CN109502645A - A kind of preparation method and application of vanadic anhydride overlong nanowire material - Google Patents
A kind of preparation method and application of vanadic anhydride overlong nanowire material Download PDFInfo
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- CN109502645A CN109502645A CN201910038538.4A CN201910038538A CN109502645A CN 109502645 A CN109502645 A CN 109502645A CN 201910038538 A CN201910038538 A CN 201910038538A CN 109502645 A CN109502645 A CN 109502645A
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- vanadic anhydride
- deionized water
- overlong nanowire
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- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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Abstract
The present invention provides a kind of preparation methods of vanadic anhydride overlong nanowire material, ammonium metavanadate and dibenzyl sulfide are dissolved in deionized water according to a certain percentage, precursor solution is obtained by hydrothermal synthesis method, precursor solution is washed with deionized water and dehydrated alcohol respectively, it is dried in 60 DEG C of baking ovens, prepares vanadic anhydride overlong nanowire material in Muffle furnace annealing.The method of the present invention can prepare the vanadic anhydride material that nanowire length is 300 μm, the conductivity of material can be increased substantially and improve chemical property, specific surface area by improving material goes to increase the active site reacted, and the conductivity for improving material is gone secondly by the raising of oxygen vacancy concentration.The advantages that this method preparation process is simple, easy control of reaction conditions, consumes energy low, at low cost, is suitable for industrialized production.
Description
Technical field
The present invention relates to supercapacitors, more particularly to vanadic anhydride overlong nanowire and its in supercapacitor
Using.
Background technique
The exhaustion of fuel source and the discharge of greenhouse gases can all lead to the increase in demand to sustainable energy, sustainable
The energy such as solar energy, Hydrogen Energy and wind energy are all the following effective workarounds for solving these worries.However, due to generating electricity greatly
The fluctuation of amount, electric energy must be stored effectively, to meet the needs of to energy.In these various energy storage devices
In, battery and supercapacitor represent two kinds of leading electrochemical energy storage technologies.Lithium ion battery is due to high energy density quilt
It is widely used in electronic device.However, battery can generate at high power since resistance loss electronics and ion transmission are slow
Heat and Li dendrite can be generated in use, this may cause serious safety problem.Therefore scientists are concern
Focused on supercapacitor direction.But the main electrode material of supercapacitor is carbon material, due to carbon material
Energy density is lower, is not able to satisfy the demand of present electronic device, therefore, a kind of electrode material of high-energy density of research and development
Become present problem to be solved.
Vanadic anhydride material is a kind of material of electrochemical performance, have theoretical specific capacity big, voltage window mouth width,
The advantages that energy density is big, but the disadvantages of its electronic conduction rate is low, and ion transmission speed is slow, limits its development, therefore
It needs to be modified vanadic anhydride, in order to achieve the above objectives, scientists attempt to aoxidize two using the five of various patterns
Vanadium attracts to improve chemical property .1D nano material (nano wire (NWs)/nanorods/nanotubes/nanofibers)
The concern of extensive crowd, due to its unique functional character by various interest.Nano wire be these structures wherein it
One, possess many practical properties, such as crystallinity, the size composition well controlled and electronics radial transport, in electrochemical energy storage
Middle nano wire will be helpful to manufacture nano-scale systems and useful equipment.In the past few decades, nano wire is in energy storage
For application potential in exploring always, their advantage can partially meet expectation of the people to electrode material.The advantages of nano wire
Be summarized as follows: 1) nano wire provides a kind of direct way of electronics transfer.2) nano wire offer surface area is bigger, electrode-electric
Solution matter contact area is bigger, and charge/discharge time is shorter.3) nano wire is adapted to volume expansion, and lattice is inhibited to collapse.4) it receives
Rice noodles have excellent mechanical flexibility and Young's modulus, this has important meaning for making microcosmic electronic device flexible
Justice.
Therefore during this investigation it turned out, we prepare vanadic anhydride overlong nanowire material by the method for hydrothermal synthesis,
And system research can be carried out to its microscopic appearance and electrochemistry, it is believed that be by this method supercapacitor industrialization hair
Exhibition contributes.
Summary of the invention
The present invention is directed to overcome existing technological deficiency and achievement to limit, proposition develops a kind of vanadic anhydride overlength nanometer
The preparation method of wire material contacts electrolyte preferably with electrode material, provides more by improving the specific surface area of material
More active sites;By introduce Lacking oxygen, increase the concentration of Lacking oxygen, improve the electric conductivity of material, increase electronics and from
The transmission speed of son enhances the fake capacitance capacity of device, and then improves the energy energy and power density of capacitor.
