CN108394881A - A kind of preparation method of lithium ion anode material nm delta-VOPO4 - Google Patents
A kind of preparation method of lithium ion anode material nm delta-VOPO4 Download PDFInfo
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- CN108394881A CN108394881A CN201810134313.4A CN201810134313A CN108394881A CN 108394881 A CN108394881 A CN 108394881A CN 201810134313 A CN201810134313 A CN 201810134313A CN 108394881 A CN108394881 A CN 108394881A
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- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 37
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000010405 anode material Substances 0.000 title claims abstract description 29
- 229910000540 VOPO4 Inorganic materials 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 20
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- 238000013019 agitation Methods 0.000 claims abstract description 8
- KJDNAUVRGACOHX-UHFFFAOYSA-N sulfuric acid;vanadium Chemical compound [V].OS(O)(=O)=O KJDNAUVRGACOHX-UHFFFAOYSA-N 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 229910000474 mercury oxide Inorganic materials 0.000 claims abstract description 6
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 6
- 238000000967 suction filtration Methods 0.000 claims abstract description 6
- 229910000351 vanadium(III) sulfate Inorganic materials 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000001238 wet grinding Methods 0.000 claims abstract description 6
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 3
- 238000012545 processing Methods 0.000 claims abstract description 3
- 238000002604 ultrasonography Methods 0.000 claims abstract description 3
- UUUGYDOQQLOJQA-UHFFFAOYSA-L vanadyl sulfate Chemical compound [V+2]=O.[O-]S([O-])(=O)=O UUUGYDOQQLOJQA-UHFFFAOYSA-L 0.000 claims abstract description 3
- 238000005119 centrifugation Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000005242 forging Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- FNLJLQUTIUDEHI-UHFFFAOYSA-N phosphoric acid vanadium Chemical compound [V].OP(O)(O)=O FNLJLQUTIUDEHI-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 description 8
- 239000002086 nanomaterial Substances 0.000 description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- 229910052744 lithium Inorganic materials 0.000 description 5
- 229920002620 polyvinyl fluoride Polymers 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011236 particulate material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
- C01B25/372—Phosphates of heavy metals of titanium, vanadium, zirconium, niobium, hafnium or tantalum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
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- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a kind of lithium ion anode material nm delta VOPO4Preparation method, steps are as follows：By vanadic sulfate V2(SO4)3It is added in deionized water, strong magnetic agitation makes it fully dissolve, and is configured to sulfuric acid vanadium solution；The mixed solution of hydrogen peroxide and phosphoric acid is slowly added to obtain mixed solution in above-mentioned sulfuric acid vanadium solution；Then reaction kettle that mixed solution is put into polytetrafluoroethylene (PTFE) carries out hydro-thermal reaction；After reaction, the yellow mercury oxide of acquisition is subjected to centrifugal filtration, and carries out high-temperature calcination in Muffle furnace, taken out after calcining furnace cooling；Using wet grinding, the product of acquisition is ground in absolute ethyl alcohol, and to ground nm delta VOPO4Progress ultrasound, suction filtration, washing and drying and processing are add to deionized water to get target product.Lithium ion anode material prepared by the present invention possesses fabulous δ VOPO4Microstructure, unique layer structure provide thinking for improving anode material for lithium-ion batteries cycle performance.
Description
Technical field
The invention belongs to technical field of new energy material preparation, and in particular to a kind of high circulation performance lithium ion cell positive
Material nano δ-VOPO4Preparation method.
Background technology
For lithium ion battery because it is with high working voltage, high-energy density, self-discharge rate is low, has extended cycle life, and uses temperature
It is wider to spend range, without memory effect, the advantages that open-circuit voltage is high, has been widely used in such as laptop, hand
Machine, the field of mobile equipment such as camera, is gradually replacing traditional energy.However in the extension process of lithium ion battery,
Various problem is encountered, is exactly that its ring performance is poor there are one important problem, in smart mobile phone field, mobile phone uses
Time does not exceed generally 2 years, and for charging times after more than 500 times, specific capacity is opposite to have prodigious loss.
Invention content
For problems of the prior art, the present invention provides a kind of lithium ion anode material nm delta-VOPO4System
Preparation Method, lithium ion anode material nm delta-VOPO obtained4, since its unique lattice structure is in lithium ion cell positive material
There is fabulous effect in terms of the cycle of material.
