CN102534731A - Method for preparing vanadium dioxide film through electrophoretic deposition - Google Patents
Method for preparing vanadium dioxide film through electrophoretic deposition Download PDFInfo
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- CN102534731A CN102534731A CN2012100205002A CN201210020500A CN102534731A CN 102534731 A CN102534731 A CN 102534731A CN 2012100205002 A CN2012100205002 A CN 2012100205002A CN 201210020500 A CN201210020500 A CN 201210020500A CN 102534731 A CN102534731 A CN 102534731A
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- vanadium dioxide
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D13/00—Electrophoretic coating characterised by the process
- C25D13/02—Electrophoretic 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
Technical field
The present invention relates to electronic material and devices field, refer more particularly to a kind of method for preparing vanadium dioxide film through electrophoretic deposition.
Background technology
Vanadium dioxide is a kind of typical thermic phase change materials, in known phase change material, changes temperature mutually near room temperature, and it reversible structure takes place in the time of 68 ℃ changes mutually, changes to the pyritous rutile structure from cryogenic monocline.When being lower than phase transition temperature, present the semi-conductor phase, resistivity; The transmitance of susceptibility and infrared light is all very high, and when being higher than phase transition temperature, presents metallographic phase; Resistivity, the transmitance of susceptibility and infrared light is all undergone mutation, and drops to very low; Has very significantly infrared switch, electrical switch and magnetics switch character.Simultaneously it is carried out high volence metal ion and mix, can realize artificial adjustment, and its reversible electricity, magnetics and infrared switch character are constant its phase transition temperature.Based on the excellent optics of vanadium dioxide, electricity and magnetic property, it is at the smart window material of buildings, thermistor, optoelectronic switch, there is huge potential application aspects such as optical storage.
Vanadium dioxide has excellent optics, and electricity and magnetic property are impelling people to its research that does not stop, and have developed a lot of method and technologies that prepare vanadium dioxide.Chinese patent (publication number CN101559981A) adopts combustion method to prepare vanadium dioxide; Chinese patent (publication number CN1522965A) adopts Hydrothermal Preparation vanadium dioxide or the like; But the optics of vanadium dioxide; The form of promoting the use of mainly of electricity and magnetics switch character with vanadium dioxide film, and lack the method that effectively prepares vanadium dioxide film at present, it is promoted the use of received great restriction.Though Chinese patent (publication number CN101280413A); Chinese patent (publication number CN101265036A) all adopts method low temperature depositing vanadium dioxide film on glass substrate of magnetron sputtering plating, but becomes the method for phase very easily to generate the impurity phase after its first film forming, and its glass substrate needs heat; Cause too high energy consumption; Do not reach the purpose of energy-saving and emission-reduction, also inevitably use large-scale magnetron sputtering equipment, not only increased production cost; But also need precise parameters control; Be unfavorable for large-scale preparation, also largely limit promoting the use of of vanadium dioxide, the method for preparing vanadium dioxide film of therefore developing a kind of simple and efficient is the difficult point of a technology.
Electrophoretic deposition is meant the effect that relies on DC electric field; Make directed the moving of charged particle in colloid or the suspension-s; And be deposited on the definite shape electrode with opposite charges; Any solid material that can process fine particles (particle diameter is not more than 30 microns) or colloidal sol can carry out electrophoretic deposition, and its scope of application comprises metal, polymkeric substance, carbide, oxide compound and inorganic salts etc.Electrophoretic deposition applies it to the preparation field of vanadium dioxide film as present also nobody of method that a kind of simple and efficient prepares film.
Summary of the invention
The present invention just is being based on electrophoretic deposition technique and is accomplishing, and the present invention adopts simple method, and directly electrophoretic deposition is successfully prepared vanadium dioxide film on different conductive substrates; And electrochemical reaction do not take place on the electrode; Do not change the structure and the character of hypovanadic oxide powder, XianCheng is the back film forming mutually, has overcome to become mutually after the first film forming in the existing technology of preparing to cause that a lot of dephasigns are arranged in the film; And then have a strong impact on its optics, the shortcoming of electricity and magnetics switch character.Technology 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, and is economical pollution-free, is fit to promote the use of on a large scale.
