CN103979607A - Vanadium oxide nanopillar array with thermochromism and preparation method thereof - Google Patents
Vanadium oxide nanopillar array with thermochromism and preparation method thereof Download PDFInfo
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Abstract
The invention provides a vanadium oxide nanopillar array with thermochromism and a preparation method thereof. The nano-array is a core-shell structure, wherein the core is an oxide A, a second layer is a VO2 layer with thermochromism and a third layer is air or an oxide B so as to form a structure of oxide A/VO2/air or oxide A/VO2/oxide B. According to the preparation method, a transparent oxide nanopillar array is prepared by a physical or chemical method to be used as a template; and then a vanadium-containing solution is adhered and heat treatment or hydrothermal reaction is carried out to obtain a vanadium dioxide nanopillar array, or a layer of oxide shell is deposited on the array so as to form the vanadium dioxide sandwich nanopillar array with thermochromism. Due to adjustment of porosity and matching of refractive index, visible light transmittance and solar adjustment rate of a whole vanadium dioxide film can be raised. Thus, the nanopillar array provided by the invention can be better applied in the field of thermochromatic intelligent window.
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 treatment consists technology and wet-chemical treatment technology, belong to energy-conserving and environment-protective field of new.
Background technology
The optics that nano material is unique because meeting produces, electricity and magnetic performance, be subject to people's favor.One-dimensional nano-array is because of its regular nanostructure, and electric transmission effect fast, is improving 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 isomrs, as A, and B, C, the phases such as M/R.Wherein, M/R has reversible thermal induced phase transition process near 68 degree, because being favored 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, to obtain the C phase VO perpendicular to substrate
2nano-array, the ability (ACS Nano, 2008,2,1492-1496) that it has good ultraviolet catalytic performance and produces 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 the VO that thickness is 20um on vanadium paper tinsel by anodised method
2porous-film, has the performance (Adv.Mater.2012,24,1571-1575) of good phase transformation, but because the Thickness Ratio of film is 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 the technology preparation of a gentleer easy row to be applicable to the VO of smart window
2nano-array is the key of 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 large (specific refractory power is greater than 3.0) of refractive index ratio, 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 the problem that prior art exists, the present invention utilizes ripe transparent oxide (specific refractory power is less than 2.5) nano-array as template, and VO grows on oxide compound A array
2shell, the VO obtaining like this
2the complex refractive index of the film that nano-pillar forms is reduced, and its visible light transmissivity can be improved.In addition, for 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 VO that therefore prepared by 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, it is characterized in that this nano-array is nucleocapsid structure, and wherein kernel is oxide compound A, and the second layer is the VO with thermocolour function
2layer, the 3rd layer is air or oxide compound B, forms oxide compound AVO
2air or oxide compound AVO
2oxide compound B structure.
The described VO with thermocolour function
2(M/R) nano-array is perpendicular to substrate, and the diameter of the cylinder of oxide compound A and spacing 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, Nb, Mo, Ti, Sn, Mg, at least one in F, 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 are selected from titanium oxide, silicon oxide, zirconium white, zinc oxide, stannic oxide, cerium oxide.
The preparation providing 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 preparing transparent oxide taking physics or chemical method is as template, postadhesion is heat-treated containing the solution of vanadium again or hydro-thermal reaction obtains the nano column array of vanadium dioxide, or deposit again the shell of one deck oxide compound thereon, form the nano column array of the vanadium dioxide sandwich with thermocolour performance.
When final product structure is oxide compound AVO
2when air, step is as follows:
(1) in substrate, prepare the nano column array of oxide compound A with hydrothermal method or physical vaporous deposition;
(2) nano column array of (1) gained is put into the solution that contains vanadium pure or dopant ion, allow on nano-array vanadium ion in load, the nano column array of vanadium ion that obtained load;
(3) nano column array of (2) is carried out to vacuum or protective atmosphere thermal 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 AVO
2when 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 being enclosed with the nano column array of oxide compound B.
Extent of reaction is controlled by monitoring each layer thickness.
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, and titanium isopropylate, zirconium oxychloride, zinc acetate, tin chloride, 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.
