CN108659812A - A kind of efficient thermochromism composite nano-powder of nucleocapsid and preparation method thereof - Google Patents
A kind of efficient thermochromism composite nano-powder of nucleocapsid and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of efficient thermochromism composite nano-powders of nucleocapsid, and the composite granule is with VO2Layer is stratum nucleare, and tungsten bronze compound layer is shell；The VO2Layer is vanadium dioxide nano powder, and minimum size is no more than 100nm in three-dimensional dimension, and the tungsten bronze compound layer is MxWO3, wherein M is selected from NH4+, Cs+, K+, Na+Or Li+Any one of；The value range of x is 0.01~0.8；The thickness of tungsten bronze compound layer is less than 60nm, and the infrared absorption characteristic using tungsten bronze material makes shell absorb heat, passes through closely coupled nucleocapsid flash heat transfer to stratum nucleare VO2Particle causes its heating to undergo phase transition, makes VO with this to reduce2Required environment temperature is undergone phase transition, VO is improved2Thermal response speed, shorten the phase transformation reaction time, achieve the effect that efficient thermochromism.
Description
Technical field：
The present invention relates to energy conservation and environmental protection field of new materials, and in particular to a kind of efficient thermochromism nanometer of nucleocapsid is multiple
Close powder and preparation method thereof.
Background technology：
With global non-renewable energy resources increasingly depleted and the continuous aggravation of traditional fossil energy pollution problem, new energy
Development and utilization have become the research hotspot and development trend of countries in the world.Solar energy is not only resourceful, inexhaustible use
It is inexhaustible, and be a kind of perfect clean energy resource to environment without any pollution.The most common Land use systems of solar energy are daylighting
Illumination, but we can also penetrate the heat of sunlight (near infrared band) while using sunlight (visible light wave range) daylighting
Amount.When summer temp is higher, it is therefore desirable to be able to stop that the heat of infrared region is got in reduce air conditioner load, winter temperature
It is indoor to need to take in more infrared region heats to warm oneself again when relatively low.Therefore, develop it is a kind of according to seasonal variations to sunlight
Regulation and control, intelligent and high-efficiency utilize solar energy, and the material with thermochromic function is particularly important.
Vanadium dioxide (VO2) it is a kind of most common thermochromic material, it is semiconductor under low-temperature condition, is to infrared region
It penetrates, is metal phase under the condition of high temperature, to the shielded effect of infrared region.VO2The phase transformation in high/low temperature after film is made
Cheng Zhong, visible region can keep higher transmitance.By VO2Applied on glass door and window, pass through the change of sense ambient temperature
Change, can intelligent control incident light transmission, reflection or absorption, at all seasons in make full use of sunlight, realize intelligent height
Effect utilizes the purpose of solar energy.Traditional VO2Thermochromism glass is prepared using Physical (magnetron sputtering etc.), but this
Kind method is of high cost, complex process, is difficult to realize large area production.Another kind is first to synthesize VO using chemical method2Nano-powder,
Again by nano-powder with macromolecule is compound is configured to slurry or mixed liquor, glass or plastic film can be coated uniformly on, obtained
Glass with thermochromic function or plastic foil, are finally applied on glass door and window.Compared with former approach, the latter has
It is of low cost, simple for process, easy the advantages such as to mass produce, be widely used.However, VO2Phase transition temperature it is high, thermal response is slow
The shortcomings of, its practical application is hindered significantly.Chinese patent CN102120615A discloses a kind of thermochromism vanadium dioxide material
The preparation method and application of material, Figure 12 can be seen that temperature-rise period phase transition temperature is up to 72 DEG C, significantly limit its reality
Using.Chinese patent CN102295312B, CN104030356B and CN104030355B can reduce by two by adulterating elements such as w
The phase transition temperature of vanadium oxide, but the crystallinity and latent heat of phase change of vanadium dioxide are reduced simultaneously, it is suppressed that its sunlight modulability
Can, cause its energy-saving efficiency to substantially reduce.And for raising VO2Thermal response characteristics, shorten the phase transformation response time, rarely have so far
Research.
