CN102241482A - Intelligent temperature-control vanadium dioxide composite multifunctional thin film and preparation method thereof - Google Patents
Intelligent temperature-control vanadium dioxide composite multifunctional thin film and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an intelligent temperature-control vanadium dioxide nano composite multifunctional thin film and a preparation method thereof, and is characterized in that the nano composite thin film is VO2/SiO2, VO2/ZnO, VO2/ZrO2 or VO2/TiO2. The composite thin film consists of nano particles, wherein the size of the nano particles is kept between 10 and 500 nanometers, and the thickness of the composite thin film is 50 to 3,000 nanometers. In the invention, a wet chemical solution process is adopted, vanadium pentoxide (V2O5) powder serving as a precursor is uniformly dispersed and dissolved in a weakly reducing organic solvent to form a VOx thin film (x is more than 2.0 and less than 2.5), and the vanadium dioxide (VO2) thin film is formed by post treatment; and the nano composite thin film is prepared by a sol-gel technique. The VO2 nano composite thin film system based on co-doping and interface synergetic effect has high visible light transmittance, high infrared thermosensitive property, hydrophilic and photocatalytic functions and other functions, and a bright prospect.
Description
Technical field
The present invention is specifically related to intelligent temperature control vanadium dioxide nano composite multifunction film and preparation method thereof, belongs to VO
2The nano compound film field.
Background technology
Vanadium dioxide (VO
2) be a kind of typical thermal induced phase transition compound, 68 ℃ of transformation temperatures, be accompanied by phase transformation, reversible mutation all can take place in many photoelectric characteristics such as transmitance of its resistivity, susceptibility, light, and these remarkable performances make film in fields such as smart window, optoelectronic switch, lasing safety, optical storages high using value be arranged.
VO
2The compositional range of stable existence is narrow, therefore prepares high purity VO
2Film is difficulty comparatively.People have done a lot of work and have studied VO for this reason
2The preparation of film.Present VO
2The preparation method of film mainly contains sputtering method [(1) E.M.Heckman, L.P.Gonzalez, S.Guha.Thin Solid Films 518 (2009) 265; (2) M.B.Sahana, M.S.Dharmaprakash, S.A.Shivashankar.J.Mater.Chem.12 (2002) 333.] chemical Vapor deposition process [(1) T.D Manning, I.P Parkin, M.E Pemble, et al.Chem.Mater.16 (2004) 744; (2) T.D Manning, I.P Parkin, C.Blackman, et al.J.Mater Chem 15 (2005) 4560.], [Curr.Appl.Phys.10 (2010) 508 for (1) F.B.Dejene, R.O.Ocaya for pulsed laser deposition; (2) G.Garry, O.Durand, A.Lor dereau.Thin Solid Films 453/454 (2004) 427.] and sol-gel method [(1) S.Yamamoto, N Kasai, Y.Shimakawa, Chem.Mater.21 (2009) 198; (2) M.Pan, H.Zhong, S.Wang, et al.J.Crystal rowth 265 (2004) 121; (3)] T.J.Hanlon, J.A.Coath, M.A.Richardson.Thin Solid Films 436 (2003) 269; (4) D.P.Partlow, S.R.Gurkovich., K.C.Radford, et al.J.Appl.Phys.70 (1991) 443.] etc.VO for pure phase
2Film, although near infrared, infrared band temperature is had good regulation and control performance, it affects practical application at the lower transmittance of visible light wave range.
Summary of the invention
The object of the present invention is to provide intelligent temperature control vanadium dioxide nano composite multifunction film and preparation method thereof, the technical barrier that solve is how to guarantee VO
2In the time of the good temperature control performance of film, improve VO
2Film is realized multifunction in visible light wave range iuuminting rate.The present invention adopts the wet chemical solution method, with Vanadium Pentoxide in FLAKES (V
2O
5) powder is as presoma, by wet chemical solution method homodisperse and dissolving in the week reduction organic solvent, goes up preparation VO by lifting coating process or spin coating coating process at substrate (being substrate)
xFilm (2.0＜x＜2.5) forms vanadium dioxide (VO through aftertreatment
2) film; By sol-gel technique, preparation VO
2/ SiO
2, VO
2/ ZnO, VO
2/ ZrO
2Or VO
2/ TiO
2Etc. nano combined multi-function membrane.
