CN106207150A - A kind of atomizing freeze drying prepares the method for lithium cell negative pole material lithium titanate - Google Patents
A kind of atomizing freeze drying prepares the method for lithium cell negative pole material lithium titanate Download PDFInfo
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- CN106207150A CN106207150A CN201610841637.2A CN201610841637A CN106207150A CN 106207150 A CN106207150 A CN 106207150A CN 201610841637 A CN201610841637 A CN 201610841637A CN 106207150 A CN106207150 A CN 106207150A
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- lithium titanate
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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
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
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Abstract
The invention discloses a kind of method that atomizing freeze drying prepares lithium cell negative pole material lithium titanate, it is stoichiometrically to weigh dispensing with Ti compound, Li compound, metal-oxide M, it is scattered in distilled water, after sand milling, with liquid nitrogen and liquid petroleum gas (liquid propane gas) as cryogen, by atomizing freeze drying pelletizing, after calcining, obtain the lithium titanate material of M doping vario-property.Present invention process is simple, and controllability is strong, and resulting materials high rate capability is excellent, is applicable to commercial production lithium titanate anode material.
Description
Technical field
The present invention relates to the preparation method of a kind of battery electrode material, particularly relate to a kind of atomizing freeze drying and prepare lithium
The method of battery negative pole material of lithium titanate.
Background technology
At present, the negative material of business-like lithium ion battery uses carbon negative pole material mostly, but carbon negative pole material is still
There are some defects: react with electrolyte in discharge process first formation surface passivated membrane, result in coulomb effect first
Rate is relatively low；Carbon electrode is close with the electrode potential of lithium metal, when battery overcharge, can form Li dendrite and cause short circuit, causes
Safety problem etc..
Lithium titanate is increasingly becoming the focus of research as the lithium ion battery negative material received much concern in recent years.Its tool
There is plurality of advantages: (1) lithium titanate crystal structure during Lithium-ion embeding is deviate from can keep the stability of height, and makes
It has excellent cycle performance and stable discharge voltage, is referred to as " zero strain " material；(2) lithium titanate is relative to metal
The current potential of lithium is 1.55V, far above the recovery voltage of most electrolyte, can avoid the reduction of electrolyte and the generation of passivating film,
The generation of lithium metal can be stoped simultaneously, there is the most excellent cycle performance and security performance；(3) lithium titanate is being charged to point crystalline substance
When stone structure and rock salt structure two-phase section, there is platform in voltage, utilizes this point, the instruction that can terminate as charging；(4) metatitanic acid
Lithium electrochemical diffusion coefficient at normal temperatures is 2 × 10-8cm2·s-1, big 1 order of magnitude than carbon negative pole material, charge-discharge velocity is very
Hurry up.
But, lithium titanate is a kind of insulant, its poorly conductive, and when high current charge-discharge, capacity attenuation is fast, multiplying power
Poor-performing, limits its application.Existing lithium titanate preparation method is predominantly spray-dried and solid phase method, in preparation process
Middle employing element doping and material with carbon-coated surface, although above method can solve lithium titanate material electronic conductivity to a certain extent
The problem of difference, but its chemical property is the most undesirable.
Summary of the invention
It is an object of the invention to provide a kind of method that atomizing freeze drying prepares lithium battery cathode material lithium titanate, solve
The certainly problem in background technology.
The present invention realizes by the following technical solutions:
The present invention is directed to the existing shortcoming preparing lithium titanate, obtained the Modified Titanium of excellent performance by atomizing freeze drying legal system
Acid lithium material.
1. the method that an atomizing freeze drying prepares lithium cell negative pole material lithium titanate, it is characterised in that described lithium titanate
Molecular formula be Li4MxTi5-xO12, in formula, M is doping vario-property element 0 ＜ x ＜ 0.1, specifically comprises the following steps that
S1: by Li compound, Ti compound and metal-oxide M, Li:(Ti+M in molar ratio)=0.75～0.90 uniform
After mixing, being dispersed in distilled water, solid content is 15%～30%, and the slurry after dispersion is transferred to sand milling 0.5 in sand mill
～2h；
S2: being sprayed to the slurry of S1 medium sand milled in cryogen produce and freeze product, freezing product, to carry out vacuum cold
Lyophilizing dry certain time, make water in products decilitre China disappear, obtain porous spherical lithium titanate precursor；
S3: the porous spherical lithium titanate precursor obtained in S2 is put in atmosphere furnace to replace atmosphere sintering in two steps certain
The porous spherical lithium titanate anode material of M doping vario-property: Li is i.e. obtained after time4MxTi5-xO12。
In the present invention, the Li compound described in S1 is Li2CO3、LiOH·H2O、CH3At least one in COOLi, Ti
Compound is rutile TiO2, anatase titanium dioxide TiO2、H2TiO3In at least one, metal M oxide is Nd2O3、V2O5、
Nb2O5、Ta2O5、MoO3In at least one.