Invention content：
The purpose of the present invention is be directed to existing VO2The problem of thermochromic material phase transition temperature height, thermal response difference, provides one
The efficient thermochromism composite nano-powder and preparation method thereof of kind nucleocapsid, the composite granule is with VO2For stratum nucleare, tungsten bronze
Compound is shell, using the infrared absorption characteristic of tungsten bronze, so that particle shell is absorbed heat, passes through closely coupled nucleocapsid
Flash heat transfer gives stratum nucleare VO2Its heating is set to undergo phase transition, to improve VO2Thermal response speed, shorten the phase transformation response time, and
And it reduces and makes VO2Undergo phase transition required environment temperature.
The present invention is achieved by the following technical programs：
A kind of efficient thermochromism composite nano-powder of nucleocapsid, the composite granule is with VO2Layer is stratum nucleare, tungsten bronze
Compound layer is shell；The VO2Layer is vanadium dioxide nano powder, and minimum size is no more than in three-dimensional dimension
100nm, size is not more than 100nm in preferably three dimensions, and shape is subsphaeroidal, elliposoidal, cylinder, flake, side
Bulk, polygon etc.；The tungsten bronze compound layer is MxWO3, wherein M is selected from NH4+, Cs+, K+, Na+Or Li+In any
Kind；The value range of x is 0.01~0.8；The thickness of tungsten bronze compound layer is less than 60nm, preferably not greater than 50nm.
The preparation method of the efficient thermochromism composite nano-powder of the nucleocapsid, includes the following steps：
A) by VO2Powder is scattered in solvent, VO2It is 1-50% in the mass percentage concentration of solvent, adds surface modification
Agent, the coating material and VO2Mass ratio be 0.5~6:1, mixing obtains the VO of surface modification2Mixed liquor A；It is described
Coating material is selected from polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone, poly- acetimide, acrylate copolymer, silane
At least one of coupling agent, fluorine-containing surfactant；
B) tungsten bronze presoma and doping element compound are added in above-mentioned mixed liquor A, being sufficiently mixed stirring keeps tungsten green
Copper presoma is attached to the surface of vanadium dioxide particle, adds reducing agent, and 25-180 DEG C of isothermal reaction obtains mixed liquid B；Tungsten
Bronze presoma and VO2Mass ratio be 0.1-5:1；The doping element compound is with tungsten bronze forerunner's body mass ratio
0.01-0.8:1；The mass ratio of reducing agent and tungsten bronze presoma is 0.1-20:1；Doping element compound is selected from ammonium hydroxide, chlorination
Ammonium, ammonium sulfate, ammonium hydrogen carbonate, cesium hydroxide, cesium chloride, cesium sulfate, ammonium nitrate, cesium carbonate, potassium hydroxide, potassium chloride, sulfuric acid
Potassium, potassium nitrate, cesium nitrate, potassium carbonate, sodium hydroxide, sodium chloride, sodium sulphate, sodium nitrate, sodium carbonate, lithium hydroxide, lithium chloride,
At least one of lithium sulfate, lithium nitrate, lithium carbonate；
C) solid phase components in above-mentioned mixed liquid B are subjected to centrifugation, vacuum drying treatment at 100 DEG C obtains tungsten blueness
The hypovanadic oxide powder C of copper presoma cladding；
D) above-mentioned powder C is placed in 100-600 DEG C of heat treatment in heating furnace, obtains the nucleocapsid for being coated with tungsten bronze
Thermochromism composite nano-powder.
VO described in step a)2Selected from A phases VO2, B phases VO2, M/R phases VO2, P phases VO2At least one of.
Step a) the solvents be selected from water, methanol, ethyl alcohol, sorbierite, normal propyl alcohol, isopropanol, ethylene glycol, benzyl alcohol, oneself
Alkane, toluene, dimethylbenzene, ethyl acetate, butyl acetate, acetone, espeleton, glycol monoethyl ether, propylene glycol methyl ether acetate,
At least one of oleic acid, oleyl amine.
In step b), tungsten bronze presoma in wolframic acid, sodium tungstate, ammonium tungstate, tungsten hexachloride, tungstic acid at least
It is a kind of；Reducing agent is selected from least one of citric acid, acetic acid, oleic acid, hydrochloric acid, oxalic acid, urea, sodium borohydride.
