CN103978203B - A kind of spectrum local decorated thermocolour composite nano-powder and preparation method thereof - Google Patents
A kind of spectrum local decorated thermocolour composite nano-powder and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of spectrum local decorated thermocolour composite nano-powder and preparation method thereof. This powder body is by VO2The MULTILAYER COMPOSITE nucleocapsid structure of layer, layer of precious metal, transparent oxide layer composition, wherein VO2Layer is as stratum nucleare, and layer of precious metal and transparent oxide layer lay respectively at the second layer or third layer. The present invention by being coated with layer of precious metal and transparent oxide layer at vanadium dioxide nano particle surface, it is possible not only to improve the stability of vanadium dioxide nano granule, the spectral characteristic of vanadium dioxide nano powder can also be regulated, regulate its transmitted colour and reflected colour, to reach to improve the purpose of its hypovanadic oxide powder color. This powder body can be widely used for the field such as heat insulating coat and pad pasting, can be applicable to intelligent energy-saving coating, it is also possible to for the heat insulation occasion such as glass and exterior wall.
Description
Technical field
The present invention relates to thermochromic function composite nano powder in chemical field and Material Field and preparation method thereof.
Technical background
In China, building energy consumption accounts for about the 30% of society's total energy consumption, and wherein the energy consumption of heating and air-conditioning accounts for the 55% of building energy consumption. In modern architecture, the area ratio that glass accounts for exterior wall is increasing, is delivered in winter and summer according to measuring and calculating by the heat that windowpane carries out and accounts for 48% and 71% respectively. Regulating indoor temperature according to air-conditioning, cryogenic temperature improves 2 degree, and cooling load reduces about 20%; Heating temperature and turn down 2 degree, heating load reduces about 30%, energy consumption can be greatly decreased by pasting thermal isolation film or coating heat insulating coat on glass.
Vanadium dioxide is the material that reversible transition can occur, before and after phase transformation, and its optical property generation significant change. When temperature is higher than phase transition temperature, vanadium dioxide is the R phase of metallic state, it is possible to stopping the infrared ray in the sun, when temperature is lower than phase transition temperature, vanadium dioxide is the M phase of semiconductor form, it is possible to allow sunlight is unobstructed to be passed through.Therefore, the temperature switch effect of vanadium dioxide is utilized, it is possible to the Energy Saving Windows port system of preparation intelligence completely.
At present, preparation Thermochromic smart window glass mainly has two kinds, and one is to adopt magnetron sputtering to prepare VO2Thin film, another kind is to adopt chemosynthesis VO2Nano-powder, then powder body is made coating, it is coated on glass surface or transparent plastic, obtains glass or the pad pasting with energy-saving effect. Optical computing (J.Appl.Phys., 2010,108; 063525) show; if vanadium dioxide nano powder can be scattered in other residuites, can retain on the basis of vanadium dioxide optics performance of control, improve visible light transmissivity to realistic scale; thin film prepared by the method; method is simple, it is simple to scale, not only existing windowpane can be carried out reducing energy consumption; can also be coated on various substrates, expand the application of vanadium dioxide film. But, owing to the vanadium dioxide absorption in visible region is relatively larger, presents khaki, not easily received by people, therefore, improve vanadium dioxide color in use and there is important practical value. Thin film for sputtering sedimentation, patent CN101269918B discloses and utilizes multi-layer film structure to design, improve the reflection of vanadium dioxide film and the method for transmitted spectrum, but owing to the design of multilayer film is the modification of full spectrum, while improving visible region spectrum, also other wave band can be produced impact, and complex procedures, the cost of thin film can be improved greatly. Patent CN101205120BG discloses the noble metal nano particles spectrum local decorated characteristic to the vanadium dioxide film of sputtering sedimentation, utilize noble metal at the visible local plasmon resonance absworption peak to infrared band, it is possible to spectrum to be carried out local decorated and do not affect the characteristic of other spectral regions. But, the modification of the thin film spectrum for being formed by hypovanadic oxide powder, it is still blank out so far.
Summary of the invention
The present invention is by carrying out local Spectral modification to vanadium dioxide nano powder surface, from realizing thin film spectrum local decorated that hypovanadic oxide powder is formed, with the purpose of this transmitted colour reaching to improve thin film and reflected colour.
