CN109950523A - Lithium ion battery negative material transition metal oxide/carbon preparation method - Google Patents
Lithium ion battery negative material transition metal oxide/carbon preparation method Download PDFInfo
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- CN109950523A CN109950523A CN201910193370.4A CN201910193370A CN109950523A CN 109950523 A CN109950523 A CN 109950523A CN 201910193370 A CN201910193370 A CN 201910193370A CN 109950523 A CN109950523 A CN 109950523A
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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
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- 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 invention discloses a kind of transition metal oxide/carbon lithium ion cell negative electrode material preparation methods, the steps include: nitric acid dissolving metal salts in n,N-Dimethylformamide solution, persistently stir at room temperature, form solution A；Ethylenediamine tetra-acetic acid is dissolved in the n,N-Dimethylformamide solution containing triethylamine, is persistently stirred at room temperature, solution B is formed；Solution A is added in solution B, is persistently stirred at room temperature, precipitating is formed；Presoma is dried in vacuo to obtain after gained precipitating cleaning；Gained presoma obtains final product through 350 ± 10 DEG C of 100 ~ 150min of calcining.Transition metal oxide/carbon is prepared using this method, step is simply convenient for industrialization large-scale production, and the product grain of synthesis is uniformly tiny, guarantees the circulation volume and chemical property of material.
Description
Technical field
The invention belongs to lithium ion battery material and electrochemical field, it is related to a kind of preparing transition metal oxide/carbon lithium
The preparation method of ion battery cathode material.
Background technique
The features such as lithium ion battery is due to energy density height, high power and memory-less effect, is widely used in consumption electricity
Sub- product and new-energy automobile power battery.The negative electrode material of lithium ion battery is its important component part, affects electrification
Learn one of the main bottleneck of performance.However, the negative electrode material for the lithium ion battery being commercialized at present is graphite type material, theory is held
Amount is only 372 mAh g-1, and there are serious safety problems during high rate charge-discharge, have been unable to satisfy people increasingly
The demand of growth, especially in new-energy automobile power battery.Therefore research and development novel anode material is most important.
Transition metal oxide material is due to theoretical reversible specific capacity, cheap, resourceful and nothing with higher
Features of pollution, it has also become one of the research hotspot of novel cathode material for lithium ion battery in recent years.However, they are in charge and discharge
Caused biggish volume change causes cyclical stability difference and high rate performance low in journey, limits its further development.Pass through
Carbon coating is considered a kind of effective ameliorative way.Zhao et al. (Adv. Funct. Mater., 2017,27,
1605017) it utilizes and prepares by the Co of 5-10 nm3O4The Co of the 3D meso-hole structure of nano particle composition3O4Material, in electric current
Density is 100 mA g-11033 mAh g are shown under current density-1Reversible specific capacity.Lin et al. (Angew. Chem.
Int. Ed., 2017,129,1895) synthesize poly-dopamine cladding SnO2Composite material shows excellent stable circulation
Property and high rate performance.Huang et al. (Adv. Mater, 2014,26,6622-6628) is precursor synthesis using MOF-Fe
The Fe of meso-hole structure out2O3The composite material of/C is 200 mA g in current density-1Shi Xunhuan 50 is enclosed, and specific discharge capacity reaches
911 mAh g-1。
Currently, hydro-thermal method and solvent-thermal method etc. can synthesize transition metal oxide/carbon material of different-shape, but
Hydro-thermal method and solvent heat are prepared suitable for laboratory, are unable to satisfy the demand that business is produced in enormous quantities；Although solid phase method is suitble to quotient
Industry metaplasia produces, but active material pattern is uncontrollable, it is easy to reunite, cause its cycle life short, significantly limit it
Commercial applications.Therefore guaranteeing the circulation volume of material and commercially producing, needing to carry out the preparation process of the material excellent
Change and improves.
Summary of the invention
Transition metal oxide/carbon lithium ion battery composite cathode material side is prepared the purpose of the present invention is to provide a kind of
Method can not only keep considerable high rate performance and cyclical stability by this method, but also commercial applications may be implemented.