The isothermal reaction time is 0.5-4h in step b).
Step d) heat treatment times are 0.5-8h.
The present invention also protects the application of the efficient thermochromism composite nano-powder of the nucleocapsid, is used to prepare efficiently
Thermochromism VO2Film is applied to glass pane, building glass, vehicle glass, efficiently utilizes and regulates and controls sunlight, can make room
It is interior or interior be attained by comfortable temperature range at all seasons.
Beneficial effects of the present invention are as follows：
1) structure is with VO2Layer is stratum nucleare, the nucleocapsid that tungsten bronze compound layer is shell, utilizes the red of tungsten bronze material
Outer absorption characteristic makes shell absorb heat, and passes through closely coupled nucleocapsid flash heat transfer to stratum nucleare VO2Particle leads to its heating hair
Raw phase transformation, makes VO with this to reduce2Required environment temperature is undergone phase transition, VO is improved2Thermal response speed, shorten phase transformation reaction
Time achievees the effect that efficient thermochromism.
2) the efficient thermochromism composite nano-powder for the nucleocapsid that the present invention obtains can be used for preparing efficient thermotropic
Color VO2Film is applied on glass pane, when summer temperature is higher, makes VO after tungsten bronze heat absorption2Particle, which is rapidly heated, occurs phase
Become, can stop the heat of sunlight infrared region；When winter temperature is relatively low, the heat that tungsten bronze absorbs causes with ambient temperature equilibrium
VO2Particle temperature it is relatively low can not phase transformation, can pass through the heat of sunlight infrared region, and before phase change after, tungsten bronze and VO2Can
There is higher visible light transmittance rate in light-exposed area, does not interfere with daylighting, this thermochromic film is applied to building glass, glass of automobile
Glass etc., efficiently utilizes and regulation and control sunlight can make indoor or car that can reach at all seasons in the case where not influencing daylighting
To comfortable temperature range, have a good application prospect.
Description of the drawings：
Fig. 1 is the structural schematic diagram of the efficient thermochromism composite nano-powder of the nucleocapsid of the present invention；
Wherein, 1, VO2Layer, 2, tungsten bronze compound layer.
Specific implementation mode：
It is the further explanation to the present invention below, rather than limiting the invention.
Embodiment 1：
It is the A phases VO of 90nm to take 5g grain sizes2, it is 30%VO to be added in a certain amount of water and be configured to mass concentration2Suspension,
25g polyvinyl alcohol is added, 30min is mixed；0.5g ammonium tungstates and 0.015g ammonium chlorides is added, 30min is mixed, makes tungsten
The presoma of bronze is attached to VO2The surface of particle adds 10g citric acids, and 80 DEG C of isothermal reaction 1.5h obtain suspension,
It is dried in vacuo after centrifugation, at 100 DEG C and obtains the VO of tungsten bronze presoma cladding2Powder；Obtained powder is put into and is added
In hot stove, it is heat-treated 2h at 400 DEG C, obtains VO2@(NH4)0.1WO3Nuclear shell structure nano composite granule, wherein stratum nucleare VO2For M/R
Phase, shell (NH4)0.1WO3Thickness be 20nm.The VO of preparation2@(NH4)0.1WO3Nuclear shell structure nano composite granule can make VO2's
The phase transformation reaction time shortens 1min.
Embodiment 2
It is the B phases VO of 20nm to take 5g grain sizes2, it is 1%VO to be added in a certain amount of ethylene glycol and be configured to mass concentration2It suspends
2.5g polyethylene glycol is added in liquid, and 30min is mixed；10g sodium tungstates and 1.5g sodium sulphate is added, 30min is mixed, makes
The presoma of tungsten bronze is attached to VO2The surface of particle adds 10g oxalic acid, and 180 DEG C of isothermal reaction 0.5h obtain suspension,
It is dried in vacuo after centrifugation, at 100 DEG C and obtains the VO of tungsten bronze presoma cladding2Powder；Obtained powder is put into and is added
In hot stove, it is heat-treated 0.5h at 600 DEG C, obtains VO2@Na0.5WO3Nuclear shell structure nano composite granule, wherein stratum nucleare VO2For M/R
Phase, shell Na0.5WO3Thickness be 5nm.The VO of preparation2@Na0.5WO3Nuclear shell structure nano composite granule can make VO2Phase transformation it is anti-
Shorten 3min between seasonable.