Adopt the method that hypovanadic oxide powder and other residuite compound prepare thin film; there is cost low, it is easy to the feature of large-scale, can be not only used for the transformation of the energy-saving of original windowpane; and can be coated on various substrates, expand the application of vanadium dioxide. But Intrinsic Gettering and the high refractive index due to vanadium dioxide, cause that the coating of the vanadium dioxide transmitance in visible region is relatively low, coating color is khaki, not popular, therefore, improve the visible light transmissivity of vanadium dioxide and the reflected colour of coating, there is critically important using value. Core innovative point of the present invention is to utilize modified with noble metals intelligence Vanadium dioxide composite powder, and the stability and non-oxidizability that improve hypovanadic oxide powder are also had good effect by the nucleocapsid structure by being formed simultaneously.
The present invention provides a kind of spectrum local decorated thermocolour composite nano-powder, by VO2The nucleocapsid structure of layer, layer of precious metal, transparent oxide layer composition, wherein VO2Layer is as stratum nucleare, and layer of precious metal and transparent oxide layer lay respectively at the second layer or third layer, it is preferred to transparent oxide is third layer.
Described VO2Layer is the vanadium dioxide nano powder of M/R phase, size minimum in its three-dimensional dimension is less than 100nm, preferably in three dimensions, size is not more than 100nm, and its shape can be subsphaeroidal, oval, flake, square block, polygon, cylindrical etc., phase transition temperature is adjustable at-20-70oC, it is preferred to 25-60oC is adjustable.
Described layer of precious metal is selected from gold, and silver, the one in copper, the thickness of layer of precious metal is not more than 50nm, it is contemplated that the layer of precious metal regulating effect to visible ray, is further preferably not greater than 20nm.
Described transparent oxide layer is selected from titanium oxide, silicon oxide, aluminium oxide, cerium oxide, stannum oxide, zinc oxide, zirconium oxide, niobium oxide, tantalum oxide, hafnium oxide, Scia, Indium sesquioxide., the one in yittrium oxide. The thickness of oxide skin(coating) is less than 1um, it is preferred to be not more than 100nm.
The preparation method that the present invention also provides for above-mentioned spectrum local decorated thermocolour composite nano powder, comprises the following steps:
(1) hypovanadic oxide powder is scattered in the disperse medium containing dispersing aid, obtains mixture A;
(2) in described mixture A, add the solution containing precious metal ion and reducing agent, after stirring, be obtained by reacting the vanadium dioxide nano powder having wrapped up noble metal;
(3) vanadium dioxide nano powder having wrapped up noble metal is added in the disperse medium containing dispersing aid, obtain mixture B;
(4) in mixture B, add the solution containing transparent oxide presoma, after reacted, obtain the hypovanadic oxide powder of cladding noble metal and transparent oxide successively.
That above operation obtains is VO2Layer is as stratum nucleare, and layer of precious metal is positioned at the second layer, and transparent oxide layer is positioned at the product of third layer.
Obtaining transparent oxide layer and be positioned at the second layer, layer of precious metal is positioned at the hypovanadic oxide powder of third layer, it is only necessary to operation (2) and (4) are exchanged.
Disperse medium in operation (1) or (3) is methanol, ethanol, isopropanol, ethyl acetate, butyl acetate, toluene, chloroform, dimethylformamide, dimethyl sulfoxide, dichloroethanes, the one in acetone. Wherein, the weight ratio of hypovanadic oxide powder and disperse medium is 1:1-1:1000, is more preferably 1:5-1:100.
The dispersing aid added in operation (1) or (3) can be polyvinyl alcohol, polyvinylpyrrolidone, organic silicon surfactant, the one in fluorine-containing surfactant. Operation (1) or (3) add the described dispersing aid of the 0.02-2 weight % of disperse medium.
Layer of precious metal is obtained by reacting by the solution containing precious metal ion and reducing agent, and metal ion solution is selected from gold chloride, and silver nitrate, the one in copper nitrate, reducing agent is preferably sodium borohydride.
Described oxide is obtained by transparent oxide presoma, and described transparent oxide presoma is selected from butyl titanate, isopropyl titanate, tetraethyl orthosilicate, methyl silicate, aluminum nitrate, cerium chloride, stannic chloride, zirconium oxychloride, zinc nitrate, zinc acetate, niobium chloride, tantalic chloride, hafnium chloride, indium chloride, the one in Yttrium chloride(Y2Cl6).
