CN103979607B - A kind of vanadium oxide nano column array with thermocolour performance and preparation method thereof - Google Patents
A kind of vanadium oxide nano column array with thermocolour performance and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of vanadium oxide nano column array with thermocolour performance and preparation method thereof.This nano-array is nucleocapsid structure, and wherein kernel is oxide compound A, and the second layer is the VO with thermocolour function
2layer, third layer is air or oxide compound B, forms oxide compound A@VO
2@air or oxide compound A@VO
2@oxide compound B structure.Preparation method of the present invention prepares the nano column array of transparent oxide for template with physics or chemical method, postadhesion is heat-treated containing the solution of vanadium again or hydro-thermal reaction obtains the nano column array of vanadium dioxide, or deposit the shell of one deck oxide compound more thereon, form the nano column array with the vanadium dioxide sandwich of thermocolour performance.The adjustment of nano column array in the present invention due to porosity and the coupling of specific refractory power, can improve overall visible light transmissivity and the sun power regulation rate of vanadium dioxide film, makes it better be applied to thermocolour smart window field.
Description
Technical field
The present invention relates to thermochromism vanadium oxide nano column array in energy-saving material field and preparation method thereof, relate to hydrothermal technology and wet-chemical treatment technology, belong to energy-conserving and environment-protective field of new.
Background technology
Nano material is because producing unique optics, and electricity and magnetic performance, be subject to the favor of people.One-dimensional nano-array, because its regular nanostructure, fast electric transmission effect, at raising solar battery efficiency, strengthens the light extraction efficiency of LED, improves the aspects such as Chu Qing and is widely used.Vanadium dioxide is a kind of phase change material, has a lot of isomr, as phases such as A, B, C, M/R.Wherein, M/R phase has reversible thermal induced phase transition process near 68 degree, is favored because may be used for thermocolour smart window.But, at VO
2(M/R), in the preparation process of film, 0 peacekeeping 1 is tieed up structure and is all studied often, but is still blank out for the research of the nano-array perpendicular to substrate.The people such as Wang utilize the method for thermal evaporation on silicon chip, obtain C phase VO perpendicular to substrate
2nano-array, its ability (ACS Nano, 2008,2,1492-1496) that there is good ultraviolet catalytic performance and produce hydrogen.Patent CN102994951A points out can obtain difform VO by the inclined deposition technology in gas phase in thing
2nano-array, can improve VO
2the visible light transmissivity of film and sun power regulation rate, but be limited to the size of equipment, available VO
2the size of nano-array is very limited, and the film that the method obtains is non-crystalline state, needs follow-up thermal treatment to obtain having the VO of phase transition function
2film, this can cause caving in of nanostructure and degenerate.The people such as Yang have prepared by anodised method the VO that thickness is 20um on vanadium paper tinsel
2porous-film, has the performance (Adv.Mater.2012,24,1571-1575) of good phase transformation, but due to the Thickness Ratio of film comparatively large and prepare on vanadium paper tinsel, this film can not be used for smart window.In addition, in electrochemical method, owing to using the electrolytic solution with severe corrosive, toxicity and pollution level are all larger, therefore, find a gentleer easy technology preparation to be applicable to the VO of smart window
2nano-array is the key implementing this technology.
In addition, VO
2as smart window material, the not high and sun power regulation rate of visible light transmissivity is undesirable is that this material of restriction moves towards two practical large bottlenecks.This is mainly limited by its Intrinsic Gettering height and refractive index ratio comparatively large (specific refractory power is greater than 3.0), can produce strong surface reflection in visible region, therefore the structure of design refractive indices coupling is to reduce light refractive index and surface reflection has great importance.
Summary of the invention
The object of this invention is to provide a kind of vanadium oxide nano column array with thermocolour performance and preparation method thereof.
In the face of prior art Problems existing, the present invention utilizes ripe transparent oxide (specific refractory power is less than 2.5) nano-array as template, and oxide compound A array grows VO
2shell, the VO obtained like this
2the complex refractive index of the film that nano-pillar is formed is reduced, and its visible light transmissivity can be improved.In addition, in order to VO
2layer is protected, and can deposit one deck oxide compound B again, forms the nano-pillar with sandwich structure, so not only can improve transmitance and the sun power regulation rate of visible ray, can also improve VO
2the stability of nano column array, the therefore VO for preparing of this technology
2(M/R) nano-array is expected to be applied to thermocolour smart window field.
