CN108483934A - A kind of tungsten bronze/silica dioxide gel heat-insulation functional material and preparation method thereof - Google Patents
A kind of tungsten bronze/silica dioxide gel heat-insulation functional material and preparation method thereof Download PDFInfo
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- CN108483934A CN108483934A CN201810270924.1A CN201810270924A CN108483934A CN 108483934 A CN108483934 A CN 108483934A CN 201810270924 A CN201810270924 A CN 201810270924A CN 108483934 A CN108483934 A CN 108483934A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/23—Mixtures
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
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Abstract
The invention discloses a kind of tungsten bronze/silica dioxide gel heat-insulation functional materials and preparation method thereof, and the functional material is using silica and tungsten bronze as primary raw material, and by 100% silica of mass fraction, 10 15% tungsten bronzes are combined；Preparation method is：Transparent silica dioxide gel is first prepared under the catalysis of catalyst with sol-gal process, it is spare after aged, dilution, filtering；Function tungsten bronze nano-particle is scattered in liquid alcohol, through grinding for several times, ultrasound, then with silica dioxide gel be mixed；On the glass sheet with coating by gained functional paint, dry, sintering, then repeatedly spin coating, until film thickness reaches required thickness.Function film made from this method maintains good near-infrared shielding properties compared with common organic film, and thermal stability is remarkably improved.
Description
Technical field
The invention belongs to transparent figure layer technical fields, and in particular to a kind of tungsten bronze/silica dioxide gel heat insulating function material
Material and preparation method thereof.
Background technology
With increasing substantially for China's construction area, the building energy consumption problem brought therewith is increasingly severe, supplies the energy
Should and ecological environment all exert heavy pressures on.Currently, China's building energy consumption accounts for about the 30% of social total energy consumption.In these energy consumptions
In, the air conditioning energy consumption of the heating energy consumption of north of china in winter and southern summer account for major part.Door glass area accounts for about building external
The 30% of structural area is the main thoroughfare that building carries out energy exchange with environment, is the main portions for causing building energy consumption,
Energy dissipation accounts for about the 2/3 of building total energy consumption.Transparent heat-insulated material can keep visible light daylighting and the penetrating premise of vision
Under, the radiation of masking near infrared light (wave-length coverage 1000-2500nm), to reduce the intake of solar energy, then summer can be effective
Reduction air conditioning energy consumption, winter reduces indoor heat and spreads outward, realizes the purpose of building energy conservation.
In recent years, using nano-particle is dispersed in clear coat with obstruct the research of near infrared light have it is prodigious into
Exhibition is applied the energy expenditure that can reduce air-conditioning on the glass of building or automobile, and then reduces greenhouse gases
Discharge.Traditional Energy Saving Windows (electrochomeric glass, gas-discoloration glass etc.) have complicated structure, and it is defeated to also need to energy sometimes
Enter, the clear coat for being dispersed with near-infrared isolation nano-particle is relatively easy, more efficient at energy saving aspect.
Near-infrared masking material generally refers to have to be absorbed or reflection near infrared light and not influence its visible light saturating compared with strong
A kind of film material with function crossed.More well-known near-infrared screen nano material has following a few classes：Noble metal (Ag, Au
Deng), conductor oxidate (ATO, ITO etc.), rare-earth hexboride compound (LaB6, PrB6, NdB6).Surface plasma resonance makes this
A little nano materials have the property of shielding near-infrared, but each has advantage and disadvantage again：Film containing noble metal exists
The transmitance of visible light region is relatively low；ATO, ITO stablize and have in visible light region very high transmitance relatively, but they are only
The near infrared light that wavelength is more than 1500nm can effectively be covered；Hexaboride heat-barrier material can only shield the near-infrared of certain section of wavelength
Light, and since rare-earth hexboride compound hardness is larger, must be ground in preparation process.
