CN103102083A - Preparation method of nano antimony tin oxide transparent insulation film - Google Patents
Preparation method of nano antimony tin oxide transparent insulation film Download PDFInfo
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- CN103102083A CN103102083A CN2013100597450A CN201310059745A CN103102083A CN 103102083 A CN103102083 A CN 103102083A CN 2013100597450 A CN2013100597450 A CN 2013100597450A CN 201310059745 A CN201310059745 A CN 201310059745A CN 103102083 A CN103102083 A CN 103102083A
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- 238000009413 insulation Methods 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- SKRWFPLZQAAQSU-UHFFFAOYSA-N stibanylidynetin;hydrate Chemical compound O.[Sn].[Sb] SKRWFPLZQAAQSU-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 32
- 239000011521 glass Substances 0.000 claims abstract description 29
- 239000002002 slurry Substances 0.000 claims abstract description 26
- 238000000576 coating method Methods 0.000 claims abstract description 23
- 239000004814 polyurethane Substances 0.000 claims abstract description 23
- 229920002635 polyurethane Polymers 0.000 claims abstract description 22
- 239000011248 coating agent Substances 0.000 claims abstract description 18
- 239000006185 dispersion Substances 0.000 claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 10
- 238000004528 spin coating Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract 3
- 239000002270 dispersing agent Substances 0.000 claims abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000000498 ball milling Methods 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- 239000013530 defoamer Substances 0.000 claims description 7
- 230000008719 thickening Effects 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 4
- 239000011324 bead Substances 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 239000003973 paint Substances 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- 238000002955 isolation Methods 0.000 claims 2
- GVFOJDIFWSDNOY-UHFFFAOYSA-N antimony tin Chemical group [Sn].[Sb] GVFOJDIFWSDNOY-UHFFFAOYSA-N 0.000 claims 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Natural products OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical group CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims 1
- 238000004506 ultrasonic cleaning Methods 0.000 claims 1
- 238000002156 mixing Methods 0.000 abstract description 6
- 230000004888 barrier function Effects 0.000 abstract description 4
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000002518 antifoaming agent Substances 0.000 abstract 1
- 238000007611 bar coating method Methods 0.000 abstract 1
- 239000011858 nanopowder Substances 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 239000002562 thickening agent Substances 0.000 abstract 1
- 238000002834 transmittance Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 8
- 238000004140 cleaning Methods 0.000 description 6
- 230000001276 controlling effect Effects 0.000 description 5
- 238000002791 soaking Methods 0.000 description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000003125 aqueous solvent Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000000411 transmission spectrum Methods 0.000 description 2
- 240000007762 Ficus drupacea Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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Abstract
The invention discloses a preparation method of a nano antimony tin oxide (ATO) transparent insulation film. The method comprises following steps: 1) preparation of a nano ATO slurry: mixing an ATO nanopowder and a dispersant according to proportion and stirring thoroughly, and regulating a pH value to prepare the nano ATO slurry; 2) preparation of a nano ATO thermal insulation coating: mixing the nano ATO slurry and aqueous polyurethane, adjusting a pH value, adding a leveling agent, a defoaming agent and a thickener for dispersion, so as to prepare a nano thermal insulation coating; and 3) preparation of a transparent insulation film: immersing a clean glass substrate in the prepared nano thermal insulation coating liquid, and preparing a transparent film on the glass substrate by using a spin coating method / Czochralski method / bar coating method. The nano ATO transparent thermal insulation film prepared by the method provided by the invention has high visible light transmittance and infrared barrier property, and is suitable for building thermal insulation glass. The film preparation process is simple, environment-friendly, low-cost, and can form a uniform film with large area.
Description
Technical field
The invention belongs to nano insulating glass technical field for building, be specially a kind of preparation method of nano antimony tin oxide transparent heat insulation diaphragm.
