CN107742716A - A kind of electrode material of lithium ion battery and preparation method thereof - Google Patents
A kind of electrode material of lithium ion battery and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
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- 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
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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Abstract
The invention belongs to electrochemistry, materials chemistry and electrochmical power source product technical field, more particularly, to a kind of electrode material of lithium ion battery and preparation method thereof.The chemical formula of electrode material provided by the present invention is MNb11O29, the M is Al, Ga or Cr.Electrode material provided by the invention has the advantages that theoretical specific capacity is high, security performance is high, reversible specific capacity is high, coulombic efficiency is high and cycle performance is excellent as lithium ion battery negative material.Preparation method synthesis technique provided by the invention is simple, suitable for the high power device discharge and recharge such as electric automobile, is had broad application prospects in field of lithium ion battery.The present invention provides more choices for M Nb O materials for lithium ion battery negative material, is had broad application prospects in lithium ion battery for electric automobile field, accelerates the popularization of electric automobile.
Description
Technical field
The invention belongs to electrochemistry, materials chemistry and electrochmical power source product technical field, more particularly, to a kind of secondary
Electrode material of lithium ion battery and preparation method thereof.
Background technology
Due to have the advantages that high energy output, high conversion efficiency, length storage life, lithium ion battery is recognized
To may be used as the very promising energy of electric automobile.As traditional commercialization negative material, graphite has high ratio
Capacity（372 mAh g in theory-1）, in addition, cost is low, it is also its advantage to have extended cycle life etc..However, its operating potential is very
Low, after below 1V is discharged into for the first time, electrolyte starts to decompose, and one layer of solid electrolyte interface film is formed in negative terminal surface.
In high rate charge-discharge, solid electrolyte interface film is easily caused lithium metal and is separated out in carbon electrodes and form dendrite, lithium branch
Brilliant presence may cause the short circuit of battery, and then bring serious potential safety hazard.In addition the lithium ion diffusion coefficient of graphite is low,
It result in the high rate performance of its difference.These problems all hinder application of the graphite in high performance lithium ion battery.Therefore, develop
Negative material with good chemical property is very necessary, specifically includes high security, reversible specific capacity, forthright again
Energy and cyclical stability.
In numerous negative materials, M-Ti-O compound-materials have been done extensive research, because they have safety
Operating potential（Ti3+ / Ti4+）, so as to suppress the formation of the reduction of electrolyte and Li dendrite.Wherein, " zero strain " Li4Ti5O12
Material is to be studied widest M-Ti-O negative materials.Li4Ti5O12By it is modified can have it is safe and stable, quickly fill
The advantages of electric discharge, but its intrinsic low theoretical capacity（Only 175 mAh g-1）Limit its application.
In order to solve this problem, M-Nb-O negative materials have been carried out research and have been used as replacing for M-Ti-O negative materials
For material.Compared with M-Ti-O materials, M-Nb-O materials equally have the operating potential of safety（Nb3+ / Nb4+And Nb4+ / Nb5 +）.Due to Nb3+And Nb5+Between have the transfers of two electronics, M-Nb-O materials have higher theoretical capacity.In addition, M-Nb-O
Material is compared to Li4Ti5O12With more open space structure, the conduction of lithium ion is more beneficial for, therefore M-Nb-O materials have
There is more preferable chemical property.However, the M-Nb-O negative materials being up to the present developed are extremely limited, predominantly Ti-Nb-
O negative materials.Therefore, the more M-Nb-O negative materials with good chemical property are explored and are used for lithium ion battery
It is very necessary.
The content of the invention
It is used for the situation of lithium ion battery for few M-Nb-O materials in the prior art, it is an object of the invention to provide
A kind of electrode material of new secondary lithium battery, it is intended to solve only that a small number of M-Nb-O materials are available is used as lithium ion
Cell negative electrode material and the problem of cause electric automobile to promote.
Present invention also offers a kind of preparation method of the electrode material of secondary lithium battery.