Tungsten bronze (MxWO3, M Na+, K+,Rb+,Cs+And NH4 +) had in recent years as most promising heatshield material
Report, visible light transmittance are high, can cover the near infrared light that wavelength is more than 1000nm, thus with more excellent close red
Outer screening performance.In existing technology, Chinese patent CN104528829A discloses caesium tungsten bronze raw powder's production technology；And
Chinese patent CN104726040A discloses a kind of preparation method of the PVB slurries containing tungsten bronze；Xiaoyong Wu etc.
(Nanoscale.2015.7(40):17048-17054.) prepare novel CsxWO3/ ZnO smart window coating materials, not only have
There is excellent heat-proof quality, moreover it is possible to the harmful NO gases in air be catalytically decomposed under the action of light, but technique is relative complex；
In addition Jingxiao Liu et al. (Applied Surface Science.2014.309:175-180.) elaborate the choosing of dispersant
Select has very important influence to the near-infrared shielding properties of tungsten bronze nano-particle.
Invention content
For the deficiency of existing issue, the object of the present invention is to provide a kind of tungsten bronze/silica dioxide gel heat insulating functions
Material and preparation method thereof；The present invention is directed to prepare the transparent heat-insulated coating haveing excellent performance, while optimizing manufacture craft, improves
The thermal stability of clear coat reduces application cost.
The present invention solve its technical problem the technical solution adopted is that：
A kind of tungsten bronze/silica dioxide gel heat-insulation functional material, using silica and tungsten bronze as primary raw material, by matter
100% silica of score is measured, 10-15% tungsten bronzes are combined.
As the optimal technical scheme of the application, the silica is to use sol-gel legal system through catalyst
, any one of catalyst in hydrochloric acid, sulfuric acid or ammonium hydroxide.
The preparation method of above-mentioned tungsten bronze/silica dioxide gel heat-insulation functional material, includes the following steps：
(1) by volume 1:1 takes ethyl orthosilicate and absolute ethyl alcohol to be mixed, and is heated to reflux, adds catalyst, continues
The back flow reaction 2h at 70-80 DEG C more than closed ageing is for 24 hours diluted with liquid alcohol, is stirred, use is micro- at room temperature after reaction
Membrane filtration is filtered in hole, obtains silica dioxide gel；
(2) it weighs tungsten bronze nano-particle to be scattered in ethyl alcohol, grinding, ultrasound, are then stirred with silica dioxide gel respectively
Mixing is mixed, functional paint is obtained；
(3) clean glass substrate is taken, functional paint coating obtained by step (2) is on the glass substrate, natural at room temperature
It is dry, 200 DEG C of sintering are then warming up to the heating rate of 1 DEG C/min；
(4) step (3) is repeated, until gained film reaches the thickness of requirement on glass substrate.
As the optimal technical scheme of the application, tungsten bronze nano-particle is CsxWO3 in the step (2), specific to prepare
Method is as follows：
(1) tungsten chloride is dissolved in absolute ethyl alcohol, is vigorously stirred, obtain yellow solution, a hydronium(ion) is then added
Cesium oxide waits for solution after mixing, and acetic acid is added；
(2) gained precursor solution is transferred in autoclave, is reacted at 160-240 DEG C；Gained navy blue is produced
After product are centrifuged, washed respectively with water and ethyl alcohol, be finally dried in vacuo again to get.
As the optimal technical scheme of the application, the glass substrate in the step (3) uses absolute ethyl alcohol ultrasound clear first
It washes, sulfuric acid cleaned, surface hydroxylation, last deionized water is then used to be cleaned by ultrasonic.
As the optimal technical scheme of the application, catalyst is hydrochloric acid in the step (1), a concentration of 0.01mol/L.
As the optimal technical scheme of the application, the alcohol selected in the step (1) is ethyl alcohol or ethylene glycol.
As the optimal technical scheme of the application, painting method is spin-coating method or extraction in the step (3).
When preferably, using spin-coating method, rotating speed 3000r/min, time 20s.