The present invention utilizes modified with noble metals intelligence Vanadium dioxide composite powder, vanadium dioxide nano powder surface is carried out local Spectral modification, from realizing thin film spectrum local decorated that hypovanadic oxide powder is formed, with the purpose of this transmitted colour reaching to improve thin film and reflected colour. In addition; owing to vanadium dioxide nano powder is prone to oxidation in malaria; thus affecting its performance and the service life of material can being shortened; therefore coating noble metal layer in vanadium dioxide nano powder surface can not only modify the spectral characteristic of vanadium dioxide, more can hypovanadic oxide powder be played a protective role. The present invention by being coated with layer of precious metal and transparent oxide layer at vanadium dioxide nano particle surface, it is possible not only to improve the stability of vanadium dioxide nano granule, the spectral characteristic of vanadium dioxide nano powder can also be regulated, regulate its transmitted colour and reflected colour, to reach to improve the purpose of its hypovanadic oxide powder color. This powder body can be widely used for the field such as heat insulating coat and pad pasting, can be applicable to intelligent energy-saving coating, it is also possible to for the heat insulation occasion such as glass and exterior wall.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the spectrum local decorated thermocolour composite nano-powder prepared by the present invention, and wherein figure a is 123 structures, and figure b is 132 structures.
Wherein 1 is VO2Layer, 2 is layer of precious metal, and 3 is transparent oxide layer.
Detailed description of the invention
The present invention is further illustrated below in conjunction with the drawings and specific embodiments.
The method of the present invention, including step: hypovanadic oxide powder is scattered in the disperse medium containing dispersing aid by (1), obtains mixture A; (2) in described mixture A, add the solution containing precious metal ion and reducing agent, after stirring, be obtained by reacting the vanadium dioxide nano powder having wrapped up noble metal; (3) vanadium dioxide nano powder having wrapped up noble metal is added in the disperse medium containing dispersing aid, obtain mixture B; (4) in mixture B, add the solution containing transparent oxide presoma, after reacted, obtain the hypovanadic oxide powder of cladding noble metal and transparent oxide successively. Obtain noble metal hypovanadic oxide powder on transparent oxide, it is only necessary to operation (2) and (4) are exchanged.
Specifically, high-speed stirred dispersion after the disperse medium elder generation ultrasonic disperse containing dispersing aid of hypovanadic oxide powder that weight percent content is 1-50% and 50-99% can be mixed to get mixture A, the solution containing precious metal ion and reducing agent is added afterwards in mixture A, under constant temperature 0-200 degree after stirring reaction, pass through centrifugation, obtain having wrapped up the vanadium dioxide nano powder of noble metal after 110 degree of lower vacuum dryings, then this powder body is joined in the disperse medium containing dispersing aid, obtain mixture B, mixture B adds the solution containing transparent oxide presoma, under constant temperature 0-200 degree after stirring reaction, pass through centrifugation, 110 degree of lower vacuum dryings obtain VO2Stratum nucleare has wrapped up the vanadium dioxide nano powder of noble metal and transparent oxide successively. To obtain VO2Stratum nucleare has wrapped up the vanadium dioxide nano powder of transparent oxide and noble metal successively, it is necessary to the order of mixture A and B is exchanged.
According to the thermocolour composite nano-powder that said method prepares, it is by VO2The MULTILAYER COMPOSITE nucleocapsid structure of layer, layer of precious metal, transparent oxide layer composition, wherein VO2Layer is as stratum nucleare, and layer of precious metal and transparent oxide layer lay respectively at the second layer or third layer. Described VO2Layer is the vanadium dioxide nano powder of M/R phase, and size minimum in its three-dimensional dimension is less than 100nm. Described layer of precious metal is selected from gold, and silver, the one in copper, the thickness of layer of precious metal is for being not more than 50nm. Extent of reaction controls to be completed by the thickness of each layer of monitoring.
Wherein, in the operation mixed with disperse medium by hypovanadic oxide powder, the weight ratio of hypovanadic oxide powder and disperse medium is 1:1-1:1000, it is preferred that for 1:5-1:100. When the weight ratio of hypovanadic oxide powder is too small, then hypovanadic oxide powder contacts weak effect with the presoma of wrappage, when the weight ratio of hypovanadic oxide powder is excessive, is unfavorable for the powder body fully dispersed and moistening in disperse medium, affects the covered effect in later stage.
