CN102241967A - Three-dimensional ordered macroporous perovskite thermochromatic material and preparation method thereof - Google Patents
Three-dimensional ordered macroporous perovskite thermochromatic material and preparation method thereof Download PDFInfo
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- CN102241967A CN102241967A CN2011101221120A CN201110122112A CN102241967A CN 102241967 A CN102241967 A CN 102241967A CN 2011101221120 A CN2011101221120 A CN 2011101221120A CN 201110122112 A CN201110122112 A CN 201110122112A CN 102241967 A CN102241967 A CN 102241967A
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Abstract
The invention discloses a three-dimensional ordered macroporous perovskite thermochromatic material and a preparation method thereof. The preparation method comprises the following steps of: depositing monodisperse polystyrene (PS) colloid microspheres on a clean and dry quartz glass sheet by adopting a vertical deposition method, and assembling into a three-dimensional ordered PS colloid crystal template; filling a precursor solution of La1-xAxMnO3 (A=Ca and/or Sr; and x is more than 0 and less than 3) in clearances of the PS colloid crystal template; and drying and calcining to remove the PS colloid crystal template to obtain the three-dimensional ordered macroporous perovskite thermochromatic material, wherein the surface and interior of the three-dimensional ordered macroporous perovskite thermochromatic material are provided with submicron-scale holes. The three-dimensional ordered macroporous perovskite thermochromatic material keeps the thermochromatic property of the conventional bulk material, and has a periodically arranged three-dimensional space net structure; and in the preparation method for the material, material consumption is low and components are uniformly mixed.
Description
Technical field
The invention belongs to the thermochromic material technology, particularly a kind of three-dimensional ordered macroporous uhligite thermochromic material and preparation method thereof.
Background technology
The lanthanum manganate of doping strontium and calcium is the thermochromism variable emissivity material with perovskite structure, and this material has good prospects for application in the thermal control field of spacecraft.Studies show that when temperature changed, the emittance of perovskite oxide material surface thermal radiation produced bigger variation between 173K-373K.When being lower than phase transition temperature, temperature shows as metallicity than low-launch-rate; And when being higher than phase transition temperature, temperature shows as the isolator of higher emissivity.The thermal control coating that utilizes thermochromic material to make, be covered on the temperature controlling instruments surface, can regulate self radiation characteristic automatically according to the temperature levels of equipment, thereby the exchange of the quantity of radiant energy between operating device and the external environment realizes the intelligent control to device temperature.
But just from changing the radiation characteristic on material properties angle research thermochromic function surface, in fact, the variation of thermochromic function material surface microstructure features also can cause the change of surface emissivity characteristic in research in the past.For example, document 1 (Genchu Tang, Thermochromic properties of manganese oxides La
1-xA
xMnO
3(A=Ca, Ba), Materials Letters, 2008) adopt solid reaction process to prepare big blocky uhligite thermochromic material, but do not consider the influence of the variation of material surface microstructure features to the surface emissivity characteristic; Document 2 (MasahiroSadakane, Facile procedure to prepare three-dimensionally ordered macroporous (3DOM) perovskite-type mixed metal oxides by colloidal crystal templating method, Chem Mater, 2005) adopt glue crystal template method to prepare three-dimensional ordered macroporous perovskite material, but be not pressed into the film like material, this has also influenced the application of this type of material in intelligent thermal control process.Three-dimensional ordered macroporous (3DOM) material is meant the aperture in submicron order yardstick (0.1～1.0 micron) scope, and the tridimensional network material that pore distribution is even, arrangement is periodically strong.If the material preparation of uhligite thermochromic function is become three-dimensional ordered macroporous structure, not only the change of temperature can cause the variation of surface emissivity characteristic, and the change of surface micro-structure also can be played the effect of reconciliation statement surface radiation characteristic.
Summary of the invention
The object of the present invention is to provide good three-dimensional ordered macroporous uhligite thermochromic material of a kind of thermochromic properties and preparation method thereof.The constructional feature of this material is to be substrate with the quartz glass plate, and material is deposited on the three-dimensional ordered macroporous uhligite thermochromic material of formation on the quartz glass plate.
