CN106207149A - A kind of method preparing submicron order lithium titanate material - Google Patents
A kind of method preparing submicron order lithium titanate material Download PDFInfo
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- CN106207149A CN106207149A CN201510217782.9A CN201510217782A CN106207149A CN 106207149 A CN106207149 A CN 106207149A CN 201510217782 A CN201510217782 A CN 201510217782A CN 106207149 A CN106207149 A CN 106207149A
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Abstract
The invention provides a kind of method preparing submicron order lithium titanate material, this method includes preparing Li with sol-gal process4Ti5O12Precursor solution, electrostatic spinning obtains sub-micron fibers Li4Ti5O12Presoma, under air atmosphere, calcining obtains the nano lithium titanate fiber of submicron.The advantages such as the method technique that the present invention provides is simple, spinning is with low cost, technique is controlled, the high and good processability to prepared submicron lithium titanate material tap density.
Description
Technical field
The present invention relates to lithium ion battery negative material, be specifically related to one and prepare submicron order lithium titanate anode
The method of material.
Background technology
The performance of lithium ion battery depends on positive and negative pole material, Li4Ti5O12" zero is had as cell negative electrode material
Strain ", features such as cycle performance is highly stable, and its surface is formed without passivating film, it is to avoid lithium metal is brilliant
The formation of branch, security performance is better than carbon negative pole material, and its electrochemical diffusion coefficient than carbon negative pole material big 1 number
Magnitude, charge/discharge rates is quickly.Additionally, Li4Ti5O12Synthesis material enrich, environmentally safe.
Electrostatic spinning technique technique is simple, cheap for manufacturing cost, can quickly obtain distribution of fiber diameters from several nanometers
To several microns and superfine fibre various in style, also it is to be recognized batch production to manufacture nano-fiber material potentiality
One of important method.What method of electrostatic spinning was prepared has the nano-fiber material of 3-D solid structure, not only
Possessing the characteristics such as nanoparticle size is small, specific surface area is big, it also has that mechanical stability is good, fiber simultaneously
The advantages such as membrane aperture is little, porosity is high, fiber seriality is good, thus can basic as nano science total number
Construct primitive, be widely used in the fields such as information, the energy, environment, biomedicine, national security.
Summary of the invention
It is an object of the invention to provide one and prepare submicron order Li4Ti5O12The method of negative material, passes through
Electrostatic spinning assisting sol gel technique, obtains a kind of uniform diameter and the submicron Li not reunited4Ti5O12Fine
Dimension negative material.
It is an object of the invention to the realization of following technical scheme:
The method preparing submicron order lithium titanate material that the present invention provides, this method comprises the steps:
A. prepare solution A: with from PVP (polyvinylpyrrolidone), PVB (polyvinyl butyral resin),
DMF (DMF), PAN (polyacrylonitrile), PVA (polyvinyl alcohol), PLA (gather
Lactic acid), a kind of polymer of selecting in one group of polymer forming of PEO (poly(ethylene oxide)) be dissolved in dehydrated alcohol system
Standby mass concentration is the solution A of 0.02～0.2g/mL；
B. solution B is prepared:
1) from lithium acetate, EINECS 212-761-8, isopropyl lithium alkoxide, lithium nitrate, lithium carbonate, Lithium Citrate de, lithium chloride,
Lithium oxalate, long-chain or short-chain alkyl lithium are selected a kind of lithium compound and is dissolved in dehydrated alcohol and makes mass concentration and be
0.03g～0.2g/mL solution；
2) again in the ratio of Li:Ti=0.8～1.0:1 in step 1) gained solution adds from tetraisopropyl titanate,
A kind of titanium compound selected in the chloride of titanium, butyl titanate, and add the acid hydrolysis as titanium compound
Inhibitor, obtained solution B；
C. precursor solution: be 4～6:5 to mix homogeneously and obtain presoma with volume ratio by solution A and B solution
Solution；
D. precursor solution is carried out electrostatic spinning, obtain 0.2～1.8mm thick white film, dry under room temperature
Dry stable.