In above-mentioned preparation section, dispersing aid used is polyvinyl alcohol, polyvinylpyrrolidone, organic silicon surfactant, dodecyl sodium sulfate, polyacrylic acid, silane coupler, one or more in titanate coupling agent or the dispersing aid known altogether in the industry. Dispersing aid is mainly used in reducing the surface tension of solution, improves the solvent moistening at powder surface, thus improving dispersion effect. The 0.02-2 weight % that addition is disperse medium of dispersing aid in operation (1) and (3);It is preferably 0.05-1 weight %.
Raw material, reagent that said method adopts can pass through to buy the synthesis of commercially available or traditional chemical transform mode and prepare. Unless otherwise defined or described herein, the same meaning that all specialties used herein are familiar with scientific words and those skilled in the art. Additionally, any similar with described content or that be equal to method and material all can be applicable in the inventive method. The other side of the present invention, due to this disclosure, will be appreciated that to those skilled in the art.
By the following examples the present invention is described in more details.
Embodiment 1
First is the VO of 80nm 2g particle diameter2(M) add in the 10g ethanol containing 0.02 weight % polyvinylpyrrolidone, stir 30min; Add the aqueous solution 50ml of the sodium borohydride of the aqueous solution 5ml and 1 weight % of 0.1 weight % silver nitrate, after stirring 5 hours, obtain Lycoperdon polymorphum Vitt suspension, by centrifugation after precipitation, vacuum drying, obtain the VO that Ag thickness is 10nm2The composite nano-powder of Ag; Then this powder body of 0.2g is distributed in the 1g ethanol containing 0.02 weight % polyvinylpyrrolidone, stirs 1 hour; Adjust pH value to 3, add 1ml tetraethyl orthosilicate, after stirring 120 minutes, dry 2 hours under 110 degree after centrifugation, obtain SiO2Thickness is the VO of 100nm2AgSiO2Powder body.
Embodiment 2
First 2g phase transition temperature be 60 degree, particle diameter be the VO of 40nm2(M) add in the 30g toluene containing 0.04% polyvinyl alcohol, stir 30min; Add the aqueous solution 50ml of the sodium borohydride of the aqueous solution 5ml and 2 weight % of 2 weight % silver nitrate, after stirring 5 hours, obtain Lycoperdon polymorphum Vitt suspension, by centrifugation after precipitation, vacuum drying, obtain the VO that Ag layer thickness is 2nm2The composite nano-powder of Ag; Then this powder body of 0.2g is distributed in the 3g chloroform containing 0.04 weight % polyvinyl alcohol, after stirring 1 hour, adjusts pH value to 3; Adding the saturated aqueous solution of 10ml zinc nitrate, after stirring 120 minutes, dry 2 hours after centrifugation under 110 degree, ZnO thickness is the VO of 50nm2The powder body of AgZnO.
Embodiment 3
First 2g phase transition temperature be 45 degree, particle diameter be the VO of 20nm2(R) add in the 50g dimethylformamide containing 1% organic silicon surfactant, after stirring 1 hour, adjust pH value to 3; Add the saturated aqueous solution of 10ml aluminum nitrate, after stirring 120 minutes, dry 2 hours under 110 degree after centrifugation, obtain Al2O3Layer thickness is the VO of 20nm2Al2O3Composite nano-powder; Then this powder body of 0.2g is distributed in the 5g dimethylformamide containing 0.04 weight % organic silicon surfactant and stirs 30min, add the aqueous solution 50ml of the sodium borohydride of the silver nitrate aqueous solution 5ml and 2 weight % of 10 weight %, after stirring 5 hours, obtain Lycoperdon polymorphum Vitt suspension, by centrifugation after precipitation, vacuum drying, obtains the VO that Ag layer thickness is 20nm2Al2O3The powder body of Ag.
