 6C multiplying power circulate respectively after 20 times and still have 134.5mAh/g.
Embodiment 3:
Take 1.8g titanium dioxide, 0.1gPVDF and 0.1g carbon nanotube, grind in mortar and fully mix half an hour, get 0.2g mixture and put into mould, suppress 1 minute under 20MPa pressure in flakes.Compressing tablet is done positive pole, selects CR2032 button cell shell, according to the der group packed battery of negative electrode casing, spring piece, pad, lithium sheet, barrier film, positive pole, anode cover, drip 5 lithium-ion battery electrolytes, prepare button cell with sealing machine sealing.Be put on cell tester by the button cell of preparation, 0.05C constant-current discharge is to the capacity of 48.24mAh.Take out the titanium dioxide after embedding lithium, in retort furnace, 400 DEG C of insulations obtain lithium titanate in 24 hours.
By the lithium titanate of gained and conductive agent acetylene black, binding agent PVDF in mass ratio 80:10:10 mix, add NMP and mixture is modulated into slurry, evenly be coated on aluminium foil, 80 DEG C of dryings 6 hours, 120 DEG C of vacuum-drying, 12 hours obtained pole pieces, pole piece is transferred in glove box, with metallic lithium for be assembled into CR2032 type button cell to pole.
By the battery of this case making, 0.2C multiplying power first discharge specific capacity reaches 184.1mAh/g, and after 2 times, 1C multiplying power, 3C multiplying power and 6C multiplying power circulate respectively after 20 times and still have 84.1mAh/g.
Embodiment 4:
Take 1.6g titanium dioxide, 0.2gPTFE, 0.1g carbon nanotube and 0.1g Graphene, grind in mortar and fully mix half an hour, get 0.2g mixture and put into mould, suppress 1 minute under 20MPa pressure in flakes.Compressing tablet is done positive pole, selects CR2032 button cell shell, according to the der group packed battery of negative electrode casing, spring piece, pad, lithium sheet, barrier film, positive pole, anode cover, drip 5 lithium-ion battery electrolytes, prepare button cell with sealing machine sealing.Be put on cell tester by the button cell of preparation, 0.05C constant-current discharge is to the capacity of 42.88mAh.Take out the titanium dioxide after embedding lithium, in retort furnace, 1000 DEG C of insulations obtain lithium titanate in 5 hours.
By the lithium titanate of gained and conductive agent acetylene black, binding agent PVDF in mass ratio 80:10:10 mix, add NMP and mixture is modulated into slurry, evenly be coated on aluminium foil, 80 DEG C of dryings 6 hours, 120 DEG C of vacuum-drying, 12 hours obtained pole pieces, pole piece is transferred in glove box, with metallic lithium for be assembled into CR2032 type button cell to pole.
By the battery of this case making, 0.2C multiplying power first discharge specific capacity reaches 177.3mAh/g, still has 129.7mAh/g after 2 times after 100 circulations of 1C multiplying power.
Claims (10)
1. a preparation method for high purity lithium titanate anode material, is raw material with titanium dioxide, it is characterized by, after comprising the steps: that titanium dioxide, binding agent, conductive agent mix by (1), and tabletted; (2) with the sheet of compacting in step (1) for positive pole, lithium sheet is that negative pole is assembled into battery, calculates the electricity that embedding lithium needs, electric discharge instrument discharges according to the quality of titanium dioxide and the ratio of lithium titanium; (3), after discharge off, take out the titanium dioxide of embedding lithium, the high temperature anneal obtains lithium titanate product.
2. the preparation method of high purity lithium titanate anode material according to claim 1, is characterized in that: described titanium dioxide is nano particle, and granular size is 25nm.
3. the preparation method of high purity lithium titanate anode material according to claim 1, it is characterized in that: described binding agent is polyvinylidene difluoride (PVDF) or tetrafluoroethylene, conductive agent is one or more in acetylene black, SuperP, Ketjen black, KS-6, carbon nanotube and Graphene.
4. the preparation method of high purity lithium titanate anode material according to claim 1, it is characterized in that: in step (1), the quality proportioning of described titanium dioxide, binding agent, conductive agent is 60-90:5-20:5-20, and the blending means of three is ball milled or polishing.
5. the preparation method of high purity lithium titanate anode material according to claim 1, is characterized in that: in step (2), and the mol ratio of lithium titanium is 4:5, and electric discharge instrument is cell tester or electrochemical workstation, and discharging current is at below 0.1C.
6. the preparation method of high purity lithium titanate anode material according to claim 1, is characterized in that: in step (3), and described annealing temperature is 400-1000 DEG C, and annealing time is 5-24h.
7. the preparation method of high purity lithium titanate anode material according to claim 6, is characterized in that: described annealing temperature is 400-700 DEG C.
8. the preparation method of the high purity lithium titanate anode material according to claim 6 or 7, is characterized in that: described annealing temperature is 550 DEG C.
9. utilize method described in claim 1 to prepare preparation that products obtained therefrom is applied to CR2032 type button cell.
10. the preparation of CR2032 type button cell according to claim 9, it is characterized in that: lithium titanate is mixed by the mass ratio of 80:10:10 with acetylene black, polyvinylidene difluoride (PVDF), add 1-Methyl-2-Pyrrolidone and mixture is modulated into slurry, evenly be coated on aluminium foil, drying 6 hours at 80 DEG C, at 120 DEG C, vacuum-drying 12 hours obtained pole pieces, transfer to pole piece in glove box, with metallic lithium for be assembled into CR2032 type button cell to pole.
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| CN201510328775.6A CN105036182B (en) | 2015-06-15 | 2015-06-15 | A kind of preparation method and applications of high-purity lithium titanate anode material |
| PCT/CN2016/084173 WO2016202173A1 (en) | 2015-06-15 | 2016-05-31 | Method for preparing high-purity lithium titanate negative electrode material and use thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105514416A (en) * | 2016-01-25 | 2016-04-20 | 山东玉皇新能源科技有限公司 | Preparing method and application of high-purity lithium manganate anode material |
| CN105731549A (en) * | 2016-01-25 | 2016-07-06 | 山东玉皇新能源科技有限公司 | Preparation method and application of high-purity lithium cobalt oxide cathode material |
| WO2016202173A1 (en) * | 2015-06-15 | 2016-12-22 | 山东玉皇新能源科技有限公司 | Method for preparing high-purity lithium titanate negative electrode material and use thereof |
| WO2017005077A1 (en) * | 2015-07-09 | 2017-01-12 | 山东玉皇新能源科技有限公司 | Electrochemical preparation method for perovskite-type solid electrolyte lithium-lanthanum-titanium oxide compound |
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| CN105036182B (en) * | 2015-06-15 | 2017-03-08 | 山东玉皇新能源科技有限公司 | A kind of preparation method and applications of high-purity lithium titanate anode material |
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| CN105731549A (en) * | 2016-01-25 | 2016-07-06 | 山东玉皇新能源科技有限公司 | Preparation method and application of high-purity lithium cobalt oxide cathode material |
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