CN106848251A - A kind of preparation method of CNT lithium titanate composite anode material - Google Patents
A kind of preparation method of CNT lithium titanate composite anode material Download PDFInfo
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- CN106848251A CN106848251A CN201710155305.3A CN201710155305A CN106848251A CN 106848251 A CN106848251 A CN 106848251A CN 201710155305 A CN201710155305 A CN 201710155305A CN 106848251 A CN106848251 A CN 106848251A
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- H—ELECTRICITY
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- 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
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- H01M4/364—Composites as mixtures
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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 proposes a kind of preparation method of CNT lithium titanate composite anode material：By carbon nanotube powder ultrasonic disperse in solvent, carbon nano-tube solution A is obtained；Under stirring or ultrasound condition, by Li source compound, titanium source compound and catalyst addition solution A, pH value is adjusted, obtain solution B；Solution B is processed using liquid phase method, the solid that then will be obtained is dried treatment, obtained CNT lithium titanate compound precursor powder；Precursor powder is calcined in inert gas, required CNT lithium titanate composite anode material is obtained after cooling.Beneficial effects of the present invention are as follows：CNT lithium titanate composite anode material obtained in the method for the invention has electronic conductivity and ionic conductivity higher；Phase purity is high, with good cyclical stability；It is easily achieved large-scale production.
Description
Technical field
The present invention relates to technical field of battery electrode materials, a kind of CNT lithium titanate composite anode material is particularly related to
Preparation method.
Background technology
Under the overall situation for advocating energy-conserving and environment-protective, inexpensive, free of contamination electrochemical energy storage device is studied as people
Key areas, wherein, the research and development of lithium ion battery and ultracapacitor and application maintain the leading position all the time.Lithium ion battery
Played an important role in people's daily life with ultracapacitor, for example, portable electronic such as mobile phone, notebook computer sets
It is standby that electric energy is provided, energy regenerating is used in plug-in hybrid electric automobile and for motor provides electric energy etc..
Ultracapacitor has the advantages that power density is high, has extended cycle life, and can be battery or combustion in terms of energy stores
Material battery provides back-up source, wherein with hybrid super capacitor as optimal.The cycle life master of hybrid super capacitor
Depend on the degree of discharge of used battery electrode material.Due to conventional batteries electrode material intermediate ion deintercalation speed compared with
Slowly, the cyclic reversibility and high power charging-discharging of hybrid super capacitor capacity are limited.Therefore, suitable electrode is selected
Material is most important to improving the chemical property of hybrid super capacitor.
Lithium titanate electrode material has the characteristics such as capacity is big, electrode potential is low, have extended cycle life because of it, disclosure satisfy that mixing
Requirement of the type ultracapacitor to electrode material.Have as the negative material of hybrid super capacitor with lithium titanate following excellent
Point：(1) theoretical specific capacity of lithium titanate is high；(2) its skeleton structure is almost unchanged in charge and discharge process, special with " zero strain "
Property, stable cycle performance；(3) intercalation potential is high, is difficult precipitating metal lithium, eliminates potential safety hazard；(4) lithium ion in lithium titanate
Diffusion coefficient is about 10 times of graphite, with large current density electrical dominance.Based on above-mentioned various advantages, lithium titanate is that mixed type surpasses
The level preferable negative pole candidate material of capacitor.However, there is also following shortcoming as cell negative electrode material with lithium titanate：Lithium ion expands
Dissipate coefficient low；Electronic conductivity is low；Charge-discharge performance is poor under the conditions of high current.Therefore, the electric capacity of electrode is made with lithium titanate material
Device high rate performance is poor, greatly constrains its industrialization process.
CNT is a kind of nano-scale tubular structure material that early 1990s find, it is by individual layer or many
The seamless hollow pipe of layer graphene piece curling, with following unusual physical and chemical performance：Unique hollow structure, well
Electric conductivity, larger specific surface area, with suitable electrolyte ion migration hole, and interaction winding can form a nanometer chi
The network structure of degree.Based on above-mentioned characteristic, CNT is also considered as the preferable electrode material of ultracapacitor, draws in recent years
Extensive concern is played.
