CN102241482B - 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 PDF

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CN102241482B
CN102241482B CN 201110112483 CN201110112483A CN102241482B CN 102241482 B CN102241482 B CN 102241482B CN 201110112483 CN201110112483 CN 201110112483 CN 201110112483 A CN201110112483 A CN 201110112483A CN 102241482 B CN102241482 B CN 102241482B
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CN102241482A (en
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黄富强
李德增
丁尚军
赵伟
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Shanghai Institute of Ceramics of CAS
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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

Intelligent temperature-control vanadium dioxide composite multifunctional thin film and preparation method thereof
Technical field
The present invention is specifically related to Intelligent temperature-control vanadium dioxide composite multifunctional thin 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 occur 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 2Thin film technology.Present VO 2The thin film technology method 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 performance of control, 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 composite multifunctional thin 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 Uniform Dispersion and dissolving in the week reduction organic solvent, by lifting coating process or spin coating coating process at the upper preparation of substrate (being substrate) VO 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, 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 comprised 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 is that substrate is the substrate that does not contain Na simple glass, silica glass, sapphire or contain the Rutile Type structure;
When 4. making the precursor aqueous solution that contains vanadium in step 1, churning time is 2-5 hour; H in step 1 2In/Ar mixed atmosphere, the hydrogen volume percentage composition is 4%-6%; 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 is for improving its visible region transmitance and good infrared sensitive characteristic, realizes hydrophilic and the multifunction such as photochemical catalysis, and wide prospect is provided.In preferred embodiment, VO 2Film metal-insulator film transformation temperature is 63 ℃, and before and after wavelength 2500nm place's phase transformation, the printing opacity rate variance is 60%, VO 2/ SiO 2Nano compound film visible region transmittance is than VO 2The film raising (sees embodiment 1 for details) more than 16%.
The below describes the present invention in detail.
A) material preparation
(1) V0 2Thin film technology:
Use V 2O 5Powder, phenylcarbinol and Virahol stirred 2-5 hour under 80 ℃ of oil bath conditions with the mixed in molar ratio of 1: 4: 50, 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/Ar mixed atmosphere (hydrogen volume content 4-6%) can form the VO of pure phase after 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; To be prepared with 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.Be placed in ultra-clean baking oven, under 100 ℃ of conditions, dry 5-30min can obtain required nano combined multi-function membrane.
B) sample characterization and performance evaluation
(1) phase of film and morphology characterization
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) come 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 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 is for improving its visible region transmitance and good infrared sensitive characteristic, realizes hydrophilic and the multifunction such as photochemical catalysis, 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 nano compound film sample metal-insulator phase transition;
Fig. 3 VO 2/ SiO 2The transmittance figure at 2500nm place, nano compound film sample metal-insulator phase transition front and back.
Embodiment
The below introduces embodiments of the invention, and to understanding of the present invention, but the present invention is limited to absolutely not embodiment with further increase.
Embodiment 1:
Use V 2O 5Powder, phenylcarbinol and Virahol stirred 2 hours under 80 ℃ of conditions with the mixed in molar ratio of 1: 4: 50, 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 2In/Ar mixed atmosphere (hydrogen volume content 4%), reduction is 3 hours, can form the VO of crystallization after 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, then dry 10min can obtain required VO under 100 ℃ 2/ SiO 2Nano compound film.
That Fig. 1 is corresponding is VO 2/ SiO 2The surface topography SEM figure of nano compound film, substrate/VO 2, VO 2/ SiO 2And SiO 2Exist obvious boundary between/air, use in the drawings black dotted lines in order to sign, SiO 2Granular size is 20-50nm, VO 2Particle size distribution is 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, along with the temperature fast-descending, 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 rapidly again transparently, 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 13% left and right, and at infrared band, has also improved the transmitance (solid line in Fig. 2) of light, has improved the thermochromic 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 the mixed in molar ratio of 1: 4: 50, by spin coating coating technique (speed is 3000r/min), and preparation VO xFilm (2.0＜x＜2.5) is then at 410 ℃, H 2In/Ar mixed atmosphere (hydrogen volume content 4%), reduction is 3 hours, can form the VO of crystallization after 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, then dry 10min can obtain required VO under 100 ℃ 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 the mixed in molar ratio of 1: 4: 50; 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, then under the stirring at room condition, obtain VO 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 2In/Ar mixed atmosphere (hydrogen volume content 4%), reduction is 3 hours, can form the VO of crystallization after 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 the mixed in molar ratio of 1: 4: 50, by lifting coating technique (speed is 50mm/min), preparation VO xFilm (2.0＜x＜2.5) is then at 410 ℃, H 2In/Ar mixed atmosphere (hydrogen volume content 4%), reduction is 3 hours, can form the VO of crystallization after naturally cooling 2Film.By sol-gel technique, the 8.23g zinc acetate is added forerunner's colloidal sol of making ZnO in the solution of 50ml thanomin (1.9g) and ethylene glycol monomethyl ether; By lifting coating technique (speed is 50mm/min), preparation VO 2/ ZnO nano laminated film, then dry 10min can obtain required VO under 100 ℃ 2/ ZnO nano laminated film.
Prepared VO 2The surface topography SEM figure of/ZnO nano laminated 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 the mixed in molar ratio of 1: 4: 50; Simultaneously by sol-gel technique, the 8.23g zinc acetate is added forerunner's colloidal sol of making ZnO in the solution of 50ml thanomin (1.9g) and ethylene glycol monomethyl ether, then under the stirring at room condition, obtain VO 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 laminated film is then at 410 ℃, H 2In/Ar mixed atmosphere (hydrogen volume content 4%), reduction is 3 hours, can form the VO of crystallization after naturally cooling 2-ZnO nano laminated 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 the mixed in molar ratio of 1: 4: 50, by lifting coating technique (speed is 50mm/min), preparation VO xFilm (2.0＜x＜2.5) is then at 410 ℃, H 2In/Ar mixed atmosphere (hydrogen volume content 6%), reduction is 3 hours, can form the VO of crystallization after naturally cooling 2Film.By sol-gel technique, with 0.25molL -1ZrOCl 28H 2O prepares ZrO by the Hydrothermal Synthesis approach 2Forerunner's colloidal sol; By lifting coating technique (speed is 50mm/min), preparation VO 2Nano compound film, then dry 10min can obtain required VO under 100 ℃ 2/ ZrO 2Nano compound film.
Prepared VO 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 the mixed in molar ratio of 1: 4: 50; Simultaneously by sol-gel technique, with 0.25mol L -1ZrOCl 28H 2O prepares ZrO by the Hydrothermal Synthesis approach 2Forerunner's colloidal sol, then under the stirring at room condition, obtain VO 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 2In/Ar mixed atmosphere (hydrogen volume content 4%), reduction is 3 hours, can form the VO of crystallization after 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 the mixed in molar ratio of 1: 4: 50, by lifting coating technique (speed is 50mm/min), preparation VO xFilm (2.0＜x＜2.5) is then at 410 ℃, H 2In/Ar mixed atmosphere (hydrogen volume content 4%), reduction is 3 hours, can form the VO of crystallization after 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, then dry 10min can obtain required VO under 100 ℃ 2/ TiO 2Nano compound film.
Prepared VO 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 the mixed in molar ratio of 1: 4: 50; 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, then under the stirring at room condition, obtain VO 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 2In/Ar mixed atmosphere (hydrogen volume content 4%), reduction is 3 hours, can form the VO of crystallization after naturally cooling 2-TiO 2Nano compound film.All the other are with embodiment 1.