E., under air atmosphere, prepared described thin film is calcined in Muffle furnace, obtains the nanometer of submicron
Lithium titanate fiber.
In first optimal technical scheme of the described method preparing submicron order lithium titanate material, institute in step a
The polymer stated is PVP (polyvinylpyrrolidone), PVB (polyvinyl butyral resin) or DMF (N,
Dinethylformamide).
In second optimal technical scheme of the described method preparing submicron order lithium titanate material, institute in step a
The molecular weight of the polymer stated is 360000-1300000；
In 3rd optimal technical scheme of the described method preparing submicron order lithium titanate material, institute in step b
The lithium compound stated is lithium acetate, EINECS 212-761-8, Lithium Citrate de, lithium chloride, lithium oxalate, long-chain or short-chain alkyl
Lithium.
In 4th optimal technical scheme of the described method preparing submicron order lithium titanate material, institute in step b
The titanium compound stated is tetraisopropyl titanate or butyl titanate.
In 5th optimal technical scheme of the described method preparing submicron order lithium titanate material, institute in step b
The lithium compound stated is Li:Ti=0.8～0.9:1 with the mol ratio of titanium compound.
In 6th optimal technical scheme of the described method preparing submicron order lithium titanate material, institute in step b
The acid stated is nitric acid, hydrochloric acid, acetic acid, tartaric acid, oxalic acid, malic acid, citric acid, ascorbic acid, benzene first
One in acid, salicylic acid, caffeic acid or a combination thereof.
In 7th optimal technical scheme of the described method preparing submicron order lithium titanate material, institute in step b
The volume ratio stating acid and dehydrated alcohol is 1～2:4.
In 8th optimal technical scheme of the described method preparing submicron order lithium titanate material, institute in step d
The technological parameter stating electrostatic spinning is: flow is 1.5～2.5mL/h；Running voltage is 8～25KV, receives plate
Distance is 5～15cm.
In 9th optimal technical scheme of the described method preparing submicron order lithium titanate material, institute in step e
The condition stating calcining is: calcining heat 600～800 DEG C；Calcination time is 4-12h；Heating rate is 1～5 DEG C
/min。
Comparing with immediate prior art, the technical scheme that the present invention provides has a following excellent effect:
1) technological operation of the inventive method is simple, spinning is with low cost, and manufacturing cycle is only 32-36h；
2) lithium titanate fibre diameter can be accurately controlled by the inventive method, forms Li4Ti5O12Granule
Homodisperse unique nanofibrous structures, hence it is evident that improve the particle agglomeration phenomenon of material, it is possible to more give full play to
The charge-discharge performance of lithium titanate material, multiplying power property；
3) pure phase submicron order lithium titanate fibrous material prepared by the inventive method has more preferable tap density,
Materials processing performance is substantially better than nano material, the technique controlling difficulty in electrode slurry modulation, coating procedure
Nano material relatively substantially reduces, and the hygroscopicity of submicron material is significantly less than nano material, reduces electricity
The environmental Kuznets Curves cost of pond production and energy consumption.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the lithium titanate prepared by distinct methods, wherein (a) solid phase method, (b) hydro-thermal
Method, (c) sol-gal process, (d) the inventive method (embodiment 6)；
Fig. 2 is the XRD figure of lithium titanate prepared by embodiment of the present invention 3-6；
Fig. 3 is the SEM figure of lithium titanate prepared by embodiment of the present invention 3-6, wherein (a) embodiment 3, (b)
Embodiment 4, (c) embodiment 5, (d) embodiment 6；
Fig. 4 is embodiment of the present invention 3-6 product specific capacity result under different multiplying, and wherein PVP adds
Amount 1g, 2g, 3g, 4g the most corresponding embodiment 3, embodiment 4, embodiment 5, the product of embodiment 6.
Detailed description of the invention
Elaborating embodiments of the invention below, the present embodiment is carried out premised on technical solution of the present invention
Implement, give detailed embodiment and concrete operating process, but under protection scope of the present invention is not limited to
The embodiment stated.
