CN108807890A - A kind of ternary nano porous nickel vanadium manganese oxide electrode material and preparation method thereof - Google Patents
A kind of ternary nano porous nickel vanadium manganese oxide electrode material and preparation method thereof Download PDFInfo
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- CN108807890A CN108807890A CN201810567440.3A CN201810567440A CN108807890A CN 108807890 A CN108807890 A CN 108807890A CN 201810567440 A CN201810567440 A CN 201810567440A CN 108807890 A CN108807890 A CN 108807890A
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- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- 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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
The present invention provides a kind of preparation methods of ternary nano porous nickel vanadium manganese oxide electrode material, include the following steps:The preparation of alloy strip:Nickel vanadium manganese Metal particle is prepared into 20-50 μm of band by getting rid of band, and the wherein atom content of Mn is 60-70%, and the atom content of Ni is 20-30%, and the atom content of V is 5-20%.The non-single phase solid solution of alloy prepared by the present invention is two-phase alloys, is prepared into porous structure by chemical removal alloying, preparation process is simple, and raw material is cheap, can be used for mass producing.Porous structure prepared by the present invention can greatly strengthen the specific surface area of material to increase the specific capacity of material, and can play and provide cushioning effect in material charge and discharge process for volume expansion, improve the cyclical stability of material.
Description
Technical field
The invention belongs to porous electrode Material Fields, more particularly, to a kind of ternary nano porous nickel vanadium manganese oxide electrode
Material and preparation method thereof.
Background technology
In recent years, environmental pollution and energy crisis become one of the topic of people's growing interest, at present fossil fuel conduct
Main energy sources are faced with the problem of increasingly reducing.And the harmful substance of the burning generation of fossil fuel is detrimental to health and oneself
Right environment.Solar energy, the regenerative resources such as wind energy have attracted attention, but regenerative resource tool protected from environmental
There is discontinuity, prepares a kind of energy storage device and become storing these instable energies and solve the key of Renewable Energy Development.
Lithium ion battery is due to having high working voltage in energy storage device, and elevated operating temperature range, height ratio capacity, self discharge is small, cycle
Long lifespan, it is environmentally protective the advantages that become solve energy crisis ideal chose.
With extensive use of the lithium ion battery in electronic device and electric vehicle, people are to performance of lithium ion battery
It is required that being also continuously improved.Negative material is one of the key factor for determining battery overall performance in lithium ion battery, at present business
It is still carbon material to change negative material, and carbon material theoretical specific capacity is 372mAh/g, cannot meet people and increasingly improve
Requirement.
Metal oxide does negative material and has higher theoretical specific capacity compared with carbon material, and prepares simply, and cost is relatively low.
Higher specific capacity is wherein obtained by the synergistic effect of NiVMn alloyed oxides, nano-porous structure provides more active sites
Point, the material specific capacity may be up to 914mAh/g, and have preferable cyclical stability.It spends alloy hair and prepares nano porous metal
Oxide ion cathode material lithium is the ideal chose for substituting carbon material.
Invention content
It finds, is closed when being prepared into ternary by getting rid of melting by the way of band using a certain proportion of NiVMn metals under study for action
Gold is prepared into nano porous metal by chemical removal alloying, then so that alloy material oxidation is made material by high temperature in air
Surface forms one layer of metal oxide, and the electrode which prepares compares carbon material electrode and has higher specific capacity, due to
Its material center portion is that metal material ensure that its good electric conductivity, and the porous structure formed can delay in charge and discharge process
Volume expansion is solved, the cyclical stability of material is improved.
In view of this, the present invention is directed to propose a kind of ternary nano porous nickel vanadium manganese oxide electrode material and its preparation side
Method.