The technical solution that realizes the object of the invention is: a kind of three-dimensional ordered macroporous uhligite thermochromic material is substrate with the quartz glass plate, material is deposited on forms three-dimensional ordered macroporous (3DOM) uhligite thermochromic material on the quartz glass plate.
A kind of preparation method of three-dimensional ordered macroporous uhligite thermochromic material, step is as follows:
The first step, adopting vertical depositing method deposits to monodispersed polystyrene PS colloid micro ball on the quartz glass plate of clean dried, is assembled into the PS colloidal crystal template that three-dimensional order is arranged;
Second step is with La
1-xA
xMnO
3(A=Ca and/or Sr; 0＜x＜0.3) precursor solution is filled in the PS glue crystal template gap and goes;
The 3rd step, remove the PS colloidal crystal template through super-dry and calcining, obtain three-dimensional ordered macroporous uhligite thermochromic material, its surface and the inner hole that is uniform-distribution with submicron-scale.
The present invention compared with prior art, its remarkable advantage: (1) keeps the thermochromic properties of existing big bulk material.The lanthanum manganate of doping strontium and calcium is the thermochromic material with perovskite structure.Three-dimensional ordered macroporous perovskite material is identical with existing big block material component, and just its surface and internal structure change, and it still has thermochromic properties.(2) has the three-dimensional space net structure of periodic arrangement.Duplicate because this material is the contrary of PS colloidal crystal template fully, it has kept the three-dimensional space network structure of high-sequential.And its pore distribution is even, and the aperture just in time is in the UV, visible light optical band in the submicron-scale scope, and this selectivity for the part light that is in the UV, visible light optical band absorbs and has important effect.(3) preparing few and each component of these material materials mixes.Because this material is directly to be prepared into the membrane structure material, the centre does not need therefore can save starting material widely through technologies such as cuttings.And various metals are to be dispersed in the solution with ionic species, and through fully stirring, metal-salt is consoluet, and this mixes much even than simple solid.(4) can measure its optical parametric easily.Because this material is directly to prepare on quartz glass plate, can be prepared into the sample of different size dimensions according to the test needs, can measure reflection, the transmitted spectrum of material so easily, optical parametrics such as emittance.
Below in conjunction with accompanying drawing the present invention is described in further detail.
Description of drawings
Fig. 1 utilizes glue crystal template legal system to be equipped with the synoptic diagram of 3DOM perovskite material.
Fig. 2 utilizes scanning electron microscope (SEM) to take 3DOM uhligite (a) La that obtains
0.8Sr
0.2MnO
3(b) La
0.7Ca
0.2Sr
0.1MnO
3The surface topography map of material.
Embodiment
The three-dimensional ordered macroporous uhligite thermochromic material of the present invention, with the quartz glass plate is substrate, material is deposited on formation three-dimensional ordered macroporous (3DOM) uhligite thermochromic material on the quartz glass plate, the hole of submicron-scale (0.1～1.0 micron) is evenly distributed on the surperficial and inner of uhligite thermochromic material, and whole material forms the spacial framework that three-dimensional order is arranged.
In conjunction with Fig. 1, the preparation method of the three-dimensional ordered macroporous uhligite thermochromic material of the present invention, step is as follows:
The first step, the preparation of polystyrene (PS) colloid micro ball:
With vinylbenzene (C
8H
8), sodium hydroxide (NaOH), Potassium Persulphate (K
2S
2O
8), Sodium styrene sulfonate (C
8H
7SO
3Na); Saleratus (KHCO
3), nitrogen (N
2), deionized water (H
2O) be raw material, adopt emulsion polymerisation process,, prepare monodispersed polystyrene (PS) colloid micro ball of particle diameter at 200～500nm by changing experiment condition.