Embodiment 1
2.0g polyvinylpyrrolidone (PVP 360000) is put in 20mL dehydrated alcohol, stirring until
It is completely dissolved, obtains solution A.5.15g anhydrous lithium acetate is joined 10mL dehydrated alcohol and 20mL vinegar
In acid, stirring is until being completely dissolved, according still further to the mol ratio of Li:Ti=4:5, by 3.382g tetraisopropyl titanate
Being slowly dropped in the lithium acetate solution prepared, stirring, until solution clarification, obtains solution B；By solution A
Mix with the volume ratio of 4:5 with solution B, stir 1 hour under room temperature, obtain electrostatic spinning precursor solution,
Precursor solution viscosity is 52cP.
Arranging electrostatic spinning process parameter: flow is 1.5mL/h, running voltage is 12KV, receives plate distance
For 10cm.Carry out after electrostatic spinning obtains 1.8mm white film, in air atmosphere, with Muffle furnace 800 DEG C
High-temperature calcination obtains lithium titanate fibrous material in 5 hours.
Above-mentioned submicron lithium titanate fibrous material, a diameter of 260nm, a length of 10-30um, 0.1C discharge
Capacity be 171.22mAh/g, 5C discharge capacity be 108.23mAh/g.
Embodiment 2
2.0g polyvinyl butyral resin (PVP 360000) is put in 20mL dehydrated alcohol, stirring until
It is completely dissolved, obtains solution A.5.15g anhydrous lithium acetate is joined 6mL dehydrated alcohol and 20mL acetic acid
In, 18.2g tetraisopropyl titanate, until being completely dissolved, according still further to the mol ratio of Li:Ti=4:5, is delayed by stirring
Slowly being added drop-wise in the lithium acetate solution prepared, stirring, until solution clarification, obtains solution B；By solution A
Mix with the volume ratio of 6:5 with solution B, stir 1 hour under room temperature, obtain electrostatic spinning solution, presoma
Solution viscosity is 65cP.
Arranging electrostatic spinning process parameter is: flow is 2.5mL/h, and running voltage is 15KV, receive plate away from
From for 15cm.Carry out after electrostatic spinning obtains 1.5mm white film, in air atmosphere, with Muffle furnace 600 DEG C
High-temperature calcination obtains lithium titanate fibrous material in 8 hours.
Above-mentioned submicron lithium titanate fibrous material, a diameter of 220nm, a length of 5-30um, 0.1C discharge
Capacity be 173.01mAh/g, 5C discharge capacity be 110.58mAh/g.
Embodiment 3
Joining in 30mL dehydrated alcohol by 1.0g polyvinylpyrrolidone (PVP 360000), stirring is straight
To being completely dissolved, obtain solution A.1.666g anhydrous lithium acetate is joined 5mL dehydrated alcohol and 10mL
In acetic acid, stirring is until being completely dissolved, according still further to the mol ratio of Li:Ti=4.28:5, by different for 8.382g metatitanic acid four
Propyl ester is slowly dropped in the lithium acetate solution prepared, and stirring, until solution clarification, obtains solution B；By molten
Liquid A mixes with the volume ratio of 1:1 with solution B, stirs 1 hour, obtain electrostatic spinning presoma under room temperature
Solution, precursor solution viscosity is 11cP.
Arranging electrostatic spinning process parameter: flow is 1.5mL/h, running voltage is 15KV, receives plate distance
For 10cm.Carry out after electrostatic spinning obtains 1.8mm white film, in air atmosphere, with Muffle furnace 800 DEG C
High-temperature calcination obtains lithium titanate fibrous material in 12 hours.
Above-mentioned submicron lithium titanate fibrous material, in XRD figure such as Fig. 2 shown in (a), without any dephasign.
A diameter of 230nm, a length of 20-30um, in Electronic Speculum figure such as Fig. 3 shown in (a), 0.1C discharge capacity is
198.50mAh/g, 10C discharge capacity is 75.11mAh/g.
