CN106531987A - Preparation method of lithium titanate material - Google Patents
Preparation method of lithium titanate material Download PDFInfo
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- CN106531987A CN106531987A CN201610912490.1A CN201610912490A CN106531987A CN 106531987 A CN106531987 A CN 106531987A CN 201610912490 A CN201610912490 A CN 201610912490A CN 106531987 A CN106531987 A CN 106531987A
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- H01M4/36—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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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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- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a preparation method of a lithium titanate material. The method comprises the following steps of (1) a high-temperature solid phase method, namely mixing lithium carbonate with titanium dioxide at a certain ratio, burning in vacuum or a protective gas atmosphere and naturally cooling the mixture to prepare a lithium titanate raw material; (2) carbon (CB) coating treatment, namely mixing a carbon source with lithium titanate raw material powder obtained in the step (1) evenly, burning in vacuum or the protective gas atmosphere, and naturally cooling the mixture to obtain a carbon-coated lithium titanate material; and (3) PE surface modification, namely mixing the carbon-coated lithium titanate material obtained in the step (2) with PE powder evenly, burning in vacuum or the protective gas atmosphere, and naturally cooling the mixture to obtain a CB/PE polymer material-coated lithium titanate material. According to the lithium titanate material prepared by the preparation method of the lithium titanate material provided by the invention, a CB/PE polymer-based conductive material coats the lithium titanate surface, and a current collector is good in bonding effect and not liable to fall off, and has good rate capability and bonding strength.
Description
【Technical field】
A kind of the present invention relates to technical field of lithium ion, more particularly to preparation method of lithium titanate material.
【Background technology】
Lithium titanate (Li4Ti5O12) increasingly receive publicity as a kind of new lithium ion battery negative material, which has
Following advantage：In charge and discharge process, there is no crystal formation change, Volume Changes are less than 1%, are referred to as " zero strain material ", circulate
Excellent performance；Higher oxidation-reduction potential (1.5VvsLi), is not reacted with conventional electrolyte, and security is good；Environment friend
It is good, easily prepare, low cost.
Lithium titanate material has higher lithium ion diffusion coefficient, is 2 × 10 at 25 DEG C-8cm2/ s, however, Li4Ti5O12
Electrical conductivity it is low by (10-13S·cm-1), belong to insulator, cause its high rate capability poor, be unfavorable for fast charging and discharging；Meanwhile, titanium
Sour lithium material is poor with the caking property of collector (Copper Foil, aluminium foil), and higher interface impedance further affects its circulation
Energy.
In consideration of it, real be necessary to provide a kind of preparation method of new lithium titanate material to overcome disadvantages described above.
【The content of the invention】
It is an object of the invention to provide a kind of preparation method of new lithium titanate material, using the method that the present invention is provided
Active material of the prepared lithium titanate material as lithium ion battery negative, lithium ion battery charging capacity are high, first efficiency
Height, with well filling high rate performance and stable cycle performance soon.
To achieve these goals, the present invention provides a kind of preparation method of lithium titanate material, comprises the steps：
Step one：High temperature solid-state method：Lithium carbonate and titanium dioxide are mixed by a certain percentage, in vacuum or protective gas atmosphere
Middle calcining is enclosed, natural cooling prepares lithium titanate raw material；
Step 2：The process of carbon (CB) cladding：The lithium titanate raw material powder that carbon source and step one are obtained is mixed, in vacuum
Or calcine in protective gas atmosphere, natural cooling obtains carbon coating lithium titanate material；
Step 3：PE surface modifications：The carbon coating lithium titanate material that step 2 is obtained uniformly is mixed with PE powder, true
Calcine in empty or protective gas atmosphere, natural cooling, obtain the lithium titanate material of CB/PE macromolecular materials cladding.
Lithium titanate material prepared by the preparation method of the lithium titanate material provided compared to prior art, the present invention,
Lithium titanate Surface coating CB/PE polymer based conducting materials, can form effective conductive network, and specific insulation is less than
1010Ω·cm；Meanwhile, can coordinate with PVDF conductive agents well in battery formula, collector adhesive effect is good, is difficult
Come off, need not be with expensive carbon-coated aluminum foils, painting carbon Copper Foil as collector, with good high rate performance and bonding when making
Intensity.