In order to achieve the above objectives, the technical proposal of the invention is realized in this way:
A kind of preparation method of ternary nano porous nickel vanadium manganese oxide electrode material, includes the following steps:
(1) preparation of alloy strip:Nickel vanadium manganese Metal particle is prepared into 20-50 μm of band by getting rid of band, wherein Mn's
Atom content is 60-70%, and the atom content of Ni is 20-30%, and the atom content of V is 5-20%;
(2) removal alloying is handled:Alloy strip prepared by step (1) carries out chemical removal alloying processing, by metal Mn
Partial corrosion, which falls, is prepared into porous metals, and the atom content of Mn is 20-40% after corrosion;
(3) high-temperature oxydation:The porous metals corroded in step (2) are heated in sintering furnace high temperature, heat preservation prepares nanometer
Porous metal oxide;
(4) it grinds:By step (3) prepare nano porous metal oxide be put into mortar be fully ground to particle be it is micro-
Meter level obtains metal oxide powder;
(5) electrode is applied:Metal oxide powder prepared by step (4) and Kynoar (PVDF), acetylene black and N-
Methyl pyrrolidone (NMP) is uniformly mixed is fully ground according to a certain percentage, and by the mixture blade applicator after grinding in copper
Electrode slice is scraped on foil obtains electrode material;
(6) assembled battery:By step (5) obtained electrode material as being assembled into lithium ion battery in anaerobism glove box;
(7) chemical property of battery and electrode material is tested.
Preferably, W metal, V, Mn choose the particle of a diameter of 1-3mm in the step (1), and the band rotating speed that gets rid of is
1200rad/s-1800rad/s。
Preferably, the caustic solution in the step (2) is chemical corrosion method, and solution is that weakly acidic ammonium sulfate is molten
Liquid, corrosion temperature are 50-70 DEG C, etching time 4-8h.
Preferably, the temperature that the step (3) is heated in sintering furnace is 200-400 DEG C, soaking time 1-5h.
Preferably, the nano porous metal of the step (3) high-temperature oxydation is positioned over by the grinding in the step (4) grinds
4-10h is fully ground in alms bowl, until micron powder of the linishing at grey black.
Preferably, the mixed proportion of metal oxide powder in the step (5), acetylene black and PVDF are 8: 1: 1, mixing
The suitable NMP dispersion mixings of drop after uniformly, the electrode slice of different-thickness is made in slurry on copper foil after sizing mixing uniformly, by electrode slice
Dry 6-12h is placed in vacuum drying chamber.
Compared with the existing technology, the preparation of a kind of ternary nano porous nickel vanadium manganese oxide electrode material of the present invention
Method has the advantage that:
1) the non-single phase solid solution of alloy prepared by the present invention is two-phase alloys, is prepared by chemical removal alloying porous
Structure.
2) electrode material preparation process of the invention is simple, and raw material is cheap, can be used for mass producing.
It is a further object of the present invention to provide excessively a kind of ternary nano porous nickel vanadium manganese prepared using above-mentioned preparation method
Oxide electrode material, compared with prior art:
1) porous structure for preparing of the present invention can greatly strengthen the specific surface area of material to increase the specific capacity of material,
And can play and provide cushioning effect in material charge and discharge process for volume expansion, improve the cyclical stability of material.
2) ternary nano porous metal oxide electrode material prepared by the present invention is in current density 50mA/g to 1000mA/
G specific capacities are up to 300-950mAh/g, and specific capacity conservation rate is 90% or more after cycle 230 is enclosed, and have good comprehensive electrochemistry
Performance.
Description of the drawings
Fig. 1 is that NiVMn alloy strips are ground at 50 DEG C after corrosion oxidation in the ammonium sulfate of 1mol/L in embodiment 1
SEM figure;
Fig. 2 is that NiVMn materials are fabricated to the multiplying power song that negative electrode of lithium ion battery is assembled into button cell test in embodiment 1
Line chart;
Fig. 3 is that NiVMn materials are assembled into the discharge cycle performance test chart tested after button cell in embodiment 1.
Specific implementation mode
In addition to being defined, technical term used in following embodiment has universal with those skilled in the art of the invention
The identical meanings of understanding.Test reagent used in following embodiment is unless otherwise specified conventional biochemical reagent;It is described
Experimental method is unless otherwise specified conventional method.
Following embodiment can make those skilled in the art that the present invention, but protection scope of the present invention be more fully appreciated
It is not limited to following embodiments.