Tungsten bronze provided by the invention/silica dioxide gel heat-insulation functional material and preparation method thereof, with prior art phase
Than having the advantages that：
(1) silica dioxide gel of the invention with tungsten bronze is compound prepares function film on the glass substrate, due to SiO2
Smooth, fine and close, defect the is seldom characteristic of gel mould, compared with common organic film, sintered silica membrane has preferably
Thermal stability；
(2) present invention goes out to prepare SiO by experimental exploring2The optimum process of gel mould changes titanium dioxide on this basis
The proportioning of silicon and tungsten bronze nano-particle, finally found that can be by the transmitance of 1200nm wavelength near infrared lights by 90% in tungsten bronze
It is reduced to 10%.
Description of the drawings
Fig. 1 is the UV-Vis-NIR spectrograms of the glass coated with tungsten bronze/silica dioxide gel function film.It is wherein bent
What line a was indicated is the near-infrared shielding properties figure of embodiment 1；What curve b was indicated is the near-infrared shielding properties figure of embodiment 2；
What curve c was indicated is the near-infrared shielding properties figure of embodiment 3；Curve d is the transmitance of the silica dioxide gel coating of blank
Curve；
Fig. 2 be embodiment 2 tungsten bronze/silica dioxide gel function film SEM figure (be followed successively by 1200X from left to right,
100000X)。
Specific implementation mode
The present invention is described in further details with reference to embodiments.Production is not specified in agents useful for same or instrument and equipment
Manufacturer, it is accordingly to be regarded as the conventional products that can be bought by market.
Embodiment 1：
(1) it takes 5ml ethyl orthosilicates and 5ml absolute ethyl alcohols to be mixed, 1.61ml0.1mol/L is added dropwise after being heated to reflux
Dilute hydrochloric acid, continue at 70 DEG C back flow reaction 2h；Closed ageing is 1 with volume ratio for 24 hours at room temperature after reaction:3 second
Alcohol dilutes, and stirring 10min obtains SiO with the micro porous filtration membrane filtration of 0.2um2Gel；
(2) 0.05g Cs are weighedxWO3Nano-particle is scattered in ethyl alcohol, respectively grinding, ultrasound 3 times, then with SiO2It is solidifying
Glue is stirred, CsxWO3Mass fraction be 10%, obtain functional paint；
(3) clean glass substrate is taken, on the glass substrate by functional paint spin coating；Spin coating rotating speed 3000r/min, time
20s；The glass plate of function film is coated in natural drying at room temperature, 200 DEG C of burnings are then warming up to the heating rate of 1 DEG C/min
Knot；
(4) step 3 is repeated, until gained film reaches the thickness of requirement on glass plate；The near-infrared screen of last test glass
Cover performance.
In the transmittance curve of glass coating made from the method such as Fig. 1 shown in curve a, it is seen that light transmission rate 52%,
Near infrared light transmitance is about 17%.
Embodiment 2：
(1) it takes 5ml ethyl orthosilicates and 5ml absolute ethyl alcohols to be mixed, 1.61ml0.1mol/L is added dropwise after being heated to reflux
Dilute hydrochloric acid, continue at 80 DEG C back flow reaction 2h；Closed ageing is 1 with volume ratio for 24 hours at room temperature after reaction:2 second
Alcohol dilutes, and stirring 10min obtains SiO with the micro porous filtration membrane filtration of 0.2um2Gel；
(2) 0.05g tungsten bronze nano-particles are weighed to be scattered in ethyl alcohol, respectively grinding, ultrasound 3 times, then with SiO2It is solidifying
Glue is stirred, CsxWO3Mass fraction be 15%, obtain functional paint；
(3) clean glass substrate is taken, on the glass substrate by functional paint spin coating；Spin coating rotating speed 2000r/min, time
20s；The glass plate of function film is coated in natural drying at room temperature, 200 DEG C of burnings are then warming up to the heating rate of 1 DEG C/min
Knot；
(4) step 3 is repeated, until gained film reaches the thickness of requirement on glass plate；The near-infrared screen of last test glass
Cover performance.
In the transmittance curve of glass coating made from the method such as Fig. 1 shown in curve b, it is seen that light transmission rate 63%,
Near infrared light transmitance is about 7%.