The present invention has the vanadium oxide nano column array of thermocolour performance, and it is characterized in that this nano-array is nucleocapsid structure, wherein kernel is oxide compound A, and the second layer is the VO with thermocolour function
2layer, third layer is air or oxide compound B, forms oxide compound A@VO
2@air or oxide compound A@VO
2@oxide compound B structure.
The described VO with thermocolour function
2(M/R) nano-array is perpendicular to substrate, and diameter and the spacing of the cylinder of oxide compound A are all less than 1um, and diameter is preferably 50-500nm, and spacing is preferably 10-500nm, and the height of cylinder is not more than 200nm, is preferably 100-200nm; VO
2the thickness of layer is not more than 100nm, is preferably 10-100nm; The thickness of oxide compound B layer is not more than 100nm, is preferably 0-100nm.
Preferably, the described VO with thermocolour function
2(M/R) nano-array be vanadium dioxide pure or doping M phase or R phase, the element of doping is selected from W, at least one in Nb, Mo, Ti, Sn, Mg, F, and the volumetric molar concentration of doped element is 0-2at%.
Preferably, the described VO with thermocolour function
2(M/R) the oxide compound A in nano-array vanadium oxide nano column array or oxide compound B is selected from titanium oxide, silicon oxide, zirconium white, zinc oxide, stannic oxide, cerium oxide.
The preparation provided in the present invention has the vanadium oxide nano column array [VO of thermocolour performance
2(M/R) nano column array] method, the nano column array of transparent oxide is prepared for template with physics or chemical method, postadhesion is heat-treated containing the solution of vanadium again or hydro-thermal reaction obtains the nano column array of vanadium dioxide, or deposit the shell of one deck oxide compound more thereon, form the nano column array with the vanadium dioxide sandwich of thermocolour performance.
When final product structure is oxide compound A@VO
2during@air, step is as follows:
(1) in substrate, the nano column array of oxide compound A is prepared with hydrothermal method or physical vaporous deposition;
(2) nano column array of (1) gained is put into the solution of the vanadium containing pure or dopant ion, to allow on nano-array vanadium ion in load, obtain the nano column array of load vanadium ion;
(3) nano column array of (2) is carried out vacuum or N2shielded heat-treatment, or put into reactor and carry out hydro-thermal reaction, obtain VO
2the nano column array of parcel oxide compound A;
When final product structure is oxide compound A@VO
2during@oxide compound B structure, also comprise the steps:
(4) nano-pillar in (3) is put into the precursor solution of oxide compound B, retort furnace thermal treatment or hydro-thermal reaction obtain the nano column array being enclosed with oxide compound B.
Extent of reaction is by monitoring each layer thickness to control.
Described is selected from VOSO containing vanadium solution
4the aqueous solution, VO (acac)
2methanol solution, VOC
2o
4the aqueous solution, NH
4vO
3the aqueous solution or VO (C
3h
7)
3aqueous isopropanol in one, concentration is not more than 1M.
Described precursor solution is selected from tetraethoxy, butyl (tetra) titanate, titanium isopropylate, zirconium oxychloride, zinc acetate, tin chloride, and the one in Cerium II Chloride, concentration is not more than 0.1M.
Described substrate is selected from silica glass, borosilicate glass, transparent conducting glass, sapphire, the one in sheet mica.
The adjustment of nano column array in the present invention due to porosity and the coupling of specific refractory power, can improve overall visible light transmissivity and the sun power regulation rate of vanadium dioxide film, makes it better be applied to thermocolour smart window field.Nano column array prepared by the present invention, due to the size of cylinder and spacing adjustable, the optical characteristics that non-nano array does not possess can be produced, as optical anisotropy and angular selectivity etc., VO can be improved significantly
2(M/R) visible light transmissivity of film and sun power regulation rate, be aided with the design of nucleocapsid structure, VO
2(M/R) specific refractory power of layer and luminous reflectance can reduce further, therefore VO
2(M/R) visible light transmissivity of pillar array and sun power regulation rate can be greatly improved, and the design of sandwich structure, greatly improve VO again
2(M/R) stability of nano column array, the therefore VO for preparing of this technology
2(M/R) film can improve visible light transmissivity and sun power regulation rate to realistic scale.
