CN108975388A - A kind of one-pot synthesis LiEuTiO4The method of lithium ion battery anode material - Google Patents
A kind of one-pot synthesis LiEuTiO4The method of lithium ion battery anode material Download PDFInfo
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Abstract
The invention discloses a kind of one pot process LiEuTiO4The method of lithium ion battery anode material.The LiEuTiO synthesized by this method4Lithium ion battery anode material, than the LiEuTiO using the substep synthetic method preparation being previously reported4Anode material has better chemical property.The technology of the present invention greatly optimizes the substep synthetic technology reported in the past, so that the generated time and cost of labor of the material are largely reduced, so that the material in following industrialization and commercialization process advantageously, with good application prospect.
Description
Technical field
The present invention relates to lithium ion battery anode material technical field more particularly to a kind of one-pot synthesis LiEuTiO4Lithium
The method of ion battery anode material.
Background technique
As coal, petroleum, natural gas this three big main energy sources reserves are increasingly reduced, and a series of environment thus caused
Problem is got growing concern for, it was recognized that keep the sustainable development of the mankind, the energy and environment are to enter 21 generation
Two serious problems that discipline must face, and develop and clean reproducible new energy, such as electrochemical energy storage and Hydrogen Energy, it will become
Most one of the technical field of decisive influence in world economy.So hot spot of the energy storage material at current research.
In electrochemical energy storage, lithium ion battery has the advantages that high voltage, high capacity and high-energy, and cycle life
Length has a safety feature, and keeps it many-sided with wide in portable electronic device, electric car, space technology, national defense industry etc.
Application prospect, become the research hotspot widely paid close attention in recent years, it is considered to be most promising energy storage device.
Graphite as anode material for lithium-ion battery on the market is held very much due to its lower insertion current potential (about 0.1V) at present
The Li dendrite problem of negative regions is easily caused, so as to cause safety problem.Recently the study found that Li4Ti5O12As negative electrode material
Possess higher insertion current potential, does not easily cause Li dendrite problem, but since its high insertion current potential causes the energy of battery close
The reduction of degree, to influence the energy density of battery.
Recently studies have found that lithium ion battery anode material LiEuTiO4Insertion current potential it is lower, about 0.8V, the electricity
Position is enough cell safety problem caused by avoiding the formation of Li dendrite, while also can guarantee that the energy density of lithium battery increases.To the greatest extent
Pipe LiEuTiO4The performance of material is very good, but the method for preparing the material reported at present is all complex, the material
Usually pass through lithium ion and NaEuTiO4In sodium ion exchange, by multistep synthesize obtain, preparation step is lengthy and tedious, preparation cost
It is very high.The industrial application higher cost for making the material in this way, to be commercialized difficulty.The one pot process material is used herein
Material, reduces manufacturing cost, so that its commercialization is advantageously.
Summary of the invention
The present invention uses liquid phase plasma body technique (SPT), anti-using liquid phase plasma with independent intellectual property rights
Device is answered (utility model patent: 201420301030.1), to pass through one pot process LiEuTiO4.Illustrate below the invention patent
In, pass through the LiEuTiO of one pot process4Referred to as are as follows: OSR-LiEuTiO4;According to the preparation of former report method multistep
LiEuTiO4Referred to as are as follows: MSR-LiEuTiO4.OSR-LiEuTiO prepared by the present invention4Show preferable chemical property.
When in 0.01-3V voltage range with 0.1Ag-1When circulation, discharge capacity is 237.3mAhg for the first time-1, and followed at 100 times
There is good capacity retention ratio 97.0% after ring.In addition, it is in 5 Ag-1When have 156.2 mAhg-1Height ratio capacity.
The present invention adopts the following technical scheme that:
(1) by LiCl, EuCl3Titanium (TALH), which is closed, with two (2 hydroxy propanoic acid) two hydroxide diammoniums is blended and dissolved in chlorination 1- fourth
In the ionic liquid of base -3- methylimidazole ([BMIM] Cl), it is transferred in liquid phase plasma reactor according;
(2) by O2It is passed through in solution;
(3) it carries out liquid phase plasma precursor reactant 30 minutes, is vigorously stirred simultaneously.Between two electrodes of liquid phase plasma reactor according
Electric field be 750Vcm-1;
(4) products therefrom is washed repeatedly with deionized water;
(5) it is dry at 80 DEG C.