Second step, the assembling of polystyrene (PS) glue crystal template
Adopting vertical depositing method deposits to monodispersed polystyrene PS colloid micro ball on the quartz glass plate of clean dried, is assembled into the PS colloidal crystal template (being called for short the glue crystal template) that three-dimensional order is arranged; PS glue crystal template is prepared by vertical deposition method by the PS colloid micro ball, the detailed process of vertical deposition is: the vertical immersion of quartz glass plate of clean dried filled in the weighing bottle of PS colloid micro ball solution, this device left standstill 0.5-1.5 days under 35-45 ℃ and 60% relative humidity, will form one deck colloidal crystal template on quartz glass plate surface, then this colloidal crystal template at 75-85 ℃ of following thermal treatment 1～3h.
The 3rd step, the filling of metal salt solution
With La
1-xA
xMnO
3(A=Ca and/or Sr; 0＜x＜0.3) precursor solution is filled in the PS glue crystal template gap and goes; The preparation of precursor solution: with ethanol is solvent, and nitrate and the manganous acetate of La, Ca, Sr is mixed with the precursor solution that volumetric molar concentration is 0.2～1.0mol/L.The filling of precursor solution: adopt dipping-method of pulling up that precursor solution is filled in the glue crystal template gap and go, the detailed process of flooding-lifting is: at first vertically immerse the glue crystal template in the precursor solution, dipping 5～20min at the uniform velocity pulls out the glue crystal template with the pull rate of 1～5cm/min then.
The 4th step, the removal of polystyrene (PS) glue crystal template
Remove the PS colloidal crystal template through super-dry and calcining, obtain three-dimensional ordered macroporous uhligite thermochromic material, its surface and the inner hole that is uniform-distribution with submicron-scale.Wherein, drying temperature is 30～60 ℃, and be 1～3h time of drying.Calcination process: on one side with the speed bubbling air of 10～50mL/min, on one side with the speed elevated temperature of 1～5 ℃/min; Temperature is from being incubated 1～3h after room temperature is raised to 350 ℃ to remove the crystal template that removes photoresist, and is incubated 3h after continuing to be warming up to 600～800 ℃.
Three-dimensional ordered macroporous uhligite thermochromic material by method for preparing, different with the structure of big block uhligite thermochromic material densification, the surface of this material and inside are uniform-distribution with the hole of submicron-scale (0.1～1.0 micron), and whole material forms the spacial framework that three-dimensional order is arranged.
Fig. 1 utilizes glue crystal template legal system to be equipped with the synoptic diagram of 3DOM perovskite material, for verifying the feasibility of this method, with La
0.8Sr
0.2MnO
3And La
0.7Ca
0.2Sr
0.1MnO
3Material be prepared as example, adopt glue crystal template method to prepare three-dimensional ordered macroporous La respectively
0.8Sr
0.2MnO
3And La
0.7Ca
0.2Sr
0.1MnO
3The uhligite thermochromic material.X-ray diffraction analysis knows that the material of two kinds of different componentss all forms single-phase perovskite structure.
Embodiment 1
La
0.8Sr
0.2MnO
3The preparation of material:
1, adopt emulsion polymerisation process, it is good to prepare monodispersity by the control synthesis condition, and median size is about polystyrene (PS) colloid micro ball of 220nm;
2, the vertical immersion of quartz glass plate with clean dried fills in the weighing bottle of PS colloid micro ball solution, and adopting vertical depositing method deposits to monodispersed PS colloid micro ball on the quartz glass plate, is assembled into the PS glue crystal template that three-dimensional order is arranged;
3, select for use ethanol to make solvent, press La (NO
3)
36H
2O: Sr (NO
3)
2: Mn (CH
3COO)
24H
2O=0.8: 0.2: 1 ratio takes by weighing metal nitrate and acetate preparation precursor solution.PS glue crystal template soaked 5 minutes in precursor solution after, template is at the uniform velocity pulled out with the speed of 2cm/min, put into baking oven then immediately dry 1 hour;
4, the sample that obtains put in the tube furnace calcined, on one side with the speed bubbling air of 20mL/min, on one side with the speed elevated temperature of 1 ℃/min, treat temperature be raised to 350 ℃ after insulation 2 hours to remove the crystal template that removes photoresist, continue to be warming up to 600 ℃ of insulations 3 hours.Behind naturally cooling, can obtain three-dimensional ordered macroporous La
0.8Sr
0.2MnO
3Perovskite material.
