CN105036182B - A kind of preparation method and applications of high-purity lithium titanate anode material - Google Patents
A kind of preparation method and applications of high-purity lithium titanate anode material Download PDFInfo
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- CN105036182B CN105036182B CN201510328775.6A CN201510328775A CN105036182B CN 105036182 B CN105036182 B CN 105036182B CN 201510328775 A CN201510328775 A CN 201510328775A CN 105036182 B CN105036182 B CN 105036182B
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- C01G23/00—Compounds of titanium
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- 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
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Abstract
The invention belongs to field of lithium ion battery, particularly disclose a kind of preparation method and applications of high-purity lithium titanate anode material.This preparation method, with titanium dioxide as raw material, it is characterized by：After titanium dioxide, binding agent, conductive agent mix homogeneously, tabletted；With the piece of compacting as positive pole, lithium piece is assembled into battery for negative pole, and the ratio of the quality according to titanium dioxide and lithium titanium calculates the electricity that embedding lithium needs, and discharges on electric discharge instrument；After discharge off, take out the titanium dioxide of embedding lithium, the high temperature anneal obtains lithium titanate product.The present invention is prepared for lithium titanate material by electrochemistry and high-temperature process, and the lithium titanate purity of preparation is high, and the battery specific capacity of assembling is high, and cycle performance is excellent.
Description
（One）Technical field
The invention belongs to field of lithium ion battery, particularly to a kind of preparation method of high-purity lithium titanate anode material and
Its application.
（Two）Background technology
Lithium titanate attracts wide attention as lithium ion battery negative material, and lithium titanate belongs to spinel structure, its
Structure can provide three-dimensional passage for the diffusion of lithium ion, during the embedded of lithium ion and abjection, the structure cell of lithium titanate
Parameter and change in volume very little, are referred to as " zero strain " material.Extremely low change in volume and sufficient lithium ion duct are so that metatitanic acid
Lithium has extremely excellent cycle performance and high rate charge-discharge performance.
The common preparation method of lithium titanate mainly has solid reaction process, sol-gal process and hydro-thermal reaction method etc. at present.Gu
Phase method process is simple, but often it is difficult to ensure that batch mixing uniformly, and long-time high-temperature calcination leads to energy consumption higher, lithium salts is at high temperature
Volatilization causes product purity relatively low；Sol-gal process product purity is high, and granular size is controlled, but the titanate esters using high cost
Lead to cost very high for raw material, be mainly used in laboratory research；Hydro-thermal method product purity is high, low cost, but uses High Temperature High Pressure
System, equipment requirements are high, put into larger.
Electrochemical method is simple, clean energy, and low cost, is a kind of preferable synthetic method.Chinese patent CN103290426A
Disclose " a kind of preparation method of lithium titanate ", be negative electrode using titanium dioxide, graphite is anode, the alkali halide of melting
For electrolyte, it is electrolysed under high temperature, after annealing, obtains lithium titanate.The method can obtain purer lithium titanate, but production process needs
Want high temperature fused state, titanium lithium ratio is difficult to precise control and hinders its commercial Application.
（Three）Content of the invention
The present invention is in order to make up the deficiencies in the prior art, there is provided a kind of be produced on a large scale, height that battery performance is good
The preparation method and applications of purity lithium titanate anode material.
The present invention is achieved through the following technical solutions：
A kind of preparation method of high-purity lithium titanate anode material, with titanium dioxide as raw material, comprises the steps：
（1）After titanium dioxide, binding agent, conductive agent mix homogeneously, tabletted；
（2）With step（1）The piece of middle compacting is positive pole, and lithium piece is assembled into battery for negative pole, according to the quality of titanium dioxide
Calculate, with the ratio of lithium titanium, the electricity that embedding lithium needs, electric discharge instrument discharges；
（3）After discharge off, take out the titanium dioxide of embedding lithium, the high temperature anneal obtains lithium titanate product.
The more excellent technical scheme of the present invention is：
Described titanium dioxide is nano-particle, and granular size is 25nm；Bulky grain increased the difficulty of Lithium-ion embeding, can
Embedding lithium can be caused uneven, reduce purity, short grained relatively costly, operating difficultiess, the titanium dioxide granule of 25nm is current
Ripe commercial materials, are the optimum sizes of combination property.