Embodiment 4
First 2g phase transition temperature be 30 degree, the VO of particle diameter 50nm2(M) add in the 80g ethanol containing 1.2% dodecyl sodium sulfate, stirring 30min, add the aqueous solution 50ml of the sodium borohydride of the aqueous solution 5ml and 1 weight % of 0.2 weight % gold chloride, after stirring 5 hours, obtain Lycoperdon polymorphum Vitt suspension, by centrifugation after precipitation, vacuum drying, obtain the VO that Au layer thickness is 6nm2The composite nano-powder of Au, is then distributed to this powder body of 0.2g in the 1g isopropanol containing 1.2 weight % dodecyl sodium sulfates, after stirring 1 hour, adjust pH value to 3, add 0.2ml butyl titanate, after stirring 120 minutes, dry 2 hours under 110 degree after centrifugation, obtain TiO2Thickness is the VO of 100nm2AuTiO2Powder body.
Embodiment 5
First 2g phase transition temperature be 25 degree, the VO of particle diameter 30nm2(M) add in the 100g dichloroethanes containing 1% polyvinylpyrrolidone, stirring 30min, add the aqueous solution 50ml of the sodium borohydride of the aqueous solution 5ml and 1 weight % of 4 weight % copper nitrates, after stirring 5 hours, obtain Lycoperdon polymorphum Vitt suspension, by centrifugation after precipitation, vacuum drying, obtain the VO of Cu layer thickness 2nm2The composite nano-powder of Cu, is then distributed to this powder body of 0.2g in the 1g acetone containing 1 weight % polyvinylpyrrolidone, after stirring 1 hour, adjust pH value to 3, add the saturated aqueous solution of 2ml zirconium oxychloride, after stirring 120 minutes, dry 2 hours under 110 degree after centrifugation, obtain ZrO2Thickness is the VO of 30nm2CuZrO2Powder body.
Embodiment 6
First 2g phase transition temperature be 25 degree, particle diameter be the VO of 100nm2(R) join in the 200g ethanol containing 1 weight % polyvinylpyrrolidone, stirring 30min, add the aqueous solution 50ml of the sodium borohydride of the aqueous solution 5ml and 1 weight % of 2 weight % copper nitrates, after stirring 5 hours, obtain Lycoperdon polymorphum Vitt suspension, by centrifugation after precipitation, vacuum drying, obtain having wrapped up VO2The composite nano-powder of Cu, is then distributed to this powder body of 0.2g in the 20g ethanol containing 1 weight % polyvinylpyrrolidone, after stirring 1 hour, adjust pH value to 3, add the saturated aqueous solution of 1ml stannic chloride, after stirring 120 minutes, dry 2 hours under 110 degree after centrifugation, obtain SnO2Thickness is the VO of 20nm2CuSnO2Powder body.
Embodiment 7
First 2g phase transition temperature be 60 degree, particle diameter be the VO of 80nm2(M) add in the 30g acetone containing 0.04% fluorine-containing surfactant, stirring 30min, add the aqueous solution 50ml of the sodium borohydride of the aqueous solution 5ml and 2 weight % of 2 weight % silver nitrate, after stirring 5 hours, obtain Lycoperdon polymorphum Vitt suspension, by centrifugation after precipitation, vacuum drying, obtain the VO that Ag layer thickness is 8nm2The composite nano-powder of Ag, then this powder body of 0.2g is distributed in the 3g dimethyl sulfoxide containing 0.04 weight % fluorine-containing surfactant, after stirring 1 hour, adjust pH value to 3, add the saturated alcoholic solution of 2ml niobium chloride, after stirring 120 minutes, dry 2 hours under 110 degree after centrifugation, obtain Nb2O5Thickness is the VO of 30nm2AgNb2O5Powder body.
Embodiment 8
First 2g phase transition temperature be 60 degree, particle diameter be the VO of 50nm2(M) add in the 80g dimethyl sulfoxide containing 1.5% fluorine-containing surfactant, after stirring 30min, adjust pH value to 3, add the saturated acetone soln of 0.2ml cerium chloride, after stirring 120 minutes, dry 2 hours under 110 degree after centrifugation, obtain CeO2Thickness is the VO of 10nm2CeO2Powder body. Then this powder body of 0.2g is added in the 8g chloroform containing 1.5 weight % fluorine-containing surfactants, dispersion stirring 30min, add the aqueous solution 50ml of the sodium borohydride of the aqueous solution 5ml and 2 weight % of 2 weight % copper nitrates, after stirring 5 hours, obtain Lycoperdon polymorphum Vitt suspension, by centrifugation after precipitation, vacuum drying, obtain the VO that Cu layer thickness is 4nm2CeO2The composite nano-powder of Cu.
