CN105129844A - Modified lithium battery lithium titanate negative electrode material preparation method - 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
- H01M4/485—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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- 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 present invention discloses a modified lithium titanate negative electrode material preparation method, which comprises: (1) preparing lithium titanate; (2) mixing the lithium titanate, a phenol formaldehyde resin and nanometer tin powder to obtain a uniform slurry; (3) carrying out spray drying to obtain lithium titanate powder; (4) uniformly mixing the powder obtained in the step (3) and asphalt powder; and (5) carrying out high temperature treatment on the powder obtained in the step (4) under the protection of an inert gas so as to obtain the modified lithium titanate negative electrode material, wherein the raw materials are used according to the weight part ratio. According to the present invention, the lithium titanate can be prepared through the solid-phase method, and the method has advantages of simple process, low manufacturing cost, short production cycle and the like.
Description
Technical field
The present invention relates to a kind of preparation method of lithium ion battery negative material, specifically
a kind of preparation method of modified lithium battery lithium titanate anode material.
Background technology
Be widely used in mobile telephone at present, it is large that lithium ion battery in the electronic products such as notebook computer has specific energy, specific power is high, self-discharge is little, good and the quickly-chargeable of cycle characteristics and efficiency is high, operating temperature range is wide, the advantages such as non-environmental-pollution, lithium ion battery used in the market, substantially be all be negative pole with carbon material, but carbon material is negative pole also has some to be difficult to the weakness overcome in actual applications, such as, react with electrolytic solution in discharge process formation surface passivated membrane first, cause the consumption of electrolytic solution and coulombic efficiency is lower first, the current potential of carbon dioxide process carbon electrode and the current potential of metallic lithium very close, when the battery is overcharged, the easy precipitating metal lithium of carbon electrodes, thus may short circuit be caused, and then cause battery explosion.In order to solve the safety problem of lithium cell, people have done large quantifier elimination.Spinel Li4Ti5O12 is as one
novelion secondary battery cathode material lithium, compared with other business-like material, advantages such as having good cycle, do not react with electrolytic solution, safety performance is high, charge and discharge platform is steady is one of the most excellent lithium ion battery negative material received much concern in recent years.
Compared with carbon negative electrode material, lithium titanate has a lot of advantages, wherein, the deintercalation of lithium ion in lithium titanate is reversible, and lithium ion is embedding or is deviating from the process of lithium titanate, its crystal formation does not change, volume change is less than 1%, therefore be called as " zero strain material ", can avoid causing structural damage due to the flexible back and forth of electrode materials in charge and discharge cycles, thus improve cycle performance and the work-ing life of electrode, decrease and increase with cycle index and bring specific storage significantly to decay, there is the cycle performance more excellent than Carbon anode; But, because lithium titanate is a kind of insulating material, its specific conductivity is low, thus cause the application in lithium electricity to there is the poor problem of high rate performance, lithium titanate material theoretical specific capacity is 175mAh/g simultaneously, and actual specific capacity is greater than 160mAh/g, has the shortcomings such as gram volume is lower, therefore, it is very necessary for carrying out modification for lithium titanate.
And tin is a kind of negative material being hopeful to replace carbon material most, this is because tin has the height gram specific storage up to 994mAh/g.People have carried out this kind of material and have studied widely in recent years, and make some progress.But in reversible lithium storage process, metallic tin volumetric expansion is remarkable, and cause cycle performance to be deteriorated, capacity is decayed rapidly, is therefore difficult to the requirement meeting scale operation.For this reason, by introducing the non-metallic elements such as carbon, carrying out stable metal tin in the mode of alloying or compound, slowing down the volumetric expansion of tin.Carbon can stop the direct contact between tin particles, suppresses the reunion of tin particles and grows up, playing the effect of buffer layer.
Research shows, the tin of small particle size or its alloy all improve a lot on capacity or on cycle performance, when the particle of alloy material reaches nano level, volumetric expansion in charge and discharge process can alleviate greatly, performance also can increase, but nano material has larger surface energy, easily reunites, efficiency for charge-discharge can be made on the contrary to reduce and accelerate the decay of capacity, thus counteract the advantage of nano particle.Another research tendency improving tin negative pole performance is exactly prepare matrix material or the alloy of tin and other material, and wherein, the tin/carbon composite prepared in conjunction with the stability of carbon material and the height ratio capacity characteristic of tin shows huge application prospect.
Summary of the invention
Technical problem solved by the invention is to provide
a kind of preparation method of modified lithium battery lithium titanate anode material, to solve the problem proposed in above-mentioned background technology.