【Description of the drawings】
Fig. 1 is the SEM figures of lithium titanate material prepared by the embodiment of the present invention；
Fig. 2 is the charging measurement curve map of the button cell of lithium titanate material prepared by the embodiment of the present invention；
Fig. 3 is the multiplying power test curve figure of the full battery of lithium titanate material prepared by the embodiment of the present invention；
Fig. 4 is the 6C cyclic curve figures of the full battery of lithium titanate material prepared by the embodiment of the present invention.
【Specific embodiment】
In order that the purpose of the present invention, technical scheme and Advantageous Effects become apparent from understanding, below in conjunction with accompanying drawing and
Specific embodiment, the present invention will be described in further detail.It should be appreciated that being embodied as described in this specification
Mode is not intended to limit the present invention just for the sake of explaining the present invention.
The present invention provides the preparation method of lithium titanate material, comprises the steps：
Step one：High temperature solid-state method：Lithium carbonate and titanium dioxide are mixed by a certain percentage, in vacuum or protective gas atmosphere
Middle calcining is enclosed, natural cooling prepares lithium titanate raw material；
Step 2：The process of carbon (CB) cladding：The lithium titanate raw material powder that carbon source and step one are obtained is mixed, in vacuum
Or calcine in protective gas atmosphere, natural cooling obtains carbon coating lithium titanate material；
Step 3：PE surface modifications：The carbon coating lithium titanate material that step 2 is obtained is uniform with PE (polyethylene) powder
Mixing, calcines in vacuum or protective gas atmosphere, natural cooling, obtains the lithium titanate material of CB/PE macromolecular materials cladding.
Embodiment：
1st, by Li：Ti=0.85：1 proportioning weighs lithium carbonate and titanium dioxide, is mixed as solvent with absolute ethyl alcohol, and
And with ball mill in argon gas atmosphere ball milling 12 hours, the lithium carbonate and titanium dioxide mixture of gained are put in into 85 DEG C of vacuum and are dried
Dry in case, remove solvent, the lithium carbonate and titanium dioxide mixture that remove solvent are positioned in high-temperature atmosphere electric furnace, take out true
Sky, is passed through 99.95% nitrogen shielding gas, is warmed up to 850 DEG C with 5 DEG C/min of speed, and is kept for 12 hours at this temperature,
Room temperature is naturally cooled in nitrogen atmosphere, and stopping is passed through nitrogen, obtains white lithium titanate powder；
2nd, by the lithium titanate powder for obtaining and glucose in mass ratio 100:10 uniform mixing, are subsequently placed in ball mill,
Ball milling 6 hours in argon gas atmosphere；The lithium titanate powder and glucose mixture of ball milling are placed in into high-temperature atmosphere electric furnace, take out true
Sky, leads to 99.9% nitrogen shielding gas, is then warmed up to 900 DEG C with 5 DEG C/min of speed, and is kept for 6 hours at this temperature,
Room temperature is naturally cooled in nitrogen atmosphere, stopping is passed through nitrogen, obtain black carbon (CB) cladding lithium titanate powder；
3rd, the lithium titanate powder for coating the carbon for obtaining (CB) is by 1:9 ratio adds absolute ethyl alcohol as in solvent, high
Speed stirring, ultrasonic disperse 30min；By 10：2 ratio adds PE powder, high-speed stirred, ultrasonic wave dispersion 30min, 85 DEG C of air
Middle solvent evaporated；Solvent evaporated is obtained material to be positioned in high-temperature atmosphere, argon gas atmosphere protection is passed through, with the speed of 5 DEG C/min
Degree is warming up to 250 DEG C, and keeps 6h at this temperature, naturally cools to room temperature, and the lithium titanate powder of the CB/PE claddings of black is obtained
End.
The invention provides the lithium titanate powder of the CB/PE claddings prepared using the inventive method is used as negative electrode active material
Button cell and full battery assembling and test, specific experiment process and result it is as follows：
1st, the making and test of button cell
Active material of the lithium titanate of the CB/PE claddings prepared using above-described embodiment as negative pole, Super-P are conduction
Pole, segregation PVF (PVDF) are binding agent, successively according to 90：5：5 ratio mixes and grinds with 1-METHYLPYRROLIDONE (NMP)
Slurry is obtained after mill.Slurry is coated on copper foil of affluxion body, punching after vacuum drying, the positive polar circle of a diameter of 10mm is obtained
Piece.
Test Selection of Battery CR2032 button cells, metal lithium sheet of the negative pole from diameter 14mm, electrolyte select concentration
For the LiPF of 1mol/L6/EC+DMC+EMC(1：1：1), and containing 0.5%LiODFB, 3%PS3, with negative electrode casing, shell fragment, pad,
Battery is packaged by lithium piece, electrolyte, barrier film, positive plate, pad, the order of anode cover, and whole process is all filled with argon gas
Glove box in complete.