In the present invention, the cryogen described in S2 is liquid nitrogen and liquid petroleum gas (liquid propane gas), and its volume ratio is 1:1～2, described vacuum
Cryogenic temperature is-40～-80 DEG C, and sublimation drying is 8～24h.
In the present invention, in the two steps alternately atmosphere sintering described in S3, first step sintering temperature is 350～500 DEG C, sintering
Atmosphere is air, and sintering time is 4～8h, and second step sintering temperature is 700～900 DEG C, and sintering atmosphere is in nitrogen or argon
One, sintering time is 8～15h.
Beneficial effect: the lithium titanate precursor using the atomizing freeze drying method of the present invention to prepare is surface and internal porous
Spherical products, be different from mesopore, the Conglobation type product of spray drying and drying the lamellar of pulverizing, Pedicellus et Pericarpium Trapae completely
Shape, the lyophilisation product of needle-like；In calcination process, the present invention uses air pre-burning and noble gas calcining two steps annealing method,
The advantage of the method is, Li compound decomposes more preferably in air atmosphere, calcines and can suppress under inert non-oxidizing property atmosphere
The growth of lithium titanate crystal grain, material particle size is evenly distributed and has few part Ti3+Generation, be conducive to improving lithium titanate material
Electric conductivity；The lithium titanate anode material using our bright synthesis has the big rate discharge characteristic of excellence.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the embodiment of the present invention 1 product lithium titanate；
Fig. 2 is the SEM figure of comparative example 1 product lithium titanate of the present invention；
Fig. 3 is the embodiment of the present invention 1 and comparative example 1 product high rate performance comparison diagram.
Detailed description of the invention
For the technological means making the present invention realize, creation characteristic, reach purpose and be easy to understand with effect, below knot
Conjunction is specifically illustrating, and the present invention is expanded on further.
Embodiment 1
Li:(Ti+Nb in molar ratio)=0.805, Ti:Nb=4.95:0.05, weigh Li2CO3, rutile TiO2、
Nb2O5Uniformly being scattered in distilled water after mixing, solid content is 20%, and the slurry after dispersion is transferred to sand milling 1h in sand mill
After, it is sprayed to slurry in the cryogen that liquid nitrogen and liquid petroleum gas (liquid propane gas) mix according to volume ratio 1:1.5 ratio produce freeze product, will
Freeze product and carry out vacuum lyophilization 18 hours at-60 DEG C, make water in products decilitre China disappear, obtain porous spherical metatitanic acid
Lithium presoma, switches to the lower 800 DEG C of sintering of nitrogen atmosphere after presoma is placed in the lower 400 DEG C of pre-burning 5h of air atmosphere in atmosphere furnace
9h obtains target product porous spherical lithium titanate anode material: Li4Nb0.05Ti4.95O12As shown in Figure 1.
The material of embodiment 1 and metal lithium sheet form 2032 button cells uses blue electricity battery test system at 25 DEG C
Testing, test voltage scope 1.0～3.0V, first discharge specific capacity (0.1C) is that 169.7mAh/g, 5C discharge capacity can
Reach 1C discharge capacity after 157mAh/g, 10C discharge capacity reaches 142mAh/g, and 500 circulations and still can reach 152mAh/g.