Promptly; The present invention provides a kind of method for preparing vanadium dioxide film through electrophoretic deposition; Its XianCheng is the back film forming mutually; Having solved present preparation vanadium dioxide film needs to become phase after the first film forming, thereby causes having a lot of dephasigns in the film, and then has a strong impact on the problem of its optics, electricity and magnetics switch character.The existing preparation technology also needs the main equipment of expensive, the control complicated parameter, and also have raw material availability not high, shortcoming such as can not prepare in a large number, increased production cost virtually, 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, and its concrete technical scheme is following:
(1) hypovanadic oxide powder is joined in the solvent, form suspension-s or colloidal sol;
(2) in suspension-s that step (1) obtains or colloidal sol, add elemental iodine, be uniformly dispersed;
(3) put into electrode in the suspension-s that in step (2), obtains, the beginning electrophoretic deposition;
(4) with the film drying that on electrode, obtains in the step (3), obtain vanadium dioxide film.
The present invention also provides a kind of vanadium dioxide film, and it obtains through the aforesaid method manufacturing.
The vanadium dioxide film of the present invention's preparation directly adopts hypovanadic oxide powder commercially available or that prepare in advance, adds solvent and a spot of elemental iodine, mixes; After ultra-sonic dispersion is even,, puts into cleaned electrode then and begin the electrophoretic deposition plated film as electrophoretic deposition liquid; This method does not need main equipment, does not change the structure and the character of deposition front and back hypovanadic oxide powder, and its technology is simple; Workable, film forming speed is fast, easily control; Raw material availability is high, and waste liquid can recycled for multiple times, is fit to large-scale production.
Description of drawings
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 embodiment 1 deposition preparation back vanadium dioxide film.
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 present invention provides a kind of and prepares the method for vanadium dioxide film through electrophoretic deposition, said method comprising the steps of:
(1) hypovanadic oxide powder is joined in the solvent, form suspension-s or colloidal sol;
(2) in suspension-s that step (1) obtains or colloidal sol, add elemental iodine, be uniformly dispersed;
(3) put into electrode in the suspension-s that in step (2), obtains, the beginning electrophoretic deposition;
(4) with the film drying that on electrode, obtains in the step (3), obtain vanadium dioxide film.
The present invention also provides a kind of preparation vanadium dioxide film for preparing the method preparation of vanadium dioxide film through said electrophoretic deposition.
Wherein,, make suspension particle be with electric charge more easily through adding a certain amount of elemental iodine, as not adding a spot of iodine, sedimentary less efficient some, add iodine, in the 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 that uses among the present invention adopts general commercially available prod to get final product, and also can adopt the following steps preparation, with 20ml formaldehyde and 0.0025mol V
2O
5Mix, add the 60ml deionized water behind the about 1h of magnetic agitation and transfer in the 100ml autoclave, keep 24h down at 180 ℃, naturally cool to room temperature, the collecting precipitation thing is used deionized water and absolute ethanol washing 5～6 times respectively.In baking oven, dry 10h at last under 60 ℃, obtain bluish grey VO
2(B) powder.The powder that obtains is placed the tubular type retort furnace, and 500 ℃ of thermal treatment 6h naturally cool to room temperature then in argon atmosphere, promptly obtain VO
2(M) powder.
Preferred 0.05～the 16.00mg/ml of concentration of vanadium dioxide, more preferably 0.2～1.8mg/ml in the step (1).
The solvent that uses in the step (1) is generally: alcohols, and like ethanol, Virahol etc.; Ketone, like acetone, methyl ethyl diketone etc.; The cathode electrodip painting class is like vinylformic acid system etc.; And the mixing solutions of the arbitrary combination of above solution.
Churning time in the step (1) is preferably 5～90 minutes.