Claims (4)

1. the method for a laminated film, described nano compound film is VO 2/ SiO 2, VO 2/ ZnO, VO 2/ ZrO 2Or VO 2/ TiO 2, it is characterized in that with V 2O 5Powder is presoma, by the standby 2.0＜x of wet chemical solution legal system＜2.5VO 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 2Thin film technology: use V 2O 5Powder, phenylcarbinol and Virahol stir under 80 ℃ of oil bath conditions with the mixed in molar ratio of 1: 4: 50, 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 mixed atmosphere, can form the VO of pure phase after 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) is prepared with 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, then prepare complex thin film structure by lifting coating technique or spin coating coating technique; Be placed at last baking oven, under 100 ℃ of conditions, dry 5-30min can obtain required nano combined multi-function membrane.
2. by preparation method claimed in claim 1, it is characterized in that the substrate of selecting is that substrate is the substrate that does not contain Na simple glass, silica glass, sapphire or contain the Rutile Type structure.
3. by preparation method claimed in claim 2, it is characterized in that: when 1. making the precursor aqueous solution that contains vanadium in step 1, churning time is 2-5 hour; 2. H in step 1 2In/Ar mixed atmosphere, the hydrogen volume percentage composition is 4%-6%; 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.
4. by preparation method claimed in claim 2, 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.
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