CN105529449A - Lithium titanate electrode material and preparation method thereof - Google Patents
Lithium titanate electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a lithium titanate electrode material and a preparation method thereof. The preparation method of the lithium titanate electrode material comprises the following steps: (1) mixing N-methylpyrrolidone and polyvinylpyrrolidone, and then adding a carbon nanotube and graphene for stirring to obtain slurry A; (2) feeding the slurry A to a grinding machine, adding zirconium oxide particles for grinding at the rotating speed of 150-250r/min for 60-300 minutes, and adding lithium titanate to the ground slurry A for mixing and stirring to obtain slurry B; and (3) carrying out drying treatment on the slurry B to obtain the lithium titanate electrode material. Compared with the prior art, according to the lithium titanate electrode material, the battery capacity is improved by 1%-3%; the discharge rate is improved by 1%-2%; rapid charging is achieved; and meanwhile, the heating problem in the high-rate charge-discharge process of a battery can be solved.
Description
Technical field
The present invention relates to field of lithium ion battery, particularly relate to a kind of lithium titanate electrode material and preparation method thereof.
Background technology
Along with electric automobile, the greatly developing of energy storage industry, the research and development of the lithium ion battery of Large Copacity, long-life, high safety, quick charge receive vast concern.
The lithium titanate of spinel structure is called as " zero strain " material, and the advantages such as its fail safe is high, charge-discharge performance good, cycle performance is excellent, charging/discharging voltage platform stable, as cathode material of lithium-ion power battery, have good development prospect.But, the native electronic conductive capability of lithium titanate material and ion conductivity on the low side, therefore when high current charge-discharge, capacitance fall-off is fast, and high rate performance is poor, constrains it greatly as the application of high magnification negative material in lithium-ion-power cell.
At present, lithium titanate and the conductive agent (as Graphene, super conductive black) with excellent conductive capability mainly carry out composite mixedly preparing electrode slurry, to make up the above-mentioned defect that lithium titanate material exists by prior art.But be subject to the restriction of its preparation and stirring means, Graphene is difficult to be uniformly dispersed in the slurry, the performance such as battery capacity, discharge-rate of obtained electrode is all undesirable, and mostly adopts organic solvent to disperse, and easily causes environmental pollution when removal of solvents.
Summary of the invention
Based on this, the object of this invention is to provide a kind of preparation method of lithium titanate electrode material.
A preparation method for lithium titanate electrode material, comprises the steps:
(1) Graphene, carbon nano-tube stirring is added by after 1-METHYLPYRROLIDONE, polyvinylpyrrolidone mixing, the mass concentration controlling Graphene is 2% ~ 3%, the mass concentration of carbon nano-tube is 1% ~ 3%, and the mass concentration of polyvinylpyrrolidone is 3% ~ 5%, obtains slurry A;
(2) described slurry A is dropped into grinder and adds zirconia particles grind, rotating speed 150 ~ 250r/min, grinding 60 ~ 300min, then add lithium titanate in the slurry A after grinding and carry out mix and blend, the weight ratio controlling the slurry A after grinding and lithium titanate is (5.5:4.5) ~ (6:4), obtains slurry B;
(3), after described slurry B being carried out drying process, described lithium titanate electrode material is obtained.
Wherein in an embodiment, described in step (3), the technological parameter of dry process is: first described slurry B input spray dryer is carried out high temperature 300 ~ 400 DEG C of spraying dry and obtain coated lithium titanate material presoma; Again described coated lithium titanate material presoma is dropped into high temperature kiln and carry out high temperature 600 ~ 800 DEG C calcining 10-15h under nitrogen protection.
Wherein in an embodiment, the technological parameter stirred described in step (1) is: adopt double planetary mixer, and revolution linear velocity 5 ~ 15m/s, rotation wire speed 15 ~ 25m/s, stirs 30 ~ 60min.
Wherein in an embodiment, described in step (2), the technological parameter of mix and blend is: adopt double planetary mixer, and revolution linear velocity 5 ~ 15m/s, rotation wire speed 15 ~ 25m/s, stirs 60 ~ 150min.
Wherein in an embodiment, described in step (2), the diameter of zirconia particles is 0.5 ~ 1mm.
Wherein in an embodiment, after dry process described in step (3), also comprise cooling step: under the lithium titanate material after described drying process is placed in low humidity 0.5 ~ 1%RH environment, be cooled to room temperature.
Another object of the present invention is to provide a kind of lithium titanate electrode material.