Embodiment 4
Joining in 30mL dehydrated alcohol by 2.0g polyvinylpyrrolidone (PVP 360000), stirring is straight
To being completely dissolved, obtain solution A.1.666g anhydrous lithium acetate is joined 5mL dehydrated alcohol and 10mL
In acetic acid, stirring is until being completely dissolved, according still further to the mol ratio of Li:Ti=4.28:5, by different for 8.382g metatitanic acid four
Propyl ester is slowly dropped in the lithium acetate solution prepared, and stirring, until solution clarification, obtains solution B；By molten
Liquid A mixes with the volume ratio of 1:1 with solution B, stirs 1 hour, obtain electrostatic spinning presoma under room temperature
Solution, precursor solution viscosity is 38cP.
Arranging electrostatic spinning process parameter: flow is 1.5mL/h, running voltage is 15KV, receives plate distance
For 10cm, carry out after electrostatic spinning obtains 1.8mm white film, in air atmosphere, with Muffle furnace 800 DEG C
High-temperature calcination obtains lithium titanate fibrous material in 12 hours.
Above-mentioned submicron lithium titanate fibrous material, in XRD figure such as Fig. 2 shown in (b), without any dephasign.
A diameter of 270nm, a length of 30-45um, in Electronic Speculum figure such as Fig. 3 shown in (b).0.1C discharge capacity is
170.51.54mAh/g, 10C discharge capacity is 81.22mAh/g.
Embodiment 5
Joining in 30mL dehydrated alcohol by 3.0g polyvinylpyrrolidone (PVP 360000), stirring is straight
To being completely dissolved, obtain solution A.1.666g anhydrous lithium acetate is joined 5mL dehydrated alcohol and 10mL
In acetic acid, stirring is until being completely dissolved, according still further to the mol ratio of Li:Ti=4.28:5, by different for 8.382g metatitanic acid four
Propyl ester is slowly dropped in the lithium acetate solution prepared, and stirring, until solution clarification, obtains solution B；By molten
Liquid A mixes with the volume ratio of 1:1 with solution B, stirs 1 hour, obtain electrostatic spinning presoma under room temperature
Solution, precursor solution viscosity is 74cP.
Arranging electrostatic spinning process parameter: flow is 1.5mL/h, running voltage is 15KV, receives plate distance
For 10cm.Carry out after electrostatic spinning obtains 1.8mm white film, in air atmosphere, with Muffle furnace 800 DEG C
High-temperature calcination obtains lithium titanate fibrous material in 12 hours.
Above-mentioned submicron lithium titanate fibrous material, in XRD figure such as Fig. 2 shown in (c), without any dephasign.
A diameter of 3600nm, a length of 50-60um, in Electronic Speculum figure such as Fig. 3 shown in (c).0.1C discharge capacity is
148.33mAh/g, 2C discharge capacity is 118.43mAh/g.
Embodiment 6
Joining in 30mL dehydrated alcohol by 4.0g polyvinylpyrrolidone (PVP 360000), stirring is straight
To being completely dissolved, obtain solution A.1.666g anhydrous lithium acetate is joined 5mL dehydrated alcohol and 10mL
In acetic acid, stirring is until being completely dissolved, according still further to the mol ratio of Li:Ti=4.28:5, by different for 8.382g metatitanic acid four
Propyl ester is slowly dropped in the lithium acetate solution prepared, and stirring, until solution clarification, obtains solution B；By molten
Liquid A mixes with the volume ratio of 1:1 with solution B, stirs 1 hour, obtain electrostatic spinning presoma under room temperature
Solution, precursor solution viscosity is 117cP.
Arranging electrostatic spinning process parameter: flow is 1.5mL/h, running voltage is 15KV, receives plate distance
For 10cm.Carry out after electrostatic spinning obtains 1.8mm white film, in air atmosphere, with Muffle furnace 800 DEG C
High-temperature calcination obtains lithium titanate fibrous material in 12 hours.
