CN102633444B - Method for preparing optical window material - Google Patents
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Abstract
The invention relates to a method for preparing an optical window material and belongs to the technical field of application of functional nanometer materials. According to the method, the alternately layered self-assembly technology is adopted, the essence is to utilize ligand interactions among nanometer particle indium tin oxide or/and zinc oxide and macromolecule polyethyleneimine, and a stable macromolecule/nanometer particle composite film is formed by depending on the binding force, especially the alternate self-assembly combined with the ultrasonic technology. A polyethyleneimine/indium tin oxide nanometer particle composite film prepared by the method has good pellucidness, and the transmissivity of a visible region is greatly improved. Compared with the methods of sputtering and the like for preparing the nanometer film, the method is simple in facility request, convenient in operation and strong in controllability and is not limited by the size and the shape of a substrate as well as whether the substrate is a plane.
Description
Technical field
The invention belongs to functional nanomaterials technical field, relate generally to a kind of based on prepared optical window material of the interactional alternately stratiform package technique of supramolecule and preparation method thereof.The optical window material of this invention not only has the two isolated effects of good UV-light/near infrared light, isolated effect controllability and good visible light permeability, and this inventive method is easy and simple to handle, equipment requirements is simple, fabrication cycle is short, is not subject to substrate sizes, shape, the whether restriction such as plane.
Background technology
Sunlight is the principal light source of earth illumination, is the assurance that the mankind depend on for existence.In recent years, be accompanied by increasingly sharpening of mankind's activity, depletion of the ozone layer is serious, and environmental problem is increasingly outstanding, and sunlight is when guaranteeing mankind's daily need, and a large amount of harm rays that wherein contain have had influence on the mankind's orthobiosis gradually.Excessive solar radiation can all be brought tremendous influence to HUMAN HEALTH, article, energy-conserving and environment-protective etc.: (1) impact on human body.Mainly refer to the injury that ultraviolet ray causes eyesight skin, eyesight and infrared rays.Over-exposure, in ultraviolet ray, can make skin surface general red, loses former flexiblely, tarnishes, and skin aging, even canceration can occur.Eyes are subject to uviolizing for a long time, can cause cornea, retina, crystalline chain etc. impaired, visual deterioration, vertical line pain, the symptom such as shed tears.High-intensity infrared rays can make tissue necrosis, protein coagulating, and the cataract causing as short infrared, day photosensitiveness retina choroid burn etc., meanwhile, infrared rays also can aggravate UV-induced skin carcinoma.(2) impact on article.In many indoor and cars, article can fade under periods of direct sunlight.Seeing through of harmful light, can cause the fading of the article such as instrument desk, seat in indoor carpet, family property, artwork, curtain and car, aging etc.(3) impact on energy-conserving and environment-protective.Infrared rays has obvious heat effect, especially near infrared part.Buildings or transportation means for operation air-conditioning system, the heat effect that a large amount of infrared rays causes, can increase the weight of the burden of air-conditioning system, increases energy consumption.Therefore, rationally utilize sunlight, when guaranteeing that visible ray sees through, isolated excessive ultraviolet ray, infrared rays become an important research topic.
Conventional solution to the problems described above mainly contains and uses heat reflection metal coating glass, mounts sunshade heat insulation film etc.But above product exists following shortcoming: visible light permeability is poor, can not be made full use of it; Reflectivity is high, and the secondary light causing is polluted comparatively serious; Metal coating is oxidizable, and impact completely cuts off and transparent effect.By comparison, utilize functional nanomaterials to process glass surface, preventing ultraviolet/near infrared light the radiative material obtaining, there is the features such as antiradar reflectivity, high-clarity, and its making method is simple and easy, the cycle is short, material is easy to get, therefore, utilize functional nanomaterials (if tin indium oxide is because it has the two isolated property of UV-light/infrared light and visible transparent, be widely used with various optical coatings in; Zinc oxide is a kind of transparent anti-ultraviolet anti-biotic material, is usually used in the makeup such as sunscreen) research of preparing preventing ultraviolet/near infrared light radiation transparent material certainly will cause extensive concern.