Embodiment 2
Li:(Ti+Nd in molar ratio)=0.82, Ti:Nd=4.95:0.05, weigh Li2CO3, rutile TiO2、Nd2O3
Uniformly being scattered in distilled water after mixing, solid content is 18%, is transferred in sand mill after sand milling 0.5h by the slurry after dispersion,
It is sprayed to slurry in the cryogen that liquid nitrogen and liquid petroleum gas (liquid propane gas) mix according to volume ratio 1:2 ratio produce freeze product, will freeze
Product carries out vacuum lyophilization 16 hours at-50 DEG C, makes water in products decilitre China disappear, before obtaining porous spherical lithium titanate
Drive body, switch to the lower 775 DEG C of sintering 8h of nitrogen atmosphere after presoma is placed in the lower 435 DEG C of pre-burning 4h of air atmosphere in atmosphere furnace and obtain
To target product porous spherical lithium titanate anode material: Li4Nd0.05Ti4.95O12。
The material of embodiment 2 and metal lithium sheet form 2032 button cells uses blue electricity battery test system at 25 DEG C
Testing, test voltage scope 1.0～3.0V, first discharge specific capacity (0.1C) is that 168.9mAh/g, 5C discharge capacity can
Reach 1C discharge capacity after 152mAh/g, 10C discharge capacity reaches 138mAh/g, and 500 circulations and still can reach 150mAh/g.
Embodiment 3
Li:(Ti+V in molar ratio)=0.80, Ti:V=4.95:0.06, weigh Li2CO3, rutile TiO2、V2O5All
Being scattered in distilled water after even mixing, solid content is 25%, is transferred in sand mill after sand milling 1.5h by the slurry after dispersion, will
Slurry is sprayed in the cryogen that liquid nitrogen and liquid petroleum gas (liquid propane gas) mix according to volume ratio 1:1 ratio produce freeze product, will freeze product
Thing carries out vacuum lyophilization 20 hours at-40 DEG C, makes water in products decilitre China disappear, obtains porous spherical lithium titanate forerunner
Body, switches to the lower 850 DEG C of sintering 8h of nitrogen atmosphere and obtains after presoma is placed in the lower 400 DEG C of pre-burning 4h of air atmosphere in atmosphere furnace
Target product porous spherical lithium titanate anode material: Li4V0.06Ti4.94O12。
The material of embodiment 3 and metal lithium sheet form 2032 button cells uses blue electricity battery test system at 25 DEG C
Testing, test voltage scope 1.0～3.0V, first discharge specific capacity (0.1C) is that 170.3mAh/g, 5C discharge capacity can
Reach 1C discharge capacity after 150mAh/g, 10C discharge capacity reaches 137mAh/g, and 500 circulations and still can reach 149mAh/g.
Comparative example 1:
Li:(Ti+Nb in molar ratio)=0.805, Ti:Nb=4.95:0.05, weigh Li2CO3, rutile TiO2、
Nb2O5Uniformly being scattered in distilled water after mixing, solid content is 20%, and the slurry after dispersion is transferred to sand milling 1h in sand mill
After, the spray drying that slurry carries out routine obtains lithium titanate precursor, and presoma is placed in atmosphere furnace under air atmosphere 400
DEG C pre-burning 5h, then rise under 800 DEG C of air atmospheres, sinter 9h and obtain target product lithium titanate anode material: Li4Nb0.05Ti4.95O12
As shown in Figure 2.
The material of comparative example 1 and metal lithium sheet form 2032 button cells uses blue electricity battery test system at 25 DEG C
Testing, test voltage scope 1.0～3.0V, first discharge specific capacity (0.1C) is that 166.7mAh/g, 5C discharge capacity is
142mAh/g, 10C discharge capacity is 128mAh/g, and after 500 circulations, 1C discharge capacity is 140mAh/g.
Can be seen that lithium titanate sphericity prepared by the present invention is more preferable from the SEM figure of embodiment 1 and comparative example 1, aperture is more
Little, dispersion is more preferable；The lithium titanate anode material that from the point of view of the performance test results prepared by the present invention is in discharge capacity, the most forthright
Energy, capability retention aspect are significantly better than that customary preparation methods.
The ultimate principle of the present invention and principal character and advantages of the present invention, the technology of the industry have more than been shown and described
Personnel, it should be appreciated that the present invention is not restricted to the described embodiments, simply illustrating this described in above-described embodiment and description
The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, and these become
Change and improvement both fall within scope of the claimed invention, claimed scope by appending claims and
Equivalent defines.
