CN106431000A - Oxide film of porous structure and preparation method and application of oxide film - Google Patents
Oxide film of porous structure and preparation method and application of oxide film Download PDFInfo
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- CN106431000A CN106431000A CN201510483224.7A CN201510483224A CN106431000A CN 106431000 A CN106431000 A CN 106431000A CN 201510483224 A CN201510483224 A CN 201510483224A CN 106431000 A CN106431000 A CN 106431000A
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- sull
- substrate
- loose structure
- crystal grain
- oxide film
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 35
- 239000013078 crystal Substances 0.000 claims abstract description 30
- 239000011248 coating agent Substances 0.000 claims abstract description 13
- 238000000576 coating method Methods 0.000 claims abstract description 13
- 230000007704 transition Effects 0.000 claims abstract description 6
- 239000012212 insulator Substances 0.000 claims abstract description 5
- 229910021542 Vanadium(IV) oxide Inorganic materials 0.000 claims description 19
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 claims description 19
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- 238000002425 crystallisation Methods 0.000 claims description 12
- 230000008025 crystallization Effects 0.000 claims description 12
- 239000010409 thin film Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 9
- 239000012530 fluid Substances 0.000 claims description 9
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 8
- 229910000077 silane Inorganic materials 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 238000004134 energy conservation Methods 0.000 claims description 6
- 239000004094 surface-active agent Substances 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 5
- -1 octadecyl trichlorosilane alkane Chemical class 0.000 claims description 5
- 229920002521 macromolecule Polymers 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 239000002019 doping agent Substances 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 230000000873 masking effect Effects 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 238000004528 spin coating Methods 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 230000008859 change Effects 0.000 abstract description 5
- 238000002834 transmittance Methods 0.000 abstract 2
- 239000007788 liquid Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 12
- 239000010408 film Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 5
- 239000010410 layer Substances 0.000 description 4
- 239000004984 smart glass Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000000584 ultraviolet--visible--near infrared spectrum Methods 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- 230000001154 acute effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- UUUGYDOQQLOJQA-UHFFFAOYSA-L vanadyl sulfate Chemical compound [V+2]=O.[O-]S([O-])(=O)=O UUUGYDOQQLOJQA-UHFFFAOYSA-L 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Surface Treatment Of Glass (AREA)
Abstract
The invention discloses an oxide film of a porous structure. The oxide film comprises a substrate and oxide crystal grains covering the substrate; the oxide crystal grains are of crystal structures in metal-insulator transition and display regular annular structures, and the oxide crystal grains of the annular structures cover the substrate to form the continuous oxide film, wherein the inner diameter of the annular structures of the oxide crystal grains ranges from 30 nanometers to 3,000 nanometers. A preparation method of the oxide film comprises a step A of substrate pretreatment; a step B of coating liquid preparation; a step C of film preparation. The oxide film of the porous structure can be used for making building energy saving windows, windows of mobile transportation facilities, shun-shading canopies and the like. The oxide film has ultrahigh visible light transmittance, and the peak value exceeds 90% and reaches 97% to the maximum. Meanwhile, the oxide film of the porous structure has the characteristic of sun infrared light regulation controlled by temperature, and the solar energy transmittance change rate is larger than 4% at high and low temperature.
Description
Technical field
The invention belongs to energy-conservation and solar energy generation technology field, more particularly, to a kind of have sull of loose structure and its preparation method and application.
Background technology
Energy-conservation window setting technique be building and vehicle glass energy-conservation important way, but existing Energy Saving Windows typically only have adjust sunlight heat pass through function it is impossible to and electricity generation system, especially solar photovoltaic generation system combination, single function, comprehensive energy efficiency is relatively low.
Common window-glass power-saving technology generally relies on glass surface film layer, and this film layer can absorb, reflects or partially absorb part reflected sunlight, thus adjusting the transmitance of the especially infrared section of sunlight, reaches the purpose of energy-conservation.More satisfactory Energy Saving Windows include the smart window using technology such as the gentle causes of electroluminescent, thermic.These Energy Saving Windows can be passed through extra electric field, ambient temperature respectively or be passed through the gas and changing curve of spectrum, change the transmitance of infrared section.The material that these Energy Saving Windows realize energy-saving effect mainly includes macromolecule（Organic）, metal and metal-oxide and its mixture.Rutile Type（R phase）Vanadium dioxide is a kind of metal-oxide with thermal induced phase transition property.Occur by low temperature monoclinic phase at 68 DEG C（M phase）To high temperature Rutile Type（R phase）Reversible phase in version.Along with this structure change, all there is acute variation so as to have good application prospect in terms of smart window, thermistor material, infrared detecting materials in the physical property such as its electrical conductivity, susceptibility, light transmission rate.