Background technology
Growing tension along with Energy resources, China has made take less energy-consumption, low has polluted, low emission is the Development patterns of the low-carbon economy on basis, building energy conservation is the important component part of low-carbon economy industry development, at present, heat-insulating glass mainly contains double glazing, vacuum glass, Low-E glass, solar-control glazing and pad pasting glass etc., the price of these glass is numerous and diverse due to technique, the expensive large-scale application that is difficult to, so simple, the cheap high-quality transparent heat insulating glass of development technology is still one of focus of research.The material of suitable preparation transparent heat insulating glass should be chosen has optionally semiconductor material to solar spectrum, as indium tin oxide target (ITO) and tin-antiomony oxide (ATO), wherein the deposit due to indium raw material in ITO reduces day by day, price is high, and the ATO cost is relatively low, and application prospect is comparatively wide.Nano ATO is a kind of common semiconductor material, and its film has higher visible light transmissivity and infrared barrier, and nano ATO is applied to prepare in coating transparent heat insulation diaphragm, has a high using value heat-insulating is on glass.
The method for preparing the nano ATO film in prior art has: direct current magnetron sputtering process, chemical Vapor deposition process, electron-beam vapor deposition method and sol-gel method etc., these preparation methods exist that equipment requirements is high, the film particles yardstick is difficult to control and can't the Large-Area-Uniform film forming etc. shortcoming, and the nano ATO powder is directly applied in coating, be well dispersed in aqueous solvent by ball milling, ultrasonic, high-speed stirring, making the ATO nano paint and film, is that a kind of simple and convenient preparation has the method for the thermal insulation film consistent with coating property.In preparation process, owing to having used aqueous solvent, avoided the pollution of organic solvent to environment, prepared nano ATO slurry and aqueous polyurethane are a kind of transparent heat insulating dopes, have with low cost, the advantages such as manufacture craft simple, easy construction.Utilize spin-coating method/crystal pulling method/line rod coating method to film and can not only guarantee that prepared film particle diameter is consistent with raw material, thickness is controlled, but and the simple Large-Area-Uniform film forming of equipment.The standby transparent heat insulation diaphragm of this legal system has good effect of heat insulation, high visible light transmissivity, has good market outlook and high promotional value in the building glass field.
Summary of the invention
The object of the invention is to propose a kind of simple, cost is low, efficient is high method for preparing the nano antimony tin oxide transparent heat insulation diaphragm.
the present invention is a kind of preparation method of nano antimony tin oxide transparent heat insulation diaphragm, concrete steps are: by certain dispersion agent (dehydrated alcohol, deionized water or propyl carbinol) mix than fully with the nano ATO powder, regulating the pH value of mixture is advisable at 7～8 meta-alkalescences, mixture is put into ball mill, disperse in ultra-sonic generator or magnetic stirring apparatus, add simultaneously stablizer, obtain scattered nano ATO slurry system, wherein the ball milling ball is the agate bead of diameter 2～2.8 cm, rotating speed is 250r/min, Ball-milling Time is more than 4h, the ultrasonic generator frequency is 20000Hz, magnetic agitation speed is 100 r/min.The nano ATO slurry that makes is mixed with aqueous polyurethane, regulate pH value 7～8, carry out again ball milling, ultrasonic or magnetic stirring apparatus fully disperses, in dispersion process, defoamer, flow agent, thickening material are added in aqueous polyurethane according to 0.1wt%, 4wt%, 0.2wt% respectively successively, make the nano ATO thermal insulating coating.To clean 15 min in acetone, dehydrated alcohol and deionized water for ultrasonic respectively with the common slide glass that the NaOH solution soaking is crossed, utilize spin-coating method, crystal pulling method or line rod coating method, directly plated film on the substrate of glass of cleaning, control certain thickness and be prepared into the nano antimony tin oxide transparent heat insulation diaphragm.
Beneficial effect of the present invention:
The prepared film of the present invention has high visible light transmissivity and infrared barrier, but the simple environmental protection of preparation process technique, the low Large-Area-Uniform film forming of cost is applicable to heat-insulating glass.
The present invention adopts nano ATO powder and aqueous polyurethane to be mixed with the nano ATO thermal insulating coating, has avoided traditional coating with an organic solvent to pollute.
