CN102534731B - Method for preparing vanadium dioxide film through electrophoretic deposition - Google Patents

Method for preparing vanadium dioxide film through electrophoretic deposition Download PDF

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Publication number
CN102534731B
CN102534731B CN201210020500.2A CN201210020500A CN102534731B CN 102534731 B CN102534731 B CN 102534731B CN 201210020500 A CN201210020500 A CN 201210020500A CN 102534731 B CN102534731 B CN 102534731B
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vanadium dioxide
dioxide film
film
electrophoretic deposition
deposition
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CN102534731A (en
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张建武
侯纪伟
阮奇峰
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University of Science and Technology of China USTC
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University of Science and Technology of China USTC
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Priority to PCT/CN2013/070699 priority patent/WO2013107392A1/en
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D13/00Electrophoretic coating characterised by the process
    • C25D13/02Electrophoretic coating characterised by the process with inorganic material

Abstract

The invention provides a method for preparing a vanadium dioxide film, which is characterized in that vanadium dioxide powder is added in solvent, and then quantitive iodine is added in mixed liquor; and ultrasonic dispersion is carried out so as to prepare suspending liquid with better dispersion, and the suspending liquid is used as electrophoretic deposition liquid. A conducting substrate is used as an electrode, and a DC (Direct Current) power supply is used for providing voltage or current; the electrode is put in vanadium dioxide suspending liquid; in addition, a vanadium dioxide deposition film is directly obtained on the electrode by adjusting voltage, current, deposition time and the like, and then is dried through natural air or is baked. The method has the characteristics as follows: a phase are formed at first and then the film is formed; electrochemical reactions do not occur on the electrode; the phase of the powder is not changed before and after deposition; and the disadvantage in the prior preparation art that the film is not pure because the film is formed at first and then the phase is formed can be overcome. The thickness of the film that is prepared by adopting the method can be controlled; the process is simple; the reaction conditions are mild; the deposition time is short; the film growth speed is high; the stability is high; waste liquor can be recycled; economy and no pollution are achieved; and the method is suitable for large area production and mass production.