Nano column array in the present invention, due to the adjusting of 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.The nano column array that the present invention is prepared, because size and the spacing of cylinder are adjustable, can produce the optical characteristics that non-nano array does not possess, and as optical anisotropy and angular selectivity etc., can improve significantly VO
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 and the luminous reflectance of layer can further reduce, therefore VO
2(M/R) visible light transmissivity of cylinder array and sun power regulation rate can be greatly improved, and the design of sandwich structure has improved again VO greatly
2(M/R) stability of nano column array, the VO that therefore prepared by this technology
2(M/R) film can improve visible light transmissivity and sun power regulation rate to realistic scale.
Brief description of the drawings
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
Further illustrate the present invention below in conjunction with specific embodiment.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.
Embodiment 1:
FTO conductive glass is put into the solution that contains 0.05M butyl (tetra) titanate, proceed to in teflon-lined stainless steel hydrothermal reaction kettle, 150 degree insulation 30 minutes, utilizing hydrothermal method preparative column diameter on FTO conductive glass is 90nm, intercolumniation is 10nm, post height is the vertical nano column array of the titanium oxide of 200nm, then TiOx nano post array is put into and is contained 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 insulation 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 of parcel, then VO
2(M) nano-pillar is put into the solution of 0.02M butyl (tetra) titanate, and after 150 degree hydro-thermal reactions, obtaining thickness is the titanium oxide parcel VO of 60nm
2the array of nano-pillar.
Embodiment 2:
Borosilicate glass are put into and contained 0.02MZn
2+solution in, proceed to in teflon-lined stainless steel cauldron, 80 degree insulation 10 minutes, utilize hydrothermal method on borosilicate glass, to prepare diameter for 50nm, spacing is 100nm, be highly the vertical nano column array of zinc oxide of 150nm, then zinc-oxide nano column array put into and contained 2at%Mg
2+the 0.01MVO (acac) of ion
2the aqueous solution in soak after 30 minutes, under vacuum condition, thermal treatment obtains the Mg that thickness is 20nm
2+ion doping VO
2(M) zinc-oxide nano column array of parcel, then VO
2(M) solution that nano-pillar is put into 0.05M tetraethoxy soaks after 10 minutes and takes out, and in retort furnace 300 degree, dries, and obtaining thickness is the silicon oxide-wrapped VO of 100nm
2(M) array of nano-pillar.
Embodiment 3:
It is 200nm that deposited by electron beam evaporation method is prepared diameter on sapphire, and spacing is 200nm, is highly the vertical nano-array of stannic oxide of 100nm, then the nano-pillar of stannic oxide is put into the 0.5M VOC that contains 1.5at%F-ion
2o
4the aqueous solution in, after hydro-thermal reaction, obtain thickness and be the M phase VO of the F-doping of 100nm
2(M) the tin oxide nano post array of parcel, then VO
2(M) solution that nano-pillar is put into 0.02M zinc acetate soaks after 20 minutes and takes out, and in retort furnace, dries, 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 vertical nano-array of cerium oxide of 200nm, then the nano-pillar of cerium oxide is put into and is contained 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 of parcel, then VO
2(R) nano-pillar is put into the solution of 0.02M titanium isopropylate, proceeds to in teflon-lined stainless steel cauldron, and 200 degree insulation 10 minutes, after hydro-thermal reaction, obtaining thickness was the titanium oxide parcel VO of 50nm
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 vertical nano-array of zirconium white of 200nm, then zirconic nano-pillar is put into and is contained 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 zirconium white nano column array of parcel, then VO
2(R) nano-pillar is put into the solution of 0.1M Cerium II Chloride, proceeds to in teflon-lined stainless steel cauldron, and 160 degree insulation 60 minutes, after hydro-thermal reaction, obtaining thickness was the cerium oxide parcel VO of 40nm
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 vertical nano-array of silicon oxide of 200nm, then the nano-pillar of silicon oxide is put into and is contained 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 of parcel, then VO
2(M) nano-pillar is put into the solution of 0.1M tin chloride, proceeds to in teflon-lined stainless steel cauldron, and 100 degree insulation 120 minutes, after hydro-thermal reaction, obtaining thickness was the stannic oxide parcel VO of 40nm
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 vertical nano-array of cerium oxide of 200nm, then the nano-pillar of cerium oxide is put into and is contained 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 of parcel, then VO
2(M) nano-pillar is put into the solution of 0.1M zirconium oxychloride, proceeds to in teflon-lined stainless steel cauldron, and 140 degree insulation 120 minutes, after hydro-thermal reaction, obtaining thickness was the zirconium white parcel VO of 80nm
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 vertical nano-array of silicon oxide of 200nm, then the nano-pillar of silicon oxide is put into and is contained 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 of parcel.