Embodiment 3：
(1) it takes 5ml ethyl orthosilicates and 5ml absolute ethyl alcohols to be mixed, 1.61ml0.1mol/L is added dropwise after being heated to reflux
Dilute hydrochloric acid, continue at 70 DEG C back flow reaction 2h；Closed ageing is 1 with volume ratio for 24 hours at room temperature after reaction:3 second
Alcohol dilutes, and stirring 10min obtains SiO with the micro porous filtration membrane filtration of 0.2um2Gel；
(2) 0.05g tungsten bronze nano-particles are weighed to be scattered in ethyl alcohol, respectively grinding, ultrasound 3 times, then with SiO2It is solidifying
Glue is stirred, CsxWO3Mass fraction be 15%, obtain functional paint；
(3) clean glass substrate is taken, on the glass substrate by functional paint spin coating；Spin coating rotating speed 3000r/min, time
20s；The glass plate of function film is coated in natural drying at room temperature, 200 DEG C of burnings are then warming up to the heating rate of 1 DEG C/min
Knot；
(4) step 3 is repeated, until gained film reaches the thickness of requirement on glass plate；The near-infrared screen of last test glass
Cover performance.
In the transmittance curve of glass coating made from the method such as Fig. 1 shown in curve c, it is seen that light transmission rate 71%,
Near infrared light transmitance is about 6%；The scanning electron microscope (SEM) photograph of coating is as shown in Figure 2 on glass plate, it can be seen that coating is smooth, causes
Close, defect is less.
Embodiment 4：
(1) it takes 5ml ethyl orthosilicates and 5ml absolute ethyl alcohols to be mixed, 1.61ml0.1mol/L is added dropwise after being heated to reflux
Dilute hydrochloric acid, continue at 70 DEG C back flow reaction 2h；Closed ageing is 1 with volume ratio for 24 hours at room temperature after reaction:3 second
Alcohol dilutes, and stirring 10min obtains silica dioxide gel with the micro porous filtration membrane filtration of 0.2um；
(2) clean glass substrate is taken, on the glass substrate by silica dioxide gel spin coating；Spin coating rotating speed 3000r/min,
Time 20s；The glass plate of function film is coated in natural drying at room temperature, is then warming up to 200 DEG C with the heating rate of 1 DEG C/min
Sintering；
(4) step 3 is repeated, until gained film reaches the thickness of requirement on glass plate；The near-infrared screen of last test glass
Cover performance.
It is merely coated with made from the method in the transmittance curve such as Fig. 1 of the glass coating of silica dioxide gel shown in curve d,
Visible light transmittance is close to 90%, and near infrared light transmitance is higher than 90%, and the peak occurred between wherein 800-900nm is when measuring
Instrument automatically switches caused by light source.
The protection content of the present invention is not limited to above example.Without departing from the spirit and scope of the invention, originally
Field technology personnel it is conceivable that variation and advantage be all included in the present invention, and with the attached claims be protection
Range.
Claims (9)
1. a kind of tungsten bronze/silica dioxide gel heat-insulation functional material, which is characterized in that with silica and tungsten bronze be main
Raw material, by 100% silica of mass fraction, 10-15% tungsten bronzes are combined.
2. tungsten bronze according to claim 1/silica dioxide gel heat-insulation functional material, which is characterized in that the dioxy
SiClx is made using sol-gel method, any one of catalyst in hydrochloric acid, sulfuric acid or ammonium hydroxide through catalyst.
3. the preparation method of tungsten bronze described in claim 1/silica dioxide gel heat-insulation functional material, which is characterized in that packet
Include following steps：
(1) by volume 1:1 takes ethyl orthosilicate and absolute ethyl alcohol to be mixed, and is heated to reflux, adds catalyst, continues
Back flow reaction 2h at 70-80 DEG C more than closed ageing is for 24 hours diluted with liquid alcohol at room temperature after reaction, stirs, use micropore
Membrane filtration is filtered, silica dioxide gel is obtained；
(2) it weighs tungsten bronze nano-particle to be scattered in ethyl alcohol, respectively grinding, ultrasound, it is then mixed with silica dioxide gel stirring
It closes, obtains functional paint；
(3) clean glass substrate is taken, functional paint coating obtained by step (2) on the glass substrate, is spontaneously dried at room temperature,
Then heating sintering；
(4) step (3) is repeated, until gained film reaches the thickness of requirement on glass substrate.