The used to achieve these goals technical scheme of the present invention is：
The invention provides a kind of electrode material of lithium ion battery, the chemical formula of the electrode material is MNb11O29, the M
For Al, Ga or Cr.
Present invention also offers a kind of preparation method of above-mentioned electrode material, including solid reaction process or method of electrostatic spinning；
The solid reaction process comprises the following steps：
By silicon source, gallium source or chromium source sinter after being mixed with niobium source by high-energy ball milling, produce electrode material MNb11O29Powder；
The mol ratio in source of aluminium, gallium source or chromium source and niobium source is 1:11；
The method of electrostatic spinning comprises the following steps：
（1）By 0.001 mol silicon sources, gallium source or chromium source, 2 mL hydrolysis-resisting agents, 1 g adhesives are dissolved in shape in 10 mL organic solvents
Into aluminum solutions, Gallium solution or chromium solution；
（2）0.011 mol niobiums source is dissolved in formation niobium solution in 5 mL organic solvents；
（3）By aluminum solutions, Gallium solution or chromium solution by electrostatic spinning obtain fiber after being well mixed with niobium solution, and fiber is entered
Row drying and processing；
（4）Fiber after drying is sintered, obtains electrode material MNb11O29Powder.
Further, source of aluminium is alundum (Al2O3) or aluminium salt；The gallium source is gallic oxide or gallium salt；Chromium source is
Chrome green or chromic salts；
The aluminium salt is aluminium acetylacetonate or aluminum acetate；The gallium salt is acetylacetone,2,4-pentanedione gallium or acetic acid gallium；The chromic salts is acetyl
Acetone chromium or chromic acetate.
Further, the niobium source is niobium pentaoxide, niobium powder, niobium oxalate or ethanol niobium.
Electrode material prepared by the present invention, the condition of electrostatic spinning is in its preparation process：Needle diameter is 21 G, note
Emitter capacity is 10 mL, and the distance of syringe needle and receiver board is 15 cm, and solution flow rate is 0.5 mm per minute, and voltage is 15 kV.
Further, the hydrolysis-resisting agent is acetic acid or citric acid.
Further, described adhesive is polyvinylpyrrolidone or polyacrylonitrile.
Further, the organic solvent is DMF or ethanol.
In above-mentioned preparation method, the temperature of the drying is 80 DEG C；The temperature of the sintering is 750-1400 DEG C, during sintering
Between be 2-6 h.
Each raw material used in above-mentioned preparation method is commercially available unless otherwise instructed.
In the present invention, the electrode material of secondary lithium battery is AlNb respectively11O29, GaNb11O29And CrNb11O29；
Wherein AlNb11O29Theoretical specific capacity be 389 mAh g-1, GaNb11O29Theoretical specific capacity be 379 mAh g-1,
CrNb11O29Theoretical specific capacity be 383 mAh g-1.Three kinds of materials all have of a relatively high operating potential, therefore with very
Good security.In addition, these materials all have good chemical property, pass through AlNb made from solid phase method11O290.1
Discharge and recharge initial coulomb efficiency is up to 96.3% under C multiplying powers, and reversible specific capacity is up to 257 mAh g-1, it is reversible under 10 C multiplying powers
Specific capacity is still 67 mAh g-1, also surplus 83.3% capacity after 200 circle circulations.Pass through GaNb made from solid phase method11O29
Discharge and recharge initial coulomb efficiency is up to 94.4% under 0.1 C multiplying powers, and reversible specific capacity is up to 255 mAh g-1, under 10 C multiplying powers
Reversible specific capacity is still 124 mAh g-1, also surplus 97.5% capacity after 200 circle circulations.By made from solid phase method
CrNb11O29Discharge and recharge initial coulomb efficiency is up to 93.8% under 0.1 C multiplying powers, and reversible appearance proportion is up to 278 mAh g-1,
Reversible specific capacity is still 148 mAh g under 10 C multiplying powers-1, also surplus 96.1% capacity after 200 circle circulations.Pass through Static Spinning
AlNb made from silk method11O29Discharge and recharge initial coulomb efficiency is up to 90.4% under 0.1 C multiplying powers, and reversible specific capacity is up to 253
mAh g-1, reversible specific capacity is still 123 mAh g under 10 C multiplying powers-1, also surplus 94.3% capacity after 200 circle circulations.