This shows that 1. described nano compound film is VO
2/ SiO
2, VO
2/ ZnO, VO
2/ ZrO
2Or VO
2/ TiO
2
2. described laminated film is made up of nano particle, and its size control is at 10-500nm, and the thickness of laminated film is 50-3000nm;
3. the substrate of selecting for use is that substrate is the substrate that does not contain Na simple glass, silica glass, sapphire or contain the rutile phase structure;
Churning time is 2-5 hour when 4. making the precursor aqueous solution that contains vanadium in the step 1; H in the step 1
2The hydrogen volume percentage composition is 4%-6% in the/Ar mixed atmosphere; Recovery time is 2-5 hour; The described speed that lifts coating technique of step 1 is 40-60mn/min, and the speed of described spin coating coating technique is 2500-3500 rev/min;
5. the described pull rate of step 2 is controlled in the 10-200mm/min scope, and spin speed is controlled at 1000-20000 rev/min.
6. the synergistic VO in codoped and interface
2The nano compound film system realizes multifunctions such as hydrophilic and photochemical catalysis for improving its visible region transmitance and good infrared sensitive characteristic, and wide prospect is provided.In preferred embodiment, VO
2Film metal-insulator film transformation temperature is 63 ℃, and the printing opacity rate variance is 60% before and after the phase transformation of wavelength 2500nm place, VO
2/ SiO
2Nano compound film visible region transmittance is than VO
2The film raising (sees embodiment 1 for details) more than 16%.
Describe the present invention below in detail.
A) material preparation
(1) V0
2The preparation of film:
Use V
2O
5Powder, phenylcarbinol and Virahol stirred 2-5 hour under 80 ℃ of oil bath conditions with 1: 4: 50 mixed in molar ratio, obtained the precursor aqueous solution of vanadium; By lifting coating technique or spin coating coating technique, preparation VO
xFilm (2.0＜x＜2.5) is then at 410 ℃, H
2Reductase 12-5 hour in the/Ar mixed atmosphere (hydrogen volume content 4-6%) can form the VO of pure phase behind the naturally cooling
2Film.
(2) V0
2The nano compound film preparation:
By sol-gel technique, adopt metal alkoxide, preparation SiO
2, ZnO, ZrO
2Or TiO
2Deng forerunner's colloidal sol; Preparation there is VO
2Vertically, at the uniform velocity (10-200mm/min) or spin coating coating technique (1000-20000r/min) be from SiO by lifting coating technique for the substrate of film
2, ZnO, ZrO
2Or TiO
2Deng forerunner's colloidal sol in prepare precursor thin film; Perhaps, at first prepare VO
2-SiO
2, VO
2-ZnO, VO
2-ZrO
2Or VO
2-TiO
2Deng compound precursor colloidal sol, then by lifting coating technique or the spin coating coating technique prepares complex thin film structure.Place the ultra-clean baking oven, dry 5-30min can obtain required nano combined multi-function membrane under 100 ℃ of conditions.
B) sample characterization and performance evaluation
(1) thing of film characterizes with pattern
Gained film sample of the present invention is passed through field emission scanning electron microscope (FE-SEM, Hitachi S-4800) viewing film surface and cross-section morphology; By with field transmission Electronic Speculum (TEM, JEM2100F) viewing film structure; By atomic force microscope (AFM, Japanese Seiko II SPI3800V ﹠amp; The spa300HV type) comes the surfaceness of viewing film; Come the thickness of measure sample by Dektak150 type surface profiler; By X-ray powder diffraction instrument (Rigaku D/Max-2550V) analysed film thing phase.
(2) optical property characterizes
With the transmitance of the resulting film of the present invention with ultraviolet-visible-near infrared spectrometer (Hitachi U4100) testing film.
Be characterised in that codoped and the synergistic VO in interface by nano compound film provided by the invention
2The nano compound film system realizes multifunctions such as hydrophilic and photochemical catalysis for improving its visible region transmitance and good infrared sensitive characteristic, and wide prospect is provided.
Description of drawings
Fig. 1 VO
2/ SiO
2Nano compound film sample section pattern SEM figure;
Fig. 2 VO
2Film, VO
2/ SiO
2Transmittance figure before and after the nano compound film sample metal-insulator phase transition;
Fig. 3 VO
2/ SiO
2The transmittance figure at 2500nm place before and after the nano compound film sample metal-insulator phase transition.
Embodiment
Introduce embodiments of the invention below, to understanding of the present invention, but the present invention is limited to embodiment absolutely not with further increase.