Embodiment 2
La
0.7Ca
0.2Sr
0.1MnO
3The preparation of material:
Adopt the method identical, press La (NO with embodiment 1
3)
36H
2O: Ca (NO
3)
24H
2O: Sr (NO
3)
2: Mn (CH
3COO)
24H
2O=0.7: 0.2: 0.1: 1 ratio takes by weighing metal nitrate and acetate preparation precursor solution.Prepare three-dimensional ordered macroporous La
0.7Ca
0.2Sr
0.1MnO
3Perovskite material.
Fig. 2 (a) and (b) be the three-dimensional ordered macroporous La for preparing
0.8Sr
0.2MnO
3And La
0.7Ca
0.2Sr
0.1MnO
3The microtexture shape appearance figure of perovskite material.The structure height of three-dimensional ordered macroporous material is orderly, and pore distribution is even, all is interconnected by regularly arranged aperture between each macropore, thereby forms the spacial framework that a three-dimensional order is arranged.X-ray diffraction analysis knows that the material of two kinds of different componentss all forms single-phase perovskite structure.
Claims (8)
1. a three-dimensional ordered macroporous uhligite thermochromic material is characterized in that: be substrate with the quartz glass plate, material be deposited on form three-dimensional ordered macroporous (3DOM) uhligite thermochromic material on the quartz glass plate.
2. three-dimensional ordered macroporous uhligite thermochromic material according to claim 1, it is characterized in that: the hole of submicron-scale is evenly distributed on the surperficial and inner of uhligite thermochromic material, and whole material forms the spacial framework that three-dimensional order is arranged.
3. the preparation method of a three-dimensional ordered macroporous uhligite thermochromic material is characterized in that step is as follows:
The first step, adopting vertical depositing method deposits to monodispersed polystyrene PS colloid micro ball on the quartz glass plate of clean dried, is assembled into the PS colloidal crystal template that three-dimensional order is arranged;
Second step is with La
1-xA
xMnO
3(A=Ca and/or Sr; 0＜x＜0.3) precursor solution is filled in the PS glue crystal template gap and goes;
The 3rd step, remove the PS colloidal crystal template through super-dry and calcining, obtain three-dimensional ordered macroporous uhligite thermochromic material, its surface and the inner hole that is uniform-distribution with submicron-scale.
4. the preparation method of three-dimensional ordered macroporous uhligite thermochromic material according to claim 3, it is characterized in that: PS glue crystal template is prepared by vertical deposition method by the PS colloid micro ball, the detailed process of vertical deposition is: the vertical immersion of quartz glass plate of clean dried filled in the weighing bottle of PS colloid micro ball solution, this device left standstill 0.5-1.5 days under 35-45 ℃ and 60% relative humidity, will form one deck colloidal crystal template on quartz glass plate surface, then this colloidal crystal template at 75-85 ℃ of following thermal treatment 1～3h.
5. the preparation method of three-dimensional ordered macroporous uhligite thermochromic material according to claim 3, it is characterized in that the preparation of precursor solution: be solvent with ethanol, nitrate and the manganous acetate of La, Ca, Sr is mixed with the precursor solution that volumetric molar concentration is 0.2～1.0mol/L.
6. the preparation method of three-dimensional ordered macroporous uhligite thermochromic material according to claim 3, it is characterized in that the filling of precursor solution: adopt dipping-method of pulling up that precursor solution is filled in the glue crystal template gap and go, the detailed process of flooding-lifting is: at first vertically immerse the glue crystal template in the precursor solution, dipping 5～20min at the uniform velocity pulls out the glue crystal template with the pull rate of 1～5cm/min then.
7. the preparation method of three-dimensional ordered macroporous uhligite thermochromic material according to claim 3 is characterized in that: drying temperature is 30～60 ℃, and be 1～3h time of drying.
8. the preparation method of three-dimensional ordered macroporous uhligite thermochromic material according to claim 3 is characterized in that calcination process: on one side with the speed bubbling air of 10～50mL/min, on one side with the speed elevated temperature of 1～5 ℃/min; Temperature is from being incubated 1～3h after room temperature is raised to 350 ℃ to remove the crystal template that removes photoresist, and is incubated 3h after continuing to be warming up to 600～800 ℃.