Description

A kind of method of preparing vanadium dioxide film by electrophoretic deposition
Technical field
The present invention relates to electronic material and devices field, refer more particularly to a kind of method of preparing vanadium dioxide film by electrophoretic deposition.
Background technology
Vanadium dioxide is a kind of typical thermic phase change materials, changes mutually temperature and approach room temperature most in known phase change material, and it in the time of 68 ℃, reversible structure occurs and changes mutually, and the rutile structure from the monocline of low temperature to high temperature changes.During lower than phase transition temperature, present semi-conductor phase, resistivity, the transmitance of susceptibility and infrared light is all very high, and during higher than phase transition temperature, present metallographic phase, resistivity, the transmitance of susceptibility and infrared light is all undergone mutation, and drops to very low, there is very significantly infrared switch, electrical switch and magnetics switch character.It is carried out to high volence metal ion doping simultaneously, can realize the artificial adjustment to its phase transition temperature, and its reversible electricity, magnetics and infrared switch character are constant.Optics based on vanadium dioxide excellence, electricity and magnetic property, it is at the smart window material of buildings, thermistor, optoelectronic switch, there is huge potential application the aspects such as optical storage.
Vanadium dioxide has excellent optics, and electricity and magnetic property are impelling people ceaselessly to study it, has developed method and the technique of much preparing vanadium dioxide.Chinese patent (publication number CN101559981A) adopts combustion method to prepare vanadium dioxide, Chinese patent (publication number CN1522965A) adopts hydrothermal method to prepare vanadium dioxide etc., but the optics of vanadium dioxide, the form with vanadium dioxide film of promoting the use of mainly of electricity and magnetics switch character, and current shortage is effectively prepared the method for vanadium dioxide film, it is promoted the use of and be greatly limited.Although Chinese patent (publication number CN101280413A), Chinese patent (publication number CN101265036A) all adopts method low temperature depositing vanadium dioxide film in glass substrate of magnetron sputtering plating, but after its first film forming, become the method for phase very easily to generate impurity phase, its glass substrate needs heat, cause too high energy consumption, do not reach the object of energy-saving and emission-reduction, also inevitably use large-scale magnetron sputtering equipment, not only increased production cost, but also need accurate parameter to control, be unfavorable for large-scale preparation, also limited to a great extent promoting the use of of vanadium dioxide, therefore a kind of develop simple and efficient the method for preparing vanadium dioxide film is the difficult point of a technology.
Electrophoretic deposition refers to the effect that relies on DC electric field, make the charged particle displacement in colloid or suspension, and be deposited on the definite shape electrode with opposite charges, the any solid material that can make fine particles (particle diameter is not more than 30 microns) or colloidal sol, can carry out electrophoretic deposition, its scope of application comprises metal, polymkeric substance, carbide, oxide compound and inorganic salts etc.A kind of method that electrophoretic deposition is prepared film as simple and efficient is gone back the preparation field that nobody applies it to vanadium dioxide film at present.
Summary of the invention
The present invention completes based on electrophoretic deposition technique just, the present invention adopts simple method, in different conductive substrates, directly electrophoretic deposition is successfully prepared vanadium dioxide film, and on electrode, there is not electrochemical reaction, do not change structure and the character of hypovanadic oxide powder, XianCheng mutually after film forming, overcome in existing technology of preparing to become after first film forming and caused mutually in film, having a lot of dephasigns, and then have a strong impact on its optics, the shortcoming of electricity and magnetics switch character.Technique of the present invention is simple, and without any need for main equipment, reaction conditions is gentle, and film forming speed is fast, and stability is high, and waste liquid can recycle, economical pollution-free, is applicable to promoting the use of on a large scale.
; the invention provides a kind of method of preparing vanadium dioxide film by electrophoretic deposition; its XianCheng is rear film forming mutually; solved after preparing at present the first film forming of vanadium dioxide film needs and become phase; thereby cause existing in film a lot of dephasigns, and then have a strong impact on the problem of its optics, electricity and magnetics switch character.Existing technology of preparing also needs the high main equipment of price, controls complicated parameter, and also have raw material availability not high, the shortcoming such as can not prepare in a large number, virtually increased production cost, limited it and promoted the use of.And the present invention has overcome many weak points of existing technology of preparing, the perfect preparation method of vanadium dioxide film, its concrete technical scheme is as follows:
(1) hypovanadic oxide powder is joined in solvent, form suspension or colloidal sol;
(2) in the suspension obtaining to step (1) or colloidal sol, add elemental iodine, be uniformly dispersed;
(3) in the suspension obtaining in step (2), put into electrode, start electrophoretic deposition;
(4) by the film drying obtaining in step (3), obtain vanadium dioxide film on electrode.
The present invention also provides a kind of vanadium dioxide film, and it obtains by aforesaid method manufacture.