Embodiment 1
A kind of preparation method of ternary nano porous nickel vanadium manganese oxide electrode material, includes the following steps:
(1) preparation of alloy strip:The atom content ratio of Ni, V, Mn are 25: 15: 60, with getting rid of the mode of band by Ni, V, Mn
It is 20um that thickness, which is made, in metallic particles under the rotating speed of 1200rad/s-1800rad/s under protection of argon gas, and width is the conjunction of 2mm
Gold bar band;
(2) removal alloying prepares nano porous metal:The alloy strip of step (1) is placed in beaker to the sulphur for using 1mol/L
Sour ammonium spontaneous corrosion 6h at 50 DEG C, and change an ammonium sulfate per 2h;
(3) high-temperature oxydation:Nano porous metal band deionized water prepared by step (2) is fully rinsed 3 times, it is ensured that
Material is placed in 50 DEG C of dry 4-6h in air dry oven after no ammonium sulfate remnants.Metal band after drying is placed in high temperature to burn
300 DEG C are warming up to 10 DEG C/min rates in freezing of a furnace, keeps the temperature 2h.
(4) it grinds:The metal material that step (3) aoxidizes is fully ground to grey black micron powder;
(5) electrode is applied:The ground metal oxide powder of step (4) is done into cathode according to metal oxide powder 80mg
Material, PVDF10mg do conductive agent, and acetylene black 10mg makees binder and is fully ground uniformly, drips 0.8mlNMP dispersion mixings, fully
1h is ground, scrapes the electrode slice that thickness is 200um after sizing mixing uniformly on copper foil, electrode slice is placed in vacuum drying chamber dry
12h;
(6) assembled battery:Dried electrode slice is placed in anaerobism glove box and is assembled into button cell;
(7) chemical property is tested:Assembled battery carries out high rate performance with blue electric battery test system and follows respectively
Ring stability test, test result are shown in Fig. 1, Fig. 2, Fig. 3.
Fig. 1 is that NiVMn alloy strips are ground at 50 DEG C after corrosion oxidation in the ammonium sulfate of 1mol/L in embodiment 1
SEM figures, by particle diameter after material grinding known to this figure in 5-50um ranges, illustration be after amplification material surface formed it is more
Pore structure.
Fig. 2 is that NiVMn materials are fabricated to the multiplying power song that negative electrode of lithium ion battery is assembled into button cell test in embodiment 1
Line chart, by material known to this figure when current density is that 1000mA/g is restored to 50mA/g, specific capacity can remain 89.2%,
High rate performance is preferable.
Fig. 3 is that NiVMn materials are assembled into the discharge cycle performance test chart tested after button cell in embodiment 1,
The above specific capacity conservation rate, which is enclosed, by material circulation 200 known to this figure can reach 90% or more.
Embodiment 2
(1) preparation of alloy strip:The preparation of alloy strip:The atom content ratio of Ni, V, Mn are 15: 15: 70, with getting rid of band
Mode be made under the rotating speed of 1200rad/s-1800rad/s under protection of argon gas thickness be 20um, width be 2mm alloy
Band.
(2) removal alloying prepares nano porous metal:The alloy strip of step (1) is placed in beaker to the sulphur for using 1mol/L
Sour ammonium spontaneous corrosion 6h at 50 DEG C, and change an ammonium sulfate per 2h.
(3) high-temperature oxydation:Nano porous metal band deionized water prepared by step (2) is fully rinsed 3 times, it is ensured that
Material is placed in 50 DEG C of dry 4-6h in air dry oven after no ammonium sulfate remnants.Metal band after drying is placed in high temperature to burn
300 DEG C are warming up to 10 DEG C/min rates in freezing of a furnace, keeps the temperature 4h.
(4) it grinds:The metal material that step (3) aoxidizes is fully ground to grey black micron powder.
(5) electrode is applied:The ground metal oxide powder of step (4) is done into cathode according to metal oxide powder 80mg
Material, PVDF10mg do conductive agent, and acetylene black 10mg makees binder and is fully ground uniformly, drips 0.8mlNMP dispersion mixings, fully
1h is ground, scrapes the electrode slice that thickness is 200um after sizing mixing uniformly respectively on copper foil.Electrode slice is placed in vacuum drying chamber and is done
Dry 12h.
(6) assembled battery:Dried electrode slice is placed in anaerobism glove box and is assembled into button cell.