The amount of [BMIM] Cl liquid is 20mL in step (1);
The amount of LiCl is 2 mmol in step (1);
EuCl in step (1)3Amount be 1 mmol;
The amount of TALH is 1 mmol in step (1);
O in step (2)2Flow velocity is 5mLmin-1;
Electric field in step (3) between two electrodes of liquid phase plasma reactor according is 750Vcm-1;
The reaction time is 30min in step (3).
The positive effect of the present invention is as follows:
1) present invention goes out OSR-LiEuTiO using one pot process4Anode of lithium cell material, with the preparation reported at present
LiEuTiO4The method of anode material is compared, and this method operating procedure is simple, time-consuming short to be more conducive to its industrialization.
2) LiEuTiO prepared by the present invention4Anode of lithium cell material, performance were better than according to former report method multistep system
Standby MSR-LiEuTiO4The LiEuTiO reported at present4Anode material (Chem. Commun. 2017;53:7800-3).
Detailed description of the invention
Fig. 1 is the OSR-LiEuTiO of 1 one-pot synthesis of embodiment4The XRD diffraction refine knot of lithium ion battery anode material
Fruit.
Fig. 2 is the OSR-LiEuTiO of 1 one-pot synthesis of embodiment4The Ti 2p XPS map of lithium ion battery anode material
(a) and Eu 3d XPS map (b).
Fig. 3 is the OSR-LiEuTiO of 1 one-pot synthesis of embodiment4The SEM photograph of lithium ion battery anode material.
Fig. 4 is the MSR-LiEuTiO prepared according to former report method multistep4The SEM of lithium ion battery anode material shines
Piece.
Fig. 5 is the OSR-LiEuTiO of 1 one-pot synthesis of embodiment4Lithium ion battery anode material and according to former report side
The MSR-LiEuTiO of fado step preparation4It is 1mVs in sweep speed-1When cyclic voltammogram;.
Fig. 6 is the OSR-LiEuTiO of 1 one-pot synthesis of embodiment4Lithium ion battery anode material and according to former report side
The MSR-LiEuTiO of fado step preparation4It is 0.1 Ag in multiplying power-1When discharge curve for the first time.
Fig. 7 is the OSR-LiEuTiO of 1 one-pot synthesis of embodiment4Lithium ion battery anode material and according to former report side
The MSR-LiEuTiO of fado step preparation4It is 0.1 Ag in multiplying power-1When cycle performance figure.
Fig. 8 is the OSR-LiEuTiO of 1 one-pot synthesis of embodiment4Lithium ion battery anode material and according to former report side
The MSR-LiEuTiO of fado step preparation4Cycle performance figure under different multiplying
Fig. 9 is the OSR-LiEuTiO of 1 one-pot synthesis of embodiment4Lithium ion battery anode material and LiEuTiO reported in the literature4
Material (Chem. Commun. 2017;53:7800-3) performance under different multiplying compares figure.
Specific embodiment
The following examples are a further detailed description of the invention.
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment 1
To achieve the above object, the LiEuTiO of one-pot synthesis4The preparation step of lithium ion battery anode material are as follows:
1) by 2 mmol LiCl, 1 mmol EuCl3Titanium (TALH) is closed with 1 mmol bis- (2 hydroxy propanoic acid), two hydroxide diammonium
It is blended and dissolved in the ionic liquid of 20 mL chlorination 1- butyl -3- methylimidazoles ([BMIM] Cl), is transferred to liquid phase plasma
In reactor according;
2) by O2It is passed through in solution.O2Flow velocity is 5mLmin-1;
3) it carries out liquid phase plasma precursor reactant 30 minutes, is vigorously stirred simultaneously.Between two electrodes of liquid phase plasma reactor according
Electric field be 750Vcm-1;
4) products therefrom is washed repeatedly with deionized water;
5) it is dry at 80 DEG C.