Claims (4)
1. the method that an atomizing freeze drying prepares lithium cell negative pole material lithium titanate, it is characterised in that dividing of described lithium titanate
Minor is Li4MxTi5-xO12, in formula, M is doping vario-property element 0 ＜ x ＜ 0.1, specifically comprises the following steps that
S1: by Li compound, Ti compound and metal-oxide M, Li:(Ti+M in molar ratio)=0.75～0.90 uniformly mix
After, it being dispersed in distilled water, solid content is 15%～30%, and the slurry after dispersion is transferred to sand milling 0.5～2h in sand mill；
S2: be sprayed to the slurry of S1 medium sand milled in cryogen produce and freeze product, product will be freezed and carry out vacuum freezing and do
Dry certain time, make water in products decilitre China disappear, obtain porous spherical lithium titanate precursor；
S3: the porous spherical lithium titanate precursor obtained in S2 is put in atmosphere furnace and replace atmosphere sintering certain time in two steps
After i.e. obtain the porous spherical lithium titanate anode material of M doping vario-property: Li4MxTi5-xO12。
A kind of atomizing freeze drying prepares the method for lithium cell negative pole material lithium titanate, and its feature exists
In, the Li compound described in S1 is Li2CO3、LiOH·H2O、CH3At least one in COOLi, Ti compound is rutile
Type TiO2, anatase titanium dioxide TiO2、H2TiO3In at least one, metal M oxide is Nd2O3、V2O5、Nb2O5、Ta2O5、MoO3In
At least one.
A kind of atomizing freeze drying prepares the method for lithium cell negative pole material lithium titanate, and its feature exists
In, the cryogen described in S2 is liquid nitrogen and liquid petroleum gas (liquid propane gas), and its volume ratio is 1:1～2, and described vacuum freezing temperature is-40
～-80 DEG C, sublimation drying is 8～24h.
A kind of atomizing freeze drying prepares the method for lithium cell negative pole material lithium titanate, and its feature exists
In, in the two steps alternately atmosphere sintering described in S3, first step sintering temperature is 350～500 DEG C, and sintering atmosphere is air, sintering
Time is 4～8h, and second step sintering temperature is 700～900 DEG C, and sintering atmosphere is the one in nitrogen or argon, sintering time
It is 8～15h.
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Cited By (6)
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| CN108511713A (en) * | 2018-03-27 | 2018-09-07 | 浙江大学 | A kind of preparation method of sub-micron lithium titanate cathode material |
| CN110563031A (en) * | 2019-09-16 | 2019-12-13 | 广东工业大学 | Lithium titanate negative electrode material, preparation method thereof and battery |
| CN110690431A (en) * | 2019-10-16 | 2020-01-14 | 桑顿新能源科技(长沙)有限公司 | Preparation method of lithium titanate/anatase/rutile three-phase composite material |
| WO2021100282A1 (en) * | 2019-11-20 | 2021-05-27 | 日本碍子株式会社 | Lithium titanate sintered body plate |
| CN113087524A (en) * | 2021-04-14 | 2021-07-09 | 上海交通大学 | Nano zirconium oxide spherical powder and preparation method thereof |
| CN114314647A (en) * | 2021-11-30 | 2022-04-12 | 台州闪能科技有限公司 | A kind of high-density nano-lithium titanate material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113087524A (en) * | 2021-04-14 | 2021-07-09 | 上海交通大学 | Nano zirconium oxide spherical powder and preparation method thereof |
| CN114314647A (en) * | 2021-11-30 | 2022-04-12 | 台州闪能科技有限公司 | A kind of high-density nano-lithium titanate material and preparation method thereof |
| CN114314647B (en) * | 2021-11-30 | 2024-03-22 | 台州闪能科技有限公司 | High-compactness nano lithium titanate material and preparation method thereof |
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Address after: 411201 Hunan province Xiangtan City Jiuhua Demonstration Zone No. 78 West Benz Applicant after: Thornton Amperex Technology Limited Address before: 411100 Hunan province Xiangtan City Jiuhua Demonstration Zone No. 78 West Benz Applicant before: Hunan Sounddon New Energy Co., Ltd. |
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Application publication date: 20161207 |
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| RJ01 | Rejection of invention patent application after publication |