CN107779905A - A kind of preparation method of vanadium oxide nanobelt - Google Patents
A kind of preparation method of vanadium oxide nanobelt Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of vanadium oxide nanobelt, comprise the following steps:(1) vanadium paper tinsel and platinized platinum part is taken to immerse in the electrolyte of electrolytic cell, wherein, vanadium paper tinsel switches on power as negative electrode as anode, platinized platinum, starts anodic oxidation reactionses, until the vanadium paper tinsel part immersed in electrolyte is all dissolved;(2) reaction solution is separated, dries, obtain vanadium oxide aggregate;(3) vanadium oxide aggregate is added in ethanol solution again, be cleaned by ultrasonic, obtained suspension and stand free settling, isolated precipitation, dry, that is, obtain vanadium oxide nanobelt.Compared with prior art; the present invention can simple reaction at normal temperatures and pressures, high yield and vanadium oxide nanobelt can be prepared on a large scale; have the characteristics that technique is simple and convenient to operate, energy consumption is low, it is easily controllable, be easy to amplify large-scale production; in addition; acceptable continuous production line balance; only need to be continuously added two kinds of water, vanadium paper tinsel reactants, be just able to continuously to obtain vanadium oxide nanobelt.
Description
Technical field
The present invention relates to a kind of preparation method of vanadium oxide, more particularly, to a kind of preparation method of vanadium oxide nanobelt.
Background technology
Vanadium oxide nanobelt (VXG) is a kind of transition metal oxide in crystalline state of two-dimensional layered structure, interlayer key
Compared with V2O5V-O keys much weaker in crystal.Insertion reaction is relatively slow in crystal, and room temperature a few houres or a few minutes in nanobelt
With regard to that can be completely embedded into clock.Vanadium oxide nanobelt can allow various metals cation to be embedded in, and be a kind of splendid inlaid scheme, because
This turns into one of selection of the great potential quality of lithium storage battery positive electrode.
Application number CN201410485637.4 Chinese patent application a kind of Vanadium pentoxide nanobelt and its normal temperature close
Into method and application, a kind of normal temperature synthesis method of Vanadium pentoxide nanobelt of disclosure of the invention, add into the vanadium source aqueous solution
Mineralizer, then the vanadium source aqueous solution added with mineralizer is placed under normal temperature condition and stirred, after reaction completely, washing collection obtains
Vanadium pentoxide nanobelt;Vanadium pentoxide nanobelt is uniform overlength nanobelt, and its length is 10-20 microns, and five aoxidize two
The width of vanadium nanobelt is 20-50 nanometers.The problem of above method is present be:1st, reaction time is indefinite, when anti-does not know
It should complete;2nd, be not suitable for streamline continuously generate, course of reaction be once produce it is a certain amount of.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of vanadium oxide nanobelt
Preparation method.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of vanadium oxide nanobelt, comprises the following steps:
(1) vanadium paper tinsel and platinized platinum part is taken to immerse in the electrolyte of electrolytic cell, wherein, vanadium paper tinsel is as anode, and platinized platinum is as cloudy
Pole, switch on power, start anodic oxidation reactionses, until the vanadium paper tinsel part immersed in electrolyte is all dissolved;
(2) reaction solution is separated, dries, obtain vanadium oxide aggregate;
(3) vanadium oxide aggregate is added in ethanol solution again, is cleaned by ultrasonic, obtained suspension and stand free settling,
Precipitation is centrifugally separating to obtain, dries, that is, obtains vanadium oxide nanobelt.
Preferably, vanadium paper tinsel also passes through following preprocessing process before use in step (1):Vanadium paper tinsel is cut into 2cm × 2cm
Size, polished using 1200 mesh sand paper, remove the oxide layer on surface, it is clean using distilled water flushing, dry standby.