Described binding agent is Kynoar or politef, and conductive agent is acetylene black, Super P, Ketjen black, KS-
6th, one or more of CNT and Graphene.Binding agent ensure that the intensity of tabletting, but can affect leading of tabletting too much
Electrically and increase cost, do not have cementation very little, mass fraction is optimal proportion for 5～20%.Conductive agent ensure that tabletting
Electric conductivity in discharge process, but the difficulty of film-making can be affected too much and increase cost, act on inconspicuous, mass fraction very little
It is optimal proportion for 5～20%；Described titanium dioxide, binding agent, the quality proportioning of conductive agent are 60-90:5-20:5-20, three
Mixed method be ball-milling method or polishing.
Step（2）In, the mol ratio of lithium titanium is 4:5, then the electricity required for the embedded corresponding amount lithium of certain mass titanium dioxide
Measuring computing formula is：MAh, wherein m are the grams of titanium dioxide, and M is titanium dioxide
Molecular weight, the lithium-inserting amount discharging into now titanium dioxide is exactly 0.8；Electric discharge instrument is cell tester or electrochemical operation
Standing in and meeting the cell tester as far as possible selecting lower range under conditions of range, discharge current controls in below 0.1C it is ensured that lithium
Ion can be uniformly embedded in titanium dioxide.
Step（3）In, described annealing temperature be 400-1000 DEG C, preferably 400-700 DEG C it is further preferred that
550℃；Annealing time is 5-24h it is therefore an objective to utilize the oxygen of in the air, and the restructuring of lithium titanyl forms lithium titanate.
Prepare the preparation that products obtained therefrom is applied to CR2032 type button cell using the method for the invention, its feature exists
In：Lithium titanate is pressed 80 with acetylene black, Kynoar:10:10 mass ratio mixing, addition 1-Methyl-2-Pyrrolidone will
Mixture is modulated into slurry, is coated uniformly on aluminium foil, is dried 6 hours at 80 DEG C, and vacuum drying at 120 DEG C is obtained for 12 hours
Pole piece, pole piece is transferred in glove box, is that pole is assembled into CR2032 type button cell with lithium metal.
The present invention is prepared for lithium titanate material by electrochemistry and high-temperature process, and the lithium titanate purity of preparation is high, assembling
Battery specific capacity is high, and cycle performance is excellent.
The present invention can be with precise control lithium titanium ratio, and raw material is cheaply it is only necessary to use business-like nanometer titanium dioxide titanium
Material, can be obtained by lithium titanate by electrochemistry and two steps of high-temperature process, according to the quality of titanium dioxide, controls discharge capacity
The amount of lithium can be embedded it is ensured that the purity of lithium titanate with precise control.By the battery of present invention preparation, first discharge specific capacity reaches
To 160 mAh/g, under larger multiplying power, circulation volume is unattenuated.
（Four）Brief description
The present invention is further illustrated below in conjunction with the accompanying drawings.
Fig. 1 is the XRD figure of the lithium titanate material of the embodiment of the present invention 1 preparation；
Fig. 2 is the high rate performance test chart of the lithium ion battery that lithium titanate material prepared by the embodiment of the present invention 2 is made；
Fig. 3 is that the charge-discharge performance of the lithium ion battery that lithium titanate material prepared by the embodiment of the present invention 1 is made is surveyed
Attempt；
Fig. 4 is that the charge-discharge performance of the lithium ion battery that lithium titanate material prepared by the embodiment of the present invention 4 is made is surveyed
Attempt.
（Five）Specific embodiment
Below by specific embodiments, the present invention is described in further detail, but these embodiments are only that citing
Illustrate, the scope of the present invention is not defined.
Embodiment 1：
Weigh 1.6g titanium dioxide, 0.2g PVDF and 0.2g acetylene black, in mortar, grinding half an hour is sufficiently mixed uniformly,
Take 0.2g mixture to put into mould, suppress 1 minute under 20MPa pressure in flakes.Tabletting is done positive pole, from CR2032 button cell
Shell, according to negative electrode casing, spring leaf, pad, lithium piece, barrier film, positive pole, anode cover order assembled battery, 5 lithium-ion electrics of Deca
Pond electrolyte, prepares button cell with sealing machine sealing.The button cell of preparation is put on cell tester, 0.05C constant current
It is discharged to the capacity of 42.88mAh.Take out the titanium dioxide after embedding lithium, 550 DEG C of insulations in Muffle furnace 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 mixing, add NMP
（1- methyl -2 ketopyrrolidine）Mixture is modulated into slurry, is coated uniformly on aluminium foil, 80 DEG C of dryings 6 hours, 120 DEG C of vacuum
12 hour prepared pole piece is dried, pole piece is transferred in glove box, is that pole is assembled into CR2032 type button cell with lithium metal.