To achieve the above object, the technical solution adopted by the present invention is that: weigh a certain amount of ammonium metavanadate and dibenzyl sulfide
Ether is dissolved in deionized water, is stirred certain time, is put into reaction kettle and reacts certain temperature, then passes through deionized water and anhydrous
Ethyl alcohol centrifuge washing, drying, is heat-treated in Muffle furnace, obtains overlong nanowire vanadic anhydride.This method technique letter
Single, gained vanadic anhydride overlong nanowire can quickly carry out discharge and recharge reaction, and the transmission speed of electronic and ionic faster, has
Better chemical property, can be used for supercapacitor and field of lithium ion battery.Specific synthesis step is as follows:
0.585 g ammonium metavanadate is weighed, mass ratio is the 0.0029 g dibenzyl sulfide of 0.5 %, is dissolved in 30-40 ml deionization
In water, 2 h are stirred, being put into temperature in the reaction kettle of 50 ml is 180-200 DEG C, soaking time 24-36 h, then passes through deionization
Water and dehydrated alcohol centrifuge washing are dried, the 400-500 DEG C of heat treatment 3-5 under argon atmosphere in Muffle furnace in 60 DEG C of 24 h
H obtains vanadic anhydride overlong nanowire;
(1) a certain amount of ammonium metavanadate is weighed, dibenzyl sulfide is dissolved in deionized water, stirs 2 h.Wherein deionized water
Amount is 30-40 ml;
(2) step (1) resulting solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), at 180-200 DEG C,
Carry out hydro-thermal reaction 24-36 h.The wherein temperature of hydrothermal reaction kettle are as follows: 180-200 DEG C, the hydro-thermal time are as follows: 24-36 h;
(3) the product utilization centrifuge after hydro-thermal reaction is separated by solid-liquid separation again, and solid to gained with deionized water and ethyl alcohol
Body product is repeatedly washed, and obtained solid product is placed in drying box, 60 DEG C of dryings;
(4) it is subsequently placed in alumina crucible and is put into Muffle furnace, 3-5 h is heat-treated at 400-500 DEG C, obtains vanadic anhydride
Overlong nanowire.Wherein in the temperature of Muffle furnace are as follows: 400-500 DEG C, the reaction time are as follows: 3-5 h.
Detailed description of the invention
Fig. 1 is V2O5The XRD spectrum of nano material.
Fig. 2 is V2O5The FESEM of nano material schemes.
Fig. 3 is V2O5The TEM of nano material schemes.
Fig. 4 is V2O5Nano material sweeps the cyclic voltammetry curve under speed in difference.
Fig. 5 is V2O5The charge and discharge electrograph under different current densities of nano material.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is further described, but is not limited to protection scope of the present invention.
Embodiment 1
A kind of preparation method of vanadic anhydride overlong nanowire material, with ammonium metavanadate, dibenzyl sulfide is primary raw material, is led to
It crosses hydrothermal synthesis method and vanadic anhydride overlong nanowire is made, comprising the following steps:
(1) a certain amount of ammonium metavanadate is weighed, dibenzyl sulfide is dissolved in deionized water, stirs 2 h.The wherein amount of deionized water
For 40 ml;
(2) step (1) resulting solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), at 180 DEG C, is carried out
24 h of hydro-thermal reaction;
(3) the product utilization centrifuge after hydro-thermal reaction is separated by solid-liquid separation again, and solid to gained with deionized water and ethyl alcohol
Body product is repeatedly washed, and obtained solid product is placed in drying box, 60 DEG C of dryings;
(4) it is subsequently placed in alumina crucible and is put into Muffle furnace, 5 h are heat-treated at 500 DEG C, obtain vanadic anhydride overlength and receive
Rice noodles.
Embodiment 2
A kind of preparation method of vanadic anhydride overlong nanowire material, with ammonium metavanadate, dibenzyl sulfide is primary raw material, is led to
It crosses hydrothermal synthesis method and vanadic anhydride overlong nanowire is made, comprising the following steps:
(1) a certain amount of ammonium metavanadate is weighed, dibenzyl sulfide is dissolved in deionized water, stirs 2 h.The wherein amount of deionized water
For 30 ml;
(2) step (1) resulting solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), at 200 DEG C, is carried out
24 h of hydro-thermal reaction;
(3) the product utilization centrifuge after hydro-thermal reaction is separated by solid-liquid separation again, and solid to gained with deionized water and ethyl alcohol
Body product is repeatedly washed, and obtained solid product is placed in drying box, 60 DEG C of dryings;
(4) it is subsequently placed in alumina crucible and is put into Muffle furnace, 5 h are heat-treated at 500 DEG C, obtain vanadic anhydride overlength and receive
Rice noodles.
