CN108975403A - A kind of variable composition vanadium oxide nanobelt and its synthetic method and application - Google Patents
A kind of variable composition vanadium oxide nanobelt and its synthetic method and application Download PDFInfo
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- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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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
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
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- 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
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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
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- H01M4/02—Electrodes composed of, or comprising, active material
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention belongs to nanometer energy storage material fields, more particularly to a kind of variable composition vanadium oxide nanobelt and its synthetic method and application, hydro-thermal reaction is carried out with presoma vanadium oxide colloidal sol and dehydrated alcohol, it or further include that reduction inducer carbon nanotube is additionally added in hydro-thermal reaction, or further include being sintered after hydro-thermal reaction, it is made respectively with V by above-mentioned differential responses combination3O7·H2O、VO2And V2O51-dimention nano band as main component.When 1-dimention nano band product is used as secondary lithium battery positive electrode active materials, excellent electrochemical lithium storage performance is shown, specific capacity is significantly higher than traditional anode material for lithium-ion batteries.This method realizes the synthesis of the one-dimensional vanadium oxide nanobelt of variable composition, process is simple, yield is higher and is easy to regulate and control by hydro-thermal and rear sintering processes.
Description
Technical field
The invention belongs to nanometer energy storage material fields, and in particular to a kind of variable composition vanadium oxide nanobelt and its synthesis side
Method and application.
Background technique
Current generation, energy and environmental problem are increasingly valued by people.With the non-renewable fossil energy of tradition
Exhaustion, find novel fungible energy source and corresponding energy-storage system be always the target of numerous researchers.Lithium-ion electric
Pond is a kind of important energy-storage units, is had been used in various portable electronic devices and power tool, such as mobile phone, notebook electricity
Brain and electric car etc., it has become energy supply carrier indispensable in the daily production of people and life.But its performance can not expire
The requirement of the current all kinds of new function devices of foot, therefore the performance for constantly promoting lithium ion battery is the only way which must be passed of future development.
In lithium ion battery, electrode material is the key that influence its performance to play, using Si, Sn and respective metal oxide as representative
Novel anode material huge number, specific capacity is thousands of easily, much higher than the positive electrode of current commercialization, so exploitation high capacity
Positive electrode is of great significance.
Vanadium oxide is a kind of lithium ion cell positive candidate material with high embedding lithium specific capacity, in recent years by researcher
Extensive concern, wherein Vanadium valence is generally adjustable between+3 to+5 valences, when be used as anode material for lithium-ion batteries when, embody compared with
High embedding lithium capacity, specific capacity are generally significantly higher than the LiFePO of current commercialization4、LiCoO2、LiMn2O4、LiNiO2And its
Their doped and compounded material (specific capacity is generally between 140-160mAh/g).It is visible much about vanadium oxide nanosizing in document
Modified report, such as zero dimension VOxNano particle/ball, one-dimensional VOxNano wire, nanotube, nanofiber and nanobelt etc., two dimension
VOxReceive piece, nano-plates etc. and numerous three-dimensional structure VOxNanometer hierarchical structure.These nanostructures itself and their phases
The nanocomposite answered shows very high specific capacity and excellent storage lithium performance.If the vanadium in vanadium oxide nanoparticle material
Valence state is+5 valences, and the specific capacity when being embedded in 3 lithium ions can be more than 400mAh/g.In the conjunction of above-mentioned vanadium oxide nanoparticle material
Cheng Zhong is related to many technologies, such as physical/chemical vapor deposition, Electrospun, electro-deposition, reverse micelle, collosol and gel, hydro-thermal and each
Template etc. under class wet-chemical environment, but in the method, much use accurate equipment, cumbersome preparation process and height
The relatively severe conditions such as pressure, vacuum.
Summary of the invention
In view of the above technical problems, the present invention provides a kind of variable composition vanadium oxide nanobelt and its synthetic method and answers
With, it is higher to obtain a kind of yield, and process flow is simple, is easy to the preparation method of regulation.
The specific technical proposal is: a kind of variable composition vanadium oxide nanobelt, with presoma vanadium oxide colloidal sol and dehydrated alcohol
Progress hydro-thermal reaction perhaps further includes that reduction inducer carbon nanotube is additionally added in hydro-thermal reaction or further includes that hydro-thermal is anti-
Should after be sintered, by above-mentioned differential responses combination respectively be made with V3O7·H2O、VO2And V2O5It is as main component one-dimensional
Nanobelt.