Alternately stratiform self-assembling technique is a kind of based on the interactional novel thin film technology of preparing of supramolecule, utilize intermolecular non covalent bond reactive force, as electrostatic force, Van der Waals force, coordination, close hydrophobic interaction etc., realize difference in functionality material and in substrate, alternately grow into film.Utilize alternately stratiform self-assembling technique, select to have the nano material of specific function, can prepare several functions film.Than traditional film technique, as sputtering technology, gas phase deposition technology, electron beam coating technique etc., the advantage such as that the method has is easy to operate, apparatus and process requirement is simple, and to the size of substrate, shape, whether plane does not require, be a kind ofly to have compared with the new technology of great development potentiality.
Therefore,, in conjunction with replacing stratiform self-assembling technique and functional nanomaterials, constructing preventing ultraviolet/infrared radiation transparent material will become study hotspot.
Summary of the invention
The object of the invention is to provide a kind of preparation method based on the interactional optical window material of supramolecule, main ultrasonic auxiliary immersion package technique and the spin coating package technique of adopting, in substrate, construct macromolecule/nano particle laminated film, realize two isolation performances of ultraviolet, UV-light/near infrared light.
A kind of preparation method based on the interactional optical window material of supramolecule, it is characterized in that: this invention adopts alternately stratiform self-assembling technique, its essence is the Coordination interaction utilizing between nanoparticle and polymer, rely on this linkage force, form stable macromolecule/nano particle laminated film, especially in conjunction with the alternately self-assembly of ultrasonic technique.
A kind of preparation method based on the interactional optical window material of supramolecule of the present invention, is characterized in that, in conjunction with ultrasonic technique or spin coating and stratiform self-assembling technique alternately, specifically comprises the following steps:
1), quartz plate or silicon chip are cleaned by washing lotion, then use washed with de-ionized water quartz plate, silicon chip, with nitrogen, dry up;
2), by step 1) in the substrate of gained be placed in macromolecular solution A, standing, after reaching capacity, take out, with coordinative solvent, rinse nitrogen drying under room temperature;
3), by step 2) in the substrate of gained be placed in nano-particle solution B, under ultrasound condition, soak, after reaching capacity, take out, with coordinative solvent, rinse nitrogen drying under room temperature;
4), repeating step 2 alternately) and step 3), until the macromolecule/nano particle laminated film of the required number of plies is gone up in substrate surface assembling.
The preparation method of another kind of the present invention based on the interactional optical window material of supramolecule, is characterized in that, comprises the following steps:
1), will at the bottom of quartz plate or silicon wafer-based, by washing lotion, clean, then use washed with de-ionized water quartz plate, silicon chip, with nitrogen, dry up;
2), in step 1) in the substrate of gained, rotary coating macromolecular solution A, then rotary coating coordinative solvent at least 2 times; Preferably 3-5 time.
3), in step 2) in the substrate of gained, rotary coating nano-particle solution C carries out self-assembly, then rotary coating coordinative solvent, washes away the nanoparticle of unnecessary physical adsorption;
4), repeating step 2 alternately) and step 3) repeatedly, until the macromolecule/nano particle laminated film of the upper required number of plies of substrate surface assembling, taking-up, what obtain is optical window material.
Aforesaid method of the present invention, is to carry out self-assembly in a side of substrate, or in both sides, carries out self-assembly respectively simultaneously.
The preparation method of another kind of the present invention based on the interactional optical window material of supramolecule, is characterized in that, comprises the following steps:
1), quartz plate or silicon chip are cleaned by washing lotion, then use washed with de-ionized water quartz plate, silicon chip, with nitrogen, dry up;
2), by step 1) in the substrate of gained be placed in macromolecular solution A, standing, after reaching capacity, take out, with coordinative solvent, rinse nitrogen drying under room temperature;
3), by step 2) in the substrate of gained be placed in nano-particle solution B, under ultrasound condition, soak, after reaching capacity, take out, with coordinative solvent, rinse nitrogen drying under room temperature;
4), repeating step 2 alternately) and step 3), until the macromolecule/nano particle laminated film of the required number of plies is gone up in substrate surface assembling;
5), with vitriol oil cleaning step 4) in a side a of the substrate that obtains, wash the laminated film of assembling, by washed with de-ionized water, nitrogen drying under room temperature;
6), in step 5) in a side of substrate of gained, rotary coating macromolecular solution A, then rotary coating coordinative solvent at least 2 times; Preferably 3-5 time;
7), in step 6) in a side of substrate of gained, rotary coating nano-particle solution C carries out self-assembly, then rotary coating coordinative solvent, washes away the nanoparticle of unnecessary physical adsorption;
8), repeating step 6 alternately) and step 7) repeatedly, until the macromolecule/nano particle laminated film of the upper required number of plies of substrate surface assembling, taking-up, what obtain is optical window material;
9), by controlling step 4) and step 8) multiplicity, can regulate the window material obtaining.Window material has the isolated effect of UV-light/infrared light.