OSR-LiEuTiO prepared by embodiment 14Experiment and calculating XRD spectrum it is shown in Figure 1.A, b and c lattice
Parameter is respectively 1.13971,0.53593 and 0.53580 nm.Its with it is reported in the literature consistent.Ti 2p and the Eu 3d of sample
XPS spectrum is as shown in Fig. 2 a and b.The peak XPS outstanding corresponds respectively to Eu at 1165.0 and 1135.0eV3+ 3d3/2And Eu3+
3d5/2(3d4f6), show OSR-LiEuTiO4The oxidation state of middle Eu is+3.Meanwhile the valence state of Ti is+4, two of them peak difference
For 465.3 and 459.6eV, Ti is corresponded respectively to4+ 2p1/2And Ti4+ 2p3/2。
SEM image in Fig. 3 shows OSR-LiEuTiO4It is average grain diameter uniform and with about 160nm, it is small
In us according to LiEuTiO prepared by report multistep synthetic method before4(MSR-LiEuTiO4) (Fig. 4) average grain
Diameter.In addition, it has 121.3 m2g-1High-specific surface area, be greater than MSR-LiEuTiO4(16.6 m2g-1) specific surface area.Cause
This, OSR-LiEuTiO4It is expected to be used as cathode material for high capacity lithium ion battery, because of its high-specific surface area and smaller grain
Diameter will promote the infiltration of electrolyte and shorten ion/electrons spread distance.
In addition to this, it is investigated OSR-LiEuTiO4As the anode material of lithium ion battery (LIB), MSR- is used
LiEuTiO4It is compared.Cyclic voltammogram shows OSR-LiEuTiO4It shows to compare MSR-LiEuTiO4Better Li+Storage
Performance (Fig. 5).Two peaks near 0.8V and 1.0V correspond respectively to Li+Intercalation/deintercalation peak.OSR-LiEuTiO4It is lower
Li+Deviate from current potential and its higher Li+Insertion current potential shows its Li during circulation+Intercalation/deintercalation invertibity ratio MSR-
LiEuTiO4More preferably.In addition, OSR-LiEuTiO4The area of cyclic voltammetry curve is much higher than MSR-LiEuTiO4, show that it has
Higher capacity.
Fig. 6 is two kinds of samples in 0.1 Ag-1Initial charge/discharge curve under charge-discharge magnification.MSR-LiEuTiO4It is initial
Discharge capacity is 74.8mAhg-1, reversible charging capacity is 55.6mAhg-1.Its irreversible capacitance loss reaches 26.7%.
In addition, OSR-LiEuTiO4Initial discharge capacity be 237.3mAhg-1, it is greater than the LiEuTiO being previously reported4
(219.2mAhg-1) maximum specific capacity (Chem. Commun. 2017;53:7800-3).In addition, the initial charge of sample is held
Amount is 213.8mAhg-1, initial capacity loss is only 10.1%.OSR-LiEuTiO4Good Li+Storge quality is attributable to it
Higher specific surface area.
Fig. 7 shows two kinds of samples in 0.1Ag-1Cycle performance under charge-discharge magnification.After 75 circulations, MSR-
LiEuTiO4Reversible capacity be only 39.2 mAhg-1, capacitance loss 22.0%.In contrast, OSR-LiEuTiO4Even if
It is also showed that lower capacity attenuation (10.0%) after 100 circulations, and reversible capacity is 208.7mAhg-1。
Fig. 8 compares two kinds of samples in 0.2-5.0Ag-1Rate capability under charge-discharge magnification.OSR-LiEuTiO4Can
Inverse capacity is in 0.2 Ag-1When be 204.3 mAhg-1, in 5.0 Ag-1When be 144.9mAhg-1.Coulombic efficiency is about accordingly
92.7%.And MSR-LiEuTiO4In 0.2 Ag-1In the case of capacity be only 45.9mAhg-1, in 5.0 Ag-1Lower capacity is only
7.2mAhg-1.This significant difference between two kinds of materials, especially at the high velocities, this is attributed to OSR-LiEuTiO4Compared with
Small particle and high specific surface area, make Li+With electronics in LiEuTiO4There is faster diffusion rate in body phase.When charge and discharge times
Rate becomes 0.1 Ag again-1When, specific capacity is restored to 213.8 mAhg-1.In addition, the OSR-LiEuTiO prepared by us4Charge and discharge times
Rate performance is also superior to LiEuTiO reported in the literature4(Chem. Commun. 2017;53:7800-3) (Fig. 9).