Embodiment 1:
Use V
2O
5Powder, phenylcarbinol and Virahol stirred 2 hours under 80 ℃ of conditions with 1: 4: 50 mixed in molar ratio, made the presoma of vanadium; By lifting coating technique (speed is 50mm/min), preparation VO
xFilm (2.0＜x＜2.5) is then at 410 ℃, H
2Reduction is 3 hours in the/Ar mixed atmosphere (hydrogen volume content 4%), can form the VO of crystallization behind the naturally cooling
2Film.By sol-gel technique, with analytically pure tetraethoxy, dehydrated alcohol, ammoniacal liquor and deionized water, according to 1: 10: 0.2-0.5: 0.1 volume ratio prepares SiO
2Forerunner's colloidal sol; By lifting coating technique (speed is 50mm/min), preparation VO
2/ SiO
2Laminated film, dry 10min can obtain required VO under 100 ℃ then
2/ SiO
2Nano compound film.
Fig. 1 correspondence be VO
2/ SiO
2The surface topography SEM figure of nano compound film, substrate/VO
2, VO
2/ SiO
2And SiO
2Exist obvious limit between/air, use black dotted lines in the drawings in order to indicate SiO
2Granular size is 20-50nm, VO
2Grain size is distributed in the 80-120nm scope.
Fig. 2 is VO
2/ SiO
2Transmittance figure before and after the film sample metal-insulator phase transition, dotted line can be seen from Fig. 2, in the process of heating, VO
2Film remains unchanged at the transmittance of visible region, then along with temperature descends fast, reduces to 10% at wavelength 2500nm place from 70% near infrared, infrared transmittance, has changed 60%; And in the process of naturally cooling, return to transparently again rapidly, embodied good metal-insulator phase transition characteristic.By at VO
2Film surface prepares SiO
2Film is realized the anti-reflection synergy of infrared regulation and control-visible light, and at visible light wave range, transmittance has improved about 13%, and at infrared band, has also improved the transmitance (solid line among Fig. 2) of light, has improved temperature induced color changing material temperature control performance; While VO
2Film has still kept good metal-insulator phase transition performance (Fig. 3).The synergistic VO in codoped and interface
2/ SiO
2Nano combined system provides wide prospect for improving its visible region transmitance and good infrared sensitive characteristic.
Embodiment 2:
Use V
2O
5Powder, phenylcarbinol and Virahol stirred 5 hours under 80 ℃ of conditions with 1: 4: 50 mixed in molar ratio, by spin coating coating technique (speed is 3000r/min), and preparation VO
xFilm (2.0＜x＜2.5) is then at 410 ℃, H
2Reduction is 3 hours in the/Ar mixed atmosphere (hydrogen volume content 4%), can form the VO of crystallization behind the naturally cooling
2Film.By sol-gel technique, with analytically pure tetraethoxy, dehydrated alcohol, ammoniacal liquor and deionized water, according to 1: 10: 0.2-0.5: 0.1 volume ratio prepares SiO
2Forerunner's colloidal sol; By spin coating coating technique (speed is 3000r/min), preparation VO
2Nano compound film, dry 10min can obtain required VO under 100 ℃ then
2/ SiO
2Nano compound film.All the other are with embodiment 1.
Embodiment 3:
Use V
2O
5Powder, phenylcarbinol and Virahol stirred 2 hours under 80 ℃ of conditions with 1: 4: 50 mixed in molar ratio; By sol-gel technique, with analytically pure tetraethoxy, dehydrated alcohol, ammoniacal liquor and deionized water, according to 1: 10: 0.2-0.5: 0.1 volume ratio prepares SiO simultaneously
2Forerunner's colloidal sol, under the stirring at room condition, obtain VO then
x-SiO
2The compound precursor colloidal sol of (2.0＜x＜2.5); By lifting coating technique (speed is 50mm/min), preparation VO
x-SiO
2Nano compound film is then at 410 ℃, H
2Reduction is 3 hours in the/Ar mixed atmosphere (hydrogen volume content 4%), can form the VO of crystallization behind the naturally cooling
2-SiO
2Nano compound film.All the other are with embodiment 1.
Embodiment 4:
Use V
2O
5Powder, phenylcarbinol and Virahol stirred 2 hours under 80 ℃ of conditions with 1: 4: 50 mixed in molar ratio, by lifting coating technique (speed is 50mm/min), preparation VO
xFilm (2.0＜x＜2.5) is then at 410 ℃, H
2Reduction is 3 hours in the/Ar mixed atmosphere (hydrogen volume content 4%), can form the VO of crystallization behind the naturally cooling
2Film.By sol-gel technique, with the forerunner's colloidal sol of preparation ZnO in the solution of 8.23g zinc acetate adding 50ml thanomin (1.9g) and ethylene glycol monomethyl ether; By lifting coating technique (speed is 50mm/min), preparation VO
2/ ZnO nano compound film, dry 10min can obtain required VO under 100 ℃ then
2/ ZnO nano compound film.
