CN104327579A - Monodisperse conductive heat-insulation mesoporous material as well as preparation method and application thereof - Google Patents
Monodisperse conductive heat-insulation mesoporous material as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a monodisperse conductive heat-insulation mesoporous material as well as a preparation method and application thereof. A heat-insulation tin antimony oxide precursor is prepared by adopting a solvothermal method; and a monodisperse tin antimony oxide conductive heat-insulation material is prepared by carrying out high-temperature calcining on the heat-insulation tin antimony oxide precursor. The electric conductivity of the material prepared by the method can reach 8.68*10<-2>omega*cm; and the powder is dispersed into polyurethane to prepare a heat shielding coating with stable performances. The heat shielding coating can be used for preparing a uniform and transparent heat-insulation film in a large area; and compared with blank glass, the heat insulation rate of the thin film can be more than 40%. The heat shielding material has good chemical and photo-thermal stable performances and the heat shielding efficiency is high, so that the heat shielding material can be used for manufacturing building glass heat-insulation thin films, heat-insulation conductive coatings and the like which are applied to buildings, automobiles, pipelines, storage tanks and the like. Furthermore, the preparation process is simple and easy to operate; the raw materials are cheap and easy to obtain and are suitable for industrial production; and a reaction process has the characteristics of greenness and environmental friendliness, low energy consumption, high benefits and the like.
Description
Technical field
The present invention relates to a kind of single dispersing conductive heat insulation mesoporous material and preparation method thereof, and application and this single dispersing conductive heat insulation mesoporous material preparing the application on transparent heat insulation diaphragm.
Background technology
Energy-saving and environmental protection have become the two principal themes of the world today.
Based on transparent conductive oxide (TCOs) by the transparent unique combination of electroconductibility and visible region, TCO material part in instantly many and emerging photoelectric device is made to play key player.Photodiode (LED) and liquid crystal display (LCD) technology are all make single pixel signal effectively transmit the switch realizing valid pixel by coating layer of transparent conductive oxide, ensure that the light produced can efficiently through conductive layer simultaneously.Flat-panel monitor mainly adopts ITO and IZO coating costly in the market, but for meeting the requirement that market is increased increasingly to display screen technology, research and development high-performance and low-cost transparent conductive oxide is extremely urgent.
In addition, it is exactly functional glass that another of TCO material is mainly applied.When the electrochromic clipping absorption layer in two tco layers applies certain voltage, glass can be dimmed or opaque.When this is owing to flowing through conductive oxide when the voltage applied, enliven absorption layer dimmed.Therefore oxide coating must be highly transparent in visible region, and just can make when absorption layer is inactive, electrochomeric glass can be used as ordinary window.For TCO material, although electrochromic still rests on market bud, building glass is a larger mainstream market.Due to TCOs, there is reflective infrared and absorb the light selectivity of ultraviolet, TCO is coated on glass, can obtain a kind ofly reducing thermal radiation and scattering and disappearing, reduce the low-radiation glass window of uv damage.Thus, the application of TCOs has heat-insulation and heat-preservation, improves Energy efficiency, reduces economic benefit and the social benefits such as energy consumption cost.
For this class material of TCO, ITO is most typical representative.The film prepared based on material has excellent electroconductibility and high light transmittance, make it be widely used in photoelectric device and Heat insulation type adhering film field, but the main component indium of ITO is expensive, thus researches and develops cheap high performance equivalent material and have huge commercial value.In recent years, because tin-antiomony oxide material shows good conductive heat insulation performance, preparation method has attracted more investigator.In order to obtain more excellent photoelectric properties, more investigator is devoted to the specific surface area improving tin-antiomony oxide material, but for preparing for transparent heat insulation diaphragm, the high dispersing of powder is the difficult point of research always.
The object of the invention is to prepare single dispersing by simple and direct effective chemical process and the tin-antiomony oxide conductive heat insulation material with high-specific surface area.The thermal barrier coatings prepared based on this material big area can prepare homogeneous transparent thermal isolation film, and heat insulation rate reaches more than 50%.In addition, preparation technology of the present invention is simple to operation, and raw material is cheap and easy to get, and be applicable to suitability for industrialized production, reaction process has environmental protection, less energy-consumption, high benefit feature.
Summary of the invention
The object of the invention is for the defect existing for above-mentioned prior art, an industrial production process being to provide a kind of monodisperse mesoporous lagging material, two application being to provide a kind of transparent heat insulation diaphragm.
For solving the problems of the technologies described above, technical scheme of the present invention is as follows:
Monodisperse mesoporous lagging material of the present invention take tin tetrachloride as matrix, antimony dopant element, adds appropriate tensio-active agent obtained with solvent thermal process.