In order to achieve the above object, the present invention realizes by the following technical solutions:
a kind of preparation method of modified lithium battery lithium titanate anode material, raw material, according to weight ratio, comprises following processing step:
(1) according to n(Li): the ratio of n(Ti)=0.84 ~ 0.87 takes lithium salts, titanium dioxide, with ball mill, both are carried out ball milling mixing 4 ~ 10 hours, then by the powder that mixes in atmosphere, 700 ~ 850 DEG C are warming up to the speed of 5 ~ 10 DEG C/min, be incubated 4 ~ 6h again, then naturally cool to room temperature, obtain lithium titanate anode material;
(2) by lithium titanate, resol, nanometer glass putty according to 100:5 ~ 20:5 ~ 10, solid content is the ratio of 20% ~ 40%, first take a certain amount of nanometer glass putty and put into spirit solvent, and ultrasonic disperse, then resol and lithium titanate is added respectively, the hexamethylenetetramine simultaneously adding amount of resin 3% ~ 5%, as resin curing agent, constantly stirs, and is mixed into even slurry;
(3) slurry then step (2) mixed, by spraying dry, obtains the lithium titanate powdery being coated with nanometer tin and phenolic resin blend;
(4) powder that step (3) obtains is mixed with the ratio of pitch powder according to 100:5 ~ 20; then by powder under the protection of rare gas element; 800 ~ 1000 DEG C are warming up to the speed of 1 ~ 5 DEG C/min; be incubated 1 ~ 5h again; Temperature fall, sieves after cooling and namely obtains heavy body graphite-doping lithium titanate anode material.
Further, described in step (1) for lithium salts be one in Lithium Acetate, Lithium Sulphate, lithium oxalate, Quilonum Retard, lithium hydroxide.
Further, the titanium dioxide described in step (1) is the one in anatase titanium dioxide or metal and stone type titanium dioxide.
Further, the particle diameter of the nanometer glass putty described in step (2) is not more than 100 nanometers.
Further, in step (3), the inlet temperature of spray-dired warm air is 150 DEG C ~ 200 DEG C, and temperature out is 40 DEG C ~ 70 DEG C.
Further, pitch powder described in step (4) comprises the powder prepared by one or more the mixture in coal-tar pitch, petroleum pitch, modified pitch, mesophase pitch, the condensation polycyclic polynuclear aromatic hydrocarbon that obtained by asphalt modifier, softening temperature is at 100--280 DEG C, and median size is 2 ~ 5 μm.
beneficial effect:
(1) advantages such as preparing lithium titanate by solid phase method, have that technique is simple, low cost of manufacture, cycle of making are short;
(2) by selecting nanometer glass putty, avoid the volume effect that glass putty produces when discharge and recharge because particle diameter is comparatively large, ensure that the stability in charge and discharge process of material, simultaneously and lithium titanate carry out compound coating process, solve the shortcomings such as single lithium titanate anode material capacity is on the low side;
(3) resin is in heat treatment process, and the small molecules in resin is too much, and the surface of coated rear material can be caused in overflow process to produce too much space, and the volume effect of buffering glass putty can be played in these spaces, ensures the stable of material system;
(4) by last pitch, secondary carries out to material coated, reduce the specific surface area of material, improve the first charge-discharge efficiency of material;
(5) by adding resin curing agent---hexamethylenetetramine in preceding step, allow resin in spray drying step by thermofixation, therefore can not melting because second time is heated, avoiding the later stage serious problem of luming after causing high temperature sintering because adding pitch again.
Embodiment
Reaching object to make technique means of the present invention, creation characteristic, workflow, using method and effect is easy to understand, below in conjunction with specific embodiment, setting forth the present invention further.
Embodiment 1
According to n(Li): n(Ti)=0.84, take 1000g Quilonum Retard and 2572g titanium dioxide, put into after ball mill carries out ball milling mixing 8h, by the powder that mixes in atmosphere, 800 DEG C are warming up to the speed of 10 DEG C/min, be incubated 4h again, then naturally cool to room temperature, obtain lithium titanate anode material; Above-mentioned lithium titanate powdery is taken 2000g, according to by lithium titanate, resol, nanometer glass putty according to 100:10:5, solid content is the ratio of 30%, the spirit solvent of 5366g put into by the nanometer glass putty taking 100g, and ultrasonic disperse, then add resol and the lithium titanate of 200g respectively, add the hexamethylenetetramine 6g of amount of resin 3% simultaneously, continuous stirring, is mixed into even slurry; Again slurry is carried out spraying dry; obtain the lithium titanate powdery being coated with nanometer tin and phenolic resin blend; after again powder being mixed according to the ratio of 100:5 with pitch powder; under the protection of rare gas element; 1000 DEG C are warming up to the speed of 5 DEG C/min; be incubated 3h again, Temperature fall, sieve after cooling and namely obtain graphite-doping lithium titanate anode material.