To achieve the goals above, the invention adopts the following technical scheme:
Lithium ion battery negative material, chemical formula TMO/C, preparation method are specific as follows:
A, nitric acid dissolving metal salts are persistently stirred at room temperature in n,N-Dimethylformamide (DMF) solution, forms solution A；
B, ethylenediamine tetra-acetic acid is dissolved in the DMF solution containing triethylamine, is persistently stirred at room temperature, form solution B；
C, solution A is added in solution B, is persistently stirred at room temperature, form precipitating；
D, presoma is dried in vacuo to obtain after the cleaning of gained precipitating；
E, gained presoma obtains final product through 350 ± 10 DEG C of calcining 2h.
Preferably, in step a, the nitric acid metal salt is any one in cobalt nitrate, manganese nitrate and nickel nitrate, concentration
For 25-50mg/ml.
Preferably, in step b, triethylamine is the 3 ~ 4% of DMF mass.
Preferably, in step c, the molar ratio of the nitric acid metal salt in the ethylenediamine tetra-acetic acid and solution A in solution B is 1:
1。
Preferably, in step d, 12h is dried in vacuo at 60 DEG C after gained precipitating cleaning and obtains presoma.
Preferably, in step d, gained precipitating is alternately cleaned using DMF solution and deionized water.
Compared with prior art, transition metal oxide/carbon compound electric is prepared using in-situ method at room temperature in the present invention
Pole material can solve the problems such as preparation process brought by hydro-thermal method and solvent-thermal method is complicated, and synthesizing mean is simple, be easy big
It is prepared by batch.It is dispersed in carbon net array using the nano particle that the method for the present invention synthesizes, shows excellent electrochemistry
Performance.Synthesizing lithium ion battery negative electrode material transition metal oxide/carbon preparation method, step are simply convenient for work in the present invention
Industryization large-scale production.
Detailed description of the invention
Fig. 1 is lithium ion battery negative material cobaltosic oxide/carbon scanning electron microscope (SEM) photograph of 2 pyrolysismethod of embodiment synthesis.
Fig. 2 is lithium ion battery negative material cobaltosic oxide/carbon XRD diagram of 2 pyrolysismethod of embodiment synthesis.
Fig. 3 is lithium ion battery negative material cobaltosic oxide/carbon initial charge/discharge of 2 pyrolysismethod of embodiment synthesis
Curve graph.
Fig. 4 is lithium ion battery negative material cobaltosic oxide/carbon high rate performance figure of 2 pyrolysismethod of embodiment synthesis.
Fig. 5 is that the lithium ion battery negative material four of 2 pyrolysismethod of embodiment synthesis aoxidizes three aunts/carbon cycle performance figure.
Specific embodiment
Below with reference to embodiment, the invention will be further described, but not as a limitation of the invention.
Embodiment 1(is without triethylamine)
It takes 1.0 g, tetra- nitric hydrate cobalt to be dissolved into the DMF of 40ml, persistently stirs at room temperature, form solution.Then 1.2g is taken
Ethylenediamine tetra-acetic acid be dissolved in the DMF solution of 40ml, metal salt solution is added in edta solution, continue
It is stirred at room temperature 30 minutes, does not form precipitating, presoma can not be obtained.
Embodiment 2
It takes 1.0 g, tetra- nitric hydrate cobalt to be dissolved into the DMF of 40ml, persistently stirs at room temperature, form solution.Then 1.2g is taken
Ethylenediamine tetra-acetic acid and the triethylamine of 1.5ml be dissolved in the DMF solution of 40ml, metal salt solution is added to ethylenediamine tetraacetic
In acetic acid solution, continue to be stirred at room temperature 30 minutes, forms precipitating.Above-mentioned precipitating is collected into cleaning and is transferred to vacuum oven for several times
In 60 DEG C 12 hours, obtain presoma.
Take the presoma grinding being dried to obtain is placed on 350 DEG C of nitrogen atmosphere calcining 2h in tube furnace, grinds after taking-up
Obtained powder sample is target product Co3O4/ C (Fig. 1), pattern Co3O4Particle is embedded in carbon net array (as schemed
2).