4. the preparation method of tungsten bronze according to claim 3/silica heat-insulation functional material, which is characterized in that institute
It is CsxWO3 to state tungsten bronze nano-particle in step (2), and specific preparation method is as follows：
(1) tungsten chloride is dissolved in absolute ethyl alcohol, is vigorously stirred, obtain yellow solution, hydronium(ion) oxidation is then added
Caesium waits for solution after mixing, and acetic acid is added；
(2) gained precursor solution is transferred in autoclave, is reacted at 160-240 DEG C；Gained navy blue product passes through
After centrifugation, washed respectively with water and ethyl alcohol, be finally dried in vacuo again to get.
5. the preparation method of tungsten bronze according to claim 3/silica heat-insulation functional material, which is characterized in that institute
The glass substrate stated in step (3) is cleaned by ultrasonic with absolute ethyl alcohol first, is then used sulfuric acid cleaned, surface hydroxylation, is finally gone
Ionized water is cleaned by ultrasonic.
6. the preparation method of tungsten bronze according to claim 3/silica heat-insulation functional material, which is characterized in that institute
It is hydrochloric acid to state catalyst in step (1), a concentration of 0.01mol/L.
7. the preparation method of tungsten bronze according to claim 3/silica heat-insulation functional material, which is characterized in that institute
It is ethyl alcohol or ethylene glycol to state the alcohol selected in step (1).
8. the preparation method of tungsten bronze according to claim 3/silica heat-insulation functional material, which is characterized in that institute
It is spin-coating method or extraction to state painting method in step (3).
9. the preparation method of tungsten bronze according to claim 8/silica heat-insulation functional material, which is characterized in that make
When with spin-coating method, rotating speed 3000r/min, time 20s.
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| CN110154182A (en) * | 2019-06-10 | 2019-08-23 | 浙江农林大学 | A kind of bionical live standing tree generates the preparation method of negative oxygen ion engineered wood |
| CN111589382A (en) * | 2020-05-14 | 2020-08-28 | 大连工业大学 | Ptn-MxWO3/SiO2Composite aerogel and preparation method thereof |
| CN112573925A (en) * | 2021-02-22 | 2021-03-30 | 山东合创明业精细陶瓷有限公司 | High-performance electromagnetic shielding NdB6/SiO2Complex phase ceramic material and preparation method thereof |
| CN115011148A (en) * | 2022-04-28 | 2022-09-06 | 中国科学院合肥物质科学研究院 | Sprayable solar photo-thermal conversion functional gel and preparation method and application thereof |
| CN115449254A (en) * | 2022-09-22 | 2022-12-09 | 华南理工大学 | Cesium tungsten bronze/silicon dioxide hollow microsphere composite material and preparation method and application thereof |
| CN115491791A (en) * | 2022-09-29 | 2022-12-20 | 中国人民解放军海军工程大学 | Preparation method of silicon dioxide/cesium tungsten bronze near-infrared shielding composite fiber |
| CN116553836A (en) * | 2023-07-08 | 2023-08-08 | 内蒙古科技大学 | Tungsten bronze doped heat insulation glass and preparation method thereof |
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| CN115491791A (en) * | 2022-09-29 | 2022-12-20 | 中国人民解放军海军工程大学 | Preparation method of silicon dioxide/cesium tungsten bronze near-infrared shielding composite fiber |
| CN116553836A (en) * | 2023-07-08 | 2023-08-08 | 内蒙古科技大学 | Tungsten bronze doped heat insulation glass and preparation method thereof |
| CN116553836B (en) * | 2023-07-08 | 2023-09-22 | 内蒙古科技大学 | Tungsten bronze doped heat insulation glass and preparation method thereof |
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