Preferably, the electrolyte described in step (1) is made into using following methods:
First, in terms of every 100mL water solution As, 1-2g NaCl, 0.01-0.1g KCl, 0.1-1g CaCl are weighed2·
2H2O、0.1-1g MgCl2·6H2O, water is added to be configured to 100mL water solution As;
Then, then 0.5-2mL solution As and 0.1-1g nitric acid are taken, is diluted with water, is made into electrolyte described in 60mL.
Preferably, the spacing of two electrodes is 1-3cm, and the voltage control of energization is 1-10V.
Preferably, separation process is specially:Take and be transferred to by electrolyte and precipitation anabolic reaction solution in centrifuge tube, centrifuged
Separation, rotating speed 6000-8000r/min is controlled, time 5-10min, pours out supernatant, added deionized water washing, rock shape
Into suspension, centrifuge again, get rid of supernatant, washing is multiple repeatedly, that is, completes separation process, obtain wet vanadium oxide
Aggregate;
Drying process is specially:Take the wet vanadium oxide aggregate after separation to be transferred in drying box, done at 40-60 DEG C
Dry 3-5h.
Preferably, in step (3):The addition of vanadium oxide aggregate and ethanol ratio is (0.5-1) g:(20-50)mL.
Preferably, the process conditions of ultrasonic disperse are:Supersonic frequency is 30-50kHz, power 100-300W, when ultrasonic
Between be 2-10h.
Preferably, in step (3), dry temperature is 20-40 DEG C, drying time 2-10h.
The forming process of vanadium oxide nanometer is as follows, and under electric field action, oxidation reaction generation vanadium oxygen occurs for the vanadium paper tinsel of anode
Ion enters the aqueous solution:
V+H2O–5e-→(VO2)++4H+
V+H2O–4e-→(VO)2++2H+
Effects of ion concentration gradually increases, and reaches some concentration, and vanadium oxonium ion hydrolyzes:
2(VO2)++H2O→V2O5+2H+
(VO)2++4(VO2)++3H2O→V5O12+6H2O
In hydrolytic process, H2O can enter in the layered crystal of vanadium oxide nanobelt.
Wherein, the salt component in the present invention mainly influences the resistance value of electrolyte, and acid constituents is aoxidized using nitrate induction
The vanadium nanobelt direction of growth;Voltage influence anode potential, and then influence the chemical valence of V oxidation reaction products;The spacing of electrode and
Electric-field intensity in the area combined influence electrolyte of electrode, ionophoresis movement velocity is different under different electric-field intensity, hydrolysis
Speed is different, can influence the microscopic pattern of vanadium oxide;The purpose of ultrasonic disperse is that the vanadium oxide nanobelt of reunion scatter.
Compared with prior art, the present invention can simple reaction at normal temperatures and pressures, high yield and oxygen can be prepared on a large scale
Change vanadium nanobelt.Have the characteristics that technique is simple and convenient to operate, energy consumption is low, it is easily controllable, be easy to amplify large-scale production, most
Important advantage is can continuous production line balance, it is only necessary to is continuously added two kinds of water, vanadium paper tinsel reactants, is just able to continuously
To vanadium oxide nanobelt.
Brief description of the drawings
Fig. 1 is transmission electron microscope (TEM) photo of the vanadium oxide aggregate obtained in preparation process of the present invention;
Transmission electron microscope (TEM) photograph that Fig. 2 disperses after peeling off to form vanadium oxide nanobelt for the vanadium oxide aggregate of the present invention
Piece;
Fig. 3 is X-ray diffraction (XRD) analysis result figure of the vanadium oxide nanobelt of the present invention;
Fig. 4 is the Thermal Synthetic Analysis figure of the vanadium oxide nanobelt material of the present invention.
Embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
1st, vanadium paper tinsel pre-processes, and the vanadium paper tinsel surface of purchase there may be oxide layer, be polished using 1200 mesh sand paper, removes
The oxide layer on surface, it is clean using distilled water flushing, dry standby.