In the step (2), the concentration of the elemental iodine of adding is preferably greater than 0.0mmol/L and below the 4.0mmol/L, more preferably 0.6～2.0mmol/L; Churning time is preferably 10～60 minutes, and the ultra-sonic dispersion time is preferably 10～60 minutes.
The electrode of putting in the 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; Preferred 10～the 100V of deposition voltage, more preferably 30～50V, preferred 0.5～6.0 minute of depositing time, more preferably 1.5～2.5 minutes; The electrode keeping parallelism, the preferred 0.5～4.0cm of its spacing, more preferably 1.0～2.0cm.
The amount of the iodine that adds in film that deposition is come out on electrode in the step (4) and the step (2) has following relation; That is: if the concentration of iodine is less than or equal to 0.30mmol/L; The vanadium dioxide film deposition is arranged, if the concentration of iodine, has the vanadium dioxide film deposition greater than 0.30mmol/L on the negative electrode on the anode; The temperature of its oven dry is preferably 20～80 ℃, and drying time is preferably 20～100 minutes.
Specify the present invention through following embodiment below, 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; Adopt 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 of weighing 50mg is put in the 30ml acetone, and configuration concentration is the suspension-s of 1.67mg/ml, stirs 15 minutes;
(2) elemental iodine (traditional Chinese medicines group, analytical pure) of adding 0.021mmol in the suspension-s in step (1), ultra-sonic dispersion 20 minutes;
(3) with cleaned FTO conductive glass as electrode, size is: long 2.5cm, wide 2.0cm; Put in the suspension-s of ultra-sonic dispersion in the step (2), the voltage of 50V is provided, be added on two electrodes with direct supply; The parallel placement of two electrodes, spacing are 2.0cm, and depositing time is two minutes;
(4) sedimentary vanadium dioxide film on the negative electrode in the step (3) is put into baking oven, 40 ℃, oven dry in 30 minutes obtains the vanadium dioxide film that the FTO conductive glass is a substrate.
The XRD spectra of the hypovanadic oxide powder that present embodiment is used is shown in Figure of description 1; The FTO conductive glass that obtains be the XRD spectra of vanadium dioxide film of substrate shown in Figure of description 2, the XRD spectra after the 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.The FTO conductive glass that the present invention adopted is to be produced by NHTechno company, model TCO-15, and plating one deck 350nm is thick on the thick simple glass of 2.2mm mixes fluorine SnO
2Conductive film.
Electrochemical reaction does not take place in the XRD spectra explanation electrophoretic deposition process of vanadium dioxide film; The structure of powder and substrate does not change; Kept the structure and the character of powder fully, thereby avoided becoming phase after the first film forming in the existing at present preparation vanadium dioxide film technology; Thereby the generation dephasign, and then influence the huge shortcoming of its character.
The FTO conductive glass is that substrate vanadium dioxide film SEM picture is shown in Figure of description 3; The thickness of vanadium dioxide film is 6.4 microns; Film is not very fine and close, the FTO conductive glass be the vanadium dioxide film picture of substrate shown in Figure of description 4, even compact relatively generally; Film and FTO Conducting Glass binding ratio are better, difficult drop-off.
Embodiment 2:
(1) hypovanadic oxide powder of weighing 20mg is put in the methyl ethyl diketone solution of 30ml, and configuration concentration is the suspension-s of 0.67mg/ml, stirs 30 minutes;
(2) elemental iodine (traditional Chinese medicines group, analytical pure) of adding 0.048mmol in the suspension-s in step (1), ultra-sonic dispersion 40 minutes;
(3) with cleaned copper sheet as electrode, size is: long 3.0cm, wide 2.5cm; Put in the suspension-s of ultra-sonic dispersion in the step (2), the voltage of 30V is provided, be added on two electrodes with direct supply; The parallel placement of two electrodes, spacing are 1.0cm, and depositing time is three minutes;
(4) with in the step (3) on negative electrode sedimentary vanadium dioxide film put into baking oven, 60 ℃, 20 minutes the oven dry, obtain the vanadium dioxide film that copper sheet is a substrate.
