CN110518202A - A kind of V of self-supporting2O5/ rGO nano-array sodium-ion battery material and preparation method thereof - Google Patents
A kind of V of self-supporting2O5/ rGO nano-array sodium-ion battery material and preparation method thereof Download PDFInfo
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- CN110518202A CN110518202A CN201910718603.8A CN201910718603A CN110518202A CN 110518202 A CN110518202 A CN 110518202A CN 201910718603 A CN201910718603 A CN 201910718603A CN 110518202 A CN110518202 A CN 110518202A
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- 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
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- 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
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
Abstract
The present invention provides a kind of redox graphene (rGO) modified self-supporting V2O5The preparation method of nano-array.Specifically it will continue to be rinsed with a large amount of deionized water after the ultrasonic cleaning of nickel foam dilute hydrochloric acid.V2O5/ rGO nano-array is evenly distributed in Ni substrate, and unit area V2O5The amount of/rGO active material is 4-5 mgcm‑2.The V2O5/ rGO nano-array sodium-ion battery negative electrode tab is added after dilute hydrochloric acid adjusts solution ph to 2.0-4.0 using ammonium metavanadate as raw material, under condition of water bath heating and chemically reacts under hydrothermal conditions, obtains V after annealing in air2O5Nano-array.High temperature reduction in a nitrogen atmosphere after then being coated with GO solution to above-mentioned nano-array, obtains V2O5/ rGO nano-array.The sodium ion negative electrode material synthetic method is simple, easily operated.By V2O5The sodium ion half-cell stable cycle performance that/rGO nano-array negative electrode tab is assembled into, has potential application in sodium-ion battery.
Description
Technical field
The present invention relates to a kind of novel array type anode material of lithium-ion battery, in particular to a kind of nano-array patterns
V2O5The preparation method of/rGO sodium-ion battery array material, belongs to sodium-ion battery field.
Background technique
With rapid economic development, the importance of the energy is continuously improved.With traditional fossil energy such as coal, petroleum, natural
Gas etc. further consumes, this problems demand of energy shortage solves.Lithium ion battery is as a kind of novel energy-storing equipment, due to it
Had high-energy-density, low self-discharge rate, long-life, memory-less effect, advantages of environment protection, become research hotspot,
It is widely used in portable electronic device and electric car at present.But with the extensive use of lithium ion battery, lithium
Resource reserve deficiency becomes the lethal factor of limiting lithium ion cell development.The reserves of sodium element on earth far more than lithium, and
Sodium-ion battery working principle is similar with lithium ion battery, therefore sodium-ion battery becomes effective substitution production of lithium ion battery
Product.Stratiform transition metal oxide is always the research hotspot of energy field, wherein V2O5Due at low cost, resourceful and peace
The advantage of Quan Xinggao is widely used in supercapacitor and lithium ion battery plus-negative plate, but it is few be used for sodium ion electricity
The report of pond cathode.Due to Na+Radius is larger, V2O5Sluggish kinetics caused by electron conduction difference also causes poor
Chemical property, and then limit V2O5In further applying for sodium-ion battery.
Summary of the invention
In view of the above-mentioned problems, this patent has synthesized a kind of self-supporting V using hydro-thermal method2O5Nano-array material, by V2O5With
It is combined with three-dimensional Ni net, further by rGO coating modification, improves the electric conductivity and cyclical stability of electrode material.With it
As sodium-ion battery binder free cathode, apparent charge and discharge platform and preferable cycle performance are shown, is had great
Potential using value.
It is an object of the invention to be raw material using Ni net as substrate using ammonium metavanadate, solution ph is adjusted, it is anti-by hydro-thermal
V should be prepared using high temperature and high pressure environment2O5The presoma of nano-array obtains V after further making annealing treatment in air2O5It receives
Rice array is then added after the drying of GO solution in N2Annealing obtains self-supporting V under atmosphere2O5/ rGO nano-array.
Raw material according to the present invention is ammonium metavanadate, hydrochloric acid, Ni net and GO solution.First by inclined vanadium in material preparation process
Sour ammonium, which is placed in container and deionized water is added, is placed in 35-80o0.2-1h is stirred in C water-bath, ammonium metavanadate aqueous solution
Concentration is 0.005-0.1mol/L, and hydrochloric acid liquid is added dropwise after it is completely dissolved, and (concentration of hydrochloric acid liquid is 1-
4mol L-1) pH value of solution is adjusted to 2-4.Then the above solution is transferred in hydrothermal reaction kettle and processed Ni net is added and existed
150-200 oC hydro-thermal reaction 10-24 h, then further 350-600 in airoV is obtained after C annealing 1-5h2O5Array.