In above-mentioned three kinds of preparation methods based on the interactional optical window material of supramolecule, washing lotion is the vitriol oil and hydrogen peroxide mixed solution, and volume ratio is 8: 3-6: 4 all can.
Described macromolecular solution A is polyethyleneimine: amine aqueous solution, and its concentration is 0.5-30mg/mL, preferred 1.0mg/mL, solvent for use can polymine in this area all can, such as water, ethanol etc.
Nano-particle solution B used is tin indium oxide nano-particle solution, and its concentration is 1.0-5.0mg/mL, and solvent for use is the conventional solvent of this area solubilized tin indium oxide nanoparticle, such as ethanol, ethyl acetate, butylacetate etc.
Nano-particle solution C used, described nano-particle solution C is zinc oxide nano-particle solution, and its concentration is 1.0-5.0mg/mL, and solvent for use is the conventional solvent of this area solubilized zinc oxide nano-particle, such as ethanol, normal hexane etc.
Involved in the present invention based on the interactional alternately prepared optical window material of stratiform self-assembling technique of supramolecule, main ultrasonic auxiliary immersion package technique and the spin coating package technique of adopting, its essence is the Coordination interaction utilizing between nanoparticle and polymer, rely on this linkage force, form stable macromolecule/nano particle laminated film.After substrate is cleaned by the vitriol oil/hydrogen peroxide mixed solution, surface is with a large amount of hydroxyls.Substrate with hydroxyl is immersed in polyethyleneimine: amine aqueous solution, and polymine and substrate surface group interact, at substrate surface absorption last layer macromolecule membrane; Above-mentioned substrate is immersed after tin indium oxide nano-particle solution, due to ultrasonic booster action, tin indium oxide nanoparticle is singly dispersed in solution uniformly, utilize the Coordination interaction of tin indium oxide nanoparticle and polymine, on the macromolecule membrane surface of substrate, evenly adsorb the monodispersed tin indium oxide nanoparticulate thin films of one deck; Above-mentioned substrate is immersed after polymine macromolecular solution again, and polymine and nanoparticle generation Coordination interaction, on the nanoparticulate thin films surface of substrate, evenly adsorb layer of polyethylene imines macromolecule membrane; By substrate, at polymine macromolecular solution and tin indium oxide nano-particle solution, alternately soak assembling, can obtain uniform polymine/tin indium oxide Nanocomposites film at substrate surface.By the vitriol oil, clean a side of above-mentioned substrate, the laminated film of this side is cleaned, expose a large amount of oh groups that exist of substrate surface.Adopt spin coating package technique, in the exposed side of substrate, by replacing coating polyethylene imines macromolecular solution and zinc oxide nano-particle solution, be similar to the mechanism of action of polymine/tin indium oxide Nanocomposites film, utilize the Coordination interaction between polymer and substrate and between polymer and nanoparticle, realize at the bottom of this side group on the constructing of polymine/zinc oxide nano-particle laminated film.The optical window material preparing through above-mentioned a series of processes, when having guaranteed good visible light permeability, has the two isolated effects of excellent UV-light/near infrared light, and can, by changing alternatively stacked number of times, regulate its isolated effect.As a comparison, in research process, adopt tradition to replace stratiform assemble method and constructed polymine/tin indium oxide Nanocomposites film, result shows, polymine/tin indium oxide Nanocomposites the film that adopts the present invention to prepare has the good transparency, and it has significantly improved visible region transmitance.Than methods such as sputters, prepare nano thin-film, this invention equipment requirements is simple, easy to operate, and controllability is strong, be not subject to substrate size, shape, whether plane limits.
The invention provides three kinds of similar methods, can select voluntarily as required.For example, first method has visible transparent, the near infrared light that mainly isolated wavelength is shorter than 300nm UV-light and is longer than 1400nm; Second method mainly intercepts the UV-light that wavelength is shorter than 350nm, and visible ray and near infrared light are had to good perviousness; The third method combines first two method, when guaranteeing visible ray highly transparent, has effectively completely cut off the near infrared light that wavelength is shorter than 350nm UV-light and is longer than 1400nm.Appeal three kinds of methods and all there is isolated effect adjustability, adapt to different demands.