Pass through GaNb made from method of electrostatic spinning11O29Discharge and recharge initial coulomb efficiency is up to 96.4% under 0.1 C multiplying powers, reversible specific volume
Amount is up to 276 mAh g-1, reversible specific capacity is still 174 mAh g under 10 C multiplying powers-1, it is also surplus after 200 circle circulations
98.3% capacity.Pass through CrNb made from method of electrostatic spinning11O29Discharge and recharge initial coulomb efficiency is up under 0.1 C multiplying powers
94.9%, reversible specific capacity is up to 368 mAh g-1, reversible specific capacity is still 184 mAh g under 10 C multiplying powers-1, by 200
Also surplus 97.8% capacity after circle circulation.
Beneficial effects of the present invention are：
（1）Electrode material provided by the invention has theoretical specific capacity height, security performance as lithium ion battery negative material
The advantages that height, reversible specific capacity are high, coulombic efficiency is high and cycle performance is excellent.
（2）Preparation method synthesis technique provided by the invention is simple, suitable for the high power device discharge and recharge such as electric automobile,
Had broad application prospects in field of lithium ion battery.
（3）The present invention provides more choices for M-Nb-O materials for lithium ion battery negative material, in lithium ion
Battery has broad application prospects for electric automobile field, accelerates the popularization of electric automobile.
Brief description of the drawings
Fig. 1 is to use solid phase anti-in the preparation method of the electrode material of secondary lithium battery provided in an embodiment of the present invention
Answer the implementation process figure that method is mixed；
Fig. 2 is to use method of electrostatic spinning in the preparation method of the electrode material of secondary lithium battery provided in an embodiment of the present invention
The implementation process figure mixed；
Fig. 3 is AlNb obtained by embodiment 1, embodiment 2, embodiment 3, embodiment 21, embodiment 22 and embodiment 2311O29,
GaNb11O29And CrNb11O29XRD；
Fig. 4 is AlNb obtained by embodiment 111O29Electron micrograph；
Fig. 5 is GaNb obtained by embodiment 211O29Electron micrograph；
Fig. 6 is CrNb obtained by embodiment 311O29Electron micrograph；
Fig. 7 is embodiment 21, resulting AlNb11O29Electron micrograph；
Fig. 8 is embodiment 22, resulting GaNb11O29Electron micrograph；
Fig. 9 is embodiment 23, resulting CrNb11O29Electron micrograph；
Figure 10 is AlNb obtained by embodiment 111O29High rate performance；
Figure 11 is AlNb obtained by embodiment 2111O29High rate performance；
Figure 12 is GaNb obtained by embodiment 211O29High rate performance；
Figure 13 is GaNb obtained by embodiment 2211O29High rate performance；
Figure 14 is CrNb obtained by embodiment 311O29High rate performance；
Figure 15 is CrNb obtained by embodiment 2311O29High rate performance；
Figure 16 is AlNb obtained by embodiment 1, embodiment 2111O29Cycle performance under 10 C；
Figure 17 is GaNb obtained by embodiment 2, embodiment 2211O29Cycle performance under 10 C；
Figure 18 is CrNb obtained by embodiment 3, embodiment 2311O29Cycle performance under 10 C.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
Solid reaction process flow chart of the present invention is as shown in Figure 1；Method of electrostatic spinning flow chart is as shown in Figure 2.
Embodiment 1
By niobium pentaoxide and alundum (Al2O3) according to elemental mole ratios Al:Nb=1:11 ratio uses high energy ball mill ball milling
After method is mixed, 6 h are sintered at 1200 DEG C, you can obtain AlNb11O29Powder.
Embodiment 2
By niobium pentaoxide and gallic oxide according to elemental mole ratios Ga:Nb=1:11 ratio uses high energy ball mill ball milling
After method is mixed, 6 h are sintered at 1300 DEG C, you can obtain GaNb11O29Powder.