In the present invention prepared film be under room temperature on the substrate of glass of cleaning plated film, do not need high temperature, equipment is simple and easy to implement.
Film prepared in the present invention can form dry film at physical environment as required, and also temperature controllable is from room temperature 25
oC to 80
oC is dried in baking oven.
In the present invention, the transparency of prepared film, the thickness when volume ratio that can be by controlling different nano ATO slurries and aqueous polyurethane and plated film regulates and controls.
Test-results shows, but having, preparation method of the present invention do not need high vacuum, heat, the simple Large-Area-Uniform film forming of equipment, low cost and other advantages, prepared nano ATO transparent heat insulation diaphragm has higher visible light transmissivity and infrared barrier, aspect heat-insulating glass, have good market outlook and using value.
Description of drawings
Fig. 1 is the preparation flow figure of nano ATO slurry in embodiment 1.
Fig. 2 is the preparation flow figure of nano ATO thermal insulating coating in embodiment 1.
Fig. 3 is the XRD figure spectrum of the nano ATO thermal insulation film of embodiment 2 preparations.
Fig. 4 is the SEM figure of the nano ATO thermal insulation film of embodiment 2 preparations.
Fig. 5 is the Visible-to-Near InfaRed transmission spectrum of the nano ATO film prepared of embodiment 3.
Embodiment
Further describe the present invention below by specific embodiment:
Embodiment 1, the nano ATO powder is joined in the dispersion agent dehydrated alcohol, regulate the pH value at 7～8 meta-alkalescences, abundant dispersing and mixing, mixture is put into ball mill ball milling 20 h, add simultaneously stablizer, obtain scattered nano ATO slurry system, wherein the ball milling ball is the agate bead of diameter 2～2.8 cm, and rotating speed is 250 r/min.The nano ATO slurry and the aqueous polyurethane that make are V by volume
Nano ATO slurry: V
Aqueous polyurethane=1:4 mixes, and controlling the pH value is 7～8, then carries out Ball milling, in dispersion process, defoamer, flow agent, thickening material is added in aqueous polyurethane according to 0.1wt%, 4wt%, 0.2wt% respectively successively, makes the nano ATO thermal insulating coating.The common slide glass that to cross with the NaOH solution soaking cleans 15 min in acetone, dehydrated alcohol and deionized water for ultrasonic respectively, utilizes crystal pulling method, lifts plated film on the substrate of glass of cleaning, can change to lift number of times and control thickness, after plated film, uses baking oven 80
oThe dry 3h of C can get the nano antimony tin oxide transparent heat insulation diaphragm.Fig. 1 is the preparation flow figure of nano ATO slurry.Fig. 2 is the preparation flow figure of nano ATO thermal insulating coating.
Embodiment 2, the nano ATO powder is joined in the dispersion agent propyl carbinol, regulate the pH value at 7～8 meta-alkalescences, abundant dispersing and mixing, mixture is inserted carry out ultra-sonic dispersion 40 min in ultra-sonic generator, add simultaneously stablizer, obtain scattered nano ATO slurry system, wherein the ultrasonic generator frequency is 20000Hz.The nano ATO slurry and the aqueous polyurethane that make are V by volume
Nano ATO slurry: V
Aqueous polyurethane=1:6 mixes, and controlling the pH value is 7～8, then carries out Ball milling, in dispersion process, defoamer, flow agent, thickening material is added in aqueous polyurethane according to 0.1wt%, 4wt%, 0.2wt% respectively successively, makes the nano ATO thermal insulating coating.The common slide glass that to cross with the NaOH solution soaking cleans 15 min in acetone, dehydrated alcohol and deionized water for ultrasonic respectively, utilizes crystal pulling method, lifts plated film on the substrate of glass of cleaning, can change to lift number of times and control thickness, after plated film, uses baking oven 80
oThe dry 3h of C can get the nano antimony tin oxide transparent heat insulation diaphragm, and prepared film thickness is 10 μ m.Fig. 3 is the XRD figure spectrum of the nano ATO thermal insulation film of preparation, and Fig. 4 is the SEM figure of the nano ATO thermal insulation film of preparation.