The resulting copper sheet of present embodiment be the vanadium dioxide film picture of substrate shown in Figure of description 5, even compact relatively generally, and relatively good with copper sheet substrate bonded is placed the film difficult drop-off for a long time.
Embodiment 3:
(1) weighing 30mg hypovanadic oxide powder joins in the mixing solutions of the transparent electrocoating paint of negative electrode and water of 30ml, and wherein the volume ratio of transparent electrocoating paint of negative electrode and water is 6: 1, and configuration concentration is the suspension-s of 1.0mg/ml, stirs 80 minutes;
(2) elemental iodine (traditional Chinese medicines group, analytical pure) of adding 0.09mmol in the suspension-s in step (1), ultra-sonic dispersion 50 minutes;
(3) with cleaned FTO conductive glass as electrode, size is: long 2.5cm, wide 2.0cm; Put in the suspension-s of ultra-sonic dispersion in the step (2), the voltage of 70V is provided, be added on two electrodes with direct supply; The parallel placement of two electrodes, spacing are 2.0cm, and depositing time is three minutes;
(4) sedimentary vanadium dioxide film on the negative electrode in the step (3) is put into baking oven, 80 ℃, oven dry in 90 minutes obtains the vanadium dioxide film that the FTO conductive glass is a substrate.
The vanadium dioxide film picture that the resulting FTO conductive glass of present embodiment is a substrate compares even compact generally shown in Figure of description 6, smooth surface and FTO Conducting Glass bonded are relatively good, place film for a long time and do not come off.
Embodiment 4:
(1) weighing 5mg hypovanadic oxide powder joins in the ethanol solution of 60ml, and configuration concentration is the suspension-s of 0.08mg/ml, stirs 20 minutes;
(2) elemental iodine (traditional Chinese medicines group, analytical pure) of adding 0.006mmol in the suspension-s in step (1), ultra-sonic dispersion 30 minutes;
(3) with cleaned FTO conductive glass as electrode, size is: long 2.5cm, wide 2.0cm; Put in the suspension-s of ultra-sonic dispersion in the step (2), the voltage of 80V is provided, be added on two electrodes with direct supply; The parallel placement of two electrodes, spacing are 3.5cm, and depositing time is five minutes;
(4) sedimentary vanadium dioxide film on the anode in the step (3) is placed in the air, dries naturally, obtain the vanadium dioxide film that the FTO conductive glass is a substrate.
Embodiment 5:
(1) weighing 150mg hypovanadic oxide powder joins in the acetone soln of 20ml, and configuration concentration is the suspension-s of 7.5mg/ml, stirs 50 minutes;
(2) elemental iodine (traditional Chinese medicines group, analytical pure) of adding 0.06mmol in the suspension-s in step (1), ultra-sonic dispersion 30 minutes;
(3) with cleaned FTO conductive glass as electrode, size is: long 2.5cm, wide 2.0cm; Put in the suspension-s of ultra-sonic dispersion in the step (2), the voltage of 20V is provided, be added on two electrodes with direct supply; The parallel placement of two electrodes, spacing are 0.8cm, and depositing time is five minutes;
(4) sedimentary vanadium dioxide film on the negative electrode in the step (3) is put in the baking oven 50 ℃, oven dry in 40 minutes obtains the vanadium dioxide film that the FTO conductive glass is a substrate.
The result of above embodiment has all realized the preparation of vanadium dioxide film through accurate test.That is, method of manufacture of the present invention is compared with prior preparation method, has simple to operately, and extremely low to equipment requirements, raw material availability is high, waste liquid recycle, significant advantage such as green non-pollution.
More than combine the accompanying drawing specific embodiments of the invention to do detailed explanation; But these explanations can not be construed as limiting the scope of the invention; Protection scope of the present invention is limited the claims of enclosing, and any change on claim of the present invention basis all is regarded as protection scope of the present invention.