Accompanying drawing explanation
Fig. 1 is thermocolour nano array structure schematic diagram described in the invention.
Wherein, 1 is substrate, and 2 is oxide compound A or B, and 3 is VO
2(M/R), 4 is oxide compound B or A
Embodiment
The present invention is illustrated further below in conjunction with specific embodiment.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.
Embodiment 1:
FTO conductive glass is put into the solution containing 0.05M butyl (tetra) titanate, proceed to in teflon-lined stainless steel hydrothermal reaction kettle, 150 degree of insulations 30 minutes, hydrothermal method preparative column diameter on FTO conductive glass is utilized to be 90nm, intercolumniation is 10nm, post height is the titanium oxide vertical nanowires post array of 200nm, then TiOx nano post array is put into containing 1at%W
6+the 0.02M VOSO of ion
4the aqueous solution in, proceed to in teflon-lined stainless steel hydrothermal reaction kettle, 280 degree of insulations 3 hours, hydro-thermal reaction obtained the W that thickness is 50nm
6+the VO of ion doping
2(M) the TiOx nano post array wrapped up, then VO
2(M) nano-pillar puts into the solution of 0.02M butyl (tetra) titanate, obtains the titanium oxide parcel VO that thickness is 60nm after 150 degree of hydro-thermal reactions
2the array of nano-pillar.
Embodiment 2:
Borosilicate glass are put into containing 0.02MZn
2+solution in, proceed to in teflon-lined stainless steel cauldron, 80 degree of insulations 10 minutes, hydrothermal method is utilized to prepare diameter on borosilicate glass for 50nm, spacing is 100nm, be highly the zinc oxide vertical nanowires post array of 150nm, then zinc-oxide nano column array put into containing 2at%Mg
2+the 0.01MVO (acac) of ion
2the aqueous solution in soak after 30 minutes, thermal treatment obtains the Mg that thickness is 20nm under vacuum
2+ion doping VO
2(M) zinc-oxide nano column array wrapped up, then VO
2(M) nano-pillar puts into solution immersion taking-up after 10 minutes of 0.05M tetraethoxy, dries, obtain the silicon oxide-wrapped VO that thickness is 100nm in retort furnace 300 degree
2(M) array of nano-pillar.
Embodiment 3:
It is 200nm that deposited by electron beam evaporation method prepares diameter on sapphire, and spacing is 200nm, is highly the stannic oxide vertical nanowires array of 100nm, then the nano-pillar of stannic oxide is put into the 0.5M VOC containing 1.5at%F-ion
2o
4the aqueous solution in, obtain after hydro-thermal reaction thickness be 100nm F-doping M phase VO
2(M) the tin oxide nano post array wrapped up, then VO
2(M) nano-pillar puts into solution immersion taking-up after 20 minutes of 0.02M zinc acetate, dries in retort furnace, and obtaining thickness is 70nm zinc oxide parcel VO
2(M) array of nano-pillar.
Embodiment 4:
On sheet mica, preparing diameter with pulse laser deposition is 300nm, and spacing is 500nm, is highly the cerium oxide vertical nanowires array of 200nm, then the nano-pillar of cerium oxide is put into containing 1at%Mo
6+the 0.002M NH of ion
4vO
3the aqueous solution in soak after 30 minutes, then in reducing atmosphere, after thermal treatment, obtain the Mo that thickness is 10nm
6+the VO of ion doping
2(R) the cerium oxide nano post array wrapped up, then VO
2(R) nano-pillar puts into the solution of 0.02M titanium isopropylate, proceeds to in teflon-lined stainless steel cauldron, 200 degree of insulations 10 minutes, obtains the titanium oxide parcel VO that thickness is 50nm after hydro-thermal reaction
2(R) array of nano-pillar.