The two isolated optical window materials of UV-light/near infrared light of the present invention, are with a wide range of applications in fields such as building, traffic, environmental protection.
1, optical window material of the present invention has excellent UV-light, the two isolated effects of infrared light, and visible light permeability is good, can be used for glass for building purposes window etc.
2, optical window material of the present invention, can be widely used in the vehicle window in automobile industry, avoid in car that article long-term exposure causes under periods of direct sunlight fade, the problem such as aging.
3, optical window material of the present invention, effectively barrier material both sides heat transmits, and reduces energy waste, can, for environmental protection industry (epi), realize energy-saving and emission-reduction.
4, optical window material UV-light of the present invention, the isolated effect excellence of infrared light, visible light permeability is good.
5, optical window material of the present invention has isolated effect adjustability, is applicable to different field, occasion, meets the different demands of user.
6, optical window material preparation method of the present invention is simple, and operating process is short.
7, optical window material of the present invention is not subject to shapes of substrates, size, plane limit whether.
Accompanying drawing explanation
Fig. 1. the two isolated window materials of UV-light/near infrared light of the embodiment of the present invention 1 preparation and ultraviolet-visible-near infrared transmittance curve variation diagram of blank example.
Fig. 2. polymine/tin indium oxide Nanocomposites film of the embodiment of the present invention 5 preparations and comparative example 1 are soaked Film laminated Thin Films UV-vis-near infrared transmittance curve variation diagram of the same race of assembling preparation.
Fig. 3. polymine/tin indium oxide Nanocomposites film (one-sided 10 bilayers) scanning electron microscope diagram of the embodiment of the present invention 6 preparations.
Fig. 4. comparative example 2 is soaked polymine/tin indium oxide Nanocomposites film (one-sided 10 bilayers) scanning electron microscope diagram of assembling preparation.
Fig. 5. polymine/zinc oxide nano-particle laminated film ultraviolet-visible transmittance curve variation diagram of the embodiment of the present invention 7 preparations.
Fig. 6. polymine/zinc oxide nano-particle laminated film (one-sided 10 bilayers) scanning electron microscope diagram of the embodiment of the present invention 8 preparations.
Specific implementation method
Below in conjunction with examples of implementation and accompanying drawing, technical scheme of the present invention is further described:
Blank example:
1, select substrate---quartz plate substrate, immerse in the vitriol oil/hydrogen peroxide mixed solution (volume ratio is 7: 3), scavenging period is 60min, at room temperature water cleans, more at room temperature with nitrogen, transparent substrates surface is dried up.
2, isolation performance test: substrate is placed in to ultraviolet-visible-near infrared spectrometer, take air as scanning background, test substrate is perviousness change curve within the scope of 200-1800nm at wavelength, and record, as shown in Figure 1.
Comparative example 1 result demonstration, the transmitance of blank quartz plate within the scope of test wavelength is certain value substantially, 93%.
Embodiment 1:
1, quartz plate substrate is immersed in the vitriol oil/hydrogen peroxide mixed solution (volume ratio is 7: 3), and scavenging period is 60min, by washed with de-ionized water, with nitrogen, surface is dried up;
2, the quartz plate cleaning up is placed in to polymine ethanolic soln, concentration is 1mg/mL, and standing 10min takes out, and with dehydrated alcohol, rinses, and with nitrogen, surface is dried up;
3, the quartz plate of gained in step 2 is placed in to tin indium oxide nanoparticle ethyl acetate solution, concentration is 4mg/mL, under ultrasound condition, soaks 10min, takes out, and by ethyl acetate rinse, with nitrogen, surface is dried up;
4, replace repeating step 2 and step 3 many times, repeating to be designated as for n time one-sided is n+1 bilayer, n=19;
5, with a side a of the quartz plate obtaining in vitriol oil cleaning step 4, scavenging period is 300min, with deionized water rinsing, with nitrogen, surface is dried up;
6, a side of the quartz plate of gained in step 5, rotary coating polymine ethanolic soln, concentration is 1mg/mL, speed of rotation is 3000 rpms, and rotational time is 30s, then rotary coating ethanol 3 times, speed of rotation is 3000 rpms, and rotational time is 30s.