Embodiment 3
It is the M/R phases VO of 70nm to take 5g grain sizes2, it is 10%VO to be added in a certain amount of ethyl alcohol and be configured to mass concentration2It suspends
The poly- acetimides of 15g are added in liquid, and 30min is mixed；15g wolframic acids and 0.75g lithium carbonates is added, 30min is mixed, makes
The presoma of tungsten bronze is attached to VO2The surface of particle adds 5g urea, and 25 DEG C of isothermal reaction 4h obtain suspension, through from
It is dried in vacuo after heart precipitation, at 100 DEG C and obtains the VO of tungsten bronze presoma cladding2Powder；Obtained powder is put into heating furnace
In, it is heat-treated 8h at 100 DEG C, obtains VO2@Li0.3WO3Nuclear shell structure nano composite granule, wherein stratum nucleare VO2For M/R phases, shell
Layer Li0.3WO3Thickness be 15nm.The VO of preparation2@Li0.3WO3Nuclear shell structure nano composite granule can make VO2Phase transformation reaction
Time shortens 2min..
Embodiment 4
It is the P phases VO of 50nm to take 5g grain sizes2, it is 5%VO to be added in a certain amount of benzyl alcohol and be configured to mass concentration2It suspends
7.5g fluorine-containing surfactants are added in liquid, and 30min is mixed；20g tungstic acids and 2g cesium carbonates is added, is mixed
30min makes the presoma of tungsten bronze be attached to VO2The surface of particle, adds 20g oleic acid, and 120 DEG C of isothermal reaction 1h are obtained
Suspension is dried in vacuo after centrifugation, at 100 DEG C and obtains the VO of tungsten bronze presoma cladding2Powder；Obtained powder
It is put into heating furnace, is heat-treated 3h at 300 DEG C, obtains VO2@Cs0.3WO3Nuclear shell structure nano composite granule, wherein stratum nucleare VO2For
M/R phases, shell Cs0.3WO3Thickness be 10nm.The VO of preparation2@Cs0.3WO3Nuclear shell structure nano composite granule can make VO2Phase
Become reaction time shortening 4min..
Embodiment 5
It is the M/R phases VO of 80nm to take 5g grain sizes2, it is 20%VO to be added in a certain amount of isopropanol and be configured to mass concentration2It is outstanding
20g polyvinylpyrrolidones are added in supernatant liquid, and 30min is mixed；15g sodium tungstates and 1.2g sodium chloride is added, is mixed
30min makes the presoma of tungsten bronze be attached to VO2The surface of particle, adds 1.5g sodium borohydrides, 50 DEG C of isothermal reaction 3h,
Suspension is obtained, is dried in vacuo after centrifugation, at 100 DEG C and obtains the VO of tungsten bronze presoma cladding2Powder；What is obtained
Powder is put into heating furnace, is heat-treated 6h at 150 DEG C, is obtained VO2@Na0.4WO3Nuclear shell structure nano composite granule, wherein stratum nucleare
VO2For M/R phases, shell Na0.4WO3Thickness be 15nm.The VO of preparation2@Na0.4WO3Nuclear shell structure nano composite granule can make VO2
The phase transformation reaction time shorten 3min..
Embodiment 6
It is the B phases VO of 60nm to take 5g grain sizes2, it is 5%VO to be added in a certain amount of butyl acetate and be configured to mass concentration2It is outstanding
10g fluorine-containing surfactants are added in supernatant liquid, and 30min is mixed；15g tungsten hexachlorides and 0.9g potassium nitrate is added, is mixed
30min makes the presoma of tungsten bronze be attached to VO2The surface of particle, adds 15g citric acids, 90 DEG C of isothermal reaction 1.5h,
Suspension is obtained, is dried in vacuo after centrifugation, at 100 DEG C and obtains the VO of tungsten bronze presoma cladding2Powder；What is obtained
Powder is put into heating furnace, is heat-treated 1h at 500 DEG C, is obtained VO2@K0.2WO3Nuclear shell structure nano composite granule, wherein stratum nucleare
VO2For M/R phases, shell K0.2WO3Thickness be 10nm.The VO of preparation2@K0.2WO3Nuclear shell structure nano composite granule can make VO2's
The phase transformation reaction time shortens 2min..