Embodiment 9
First 2g phase transition temperature be 40 degree, particle diameter be the VO of 20nm2(R) add in the 150g butyl acetate containing 2% fluorine-containing surfactant, stirring 30min, add the aqueous solution 50ml of the sodium borohydride of the aqueous solution 5ml and 2 weight % of 2 weight % silver nitrate, after stirring 5 hours, obtain Lycoperdon polymorphum Vitt suspension, by centrifugation after precipitation, vacuum drying, obtain the VO that Ag layer thickness is 8nm2The composite nano-powder of Ag, is then distributed to this powder body of 0.2g in the 15g dichloroethanes containing 2 weight % fluorine-containing surfactants, after stirring 1 hour, adjust pH value to 3, add the saturated alcoholic solution of 2ml indium chloride, after stirring 120 minutes, dry 2 hours under 110 degree after centrifugation, obtain In2O3Thickness is the VO of 40nm2AgIn2O3Powder body.
Embodiment 10
First 2g phase transition temperature be 60 degree, particle diameter be the VO of 80nm2(M) add in the 120g chloroform containing 0.06% fluorine-containing surfactant, stirring 30min, add the aqueous solution 50ml of the sodium borohydride of the aqueous solution 5ml and 2 weight % of 2 weight % silver nitrate, after stirring 5 hours, obtain Lycoperdon polymorphum Vitt suspension, by centrifugation after precipitation, vacuum drying, obtain the VO that Ag layer thickness is 8nm2The composite nano-powder of Ag, is then distributed to this powder body of 0.2g in the 12g toluene containing 0.06 weight % fluorine-containing surfactant, after stirring 1 hour, adjust pH value to 3, add the saturated alcoholic solution of 2ml tantalic chloride, after stirring 120 minutes, dry 2 hours under 110 degree after centrifugation, obtain Ta2O5Thickness is the VO of 30nm2AgTa2O5Powder body.
Embodiment 11
First 2g phase transition temperature be 60 degree, particle diameter be the VO of 70nm2(M) add in the 30g ethyl acetate containing 0.08% fluorine-containing surfactant, stirring 30min, add the aqueous solution 50ml of the sodium borohydride of the aqueous solution 5ml and 2 weight % of 2 weight % silver nitrate, after stirring 5 hours, obtain Lycoperdon polymorphum Vitt suspension, by centrifugation after precipitation, vacuum drying, obtain the VO that Ag layer thickness is 8nm2The composite nano-powder of Ag, then this powder body of 0.2g is distributed in the 3g butyl acetate containing 0.08 weight % fluorine-containing surfactant, after stirring 1 hour, adjust pH value to 3, add the saturated alcoholic solution of 2ml hafnium chloride, after stirring 120 minutes, dry 2 hours under 110 degree after centrifugation, obtain HfO2Thickness is the VO of 30nm2AgHfO2Powder body.
Embodiment 12
First 2g phase transition temperature be 60 degree, particle diameter be the VO of 80nm2(M) add in the 30g methanol containing 0.05% organic silicon surfactant, stirring 30min, add the aqueous solution 50ml of the sodium borohydride of the aqueous solution 5ml and 2 weight % of 2 weight % silver nitrate, after stirring 5 hours, obtain Lycoperdon polymorphum Vitt suspension, by centrifugation after precipitation, vacuum drying, obtain the VO that Ag layer thickness is 8nm2The composite nano-powder of Ag, then this powder body of 0.2g is distributed in the 3g ethyl acetate containing 0.05 weight % organic silicon surfactant, after stirring 1 hour, adjust pH value to 3, add the saturated aqueous solution of 2ml Scium chloride (Sc4Cl12), after stirring 120 minutes, dry 2 hours under 110 degree after centrifugation, obtain Sc2O3Thickness is the VO of 30nm2AgSc2O3Powder body.
Embodiment 13
First 2g phase transition temperature be 60 degree, particle diameter be the VO of 80nm2(R) add in the 30g isopropanol containing 0.08% polyvinyl alcohol, stirring 30min, add the aqueous solution 50ml of the sodium borohydride of the aqueous solution 5ml and 2 weight % of 2 weight % silver nitrate, after stirring 5 hours, obtain Lycoperdon polymorphum Vitt suspension, by centrifugation after precipitation, vacuum drying, obtain the VO that Ag layer thickness is 8nm2The composite nano-powder of Ag, is then distributed to this powder body of 0.2g in the 3g methanol containing 0.08 weight % polyvinyl alcohol, after stirring 1 hour, adjust pH value to 3, add the saturated aqueous solution of 2ml Yttrium chloride(Y2Cl6), after stirring 120 minutes, dry 2 hours under 110 degree after centrifugation, obtain Y2O3Thickness is the VO of 30nm2AgY2O3Powder body.