In order to solve the above technical problems, the present invention uses following technical scheme：
A kind of lithium ion anode material nm delta-VOPO4Preparation method, steps are as follows：
(1) by vanadic sulfate V2(SO4)3It is added in deionized water, magnetic agitation makes it fully dissolve, and is configured to sulfuric acid vanadium solution；
(2) mixed solution of hydrogen peroxide and phosphoric acid is slowly added to obtain mixed system in above-mentioned sulfuric acid vanadium solution；
(3) reaction kettle that mixed system is put into polytetrafluoroethylene (PTFE) carries out hydro-thermal reaction；
(4) after reaction, the yellow mercury oxide of acquisition is subjected to centrifugal filtration, and carries out high-temperature calcination in Muffle furnace, wait forging
Furnace cooling is burnt but to take out afterwards；
(5) wet grinding is used, by step（4）The product obtained after calcining is ground in absolute ethyl alcohol, is added after ground
To progress ultrasound, suction filtration, washing and drying and processing in deionized water to get target product lithium ion anode material nm delta-
VOPO4。
The step（1）Middle sulfuric acid vanadium solution it is a concentration of（0.005 ~ 0.02）g/mL.
The step（1）The middle magnetic agitation time is（1~4）h.
The step（2）The volume ratio of middle hydrogen peroxide and phosphoric acid is 10:（3-4.5）, the mass fraction of hydrogen peroxide is
37.5%, the mass fraction of phosphoric acid is 85%；The volume ratio of the mixed solution and phosphoric acid vanadium solution is（1.3-1.45）:15.
The step（3）The temperature of middle hydro-thermal reaction is（160 ~ 180）DEG C, the time of hydro-thermal reaction is（45 ~ 50）
h。
The step（4）The rotating speed of centrifuge is 6000 r/min, centrifugation time 8min when middle centrifugation.
The step（4）In Muffle furnace carry out high-temperature calcination when calcination temperature be（550 ~ 650）DEG C, calcination time
For（1.5 ~ 3.5）H, heating rate are 5 DEG C/min.
The step（5）The time of middle grinding is 10-12 hours, and the ultrasonic time is 8-10 hours.
The step（5）The temperature of middle drying is（75 ~ 90）DEG C, drying time is（10 ~ 15）h.
Beneficial effects of the present invention：δ-VOPO prepared by the present invention4There is phase in terms of the cycle performance of lithium ion battery
To larger promotion.δ-VOPO4In the crystal structure figure of different directions, the δ-VOPO in structure4And H2VOPO4Be it is quite similar,
H2VOPO4δ-VOPO4, δ-VOPO can be obtained by deviating from proton by electrochemistry4It is VO6Octahedra and PO4Tetrahedron corner-sharing links
Made of.VO6Octahedron shares apex angle O above and below direction1Atom is arranged in zigzag and PO4Tetrahedron shares other four oxygen
Atom, due to VO6Middle V-O and V=O is alternately so that VO6Octahedral arrangement seems unordered, PO4Other two angle and VO6Two
A angle connection, such be deposited on c-axis generates empty tunnel, and the empty tunnel structure of zigzag is generated on [101] direction.
Lithium ion anode material prepared by the present invention possesses fabulous δ-VOPO4Microstructure, unique layer structure is for improving
Anode material for lithium-ion batteries cycle performance provides thinking.
Description of the drawings
Fig. 1 is the δ-VOPO prepared by the embodiment of the present invention 14XRD diagram.
Fig. 2 is the δ-VOPO prepared by the embodiment of the present invention 14SEM figure.
Fig. 3 is the δ-VOPO prepared by the embodiment of the present invention 14Cycle performance figure under the conditions of 0.1C.
Specific implementation mode
With reference to specific embodiment, the present invention will be further described.It should be understood that following embodiment is merely to illustrate this
The person skilled in the art of the range of invention and is not intended to limit the present invention, the field can make one according to the content of foregoing invention
A little nonessential modifications and adaptations.