Its concrete steps prepared are as follows:
1) be that 3%-15% takes SnCl by the mol ratio of Sb/Sn
4and SbCl
3and make it to be dissolved in methyl alcohol, wherein Sn element volumetric molar concentration is 17-68mmol/L;
2) tensio-active agent taking the 1-3% accounting for above-mentioned methanol quality is dissolved in above-mentioned methanol solution, stirs, and gained mixing solutions is placed in reactor, sealing, pyroreaction 5h;
3) question response still nature cold-zone is to room temperature, and reaction product is centrifugal, and by methanol wash, by even for the dry also grinding of product obtained, high-temperature calcination 2h, obtains single dispersing conductive heat insulation mesoporous material.
Step 2) described in tensio-active agent be polyvinylpyrrolidone or P123.
Step 2) temperature of reaction of described pyroreaction is 160-200 DEG C.
Step 3) calcining temperature of described high-temperature calcination is 500-800 DEG C.
The single dispersing conductive heat insulation mesoporous material prepared by aforesaid method is as follows for the preparation of the concrete operation step of transparent heat insulation diaphragm:
1) getting preceding claim single dispersing conductive heat insulation mesoporous material is scattered in urethane, and obtain heat insulation slurries after stirring, the lagging material solid content in slurries is 10-30%;
2) adopt knife coating procedure by made slurry film forming on glass substrate or transparent resin, oven drying at low temperature, obtains transparent heat insulation diaphragm; The temperature of described oven drying at low temperature is set to 60-70 DEG C.
The thermal insulating coating that the present invention is take tin-antiomony oxide as thermal insulating filling, urethane is prepared for membrane-forming agent, can be used for glass or transparent resin.By change tin-antiomony oxide in coating solid content can modulate the through performance of thermal insulation film.The present invention requires the energy-saving heat-insulating of the occasions such as good daylighting mainly for constructure screen wall glass, automotive glazing, transparent ceiling, automobile, display etc.
Compared with prior art, this material has following characteristics:
(1) from material physical chemistry character, compare the metallic red external shield material accounting for leading market status, it is easily oxidized that this product overcomes metal material, and the problems such as shielding GPS, mobile phone and tick.
(2) with regard on Material selec-tion, the present invention selects SnO
2, Sb
2o
3deng the raw material of inexpensive safety, compare the indium base TCO oxide compound such as expensive ITO (tin indium oxide), IZO (indium zinc oxide), while guarantee has close infrared shielding ability, greatly reduce production cost, become the contenders replacing ITO, IZO material.
(3) prepare compared with single film product with utilizing target material magnetic sputtering, this research all adopts Liquid preparation methods single dispersing conductive heat insulation powder, and being soluble in most of solvent and high transparent resin based on prepared powder body material, prepared nano composite material has wide Application Areas.
(4) preparation technology of the present invention is simple to operation, and raw material is cheap and easy to get, and reaction process does not have three industrial wastes substantially, has environmental protection, less energy-consumption, high yield feature, is applicable to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 a is the Wide angle X-ray diffraction figure of described different Sb doped concentration tin-antiomony oxide;
Fig. 1 b is the small angle X-ray diffraction figure of different Sb doped concentration tin-antiomony oxide;
Fig. 1 c is the Langmuir isothermal adsorption desorption curve figure of different Sb doped concentration tin-antiomony oxide;
Fig. 1 d is the graph of pore diameter distribution of different Sb doped concentration tin-antiomony oxide;
Fig. 2 is the scanning electron microscope diagram of the corresponding tin-antiomony oxide of different Sb doped concentration;
Fig. 3 is resistivity and the size of the corresponding tin-antiomony oxide powder of different Sb doped concentration;
Fig. 4 is that the ultraviolet-visible-near infrared of transparent heat insulation diaphragm is through spectrogram;
Fig. 5 is the effect of heat insulation graphic representation of transparent film.
Embodiment
Below by embodiment, the invention will be further described, and its object is only better understand content of the present invention but not limit the scope of the invention:
Embodiment 1
The preparation method of the single dispersing conductive heat insulation material that the present embodiment provides and application, concrete steps are as follows:
1) 0.175g SnCl is taken
45H
2o, 0.00341g SbCl
3(mol ratio of Sb/Sn is 3%), be dissolved in 30mL methyl alcohol, wherein Sn element volumetric molar concentration should be 17mmol/L, stirs and obtains colourless transparent solution;
2) take account for methanol quality 1% polyvinylpyrrolidone (PVP), be dissolved in above-mentioned methanol solution, after stirring colourless transparent solution, gained mixing solutions is placed in reactor, sealing, 180 DEG C of pyroreaction 5h;
3) question response still nature cold-zone is to room temperature, and reaction product is centrifugal, by methanol wash 3 times, the light yellow product that obtains is dry and after grinding evenly, 500 DEG C of high-temperature calcination 2h, can obtain single dispersing conductive heat insulation mesoporous material;
This powdered sample represents with ATO-3 in test pattern, and its wide-angle and small angle X-ray diffraction figure, Langmuir isothermal adsorption desorption curve, pore size distribution, field emission scanning electron microscope figure, resistivity and grain-size graph are shown in Fig. 1 a, 1b, 1c, 1d, Fig. 2 and Fig. 3 respectively.From these tests, prepared conductive powder sample is monodispersed tin-antiomony oxide mesoporous microsphere, and this microballoon is formed by single nanoparticle accumulation.