For the electric conductivity and cyclical stability for improving material, then by V2O5It is 2-10 mg mL that array, which immerses concentration,-11-5 in GO solution
It is dried after h, in N2Annealing obtains the self-supporting V that rGO is coated completely under environment2O5/ rGO nano-array.
The self-supporting V of invention2O5/ rGO nano-array sodium ion negative electrode material and preparation method thereof has following spy
Point:
(1) preparation cost of the present invention is low, experimentation is simple, easily operates.
(2) V that the present invention obtains2O5/ rGO nano-array covers uniformly on base material, and contact is close.
(3) V is prepared2O5/ rGO nano-array length is 5-20 μm, and width is 0.5-3.0 μm, and array is by nanometer
Particle assembles, the pattern with even porous.And rGO clad is completely covered on V2O5Array surface improves leading for array
Electrically.Array is connected integral, provides good channel for electron-transport, and guarantee its stable structure in cyclic process
Property.
(4) the self-supporting V being prepared2O5/ rGO nano-array material unit area active material quality is 4-5 mg
cm-2, V in the case where such high active substance load capacity2O5/ rGO electrode still has more stable electrochemistry cycle performance.
Detailed description of the invention:
Fig. 1 is the XRD spectrum of sample prepared by embodiment 1.
Fig. 2 is the SEM figure of sample prepared by embodiment 1.
Fig. 3 is the charge-discharge performance figure (a) and (b) cycle performance figure of sample prepared by embodiment 1
Fig. 4 is the XRD spectrum of sample prepared by embodiment 1.
Fig. 5 is the SEM figure of sample prepared by embodiment 1.
Fig. 6 is the charge-discharge performance figure (a) and (b) cycle performance figure of sample prepared by embodiment 1
Fig. 7 is the SEM figure of sample prepared by embodiment 2.
Fig. 8 is the charge-discharge performance figure (a) and (b) cycle performance figure of sample prepared by embodiment 2.
Fig. 9 is the SEM figure of sample prepared by embodiment 3.
Figure 10 is the charge-discharge performance figure (a) and (b) cycle performance figure of sample prepared by embodiment 3.
Specific embodiment:
Embodiment 1
0.01 mol ammonium metavanadate powder is placed in a beaker and is added 70 mL deionized waters, places it in 75oIn C water-bath
30 min are persistently stirred, it is 2 mol L that concentration is added dropwise after it is completely dissolved-1Hydrochloric acid solution adjust pH value to 4.0.It will
The above solution is transferred in 100 mL hydrothermal reaction kettles and nickel foam (3 × 7 cm is added2) 180o24 h of hydro-thermal reaction under C,
Middle nickel foam is leant against in water heating kettle with 60 ° of angles, and further in air 500o1 h of C annealing obtains V2O5Nano-array.With
After be dipped in 3 mL GO solution (concentration be 5mg mL-1) in, in N after drying2550 under atmosphereoIt anneals under C and obtains after 1 h
V2O5/ rGO nano-array.Fig. 1 is the V being prepared2O5The XRD spectrum of nano-array.It can be seen that in addition to Ni and NiO and V3O7
Characteristic peak except, there is V at 15.3 °, 20.3 °, 21.7 °, 25.9 °, 30.8 °, 32.2 °, 34.1 ° and 51.4 ° respectively2O5
Characteristic peak, XRD spectrum and V2O5(JCPDS No .41-1426) card is consistent.Such as Fig. 2, to the V during synthesis2O5
V after nano-array and cladding2O5/ rGO nano-array carries out SEM characterization.It can be seen that the V being prepared2O5For nano strip
Pattern, width are 2-3 μm, and length is 10-20 μm, and it is online (Fig. 2 a) to be evenly distributed in Ni.Fig. 2 b, c are respectively to recycle
The V of front and back2O5The SEM image of/rGO nano-array, it can be seen that rGO is coated on V2O5Nano-array surface, and pattern after circulation
Still maintain complete.It is assembled into sodium ion half-cell as negative electrode material, in 200 mAh g-1It is carried out under current density
Charge-discharge test, first discharge specific capacity reach 1010.7 mAh g-1, preceding 20 circle capacity attenuation to 200 mAh g-1, behind hold
Amount keeps stablizing.Still there are 140 mAh g after 200 circle circulations-1Specific capacity (Fig. 3 b), coulombic efficiency close to 100%,
Show preferable chemical property.