Prepared V O
2The surface topography SEM figure of/ZnO nano compound film demonstrates at substrate/VO
2, VO
2/ SiO
2And SiO
2Have the obvious boundary that is similar to Fig. 1 between the space, all the other are with embodiment 1.
Embodiment 5:
Use V
2O
5Powder, phenylcarbinol and Virahol stirred 2 hours under 80 ℃ of conditions with 1: 4: 50 mixed in molar ratio; By sol-gel technique, the forerunner's colloidal sol with preparation ZnO in the solution of 8.23g zinc acetate adding 50ml thanomin (1.9g) and ethylene glycol monomethyl ether under the stirring at room condition, obtains VO then simultaneously
xThe compound precursor colloidal sol of-ZnO (2.0＜x＜2.5); By lifting coating technique (speed is 50mm/min), preparation VO
x-ZnO nano compound film is then at 410 ℃, H
2Reduction is 3 hours in the/Ar mixed atmosphere (hydrogen volume content 4%), can form the VO of crystallization behind the naturally cooling
2-ZnO nano compound film.All the other are with embodiment 1.
Embodiment 6:
Use V
2O
5Powder, phenylcarbinol and Virahol stirred 2 hours under 80 ℃ of conditions with 1: 4: 50 mixed in molar ratio, by lifting coating technique (speed is 50mm/min), preparation VO
xFilm (2.0＜x＜2.5) is then at 410 ℃, H
2Reduction is 3 hours in the/Ar mixed atmosphere (hydrogen volume content 6%), can form the VO of crystallization behind the naturally cooling
2Film.By sol-gel technique, with 0.25molL
-1ZrOCl
28H
2O prepares ZrO by the hydro-thermal route of synthesis
2Forerunner's colloidal sol; By lifting coating technique (speed is 50mm/min), preparation VO
2Nano compound film, dry 10min can obtain required VO under 100 ℃ then
2/ ZrO
2Nano compound film.
Prepared V O
2/ ZrO
2The SEM figure of nano compound film demonstrates at substrate/VO
2, VO
2/ ZrO
2And ZrO
2Have the obvious boundary that is similar to Fig. 1 between/space, all the other are with embodiment 1.
Embodiment 7:
Use V
2O
5Powder, phenylcarbinol and Virahol stirred 2 hours under 80 ℃ of conditions with 1: 4: 50 mixed in molar ratio; Simultaneously by sol-gel technique, with 0.25mol L
-1ZrOCl
28H
2O prepares ZrO by the hydro-thermal route of synthesis
2Forerunner's colloidal sol, under the stirring at room condition, obtain VO then
x-ZrO
2The compound precursor colloidal sol of (2.0＜x＜2.5); By lifting coating technique (speed is 50mm/min), preparation VO
x-ZrO
2Nano compound film is then at 410 ℃, H
2Reduction is 3 hours in the/Ar mixed atmosphere (hydrogen volume content 4%), can form the VO of crystallization behind the naturally cooling
2-ZrO
2Nano compound film.All the other are with embodiment 1.
Embodiment 8:
Use V
2O
5Powder, phenylcarbinol and Virahol stirred 2 hours under 80 ℃ of conditions with 1: 4: 50 mixed in molar ratio, by lifting coating technique (speed is 50mm/min), preparation VO
xFilm (2.0＜x＜2.5) is then at 410 ℃, H
2Reduction is 3 hours in the/Ar mixed atmosphere (hydrogen volume content 4%), can form the VO of crystallization behind the naturally cooling
2Film.By sol-gel technique, with analytically pure tetrabutyl titanate, dehydrated alcohol, methyl ethyl diketone and deionized water, according to 1: 10: 0.3: 0.1 volume ratio prepares TiO
2Forerunner's colloidal sol; By lifting coating technique (speed is 50mm/min), preparation VO
2Nano compound film, dry 10min can obtain required VO under 100 ℃ then
2/ TiO
2Nano compound film.
Prepared V O
2/ TiO
2The SEM figure of nano compound film demonstrates at substrate/VO
2, VO
2/ TiO
2And TiO
2/ spatial class is similar to the boundary of Fig. 1, and all the other are with embodiment 1.