Embodiment 1
Lithium ion anode material nm delta-the VOPO of the present embodiment4Preparation method, steps are as follows：
（1）By 1.5g vanadic sulfates V2(SO4)3It is added in the deionized water of 150mL, strong magnetic agitation 2h makes it fully dissolve, and prepares
At the uniform solution of a concentration of 0.01 g/mL；
（2）The mixed solution of 85% phosphoric acid of the hydrogen peroxide of 10mL 37.5% and 3.5mL is slowly added to obtain in above-mentioned solution
Mixed system；
（3）Above-mentioned mixed system is transferred to the reaction kettles of four polyvinyl fluorides of the 200mL hydro-thermal reaction 48h at 170 DEG C；
（4）After reaction, the yellow mercury oxide obtained in step (3) is subjected to centrifugal filtration, 600 DEG C of heat preservations in Muffle furnace
2h takes out after cooling with calcining furnace；
（5）Using wet grinding, by step（4）The product of acquisition grinds 12h in absolute ethyl alcohol, and is dissolved in deionized water and surpassing
Sound 9h, suction filtration, washing and 70 DEG C of drying 15h are to get target product lithium ion anode material nm delta-VOPO4。
Fig. 1 is prepared δ-VOPO4XRD diagram, found after comparison prepare product crystal form it is excellent, purity is higher, knot
Brilliant degree is preferable.
Fig. 2 is prepared δ-VOPO4SEM figures, schemed by SEM shown in, material by being about 300 nm particulate material groups,
The slightly larger grain diameter in part is 500 nm, prepared monoclinic system δ-VOPO4Material is nanostructure, because of nanometer
Structure has many advantages, such as following as lithium ion anode material：Its micropore is more as lithium ion anode material for nano material, Chu Li
Mechanism is complicated, including adsorption storage lithium, the embedding lithium of lattice, micro-porous adsorption store lithium and the embedding lithium of lattice defect etc., therefore nano material
It is high to store lithium capacity, secondly, the grain size of nano material is small, and nano material is spread inside it for lithium ion provides shorter distance,
And embedded depth is shallower, is more advantageous to the deintercalation of lithium ion, good electrode kinetics is provided for electrode.So preparing
Monoclinic system δ-VOPO4Material both topographically has the advantages of above nano material is as lithium ion cell positive.
Fig. 3 is cycle performance curve, and under conditions of carrying out multiple charge-discharge test, there is no apparent drops for specific capacity
Low, for coulombic efficiency still above 99%, this illustrates that system reaches stable, also demonstrates under such condition, the stability of material compared with
It is good.
Embodiment 2
Lithium ion anode material nm delta-the VOPO of the present embodiment4Preparation method, steps are as follows：
（1）By 0.75g vanadic sulfates V2(SO4)3It is added in the deionized water of 150mL, strong magnetic agitation 2h makes it fully dissolve, and matches
The uniform solution of a concentration of 0.005 g/mL is made；
（2）The mixed solution of 85% phosphoric acid of the hydrogen peroxide of 10mL 37.5% and 3mL is slowly added to be mixed in above-mentioned solution
Zoarium system；
（3）Above-mentioned mixed system is transferred to the reaction kettles of four polyvinyl fluorides of the 200mL hydro-thermal reaction 50h at 160 DEG C；
（4）After reaction, the yellow mercury oxide obtained in step (3) is subjected to centrifugal filtration, is 5 DEG C/min's in heating rate
550 DEG C of heat preservation 3.5h of Muffle furnace, take out after cooling with calcining furnace；
（5）Using wet grinding, by step（4）The product of acquisition grinds 10h in absolute ethyl alcohol, and is dissolved in deionized water and surpassing
Sound 10h, suction filtration, washing, 80 DEG C of drying 12h are to get target product lithium ion anode material nm delta-VOPO4。
Embodiment 3
Lithium ion anode material nm delta-the VOPO of the present embodiment4Preparation method, steps are as follows：
（1）By 3g vanadic sulfates V2(SO4)3It is added in the deionized water of 150mL, strong magnetic agitation 2h makes it fully dissolve, and is configured to
The uniform solution of a concentration of 0.02 g/mL；
（2）The mixed solution of 85% phosphoric acid of the hydrogen peroxide of 10mL 37.5% and 4.5mL is slowly added to obtain in above-mentioned solution
Mixed system；
（3）Above-mentioned mixed system is transferred to the reaction kettles of four polyvinyl fluorides of the 200mL hydro-thermal reaction 45h at 180 DEG C；
（4）After reaction, the yellow mercury oxide obtained in step (3) is subjected to centrifugal filtration, is 5 DEG C/min's in heating rate
650 DEG C of heat preservation 1.5h of Muffle furnace, take out after cooling with calcining furnace；