The one-dimensional vanadium oxide nanometer bandwidth of the variable composition that the present invention prepares is 100~500nm, with a thickness of 50~
200nm, length are generally more than 10 μm.
The synthetic method of the variable composition vanadium oxide nanobelt, comprising the following steps:
(1) vanadium oxide colloidal sol is prepared；
By V2O5Powder raw material is dispersed in deionized water, the hydrogenperoxide steam generator of concentration 30wt% is added, at room temperature
It is sufficiently stirred, forms vanadium oxide precursor sol after reaction 2~10 hours；V2O5Raw material and hydrogenperoxide steam generator dosage, according to matter
Amount/volume ratio is 1/1~1/30, and unit is grams per milliliter；
(2) the vanadium oxide nanobelt of different component is prepared respectively according to following three kinds of methods；
(a) step (1) described vanadium oxide colloidal sol is added in dehydrated alcohol, moves into and carries out hydro-thermal reaction 1~5 in water heating kettle
It, it is V that main component is obtained after centrifugation, washing and drying3O7·H2The blackish green nanobelt of O；In this step, it is added anhydrous
Ethyl alcohol and V2O5The mass ratio of raw material is 3wt%~50wt%；
(b) step (1) described vanadium oxide colloidal sol is added in dehydrated alcohol, and disperses carbon nanotube in this colloidal sol, passed through
Yellow black suspension is obtained after sonic oscillation, which is moved into water heating kettle, after 1~5 day hydro-thermal reaction, be centrifuged,
Washing and dry obtained main component are VO2Black and blue color nanobelt；In this step, dehydrated alcohol and V is added2O5The matter of raw material
Amount is than being 50wt%~200wt%；The reduction inducer carbon nanotube and V introduced in hydro-thermal2O5The mass ratio of raw material is 5wt%
~25wt%；
(c) by V obtained in (a) method3O7·H2O nanobelt is placed under air atmosphere and is sintered 2~6 hours, obtain with
V2O5Yellow nanometer band as main component.
Wherein, the method (a) in step (2) and hydrothermal temperature described in method (b) are 110 DEG C~200 DEG C.Hydro-thermal
The compactedness of reaction kettle is percent by volume 40%~90%.
Method (b) carbon nanotube is multi-walled carbon nanotube or single-walled carbon nanotube in step (2).
Method (c) sintering temperature is at 250 DEG C~550 DEG C in step (2).
The variable composition vanadium oxide nanobelt is used for anode material for lithium-ion batteries.It is prepared by the present invention respectively with three kinds not
With component one-dimensional vanadium oxide nanobelt as main component as lithium ion cell positive in use, all having higher embedding lithium ratio
Capacity, hence it is evident that better than traditional positive electrode active materials.This aspect is derived from the storage lithium characteristic of material itself, on the other hand has benefited from oxygen
Change the advantage of vanadium material nano.
One-dimensional vanadium oxide nanobelt synthetic method of the present invention, the more cheap V of use2O5For raw material, by simple
Precursor sol, the sintering processes in hydro-thermal and air atmosphere, can get the adjustable one-dimensional vanadium oxide nanobelt of component just
Pole active material compares other synthesis technologies reported in the literature, and this method with equipment requirement, be convenient for adjusting by simple, synthetic sample
Control and the advantage that can be prepared in batches.It is higher embedding that one-dimensional vanadium oxide nanobelt obtained shows more traditional positive electrode active material
Lithium capacity, while there is good cycle performance, novel high-capacity anode time can be provided for the exploitation of high performance lithium ion battery
Material selection.