Embodiment 5:
On sheet mica, preparing diameter with laser pulse method is 500nm, and spacing is 300nm, is highly the zirconium white vertical nanowires array of 200nm, then zirconic nano-pillar is put into containing 0.5at%Nb
5+0.8M VO (the C of ion
3h
7)
3aqueous isopropanol in soak after 30 minutes, then in reducing atmosphere, after thermal treatment, obtain the VO that thickness is 80nm
2(R) the zirconia nanopowder post array wrapped up, then VO
2(R) nano-pillar puts into the solution of 0.1M Cerium II Chloride, proceeds to in teflon-lined stainless steel cauldron, 160 degree of insulations 60 minutes, obtains the cerium oxide parcel VO that thickness is 40nm after hydro-thermal reaction
2(M) array of nano-pillar.
Embodiment 6:
On sheet mica, preparing diameter with laser pulse method is 500nm, and spacing is 400nm, is highly the silicon oxide vertical nanowires array of 200nm, then the nano-pillar of silicon oxide is put into containing 0.5at%Sn
4+0.8M VO (the C of ion
3h
7)
3aqueous isopropanol in soak after 30 minutes, then in reducing atmosphere, after thermal treatment, obtain the VO that thickness is 80nm
2(M) the monox nanometer post array wrapped up, then VO
2(M) nano-pillar puts into the solution of 0.1M tin chloride, proceeds to in teflon-lined stainless steel cauldron, 100 degree of insulations 120 minutes, obtains the stannic oxide parcel VO that thickness is 40nm after hydro-thermal reaction
2(M) array of nano-pillar.
Embodiment 7:
On sheet mica, preparing diameter with laser pulse method is 500nm, and spacing is 300nm, is highly the cerium oxide vertical nanowires array of 200nm, then the nano-pillar of cerium oxide is put into containing 2at%Ti
4+0.8M VO (the C of ion
3h
7)
3aqueous isopropanol in soak after 30 minutes, then in reducing atmosphere, after thermal treatment, obtain the VO that thickness is 80nm
2(M) the cerium oxide nano post array wrapped up, then VO
2(M) nano-pillar puts into the solution of 0.1M zirconium oxychloride, proceeds to in teflon-lined stainless steel cauldron, 140 degree of insulations 120 minutes, obtains the zirconium white parcel VO that thickness is 80nm after hydro-thermal reaction
2(M) array of nano-pillar.
Embodiment 8:
On sheet mica, preparing diameter with thermal evaporation is 200nm, and spacing is 50nm, is highly the silicon oxide vertical nanowires array of 200nm, then the nano-pillar of silicon oxide is put into containing 2at%Ti
4+0.8M VO (the C of ion
3h
7)
3aqueous isopropanol in soak after 30 minutes, then in reducing atmosphere, after thermal treatment, obtain the VO that thickness is 80nm
2(M) the monox nanometer post array wrapped up.
Embodiment 9:
On sheet mica, preparing diameter with thermal evaporation is 250nm, and spacing is 300nm, is highly the silicon oxide vertical nanowires array of 200nm, then the 0.8M VO (C that the nano-pillar of silicon oxide is put into
3h
7)
3aqueous isopropanol in soak after 30 minutes, then in reducing atmosphere, after thermal treatment, obtain the VO that thickness is 80nm
2(M) the monox nanometer post array wrapped up.
Embodiment 10:
On sheet mica, preparing diameter with pulse laser deposition is 250nm, and spacing is 300nm, is highly the silicon oxide vertical nanowires array of 200nm, then the 0.1M VO (C that the nano-pillar of silicon oxide is put into
3h
7)
3aqueous isopropanol in soak after 30 minutes, then in reducing atmosphere, after thermal treatment, obtain the VO that thickness is 10nm
2(R) the monox nanometer post array wrapped up.
Claims (8)
1. there is the VO of thermocolour performance
2nano column array, it is characterized in that this nano-array is nucleocapsid structure, wherein kernel is oxide compound A, and the second layer is the VO with thermocolour function
2layer, third layer is air or oxide compound B, forms oxide compound A@VO
2@air or oxide compound A@VO
2@oxide compound B structure.