Above-mentioned submicron lithium titanate fibrous material, in XRD figure such as Fig. 2 shown in (d), without any dephasign.
A diameter of 560nm, a length of 90-100um, in Electronic Speculum figure such as Fig. 3 shown in (d).0.1C discharge capacity is
171.46mAh/g。
In Fig. 4, embodiment 3-6 gained lithium titanate material is under the multiplying power of 0.1C～10C changes, and specific capacity is all
Being gradually reduced, under same multiplying power, specific capacity has a declining tendency along with PVP addition increase.This says
Bright along with the increase of PVP addition, spun filament diameter becomes larger, and specific surface area is relatively reduced,
Thus lithium ion displacement becomes big, thus specific capacity declines.
Submicron lithium titanate prepared by above-described embodiment, preparation process is relatively simple, and effectively prevent granule
Reuniting, the negative material obtained all has preferable chemical property, can obtain under the conditions of high power charging-discharging
Discharge capacity that must be higher, cycle performance is the most highly stable simultaneously.Under room temperature condition, during 1C multiplying power, it is first
Discharge capacity has reached 174.15mAh/g, and during 20C, discharge capacity also reaches 110.53mAh/g, it is anticipated that should
Preparation method produces the submicron lithium titanate of gained and has higher commercial application value.
It is more than the section Example of the present invention, although present disclosure is made by above-mentioned section Example
It is discussed in detail, but it should be appreciated that the description above is not considered as limitation of the present invention.In this area
After technical staff has read foregoing, multiple amendment and replacement for the present invention all will be apparent from.
Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (10)
1. the method preparing submicron order lithium titanate material, this method comprises the steps:
A. solution A is prepared: be dissolved in dehydrated alcohol with a kind of polymer selected from one group of polymer that PVP (polyvinylpyrrolidone), PVB (polyvinyl butyral resin), DMF (DMF), PAN (polyacrylonitrile), PVA (polyvinyl alcohol), PLA (polylactic acid), PEO (poly(ethylene oxide)) form and prepare the solution A that mass concentration is 0.02～0.2g/mL；
B. solution B is prepared:
1) selecting a kind of lithium compound from lithium acetate, EINECS 212-761-8, isopropyl lithium alkoxide, lithium nitrate, lithium carbonate, Lithium Citrate de, lithium chloride, lithium oxalate, long-chain or short-chain alkyl lithium and be dissolved in dehydrated alcohol to make mass concentration is 0.03g～0.2g/mL solution；
2) again in the ratio of Li:Ti=0.8～1.0:1 in step 1) solution of gained adds a kind of titanium compound selected from tetraisopropyl titanate, the chloride of titanium, butyl titanate, and add the hydrolysis inhibitor acid as described titanium compound, obtained solution B；
C. precursor solution: solution A and B solution are mixed to get precursor solution with the ratio that volume ratio is 4～6:5；
D. described precursor solution is carried out electrostatic spinning, obtain 0.2～1.8mm thick white film, be dried under room temperature；
E. under air atmosphere, prepared described thin film is calcined in Muffle furnace, obtain the nano lithium titanate fiber of submicron.
The method preparing submicron order lithium titanate material the most according to claim 1, it is characterized in that the polymer described in step a be PVP (polyvinylpyrrolidone), PVB (polyvinyl butyral resin) or DMF (DMF).
The method preparing submicron order lithium titanate material the most according to claim 1, it is characterised in that the molecular weight of the polymer described in step a is 360000-1300000.
The method preparing submicron order lithium titanate material the most according to claim 1, it is characterised in that the lithium compound described in step b is lithium acetate, EINECS 212-761-8, Lithium Citrate de, lithium chloride, lithium oxalate, long-chain or short-chain alkyl lithium.
The method preparing submicron order lithium titanate material the most according to claim 1, it is characterised in that the titanium compound described in step b is tetraisopropyl titanate or butyl titanate.
The method preparing submicron order lithium titanate material the most according to claim 1, it is characterised in that the lithium compound described in step b is Li:Ti=0.8～0.9:1 with the mol ratio of titanium compound.