Lithium titanate is formed into equally distributed conductive network using carbon coating or the mode such as compound with carbon material, can be improved
The electric conductivity of lithium titanate, forthright again and cycle performance.For example, Chinese patent application (publication number CN102694177B) discloses carbon
The preparation method of lithium titanate/carbon/carbon nano tube compound is coated, the method uses titanium-containing compound and CNT susceptible to hydrolysis
After mixed atomizing drying and moulding, with soluble lithium salt ball milling mixing after high temperature sintering obtain carbon coating lithium titanate/carbon/carbon nano tube answer
Compound, effectively increases the specific capacity and high rate performance of material.But, above-mentioned lithium titanate is to adopt with the complex method of CNT
Physical mixed complex method is used, this compound interaction force is on the weak side, and lithium titanate and CNT skewness, so that
Cause final composite electronic conductivity and ionic conductivity low.
The content of the invention
The present invention proposes a kind of preparation method of CNT lithium titanate composite anode material, solves carbon in the prior art
Nanotubed titanic acid lithium composite negative pole material electronic conductivity and the low problem of ionic conductivity.
The technical proposal of the invention is realized in this way：
A kind of preparation method of CNT lithium titanate composite anode material, its method and step is as follows：(1) by CNT
Powder ultrasonic is scattered in solvent, and it is 1g/L~5g/L dispersed carbon nano-tube solution A to obtain concentration；
(2) under stirring or ultrasound condition, by Li source compound, titanium source compound and catalyst addition solution A, treat
After the solid matter of above-mentioned addition is completely dissolved, it is 3~8 to adjust pH value with ammoniacal liquor, obtains solution B；
(3) solution B is processed using liquid phase method, the solid that then will be obtained is dried treatment, is obtained carbon nanometer
Pipe lithium titanate compound precursor powder；
(4) above-mentioned CNT lithium titanate compound precursor powder is calcined 1~24 hour in inert gas, is cooled down
Required CNT lithium titanate composite anode material is obtained afterwards.
Preferably, CNT and the weight ratio of lithium titanate are 1 in the CNT lithium titanate composite anode material:
100~50: 100.
Preferably, the solvent in the step (1) is one or more in water, ethanol, ethylene glycol or acetone.
Preferably, the Li source compound in the step (2) is lithium carbonate, lithium nitrate, lithium sulfate, lithium acetate, phosphoric acid
One or more in lithium, lithium fluoride, lithium oxalate, lithium hydroxide, lithia, lithium chloride or lithium sulfide；The titanium source compound
It is butyl titanate, tetraisopropyl titanate, tetraethyl titanate, metatitanic acid methyl esters, isopropyl titanate, anatase titanium dioxide, rutile
One or more in type titanium dioxide, metatitanic acid, titanium tetrachloride, Titanium Nitrate or titanium oxalate；The catalyst is oxalic acid, lemon
One or more in acid, triethanolamine or hydrogen peroxide.
Preferably, the liquid phase method in the step (3) is sol-gel process, hydro-thermal method or microwave method；At the drying
The method of reason is that heated at constant temperature is dried, rotary evaporation is dried, is spray-dried or freeze-drying.
Preferably, the inert gas in the step (4) is argon gas, nitrogen or helium；The sintering temperature is 400 DEG C
~1200 DEG C.
Preferably, the mol ratio 4: 5~1: 1 between titanium in lithium and titanium source compound in the Li source compound；
The catalyst is 0.1: 100~50: 100 with the weight ratio of the Li source compound.
Preferably, the temperature in the sol-gel process is 20 DEG C~90 DEG C；Reaction temperature in the hydro-thermal method is
100 DEG C~300 DEG C；Reaction time in the microwave method is 5 minutes~60 minutes.
The CNT lithium titanate composite anode material prepared using the method for the invention has good electrochemistry
Energy.Specific capacity during 1C is 173mAh/g, and specific capacity during 10C is 164mAh/g.Charge and discharge cycles 1000 times under 1C multiplying powers
Afterwards, specific capacity conservation rate about 100%；Under the 10C multiplying powers after charge and discharge cycles 1000 times, specific capacity conservation rate 99% is forthright again
Well.