2nd, electrolyte is prepared, in order to weigh 60 times of concentration that the mixing salt solution accurately configured is actual use, before use
It is diluted processing.Weigh 1-2g NaCl (top pure grade), 0.01-0.1g KCl (analysis is pure), 0.1-1g CaCl2·2H2O (point
Analyse pure), 0.1-1g MgCl2·6H2O (analysis is pure) is configured to the 100ml aqueous solution (solution A), takes 0.5-2mL solution As and 0.1-
1mL nitric acid, is diluted with water, and is configured to 60mL weak solutions.
3rd, assembling electrolytic cell, the anode as electrolytic cell of vanadium paper tinsel, negative electrode of the clean platinized platinum dried as electrolytic cell, two
The spacing of electrode is 1-3cm, adds 2/3 part that electrolyte floods vanadium paper tinsel and platinized platinum, connects constant voltage dc source, adjusts voltage
To 1.0-10.0V, start anodic oxidation reactionses, vanadium paper tinsel slowly dissolves, and through 1-5h or so after a while, starts in the electrolytic solution
Solia particle is separated out, solia particle is deposited to the bottom of electrolytic cell, reacts and constantly carries out until immersing the vanadium paper tinsel part of electrolyte
All dissolving, anodic oxidation terminate, and generate vanadium oxide nanobelt aggregate.
4th, electrolytic cell has used centrifuge tube repacking to be made, and directly takes out centrifuge tube, static, reuses another centrifuge tube
Anodic oxidation reactionses are carried out, two centrifuge tubes is obtained and is equipped with electrolyte and colloidal vanadium oxide, be centrifuged, rotating speed
6000-8000r/min, time 5-10min, supernatant is poured out and (collects and recycled in reagent bottle), add deionization
Water washing, rock to form suspension, centrifuge again, get rid of supernatant, wash repeatedly three times, finally obtaining has moisture
Vanadium oxide nanobelt aggregate.
5th, vanadium oxide gel is imported in beaker, is put into drying box and is dried, it is 40-60 DEG C to set temperature, is done
Dry time 3-5h, finally give vanadium oxide nanobelt aggregate.
6th, vanadium oxide nanobelt aggregate is added in alcoholic solution, ultrasonic disperse stripping is carried out in ultrasonic cleaning machine
From obtaining vanadium oxide nanobelt suspension.
7th, vanadium oxide nanobelt suspension is stood into free settling, low temperature drying is carried out inside baking oven, finally obtains oxygen
Change vanadium nanobelt.
Embodiment 2
1st, vanadium paper tinsel pre-processes, and the vanadium paper tinsel surface of purchase there may be oxide layer, be polished using 1200 mesh sand paper, removes
The oxide layer on surface, it is clean using distilled water flushing, dry standby.
2nd, electrolyte is prepared, in order to weigh 60 times of concentration that the mixing salt solution accurately configured is actual use, before use
It is diluted processing.Weigh 1.5g NaCl (top pure grade), 0.06g KCl (analysis is pure), 0.5g CaCl2·2H2O (analysis is pure),
0.5g MgCl2·6H2O (analysis is pure) is configured to the 100ml aqueous solution (solution A), takes 1mL solution As and 0.5mL nitric acid, adds water dilute
Release, be configured to 60mL weak solutions.
3rd, assembling electrolytic cell, the anode as electrolytic cell of vanadium paper tinsel, negative electrode of the clean platinized platinum dried as electrolytic cell, two
The spacing of electrode is 2cm, adds 2/3 part that electrolyte floods vanadium paper tinsel and platinized platinum, connects constant voltage dc source, adjustment voltage is extremely
5V, start anodic oxidation reactionses, vanadium paper tinsel slowly dissolves, and through 3h or so after a while, it is micro- to start precipitation solid in the electrolytic solution
Grain, solia particle are deposited to the bottom of electrolytic cell, react constantly progress and are all dissolved up to immersing the vanadium paper tinsel part of electrolyte, positive
Pole oxidation terminates, and generates vanadium oxide nanobelt aggregate.