The Chinese invention patent of Application No. CN201110027223.3 discloses a kind of preparation method of vanadium dioxide film, and it comprises the steps：1) by hydroxyl carboxylic acid in hydrogen peroxide, and it is more than 7 with the pH value that ammonia adjusts solution；It is subsequently adding vanadium oxysulfate, obtains reaction solution, after the completion of reaction, add organic solvent, standing, generate precipitation, precipitation separation, obtain the peroxide complex of vanadium；2) by step 1) peroxide complex of gained vanadium and being dissolved in the water formation aqueous solution with additive, by described aqueous solution plated film on substrate, then after heat treatment obtain vanadium dioxide film in an inert atmosphere.But the method that it adopts can only obtain continuously, dense film, related to this structure, the visible light transmissivity peak value of thin film is usually less than 70%, typically in 40-60% it is difficult to meet the high requests to visible light transmissivity such as its Herba Plantaginis gear.
Content of the invention
In order to solve the above-mentioned problems in the prior art, it is an object of the invention to provide a kind of sull with loose structure.By to the regulation and control of the grainiess of thin film with change grainiess, making the precursor film highly crystalline in noncrystalline state, and the circulus of monolayer alignment is formed on substrate, allow the crystalline state of circulus ensure that thin film has excellent temperature control phase-change characteristic（Metal-insulator phase transition）；Circulus makes thin film have regular porous feature, and visible light transmissivity is greatly improved.Additionally, monolayer alignment and porous character also make this thin film have from antireflection, both decrease visible reflectance, also further increase visible light transmissivity.
To achieve these goals, the technical solution used in the present invention is：A kind of sull with loose structure includes substrate and covers the oxide crystallization crystal grain on substrate；Described oxide crystallization crystal grain has the crystalline texture of metal-insulator phase transition, this oxide crystallization crystal grain is in the circulus of rule, and the oxide crystallization crystal grain of circulus covers and forms continuous sull on the substrate, wherein the internal diameter of the circulus of oxide crystallization crystal grain is 30-3000 nanometer.
Preferably technical scheme, described oxide crystallization crystal grain is vanadium dioxide crystal grain.
Further preferred technical scheme, the continuous sull thickness of described formation is less than 400 nanometers.
Technical scheme still more preferably, the continuous sull thickness of described formation is less than 100 nanometers.
Another object of the present invention is to provide a kind of preparation method of the sull with loose structure, and it comprises the following steps：
Step A, substrate pretreatment
A1, first by substrate cleaning post-drying；
A2, is reconfigured at the toluene solution of the surfactant containing silane, wherein silane contents are 0.5-5%；
A3, substrate is immersed in above-mentioned toluene solution to stand to take out after a period of time and cleans, dry 1-30 minute, hollowed-out mask is placed on substrate, formed standby after pattern structure after ultraviolet irradiation certain time under 120 degrees Celsius of temperature conditionss；
Step B, coating fluid make
B1, vanadium dioxide grain dispersion is become the aaerosol solution of aqueouss or Organic；
B2, adds macromolecule dispersing agent or the inorganic sol with cementation in above-mentioned aaerosol solution, that is, coating fluid is obtained；
Step C, masking
The above-mentioned coating fluid of last layer is coated on substrate using spin coating, blade coating, spraying or typography, after drying, that is, thin film is obtained.
In described step A, the time of standing is less than 2 hours.
Drying time in described step A3 is less than 10 minutes.
Ultraviolet irradiation time in described step A3 is less than 1 hour, and ultraviolet wavelength is less than 254 nanometers.
Described substrate adopts building glass；Described vanadium dioxide crystal grain is doping property vanadium dioxide crystal grain, and dopant ion is one or more of W, Mo, Ti, Mg, F；The described surfactant containing silane is octadecyl trichlorosilane alkane.
The a further object of the present invention is to provide a kind of application of the above-mentioned sull with loose structure, and this application is to be used for making the energy-saving solar products such as building energy conservation window, the window of destination, sunshading ceiling by the sull of this loose structure.
Using above technical scheme, the electricity conversion that the sull with loose structure of the present invention solves existing energy-saving power generation thin film is low, the problems such as energy-saving effect is bad.
The sull with loose structure of the present invention has superelevation visible light transmissivity compared with dense film of the prior art, peak value more than 90%, up to 97%；Meanwhile, this thin film has temperature controlled solar infrared light control characteristic.High/low temperature passes through solar energy rate of change and is more than 4%.
The thin film of the present invention, compared with existing smart window, has further the advantage that：
1. visible light transmissivity is high, or even more preferable than the substrate transparency of existing smart window；
2. its structure is simply it is easy to manufacture and industrialization.