Concrete technical scheme is as follows:
The lithium titanate electrode material that above-mentioned preparation method prepares.
Another object of the present invention is to provide a kind of lithium titanate electrode slurry.
Concrete technical scheme is as follows:
A kind of lithium titanate electrode slurry, it is made up of above-mentioned lithium titanate electrode material, solvent and binding agent, the weight ratio of wherein said solvent and binding agent is (95-97): (3-5), and the ratio of the total weight of the weight of described lithium titanate electrode material and described solvent and binding agent is (38 ~ 48): 100.
Wherein in an embodiment, described solvent is 1-METHYLPYRROLIDONE; Described binding agent is polyvinylidene fluoride.
Another object of the present invention is to provide the preparation method of above-mentioned lithium titanate electrode slurry.
Concrete technical scheme is as follows:
A preparation method for lithium titanate electrode slurry, comprises the steps:
(1) with double planetary mixer revolution linear velocity 5 ~ 15m/s after described solvent and binding agent being mixed, rotation wire speed 15 ~ 25m/s stirs 100 ~ 200min, obtains mixed liquor;
(2) in described mixed liquor, drop into described lithium titanate electrode material, adopt double planetary mixer vacuum stirring, vacuum values-0.07 ~ 0.095MPa, revolution linear velocity 5 ~ 15m/s, rotation wire speed 15 ~ 25m/s, stirs 100 ~ 300min, obtains described lithium titanate electrode slurry.
Principle of the present invention and advantage as follows:
The preparation of lithium titanate electrode material of the present invention, adopts Graphene and carbon nano-tube to match as conductive agent, utilizes macromolecule dispersing agent (PVP, polyvinylpyrrolidone, (C
6h
9nO)
n) as dispersant agent, take 1-METHYLPYRROLIDONE as solvent, dispersion treatment is carried out to Graphene and carbon nano-tube, simultaneously by rationally arranging each preparation process and technological parameter, realize the dispersed of Graphene and carbon nano-tube and make Graphene and carbon nano-tube carry out coated on the surface of lithium titanate, effectively improve the electric conductivity of lithium titanate electrode material, its principle is as follows:
Adopt polyvinylpyrrolidone (PVP) as macromolecule dispersing agent, utilize the surface-active action of polyvinylpyrrolidone effectively can improve the peptizaiton of Graphene and carbon nano-tube, Graphene and carbon nano-tube are better disperseed, effectively promotes dispersed in 1-METHYLPYRROLIDONE of Graphene and carbon nano-tube.Then the Graphene after dispersion and carbon nano tube paste are carried out milled processed separately under certain process conditions, the more uniform Graphene of particle and carbon nano-tube can be obtained, its dispersion of further promotion, now mix with lithium titanate again, and conservative control is carried out to the weight ratio of Graphene and carbon nano tube paste and lithium titanate, Graphene and carbon nano-tube can be made in follow-up dry run to form the more uniform coating layer of form on lithium titanate surface, give full play to the electric conductivity of Graphene and carbon nano-tube, and then effectively improve capacitance and the discharge-rate of obtained electrode, be conducive to the Homogeneouslly-radiating of electrode simultaneously, reduce the appearance of the heating problem in battery rate charge-discharge process.
Further, carry out controlling to obtain better covered effect to drying process in dry run.The present invention is preferably and first carries out spraying dry high temperature 300 ~ 400 DEG C, can remove mixed slurry inside 97% ~ 98% volatile substances, is conducive to Graphene and carbon nano-tube carry out coated to lithium titanate; Again the material after coated is dropped into high temperature kiln and carry out high temperature 600 ~ 800 DEG C calcining 10 ~ 15h, the covered effect of further raising Graphene and carbon nano-tube, remove volatile substances contained by coated rear lithium titanate material simultaneously, reduce electrode polarization, make the lithium titanate material obtained have better conductive effect, promote the raising of electrode capacitance amount and discharge-rate.
Compared with prior art, the present invention has following beneficial effect:
Adopt the lithium titanate electrode material that preparation method of the present invention prepares, electric conductivity is excellent, can comparatively prior art improve battery capacity 1% ~ 8%, discharge-rate raising 1% ~ 5%, realize quick charge, the appearance of the heating problem in battery rate charge-discharge process can be reduced simultaneously.