Embodiment 3
By niobium pentaoxide and chrome green according to elemental mole ratios Cr:Nb=1:11 ratio uses high energy ball mill ball milling
After method is mixed, 6 h are sintered at 1300 DEG C, you can obtain CrNb11O29Powder.
Electrode material is prepared by solid phase method, embodiment 4-20 is as shown in table 1.
Table 1
Embodiment 21
S11：By 0.001 mol aluminium acetylacetonates, 2 mL acetic acid, 1 g polyvinylpyrrolidones, 10 mL N, N- dimethyl are dissolved in
Aluminum solutions are formed in formamide；
S12：0.011 mol ethanol niobiums are dissolved in formation niobium solution in 5 mL ethanol；
S13：Electrostatic spinning obtains fiber after aluminum solutions are well mixed with niobium solution, and needle diameter is 21 G, and syringe capacity is
The distance of 10 mL, syringe needle and receiver board is 15 cm, and solution flow rate is 0.5 mm per minute, and voltage is 15 kV, and by the fibre
Dimension carries out 80 DEG C of drying and processings；
S14：800 DEG C of 3 h of sintering are carried out to the fiber, obtain electrode material AlNb11O29Powder.
Embodiment 22
S11：By 0.001 mol acetylacetone,2,4-pentanediones gallium, 2 mL acetic acid, 1 g polyvinylpyrrolidones, 10 mL N, N- dimethyl are dissolved in
Gallium solution is formed in formamide；
S12：0.011 mol ethanol niobiums are dissolved in formation niobium solution in 5 mL ethanol；
S13：Electrostatic spinning obtains fiber after Gallium solution is well mixed with niobium solution, and needle diameter is 21 G, and syringe capacity is
The distance of 10 mL, syringe needle and receiver board is 15 cm, and solution flow rate is 0.5 mm per minute, and voltage is 15 kV, and by the fibre
Dimension carries out 80 DEG C of drying and processings；
S14：800 DEG C of 3 h of sintering are sintered to the fiber, obtain electrode material GaNb11O29Powder.
Embodiment 23
S11：By 0.001 mol chromium acetylacetonates, 2 mL acetic acid, 1 g polyvinylpyrrolidones, 10 mL N, N- dimethyl are dissolved in
Gallium solution is formed in formamide；
S12：0.011 mol ethanol niobiums are dissolved in formation niobium solution in 5 mL ethanol；
S13：Electrostatic spinning obtains fiber after chromium solution is well mixed with niobium solution, and needle diameter is 21 G, and syringe capacity is
The distance of 10 mL, syringe needle and receiver board is 15 cm, and solution flow rate is 0.5 mm per minute, and voltage is 15 kV, and by the fibre
Dimension carries out 80 DEG C of drying and processings；
S14：800 DEG C of 3 h of sintering are sintered to the fiber, obtain electrode material CrNb11O29Powder.
Electrode material is prepared by method of electrostatic spinning, embodiment 24-47 is as shown in table 2.