Embodiment 3, the nano ATO powder is joined in the dispersion agent propyl carbinol, regulate the pH value at 7～8 meta-alkalescences, abundant dispersing and mixing, mixture is put into ball mill ball milling 24h, add simultaneously stablizer, obtain scattered nano ATO slurry system, wherein the ball milling ball is the agate bead of diameter 2～2.8 cm, and rotating speed is 250 r/min.The nano ATO slurry and the aqueous polyurethane that make are respectively V by volume
Nano ATO slurry: V
Aqueous polyurethane=1:1,1:2,1:3,1:4,1:6 mix, controlling the pH value is 7～8, carry out again Ball milling, in dispersion process, defoamer, flow agent, thickening material are added in aqueous polyurethane according to 0.1wt%, 4wt%, 0.2wt% respectively successively, make the nano ATO thermal insulating coating.To clean 15 min in acetone, dehydrated alcohol and deionized water for ultrasonic respectively with the common slide glass that the NaOH solution soaking is crossed, and utilize line rod coating method, plated film on the substrate of glass of cleaning uses baking oven 80
oThe dry 3h of C can get the nano antimony tin oxide transparent heat insulation diaphragm.Fig. 5 is the Visible-to-Near InfaRed transmission spectrum of the nano ATO film prepared, at V
Nano ATO slurry: V
Aqueous polyurethaneDuring=1:6, film has higher transmission of visible light and lower ir transmissivity, and transmission of visible light is more than 80%.
Embodiment 4, and the nano ATO powder is joined in the dispersion agent deionized water, regulate the pH value at 7～8 meta-alkalescences, and fully dispersing and mixing, put into stirrer and carry out 60 in mixture
oC magnetic agitation 12h adds stablizer simultaneously, obtains scattered nano ATO slurry system.The nano ATO slurry and the aqueous polyurethane that make are V by volume
Nano ATO slurry: V
Aqueous polyurethane=1:10 mixes, and controlling the pH value is 7～8, then carries out magnetic agitation and disperse, and in dispersion process, defoamer, flow agent, thickening material is added in aqueous polyurethane according to 0.1wt%, 4wt%, 0.2wt% respectively successively, makes the nano ATO thermal insulating coating.To clean 15 min in acetone, dehydrated alcohol and deionized water for ultrasonic respectively with the common slide glass that the NaOH solution soaking is crossed, and utilize spin-coating method, plated film on the substrate of glass of cleaning uses baking oven 80
oThe dry 3h of C can get the nano antimony tin oxide transparent heat insulation diaphragm.
Claims (10)
1. the preparation method of a nano antimony tin oxide transparent heat insulation diaphragm is characterized in that the method comprises the following steps:
At first, with nano ATO powder and dispersant, regulate the pH value, use Ball milling, ultra-sonic dispersion or magnetic stirring apparatus to disperse, get nano ATO slurry; Then, the ATO nano pulp is mixed with aqueous polyurethane, add flow agent, defoamer, thickening material to disperse again to make nanometer heat isolation paint liquid; At last, the glass-based that cleans up is immersed in prepared nanometer heat isolation paint liquid, utilizes spin-coating method, crystal pulling method or line rod coating method to prepare transparent heat insulation diaphragm on substrate of glass.
2. the preparation method of a kind of nano antimony tin oxide transparent heat insulation diaphragm according to claim 1, it is characterized in that: the grain diameter of nano ATO powder is 20～100 nm, the tin antimony atoms is than being 90:10 or 95:5.
3. the preparation method of a kind of nano antimony tin oxide transparent heat insulation diaphragm according to claim 1, it is characterized in that: dispersion agent refers to dehydrated alcohol, propyl carbinol or deionized water, use Ball milling, ultra-sonic dispersion or magnetic stirring apparatus to disperse in dispersion process, wherein the ball milling ball is the agate bead of diameter 2～2.8cm, and rotating speed is 250 r/min; The ultrasonic generator frequency is 20000 Hz; Magnetic agitation speed is 100 r/min.