Accompanying drawing explanation
Fig. 1 is preparation technology's flow chart of lithium titanate electrode slurry described in one embodiment of the invention;
Fig. 2 is the charging and discharging curve figure of lithium titanate electrode slurry described in the embodiment of the present invention 1;
Fig. 3 is the charging and discharging curve figure of lithium titanate electrode slurry described in the embodiment of the present invention 2;
Fig. 4 is the charging and discharging curve figure of lithium titanate electrode slurry described in the embodiment of the present invention 3;
Fig. 5 is the charging and discharging curve figure of lithium titanate electrode slurry described in comparative example 1 of the present invention;
Fig. 6 is the charging and discharging curve figure of lithium titanate electrode slurry described in comparative example 2 of the present invention.
Embodiment
Below in conjunction with specific embodiment, lithium titanate electrode material of the present invention and preparation method thereof is described in further detail.
Embodiment 1
The preparation method of a kind of lithium titanate electrode slurry of the present embodiment, its process chart as shown in Figure 1, specifically comprises the steps:
(1) preparation of lithium titanate electrode material
(1) Graphene, carbon nano-tube stirring is added by after 1-METHYLPYRROLIDONE, polyvinylpyrrolidone mixing, the mass concentration controlling Graphene is 2%, the mass concentration of carbon nano-tube is 3%, the mass concentration of polyvinylpyrrolidone is 1%, adopt double planetary mixer, revolution linear velocity 15m/s, rotation wire speed 20m/s, stir 60min, obtain slurry A;
(2) described slurry A being dropped into grinder and adds diameter is that 0.5 ~ 1mm zirconia grinds, rotating speed 200r/min, grinding 150min, then add lithium titanate in the slurry A after grinding, the weight ratio controlling the slurry A after grinding and lithium titanate is 5.5:4.5, adopts double planetary mixer, revolution linear velocity 15m/s, rotation wire speed 18m/s, stirs 100min, obtains slurry B;
(3) first described slurry B input spray dryer is carried out high temperature 300 ~ 400 DEG C of spraying dry and obtain coated lithium titanate material presoma; Again under nitrogen protection condition; presoma after spray-dried is dropped into high temperature kiln to carry out high temperature constant temperature 600 DEG C calcining 14h and obtain coated rear lithium titanate material; to room temperature after finally cooling under low humidity 0.5%RH ~ 1%RH environment, obtain described lithium titanate electrode material, for subsequent use.
(2) preparation of lithium titanate electrode slurry
(1) with double planetary mixer revolution linear velocity 15m/s after 1-METHYLPYRROLIDONE (NMP) and polyvinylidene fluoride (PVDF) being mixed, rotation wire speed 18m/s stirs 150min, obtain mixed liquor, the weight ratio of described 1-METHYLPYRROLIDONE and polyvinylidene fluoride is 95:3;
(2) in described mixed liquor, above-mentioned lithium titanate electrode material is dropped into, the weight ratio of described lithium titanate electrode material and described 1-METHYLPYRROLIDONE is 38:100, adopt double planetary mixer vacuum stirring, vacuum values-0.07 ~ 0.095MPa, revolution linear velocity 15m/s, rotation wire speed 18m/s, stirs 200min, obtains described lithium titanate electrode slurry.
Embodiment 2
The preparation method of a kind of lithium titanate electrode slurry of the present embodiment, comprises the steps:
(1) preparation of lithium titanate electrode material
(1) Graphene, carbon nano-tube stirring is added by after 1-METHYLPYRROLIDONE, polyvinylpyrrolidone mixing, the mass concentration controlling Graphene is 3%, the mass concentration of carbon nano-tube is 1%, the mass concentration of polyvinylpyrrolidone is 2%, adopt double planetary mixer, revolution linear velocity 15m/s, rotation wire speed 15m/s, stir 30min, obtain slurry A;
(2) described slurry A being dropped into grinder and adds diameter is that 0.5 ~ 1mm zirconia grinds, rotating speed 250r/min, grinding 60min, then lithium titanate is added in the slurry A after grinding, the weight ratio controlling the slurry A after grinding and lithium titanate is 6:4, adopts double planetary mixer, revolution linear velocity 15m/s, rotation wire speed 15m/s stirs 60min, obtains slurry B;
(3) first described slurry B input spray dryer is carried out high temperature 300 ~ 400 DEG C of spraying dry and obtain coated lithium titanate material presoma; Presoma after spray-dried is dropped into high temperature kiln under nitrogen protection condition, to carry out high temperature 800 DEG C calcining 10h obtain coated rear lithium titanate material; last latter extremely about 60 DEG C of cooling under low humidity 0.5%RH ~ 1%RH environment; obtain described lithium titanate electrode material, for subsequent use.