2. the VO with thermocolour performance according to claim 1
2nano column array, is characterized in that, the described vanadium oxide nano-array with thermocolour function is perpendicular to substrate, and diameter and the spacing of the cylinder of oxide compound A are all less than 1um, and the height of cylinder is not more than 200nm; VO
2the thickness of layer is not more than 100nm; The thickness of oxide compound B layer is not more than 100nm.
3. the VO with thermocolour performance according to claim 1 and 2
2nano column array, is characterized in that, the column diameter of described oxide compound A is 50-500nm, and spacing is 10-500nm, is highly 100-200nm; VO
2the thickness of layer is 10-100nm; Oxide compound B layer is 0-100nm.
4. the VO with thermocolour performance according to claim 1
2nano column array, is characterized in that, described in there is the VO of thermocolour function
2layer, for vanadium dioxide pure or doping M phase or R phase, the element of doping is selected from W, at least one in Nb, Mo, Ti, Sn, Mg, F, and the volumetric molar concentration of doped element is 0-2at%.
5. the VO with thermocolour performance according to claim 1
2nano column array, is characterized in that, described oxide compound A or B is selected from titanium oxide or silicon oxide, zirconium white, zinc oxide, stannic oxide, cerium oxide.
6. the VO according to any one of a claim 1-4
2the preparation method of nano column array, is characterized in that,
When final product structure is oxide compound A@VO
2during@air, step is as follows:
(1) in substrate, the nano column array of oxide compound A is prepared with hydrothermal method or physical vaporous deposition;
(2) nano column array of (1) gained is put into the solution of the vanadium containing pure or dopant ion, to allow on nano-array vanadium ion in load, obtain the nano column array of load vanadium ion;
(3) nano column array of (2) is carried out vacuum or N2shielded heat-treatment, or put into reactor and carry out hydro-thermal reaction, obtain VO
2the nano column array of parcel oxide compound A;
When final product structure is oxide compound A@VO
2during@oxide compound B structure, also comprise the steps:
(4) nano-pillar in (3) is put into the precursor solution of oxide compound B, retort furnace thermal treatment or hydro-thermal reaction obtain the nano column array being enclosed with oxide compound B.
7. VO according to claim 6
2the preparation method of nano column array, is characterized in that the solution of the described vanadium containing pure or dopant ion is selected from VOSO
4the aqueous solution, VO (acac)
2methanol solution, VOC
2o
4the aqueous solution, NH
4vO
3the aqueous solution or VO (C
3h
7)
3aqueous isopropanol in one, concentration is less than 1M.
8. VO according to claim 6
2the preparation method of nano column array, it is characterized in that the precursor solution of described oxide compound B is selected from tetraethoxy, butyl (tetra) titanate, titanium isopropylate, zirconium oxychloride, zinc acetate, tin chloride, the one in Cerium II Chloride, concentration is not more than 0.1M.
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| CN104261471B (en) * | 2014-09-22 | 2016-08-24 | 常州大学 | There is the preparation method of the nanoscale vanadium of quantum size effect |
| CN104495928B (en) * | 2015-01-09 | 2016-05-18 | 中国科学院上海硅酸盐研究所 | A kind of preparation method of vanadium dioxide/zinc-oxide nano composite granule |
| CN104698511B (en) * | 2015-01-29 | 2016-09-21 | 南京理工大学 | Increase the method for vanadium oxide film near infrared band absorbance and vanadium oxide film prepared therefrom |
| CN105502496B (en) * | 2015-12-30 | 2017-03-15 | 中国人民解放军国防科学技术大学 | A kind of core shell structure vanadium dioxide/zinc sulphide composite granule and preparation method thereof |
| CN108198878A (en) * | 2016-12-08 | 2018-06-22 | 南京理工大学 | Promote the square blanket periodic structure of vanadium dioxide light absorption enhancing |
| CN109437303B (en) * | 2018-12-10 | 2020-11-13 | 哈尔滨工业大学 | VO-based2Preparation method of thermochromic intelligent thermal control device of thin film |
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| CN1522965A (en) * | 2003-09-12 | 2004-08-25 | 武汉理工大学 | Vanadium dioxide nanometer rod and preparation method thereof |
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