(7) chemical property is tested:Assembled battery carries out high rate performance with blue electric battery test system and follows respectively
Ring stability test.Test obtains material when current density is that 1000mA/g is restored to 50mA/g, and specific capacity can remain
88.6%, high rate performance is preferable, and specific capacity conservation rate is 90% or more after 200 circle of cycle.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (7)
1. a kind of preparation method of ternary nano porous nickel vanadium manganese oxide electrode material, it is characterised in that:Include the following steps:
(1) preparation of alloy strip:Nickel vanadium manganese Metal particle is prepared into 20-50 μm of band, the wherein atom of Mn by getting rid of band
Content is 60-70%, and the atom content of Ni is 20-30%, and the atom content of V is 5-20%;
(2) removal alloying is handled:Alloy strip prepared by step (1) carries out chemical removal alloying processing, by the parts metal Mn
It erodes and is prepared into porous metals, the atom content of Mn is 20-40% after corrosion;
(3) high-temperature oxydation:The porous metals corroded in step (2) are heated in sintering furnace high temperature, heat preservation prepares nanoporous
Metal oxide;
(4) it grinds:By step (3) prepare nano porous metal oxide be put into mortar be fully ground to particle be micron order
Obtain metal oxide powder;
(5) electrode is applied:Metal oxide powder prepared by step (4) and Kynoar (PVDF), acetylene black and N- methyl
Pyrrolidones (NMP) is uniformly mixed is fully ground according to a certain percentage, and by the mixture blade applicator after grinding on copper foil
It scrapes electrode slice and obtains electrode material;
(6) assembled battery:By step (5) obtained electrode material as being assembled into lithium ion battery in anaerobism glove box;
(7) chemical property of battery and electrode material is tested.
2. a kind of preparation method of ternary nano porous nickel vanadium manganese oxide electrode material according to claim 1, special
Sign is:W metal, V, Mn choose the particle of a diameter of 1-3mm in the step (1), and the band rotating speed that gets rid of is 1200rad/
s-1800rad/s。
3. a kind of preparation method of ternary nano porous nickel vanadium manganese oxide electrode material according to claim 1, special
Sign is:Caustic solution in the step (2) is chemical corrosion method, and solution is weakly acidic ammonium sulfate, corrosion temperature
Degree is 50-70 DEG C, etching time 4-8h.
4. a kind of preparation method of ternary nano porous nickel vanadium manganese oxide electrode material according to claim 1, special
Sign is:The temperature that the step (3) is heated in sintering furnace is 200-400 DEG C, soaking time 1-5h.
5. a kind of preparation method of ternary nano porous nickel vanadium manganese oxide electrode material according to claim 1, special
Sign is:The nano porous metal of the step (3) high-temperature oxydation is positioned in mortar fully by the grinding in the step (4)
4-10h is ground, until micron powder of the linishing at grey black.
6. a kind of preparation method of ternary nano porous nickel vanadium manganese oxide electrode material according to claim 1, special
Sign is:The mixed proportion of metal oxide powder in the step (5), acetylene black and PVDF are 8: 1: 1, are dripped after mixing
Suitable NMP dispersion mixings, the electrode slice of different-thickness is made in slurry on copper foil after sizing mixing uniformly, and electrode slice is placed in vacuum
Dry 6-12h in drying box.
7. according to a kind of preparation side of ternary nano porous nickel vanadium manganese oxide electrode material of claim 1-6 any one of them
Ternary nano porous nickel vanadium manganese oxide electrode material prepared by method.
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Cited By (1)
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CN113258050A (en) * | 2020-12-23 | 2021-08-13 | 天津工业大学 | Five-element high-entropy alloy oxide negative electrode material and preparation method and application thereof |
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CN107887178A (en) * | 2017-10-16 | 2018-04-06 | 天津工业大学 | A kind of nanoporous nickel vanadium manganese/oxide combination electrode and preparation method thereof |
CN107958992A (en) * | 2017-11-09 | 2018-04-24 | 天津工业大学 | Porous binary NiMn oxide lithium cell negative pole materials and preparation method thereof |
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US20170225955A1 (en) * | 2014-09-09 | 2017-08-10 | Tohoku Techno Arch Co., Ltd. | Method for producing porous graphite, and porous graphite |
CN104900907A (en) * | 2015-06-12 | 2015-09-09 | 宁德时代新能源科技有限公司 | Preparation method of slurry for lithium ion batteries |
CN107887178A (en) * | 2017-10-16 | 2018-04-06 | 天津工业大学 | A kind of nanoporous nickel vanadium manganese/oxide combination electrode and preparation method thereof |
CN107958992A (en) * | 2017-11-09 | 2018-04-24 | 天津工业大学 | Porous binary NiMn oxide lithium cell negative pole materials and preparation method thereof |
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CN113258050A (en) * | 2020-12-23 | 2021-08-13 | 天津工业大学 | Five-element high-entropy alloy oxide negative electrode material and preparation method and application thereof |
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