Embodiment 7
It is the M/R phases VO of 50nm to take 5g grain sizes2, it is 2%VO to be added in a certain amount of toluene and be configured to mass concentration2It suspends
5g silane coupling agents are added in liquid, and 30min is mixed；25g tungsten hexachlorides and 0.25g cesium hydroxides is added, is mixed
30min makes the presoma of tungsten bronze be attached to VO2The surface of particle, adds 20g acetic acid, and 60 DEG C of isothermal reaction 2.5h are obtained
Suspension is dried in vacuo after centrifugation, at 100 DEG C and obtains the VO of tungsten bronze presoma cladding2Powder；Obtained powder
It is put into heating furnace, is heat-treated 5h at 200 DEG C, obtains VO2@Cs0.01WO3Nuclear shell structure nano composite granule, wherein stratum nucleare VO2
For M/R phases, shell Cs0.01WO3Thickness be 5nm.The VO of preparation2@Cs0.01WO3Nuclear shell structure nano composite granule can make VO2's
The phase transformation reaction time shortens 1min..
Embodiment 8
It is the M/R phases VO of 100nm to take 5g grain sizes2, it is 50%VO to be added in a certain amount of oleic acid and be configured to mass concentration2It is outstanding
30g acrylate copolymers are added in supernatant liquid, and 30min is mixed；1g ammonium tungstates and 0.8g ammonium sulfate is added, is mixed
30min makes the presoma of tungsten bronze be attached to VO2The surface of particle, adds 2g hydrochloric acid, and 70 DEG C of isothermal reaction 2h are hanged
Turbid is dried in vacuo after centrifugation, at 100 DEG C and obtains the VO of tungsten bronze presoma cladding2Powder；Obtained powder is put
Enter in heating furnace, is heat-treated 4h at 250 DEG C, obtains VO2@(NH4)0.8WO3Nuclear shell structure nano composite granule, wherein stratum nucleare VO2
For M/R phases, shell (NH4)0.8WO3Thickness be 20nm.The VO of preparation2@(NH4)0.8WO3Nuclear shell structure nano composite granule can make
VO2The phase transformation reaction time shorten 4min.
Claims (10)
1. a kind of efficient thermochromism composite nano-powder of nucleocapsid, which is characterized in that the composite granule is with VO2Layer is core
Layer, tungsten bronze compound layer are shell；The VO2Layer is vanadium dioxide nano powder, minimum size in three-dimensional dimension
No more than 100nm, shape is subsphaeroidal, elliposoidal, cylinder, flake, square, polygon；The tungsten bronze chemical combination
Nitride layer is MxWO3, wherein M is selected from NH4+, Cs+, K+, Na+Or Li+Any one of；The value range of x is 0.01~0.8；Tungsten
The thickness of bronze compound layer is less than 60nm.
2. the efficient thermochromism composite nano-powder of nucleocapsid according to claim 1, which is characterized in that titanium dioxide
Size is not more than 100nm in three dimensions of vanadium nano-powder, and the thickness of tungsten bronze compound layer is not more than 50nm.