By the battery of this case making, 0.2C multiplying power first discharge specific capacity has reached 175.4 mAh/g, 1C times after 2 times
Still 155.5 mAh/g are had after 300 circulations of rate.
Embodiment 2：
Weigh 12g titanium dioxide, 4g PVDF, 2g acetylene black and 2g Super P, put into 100ml ball grinder, ratio of grinding media to material is
3:1, grind and be sufficiently mixed within 2 hours uniformly, take 0.2g mixture to put into mould, suppress 1 minute under 20MPa pressure in flakes.To press
Piece does positive pole, from CR2032 button cell shell, according to negative electrode casing, spring leaf, pad, lithium piece, barrier film, positive pole, anode cover
Order assembled battery, 5 lithium-ion battery electrolytes of Deca, prepare button cell with sealing machine sealing.Button electricity by preparation
Pond is put on cell tester, the capacity of 0.05C constant-current discharge to 32.16mAh.Take out the titanium dioxide after embedding lithium, Muffle furnace
In 750 DEG C of insulations obtain lithium titanate within 5 hours.
By the lithium titanate of gained and conductive agent acetylene black, binding agent PVDF in mass ratio 80:10:10 mixing, addition NMP will
Mixture is modulated into slurry, is coated uniformly on aluminium foil, 80 DEG C of dryings 6 hours, 12 hours prepared pole pieces of 120 DEG C of vacuum drying,
Pole piece is transferred in glove box, is that pole is assembled into CR2032 type button cell with lithium metal.
By the battery of this case making, 0.2C multiplying power first discharge specific capacity has reached 178.7 mAh/g, 1C times after 2 times
Rate, 3C multiplying power and 6C multiplying power still have 134.5 mAh/g after circulating 20 times respectively.
Embodiment 3：
Weigh 1.8g titanium dioxide, 0.1g PVDF and 0.1g CNT, in mortar, grinding half an hour is sufficiently mixed all
Even, take 0.2g mixture to put into mould, suppress 1 minute under 20MPa pressure in flakes.Tabletting is done positive pole, from CR2032 button
Battery case, according to negative electrode casing, spring leaf, pad, lithium piece, barrier film, positive pole, anode cover order assembled battery, 5 lithiums of Deca from
Sub- battery electrolyte, prepares button cell with sealing machine sealing.The button cell of preparation is put on cell tester, 0.05C
Constant-current discharge to 48.24mAh capacity.Take out the titanium dioxide after embedding lithium, 400 DEG C of insulations in Muffle furnace obtain metatitanic acid in 24 hours
Lithium.
By the lithium titanate of gained and conductive agent acetylene black, binding agent PVDF in mass ratio 80:10:10 mixing, addition NMP will
Mixture is modulated into slurry, is coated uniformly on aluminium foil, 80 DEG C of dryings 6 hours, 12 hours prepared pole pieces of 120 DEG C of vacuum drying,
Pole piece is transferred in glove box, is that pole is assembled into CR2032 type button cell with lithium metal.
By the battery of this case making, 0.2C multiplying power first discharge specific capacity has reached 184.1 mAh/g, 1C times after 2 times
Rate, 3C multiplying power and 6C multiplying power still have 84.1 mAh/g after circulating 20 times respectively.
Embodiment 4：
Weigh 1.6g titanium dioxide, 0.2g PTFE, 0.1g CNT and 0.1g Graphene, grind half an hour in mortar
It is sufficiently mixed uniformly, takes 0.2g mixture to put into mould, suppress 1 minute under 20MPa pressure in flakes.Tabletting is done positive pole, selects
CR2032 button cell shell, according to negative electrode casing, spring leaf, pad, lithium piece, barrier film, positive pole, anode cover order assembled battery,
5 lithium-ion battery electrolytes of Deca, prepare button cell with sealing machine sealing.The button cell of preparation is put into battery testing
On instrument, the capacity of 0.05C constant-current discharge to 42.88mAh.Take out the titanium dioxide after embedding lithium, in Muffle furnace, 1000 DEG C of insulations 5 are little
When obtain lithium titanate.
By the lithium titanate of gained and conductive agent acetylene black, binding agent PVDF in mass ratio 80:10:10 mixing, addition NMP will
Mixture is modulated into slurry, is coated uniformly on aluminium foil, 80 DEG C of dryings 6 hours, 12 hours prepared pole pieces of 120 DEG C of vacuum drying,
Pole piece is transferred in glove box, is that pole is assembled into CR2032 type button cell with lithium metal.