Vanadium dioxide film prepared by the present invention; directly adopt commercially available or previously prepared good hypovanadic oxide powder; add solvent and a small amount of elemental iodine; be uniformly mixed; after ultrasonic being uniformly dispersed; as electrophoretic deposition liquid, then to put into cleaned electrode and start electrophoretic deposition plated film, the method does not need main equipment; do not change structure and the character of deposition front and back hypovanadic oxide powder; its technique is simple, workable, and film forming speed is fast; easily control; raw material availability is high, and waste liquid can recycled for multiple times, is applicable to large-scale production.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of embodiment 1 presedimentary hypovanadic oxide powder.
Fig. 2 is the XRD spectra of embodiment 1 post-depositional vanadium dioxide film.
Fig. 3 is the SEM picture of vanadium dioxide film after embodiment 1 deposition preparation.
Fig. 4 is the vanadium dioxide film picture of embodiment 1 deposition preparation.
Fig. 5 is the vanadium dioxide film picture of embodiment 2 deposition preparations.
Fig. 6 is the vanadium dioxide film picture of embodiment 3 deposition preparations.
Embodiment
The invention provides a kind of method of preparing vanadium dioxide film by electrophoretic deposition, said method comprising the steps of:
(1) hypovanadic oxide powder is joined in solvent, form suspension or colloidal sol;
(2) in the suspension obtaining to step (1) or colloidal sol, add elemental iodine, be uniformly dispersed;
(3) in the suspension obtaining in step (2), put into electrode, start electrophoretic deposition;
(4) by the film drying obtaining in step (3), obtain vanadium dioxide film on electrode.
The present invention also provides a kind of and prepares the vanadium dioxide film of preparing prepared by the method for vanadium dioxide film by described electrophoretic deposition.
Wherein, by adding a certain amount of elemental iodine, make suspension particle more easily be with electric charge, if do not added a small amount of iodine, deposition less efficient some, add iodine, in organism (for example: contiguous carbonyl functional group's acetone) carbon atom generation iodization:
CH 3-CO-CH 3+I 2→ICH 2-CO-CH 2I+2H ++2I -
Hypovanadic oxide suspensoid particle absorption H +and I -thereby, be with electric charge.
The hypovanadic oxide powder using in the present invention adopts general commercially available prod, also can adopt following steps preparation, by 20ml formaldehyde and 0.0025mol V 2o 5mix, add 60ml deionized water to transfer in 100ml autoclave after the about 1h of magnetic agitation, at 180 ℃, keep 24h, naturally cool to room temperature, collecting precipitation thing, uses respectively deionized water and absolute ethanol washing 5~6 times.Finally in baking oven, at 60 ℃, dry 10h, obtain bluish grey VO 2(B) powder.The powder obtaining is placed in to tubular type retort furnace, and in argon atmosphere, 500 ℃ of thermal treatment 6h, then naturally cool to room temperature, obtain VO 2(M) powder.
The concentration of the middle vanadium dioxide of step (1) is 0.05~16.00mg/ml, more preferably 0.2~1.8mg/ml preferably.
The solvent using in step (1) is generally: alcohols, and as ethanol, Virahol etc.; Ketone, as acetone, methyl ethyl diketone etc.; Cathode electrodip painting class, as vinylformic acid system etc.; And the mixing solutions of the arbitrary combination of above solution.
Churning time in step (1) is preferably 5~90 minutes.
In step (2), the concentration of the elemental iodine adding is preferably greater than 0.0mmol/L and below 4.0mmol/L, more preferably 0.6~2.0mmol/L; Churning time is preferably 10~60 minutes, and ultrasonic jitter time is preferably 10~60 minutes.
The electrode of putting in step (3) is conducting base/conductive substrates, and this conducting base/conductive substrates is selected from stainless steel substrates, iron plate, copper sheet, silver strip, aluminium flake, platinized platinum, nickel sheet, zinc metal sheet, electrical conductivity alloy, conductive glass, conductive polymers and conductivity ceramics; Deposition voltage is 10~100V preferably, more preferably 30~50V, depositing time preferably 0.5~6.0 minute, more preferably 1.5~2.5 minutes; Electrode keeping parallelism, its spacing is 0.5~4.0cm preferably, more preferably 1.0~2.0cm.
The amount of the iodine adding in the film being deposited on electrode in step (4) and step (2) has following relation, if that is: the concentration of iodine is less than or equal to 0.30mmol/L, on anode, there is vanadium dioxide film deposition, if the concentration of iodine is greater than 0.30mmol/L, on negative electrode, there is vanadium dioxide film deposition, the temperature of its oven dry is preferably 20~80 ℃, and drying time is preferably 20~100 minutes.
Below by following embodiment, describe the present invention in detail, but do not limit content of the present invention:
Instrument and model:
Field emission scanning electron microscope, model: Sirion200.
The high-power x-ray powder diffraction instrument of TTR-III sample water flat pattern, adopts Cu-K alpha-ray 8 °/min of scanning speed, tube voltage 40KV, tube current 200mA
D.C. regulated power supply, model: IT6834
Embodiment 1:
(1) hypovanadic oxide powder that weighs 50mg is put in 30ml acetone, and the suspension that configuration concentration is 1.67mg/ml, stirs 15 minutes;
(2) to the elemental iodine (traditional Chinese medicines group, analytical pure) that adds 0.021mmol in the suspension in step (1), ultrasonic dispersion 20 minutes;
(3) with cleaned FTO conductive glass as electrode, size is: long 2.5cm, wide 2.0cm, put in the suspension of ultrasonic dispersion in step (2), the voltage of 50V is provided with direct supply, is added on two electrodes, the parallel placement of two electrodes, spacing is 2.0cm, and depositing time is two minutes;
(4) vanadium dioxide film depositing on negative electrode in step (3) is put into baking oven, 40 ℃, within 30 minutes, dry, obtain the vanadium dioxide film that FTO conductive glass is substrate.