（5）Using wet grinding, by step（4）The product of acquisition grinds 11h in absolute ethyl alcohol, and is dissolved in deionized water and surpassing
Sound 8h, suction filtration, washing and 90 DEG C of drying 10h are to get target product lithium ion anode material nm delta-VOPO4。
The basic principles and main features and advantages of the present invention of the present invention have been shown and described above.The skill of the industry
Art personnel it should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (9)
1. a kind of lithium ion anode material nm delta-VOPO4Preparation method, it is characterised in that steps are as follows：
（1）By vanadic sulfate V2(SO4)3It is added in deionized water, magnetic agitation makes it fully dissolve, and is configured to sulfuric acid vanadium solution；
（2）The mixed solution of hydrogen peroxide and phosphoric acid is slowly added to obtain mixed system in above-mentioned sulfuric acid vanadium solution；
（3）The reaction kettle that mixed system is put into polytetrafluoroethylene (PTFE) carries out hydro-thermal reaction；
（4）After reaction, the yellow mercury oxide of acquisition is subjected to centrifugal filtration, and carries out high-temperature calcination in Muffle furnace, wait forging
Furnace cooling is burnt but to take out afterwards；
（5）Using wet grinding, by step（4）The product obtained after calcining is ground in absolute ethyl alcohol, is added after ground
To progress ultrasound, suction filtration, washing and drying and processing in deionized water to get target product lithium ion anode material nm delta-
VOPO4。
2. lithium ion anode material nm delta-VOPO according to claim 14Preparation method, it is characterised in that：The step
Suddenly（1）Middle sulfuric acid vanadium solution it is a concentration of（0.005 ~ 0.02）g/mL.
3. lithium ion anode material nm delta-VOPO according to claim 14Preparation method, it is characterised in that：The step
Suddenly（1）The middle magnetic agitation time is（1~4）h.
4. lithium ion anode material nm delta-VOPO according to claim 14Preparation method, it is characterised in that：The step
Suddenly（2）The volume ratio of middle hydrogen peroxide and phosphoric acid is 10:（3-4.5）, the mass fraction of hydrogen peroxide is 37.5%, the matter of phosphoric acid
It is 85% to measure score；The volume ratio of the mixed solution and phosphoric acid vanadium solution is（1.3-1.45）:15.
5. lithium ion anode material nm delta-VOPO according to claim 14Preparation method, it is characterised in that：The step
Suddenly（3）The temperature of middle hydro-thermal reaction is（160 ~ 180）DEG C, the time of hydro-thermal reaction is（45 ~ 50）h.
6. lithium ion anode material nm delta-VOPO according to claim 14Preparation method, it is characterised in that：The step
Suddenly（4）The rotating speed of centrifuge is 6000 r/min, centrifugation time 8min when middle centrifugation.
7. lithium ion anode material nm delta-VOPO according to claim 14Preparation method, it is characterised in that：The step
Suddenly（4）In Muffle furnace carry out high-temperature calcination when calcination temperature be（550 ~ 650）DEG C, calcination time is（1.5 ~ 3.5）
H, heating rate are 5 DEG C/min.
8. lithium ion anode material nm delta-VOPO according to claim 14Preparation method, it is characterised in that：The step
Suddenly（5）The time of middle grinding is 10-12 hours, and the ultrasonic time is 8-10 hours.
9. lithium ion anode material nm delta-VOPO according to claim 14Preparation method, it is characterised in that：The step
Suddenly（5）The temperature of middle drying is（75 ~ 90）DEG C, drying time is（10 ~ 15）h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113457700A (en) * | 2021-06-24 | 2021-10-01 | 浙江大学 | Vanadium-phosphorus-oxygen catalyst for aldol condensation and preparation method and application thereof |
| WO2024113626A1 (en) * | 2022-11-30 | 2024-06-06 | 格林美（无锡）能源材料有限公司 | High-nickel ternary positive electrode material using lithium fast-ion conductor as coating layer, preparation method therefor, and application thereof |
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|---|---|---|---|---|
| CN1712406A (en) * | 2004-06-25 | 2005-12-28 | 廖立兵 | Vanadium phosphate compound with hole-channel structure and synthesis thereof |
| CN102496718A (en) * | 2011-12-29 | 2012-06-13 | 哈尔滨工业大学 | Preparation method of lithium ion battery anode material Li3V2(PO4)3 |
| CN106025275A (en) * | 2016-08-11 | 2016-10-12 | 安徽工业大学 | Vanadium phosphate sodium composite nano porous cathode material and method for preparing material by using freeze drying method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN113457700A (en) * | 2021-06-24 | 2021-10-01 | 浙江大学 | Vanadium-phosphorus-oxygen catalyst for aldol condensation and preparation method and application thereof |
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