Claims (10)
1. one kind prepares the method for vanadium dioxide film through electrophoretic deposition, may further comprise the steps:
(1) hypovanadic oxide powder is joined in the organic solvent of band polar group, form suspension-s or colloidal sol;
(2) in suspension-s that step (1) obtains or colloidal sol, add elemental iodine, be uniformly dispersed;
(3) put into electrode in the suspension-s that in step (2), obtains, the beginning electrophoretic deposition;
(4) with the film drying that on electrode, obtains in the step (3), obtain vanadium dioxide film.
2. the method for preparing vanadium dioxide film through electrophoretic deposition as claimed in claim 1; It is characterized in that: the amount of the iodine that adds in film that deposition is come out on electrode in the said step (4) and the step (2) has following relation; That is,, the vanadium dioxide film deposition is arranged on anode if the concentration of iodine is less than or equal to 0.30mmol/L; If the concentration of iodine, has the vanadium dioxide film deposition greater than 0.30mmol/L on negative electrode.
3. as claimed in claim 1ly prepare the method for vanadium dioxide film through electrophoretic deposition, it is characterized in that: the solvent that adds in the said step (1) is: alcohols, like ethanol, Virahol etc.; Ketone is like acetone, methyl ethyl diketone etc.; The cathode electrodip painting class is like vinylformic acid system etc.; And the mixed solvent of the arbitrary combination of above solvent, or the mixed solvent of more than one and water in the above solvent.
4. as claimed in claim 1ly prepare the method for vanadium dioxide film through electrophoretic deposition, it is characterized in that: in the mixing solutions that obtains in the said step (1), the concentration of hypovanadic oxide powder is 0.05～16.00mg/ml, preferred 0.2～1.80mg/ml.
5. as claimed in claim 1ly prepare the method for vanadium dioxide film through electrophoretic deposition, it is characterized in that: the elemental iodine that adds in the said step (2), the concentration of its adding is greater than 0.0mmol/L and below the 4.0mmol/L, preferred 0.6～2.0mmol/L.
6. as claimed in claim 1ly prepare the method for vanadium dioxide film through electrophoretic deposition, it is characterized in that: the dispersive time is 10～60 minutes in the said step (2).
7. the method for preparing vanadium dioxide film through electrophoretic deposition as claimed in claim 1; It is characterized in that: the electrode of putting in the said 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.
8. as claimed in claim 1ly prepare the method for vanadium dioxide film through electrophoretic deposition, it is characterized in that: deposition voltage is 10～100V in the said step (3), and preferred 40～60V, depositing time are 0.5～15.0 minute, preferred 1.0～3.0 minutes; The electrode keeping parallelism, its spacing is 0.5～4.0cm, is preferably 1.0～2.0cm.
9. as claimed in claim 1ly prepare the method for vanadium dioxide film through electrophoretic deposition, it is characterized in that: in the said step (4), the temperature of film oven dry is 20～80 ℃, and drying time is 20～100 minutes.
10. vanadium dioxide film, it utilizes, and each said method manufacturing obtains in the claim 1～9.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210020500.2A CN102534731B (en) | 2012-01-21 | 2012-01-21 | Method for preparing vanadium dioxide film through electrophoretic deposition |
| PCT/CN2013/070699 WO2013107392A1 (en) | 2012-01-21 | 2013-01-18 | Method for preparing vanadium dioxide film by electrophoresis deposition |
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|---|---|---|---|
| CN201210020500.2A CN102534731B (en) | 2012-01-21 | 2012-01-21 | Method for preparing vanadium dioxide film through electrophoretic deposition |
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| CN102534731A true CN102534731A (en) | 2012-07-04 |
| CN102534731B CN102534731B (en) | 2014-09-24 |
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| WO2013107392A1 (en) * | 2012-01-21 | 2013-07-25 | 中国科学技术大学 | Method for preparing vanadium dioxide film by electrophoresis deposition |
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