By the sample (active material) of synthesis, acetylene black (conductive agent) and PVDF(binder) according to mass ratio 7:2:1,
It is uniformly mixed in NMP, is then coated on copper foil, juxtaposition 100 DEG C drying 10 hours in a vacuum drying oven.It is cut into after taking out straight
Diameter is the electrode disk of 12mm.In this, as negative electrode tab, using metal lithium sheet as to electrode, microporous polypropylene membrane Celgard
2400 be diaphragm, and nickel foam is filler, and electrolyte is the LiPF of 1mol/L6/ EC+DMC (volume ratio 1: 1), is being full of
CR2016 type button cell is assembled in the glove box of argon gas protection.Using LAND CT2001A type (the blue electricity in Wuhan) multichannel battery
Test system and test, temperature are 25 DEG C of room temperature.
For the material synthesized under this condition in voltage range between 0.001-3.0 V, current density is 60 mA/g test
When, Co3O4The initial discharge capacity of/C can achieve 1120 mAh g-1(such as Fig. 1), in 3000 mA g of high current-1Under, it puts
Electric specific capacity can reach 300 mAh g-1(such as Fig. 4).It is 600 mA g in current density-1When, after charge and discharge cycles 200 are enclosed
Capacity may remain in 370 mAh g-1(such as Fig. 5).
Embodiment 3
It takes 2.0 g, tetra- nitric hydrate cobalt to be dissolved into the DMF of 40ml, persistently stirs at room temperature, form solution.Then 2.4g is taken
Ethylenediamine tetra-acetic acid and the triethylamine of 1.5ml be dissolved in the DMF solution of 40ml, metal salt solution is added to ethylenediamine tetraacetic
In acetic acid solution, continue to be stirred at room temperature 30 minutes, forms precipitating.Above-mentioned precipitating is collected into cleaning and is transferred to vacuum oven for several times
In 60 DEG C 12 hours, obtain presoma.
Take the presoma grinding being dried to obtain is placed on 350 DEG C of nitrogen atmosphere calcining 2h in tube furnace, grinds after taking-up
Obtained powder sample is target product.
By the sample (active material) of synthesis, acetylene black (conductive agent) and PVDF(binder) according to mass ratio 7:2:1,
It is uniformly mixed in NMP, is then coated on copper foil, juxtaposition 100 DEG C drying 10 hours in a vacuum drying oven.It is cut into after taking out straight
Diameter is the electrode disk of 12mm.In this, as negative electrode tab, using metal lithium sheet as to electrode, microporous polypropylene membrane Celgard
2400 be diaphragm, and nickel foam is filler, and electrolyte is the LiPF6/EC+DMC (volume ratio 1: 1) of 1mol/L, is being full of
CR2016 type button cell is assembled in the glove box of argon gas protection.Using LAND CT2001A type (the blue electricity in Wuhan) multichannel battery
Test system and test, temperature are 25 DEG C of room temperature.
For the material synthesized under this condition in voltage range between 0.001 ~ 3.0 V, current density is 60 mA/g test
When, Co3O4The initial discharge capacity of/C can achieve 1090 mAh g-1, in high current 3000mA g-1Under, specific discharge capacity can
Reach 289 mAh g-1.It is 600 mA g in current density-1When, capacity may remain in 310 after charge and discharge cycles 200 are enclosed
mAh g-1。
Embodiment 4
It takes 1.0 g, tetra- nitric hydrate manganese to be dissolved into the DMF of 40ml, persistently stirs at room temperature, form solution.Then 1.2g is taken
Ethylenediamine tetra-acetic acid and the triethylamine of 1.5ml be dissolved in the DMF solution of 40ml, metal salt solution is added to ethylenediamine tetraacetic
In acetic acid solution, continue to be stirred at room temperature 30 minutes, forms precipitating.Above-mentioned precipitating is collected into cleaning and is transferred to vacuum oven for several times
In 60 DEG C 12 hours, obtain presoma.
Take the presoma grinding being dried to obtain is placed on 350 DEG C of nitrogen atmosphere calcining 2h in tube furnace, grinds after taking-up
Obtained powder sample is target product.