Detailed description of the invention
Fig. 1 (a) is embodiment with V3O7·H2O one-dimensional vanadium oxide nanobelt SEM (scanning electron microscope) figure as main component；
Fig. 1 (b) is embodiment with VO2One-dimensional vanadium oxide nanobelt SEM figure as main component；
Fig. 1 (c) is embodiment with V2O5One-dimensional vanadium oxide nanobelt SEM figure as main component；
Fig. 2 (a) is embodiment with V3O7·H2O one-dimensional vanadium oxide nanobelt XRD (X-ray diffraction) figure as main component；
Fig. 2 (b) is embodiment with VO2One-dimensional vanadium oxide nanobelt XRD diagram as main component；
Fig. 2 (c) is embodiment with V2O5One-dimensional vanadium oxide nanobelt XRD diagram as main component；
Fig. 3 (a1) is embodiment with V3O7·H2O one-dimensional vanadium oxide nanobelt TEM (transmission electron microscope) figure as main component；
Fig. 3 (a2) is embodiment with V3O7·H2O one-dimensional vanadium oxide nanobelt HRTEM (high power transmission electricity as main component
Mirror) figure；
Fig. 3 (b1) is embodiment with VO2One-dimensional vanadium oxide nanobelt TEM figure as main component；
Fig. 3 (b2) is embodiment with VO2One-dimensional vanadium oxide nanobelt HRTEM figure as main component；
Fig. 3 (c1) is embodiment with V2O5One-dimensional vanadium oxide nanobelt TEM figure as main component；
Fig. 3 (c2) is embodiment with V2O5One-dimensional vanadium oxide nanobelt HRTEM figure as main component；
Fig. 4 (a) is embodiment with V3O7·H2O one-dimensional vanadium oxide nanobelt constant current charge-discharge curve as main component；
Fig. 4 (b) is embodiment with VO2One-dimensional vanadium oxide nanobelt constant current charge-discharge curve as main component；
Fig. 4 (c) is embodiment with V2O5One-dimensional vanadium oxide nanobelt constant current charge-discharge curve as main component；
Fig. 5 (a) is embodiment with V3O7·H2O one-dimensional vanadium oxide nanobelt cycle performance as main component；
Fig. 5 (b) is embodiment with VO2One-dimensional vanadium oxide nanobelt cycle performance as main component；
Fig. 5 (c) is embodiment with V2O5One-dimensional vanadium oxide nanobelt cycle performance as main component.
Specific embodiment
The present invention is specifically described and is illustrated below by example and attached drawing, it is necessary to be pointed out that the present embodiment only
For the present invention to be further detailed, it should not be understood as limiting the scope of the invention.
Embodiment 1:
One, the solation of vanadium oxide
By 0.92 gram of V2O5Powder is scattered in 50ml deionized water solution, and with hydrogen peroxide (30% mass concentration) with
The mass/volume of 1/3 (g/ml) than mixing, sufficiently react at room temperature, and orange-yellow oxidation is formed after 3 hours by magnetic agitation
Vanadium colloidal sol.
Two, with V3O7·H2O 1-dimention nano band preparation as main component
It takes 0.25ml dehydrated alcohol to be added in above-mentioned vanadium oxide colloidal sol, it is anti-that 100ml hydro-thermal is moved into after magnetic agitation mixes
It answers in kettle, after 2 days 150 DEG C of hydro-thermal reactions, obtains after centrifugation, washing and drying with V3O7·H2O as main component one
Tie up vanadium oxide nanobelt.
Obtained material detection structure such as Fig. 1 (a), Fig. 2 (a) and Fig. 3 (a1), Fig. 3 (a2) are shown, chemical property such as Fig. 4
(a) and shown in Fig. 5 (a).
Three, with VO21-dimention nano band preparation as main component
It takes 1.2ml dehydrated alcohol to be added to start in vanadium oxide colloidal sol obtained, while 0.18 gram of multi-wall carbon nano-tube is added
Pipe forms yellow black suspension through sonic oscillation, this suspension is moved into 100ml hydrothermal reaction kettle, anti-through 3 days 150 DEG C of hydro-thermals
Ying Hou, will be with VO by centrifugation, washing and dry be made2One-dimensional vanadium oxide nanobelt as main component.
Obtained material detection structure such as Fig. 1 (b), Fig. 2 (b) and Fig. 3 (b1), Fig. 3 (b2) are shown, chemical property such as Fig. 4
(b) and shown in Fig. 5 (b).
Four, with V2O51-dimention nano band preparation as main component
By hydrothermal synthesis with V3O7·H2300 DEG C of sintering 2 are small in air atmosphere for O one-dimensional vanadium oxide as main component
When, it obtains with V2O5The one-dimensional vanadium oxide nanobelt of yellow as main component.
Obtained material detection structure such as Fig. 1 (c), Fig. 2 (c) and Fig. 3 (c1), Fig. 3 (c2) are shown, chemical property such as Fig. 4
(c) and shown in Fig. 5 (c).