Table 2
（Connect table）
Fig. 3 is shown to be obtained using embodiment 1, embodiment 2, embodiment 3, embodiment 21, embodiment 22, the methods described of embodiment 23
To AlNb11O29、GaNb11O29And CrNb11O29XRD, analysis draw made of solid phase method and method of electrostatic spinning
AlNb11O29、GaNb11O29And CrNb11O29Material is pure, shows that solid phase method and method of electrostatic spinning can be prepared successfully
AlNb11O29、GaNb11O29And CrNb11O29Three materials.Fig. 4, Fig. 5, Fig. 6 show using embodiment 1, embodiment 2, implemented
The methods described of example 3 obtains AlNb11O29、GaNb11O29And CrNb11O29Electron micrograph, as can be seen from the figure three
Material is all rod-shpaed particle and uniform in size, and particle diameter is between 0.2-20 μm.Fig. 7, Fig. 8, Fig. 9 show using embodiment 21,
Embodiment 22, the methods described of embodiment 23 obtain AlNb11O29、GaNb11O29And CrNb11O29Electron micrograph, from figure
In it can be seen that AlNb11O29、GaNb11O29And CrNb11O29Material is all nanofiber, fibre diameter be respectively 400nm,
250nm and 200nm or so.Figure 10, Figure 11 are that embodiment 1, the methods described of embodiment 21 obtain AlNb respectively11O29Multiplying power figure,
Figure 12, Figure 13 are that embodiment 2, the methods described of embodiment 22 obtain GaNb respectively11O29Multiplying power figure.Figure 14, Figure 15 are real respectively
Apply example 3, the methods described of embodiment 23 obtains CrNb11O29Multiplying power figure.The AlNb made from solid phase method11O29Under 0.1 C multiplying powers
Discharge and recharge initial coulomb efficiency is up to 96.3%, and reversible specific capacity is up to 257 mAh g-1, reversible specific capacity is still under 10 C multiplying powers
For 67 mAh g-1.Pass through GaNb made from solid phase method11O29Discharge and recharge initial coulomb efficiency is up to 94.4% under 0.1 C multiplying powers,
Reversible specific capacity is up to 255 mAh g-1, reversible specific capacity is still 124 mAh g under 10 C multiplying powers-1.It is made by solid phase method
CrNb11O29Discharge and recharge initial coulomb efficiency is up to 93.8% under 0.1 C multiplying powers, and reversible appearance proportion is up to 278 mAh g-1,
Reversible specific capacity is still 148 mAh g under 10 C multiplying powers-1.Pass through AlNb made from method of electrostatic spinning11O29In 0.1 C multiplying powers
Lower discharge and recharge initial coulomb efficiency is up to 90.4%, and reversible specific capacity is up to 253 mAh g-1, the reversible specific capacity under 10 C multiplying powers
Still it is 123 mAh g-1.Pass through GaNb made from method of electrostatic spinning11O29Discharge and recharge initial coulomb efficiency is high under 0.1 C multiplying powers
Up to 96.4%, reversible specific capacity is up to 276 mAh g-1, reversible specific capacity is still 174 mAh g under 10 C multiplying powers-1.By quiet
CrNb made from electrical spinning method11O29Discharge and recharge initial coulomb efficiency is up to 94.9% under 0.1 C multiplying powers, and reversible specific capacity is up to
368 mAh g-1, reversible specific capacity is still 184 mAh g under 10 C multiplying powers-1.These materials all have excellent forthright again
Can, it is very suitable for being applied among lithium ion battery used for electric vehicle.Figure 16, Figure 17, Figure 18 are embodiment 1, embodiment respectively
21st, embodiment 2, embodiment 22, embodiment 3, the methods described of embodiment 23 obtain AlNb11O29、GaNb11O29And CrNb11O29's
Circulation figure, under 10 C after 200 times are circulated throughout, AlNb made from solid phase method11O29Still there is 83.3% specific capacity, it is quiet
AlNb made from electrical spinning method11O29Material still has 94.3% specific capacity.GaNb made from solid phase method11O29Still have
97.5% specific capacity, GaNb made from method of electrostatic spinning11O29Material still has 98.3% specific capacity.Made from solid phase method
CrNb11O29With still 96.1% specific capacity, CrNb made from method of electrostatic spinning11O29Material still has 97.8% specific volume
Amount.These materials all show excellent cycle performance, can fully meet lithium ion battery used for electric vehicle to cycle performance
It is required that.The above advantage can absolutely prove AlNb11O29、GaNb11O29And CrNb11O29It is that up-and-coming electrokinetic cell is born
Pole material.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all any modification, equivalent and improvement made within the spirit and principles of the invention etc., all should be included
Within protection scope of the present invention.
Claims (9)
1. a kind of electrode material of lithium ion battery, it is characterised in that the chemical formula of the electrode material is MNb11O29, the M
For Al, Ga or Cr.