4. the preparation method of a kind of nano antimony tin oxide transparent heat insulation diaphragm according to claim 1, it is characterized in that: the pH value of nano ATO slurry is controlled at 7～8.
5. the preparation method of a kind of nano antimony tin oxide transparent heat insulation diaphragm according to claim 1, it is characterized in that: nano ATO paint is the coating that nano ATO slurry and aqueous polyurethane are mixed with, and the volume ratio of nano ATO slurry and aqueous polyurethane is adjustable between 1:1～1:10.
6. the preparation method of a kind of nano antimony tin oxide transparent heat insulation diaphragm according to claim 1, it is characterized in that: used flow agent, defoamer and thickening material in the coating dispersion process, added in aqueous polyurethane according to 0.1wt%, 4wt%, 0.2wt% successively respectively.
7. the preparation method of a kind of nano antimony tin oxide transparent heat insulation diaphragm according to claim 1, is characterized in that: control the pH value 7～8 in the coating dispersion process.
8. the preparation method of a kind of nano antimony tin oxide transparent heat insulation diaphragm according to claim 1, it is characterized in that: prepared nano ATO transparent heat insulation diaphragm substrate is slide glass, first soak rear acetone, dehydrated alcohol and the deionized water ultrasonic cleaning 15min of using respectively through the NaOH dilute solution.
9. the preparation method of a kind of nano antimony tin oxide transparent heat insulation diaphragm according to claim 1 is characterized in that: adopt spin-coating method, crystal pulling method or line rod coating method to prepare film, the thickness of film can regulate and control between 100nm～100 μ m.
10. the preparation method of a kind of nano antimony tin oxide transparent heat insulation diaphragm according to claim 1 is characterized in that: prepared nano ATO transparent heat-insulated thin in the visible region transmissivity more than 80%, in the transmissivity of near-infrared region below 20%.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104017474A (en) * | 2014-05-12 | 2014-09-03 | 南昌大学 | Nano ATO/TiO2 Filler Waterborne Polyurethane Thermal Insulation Transparent Coating |
| CN105505174A (en) * | 2016-01-27 | 2016-04-20 | 柳州豪祥特科技有限公司 | Method for preparing ATO heat insulation film |
| CN105524538A (en) * | 2016-01-27 | 2016-04-27 | 柳州豪祥特科技有限公司 | Method for preparing ATO thermal insulation coating with jetting method |
| CN105521936A (en) * | 2016-01-27 | 2016-04-27 | 柳州豪祥特科技有限公司 | Preparation method for ATO heat insulation thin film coating |
| CN105602427A (en) * | 2016-01-27 | 2016-05-25 | 柳州豪祥特科技有限公司 | Preparation method of ATO thermal insulation coating |
| CN106243959A (en) * | 2016-08-12 | 2016-12-21 | 杨秀枝 | A kind of fenestrated membrane polyurethane insulating moulding coating and preparation method thereof |
| CN106634500A (en) * | 2016-09-19 | 2017-05-10 | 深圳市文浩科技有限公司 | Insulation coating for glass and application method thereof |
| CN106987248A (en) * | 2017-04-10 | 2017-07-28 | 江南大学 | A kind of up-conversion based on tin-antiomony oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104017474A (en) * | 2014-05-12 | 2014-09-03 | 南昌大学 | Nano ATO/TiO2 Filler Waterborne Polyurethane Thermal Insulation Transparent Coating |
| CN105505174A (en) * | 2016-01-27 | 2016-04-20 | 柳州豪祥特科技有限公司 | Method for preparing ATO heat insulation film |
| CN105524538A (en) * | 2016-01-27 | 2016-04-27 | 柳州豪祥特科技有限公司 | Method for preparing ATO thermal insulation coating with jetting method |
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Application publication date: 20130515 |