By the battery of this case making, 0.2C multiplying power first discharge specific capacity has reached 177.3 mAh/g, 1C times after 2 times
Still 129.7 mAh/g are had after 100 circulations of rate.
Claims (7)
1. a kind of preparation method of high-purity lithium titanate anode material, with titanium dioxide as raw material, it is characterized by, walk including following
Suddenly：（1）Described titanium dioxide is nano-particle, and granular size is 25nm, by titanium dioxide, binding agent, conductive agent mix homogeneously
Afterwards, tabletted；（2）With step（1）The piece of middle compacting is positive pole, and lithium piece is assembled into battery for negative pole, according to titanium dioxide
The ratio of quality and lithium titanium calculates the electricity that embedding lithium needs, and discharges, discharge current is in below 0.1C on electric discharge instrument；（3）Put
After electricity finishes, take out the titanium dioxide of embedding lithium, the high temperature anneal obtains lithium titanate product.
2. high-purity lithium titanate anode material according to claim 1 preparation method it is characterised in that：Described binding agent
For Kynoar or politef, conductive agent is acetylene black, Super P, Ketjen black, KS-6, CNT and Graphene
One or more of.
3. high-purity lithium titanate anode material according to claim 1 preparation method it is characterised in that：Step（1）In,
Described titanium dioxide, binding agent, the quality proportioning of conductive agent are 60-90:5-20:5-20, the mixed method of three is polishing.
4. high-purity lithium titanate anode material according to claim 1 preparation method it is characterised in that：Step（2）In,
The mol ratio of lithium titanium is 4:5, electric discharge instrument is cell tester or electrochemical workstation.
5. high-purity lithium titanate anode material according to claim 1 preparation method it is characterised in that：Step（3）In,
Described annealing temperature is 400-1000 DEG C, and annealing time is 5-24h.
6. high-purity lithium titanate anode material according to claim 5 preparation method it is characterised in that：Described annealing temperature
Spend for 400-700 DEG C.
7. the high-purity lithium titanate anode material according to claim 5 or 6 preparation method it is characterised in that：Described move back
Fiery temperature is 550 DEG C.
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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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| 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 |
| CN105047989B (en) * | 2015-07-09 | 2017-07-11 | 山东玉皇新能源科技有限公司 | A kind of electrochemical preparation method of Ca-Ti ore type solid electrolyte lithium lanthanum titanium oxide |
| 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 |
| CN114142080B (en) * | 2021-11-25 | 2024-04-05 | 东莞市茂盛新能源科技有限公司 | Super-capacity graphene battery and preparation method thereof |
| CN114335455B (en) * | 2021-12-06 | 2023-11-10 | 电子科技大学长三角研究院(湖州) | A method for precise fluorination of soft carbon with adjustable crystallinity and research on primary battery performance |
| CN117735599B (en) * | 2022-09-14 | 2024-12-20 | 广东科信聚力新能源有限公司 | A lithium iron titanate positive electrode material and a preparation method thereof |
| CN115632129B (en) * | 2022-10-13 | 2024-09-10 | 三峡大学 | High-capacity lithium ion battery Al negative electrode and preparation method thereof |
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| CN101488584A (en) * | 2009-03-06 | 2009-07-22 | 清华大学 | Asymmetric lithium iron phosphate cell using lithium titanate as main active substance of negative pole |
| CN103915262B (en) * | 2013-01-04 | 2017-08-11 | 深圳清华大学研究院 | The method of the pre- embedding lithium of lithium-ion capacitor negative pole |
| 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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| EP1057783A2 (en) * | 1999-06-03 | 2000-12-06 | Titan Kogyo Kabushiki Kaisha | Lithium-Titanium composite oxides, processes for preparing them and uses thereof |
| EP2328213A1 (en) * | 2009-11-26 | 2011-06-01 | Nippon Chemical Industrial Company Limited | Method for manufacturing lithium titanate for lithium secondary battery active material |
| CN102820459A (en) * | 2012-07-20 | 2012-12-12 | 合肥国轩高科动力能源有限公司 | Preparation method for synthesizing high-specific-energy lithium titanate material from mesoporous titanium dioxide |
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| CN104091939A (en) * | 2014-06-30 | 2014-10-08 | 北京工业大学 | Hydrothermal synthesis preparation method for spherical Li4Ti5O12 |
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