Beneficial effects of the present invention are：
The size Control of lithium titanate is in nanoscale in the method for the invention, and lithium titanate is equably supported on carbon nanometer
Guan Shang, therefore, obtained CNT lithium titanate composite anode material has electronic conductivity and ionic conductivity higher,
So that the hybrid super capacitor being made of it has good high-rate charge-discharge capability.
It is high using CNT lithium titanate composite anode material phase purity obtained in the method for the invention, with good
Cyclical stability.
In addition, the preparation method of CNT lithium titanate composite anode material of the present invention is easily achieved scale metaplasia
Produce.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
The accompanying drawing to be used needed for having technology description is briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is the SEM of the CNT lithium titanate composite anode material prepared by the embodiment of the present invention 2
Figure；
CNT lithium titanate composite anode materials of the Fig. 2 prepared by the embodiment of the present invention 2 is in 1C and 10C current densities
Under charging and discharging curve figure；
CNT lithium titanate composite anode materials of the Fig. 3 prepared by the embodiment of the present invention 2 is in 1C and 10C current densities
Under cycle performance figure.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
Embodiment 1
Diameter is about in the carbon nanotube powder of 2nm addition ethanol, ultrasonic disperse 1 hour, it is 3g/L's to obtain concentration
Solution A.Selection butyl titanate and lithium hydroxide are respectively as titanium source compound and Li source compound.According to lithium and titanium mole
Than the lithium hydroxide that hydrogen peroxide that 1ml concentration is 30% and 1mmol butyl titanates are added to 20ml0.4M for 0.8: 1 priority
In the aqueous solution, stirring is to being completely dissolved.The last mass ratio 7: 93 according to CNT and lithium titanate is by above-mentioned solution and solution A
Mixed.Resulting mixed solution is poured into stainless steel cauldrons of the 50ml with polytetrafluoroethylene (PTFE) as inner bag, after sealing
It is placed in air dry oven, is reacted 12 hours under the conditions of 150 DEG C.After naturally cooling to room temperature, product is poured out, passed through
Centrifugation, washing, freeze-drying, obtain compound precursor powder.The compound precursor powder that will be obtained is placed in argon gas
In environment, sintered 10 hours at a temperature of 800 DEG C, final product CNT lithium titanate composite anode material is obtained after cooling.
Embodiment 2
Diameter is about in the carbon nanotube powder of 1nm addition ethanol, ultrasonic disperse 2 hours, it is 1g/L's to obtain concentration
Solution A.Selection butyl titanate and lithium acetate are respectively as titanium source compound and Li source compound.By above-mentioned butyl titanate and
Lithium acetate is dissolved in ethanol, is configured to the solution B that concentration is 1kg/L.According to the mol ratio 0.84: 1, CNT of lithium and titanium multiple
It is 10wt.% to close mass percent in negative material, the ethanol solution of the solution B that will be prepared and oxalic acid successively while stirring plus
Enter in the ethanol solution of CNT.The pH value of above-mentioned mixed solution is adjusted to 5.6 with ammoniacal liquor.Stirring 3 is small at 30 DEG C
When, then heat to 60 DEG C, stirring to gel.Before wet gel shape material obtained above is changed into xerogel by drying
Drive body.Xerogel presoma is placed in ar gas environment, is sintered 10 hours at a temperature of 800 DEG C, final product is obtained after cooling
CNT lithium titanate composite anode material.