4th, electrolytic cell has used centrifuge tube repacking to be made, and directly takes out centrifuge tube, static, reuses another centrifuge tube
Anodic oxidation reactionses are carried out, two centrifuge tubes is obtained and is equipped with electrolyte and colloidal vanadium oxide, be centrifuged, rotating speed
7000r/min, time 8min, supernatant is poured out and (collects and recycled in reagent bottle), add deionized water washing, shake
Rolling forms suspension, centrifuges again, gets rid of supernatant, washs repeatedly three times, and the vanadium oxide that finally obtaining has moisture is received
Rice band aggregate.
5th, vanadium oxide gel is imported in beaker, is put into drying box and is dried, it is 50 DEG C to set temperature, when drying
Between 4h, finally give vanadium oxide nanobelt aggregate.
6th, vanadium oxide nanobelt aggregate is added in alcoholic solution, ultrasonic disperse stripping is carried out in ultrasonic cleaning machine
From obtaining vanadium oxide nanobelt suspension.
7th, vanadium oxide nanobelt suspension is stood into free settling, low temperature drying is carried out inside baking oven, finally obtains oxygen
Change vanadium nanobelt.
Fig. 1 is the TEM photos of isolated vanadium oxide nanobelt aggregate after anodic oxidation reactionses, can be with from photo
To find out, vanadium oxide nanobelt, which is reunited, to be arrived together, but still it is observed that banded structure.Fig. 2 then oxidations to finally obtain
The TEM figures of vanadium nanobelt, it can be seen that vanadium oxide nanobelt spreads out, the pattern of its nanobelt becomes apparent from, electricity
The analysis result of sub- diffraction meets XRD test results, and component is that component is V2O5·1.6H2O and V5O12·6H2O 6H2O.Fig. 3 is
X-ray diffraction (XRD) analysis result figure of last obtained vanadium oxide nanobelt material, it can be seen that component is
V2O5·1.6H2O and V5O12·6H2O.Fig. 4 is then the Thermal Synthetic Analysis figure of last obtained vanadium oxide nanobelt material, from figure
In as can be seen that heat analysis during, about before 130 DEG C, its Coating combination water is then Free water in vanadium oxide nanobelt
Sloughed more than 130 DEG C, oxidation reaction, V about occurs at 350 DEG C5O12It is oxidized to V2O5。
Embodiment 3
1st, vanadium paper tinsel pre-processes, and the vanadium paper tinsel surface of purchase there may be oxide layer, be polished using 1200 mesh sand paper, removes
The oxide layer on surface, it is clean using distilled water flushing, dry standby.
2nd, electrolyte is prepared, in order to weigh 60 times of concentration that the mixing salt solution accurately configured is actual use, before use
It is diluted processing.Weigh 1g NaCl (top pure grade), 0.01g KCl (analysis is pure), 0.1g CaCl2·2H2O (analysis is pure),
0.1g MgCl2·6H2O (analysis is pure) is configured to the 100ml aqueous solution (solution A), takes 0.5mL solution As and 0.1mL nitric acid, adds water
Dilution, is configured to 60mL weak solutions.
3rd, assembling electrolytic cell, the anode as electrolytic cell of vanadium paper tinsel, negative electrode of the clean platinized platinum dried as electrolytic cell, two
The spacing of electrode is 1cm, adds 2/3 part that electrolyte floods vanadium paper tinsel and platinized platinum, connects constant voltage dc source, adjustment voltage is extremely
1.0V, start anodic oxidation reactionses, vanadium paper tinsel slowly dissolves, and through 5h or so after a while, starts to separate out solid in the electrolytic solution
Particulate, solia particle are deposited to the bottom of electrolytic cell, react constantly progress and are all dissolved up to immersing the vanadium paper tinsel part of electrolyte,
Anodic oxidation terminates, and generates vanadium oxide nanobelt aggregate.