2. a kind of preparation method of electrode material as claimed in claim 1, it is characterised in that including solid reaction process or electrostatic
Spin processes；
The solid reaction process comprises the following steps：
By silicon source, gallium source or chromium source sinter after being mixed with niobium source by high-energy ball milling, produce electrode material MNb11O29Powder；
The mol ratio in source of aluminium, gallium source or chromium source and niobium source is 1:11；
The method of electrostatic spinning comprises the following steps：
（1）By 0.001 mol silicon sources, gallium source or chromium source, 2 mL hydrolysis-resisting agents, 1 g adhesives are dissolved in shape in 10 mL organic solvents
Into aluminum solutions, Gallium solution or chromium solution；
（2）0.011 mol niobiums source is dissolved in formation niobium solution in 5 mL organic solvents；
（3）By aluminum solutions, Gallium solution or chromium solution by electrostatic spinning obtain fiber after being well mixed with niobium solution, and fiber is entered
Row drying and processing；
（4）Fiber after drying is sintered, obtains electrode material MNb11O29Powder.
3. preparation method according to claim 2, it is characterised in that source of aluminium is alundum (Al2O3) or aluminium salt；It is described
Gallium source is gallic oxide or gallium salt；Chromium source is chrome green or chromic salts；
The aluminium salt is aluminium acetylacetonate or aluminum acetate；The gallium salt is acetylacetone,2,4-pentanedione gallium or acetic acid gallium；The chromic salts is acetyl
Acetone chromium or chromic acetate.
4. according to the preparation method described in claim any one of 2-3, it is characterised in that the niobium source is niobium pentaoxide, niobium
Powder, niobium oxalate or ethanol niobium.
5. preparation method according to claim 2, it is characterised in that the condition of the electrostatic spinning is：Needle diameter is
21 G, syringe capacity are 10 mL, and the distance of syringe needle and receiver board is 15 cm, and solution flow rate is 0.5 mm per minute, voltage
For 15 kV.
6. preparation method according to claim 2, it is characterised in that the hydrolysis-resisting agent is acetic acid or citric acid.
7. preparation method according to claim 2, it is characterised in that described adhesive is polyvinylpyrrolidone or poly- third
Alkene nitrile.
8. preparation method according to claim 2, it is characterised in that the organic solvent be DMF or
Ethanol.
9. according to the preparation method described in claim any one of 2-8, it is characterised in that the temperature of the drying is 80 DEG C；Institute
The temperature for stating sintering is 750-1400 DEG C, and sintering time is 2-6 h.
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| CN109360978A (en) * | 2018-10-09 | 2019-02-19 | 瑞声科技（南京）有限公司 | Lithium ion battery negative material and nonaqueous electrolyte battery |
| CN109616714A (en) * | 2018-11-26 | 2019-04-12 | 天津普兰能源科技有限公司 | The recovery method of niobium base electrode material in a kind of electrode slice |
| CN110277556A (en) * | 2018-03-16 | 2019-09-24 | 株式会社东芝 | Active material, electrode, secondary cell, battery pack and vehicle |
| WO2020098427A1 (en) * | 2018-11-13 | 2020-05-22 | 瑞声声学科技(深圳)有限公司 | Lithium ion battery negative electrode material and non-aqueous electrolyte battery |
| CN112786874A (en) * | 2021-01-29 | 2021-05-11 | 复旦大学 | Electrode material of sodium ion battery and preparation and application thereof |
| WO2022043702A1 (en) | 2020-08-28 | 2022-03-03 | Echion Technologies Limited | Active electrode material |
| WO2022080083A1 (en) * | 2020-10-16 | 2022-04-21 | マクセル株式会社 | Electrode active material for electrochemical element and method for producing same, electrode material for electrochemical element, electrode for electrochemical element, electrochemical element, and mobile object |
| CN114824252A (en) * | 2022-04-19 | 2022-07-29 | 江苏大学 | One-dimensional indium-niobium oxide cathode material for lithium ion battery and preparation method thereof |
| US11799077B2 (en) | 2020-06-03 | 2023-10-24 | Echion Technologies Limited | Active electrode material |
| US12027699B2 (en) | 2020-06-03 | 2024-07-02 | Echion Technologies Limited | Active electrode material |
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