4) take appropriate prepared lagging material, be scattered in urethane, obtain heat insulation slurries after stirring, wherein the lagging material solid content of slurries can be 15%.
5) adopt knife coating procedure by film forming on glass substrate clean for made slurry, after 60 DEG C of oven dry, namely obtain uniform heat-insulation transparent film.
Be the H103 resin that this film sample is corresponding from ATO-3 in Fig. 4: this this material is that the film of thermal insulating filling has the good transparency, and heat insulation rate is 17.89%.Wherein the method for calculation of heat insulation rate are: heat insulation rate=and through the energy T of simple glass
blank-through the energy T of sample thin film
sol, adopt following formula to calculate sunlight through energy T
sol(250-2500nm):
Embodiment 2
The preparation method of the present embodiment is identical with described in embodiment 1, and difference is SbCl
3doping (mol ratio of 0.00569g, Sb/Sn is 5%).This powdered sample represents with ATO-5 in test pattern, and its wide-angle and small angle X-ray diffraction figure, Langmuir isothermal adsorption desorption curve, pore size distribution, field emission scanning electron microscope figure, resistivity and grain-size graph are shown in Fig. 1 a, 1b, 1c, 1d, Fig. 2 and Fig. 3 respectively.The analytical results of conductive heat insulation mesoporous material prepared by the present embodiment is all similar to embodiment 1.
Be the H103 resin that this film sample is corresponding from ATO-5 in Fig. 4: this this material is that the film of thermal insulating filling has the good transparency, and heat insulation rate is 19.76%.
Embodiment 3
The preparation method of the present embodiment is identical with described in embodiment 1, and difference is SbCl
3doping (mol ratio of 0.00797g, Sb/Sn is 7%).This powdered sample represents with ATO-7 in test pattern, and its wide-angle and small angle X-ray diffraction figure, Langmuir isothermal adsorption desorption curve, pore size distribution, field emission scanning electron microscope figure, resistivity and grain-size graph are shown in Fig. 1 a, 1b, 1c, 1d, Fig. 2 and Fig. 3 respectively.The analytical results of conductive heat insulation mesoporous material prepared by the present embodiment is all similar to embodiment 1.
Be the H103 resin that this film sample is corresponding from ATO-7 in Fig. 4: this this material is that the film of thermal insulating filling has the good transparency, and heat insulation rate is 21.66%.
Embodiment 4
The preparation method of the present embodiment is identical with described in embodiment 1, and difference is SbCl
3doping (mol ratio of 0.0114g, Sb/Sn is 10%).This powdered sample represents with ATO-10 in test pattern, and its wide-angle and small angle X-ray diffraction figure, Langmuir isothermal adsorption desorption curve, pore size distribution, field emission scanning electron microscope figure, resistivity and grain-size graph are shown in Fig. 1 a, 1b, 1c, 1d, Fig. 2 and Fig. 3 respectively.The analytical results of conductive heat insulation mesoporous material prepared by the present embodiment is all similar to embodiment 1.
Be the H103 resin that this film sample is corresponding from ATO-10 in Fig. 4: this this material is that the film of thermal insulating filling has the good transparency, and heat insulation rate is 27.66%.Effect of heat insulation figure corresponding to this film sample, as shown in ATO-10 in Fig. 5 (15%), has the effect of heat insulation of 10 DEG C compared with blank glass.
Embodiment 5
The preparation method of the present embodiment is identical with described in embodiment 4, and difference is, is 25% for the preparation of the solid content of tin-antiomony oxide (ATO-10) in the slurry of film sample.This powdered sample represents with ATO-10 in test pattern, and its wide-angle and small angle X-ray diffraction figure, Langmuir isothermal adsorption desorption curve, pore size distribution, field emission scanning electron microscope figure, resistivity and grain-size graph are shown in Fig. 1 a, 1b, 1c, 1d, Fig. 2 and Fig. 3 respectively.The analytical results of conductive heat insulation mesoporous material prepared by the present embodiment is all similar to embodiment 4.
Be the H103 resin that this film sample is corresponding from ATO-10 in Fig. 4: this this material is that the film of thermal insulating filling has the good transparency, and heat insulation rate is 41.5%.Effect of heat insulation figure corresponding to this film sample, as shown in ATO-10 in Fig. 5 (25%), has the effect of heat insulation of 13 DEG C compared with blank glass.