Embodiment 9:
On sheet mica, preparing diameter with thermal evaporation is 250nm, and spacing is 300nm, is highly the vertical nano-array of silicon oxide of 200nm, the 0.8M VO (the C then nano-pillar of silicon oxide being 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 of parcel.
Embodiment 10:
On sheet mica, preparing diameter with pulse laser deposition is 250nm, and spacing is 300nm, is highly the vertical nano-array of silicon oxide of 200nm, the 0.1M VO (the C then nano-pillar of silicon oxide being 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 of parcel.
Claims (8)
1. have the vanadium oxide nano column array of thermocolour performance, 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, the 3rd layer is air or oxide compound B, forms oxide compound AVO
2air or oxide compound AVO
2oxide compound B structure.
2. the vanadium oxide nano-array with thermocolour performance according to claim 1, it is characterized in that, the described vanadium oxide nano-array with thermocolour function is perpendicular to substrate, and the diameter of the cylinder of oxide compound A and spacing 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 vanadium oxide nano-array with thermocolour performance according to claim 1 and 2, 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 vanadium oxide nano-array with thermocolour performance according to claim 1, 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, Nb, Mo, Ti, Sn, Mg, at least one in F, the volumetric molar concentration of doped element is 0-2at%.
5. the vanadium oxide nano column array with thermocolour performance according to claim 1, is characterized in that, described oxide compound A or B are selected from titanium oxide or silicon oxide, zirconium white, zinc oxide, stannic oxide, cerium oxide.
6. a preparation method for the vanadium oxide nano column array described in any one in claim 1-4, is characterized in that,
When final product structure is oxide compound AVO
2when air, step is as follows:
(1) in substrate, prepare the nano column array of oxide compound A with hydrothermal method or physical vaporous deposition;
(2) nano column array of (1) gained is put into the solution that contains vanadium pure or dopant ion, allow on nano-array vanadium ion in load, the nano column array of vanadium ion that obtained load;
(3) nano column array of (2) is carried out to vacuum or protective atmosphere thermal 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 AVO
2when 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 being enclosed with the nano column array of oxide compound B.
7. the preparation method of vanadium oxide nano column array according to claim 5, is characterized in that the described vanadium solution that contains 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. the preparation method of vanadium oxide nano column array according to claim 5, is characterized in that described precursor solution 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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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104261471A (en) * | 2014-09-22 | 2015-01-07 | 常州大学 | Preparation method of nano-sized vanadium oxide with quantum size effect |
| CN104495928A (en) * | 2015-01-09 | 2015-04-08 | 中国科学院上海硅酸盐研究所 | Preparation method of vanadium dioxide/zinc oxide nano composite powder |
| CN104698511A (en) * | 2015-01-29 | 2015-06-10 | 南京理工大学 | Method for improving absorption rate of near infrared band of vanadium oxide film and prepared vanadium oxide film thereof |
| CN105502496A (en) * | 2015-12-30 | 2016-04-20 | 中国人民解放军国防科学技术大学 | Vanadium dioxide/zinc sulfide composite powder with core-shell structure and preparation method of composite powder |
| 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 |
| CN109437303A (en) * | 2018-12-10 | 2019-03-08 | 哈尔滨工业大学 | Based on VO2Thermochromism intelligence thermal suite of film and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261471A (en) * | 2014-09-22 | 2015-01-07 | 常州大学 | Preparation method of nano-sized vanadium oxide with quantum size effect |
| 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 |
| CN104495928A (en) * | 2015-01-09 | 2015-04-08 | 中国科学院上海硅酸盐研究所 | Preparation method of vanadium dioxide/zinc oxide nano composite powder |
| CN104698511A (en) * | 2015-01-29 | 2015-06-10 | 南京理工大学 | Method for improving absorption rate of near infrared band of vanadium oxide film and prepared vanadium oxide film thereof |
| 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 |
| CN105502496A (en) * | 2015-12-30 | 2016-04-20 | 中国人民解放军国防科学技术大学 | Vanadium dioxide/zinc sulfide composite powder with core-shell structure and preparation method of composite powder |
| 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 |
| CN109437303A (en) * | 2018-12-10 | 2019-03-08 | 哈尔滨工业大学 | Based on VO2Thermochromism intelligence thermal suite of film and preparation method thereof |
| 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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