(2) preparation of lithium titanate electrode slurry
(1) by after 1-METHYLPYRROLIDONE and polyvinylidene fluoride mixing, with double planetary mixer revolution linear velocity 5m/s, rotation wire speed 25m/s, stir 100min, obtain mixed liquor, the weight ratio of described 1-METHYLPYRROLIDONE and polyvinylidene fluoride is 97:3;
(2) in described mixed liquor, above-mentioned lithium titanate electrode material is dropped into, the weight ratio of described lithium titanate electrode material and described 1-METHYLPYRROLIDONE is 48:100, adopt double planetary mixer vacuum stirring, vacuum values-0.07 ~ 0.095MPa, revolution linear velocity 13m/s, rotation wire speed 15m/s, stirs 100min, obtains described lithium titanate electrode slurry.
Embodiment 3
The preparation method of a kind of lithium titanate electrode slurry of the present embodiment, comprises the steps:
(1) preparation of lithium titanate electrode material
(1) Graphene, carbon nano-tube stirring is added by after 1-METHYLPYRROLIDONE, polyvinylpyrrolidone mixing, the mass concentration controlling Graphene is 3%, the mass concentration of carbon nano-tube is 2%, the mass concentration of polyvinylpyrrolidone is 1.5%, adopt double planetary mixer, revolution linear velocity 5m/s, rotation wire speed 25m/s, stir 60min, obtain slurry A;
(2) described slurry A being dropped into grinder and adds diameter is that 0.5 ~ 1mm zirconia grinds, rotating speed 150r/min, grinding 300min, then add lithium titanate in the slurry A after grinding, the weight ratio controlling the slurry A after grinding and lithium titanate is 6:4, adopts double planetary mixer, revolution linear velocity 5m/s, rotation wire speed 25m/s, stirs 150min, obtains slurry B;
(3) first described slurry B input spray dryer is carried out high temperature 300 ~ 400 DEG C of spraying dry and obtain coated lithium titanate material presoma; Presoma after spray-dried is dropped into high temperature kiln under nitrogen protection condition, to carry out high temperature constant temperature 700 DEG C calcining 15h obtain coated rear lithium titanate material; to room temperature after finally cooling under low humidity 0.5%RH ~ 1%RH environment; obtain described lithium titanate electrode material, for subsequent use.
(2) preparation of lithium titanate electrode slurry
(1) with double planetary mixer revolution linear velocity 10m/s, rotation wire speed 15m/s after 1-METHYLPYRROLIDONE and polyvinylidene fluoride being mixed, stir 200min, obtain mixed liquor, the weight ratio of described 1-METHYLPYRROLIDONE and polyvinylidene fluoride is 95:5;
(2) in described mixed liquor, above-mentioned lithium titanate electrode material is dropped into, the weight ratio of described lithium titanate electrode material and described 1-METHYLPYRROLIDONE is 45:100, adopt double planetary mixer vacuum stirring, vacuum values-0.07 ~ 0.095MPa, revolution linear velocity 5m/s, rotation wire speed 25m/s, stirs 300min, obtains described lithium titanate electrode slurry.
Comparative example 1
A kind of lithium titanate electrode slurry of this comparative example, its preparation method is with embodiment 1, and difference is: do not add described macromolecule dispersing agent.
Comparative example 2
A kind of lithium titanate electrode slurry of this comparative example, its preparation method is with embodiment 1, and difference is: Graphene is changed to Super-p (conductive carbon black).
The rate charge-discharge curve of lithium titanate electrode slurry described in embodiment 1-3 successively as in Figure 2-4, successively as seen in figs. 5-6, in figure, charging and discharging curve is 10C rate charge-discharge curve (10C multiplying power: 10 times of electric currents of nominal capacity carry out discharge and recharge) to the rate charge-discharge curve of lithium titanate electrode slurry described in comparative example 1-2.
After graphene coated lithium titanate of the present invention, graphene uniform is covered in lithium titanate surface, reduce link polarization between lithium titanate, graphene uniform is coated on lithium titanate surface polarization and reduces, its multiplying power discharging can be learnt by Fig. 2-4, and embodiment 1-3 moderate multiplying factor discharge and recharge effect is all better than the multiplying power discharging effect of comparative example 1-2.Can learn thus, the method for graphene coated lithium titanate of the present invention can improve lithium titanate rate charge-discharge performance.
Each technical characteristic of the above embodiment can combine arbitrarily, for making description succinct, the all possible combination of each technical characteristic in above-described embodiment is not all described, but, as long as the combination of these technical characteristics does not exist contradiction, be all considered to be the scope that this specification is recorded.