Test equipment selects new prestige Neware BTS test systems, discharge and recharge blanking voltage 1.0～3.0V of scope, test temperature
25 DEG C of degree, records the first charge-discharge capacity such as table 1 below of battery：
Table 1
Fig. 1 is the SEM figures of the lithium titanate material prepared by the embodiment of the present invention；Fig. 2 is bent for the charging of button cell 0.5C
Line.The lithium titanate material of the CB/PE claddings that as can be seen from Figure 1 prepared by the present invention has preferable pattern；As can be seen from Figure 2 this
The lithium titanate material of the CB/PE claddings of bright preparation has preferable embedding lithium platform, is close to theoretical value；As can be seen from Table 1 originally
The lithium titanate material of CB/PE claddings prepared by invention has higher charging capacity, and average charge capacity 159.05mAh/g is first
Secondary efficiency is up to 98.03%.
2nd, the making and test of full battery
Using present invention method prepare CB/PE cladding lithium titanate material as negative electrode active material, with 111 types
, used as positive active material, Ju Ti Pei Fang is as follows for ternary material：
Positive pole：NCM：SP：KS-6：PVDF=94：3：1：2；
Negative pole：LTO：SP：PVDF=90：5：5；
Positive pole does collector using aluminium foil, and negative pole (does not require the use of special painting carbon using common Copper Foil as collector
Aluminium foil applies carbon Copper Foil)；
Electrolyte：1mol/L, LiPF6/EC+DMC+EMC(1：1：1), containing 0.5%LiODFB, 3%PS.
The test data such as table 2 below of the multiplying power charge and discharge of full battery：
Table 2
Fig. 3 is the multiplying power test curve of full battery；Fig. 4 is the 6C cyclical trend figures of full battery.From the test number of full battery
According to it can be seen that using the inventive method prepare CB/PE cladding lithium titanate material, with 111 type ternary materials arrange in pairs or groups with compared with
High 6C chargings constant current ratio, can reach 95%, 6C and circulates 509 weeks, and capability retention is more than 100%, it is seen which has good fast
Fill high rate performance and stable cycle performance.Also, from the making on common Copper Foil and circulation, prepared by the inventive method
CB/PE cladding lithium titanate material there is good foil bond effect.
To sum up, the lithium titanate material prepared by the preparation method of the lithium titanate material that the present invention is provided, on lithium titanate surface
Cladding CB/PE polymer based conducting materials, can form effective conductive network, and specific insulation is less than 1010Ω·cm；Together
When, can coordinate with PVDF conductive agents well in battery formula, collector adhesive effect is good, difficult for drop-off, when making without
Need to be with expensive carbon-coated aluminum foils, painting carbon Copper Foil as collector, with good high rate performance and adhesion strength.
The present invention is not restricted to described in specification and embodiment, therefore for the personnel of familiar field
Additional advantage and modification is easily achieved, therefore in the essence of the universal limited without departing substantially from claim and equivalency range
In the case of god and scope, the present invention is not limited to specific details, representational equipment and shown here as the diagram with description
Example.
Claims (8)
1. a kind of preparation method of lithium titanate material, it is characterised in that：Comprise the steps：
Step one：High temperature solid-state method：Lithium carbonate and titanium dioxide are mixed by a certain percentage, in vacuum or protective gas atmosphere
Calcining, natural cooling prepare lithium titanate raw material；
Step 2：The process of carbon (CB) cladding：The lithium titanate raw material powder that carbon source and step one are obtained is mixed, in vacuum or guarantor
Calcine in shield atmosphere, natural cooling obtains carbon coating lithium titanate material；
Step 3：PE surface modifications：The carbon coating lithium titanate material that step 2 is obtained uniformly is mixed with PE powder, in vacuum or
Calcine in protective gas atmosphere, natural cooling, obtain the lithium titanate material of CB/PE macromolecular materials cladding.
2. the preparation method of lithium titanate material as claimed in claim 1, it is characterised in that：Lithium carbonate and two in the step one
The proportioning of titanium oxide is Li：Ti=0.85：1.
3. the preparation method of lithium titanate material as claimed in claim 2, it is characterised in that：Lithium carbonate in the step one and
Titanium dioxide absolute ethyl alcohol as solvent mix, and with ball mill in argon gas atmosphere ball milling 12 hours, by the carbon of gained
Sour lithium and titanium dioxide mixture are dried in being put in 85 DEG C of vacuum drying ovens, remove solvent.