CNT lithium titanate composite anode material form under a scanning electron microscope obtained in above-described embodiment 2 is such as
Shown in Fig. 1, it can be seen that, CNT lithium titanate composite anode material grain shape obtained above is regular, uniform in size, and
Agglomeration is light；
Electrochemical property test is carried out to CNT lithium titanate composite anode material prepared by embodiment 2.Using coating
The electrode slice of legal system available electrochemical property test.Using above-mentioned electrode slice to prepare CNT lithium titanate composite negative pole
Material carries out electrochemical property test, and method of testing is including cyclic voltammetry, AC impedence method and exchanges charge and discharge electrical method etc., test
Result is as shown in Figures 2 and 3.CNT lithium titanate composite anode material multiplying power manufactured in the present embodiment as seen from Figure 2
Performance is good；CNT lithium titanate composite anode material manufactured in the present embodiment has good circulation steady as seen from Figure 3
It is qualitative, under the conditions of heavy-current discharge, still show good cyclical stability.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, it is all in essence of the invention
Within god and principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (8)
1. a kind of preparation method of CNT lithium titanate composite anode material, it is characterised in that its method and step is as follows：(1)
By carbon nanotube powder ultrasonic disperse in solvent, it is 1g/L~5g/L dispersed carbon nano-tube solution A to obtain concentration；
(2) under stirring or ultrasound condition, by Li source compound, titanium source compound and catalyst addition solution A, treat above-mentioned
After the solid matter of addition is completely dissolved, it is 3~8 to adjust pH value with ammoniacal liquor, obtains solution B；
(3) solution B is processed using liquid phase method, the solid that then will be obtained is dried treatment, is obtained CNT titanium
Sour lithium compound precursor powder；
(4) above-mentioned CNT lithium titanate compound precursor powder is calcined 1~24 hour in inert gas, after cooling
To required CNT lithium titanate composite anode material.
2. the preparation method of a kind of CNT lithium titanate composite anode material according to claim 1, it is characterised in that
CNT and the weight ratio of lithium titanate are 1: 100~50: 100 in the CNT lithium titanate composite anode material.
3. the preparation method of a kind of CNT lithium titanate composite anode material according to claim 1, it is characterised in that
Solvent in the step (1) is one or more in water, ethanol, ethylene glycol or acetone.
4. the preparation method of a kind of CNT lithium titanate composite anode material according to claim 1, it is characterised in that
Li source compound in the step (2) is lithium carbonate, lithium nitrate, lithium sulfate, lithium acetate, lithium phosphate, lithium fluoride, lithium oxalate,
One or more in lithium hydroxide, lithia, lithium chloride or lithium sulfide；The titanium source compound is butyl titanate, metatitanic acid
Four isopropyl esters, tetraethyl titanate, metatitanic acid methyl esters, isopropyl titanate, anatase titanium dioxide, rutile titanium dioxide, metatitanic acid, four
One or more in titanium chloride, Titanium Nitrate or titanium oxalate；The catalyst is oxalic acid, citric acid, triethanolamine or hydrogen peroxide
In one or more.
5. the preparation method of a kind of CNT lithium titanate composite anode material according to claim 1, it is characterised in that
Liquid phase method in the step (3) is sol-gel process, hydro-thermal method or microwave method；The method of the dried process adds for constant temperature
Heated drying, rotary evaporation are dried, are spray-dried or freeze-drying.
6. the preparation method of a kind of CNT lithium titanate composite anode material according to claim 1, it is characterised in that
Inert gas in the step (4) is argon gas, nitrogen or helium；The sintering temperature is 400 DEG C~1200 DEG C.
7. the preparation method of a kind of CNT lithium titanate composite anode material according to claim 4, it is characterised in that
The mol ratio 4: 5~1: 1 between the titanium in lithium and titanium source compound in the Li source compound；The catalyst and the lithium
The weight ratio of source compound is 0.1: 100~50: 100.