Claims (8)
1. thermocolour composite nano-powder one kind spectrum local decorated, it is characterised in that this powder body is by VO2The MULTILAYER COMPOSITE nucleocapsid structure of layer, layer of precious metal, transparent oxide layer composition, wherein VO2Layer is as stratum nucleare, and layer of precious metal and transparent oxide layer lay respectively at the second layer and third layer, or layer of precious metal and transparent oxide layer lay respectively at third layer and the second layer;Described layer of precious metal is selected from gold, and silver, the one in copper, the thickness of layer of precious metal is for being not more than 50nm.
2. spectrum local decorated thermocolour composite nano-powder according to claim 1, it is characterised in that described VO2Layer is the vanadium dioxide nano powder of M/R phase, and size minimum in its three-dimensional dimension is less than 100nm.
3. spectrum local decorated thermocolour composite nano-powder according to claim 1 and 2, it is characterised in that described transparent oxide is selected from titanium oxide, silicon oxide, aluminium oxide, cerium oxide, stannum oxide, zinc oxide, zirconium oxide, niobium oxide, tantalum oxide, hafnium oxide, Scia, Indium sesquioxide., the one in yittrium oxide, transparent oxide layer thickness is less than 1um.
4. the preparation method according to the described spectrum local decorated thermocolour composite nano-powder of claim 1 or 2, it is characterised in that comprise the following steps:
(1) hypovanadic oxide powder is scattered in the disperse medium containing dispersing aid, obtains mixture A;
(2) adding the solution containing precious metal ion and reducing agent in described mixture A, after stirring, be obtained by reacting the vanadium dioxide nano powder having wrapped up noble metal, the concentration of precious metal ion solution is 0.1-10 weight %;
(3) vanadium dioxide nano powder having wrapped up noble metal is added in the disperse medium containing dispersing aid, obtain mixture B;
(4) in mixture B, add the solution containing transparent oxide presoma, after agitated reaction, obtain the hypovanadic oxide powder of cladding noble metal and transparent oxide successively;
That above step obtains is VO2Layer is as stratum nucleare, and layer of precious metal is positioned at the second layer, and transparent oxide layer is positioned at the product of third layer;
Obtaining transparent oxide layer and be positioned at the second layer, layer of precious metal is positioned at the hypovanadic oxide powder of third layer, it is only necessary to step (2) and (4) are exchanged.
5. the preparation method of spectrum local decorated thermocolour composite nano-powder according to claim 4, it is characterised in that the disperse medium in operation (1) or (3) is selected from methanol, ethanol, isopropanol, ethyl acetate, butyl acetate, toluene, chloroform, dimethylformamide, dimethyl sulfoxide, the weight ratio of dichloroethanes, the one in acetone, hypovanadic oxide powder and disperse medium is 1:5-1:100.
6. the preparation method of spectrum local decorated thermocolour composite nano-powder according to claim 5, it is characterized in that, the dispersing aid added in operation (1) or (3) one in polyvinyl alcohol, polyvinylpyrrolidone, organic silicon surfactant, fluorine-containing surfactant, dodecyl sodium sulfate, the 0.02-2 weight % that addition is disperse medium of dispersing aid in operation (1) or (3).
7. the preparation method of spectrum local decorated thermocolour composite nano-powder according to claim 5, it is characterised in that the described solution containing precious metal ion is selected from gold chloride, silver nitrate, the one in copper nitrate.
8. the preparation method of spectrum local decorated thermocolour composite nano-powder according to claim 5, it is characterised in that described transparent oxide presoma is selected from butyl titanate, isopropyl titanate, tetraethyl orthosilicate, methyl silicate, aluminum nitrate, cerium chloride, stannic chloride, zirconium oxychloride, zinc nitrate, zinc acetate, niobium chloride, tantalic chloride, hafnium chloride, indium chloride, the one in Yttrium chloride(Y2Cl6).
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