4. the preparation method of lithium titanate material as claimed in claim 3, it is characterised in that：Method for calcinating in the step one
It is that the lithium carbonate and titanium dioxide mixture that remove solvent are positioned in high-temperature atmosphere electric furnace, vacuumizes, be passed through 99.95% nitrogen
Gas shielded gas, is warmed up to 850 DEG C with 5 DEG C/min of speed, and is kept for 12 hours at this temperature, natural in nitrogen atmosphere
Room temperature is cooled to, stopping is passed through nitrogen, obtains lithium titanate raw material.
5. the preparation method of lithium titanate material as claimed in claim 4, it is characterised in that：Carbon source in the step 2 is Portugal
The mass ratio 100 of grape sugar, lithium titanate and glucose:10, the mixing method in the step 2 is to be placed in ball mill, in argon gas gas
Ball milling 6 hours in atmosphere.
6. the preparation method of lithium titanate material as claimed in claim 5, it is characterised in that：Method for calcinating in the step 2
It is that the lithium titanate powder that will be well mixed and glucose mixture are placed in high-temperature atmosphere electric furnace, vacuumizes, leads to 99.9% nitrogen and protect
Shield gas, is then warmed up to 900 DEG C with 5 DEG C/min of speed, and is kept for 6 hours at this temperature, naturally cold in nitrogen atmosphere
But to room temperature, stopping is passed through nitrogen, obtains carbon coating lithium titanate powder.
7. the preparation method of lithium titanate material as claimed in claim 6, it is characterised in that：Carbon coating metatitanic acid in the step 3
Lithium material with the mixed method of PE powder is：The lithium titanate powder of carbon coating is pressed into 1：During 9 ratio adds absolute ethyl alcohol, at a high speed
Stirring, ultrasonic disperse 30min；By 10：2 ratio adds PE powder, high-speed stirred, ultrasonic wave dispersion 30min, and 85 DEG C of air
Middle solvent evaporated.
8. the preparation method of lithium titanate material as claimed in claim 7, it is characterised in that：In the step 3, method for calcinating is
The material of solvent evaporated is positioned in high-temperature atmosphere, is passed through argon gas atmosphere protection, 250 is warming up to 5 DEG C of speed per minute
DEG C, and 6h is kept at this temperature, room temperature is naturally cooled to, the lithium titanate material of CB/PE macromolecular materials cladding is obtained.
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| CN201610912490.1A CN106531987A (en) | 2016-10-19 | 2016-10-19 | Preparation method of lithium titanate material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109713254A (en) * | 2018-12-05 | 2019-05-03 | 郑州中科新兴产业技术研究院 | A kind of preparation method of metal conductive oxide powder composite titanic acid lithium material |
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| CN102496707A (en) * | 2011-12-30 | 2012-06-13 | 天津力神电池股份有限公司 | Preparation method of nano-grade-carbon-clad spinel lithium titanate battery cathode material |
| CN103022462A (en) * | 2012-12-20 | 2013-04-03 | 中国东方电气集团有限公司 | Preparation method for high-conductivity lithium titanate cathode material of lithium battery |
| CN104577090A (en) * | 2014-12-23 | 2015-04-29 | 山东精工电子科技有限公司 | Method for preparing carbon and oxide composite modified lithium titanate material |
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2016
- 2016-10-19 CN CN201610912490.1A patent/CN106531987A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101567442A (en) * | 2008-07-28 | 2009-10-28 | 新乡市中科科技有限公司 | Method for preparing spinel lithium titanate |
| CN101916846A (en) * | 2010-08-19 | 2010-12-15 | 深圳市贝特瑞新能源材料股份有限公司 | Lithium ion battery cathode composite material and preparation method thereof |
| CN102496707A (en) * | 2011-12-30 | 2012-06-13 | 天津力神电池股份有限公司 | Preparation method of nano-grade-carbon-clad spinel lithium titanate battery cathode material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109713254A (en) * | 2018-12-05 | 2019-05-03 | 郑州中科新兴产业技术研究院 | A kind of preparation method of metal conductive oxide powder composite titanic acid lithium material |
| CN109713254B (en) * | 2018-12-05 | 2021-03-02 | 郑州中科新兴产业技术研究院 | Preparation method of metal oxide conductive powder composite lithium titanate material |
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