The above embodiment only have expressed several execution mode of the present invention, and it describes comparatively concrete and detailed, but can not therefore be construed as limiting the scope of the patent.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection range of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a preparation method for lithium titanate electrode material, is characterized in that, comprises the steps:
(1) carbon nano-tube, Graphene stirring is added by after 1-METHYLPYRROLIDONE, polyvinylpyrrolidone mixing, the mass concentration controlling Graphene is 2 ~ 3%, the mass concentration of carbon nano-tube is 1 ~ 3%, and the mass concentration of polyvinylpyrrolidone is 1 ~ 2%, obtains slurry A;
(2) described slurry A is dropped into grinder and adds zirconia particles grind, rotating speed 150 ~ 250r/min, grinding 60 ~ 300min, then add lithium titanate in the slurry A after grinding and carry out mix and blend, the weight ratio controlling the slurry A after grinding and lithium titanate is (5.5:4.5) ~ (6:4), obtains slurry B;
(3), after described slurry B being carried out drying process, described lithium titanate electrode material is obtained.
2. the preparation method of lithium titanate electrode material according to claim 1, it is characterized in that, described in step (3), the technological parameter of dry process is: first described slurry B input spray dryer is carried out high temperature 300 ~ 400 DEG C of spraying dry and obtain coated lithium titanate material presoma; Again described coated lithium titanate material presoma is dropped into high temperature kiln and carry out high temperature 600 ~ 800 DEG C calcining 10-15h under nitrogen protection.
3. the preparation method of lithium titanate electrode material according to claim 1, it is characterized in that, the technological parameter stirred described in step (1) is: adopt double planetary mixer, revolution linear velocity 5 ~ 15m/s, rotation wire speed 15 ~ 25m/s, stirs 30 ~ 60min.
4. the preparation method of lithium titanate electrode material according to claim 1, it is characterized in that, described in step (2), the technological parameter of mix and blend is: adopt double planetary mixer, revolution linear velocity 5 ~ 15m/s, rotation wire speed 15 ~ 25m/s, stirs 60 ~ 150min.
5. the preparation method of the lithium titanate electrode material according to any one of claim 1-4, is characterized in that, described in step (2), the diameter of zirconia particles is 0.5 ~ 1mm.
6. the preparation method of the lithium titanate electrode material according to any one of claim 1-4, it is characterized in that, after dry process described in step (3), also comprise cooling step: the lithium titanate material after described drying process is placed under humidity is the environment of 0.5 ~ 1%RH and is cooled to room temperature.
7. the lithium titanate electrode material that the preparation method of the lithium titanate electrode material described in any one of claim 1-6 prepares.
8. a lithium titanate electrode slurry, it is characterized in that, it is made up of lithium titanate electrode material according to claim 7, solvent and binding agent, the weight ratio of wherein said solvent and binding agent is (95-97): (3-5), and the ratio of the total weight of the weight of lithium titanate electrode material according to claim 7 and described solvent and binding agent is (38 ~ 48): 100.
9. lithium titanate electrode slurry according to claim 8, is characterized in that, described solvent is 1-METHYLPYRROLIDONE; Described binding agent is polyvinylidene fluoride.
10. the preparation method of the lithium titanate electrode slurry described in claim 8 or 9, is characterized in that, comprise the steps:
(1) with double planetary mixer revolution linear velocity 5 ~ 15m/s after described solvent and binding agent being mixed, rotation wire speed 15 ~ 25m/s, stirs 100 ~ 200min, obtains mixed liquor;
(2) in described mixed liquor, lithium titanate electrode material according to claim 7 is dropped into, adopt double planetary mixer vacuum stirring, vacuum values-0.07 ~ 0.095MPa, revolution linear velocity 5 ~ 15m/s, rotation wire speed 15 ~ 25m/s, stir 100 ~ 300min, obtain described lithium titanate electrode slurry.
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| CN108451522A (en) * | 2018-03-28 | 2018-08-28 | 北京华灿康国际医药研究有限公司 | A kind of Medical Devices |
| CN109037641A (en) * | 2018-08-07 | 2018-12-18 | 河源广工大协同创新研究院 | A kind of lithium ion battery MoS2The preparation method of negative electrode material |
| CN109637697A (en) * | 2018-12-24 | 2019-04-16 | 广东省稀有金属研究所 | A kind of graphene conductive slurry and preparation method thereof |
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