Embodiment 2
According to n(Li): n(Ti)=0.87, take 1000g Quilonum Retard and 2484g titanium dioxide, put into after ball mill carries out ball milling mixing 8h, by the powder that mixes in atmosphere, 800 DEG C are warming up to the speed of 10 DEG C/min, be incubated 4h again, then naturally cool to room temperature, obtain lithium titanate anode material; Above-mentioned lithium titanate powdery is taken 2000g, according to by lithium titanate, resol, nanometer glass putty according to 100:10:5, solid content is the ratio of 30%, the spirit solvent of 5366g put into by the nanometer glass putty taking 100g, and ultrasonic disperse, then add resol and the lithium titanate of 200g respectively, add the hexamethylenetetramine 6g of amount of resin 3% simultaneously, continuous stirring, is mixed into even slurry; Again slurry is carried out spraying dry; obtain the lithium titanate powdery being coated with nanometer tin and phenolic resin blend; after again powder being mixed according to the ratio of 100:5 with pitch powder; under the protection of rare gas element; 850 DEG C are warming up to the speed of 3 DEG C/min; be incubated 4h again, Temperature fall, sieve after cooling and namely obtain graphite-doping lithium titanate anode material.
Embodiment 3
According to n(Li): n(Ti)=0.87, take 1000g Quilonum Retard and 2161g titanium dioxide, put into after ball mill carries out ball milling mixing 8h, by the powder that mixes in atmosphere, 800 DEG C are warming up to the speed of 10 DEG C/min, be incubated 4h again, then naturally cool to room temperature, obtain lithium titanate anode material; Above-mentioned lithium titanate powdery is taken 2000g, according to by lithium titanate, resol, nanometer glass putty according to 100:15:5, solid content is the ratio of 30%, the spirit solvent of 5600g put into by the nanometer glass putty taking 100g, and ultrasonic disperse, then add resol and the lithium titanate of 300g respectively, add the hexamethylenetetramine 6g of amount of resin 3% simultaneously, continuous stirring, is mixed into even slurry; Again slurry is carried out spraying dry; obtain the lithium titanate powdery being coated with nanometer tin and phenolic resin blend; after again powder being mixed according to the ratio of 100:5 with pitch powder; under the protection of rare gas element; 900 DEG C are warming up to the speed of 5 DEG C/min; be incubated 3h again, Temperature fall, sieve after cooling and namely obtain graphite-doping lithium titanate anode material.
Comparative example 1
According to n(Li): n(Ti)=0.87, take 1000g Quilonum Retard and 2161g titanium dioxide, put into after ball mill carries out ball milling mixing 8h, by the powder that mixes in atmosphere, 800 DEG C are warming up to the speed of 10 DEG C/min, be incubated 4h again, then naturally cool to room temperature, obtain lithium titanate anode material.
Electrochemical property test
For the performance of modified lithium battery lithium titanate anode material prepared by inspection the inventive method, test by half-cell testing method, negative material with above embodiment and comparative example: acetylene black: PVDF(polyvinylidene difluoride (PVDF))=93:3:4(weight ratio), add appropriate NMP(N-methyl-2-pyrrolidone) furnishing pulpous state, coat on Copper Foil, within 8 hours, make negative plate through vacuum 110 DEG C of dryings; Be to electrode with metal lithium sheet, electrolytic solution is 1mol/LLiPF6/EC+DEC+DMC=1:1:1, and microporous polypropylene membrane is barrier film, is assembled into battery.Charging/discharging voltage is 1.0 ~ 2.5V, and charge-discharge velocity is 0.5C, and carry out testing to battery performance, test result is shown in
table 1.
table 1for the Performance comparision of negative material in different embodiment and comparative example
More than show and describe this
inventionultimate principle and principal character and this
inventionadvantage, the technician of the industry should understand, this
inventionbe not restricted to the described embodiments, what describe in above-described embodiment and specification sheets just illustrates this
inventionprinciple, do not departing from this
inventionunder the prerequisite of spirit and scope, this
inventionalso have various changes and modifications, these changes and improvements all fall into claimed basis
inventionin scope, this
inventionclaimed scope is defined by appending claims and equivalent thereof.