3. a kind of preparation method of the efficient thermochromism composite nano-powder of nucleocapsid described in claim 1, feature exist
In including the following steps：
A) by VO2Powder is scattered in solvent, VO2It is 1-50% in the mass percentage concentration of solvent, adds coating material,
The coating material and VO2Mass ratio be 0.5~6:1, mixing obtains the VO of surface modification2Mixed liquor A；The table
It is even that face dressing agent is selected from polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone, poly- acetimide, acrylate copolymer, silane
Join at least one of agent, fluorine-containing surfactant；
B) tungsten bronze presoma and doping element compound are added in above-mentioned mixed liquor A, is sufficiently mixed before stirring makes tungsten bronze
The surface that body is attached to vanadium dioxide particle is driven, adds reducing agent, 25-180 DEG C of isothermal reaction obtains mixed liquid B；Tungsten bronze
Presoma and VO2Mass ratio be 0.1-5:1；The doping element compound is 0.01- with tungsten bronze forerunner's body mass ratio
0.8:1；The mass ratio of reducing agent and tungsten bronze presoma is 0.1-20:1；Doping element compound is selected from ammonium hydroxide, ammonium chloride, sulphur
Sour ammonium, ammonium hydrogen carbonate, cesium hydroxide, cesium chloride, cesium sulfate, ammonium nitrate, cesium carbonate, potassium hydroxide, potassium chloride, potassium sulfate, nitre
Sour potassium, cesium nitrate, potassium carbonate, sodium hydroxide, sodium chloride, sodium sulphate, sodium nitrate, sodium carbonate, lithium hydroxide, lithium chloride, sulfuric acid
At least one of lithium, lithium nitrate, lithium carbonate；
C) solid phase components in above-mentioned mixed liquid B are subjected to centrifugation, vacuum drying treatment at 100 DEG C, before obtaining tungsten bronze
Drive the hypovanadic oxide powder C of body cladding；
D) above-mentioned powder C is placed in 100-600 DEG C of heat treatment in heating furnace, obtains the thermotropic of the nucleocapsid for being coated with tungsten bronze
Change colour composite nano-powder.
4. the preparation method of the efficient thermochromism composite nano-powder of nucleocapsid, feature exist according to claim 3
In the VO described in step a)2Selected from A phases VO2, B phases VO2, M/R phases VO2, P phases VO2At least one of.
5. according to the preparation method of the efficient thermochromism composite nano-powder of the nucleocapsid of claim 3 or 4, feature
Be, the step a) solvents be selected from water, methanol, ethyl alcohol, sorbierite, normal propyl alcohol, isopropanol, ethylene glycol, benzyl alcohol, hexane,
Toluene, dimethylbenzene, ethyl acetate, butyl acetate, acetone, espeleton, glycol monoethyl ether, propylene glycol methyl ether acetate, oil
At least one of acid, oleyl amine.
6. according to the preparation method of the efficient thermochromism composite nano-powder of the nucleocapsid of claim 3 or 4, feature
Be, in step b), tungsten bronze presoma in wolframic acid, sodium tungstate, ammonium tungstate, tungsten hexachloride, tungstic acid at least one
Kind.
7. according to the preparation method of the efficient thermochromism composite nano-powder of the nucleocapsid of claim 3 or 4, feature
It is, in step b), reducing agent is selected from least one of citric acid, acetic acid, oleic acid, hydrochloric acid, oxalic acid, urea, sodium borohydride.
8. according to the preparation method of the efficient thermochromism composite nano-powder of the nucleocapsid of claim 3 or 4, feature
It is, the isothermal reaction time is 0.5-4h in step b).
9. according to the preparation method of the efficient thermochromism composite nano-powder of the nucleocapsid of claim 3 or 4, feature
It is, step d) heat treatment times are 0.5-8h.
10. the application of the efficient thermochromism composite nano-powder of nucleocapsid described in claim 1, which is characterized in that be used for
Prepare efficient thermochromism VO2Film is applied to glass pane, building glass, vehicle glass, efficiently utilizes and regulate and control the sun
Light can make indoor or car be attained by comfortable temperature range at all seasons.
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| CN111732346A (en) * | 2020-07-01 | 2020-10-02 | 中国建材国际工程集团有限公司 | Preparation method of photochromic glass for improving speed of renaturation |
| CN111876073A (en) * | 2020-07-20 | 2020-11-03 | 中天东方氟硅材料有限公司 | Weather-resistant organic silicon transparent temperature control coating and preparation method thereof |
| CN113185863A (en) * | 2021-04-13 | 2021-07-30 | 电子科技大学 | Based on VO2Intelligent temperature control coating with core-shell structure and thermal variable emissivity |
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| CN114395324A (en) * | 2022-02-24 | 2022-04-26 | 北京国电富通科技发展有限责任公司 | Thermochromic antifouling flash silicone rubber composition |
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