Brief description
Fig. 1 is the principle schematic diagram. of the sull with loose structure being obtained in the embodiment of the present invention 1.
Fig. 2 is the surface texture schematic diagram of the mask in embodiment 1 used by the preparation method of the sull that the present invention has loose structure；
Fig. 3 is the ultraviolet-visible-near-infrared spectrum of the sull in the embodiment of the present invention 1 with loose structure.
Specific embodiment
For making the object, technical solutions and advantages of the present invention of greater clarity, with reference to instantiation, the present invention is described in more detail.It should be understood that these descriptions are simply exemplary, and it is not intended to limit the scope of the present invention.Additionally, in the following description, eliminate the description to known features and technology, to avoid unnecessarily obscuring idea of the invention.
Embodiment 1：
As shown in Figure 1 to Figure 3, a kind of preparation method of the sull with loose structure, it comprises the following steps：
Step A, substrate pretreatment
A1, first by substrate（Substrate adopts building glass）Clean post-drying；
A2, is reconfigured at the surfactant containing silane（The surfactant of the present embodiment is octadecyl trichlorosilane alkane）Toluene solution, wherein silane contents be 0.5-5%；
A3, substrate is immersed in standing a period of time in above-mentioned toluene solution（The time of standing is less than 2 hours）Take out afterwards and clean, dry 1-30 minute under 120 degrees Celsius of temperature conditionss（Preferably drying time is less than 10 minutes）, hollowed-out mask as shown in Figure 2 is placed on substrate, through ultraviolet（Ultraviolet wavelength is less than 254 nanometers）Irradiate certain time（Irradiation time is less than 1 hour）Standby after formation pattern structure afterwards；
Step B, coating fluid make
B1, vanadium dioxide grain dispersion is become the aaerosol solution of aqueouss or Organic；
B2, adds macromolecule dispersing agent or the inorganic sol with cementation in above-mentioned aaerosol solution, that is, coating fluid is obtained；
Step C, masking
The above-mentioned coating fluid of last layer is coated on substrate using spin coating, blade coating, spraying or typography, after drying, that is, thin film is obtained.
The structure of the above-mentioned prepared sull with loose structure is as shown in figure 1, it includes substrate 1 and covering vanadium dioxide crystal grain 2 on substrate 1；Described vanadium dioxide crystal grain 2 has the crystalline texture of metal-insulator phase transition, this vanadium dioxide crystal grain 2 is in the circulus of rule, and the vanadium dioxide crystal grain 2 of circulus covers and forms continuous sull 3 on described substrate 1, the internal diameter of the wherein circulus of vanadium dioxide crystal grain 2 is 30-3000 nanometer, and sull 3 thickness is less than 400 nanometers（Sull 3 thickness is less than 100 nanometers in the present embodiment）.The cross section structure of described sull 3 is identical with the mask structure shown in Fig. 2.
The ultraviolet-visible-near-infrared spectrum of the sull with loose structure as shown in Figure 3 may know that, this sull has superelevation visible light transmissivity, peak value more than 90%, up to 97%.
Embodiment 2, embodiment 2 is substantially the same manner as Example 1, and difference adopts sapphire for described substrate 1；Described vanadium dioxide crystal grain 2 is doping property vanadium dioxide crystal grain, and dopant ion is one or more of W, Mo, Ti, Mg, F.
It should be appreciated that the principle that the above-mentioned specific embodiment of the present invention is used only for exemplary illustration or explains the present invention, and be not construed as limiting the invention.Therefore, any modification, equivalent substitution and improvement done in the case of the thought without departing from the present invention and scope etc., should be included within the scope of the present invention.Additionally, claims of the present invention whole changing and modifications of being intended to fall in scope and border or the equivalents on this scope and border.
Claims (10)
1. a kind of sull with loose structure it is characterised in that：It includes substrate and covers the oxide crystallization crystal grain on substrate；Described oxide crystallization crystal grain has the crystalline texture of metal-insulator phase transition, this oxide crystallization crystal grain is in the circulus of rule, and the oxide crystallization crystal grain of circulus covers and forms continuous sull on the substrate, wherein the internal diameter of the circulus of oxide crystallization crystal grain is 30-3000 nanometer.
2. according to claim 1 a kind of sull with loose structure it is characterised in that：Described oxide crystallization crystal grain is vanadium dioxide crystal grain.
3. according to claim 2 a kind of sull with loose structure it is characterised in that：The continuous sull thickness of described formation is less than 400 nanometers.