7, a side of the quartz plate of gained in step 6, rotary coating zinc oxide nano-particle ethanolic soln, concentration is 4mg/mL, speed of rotation is 3000 rpms, and rotational time is 30s, then rotary coating ethanol 3 times, speed of rotation is 3000 rpms, and rotational time is 30s.
8, replace repeating step 6 and step 7 many times, Repeated m time is designated as one-sided m+1 bilayer, m=29.
9, isolation performance test: quartz plate substrate is placed in to ultraviolet-visible-near infrared spectrometer, take air as scanning background, and after test procedure 5 finishes respectively and after step 8 end, substrate is transmitance change curve within the scope of wavelength 200-1800nm, and record, as shown in Figure 2.
Embodiment 1 test result demonstration, after step 5 finishes, a side is coated with the quartz plate substrate of polymine/tin indium oxide Nanocomposites film, and within the scope of its wavelength 400-1000nm, visible light transmissivity maintains 90% left and right; Within the scope of 200-400nm, from 325nm, start uv transmittance and start obvious decline, until reach 0% in 200nm left and right; Within the scope of 1000-1800nm, with wavelength, increase, transmitance presents progressively downtrending, after 1600nm, basicly stable in 25% left and right.After step 8 finishes, one side is coated with polymine/tin indium oxide Nanocomposites film, and opposite side is coated with the quartz plate substrate of polymine/zinc oxide nano-particle laminated film, within the scope of its wavelength 400-1000nm, visible light transmissivity maintains 83-90%, substantially higher than 85%; Within the scope of 200-400nm, from 380nm, start uv transmittance and start to decline, and at 350nm place, sharply drop to 23%, 290nm place and be down to about 10%, 240nm and reach 0%; Within the scope of 1000-1800nm, with wavelength, increase, transmitance presents progressively downtrending, after 1600nm, basicly stable in 20% left and right.
Blank example, embodiment 1 show, this invention has effectively completely cut off the UV-light of wavelength below 350nm, transmitance lower than 25%, isolated effect is higher than 75%, and the near infrared light of wavelength more than 1000nm, is stabilized in 20% left and right in the above transmitance of 1600nm, isolated effect approaches 80%.Visible ray for wavelength at 400-800nm, this invention has effectively maintained the transparency, and transmitance is between 83-90%, substantially higher than 85%.
Embodiment 2:
1, quartz plate substrate is immersed in the vitriol oil/hydrogen peroxide mixed solution (volume ratio is 7: 3), and scavenging period is 60min, by washed with de-ionized water, with nitrogen, surface is dried up;
2, the quartz plate cleaning up is placed in to polymine ethanolic soln, concentration is 1mg/mL, and standing 10min takes out, and with dehydrated alcohol, rinses, and with nitrogen, surface is dried up;
3, the quartz plate of gained in step 2 is placed in to tin indium oxide nanoparticle ethyl acetate solution, concentration is 4mg/mL, under ultrasound condition, soaks 10min, takes out, and by ethyl acetate rinse, with nitrogen, surface is dried up;
4, replace repeating step 2 and step 3 many times, repeating to be designated as for n time one-sided is n+1 bilayer, n=19,39,59;
5, with a side a of the quartz plate obtaining in vitriol oil cleaning step 4, scavenging period is 300min, with deionized water rinsing, with nitrogen, surface is dried up;
6, a side of the quartz plate of gained in step 5, rotary coating polymine ethanolic soln, concentration is 1mg/mL, speed of rotation is 3000 rpms, and rotational time is 30s, then rotary coating ethanol 3 times, speed of rotation is 3000 rpms, and rotational time is 30s.
7, a side of the quartz plate of gained in step 6, rotary coating zinc oxide nano-particle ethanolic soln, concentration is 4mg/mL, speed of rotation is 3000 rpms, and rotational time is 30s, then rotary coating ethanol 3 times, speed of rotation is 3000 rpms, and rotational time is 30s.
8, replace repeating step 6 and step 7 many times, it is m+1 bilayer, m=29 that Repeated m time is designated as one-sided.
9, isolation performance test: quartz plate substrate is placed in to ultraviolet-visible-near infrared spectrometer, take air as scanning background, after test procedure 5 finishes respectively and after step 8 end, substrate transmitance within the scope of wavelength 200-1800nm changes, and record.
Embodiment 2 test results show, are accompanied by the increase of polymine/tin indium oxide Nanocomposites film number of plies, and the transparency of resulting product changes little; The isolated effect of near infrared significantly strengthens, and by 20%, drops to gradually 0%; The isolated effect of ultraviolet region also strengthens to some extent, but effect not obvious, this be mainly the isolated wavelength of ultraviolet due to zinc oxide longer compared with tin indium oxide due to.