Embodiment 9:
Use V
2O
5Powder, phenylcarbinol and Virahol stirred 2 hours under 80 ℃ of conditions with 1: 4: 50 mixed in molar ratio; By sol-gel technique, with analytically pure tetrabutyl titanate, dehydrated alcohol, methyl ethyl diketone and deionized water, according to 1: 10: 0.3: 0.1 volume ratio prepares TiO simultaneously
2Forerunner's colloidal sol, under the stirring at room condition, obtain VO then
x-TiO
2The compound precursor colloidal sol of (2.0＜x＜2.5); By lifting coating technique (speed is 50mm/min), preparation VO
x-TiO
2Nano compound film is then at 410 ℃, H
2Reduction is 3 hours in the/Ar mixed atmosphere (hydrogen volume content 4%), can form the VO of crystallization behind the naturally cooling
2-TiO
2Nano compound film.All the other are with embodiment 1.
Claims (9)
1. intelligent temperature control VO
2Nano compound film is characterized in that described nano compound film is VO
2/ SiO
2, VO
2/ ZnO, VO
2/ ZrO
2Or VO
2/ TiO
2
2. by the described nano compound film of claim 1, it is characterized in that described laminated film is made up of nano particle, its size control is at 10-500nm, and the thickness of laminated film is 50-3000nm.
3. by the described nano compound film of claim 1, it is characterized in that described VO
2/ SiO
2The surface topography of nano compound film demonstrates substrate/VO
2, VO
2/ SiO
2And SiO
2There is obvious limit between air, SiO
2Particle size is 20-50nm, VO
2Grain-size is 80-120nm.
4. preparation is characterized in that with V as the method for each described laminated film among the claim 1-3
2O
5Powder is a presoma, is equipped with 2.0＜x＜2.5VO by the wet chemical solution legal system
xFilm forms VO through aftertreatment
2Film; By sol-gel technique, prepare VO at last
2/ SiO
2, VO
2/ ZnO, VO
2/ ZrO
2Or VO
2/ TiO
2Nano compound film; Concrete steps comprise:
(1) VO
2The preparation of film:
Use V
2O
5Powder, phenylcarbinol and Virahol stir under 80 ℃ of oil bath conditions with 1: 4: 50 mixed in molar ratio, obtain the precursor aqueous solution of vanadium; By lifting coating technique or spin coating coating technique, preparation 2.0＜x＜2.5VO
xFilm is then at 410 ℃, H
2Reduce in/Ar the mixed atmosphere, can form the VO of pure phase behind the naturally cooling
2Film;
(2) VO
2The preparation of nano compound film:
By sol-gel technique, adopt metal alkoxide, preparation SiO
2, ZnO, ZrO
2Or TiO
2Forerunner's colloidal sol; Step (1) preparation there is VO
2The substrate of film by lift coating technique vertically, at the uniform velocity or the spin coating coating technique from SiO
2, ZnO, ZrO
2Or TiO
2Forerunner's colloidal sol in prepare precursor thin film; Perhaps, at first prepare VO
x-SiO
2, VO
x-ZnO, VO
x-ZrO
2Or VO
x-TiO
2Deng compound precursor colloidal sol, prepare complex thin film structure by lifting coating technique or spin coating coating technique then; Place baking oven at last, dry 5-30min can obtain required nano combined multi-function membrane under 100 ℃ of conditions.
5. by the described preparation method of claim 4, it is characterized in that the substrate of selecting for use is that substrate is the substrate that does not contain Na simple glass, silica glass, sapphire or contain the rutile phase structure.
6. by the described preparation method of claim 4, it is characterized in that:
Churning time is 2-5 hour when 1. making the precursor aqueous solution that contains vanadium in the step 1;
2. H in the step 1
2The hydrogen volume percentage composition is 4%-6% in the/Ar mixed atmosphere; Recovery time is 2-5 hour;
3. the described speed that lifts coating technique of step 1 is 40-60mn/min, and the speed of described spin coating coating technique is 2500-3500 rev/min.
7. by the described preparation method of claim 4, it is characterized in that the described pull rate of step 2 is controlled in the 10-200mm/min scope, spin speed is controlled at 1000-20000 rev/min.
8. by the application of the described nano compound film of claim 1, it is characterized in that VO
2/ SiO
2, VO
2/ ZnO, VO
2/ ZrO
2Or VO
2/ TiO
2Nano compound film thermochromism, visible region high permeability, hydrophilic and photocatalytic multifunctional characteristic.
9. by the described application of claim 8, it is characterized in that VO
2/ SiO
2Nano compound film drops to 10% in wavelength 2500nm place infrared light transmission rate from 70%, and in natural cooling process, returns to transparently again rapidly, demonstrates the metal-insulator phase transition characteristic, realizes the anti-reflection synergy of infrared regulation and control-visible light.
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