By the sample (active material) of synthesis, acetylene black (conductive agent) and PVDF(binder) according to mass ratio 7:2:1,
It is uniformly mixed in NMP, is then coated on copper foil, juxtaposition 100 DEG C drying 10 hours in a vacuum drying oven.It is cut into after taking out straight
Diameter is the electrode disk of 12mm.In this, as negative electrode tab, using metal lithium sheet as to electrode, microporous polypropylene membrane Celgard
2400 be diaphragm, and nickel foam is filler, and electrolyte is the LiPF of 1mol/L6/ EC+DMC+DEC (volume ratio 1: 1: 1),
CR2016 type button cell is assembled in the glove box full of argon gas protection.Using LAND CT2001A type (the blue electricity in Wuhan) multi-pass
The test of road battery test system, temperature are 25 DEG C of room temperature.
For the material synthesized under this condition in voltage range between 0.001 ~ 3.0 V, current density is 60 mA/g test
When, Mn2O3The initial discharge capacity of/C can achieve 1200 mAh g-1, in 3000 mA g of high current-1Under, specific discharge capacity
It can reach 220mAh g-1.It is 500 mA g in current density-1When, capacity may remain in 300 after charge and discharge cycles 200 are enclosed
mAh g-1。
Embodiment 5
It takes 1.0 g, tetra- nitric hydrate nickel to be dissolved into the DMF of 40ml, persistently stirs at room temperature, form solution.Then 1.2g is taken
Ethylenediamine tetra-acetic acid and the triethylamine of 1.5ml be dissolved in the DMF solution of 40ml, metal salt solution is added to ethylenediamine tetraacetic
In acetic acid solution, continue to be stirred at room temperature 30 minutes, forms precipitating.Above-mentioned precipitating is collected into cleaning and is transferred to vacuum oven for several times
In 60 DEG C 12 hours, obtain presoma.
Take the presoma grinding being dried to obtain is placed on 350 DEG C of nitrogen atmosphere calcining 2h in tube furnace, grinds after taking-up
Obtained powder sample is target product.
By the sample (active material) of synthesis, acetylene black (conductive agent) and PVDF(binder) according to mass ratio 7:2:1,
It is uniformly mixed in NMP, is then coated on copper foil, juxtaposition 100 DEG C drying 10 hours in a vacuum drying oven.It is cut into after taking out straight
Diameter is the electrode disk of 12mm.In this, as negative electrode tab, using metal lithium sheet as to electrode, microporous polypropylene membrane Celgard
2400 be diaphragm, and nickel foam is filler, and electrolyte is the LiPF of 1mol/L6/ EC+DMC (volume ratio 1: 1), is being full of
CR2016 type button cell is assembled in the glove box of argon gas protection.Using LAND CT2001A type (the blue electricity in Wuhan) multichannel battery
Test system and test, temperature are 25 DEG C of room temperature.
For the material synthesized under this condition in voltage range between 0.001 ~ 3.0 V, current density is 60 mA/g test
When, the initial discharge capacity of NiO/C can achieve 1014 mAh g-1, in high current 3000mA g-1Under, specific discharge capacity can
Reach 80 mAh g-1.It is 500 mA g in current density-1When, capacity may remain in 160 after charge and discharge cycles 200 are enclosed
mAh g-1。
Embodiment 6
Comparative example 2 takes 1.0 g, tetra- nitric hydrate cobalt to be dissolved into the DMF of 40ml, persistently stirs at room temperature, is formed molten
Liquid.Then the triethylamine of the ethylenediamine tetra-acetic acid and 3.0ml that take 1.2g is dissolved in the DMF solution of 40ml, by metal salt solution
It is added in edta solution, continues to be stirred at room temperature 30 minutes, form gelatinous precipitate.Above-mentioned precipitating is collected into cleaning number
It is secondary to be transferred to 60 DEG C 12 hours in vacuum oven, presoma can not be obtained.
Embodiment 7
Comparative example 3 takes 2.0 g, tetra- nitric hydrate cobalt to be dissolved into the DMF of 40ml, persistently stirs at room temperature, is formed molten
Liquid.Then the triethylamine of the ethylenediamine tetra-acetic acid and 3.0ml that take 2.4g is dissolved in the DMF solution of 40ml, by metal salt solution
It is added in edta solution, continues to be stirred at room temperature 30 minutes, form gelatinous precipitate.Above-mentioned precipitating is collected into cleaning number
It is secondary to be transferred to 60 DEG C 12 hours in vacuum oven, presoma can not be obtained.