Embodiment 3:
1, quartz plate substrate is immersed in the vitriol oil/hydrogen peroxide mixed solution (volume ratio is 7: 3), and scavenging period is 60min, by washed with de-ionized water, with nitrogen, surface is dried up;
2, the quartz plate cleaning up is placed in to polymine ethanolic soln, concentration is 1mg/mL, and standing 10min takes out, and with dehydrated alcohol, rinses, and with nitrogen, surface is dried up;
3, the quartz plate of gained in step 2 is placed in to tin indium oxide nanoparticle ethyl acetate solution, concentration is 4mg/mL, under ultrasound condition, soaks 10min, takes out, and by ethyl acetate rinse, with nitrogen, surface is dried up;
4, replace repeating step 2 and step 3 many times, repeating to be designated as for n time one-sided is n+1 bilayer, n=19;
5, with a side a of the quartz plate obtaining in vitriol oil cleaning step 4, scavenging period is 300min, with deionized water rinsing, with nitrogen, surface is dried up;
6, a side of the quartz plate of gained in step 5, rotary coating polymine ethanolic soln, concentration is 1mg/mL, speed of rotation is 3000 rpms, and rotational time is 30s, then rotary coating ethanol 3 times, speed of rotation is 3000 rpms, and rotational time is 30s.
7, a side of the quartz plate of gained in step 6, rotary coating zinc oxide nano-particle ethanolic soln, concentration is 4mg/mL, speed of rotation is 3000 rpms, and rotational time is 30s, then rotary coating ethanol 3 times, speed of rotation is 3000 rpms, and rotational time is 30s.
8, replace repeating step 6 and step 7 many times, it is m+1 bilayer, m=4,9,14 that Repeated m time is designated as one-sided.
9, isolation performance test: quartz plate substrate is placed in to ultraviolet-visible-near infrared spectrometer, take air as scanning background, after test procedure 5 finishes respectively and after step 8 end, substrate transmitance within the scope of wavelength 200-800nm changes, and record.
Embodiment 3 test results show, are accompanied by the increase of polymine/zinc oxide nano-particle laminated film number of plies, and the resulting product transparency changes little; The isolated effect of ultraviolet region significantly strengthens, and the isolated effect of ultraviolet that is mainly reflected in the beginning of 350nm place improves constantly.
Blank example, the demonstration of embodiment 1-3 test result, the optical window material of this invention preparation has the isolated property of excellent UV-light/near infrared light and good visible transparent, and its UV-light/near infrared light general layout effect has controllability.
Embodiment 4:
1, quartz plate substrate is immersed in the vitriol oil/hydrogen peroxide mixed solution (volume ratio is 7: 3), and scavenging period is 60min, and at room temperature water cleans, and with nitrogen, surface is dried up.
2, the quartz plate cleaning up is placed in to polymine ethanolic soln, concentration is 1mg/mL, and standing 10min takes out, and with dehydrated alcohol, rinses, and with nitrogen, surface is dried up.
3, the quartz plate of gained in step 2 is placed in to tin indium oxide nanoparticle ethyl acetate solution, concentration is 4mg/mL, under ultrasound condition, soaks 10min, takes out, and by ethyl acetate rinse, with nitrogen, surface is dried up.
4, replace repeating step 2 and step 3 many times, repeating to be designated as for n time one-sided is n+1 bilayer, n=0-7.
5, isolation performance test: substrate is placed in to ultraviolet-visible-near infrared spectrometer, take air as scanning background, test substrate changes at wavelength 200-800nm scope internal absorbance, and record.
Embodiment 4 test results show, surface is with the quartz plate of polymine/tin indium oxide Nanocomposites film, visible region is without absorption, ultraviolet region absorption peak is in 200-325nm wavelength region, n is changed to 7 from 0,245nm place absorbance is respectively 0.19,0.35,0.57,0.75,0.88,1.05,1.25,1.52, presents the linear growth trend of absorbancy to double-deck number.According to absorbancy defined formula: absorbancy=-lg (transmitance), derivation obtains, and the ultraviolet region transmitance of this quartz plate increases with double-deck number, presents progressively downtrending.