4. according to claim 3 a kind of sull with loose structure it is characterised in that：The continuous sull thickness of described formation is less than 100 nanometers.
5. a kind of preparation method of the sull with loose structure it is characterised in that：It comprises the following steps：
Step A, substrate pretreatment
A1, first by substrate cleaning post-drying；
A2, is reconfigured at the toluene solution of the surfactant containing silane, wherein silane contents are 0.5-5%；
A3, substrate is immersed in above-mentioned toluene solution to stand to take out after a period of time and cleans, dry 1-30 minute, hollowed-out mask is placed on substrate, formed standby after pattern structure after ultraviolet irradiation certain time under 120 degrees Celsius of temperature conditionss；
Step B, coating fluid make
B1, vanadium dioxide grain dispersion is become the aaerosol solution of aqueouss or Organic；
B2, adds macromolecule dispersing agent or the inorganic sol with cementation in above-mentioned aaerosol solution, that is, coating fluid is obtained；
Step C, masking
The above-mentioned coating fluid of last layer is coated on substrate using spin coating, blade coating, spraying or typography, after drying, that is, thin film is obtained.
6. according to claim 5 a kind of preparation method of the sull with loose structure it is characterised in that：In described step A, the time of standing is less than 2 hours.
7. according to claim 5 a kind of preparation method of the sull with loose structure it is characterised in that：Drying time in described step A3 is less than 10 minutes.
8. according to claim 5 a kind of preparation method of the sull with loose structure it is characterised in that：Ultraviolet irradiation time in described step A3 is less than 1 hour, and ultraviolet wavelength is less than 254 nanometers.
9. according to claim 5 a kind of preparation method of the sull with loose structure it is characterised in that：Described substrate adopts building glass；Described vanadium dioxide crystal grain is doping property vanadium dioxide crystal grain, and dopant ion is one or more of W, Mo, Ti, Mg, F；The described surfactant containing silane is octadecyl trichlorosilane alkane.
10. the sull with loose structure described in a kind of claim 1 application it is characterised in that：The sull of this loose structure is used for making building energy conservation window, the window of destination, sunshading ceiling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510483224.7A CN106431000A (en) | 2015-08-07 | 2015-08-07 | Oxide film of porous structure and preparation method and application of oxide film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510483224.7A CN106431000A (en) | 2015-08-07 | 2015-08-07 | Oxide film of porous structure and preparation method and application of oxide film |
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| CN106431000A true CN106431000A (en) | 2017-02-22 |
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| CN201510483224.7A Pending CN106431000A (en) | 2015-08-07 | 2015-08-07 | Oxide film of porous structure and preparation method and application of oxide film |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100183854A1 (en) * | 2007-09-12 | 2010-07-22 | Yoshitake Masuda | Vanadium Oxide Thin Film Pattern and Method of Fabricating the Same |
| CN101805134A (en) * | 2010-03-18 | 2010-08-18 | 中国科学院上海硅酸盐研究所 | Film-coating liquid of vanadium dioxide thin film and preparation method and application of thin film |
| CN104445987A (en) * | 2014-10-30 | 2015-03-25 | 中国建材国际工程集团有限公司 | Method for preparing thermochromism intelligent membrane glass |
| CN205011641U (en) * | 2015-08-07 | 2016-02-03 | 瀛石（上海）实业有限公司 | Oxide thin films with porous structure |
-
2015
- 2015-08-07 CN CN201510483224.7A patent/CN106431000A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100183854A1 (en) * | 2007-09-12 | 2010-07-22 | Yoshitake Masuda | Vanadium Oxide Thin Film Pattern and Method of Fabricating the Same |
| CN101805134A (en) * | 2010-03-18 | 2010-08-18 | 中国科学院上海硅酸盐研究所 | Film-coating liquid of vanadium dioxide thin film and preparation method and application of thin film |
| CN104445987A (en) * | 2014-10-30 | 2015-03-25 | 中国建材国际工程集团有限公司 | Method for preparing thermochromism intelligent membrane glass |
| CN205011641U (en) * | 2015-08-07 | 2016-02-03 | 瀛石（上海）实业有限公司 | Oxide thin films with porous structure |
Non-Patent Citations (2)
| Title |
|---|
| YANG, Y AT AL.: "Formation of Highly Ordered VO2 Nanotubular/Nanoporous Layers and Their Supercooling Effect in Phase Transitions", 《ADVANCED MATERIALS 》, vol. 24, no. 12, pages 1571 - 1575, XP071811827, DOI: 10.1002/adma.201200073 * |
| 梁倩 等: "二氧化钒纳米孔洞薄膜的光学特性", 硅酸盐学报, vol. 41, no. 12, pages 1685 - 1691 * |
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