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| CN102517015A (en) * | 2011-12-13 | 2012-06-27 | 昆明理工大学 | Three-dimensional ordered porous up-conversion luminescent material with Y2Si2O7 as substrate, and preparation method thereof |
| CN102533267A (en) * | 2011-12-22 | 2012-07-04 | 昆明理工大学 | Three-dimensional ordered macroporous up-conversion luminescent ceramic material with Lu2O3 as substrate and preparation method thereof |
| CN102584237A (en) * | 2011-12-22 | 2012-07-18 | 昆明理工大学 | Three-dimensional ordered macropore upconversion luminescent ceramic material using Al2Y4O9 as matrix and preparation method thereof |
| JP2014047307A (en) * | 2012-08-31 | 2014-03-17 | National Institute Of Advanced Industrial & Technology | Photochromic material, and method of reversible change of absorption spectrum of photochromic material |
| CN104975258A (en) * | 2015-03-28 | 2015-10-14 | 桐城市新丰彩印包装有限公司 | Preparing technology for color changing film |
| WO2016110851A1 (en) * | 2015-01-07 | 2016-07-14 | Yissum Research Development Company Of The Hebrew University Of Jerusalem Ltd | Self-assembly of perovskite for fabrication of transparent devices |
| WO2018018481A1 (en) * | 2016-07-28 | 2018-02-01 | The University Of Hong Kong | Fabrication of perovskite periodic arrays for optoelectronic applications |
| CN107973339A (en) * | 2017-11-24 | 2018-05-01 | 武汉理工大学 | The three-dimensional ordered macroporous calcium titanate photonic crystal and its synthetic method that a kind of porous nano-sheet is constructed |
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| CN102533267A (en) * | 2011-12-22 | 2012-07-04 | 昆明理工大学 | Three-dimensional ordered macroporous up-conversion luminescent ceramic material with Lu2O3 as substrate and preparation method thereof |
| CN102584237A (en) * | 2011-12-22 | 2012-07-18 | 昆明理工大学 | Three-dimensional ordered macropore upconversion luminescent ceramic material using Al2Y4O9 as matrix and preparation method thereof |
| JP2014047307A (en) * | 2012-08-31 | 2014-03-17 | National Institute Of Advanced Industrial & Technology | Photochromic material, and method of reversible change of absorption spectrum of photochromic material |
| WO2016110851A1 (en) * | 2015-01-07 | 2016-07-14 | Yissum Research Development Company Of The Hebrew University Of Jerusalem Ltd | Self-assembly of perovskite for fabrication of transparent devices |
| CN107431127A (en) * | 2015-01-07 | 2017-12-01 | 耶路撒冷希伯来大学伊森姆研究发展有限公司 | For the self assembly for the perovskite for manufacturing transparent unit |
| US10192689B2 (en) | 2015-01-07 | 2019-01-29 | Yissum Research Development Company Of The Hebrew University Of Jerusalem Ltd. | Self-assembly of perovskite for fabrication of transparent devices |
| CN104975258A (en) * | 2015-03-28 | 2015-10-14 | 桐城市新丰彩印包装有限公司 | Preparing technology for color changing film |
| WO2018018481A1 (en) * | 2016-07-28 | 2018-02-01 | The University Of Hong Kong | Fabrication of perovskite periodic arrays for optoelectronic applications |
| US11404657B2 (en) | 2016-07-28 | 2022-08-02 | The University Of Hong Kong | Method of fabricating perovskite periodic nanostructure including solid-liquid-solid phase transformation |
| CN107973339A (en) * | 2017-11-24 | 2018-05-01 | 武汉理工大学 | The three-dimensional ordered macroporous calcium titanate photonic crystal and its synthetic method that a kind of porous nano-sheet is constructed |
| CN107973339B (en) * | 2017-11-24 | 2020-04-21 | 武汉理工大学 | Three-dimensional ordered macroporous calcium titanate photonic crystal constructed by porous nanosheets and synthetic method thereof |
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Application publication date: 20111116 |