Embodiment 2:
One, the solation of vanadium oxide
By 1.82 grams of V2O5Powder is scattered in 75ml deionized water solution, and with hydrogen peroxide (30% mass concentration) with
The mass/volume of 1/2.76 (g/ml) than mixing, sufficiently react at room temperature, is formed after 4 hours orange-yellow by magnetic agitation
Vanadium oxide colloidal sol.
Two, with V3O7·H2O 1-dimention nano band preparation as main component
It takes 0.2ml dehydrated alcohol to be added in above-mentioned vanadium oxide colloidal sol, 100ml hydro-thermal reaction is moved into after magnetic agitation mixes
In kettle, after 2 days 180 DEG C of hydro-thermal reactions, obtain after centrifugation, washing and drying with V3O7·H2O is as main component one-dimensional
Vanadium oxide nanobelt.
Three, with VO21-dimention nano band preparation as main component
It takes 2.0ml dehydrated alcohol to be added to start in vanadium oxide colloidal sol obtained, while 0.2 gram of multi-walled carbon nanotube is added
Yellow black suspension is formed through sonic oscillation, this suspension is moved into 100ml hydrothermal reaction kettle, through 2 days 180 DEG C of hydro-thermal reactions
It afterwards, will be with VO by centrifugation, washing and dry be made2One-dimensional vanadium oxide nanobelt as main component.
Four, with V2O51-dimention nano band preparation as main component
By hydrothermal synthesis with V3O7·H2400 DEG C of sintering 3 are small in air atmosphere for O one-dimensional vanadium oxide as main component
When, it obtains with V2O5The one-dimensional vanadium oxide nanobelt of yellow as main component.
Embodiment 3:
One, the solation of vanadium oxide
By 1.38 grams of V2O5Powder is scattered in 140ml deionized water solution, and with hydrogen peroxide (30% mass concentration) with
The mass/volume of 1/20 (g/ml) than mixing, sufficiently react at room temperature, and orange-yellow oxygen is formed after 5 hours by magnetic agitation
Change vanadium colloidal sol.
Two, with V3O7·H2O 1-dimention nano band preparation as main component
It takes 0.25ml dehydrated alcohol to be added in above-mentioned vanadium oxide colloidal sol, it is anti-that 200ml hydro-thermal is moved into after magnetic agitation mixes
It answers in kettle, after 4 days 170 DEG C of hydro-thermal reactions, obtains after centrifugation, washing and drying with V3O7·H2O as main component one
Tie up vanadium oxide nanobelt.
Three, with VO21-dimention nano band preparation as main component
It takes 2.5ml dehydrated alcohol to be added to start in vanadium oxide colloidal sol obtained, while 0.14 gram of multi-wall carbon nano-tube is added
Pipe forms yellow black suspension through sonic oscillation, this suspension is moved into 200ml hydrothermal reaction kettle, anti-through 4 days 170 DEG C of hydro-thermals
Ying Hou, will be with VO by centrifugation, washing and dry be made2One-dimensional vanadium oxide nanobelt as main component.
Four, with V2O51-dimention nano band preparation as main component
By hydrothermal synthesis with V3O7·H2450 DEG C of sintering 4 are small in air atmosphere for O one-dimensional vanadium oxide as main component
When, it obtains with V2O5The one-dimensional vanadium oxide nanobelt of yellow as main component.
For embodiment described above only for illustrating technical idea and feature of the invention, its object is to make this field
Those of ordinary skill cans understand the content of the present invention and implement it accordingly, and the range of this patent is not limited merely to above-mentioned specific reality
Apply example, i.e., it is all according to same changes or modifications made by disclosed method, still it is included within the scope of protection of the present invention.
Claims (6)
1. a kind of variable composition vanadium oxide nanobelt, which is characterized in that carry out water with presoma vanadium oxide colloidal sol and dehydrated alcohol
Thermal response perhaps further includes that reduction inducer carbon nanotube is additionally added in hydro-thermal reaction or further includes that hydro-thermal reaction is laggard
Row sintering is made respectively with V by above-mentioned differential responses combination3O7·H2O、VO2And V2O51-dimention nano band as main component.