Embodiment 2
0.01 mol ammonium metavanadate powder is placed in a beaker and is added 70 mL deionized waters, places it in 75oIn C water-bath
30 min are persistently stirred, it is 2 mol L that concentration is added dropwise after it is completely dissolved-1Hydrochloric acid solution adjust pH value to 4.0.It will
The above solution is transferred in 100 mL hydrothermal reaction kettles and nickel foam (3 × 7 cm is added2) 180o24 h of hydro-thermal reaction under C,
Middle nickel foam is leant against in water heating kettle with 60 ° of angles, and then further in air 500oV is obtained after 1 h of C annealing2O5Nanometer
Array.Fig. 4 is the V that preparation etc. obtains2O5The XRD spectrum of nano-array.It can be seen that other than the characteristic peak of Ni, remaining peak
And V2O5(JCPDS No .41-1426) card is consistent.Such as Fig. 5, SEM characterization is carried out to it can be seen that being prepared
V2O5For nano strip pattern, width is 1-3 μm, and length is 10-20 μm, and nano particle assembles, by and uniform distribution
It is online in Ni.It is assembled into sodium ion half-cell as negative electrode material, in 200 mAh g-1Charge and discharge is carried out under current density
Electrical testing, discharge capacity reaches 1057.2 mAh g for the first time-1, preceding 50 circle capacity attenuation to 138 mAh g-1, behind capacity keep
Stablize.Still there are 87 mAh g after 200 circle circulations-1Specific capacity (Fig. 6 b), coulombic efficiency close to 100%, show compared with
Good chemical property.
Embodiment 3
0.01 mol ammonium metavanadate powder is placed in a beaker and is added 70 mL deionized waters, places it in 75oIn C water-bath
30 min are persistently stirred, it is 2 mol L that concentration is added dropwise after it is completely dissolved-1Hydrochloric acid solution adjust pH value to 2.0.It will
The above solution is transferred in 100 mL hydrothermal reaction kettles and nickel foam (3 × 7 cm is added2) 180o24 h of hydro-thermal reaction under C,
Middle nickel foam is leant against in water heating kettle with 60 ° of angles, and then further in air 500o1 h of C annealing obtains V2O5Nanometer battle array
Column.Such as Fig. 7, SEM characterization is carried out to it can be seen that the V being prepared2O5For nano-chip arrays pattern, width is 2-4 μm, long
Degree is 2-4.5 μm, is assembled by nano particle, has apparent pore structure.Half electricity is assembled in the way of embodiment 1
Pond is tested, and Fig. 8 shows V prepared by embodiment 22O5Nano-array is in 200 mAh g-1Under current density, discharge for the first time
Capacity reaches 1025.7 mAh g-1.Capacity tends towards stability after 200 circulations, and capacity maintains 85 mAh g-1, show
Preferable chemical property.
Embodiment 4
0.01 mol ammonium metavanadate powder is placed in a beaker and is added 70 mL deionized waters, places it in 75oIn C water-bath
30 min are persistently stirred, it is 2 mol L that concentration is added dropwise after it is completely dissolved-1Hydrochloric acid solution adjust pH value to 3.0.It will
The above solution is transferred in 100 mL hydrothermal reaction kettles and nickel foam (3 × 7 cm is added2) 180o24 h of hydro-thermal reaction under C,
Middle nickel foam is leant against in water heating kettle with 60 ° of angles, and then further in air 500oV is obtained after 1 h of C annealing2O5Nanometer
Array.Such as Fig. 9, SEM characterization is carried out to it can be seen that the V being prepared2O5For nano-array pattern, width is 0.5-2 μm,
Length is 5-20 μm.It assembles half-cell in the way of embodiment 1 to be tested, Figure 10 shows V prepared by embodiment 32O5
Nano-array is in 200 mAh g-1Under current density, discharge capacity reaches 1374 mAh g for the first time-1.Hold after 200 circulations
Amount tends towards stability, and capacity maintains 87 mAh g-1, show preferable chemical property.
Claims (9)
1. a kind of V of self-supporting2O5/ rGO nano-array sodium-ion battery material, it is characterised in that: the V2O5/ rGO nano-array
Assembled by nano particle, there is porous structure, V2O5/ rGO nano-array length is 5-20 μm, and width is 0.5-3.0 μ
M, with a thickness of 0.1-0.3 μm, and rGO is coated on V2O5Array surface.