4th, electrolytic cell has used centrifuge tube repacking to be made, and directly takes out centrifuge tube, static, reuses another centrifuge tube
Anodic oxidation reactionses are carried out, two centrifuge tubes is obtained and is equipped with electrolyte and colloidal vanadium oxide, be centrifuged, rotating speed
6000r/min, time 10min, supernatant is poured out and (collects and recycled in reagent bottle), add deionized water washing,
Rock to form suspension, centrifuge again, get rid of supernatant, wash repeatedly three times, finally obtain the vanadium oxide for having moisture
Nanobelt aggregate.
5th, vanadium oxide gel is imported in beaker, is put into drying box and is dried, it is 40 DEG C to set temperature, when drying
Between 5h, finally give vanadium oxide nanobelt aggregate.
6th, 0.8g vanadium oxide nanobelt aggregates are added in 35mL alcoholic solutions, ultrasound is carried out in ultrasonic cleaning machine
It is scattered to peel off, supersonic frequency 40kHz, power 200W, ultrasonic time 6h, obtain vanadium oxide nanobelt suspension.
7th, vanadium oxide nanobelt suspension is stood into free settling, low temperature drying is carried out inside baking oven, drying temperature is
It is 30 DEG C, drying time 6h, final to obtain vanadium oxide nanobelt.
Embodiment 4
1st, vanadium paper tinsel pre-processes, and the vanadium paper tinsel surface of purchase there may be oxide layer, be polished using 1200 mesh sand paper, removes
The oxide layer on surface, it is clean using distilled water flushing, dry standby.
2nd, electrolyte is prepared, in order to weigh 60 times of concentration that the mixing salt solution accurately configured is actual use, before use
It is diluted processing.Weigh 2g NaCl (top pure grade), 0.1g KCl (analysis is pure), 1g CaCl2·2H2O (analysis is pure), 1g
MgCl2·6H2O (analysis is pure) is configured to the 100ml aqueous solution (solution A), takes 2mL solution As and 1mL nitric acid, is diluted with water, configures
Into 60mL weak solutions.
3rd, assembling electrolytic cell, the anode as electrolytic cell of vanadium paper tinsel, negative electrode of the clean platinized platinum dried as electrolytic cell, two
The spacing of electrode is 3cm, adds 2/3 part that electrolyte floods vanadium paper tinsel and platinized platinum, connects constant voltage dc source, adjustment voltage is extremely
10.0V, start anodic oxidation reactionses, vanadium paper tinsel slowly dissolves, and through 1h or so after a while, starts to separate out solid in the electrolytic solution
Particulate, solia particle are deposited to the bottom of electrolytic cell, react constantly progress and are all dissolved up to immersing the vanadium paper tinsel part of electrolyte,
Anodic oxidation terminates, and generates vanadium oxide nanobelt aggregate.
4th, electrolytic cell has used centrifuge tube repacking to be made, and directly takes out centrifuge tube, static, reuses another centrifuge tube
Anodic oxidation reactionses are carried out, two centrifuge tubes is obtained and is equipped with electrolyte and colloidal vanadium oxide, be centrifuged, rotating speed
8000r/min, time 5min, supernatant is poured out and (collects and recycled in reagent bottle), add deionized water washing, shake
Rolling forms suspension, centrifuges again, gets rid of supernatant, washs repeatedly three times, and the vanadium oxide that finally obtaining has moisture is received
Rice band aggregate.
5th, vanadium oxide gel is imported in beaker, is put into drying box and is dried, it is 60 DEG C to set temperature, when drying
Between 3h, finally give vanadium oxide nanobelt aggregate.