The method preparing submicron order lithium titanate material the most according to claim 1, it is characterised in that the acid described in step b is the one in nitric acid, hydrochloric acid, acetic acid, tartaric acid, oxalic acid, malic acid, citric acid, ascorbic acid, benzoic acid, salicylic acid, caffeic acid or a combination thereof.
The method preparing submicron order lithium titanate material the most according to claim 1, it is characterised in that acid described in step b is 1～2:4 with the volume ratio of dehydrated alcohol.
The method preparing submicron order lithium titanate material the most according to claim 1, it is characterised in that the technological parameter of electrostatic spinning described in step d is: flow is 1.5～2.5mL/h；Running voltage is 8～25KV, and receiving plate distance is 5～15cm.
The method preparing submicron order lithium titanate material the most according to claim 1, it is characterised in that described in step e, the condition of calcining is: calcining heat 600～800 DEG C；Calcination time is 4-12h；Heating rate is 1～5 DEG C/min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107176622A (en) * | 2017-04-28 | 2017-09-19 | 中国电力科学研究院 | A kind of lithium titanate material and preparation method thereof |
| CN107706408A (en) * | 2017-08-17 | 2018-02-16 | 中国第汽车股份有限公司 | A kind of preparation method of nanofiber lithium titanate composite material |
| CN109590463A (en) * | 2018-12-18 | 2019-04-09 | 浙江中杭新材料科技有限公司 | A kind of preparation method of high-coercive force neodymium iron boron magnetic body |
| CN109637767A (en) * | 2018-12-18 | 2019-04-16 | 浙江中杭新材料科技有限公司 | A kind of sintering method of neodymium iron boron magnetic body |
| CN113707871A (en) * | 2021-09-02 | 2021-11-26 | 和也健康科技有限公司 | Preparation of nanobelt lithium titanate @ stone needle composite fiber material, product and application |
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| US20110049769A1 (en) * | 2008-05-06 | 2011-03-03 | Jiri Duchoslav | Method for production of inorganic nanofibres through electrostatic spinning |
| CN102820460A (en) * | 2012-08-20 | 2012-12-12 | 上海交通大学 | Electrostatic spinning method for preparing rare-earth metal doped nanometer lithium titanate |
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- 2015-04-30 CN CN201510217782.9A patent/CN106207149A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110049769A1 (en) * | 2008-05-06 | 2011-03-03 | Jiri Duchoslav | Method for production of inorganic nanofibres through electrostatic spinning |
| CN102820460A (en) * | 2012-08-20 | 2012-12-12 | 上海交通大学 | Electrostatic spinning method for preparing rare-earth metal doped nanometer lithium titanate |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107176622A (en) * | 2017-04-28 | 2017-09-19 | 中国电力科学研究院 | A kind of lithium titanate material and preparation method thereof |
| CN107706408A (en) * | 2017-08-17 | 2018-02-16 | 中国第汽车股份有限公司 | A kind of preparation method of nanofiber lithium titanate composite material |
| CN109590463A (en) * | 2018-12-18 | 2019-04-09 | 浙江中杭新材料科技有限公司 | A kind of preparation method of high-coercive force neodymium iron boron magnetic body |
| CN109637767A (en) * | 2018-12-18 | 2019-04-16 | 浙江中杭新材料科技有限公司 | A kind of sintering method of neodymium iron boron magnetic body |
| CN109637767B (en) * | 2018-12-18 | 2020-08-21 | 浙江中杭新材料科技有限公司 | Sintering method of neodymium iron boron magnet |
| CN109590463B (en) * | 2018-12-18 | 2021-03-09 | 浙江中杭新材料科技有限公司 | Preparation method of high-coercivity neodymium-iron-boron magnet |
| CN113707871A (en) * | 2021-09-02 | 2021-11-26 | 和也健康科技有限公司 | Preparation of nanobelt lithium titanate @ stone needle composite fiber material, product and application |
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Application publication date: 20161207 |