Be more than that embodiment shows, the doping of antimony has conclusive impact to the conductivity of tin-antiomony oxide material and thermoshield performance.Along with the electroconductibility of the increase tin-antiomony oxide powder of Sb doped amount strengthens, thermal shielding capability increases simultaneously, and in the present invention, ATO-10 powdered sample is optimum.When allocating heat-insulating slurry, the thermal insulating filling solid content of slurry can affect the transparency of prepared film and heat insulation intensity equally.Solid content increases, and thermal insulation film transparency reduces, and heat insulation intensity significantly increases simultaneously.The present invention's suggestion can need according to daylighting the thermal insulating coating allocating different solid content.
Claims (7)
1. a preparation method for single dispersing conductive heat insulation mesoporous material, is characterized in that: concrete steps are as follows:
1) be that 3%-15% takes SnCl by the mol ratio of Sb/Sn
4and SbCl
3and make it to be dissolved in methyl alcohol, wherein Sn element volumetric molar concentration is 17-68mmol/L;
2) tensio-active agent taking the 1-3% accounting for above-mentioned methanol quality is dissolved in above-mentioned methanol solution, stirs, and gained mixing solutions is placed in reactor, sealing, pyroreaction 5h;
3) question response still nature cold-zone is to room temperature, and reaction product is centrifugal, and by methanol wash, by even for the dry also grinding of product obtained, high-temperature calcination 2h, obtains single dispersing conductive heat insulation mesoporous material.
2. preparation method according to claim 1, is characterized in that: described tensio-active agent is polyvinylpyrrolidone or P123.
3. preparation method according to claim 1, is characterized in that: step 2) temperature of reaction of described pyroreaction is 160-200 DEG C.
4. preparation method according to claim 1, is characterized in that: step 3) calcining temperature of described high-temperature calcination is 500-800 DEG C.
5. a single dispersing conductive heat insulation mesoporous material, is prepared by the method described in claim 1-4 any one.
6. single dispersing conductive heat insulation mesoporous material according to claim 5 is for the preparation of a kind of preparation method of transparent heat insulation diaphragm, and it is characterized in that, concrete operation step is as follows:
1) the single dispersing conductive heat insulation mesoporous material got described in claim 5 is scattered in urethane, and obtain heat insulation slurries after stirring, the lagging material solid content in slurries is 10-30%;
2) adopt knife coating procedure by made slurry film forming on glass substrate or transparent resin, oven drying at low temperature, obtains transparent heat insulation diaphragm.
7. preparation method according to claim 6, is characterized in that, step 2) temperature of described oven drying at low temperature is set to 60-70 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109837027A (en) * | 2019-02-27 | 2019-06-04 | 南京巨鲨显示科技有限公司 | A kind of sterilizing monitoring indicator tape of the no printing ink transfer without residue glue |
| CN111087654A (en) * | 2019-12-31 | 2020-05-01 | 宁波柔创纳米科技有限公司 | Transparent heat-insulation anti-static film and preparation method thereof, and composite film and preparation method thereof |
| CN113078268A (en) * | 2021-03-30 | 2021-07-06 | 北京理工大学 | Method for preparing mesoporous film at low temperature by using polymer pore-forming agent |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723438A (en) * | 2009-11-13 | 2010-06-09 | 东华大学 | Method for preparing antimony-doped tin oxide nano-microspheres |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723438A (en) * | 2009-11-13 | 2010-06-09 | 东华大学 | Method for preparing antimony-doped tin oxide nano-microspheres |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109837027A (en) * | 2019-02-27 | 2019-06-04 | 南京巨鲨显示科技有限公司 | A kind of sterilizing monitoring indicator tape of the no printing ink transfer without residue glue |
| CN109837027B (en) * | 2019-02-27 | 2021-08-20 | 南京巨鲨显示科技有限公司 | Sterilization monitoring indication adhesive tape without ink transfer and adhesive residue |
| CN111087654A (en) * | 2019-12-31 | 2020-05-01 | 宁波柔创纳米科技有限公司 | Transparent heat-insulation anti-static film and preparation method thereof, and composite film and preparation method thereof |
| CN111087654B (en) * | 2019-12-31 | 2022-03-11 | 宁波柔创纳米科技有限公司 | Transparent heat-insulation anti-static film and preparation method thereof, and composite film and preparation method thereof |
| CN113078268A (en) * | 2021-03-30 | 2021-07-06 | 北京理工大学 | Method for preparing mesoporous film at low temperature by using polymer pore-forming agent |
| CN113078268B (en) * | 2021-03-30 | 2022-08-02 | 北京理工大学 | Method for preparing mesoporous film at low temperature by using polymer pore-forming agent |
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