6th, 0.5g vanadium oxide nanobelt aggregates are added in 20mL alcoholic solutions, ultrasound is carried out in ultrasonic cleaning machine
It is scattered to peel off, supersonic frequency 50kHz, power 300W, ultrasonic time 2h, obtain vanadium oxide nanobelt suspension.
7th, vanadium oxide nanobelt suspension is stood into free settling, low temperature drying is carried out inside baking oven, drying temperature is
It is 20 DEG C, drying time 2h, final to obtain vanadium oxide nanobelt.
Embodiment 5
1st, vanadium paper tinsel pre-processes, and the vanadium paper tinsel surface of purchase there may be oxide layer, be polished using 1200 mesh sand paper, removes
The oxide layer on surface, it is clean using distilled water flushing, dry standby.
2nd, electrolyte is prepared, in order to weigh 60 times of concentration that the mixing salt solution accurately configured is actual use, before use
It is diluted processing.Weigh 1.2g NaCl (top pure grade), 0.04g KCl (analysis is pure), 0.7g CaCl2·2H2O (analysis is pure),
0.5g MgCl2·6H2O (analysis is pure) is configured to the 100ml aqueous solution (solution A), takes 1.3mL solution As and 0.5mL nitric acid, adds water
Dilution, is configured to 60mL weak solutions.
3rd, assembling electrolytic cell, the anode as electrolytic cell of vanadium paper tinsel, negative electrode of the clean platinized platinum dried as electrolytic cell, two
The spacing of electrode is 2.5cm, adds 2/3 part that electrolyte floods vanadium paper tinsel and platinized platinum, connects constant voltage dc source, adjusts voltage
To 4V, start anodic oxidation reactionses, vanadium paper tinsel slowly dissolves, and through 2h or so after a while, starts to separate out solid in the electrolytic solution
Particulate, solia particle are deposited to the bottom of electrolytic cell, react constantly progress and are all dissolved up to immersing the vanadium paper tinsel part of electrolyte,
Anodic oxidation terminates, and generates vanadium oxide nanobelt aggregate.
4th, electrolytic cell has used centrifuge tube repacking to be made, and directly takes out centrifuge tube, static, reuses another centrifuge tube
Anodic oxidation reactionses are carried out, two centrifuge tubes is obtained and is equipped with electrolyte and colloidal vanadium oxide, be centrifuged, rotating speed
7000r/min, time 8min, supernatant is poured out and (collects and recycled in reagent bottle), add deionized water washing, shake
Rolling forms suspension, centrifuges again, gets rid of supernatant, washs repeatedly three times, and the vanadium oxide that finally obtaining has moisture is received
Rice band aggregate.
5th, vanadium oxide gel is imported in beaker, is put into drying box and is dried, it is 50 DEG C to set temperature, when drying
Between 4h, finally give vanadium oxide nanobelt aggregate.
6th, 1g vanadium oxide nanobelt aggregates are added in 50mL alcoholic solutions, ultrasound point is carried out in ultrasonic cleaning machine
Dissipate and peel off, supersonic frequency 30kHz, power 100W, ultrasonic time 10h, obtain vanadium oxide nanobelt suspension.
7th, vanadium oxide nanobelt suspension is stood into free settling, low temperature drying is carried out inside baking oven, drying temperature is
It is 40 DEG C, drying time 10h, final to obtain vanadium oxide nanobelt.The above-mentioned description to embodiment is led for ease of the technology
The those of ordinary skill in domain is understood that and using invention.Person skilled in the art obviously easily can implement to these
Example makes various modifications, and General Principle described herein is applied in other embodiment without by creative labor
It is dynamic.Therefore, the invention is not restricted to above-described embodiment, those skilled in the art not to depart from model of the present invention according to the announcement of the present invention
The improvement and modification that farmland is made all should be within protection scope of the present invention.