Embodiment 8
Comparative example 4 takes 1.0 g, tetra- nitric hydrate manganese to be dissolved into the DMF of 40ml, persistently stirs at room temperature, is formed molten
Liquid.Then the triethylamine of the ethylenediamine tetra-acetic acid and 3.0ml that take 1.2g is dissolved in the DMF solution of 40ml, by metal salt solution
It is added in edta solution, continues to be stirred at room temperature 30 minutes, form gelatinous precipitate.Above-mentioned precipitating is collected into cleaning number
It is secondary to be transferred to 60 DEG C 12 hours in vacuum oven, presoma can not be obtained.
Embodiment 9
Comparative example 4 takes 1.0 g, tetra- nitric hydrate nickel to be dissolved into the DMF of 40ml, persistently stirs at room temperature, is formed molten
Liquid.Then the triethylamine of the ethylenediamine tetra-acetic acid and 3.0ml that take 1.2g is dissolved in the DMF solution of 40ml, by metal salt solution
It is added in edta solution, continues to be stirred at room temperature 30 minutes, form gelatinous precipitate.Above-mentioned precipitating is collected into cleaning number
It is secondary to be transferred to 60 DEG C 12 hours in vacuum oven, presoma can not be obtained.
Claims (7)
1. a kind of transition metal oxide/carbon lithium ion cell negative electrode material preparation method, chemical formula TMO/C, step
It is rapid as follows:
A, it by nitric acid dissolving metal salts in n,N-Dimethylformamide solution, persistently stirs at room temperature, forms solution A；
B, ethylenediamine tetra-acetic acid is dissolved in the n,N-Dimethylformamide solution containing triethylamine, is persistently stirred at room temperature,
Form solution B；
C, solution A is added in solution B, is persistently stirred at room temperature, form precipitating；
D, presoma is dried in vacuo to obtain after the cleaning of gained precipitating；
E, gained presoma obtains final product through 350 ± 10 DEG C of 100 ~ 150min of calcining.
2. the method as described in claim 1, which is characterized in that nitric acid metal salt is to appoint in cobalt nitrate, manganese nitrate and nickel nitrate
It anticipates one kind.
3. the method as described in claim 1, which is characterized in that in step a, the concentration of the nitric acid metal salt in solution A is 25 ~
50mg/ml。
4. the method as described in claim 1, which is characterized in that in step b, triethylamine is n,N-Dimethylformamide quality
3~4%。
5. the method as described in claim 1, which is characterized in that in step c, in the ethylenediamine tetra-acetic acid and solution A in solution B
Nitric acid metal salt molar ratio be 1:1.
6. the method as described in claim 1, which is characterized in that in step d, be dried in vacuo at 60 DEG C after gained precipitating cleaning
12h obtains presoma.
7. the method as described in claim 1, which is characterized in that in step d, gained precipitating uses DMF solution and deionized water
Alternately clean.
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| CN110265678A (en) * | 2019-07-25 | 2019-09-20 | 河南师范大学 | A kind of preparation method and applications of the NiO@NC bifunctional electrocatalyst with core-shell structure |
| CN110627031A (en) * | 2019-09-25 | 2019-12-31 | 常熟理工学院 | Preparation method of molybdenum-doped cobalt phosphide-carbon coral sheet composite material |
| CN114044554A (en) * | 2021-10-08 | 2022-02-15 | 东北大学 | Method for degrading antibiotics by activating persulfate through photoelectric synergistic strengthening iron-based catalyst |
| CN114349061A (en) * | 2021-12-30 | 2022-04-15 | 杭州电子科技大学 | Preparation method of amorphous ferric oxide microspheres |
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| CN114044554A (en) * | 2021-10-08 | 2022-02-15 | 东北大学 | Method for degrading antibiotics by activating persulfate through photoelectric synergistic strengthening iron-based catalyst |
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Application publication date: 20190628 |