8. the preparation method of a kind of CNT lithium titanate composite anode material according to claim 5, it is characterised in that
Temperature in the sol-gel process is 20 DEG C~90 DEG C；Reaction temperature in the hydro-thermal method is 100 DEG C~300 DEG C；It is described
Reaction time in microwave method is 5 minutes~60 minutes.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107275614A (en) * | 2017-06-26 | 2017-10-20 | 合肥国轩高科动力能源有限公司 | MoS2CNT lithium titanate composite anode material and its preparation and lithium battery |
| CN108448085A (en) * | 2018-03-09 | 2018-08-24 | 桑德集团有限公司 | Lithium titanate-carbon nano tube compound material and preparation method thereof, lithium ion battery |
| CN108574094A (en) * | 2018-05-09 | 2018-09-25 | 河北银隆新能源有限公司 | Negative material and preparation method thereof for lithium ion battery |
| CN109326788A (en) * | 2018-11-20 | 2019-02-12 | 青海大学 | Negative electrode material and lithium ion battery and preparation method thereof |
| CN109727784A (en) * | 2017-10-27 | 2019-05-07 | 北京碳阳科技有限公司 | Lithium titanate/carbon material compound, negative electrode material, negative electrode tab and hybrid super capacitor |
| CN109768264A (en) * | 2019-03-06 | 2019-05-17 | 浙江工业大学 | A kind of preparation method of lithium titanate composite anode material |
| CN110416537A (en) * | 2019-08-02 | 2019-11-05 | 广东东岛新能源股份有限公司 | Lithium titanate composite anode material and preparation method thereof and lithium ion battery |
| CN110429324A (en) * | 2019-08-05 | 2019-11-08 | 安徽相源新能源有限公司 | A kind of preparation method of the modified compound lithium cell of high capacity |
| CN110611078A (en) * | 2018-06-14 | 2019-12-24 | 浙江伏打科技有限公司 | Preparation method of lithium titanate-carbon nanotube electrode material |
| CN112736236A (en) * | 2021-01-15 | 2021-04-30 | 辽宁大学 | Novel biomass carbon-coated biphase Li serving as lithium ion battery negative electrode material4Ti5O12-TiO2And uses thereof |
| CN112736234A (en) * | 2021-01-15 | 2021-04-30 | 辽宁大学 | Novel lithium ion battery cathode material based on biomass/carbon nanotube composite modified lithium titanate and application thereof |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107275614A (en) * | 2017-06-26 | 2017-10-20 | 合肥国轩高科动力能源有限公司 | MoS2CNT lithium titanate composite anode material and its preparation and lithium battery |
| CN109727784A (en) * | 2017-10-27 | 2019-05-07 | 北京碳阳科技有限公司 | Lithium titanate/carbon material compound, negative electrode material, negative electrode tab and hybrid super capacitor |
| CN108448085A (en) * | 2018-03-09 | 2018-08-24 | 桑德集团有限公司 | Lithium titanate-carbon nano tube compound material and preparation method thereof, lithium ion battery |
| CN108574094A (en) * | 2018-05-09 | 2018-09-25 | 河北银隆新能源有限公司 | Negative material and preparation method thereof for lithium ion battery |
| CN110611078A (en) * | 2018-06-14 | 2019-12-24 | 浙江伏打科技有限公司 | Preparation method of lithium titanate-carbon nanotube electrode material |
| CN110611078B (en) * | 2018-06-14 | 2021-04-02 | 浙江伏打科技有限公司 | Lithium titanate-carbon nanotube composite material and preparation method thereof |
| CN109326788A (en) * | 2018-11-20 | 2019-02-12 | 青海大学 | Negative electrode material and lithium ion battery and preparation method thereof |
| CN109768264A (en) * | 2019-03-06 | 2019-05-17 | 浙江工业大学 | A kind of preparation method of lithium titanate composite anode material |
| CN110416537A (en) * | 2019-08-02 | 2019-11-05 | 广东东岛新能源股份有限公司 | Lithium titanate composite anode material and preparation method thereof and lithium ion battery |
| CN110416537B (en) * | 2019-08-02 | 2022-05-31 | 广东东岛新能源股份有限公司 | Lithium titanate composite negative electrode material, preparation method thereof and lithium ion battery |
| CN110429324A (en) * | 2019-08-05 | 2019-11-08 | 安徽相源新能源有限公司 | A kind of preparation method of the modified compound lithium cell of high capacity |
| CN112736236A (en) * | 2021-01-15 | 2021-04-30 | 辽宁大学 | Novel biomass carbon-coated biphase Li serving as lithium ion battery negative electrode material4Ti5O12-TiO2And uses thereof |
| CN112736234A (en) * | 2021-01-15 | 2021-04-30 | 辽宁大学 | Novel lithium ion battery cathode material based on biomass/carbon nanotube composite modified lithium titanate and application thereof |
| CN112736234B (en) * | 2021-01-15 | 2024-02-20 | 辽宁大学 | Novel lithium ion battery anode material based on biomass/carbon nanotube composite modified lithium titanate and application thereof |
| CN112736236B (en) * | 2021-01-15 | 2024-02-20 | 辽宁大学 | Novel lithium ion battery anode material biomass carbon coated diphasic Li 4 Ti 5 O 12 -TiO 2 And applications thereof |
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Application publication date: 20170613 |