Claims (8)
1. a kind of preparation method of vanadium oxide nanobelt, it is characterised in that comprise the following steps:
(1) vanadium paper tinsel and platinized platinum part is taken to immerse in the electrolyte of electrolytic cell, wherein, vanadium paper tinsel connects as anode, platinized platinum as negative electrode
Energization source, start anodic oxidation reactionses, until the vanadium paper tinsel part immersed in electrolyte is all dissolved;
(2) reaction solution is separated, dries, obtain vanadium oxide aggregate;
(3) vanadium oxide aggregate is added in ethanol solution again, be cleaned by ultrasonic, obtained suspension and stand free settling, separation
Precipitated, dry, that is, obtain vanadium oxide nanobelt.
A kind of 2. preparation method of vanadium oxide nanobelt according to claim 1, it is characterised in that vanadium paper tinsel in step (1)
Also pass through following preprocessing process before use:Vanadium paper tinsel is cut into 2cm × 2cm size, beaten using 1200 mesh sand paper
Mill, removes the oxide layer on surface, clean using distilled water flushing, dries standby.
3. the preparation method of a kind of vanadium oxide nanobelt according to claim 1, it is characterised in that described in step (1)
Electrolyte be made into using following methods:
First, in terms of every 100mL water solution As, 1-2g NaCl, 0.01-0.1g KCl, 0.1-1g CaCl are weighed2·2H2O、
0.1-1g MgCl2·6H2O, water is added to be configured to 100mL water solution As;
Then, then 0.5-2mL solution As and 0.1-1g nitric acid are taken, is diluted with water, is made into electrolyte described in 60mL.
4. the preparation method of a kind of vanadium oxide nanobelt according to claim 1, it is characterised in that the spacing of two electrodes is
1-3cm, the voltage control of energization is 1-10V.
5. the preparation method of a kind of vanadium oxide nanobelt according to claim 1, it is characterised in that separation process is specific
For:Take and be transferred to by electrolyte and precipitation anabolic reaction solution in centrifuge tube, centrifuged, control rotating speed 6000-8000r/
Min, time 5-10min, pours out supernatant, adds deionized water washing, rocks to form suspension, centrifuge again, go
Supernatant is removed, washing is multiple repeatedly, that is, completes separation process, obtain wet vanadium oxide aggregate;
Drying process is specially:Take the wet vanadium oxide aggregate after separation to be transferred in drying box, 3- is dried at 40-60 DEG C
5h。
6. the preparation method of a kind of vanadium oxide nanobelt according to claim 1, it is characterised in that in step (3):Oxidation
The addition of vanadium aggregate and ethanol ratio is (0.5-1) g:(20-50)mL.
A kind of 7. preparation method of vanadium oxide nanobelt according to claim 1, it is characterised in that the technique of ultrasonic disperse
Condition is:Supersonic frequency is 30-50kHz, power 100-300W, ultrasonic time 2-10h.
8. the preparation method of a kind of vanadium oxide nanobelt according to claim 1, it is characterised in that in step (3), dry
Temperature be 20-40 DEG C, drying time 2-10h.