2. a kind of synthetic method of variable composition vanadium oxide nanobelt according to claim 1, which is characterized in that including with
Lower step:
(1) vanadium oxide colloidal sol is prepared；
By V2O5Powder raw material is dispersed in deionized water, the hydrogenperoxide steam generator of concentration 30wt% is added, at room temperature sufficiently
Stirring forms vanadium oxide precursor sol after reaction 2~10 hours；V2O5Raw material and hydrogenperoxide steam generator dosage, according to quality/
Volume ratio is 1/1~1/30, and unit is grams per milliliter；
(2) the vanadium oxide nanobelt of different component is prepared respectively according to following three kinds of methods；
(a) step (1) described vanadium oxide colloidal sol is added in dehydrated alcohol, moves into water heating kettle and carries out hydro-thermal reaction 1~5 day, passed through
It is V that main component is obtained after centrifugation, washing and drying3O7·H2The blackish green nanobelt of O；In this step, be added dehydrated alcohol with
V2O5The mass ratio of raw material is 3wt%~50wt%；
(b) step (1) described vanadium oxide colloidal sol is added in dehydrated alcohol, and disperses carbon nanotube in this colloidal sol, through ultrasound
Yellow black suspension is obtained after oscillation, and suspension immigration water heating kettle is centrifuged, is washed after 1~5 day hydro-thermal reaction
And dry obtained main component is VO2Black and blue color nanobelt；In this step, dehydrated alcohol and V is added2O5The mass ratio of raw material
For 50wt%~200wt%；The reduction inducer carbon nanotube and V introduced in hydro-thermal2O5The mass ratio of raw material be 5wt%~
25wt%；
(c) by V obtained in (a) method3O7·H2O nanobelt is placed under air atmosphere and is sintered 2~6 hours, obtains with V2O5
Yellow nanometer band as main component.
3. a kind of synthetic method of variable composition vanadium oxide nanobelt according to claim 2, which is characterized in that step
(2) hydrothermal temperature described in the method (a) and method (b) in is 110 DEG C~200 DEG C.
4. a kind of synthetic method of variable composition vanadium oxide nanobelt according to claim 2, which is characterized in that step
(2) method (b) carbon nanotube is multi-walled carbon nanotube or single-walled carbon nanotube in.
5. a kind of synthetic method of variable composition vanadium oxide nanobelt according to claim 2, which is characterized in that step
(2) method (c) sintering temperature is at 250 DEG C~550 DEG C in.
6. a kind of application of variable composition vanadium oxide nanobelt according to claim 1, which is characterized in that be used for lithium ion
Cell positive material.
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| CN110817959A (en) * | 2019-11-25 | 2020-02-21 | 清华大学 | V-shaped groove2O5Preparation method of nanobelt |
| CN110838583A (en) * | 2019-12-10 | 2020-02-25 | 华中科技大学 | Carbon nanotube/M-phase vanadium dioxide composite structure, preparation method thereof and application thereof in water-based zinc ion battery |
| CN113929140A (en) * | 2021-09-15 | 2022-01-14 | 扬州大学 | Transition metal doped V6O13Nanobelt material and preparation method and application thereof |
| CN115064679A (en) * | 2022-07-04 | 2022-09-16 | 佛山科学技术学院 | Vanadium oxide micron rod cluster and preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110817959A (en) * | 2019-11-25 | 2020-02-21 | 清华大学 | V-shaped groove2O5Preparation method of nanobelt |
| CN110817959B (en) * | 2019-11-25 | 2021-02-02 | 清华大学 | V-shaped groove2O5Preparation method of nanobelt |
| CN110838583A (en) * | 2019-12-10 | 2020-02-25 | 华中科技大学 | Carbon nanotube/M-phase vanadium dioxide composite structure, preparation method thereof and application thereof in water-based zinc ion battery |
| CN110838583B (en) * | 2019-12-10 | 2020-10-16 | 华中科技大学 | Carbon nanotube/M-phase vanadium dioxide composite structure, preparation method thereof and application thereof in water-based zinc ion battery |
| CN113929140A (en) * | 2021-09-15 | 2022-01-14 | 扬州大学 | Transition metal doped V6O13Nanobelt material and preparation method and application thereof |
| CN113929140B (en) * | 2021-09-15 | 2023-05-26 | 扬州大学 | V doped with transition metal 6 O 13 Nano belt material and preparation method and application thereof |
| CN115064679A (en) * | 2022-07-04 | 2022-09-16 | 佛山科学技术学院 | Vanadium oxide micron rod cluster and preparation method and application thereof |
| CN115064679B (en) * | 2022-07-04 | 2024-04-23 | 佛山科学技术学院 | Vanadium oxide micron rod cluster and preparation method and application thereof |
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