The present invention is successfully prepared LiEuTiO using one kettle way4Lithium ion battery anode material.The material has been reported with other
The li-ion electrode materials led, which are compared, has better chemical property.The preparation method of the material and the method phase reported in the past
Than step simplifies many, and time-consuming is short, advantageously the industrialization of the beneficial material and commercialized development.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (8)
1. a kind of one-pot synthesis LiEuTiO4The method of lithium ion battery anode material, it is characterised in that:
Specific step is as follows for synthetic method:
By 2 mmol LiCl, 1 mmol EuCl3Titanium (TALH) mixing is closed with 1 mmol bis- (2 hydroxy propanoic acid), two hydroxide diammonium
And be dissolved in the ionic liquid of 20 mL chlorination 1- butyl -3- methylimidazoles ([BMIM] Cl), it is anti-to be transferred to liquid phase plasma
It answers in device;
By O2It is passed through in solution, O2Flow velocity is 5mLmin-1;
It carries out liquid phase plasma precursor reactant 30 minutes, is vigorously stirred simultaneously, between two electrodes of liquid phase plasma reactor according
Electric field is 750Vcm-1;
Products therefrom is washed repeatedly with deionized water;
Drying at 80 DEG C by it.
2. a kind of one-pot synthesis LiEuTiO as described in claim 14The method of lithium ion battery anode material, feature exist
In: the amount of [BMIM] Cl liquid is 20mL in step (1).
3. a kind of one-pot synthesis LiEuTiO as described in claim 14The method of lithium ion battery anode material, feature exist
In: the amount of LiCl is 2mmol in step (1).
4. a kind of one-pot synthesis LiEuTiO as described in claim 14The method of lithium ion battery anode material, feature exist
In: EuCl in step (1)3Amount be 1mmol.
5. a kind of one-pot synthesis LiEuTiO as described in claim 14The method of lithium ion battery anode material, feature exist
In: the amount of TALH is 1mmol in step (1).
6. a kind of one-pot synthesis LiEuTiO as described in claim 14The method of lithium ion battery anode material, feature exist
In: O in step (2)2Flow velocity is 5mLmin-1。
7. a kind of one-pot synthesis LiEuTiO as described in claim 14The method of lithium ion battery anode material, feature exist
In: the reaction time is 30min in step (3).
8. a kind of one-pot synthesis LiEuTiO as described in claim 14The method of lithium ion battery anode material, feature exist
In: the electric field in step (3) between two electrodes of liquid phase plasma reactor according is 750Vcm-1。
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Cited By (2)
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CN110451558A (en) * | 2019-08-14 | 2019-11-15 | 成都理工大学 | A kind of preparation method of amorphous LiEuTiO4 nano vesicle |
CN111370676A (en) * | 2020-03-24 | 2020-07-03 | 电子科技大学 | Method for preparing three-dimensional porous carbon doped lithium titanate coating on surface of copper foil |
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CN106927545A (en) * | 2017-03-29 | 2017-07-07 | 成都理工大学 | The preparation method of the mesoporous amorphous B N O H nano materials of foam-like |
CN107164773A (en) * | 2016-03-07 | 2017-09-15 | 南通欧冶新材料有限公司 | A kind of TiAl intermetallic compound is electrolysed plasma surface technology for modifying |
CN107840362A (en) * | 2017-10-11 | 2018-03-27 | 成都理工大学 | Ultra-thin LiEuTiO4The preparation method of nanometer chip base layering microballoon |
CN108117096A (en) * | 2016-11-29 | 2018-06-05 | 丰田自动车株式会社 | Lithium ion battery negative material and negative electrode of lithium ion battery |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107164773A (en) * | 2016-03-07 | 2017-09-15 | 南通欧冶新材料有限公司 | A kind of TiAl intermetallic compound is electrolysed plasma surface technology for modifying |
CN108117096A (en) * | 2016-11-29 | 2018-06-05 | 丰田自动车株式会社 | Lithium ion battery negative material and negative electrode of lithium ion battery |
CN106927545A (en) * | 2017-03-29 | 2017-07-07 | 成都理工大学 | The preparation method of the mesoporous amorphous B N O H nano materials of foam-like |
CN107840362A (en) * | 2017-10-11 | 2018-03-27 | 成都理工大学 | Ultra-thin LiEuTiO4The preparation method of nanometer chip base layering microballoon |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110451558A (en) * | 2019-08-14 | 2019-11-15 | 成都理工大学 | A kind of preparation method of amorphous LiEuTiO4 nano vesicle |
CN111370676A (en) * | 2020-03-24 | 2020-07-03 | 电子科技大学 | Method for preparing three-dimensional porous carbon doped lithium titanate coating on surface of copper foil |
CN111370676B (en) * | 2020-03-24 | 2022-05-03 | 电子科技大学 | Method for preparing three-dimensional porous carbon doped lithium titanate coating on surface of copper foil |
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