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CN111646452A (en) * | 2020-06-17 | 2020-09-11 | 广东工业大学 | Nano flaky hydrated sodium vanadyl phosphate cathode material and preparation method and application thereof |
CN114573027A (en) * | 2022-03-09 | 2022-06-03 | 北方民族大学 | Vanadium pentoxide nanobelt and preparation method thereof |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1806068A (en) * | 2003-06-17 | 2006-07-19 | 凯米特电子公司 | Method of anodizing valve metal derived anode bodies and electrolyte therefor |
CN1994558A (en) * | 2006-12-19 | 2007-07-11 | 武汉理工大学 | Method for preparing unidimensional TiO2 hollow structured photocatalyst using vanadium oxide nanobelt as template |
CN101880058A (en) * | 2010-05-18 | 2010-11-10 | 暨南大学 | Method for preparing nano strip V2O5 |
CN104261472A (en) * | 2014-09-22 | 2015-01-07 | 安徽工业大学 | Vanadium pentoxide nanobelt, and room-temperature synthesis method and application of vanadium pentoxide nanobelt |
CN104577087A (en) * | 2014-12-29 | 2015-04-29 | 中国工程物理研究院化工材料研究所 | VO2(B) nanobelt, preparation method thereof, and lithium battery assembled with VO2(B) nanobelt |
CN105006561A (en) * | 2015-06-03 | 2015-10-28 | 武汉理工大学 | Vanadium oxide ultra-thin nanobelt with embedded ions and preparation method and application thereof |
CN105140502A (en) * | 2015-07-10 | 2015-12-09 | 中南大学 | Potassium-embedded vanadium pentoxide nanoribbon positive electrode material for lithium battery and preparation method therefor |
CN105836800A (en) * | 2016-03-24 | 2016-08-10 | 南京航空航天大学 | Synthetic method for dimension-controllable vanadium dioxide nano material, and lithium ion battery |
-
2017
- 2017-09-19 CN CN201710852012.0A patent/CN107779905B/en not_active Expired - Fee Related
Patent Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1806068A (en) * | 2003-06-17 | 2006-07-19 | 凯米特电子公司 | Method of anodizing valve metal derived anode bodies and electrolyte therefor |
JP2006528277A (en) * | 2003-06-17 | 2006-12-14 | ケメット エレクトロニクス コーポレイション | Method for anodizing an anode body derived from valve metal and electrolyte therefor |
CN1994558A (en) * | 2006-12-19 | 2007-07-11 | 武汉理工大学 | Method for preparing unidimensional TiO2 hollow structured photocatalyst using vanadium oxide nanobelt as template |
CN101880058A (en) * | 2010-05-18 | 2010-11-10 | 暨南大学 | Method for preparing nano strip V2O5 |
CN104261472A (en) * | 2014-09-22 | 2015-01-07 | 安徽工业大学 | Vanadium pentoxide nanobelt, and room-temperature synthesis method and application of vanadium pentoxide nanobelt |
CN104577087A (en) * | 2014-12-29 | 2015-04-29 | 中国工程物理研究院化工材料研究所 | VO2(B) nanobelt, preparation method thereof, and lithium battery assembled with VO2(B) nanobelt |
CN105006561A (en) * | 2015-06-03 | 2015-10-28 | 武汉理工大学 | Vanadium oxide ultra-thin nanobelt with embedded ions and preparation method and application thereof |
CN105140502A (en) * | 2015-07-10 | 2015-12-09 | 中南大学 | Potassium-embedded vanadium pentoxide nanoribbon positive electrode material for lithium battery and preparation method therefor |
CN105836800A (en) * | 2016-03-24 | 2016-08-10 | 南京航空航天大学 | Synthetic method for dimension-controllable vanadium dioxide nano material, and lithium ion battery |
Non-Patent Citations (4)
Title |
---|
ABDUL HAKIM SHAH: "V2O5纳米材料及其异质金属/金属氧化物纳米复合材料的制备及气敏性能研究", 《中国学位论文全文数据库》 * |
段永胜 等: "钒氧化物纳米带的合成及其去除水中Cu2+离子的研究", 《陶瓷学报》 * |
王休 等: "水热法制备二氧化钒纳米带的研究", 《西北师范大学学报(自然科学版)》 * |
陈文 等: "两种一维纳米结构钒氧化物的合成与表征", 《无机化学学报》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111646452A (en) * | 2020-06-17 | 2020-09-11 | 广东工业大学 | Nano flaky hydrated sodium vanadyl phosphate cathode material and preparation method and application thereof |
CN114573027A (en) * | 2022-03-09 | 2022-06-03 | 北方民族大学 | Vanadium pentoxide nanobelt and preparation method thereof |
CN114573027B (en) * | 2022-03-09 | 2023-08-18 | 北方民族大学 | Vanadium pentoxide nanobelt and preparation method thereof |
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