Embodiment 3
A kind of preparation method of vanadic anhydride overlong nanowire material, with ammonium metavanadate, dibenzyl sulfide is primary raw material, is led to
It crosses hydrothermal synthesis method and vanadic anhydride overlong nanowire is made, comprising the following steps:
(1) a certain amount of ammonium metavanadate is weighed, dibenzyl sulfide is dissolved in deionized water, is stirred 2 hours.Wherein deionized water
Amount is 30 ml;
(2) step (1) resulting solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), at 180 DEG C, is carried out
36 h of hydro-thermal reaction;
(3) the product utilization centrifuge after hydro-thermal reaction is separated by solid-liquid separation again, and solid to gained with deionized water and ethyl alcohol
Body product is repeatedly washed, and obtained solid product is placed in drying box, 60 DEG C of dryings;
(4) it is subsequently placed in alumina crucible and is put into Muffle furnace, 5 h are heat-treated at 500 DEG C, obtain vanadic anhydride overlength and receive
Rice noodles.
Embodiment 4
A kind of preparation method of vanadic anhydride overlong nanowire material, with ammonium metavanadate, dibenzyl sulfide is primary raw material, is led to
It crosses hydrothermal synthesis method and vanadic anhydride overlong nanowire is made, comprising the following steps:
(1) a certain amount of ammonium metavanadate is weighed, dibenzyl sulfide is dissolved in deionized water, stirs 2 h.The wherein amount of deionized water
For 30 ml;
(2) step (1) resulting solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), at 180 DEG C, is carried out
24 h of hydro-thermal reaction;
(3) the product utilization centrifuge after hydro-thermal reaction is separated by solid-liquid separation again, and solid to gained with deionized water and ethyl alcohol
Body product is repeatedly washed, and obtained solid product is placed in drying box, 60 DEG C of dryings;
(4) it is subsequently placed in alumina crucible and is put into Muffle furnace, 5 h are heat-treated at 300 DEG C, obtain vanadic anhydride overlength and receive
Rice noodles.
Embodiment 5
A kind of preparation method of vanadic anhydride overlong nanowire material, with ammonium metavanadate, dibenzyl sulfide is primary raw material, is led to
It crosses hydrothermal synthesis method and vanadic anhydride overlong nanowire is made, comprising the following steps:
(1) a certain amount of ammonium metavanadate is weighed, dibenzyl sulfide is dissolved in deionized water, stirs 2 h.The wherein amount of deionized water
For 30 ml;
(2) step (1) resulting solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), at 180 DEG C, is carried out
24 h of hydro-thermal reaction;
(3) the product utilization centrifuge after hydro-thermal reaction is separated by solid-liquid separation again, and solid to gained with deionized water and ethyl alcohol
Body product is repeatedly washed, and obtained solid product is placed in drying box, 60 DEG C of dryings;
(4) it is subsequently placed in alumina crucible and is put into Muffle furnace, 3 h are heat-treated at 500 DEG C, obtain vanadic anhydride overlength and receive
Rice noodles.
Claims (1)
1. weigh 0.585 g ammonium metavanadate, mass ratio is the 0.0029 g dibenzyl sulfide of 0.5 %, be dissolved in 30-40 ml go from
In sub- water, stir 2 h, being put into the reaction kettle of 50 ml temperature is 180-200 DEG C, soaking time 24-36 h, then by go from
Sub- water and dehydrated alcohol centrifuge washing are dried in 60 DEG C of 24 h, the 400-500 DEG C of heat treatment under argon atmosphere in Muffle furnace
3-5 h obtains vanadic anhydride overlong nanowire.
(1) a certain amount of ammonium metavanadate is weighed, dibenzyl sulfide is dissolved in deionized water, stirs 2 h.The wherein amount of deionized water
For 30-40 ml;
(2) step (1) resulting solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), at 180-200 DEG C,
Carry out hydro-thermal reaction 24-36 h.The wherein temperature of hydrothermal reaction kettle are as follows: 180-200 DEG C, the hydro-thermal time are as follows: 24-36 h;
(3) the product utilization centrifuge after hydro-thermal reaction is separated by solid-liquid separation again, and solid to gained with deionized water and ethyl alcohol
Body product is repeatedly washed, and obtained solid product is placed in drying box, 60 DEG C of dryings;
(4) it is subsequently placed in alumina crucible and is put into Muffle furnace, 3-5 h is heat-treated at 400-500 DEG C, obtains vanadic anhydride
Overlong nanowire.Wherein in the temperature of Muffle furnace are as follows: 400-500 DEG C, the reaction time are as follows: 3-5 h.
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CN112499682A (en) * | 2020-12-09 | 2021-03-16 | 北方民族大学 | V-shaped groove4+Self-doping of V2O5Nanowire and preparation method and application thereof |
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CN112499682A (en) * | 2020-12-09 | 2021-03-16 | 北方民族大学 | V-shaped groove4+Self-doping of V2O5Nanowire and preparation method and application thereof |
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