2. the V of self-supporting according to claim 12O5/ rGO nano-array sodium-ion battery material, it is characterised in that:
V2O5The quality of/rGO nano material active material is 4-5 mgcm-2。
3. the V of self-supporting according to claim 1 or 22O5The preparation method of/rGO nano-array sodium-ion battery material,
It is characterized by:
(1) weigh ammonium metavanadate and deionized water is added is placed in water-bath and continue stirring until it and be completely dissolved, into solution by
It is added dropwise to the pH value that hydrochloric acid liquid adjusts solution, then above-mentioned solution is transferred in hydrothermal reaction kettle and is placed in Ni net inclination
V is prepared in wherein hydro-thermal reaction2O5Nano-array presoma, then annealing obtains V in air2O5Nano-array；
(2) by V2O5Nano-array is dried after immersing graphene oxide solution, and the array material after being completely dried is in nitrogen atmosphere
Lower annealing obtains self-supporting V2O5/ rGO nano-array.
4. the V of self-supporting as claimed in claim 32O5The preparation method of/rGO nano-array sodium-ion battery material, feature exist
In: the concentration of ammonium metavanadate aqueous solution is 0.005-0.1mol/L in step (1), and the concentration of hydrochloric acid liquid is 1-4mol L-1,
Adjust pH value to 2-4, the solid content of GO solution is 2-10 mg mL in step (2)-1。
5. the V of self-supporting as claimed in claim 32O5The preparation method of/rGO nano-array sodium-ion battery material, feature exist
In: it is 35-80 that heating water bath, which answers temperature, in step (1)oC, heating water bath time are 0.2-1.0 h.
6. the V of self-supporting as claimed in claim 32O5The preparation method of/rGO nano-array sodium-ion battery material, feature exist
In: hydrothermal temperature is 150-200 in step (1)oC, the hydro-thermal reaction time are 10-24 h.
7. the V of self-supporting as claimed in claim 32O5The preparation method of/rGO nano-array sodium-ion battery material, feature exist
In: annealing is temperature 350-650 in air in step (1)oC, anneal 1-5 h.
8. the V of self-supporting as claimed in claim 32O5The preparation method of/rGO nano-array sodium-ion battery material, feature exist
In: annealing is in N2In, temperature 300-600oC, anneal 1-5 h.
9. the V of self-supporting of any of claims 1 or 22O5/ rGO nano-array sodium-ion battery material is preparing sodium-ion battery
Application in negative electrode tab.
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Cited By (5)
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| CN111640921A (en) * | 2020-05-22 | 2020-09-08 | 大连海事大学 | Preparation method of vanadium compound electrode material and application of vanadium compound electrode material in water-based zinc ion battery |
| CN111785956A (en) * | 2020-07-10 | 2020-10-16 | 西安交通大学 | Flexible electrode material for lithium ion battery and preparation method thereof |
| WO2022048346A1 (en) * | 2020-09-03 | 2022-03-10 | 中南大学 | Vanadium pentoxide/rgo-coated lithium nickel cobalt manganese oxide positive electrode material and preparation method therefor |
| CN114853065A (en) * | 2022-05-26 | 2022-08-05 | 三峡大学 | W-doped V 2 O 5 Preparation method of self-assembled nano-sheet ball electrode material |
| CN116613304A (en) * | 2023-07-21 | 2023-08-18 | 帕瓦(长沙)新能源科技有限公司 | Containing water V 3 O 7 Graphene anode material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111640921A (en) * | 2020-05-22 | 2020-09-08 | 大连海事大学 | Preparation method of vanadium compound electrode material and application of vanadium compound electrode material in water-based zinc ion battery |
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| CN111785956B (en) * | 2020-07-10 | 2022-04-22 | 西安交通大学 | Flexible electrode material for lithium ion battery and preparation method thereof |
| WO2022048346A1 (en) * | 2020-09-03 | 2022-03-10 | 中南大学 | Vanadium pentoxide/rgo-coated lithium nickel cobalt manganese oxide positive electrode material and preparation method therefor |
| CN114853065A (en) * | 2022-05-26 | 2022-08-05 | 三峡大学 | W-doped V 2 O 5 Preparation method of self-assembled nano-sheet ball electrode material |
| CN116613304A (en) * | 2023-07-21 | 2023-08-18 | 帕瓦(长沙)新能源科技有限公司 | Containing water V 3 O 7 Graphene anode material and preparation method and application thereof |
| CN116613304B (en) * | 2023-07-21 | 2023-10-24 | 帕瓦(长沙)新能源科技有限公司 | Containing water V 3 O 7 Graphene anode material and preparation method and application thereof |
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