Claims (6)
1. a preparation method for modified lithium battery lithium titanate anode material, raw material, according to weight ratio, is characterized in that, comprises following processing step:
(1) according to n(Li): the ratio of n(Ti)=0.84 ~ 0.87 takes lithium salts, titanium dioxide, with ball mill, both are carried out ball milling mixing 4 ~ 10 hours, then by the powder that mixes in atmosphere, 700 ~ 850 DEG C are warming up to the speed of 5 ~ 10 DEG C/min, be incubated 4 ~ 6h again, then naturally cool to room temperature, obtain lithium titanate anode material;
(2) by lithium titanate, resol, nanometer glass putty according to 100:5 ~ 20:5 ~ 10, solid content is the ratio of 20% ~ 40%, first take a certain amount of nanometer glass putty and put into spirit solvent, and ultrasonic disperse, then resol and lithium titanate is added respectively, the hexamethylenetetramine simultaneously adding amount of resin 3% ~ 5%, as resin curing agent, constantly stirs, and is mixed into even slurry;
(3) slurry then step (2) mixed, by spraying dry, obtains the lithium titanate powdery being coated with nanometer tin and phenolic resin blend;
(4) powder that step (3) obtains is mixed with the ratio of pitch powder according to 100:5 ~ 20; then by powder under the protection of rare gas element; 800 ~ 1000 DEG C are warming up to the speed of 1 ~ 5 DEG C/min; be incubated 1 ~ 5h again; Temperature fall, sieves after cooling and namely obtains graphite-doping lithium titanate anode material.
2. the preparation method of a kind of modified lithium battery lithium titanate anode material according to claim 1, is characterized in that, described in step (1) for lithium salts be one in Lithium Acetate, Lithium Sulphate, lithium oxalate, Quilonum Retard, lithium hydroxide.
3. the preparation method of a kind of modified lithium battery lithium titanate anode material according to claim 1, is characterized in that, the titanium dioxide described in step (1) is the one in anatase titanium dioxide or metal and stone type titanium dioxide.
4. the preparation method of a kind of modified lithium battery lithium titanate anode material according to claim 1, is characterized in that, the particle diameter of the glass putty described in step (2) is not more than 100 nanometers.
5. the preparation method of a kind of modified lithium battery lithium titanate anode material according to claim 1, is characterized in that, in step (3), the inlet temperature of spray-dired warm air is 150 DEG C ~ 200 DEG C, and temperature out is 40 DEG C ~ 70 DEG C.
6. the preparation method of a kind of modified lithium battery lithium titanate anode material according to claim 1, it is characterized in that, pitch powder described in step (4) comprises the powder prepared by one or more the mixture in coal-tar pitch, petroleum pitch, modified pitch, mesophase pitch, the condensation polycyclic polynuclear aromatic hydrocarbon that obtained by asphalt modifier, softening temperature is at 100--280 DEG C, and median size is 2 ~ 5 μm.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105514391A (en) * | 2016-01-22 | 2016-04-20 | 山东大学 | Lithium-metasilicate-modified lithium titanate cathode material and preparing method and application thereof |
WO2017024719A1 (en) * | 2015-08-07 | 2017-02-16 | 田东 | Preparation method for high capacity lithium-ion battery negative electrode material |
WO2017024902A1 (en) * | 2015-08-07 | 2017-02-16 | 田东 | Preparation method for modified lithium-ion battery lithium titanate negative electrode material |
CN106935822A (en) * | 2017-03-17 | 2017-07-07 | 厦门理工学院 | Lithium ion battery and the method for realizing lithium ion battery quick charge |
CN107086301A (en) * | 2017-03-17 | 2017-08-22 | 厦门理工学院 | Modified Li4Ti5O12Negative material and preparation method, application |
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CN105129844A (en) * | 2015-08-07 | 2015-12-09 | 田东 | Modified lithium battery lithium titanate negative electrode material preparation method |
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CN101232094A (en) * | 2008-02-02 | 2008-07-30 | 广州市鹏辉电池有限公司 | Lithium ion battery negative pole active materials and battery |
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WO2017024719A1 (en) * | 2015-08-07 | 2017-02-16 | 田东 | Preparation method for high capacity lithium-ion battery negative electrode material |
WO2017024902A1 (en) * | 2015-08-07 | 2017-02-16 | 田东 | Preparation method for modified lithium-ion battery lithium titanate negative electrode material |
CN105514391A (en) * | 2016-01-22 | 2016-04-20 | 山东大学 | Lithium-metasilicate-modified lithium titanate cathode material and preparing method and application thereof |
CN106935822A (en) * | 2017-03-17 | 2017-07-07 | 厦门理工学院 | Lithium ion battery and the method for realizing lithium ion battery quick charge |
CN107086301A (en) * | 2017-03-17 | 2017-08-22 | 厦门理工学院 | Modified Li4Ti5O12Negative material and preparation method, application |
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