The XRD spectra of the hypovanadic oxide powder that the present embodiment is used is as shown in Figure of description 1, the XRD spectra of the vanadium dioxide film that the FTO conductive glass obtaining is substrate is as shown in Figure of description 2, XRD spectra after electrophoretic deposition film forming is in (011), (211), (212), (220), the characteristic peak of (022) does not change, SnO 2characteristic peak be (110), (101), (200), (211), (310), (301), main source is the substrate of FTO conductive glass.FTO conductive glass Shi You NHTechno of the present invention company produces, model TCO-15, on the thick simple glass of 2.2mm, plate one deck 350nm thick mix fluorine SnO 2conductive film.
There is not electrochemical reaction in the XRD spectra explanation electrophoretic deposition process of vanadium dioxide film, the structure of powder and substrate does not change, the structure and the character that have retained powder completely, thereby avoided current existing preparation in vanadium dioxide film technology, after first film forming, become phase, thereby generation dephasign, and then affect the huge shortcoming of its character.
FTO conductive glass is that substrate vanadium dioxide film SEM picture is as shown in Figure of description 3, the thickness of vanadium dioxide film is 6.4 microns, film is not very fine and close, FTO conductive glass is that the vanadium dioxide film picture of substrate is as shown in Figure of description 4, compare generally even compact, film is combined relatively good with FTO Conducting Glass, difficult drop-off.
Embodiment 2:
(1) hypovanadic oxide powder that weighs 20mg is put in the methyl ethyl diketone solution of 30ml, and the suspension that configuration concentration is 0.67mg/ml, stirs 30 minutes;
(2) to the elemental iodine (traditional Chinese medicines group, analytical pure) that adds 0.048mmol in the suspension in step (1), ultrasonic dispersion 40 minutes;
(3) with cleaned copper sheet as electrode, size is: long 3.0cm, wide 2.5cm, put in the suspension of ultrasonic dispersion in step (2), the voltage of 30V is provided with direct supply, be added on two electrodes, the parallel placement of two electrodes, spacing is 1.0cm, depositing time is three minutes;
(4) vanadium dioxide film depositing in step (3) is put into baking oven on negative electrode, 60 ℃, within 20 minutes, dry, obtain the vanadium dioxide film that copper sheet is substrate.
The vanadium dioxide film picture that the resulting copper sheet of the present embodiment is substrate as shown in Figure of description 5, even compact relatively generally, and and copper sheet substrate combination relatively good, place for a long time film difficult drop-off.
Embodiment 3:
(1) weigh 30mg hypovanadic oxide powder and join in the transparent electrocoating paint of negative electrode of 30ml and the mixing solutions of water, wherein the volume ratio of the transparent electrocoating paint of negative electrode and water is 6: 1, and the suspension that configuration concentration is 1.0mg/ml stirs 80 minutes;
(2) to the elemental iodine (traditional Chinese medicines group, analytical pure) that adds 0.09mmol in the suspension in step (1), ultrasonic dispersion 50 minutes;
(3) with cleaned FTO conductive glass as electrode, size is: long 2.5cm, wide 2.0cm, put in the suspension of ultrasonic dispersion in step (2), the voltage of 70V is provided with direct supply, is added on two electrodes, the parallel placement of two electrodes, spacing is 2.0cm, and depositing time is three minutes;
(4) vanadium dioxide film depositing on negative electrode in step (3) is put into baking oven, 80 ℃, within 90 minutes, dry, obtain the vanadium dioxide film that FTO conductive glass is substrate.
The vanadium dioxide film picture that the resulting FTO conductive glass of the present embodiment is substrate as shown in Figure of description 6, even compact relatively generally, smooth surface and the combination of FTO Conducting Glass relatively good, places for a long time film and does not come off.
Embodiment 4:
(1) weigh 5mg hypovanadic oxide powder and join in the ethanol solution of 60ml, the suspension that configuration concentration is 0.08mg/ml, stirs 20 minutes;
(2) to the elemental iodine (traditional Chinese medicines group, analytical pure) that adds 0.006mmol in the suspension in step (1), ultrasonic dispersion 30 minutes;
(3) with cleaned FTO conductive glass as electrode, size is: long 2.5cm, wide 2.0cm, put in the suspension of ultrasonic dispersion in step (2), the voltage of 80V is provided with direct supply, is added on two electrodes, the parallel placement of two electrodes, spacing is 3.5cm, and depositing time is five minutes;
(4) vanadium dioxide film depositing on step (3) Anodic is placed in air, naturally dries, obtain the vanadium dioxide film that FTO conductive glass is substrate.
Embodiment 5:
(1) weigh 150mg hypovanadic oxide powder and join in the acetone soln of 20ml, the suspension that configuration concentration is 7.5mg/ml, stirs 50 minutes;
(2) to the elemental iodine (traditional Chinese medicines group, analytical pure) that adds 0.06mmol in the suspension in step (1), ultrasonic dispersion 30 minutes;
(3) with cleaned FTO conductive glass as electrode, size is: long 2.5cm, wide 2.0cm, put in the suspension of ultrasonic dispersion in step (2), the voltage of 20V is provided with direct supply, is added on two electrodes, the parallel placement of two electrodes, spacing is 0.8cm, and depositing time is five minutes;
(4) vanadium dioxide film depositing on negative electrode in step (3) is put in baking oven to 50 ℃, within 40 minutes, dried, obtain the vanadium dioxide film that FTO conductive glass is substrate.
The result of above embodiment, through accurate test, has all realized the preparation of vanadium dioxide film.That is, manufacture method of the present invention is compared with existing preparation method, has simple to operately, and extremely low to equipment requirements, raw material availability is high, waste liquid recycle, the significant advantage such as green non-pollution.
Below by reference to the accompanying drawings the specific embodiment of the present invention is described in detail; but these explanations can not be construed as limiting the scope of the invention; protection scope of the present invention is limited by the claims of enclosing, and any change on the claims in the present invention basis is all considered as protection scope of the present invention.

Claims (15)

1. by electrophoretic deposition, prepare a method for vanadium dioxide film, comprise the following steps:
(1) hypovanadic oxide powder is joined in the organic solvent with polar group, form suspension or colloidal sol;
(2) in the suspension obtaining to step (1) or colloidal sol, add elemental iodine, be uniformly dispersed;
(3) in the suspension obtaining in step (2), put into electrode, start electrophoretic deposition, deposition voltage is 10~100V, and depositing time is 0.5~15.0 minute; Electrode keeping parallelism, its spacing is 0.5~4.0cm;
(4) by the film drying obtaining in step (3), obtain vanadium dioxide film on electrode.
2. the method for preparing vanadium dioxide film by electrophoretic deposition as claimed in claim 1, it is characterized in that: the amount of the iodine adding in the film being deposited on electrode in described step (4) and step (2) has following relation,, if the concentration of iodine is less than or equal to 0.30mmol/L, on anode, there is vanadium dioxide film deposition, if the concentration of iodine is greater than 0.30mmol/L, on negative electrode, there is vanadium dioxide film deposition.
3. the method for preparing vanadium dioxide film by electrophoretic deposition as claimed in claim 1, is characterized in that: the solvent adding in described step (1) is: alcohols; Ketone; Cathode electrodip painting class; And the mixed solvent of the arbitrary combination of above solvent, or the mixed solvent of more than one and water in above solvent.
4. the method for preparing vanadium dioxide film by electrophoretic deposition as claimed in claim 1, is characterized in that: the solvent adding in described step (1) is: ethanol, Virahol, acetone, methyl ethyl diketone or vinylformic acid system; And the mixed solvent of the arbitrary combination of above solvent, or the mixed solvent of more than one and water in above solvent.
5. the method for preparing vanadium dioxide film by electrophoretic deposition as claimed in claim 1, is characterized in that: in the mixing solutions obtaining in described step (1), the concentration of hypovanadic oxide powder is 0.05~16.00mg/ml.
6. the method for preparing vanadium dioxide film by electrophoretic deposition as claimed in claim 1, is characterized in that: in the mixing solutions obtaining in described step (1), the concentration of hypovanadic oxide powder is 0.2~1.80mg/ml.
7. the method for preparing vanadium dioxide film by electrophoretic deposition as claimed in claim 1, is characterized in that: the elemental iodine adding in described step (2), its concentration adding is for being greater than 0.6mmol/L and below 4.0mmol/L.
8. the method for preparing vanadium dioxide film by electrophoretic deposition as claimed in claim 1, is characterized in that: the elemental iodine adding in described step (2), its concentration adding is 0.6~2.0mmol/L.
9. the method for preparing vanadium dioxide film by electrophoretic deposition as claimed in claim 1, is characterized in that: the time of disperseing in described step (2) is 10~60 minutes.
10. the method for preparing vanadium dioxide film by electrophoretic deposition as claimed in claim 1, it is characterized in that: the electrode of putting in described step (3) is conducting base/conductive substrates, this conducting base/conductive substrates is selected from stainless steel substrates, iron plate, copper sheet, silver strip, aluminium flake, platinized platinum, nickel sheet, zinc metal sheet, electrical conductivity alloy, conductive glass, conductive polymers and conductivity ceramics.
11. methods of preparing vanadium dioxide film by electrophoretic deposition as claimed in claim 1, is characterized in that: in described step (3), deposition voltage is 40~60V.
12. methods of preparing vanadium dioxide film by electrophoretic deposition as claimed in claim 1, is characterized in that: in described step (3), depositing time is 1.0~3.0 minutes.
13. methods of preparing vanadium dioxide film by electrophoretic deposition as claimed in claim 1, is characterized in that: electrode keeping parallelism in described step (3), its spacing is 1.0~2.0cm.
14. methods of preparing vanadium dioxide film by electrophoretic deposition as claimed in claim 1, is characterized in that: in described step (4), the temperature that film is dried is 20~80 ℃, and drying time is 20~100 minutes.
15. 1 kinds of vanadium dioxide films, it utilizes in claim 1~9 method manufacture described in any one to obtain.
CN201210020500.2A 2012-01-21 2012-01-21 Method for preparing vanadium dioxide film through electrophoretic deposition Expired - Fee Related CN102534731B (en)

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