Embodiment 5
1, quartz plate substrate is immersed in the vitriol oil/hydrogen peroxide mixed solution (volume ratio is 7: 3), and scavenging period is 60min, and at room temperature water cleans, and with nitrogen, surface is dried up.
2, the quartz plate cleaning up is placed in to polymine ethanolic soln, concentration is 1mg/mL, and standing 10min takes out, and with dehydrated alcohol, rinses, and with nitrogen, surface is dried up.
3, the quartz plate of gained in step 2 is placed in to tin indium oxide nanoparticle ethyl acetate solution, concentration is 4mg/mL, under ultrasound condition, soaks 10min, takes out, and by ethyl acetate rinse, with nitrogen, surface is dried up.
4, replace repeating step 2 and step 3 many times, repeating to be designated as for n time one-sided is n+1 bilayer, n=9,19,29.
5, isolation performance test: substrate is placed in to ultraviolet-visible-near infrared spectrometer, take air as scanning background, test substrate is perviousness change curve within the scope of 200-1800nm at wavelength, and record, as shown in Figure 2.
Embodiment 5 test results show, surface is with the quartz plate of polymine/tin indium oxide Nanocomposites film, and visible region is without obvious absorption, but with the increase of n, average visible light transmissivity progressively reduces, and is respectively 92%, 88%, 85%; Ultraviolet occurs in 200-325nm wavelength region isolated, along with the increase of n, 245nm place transmitance is respectively 30%, 20%, 15%, presents the rising tendency of isolated effect to double-deck number; Near infrared occurs in 1000-1800nm wavelength region isolated, transmitance reaches stationary value after wavelength is longer than 1600nm, and along with the increase of n, 1600nm place transmitance is respectively 15%, 5%, 1% left and right, presents the rising tendency of isolated effect to double-deck number.
Blank example, embodiment 4-5 show, polymine/tin indium oxide Nanocomposites film of this invention preparation, can be by regulating the alternating growth number of plies of polymine polymer and tin indium oxide nanoparticle, control its isolated ultraviolet/isolated near infrared ability, and visible light permeability is not had to larger impact.
Embodiment 6
1, at the bottom of silicon wafer-based, immerse in the vitriol oil/hydrogen peroxide mixed solution (volume ratio is 7: 3), scavenging period is 60min, and at room temperature water cleans, and with nitrogen, surface is dried up.
2, the quartz plate cleaning up is placed in to polymine ethanolic soln, concentration is 1mg/mL, and standing 10min takes out, and with dehydrated alcohol, rinses, and with nitrogen, surface is dried up.
3, the quartz plate of gained in step 2 is placed in to tin indium oxide nanoparticle ethyl acetate solution, concentration is 4mg/mL, under ultrasound condition, soaks 10min, takes out, and by ethyl acetate rinse, with nitrogen, surface is dried up.
4, replace repeating step 2 and step 3 many times, repeating to be designated as for n time one-sided is n+1 bilayer, n=0,9.
5, internal structure test: use field emission scanning electron microscope to observe the internal structure of the laminated film of silicon wafer-based basal surface covering, and record, as shown in Figure 3.
Embodiment 6 test results demonstrations, in polymine/tin indium oxide Nanocomposites film that this invention obtains, tin indium oxide nanoparticle exists with monodisperse particles shape form, and internal structure is even, regular, fine and close.
Comparative example 1
1, quartz plate substrate is immersed in the vitriol oil/hydrogen peroxide mixed solution (volume ratio is 7: 3), and scavenging period is 60min, and at room temperature water cleans, and with nitrogen, surface is dried up.
2, the quartz plate cleaning up is placed in to polymine ethanolic soln, concentration is 1mg/mL, and standing 10min takes out, and with dehydrated alcohol, rinses, and with nitrogen, surface is dried up.
3, the quartz plate of gained in step 2 is placed in to tin indium oxide nanoparticle ethyl acetate solution, concentration is 4mg/mL, soaks 10min, takes out, and by ethyl acetate rinse, with nitrogen, surface is dried up.
4, replace repeating step 2 and step 3 many times, repeating to be designated as for n time one-sided is n+1 bilayer, n=9,19,29.
5, isolation performance test: substrate is placed in to ultraviolet-visible-near infrared spectrometer, take air as scanning background, test substrate is perviousness change curve within the scope of 200-1800nm at wavelength, and record, as shown in Figure 2.
Comparative example 1 test result shows, surface is with the quartz plate of polymine/tin indium oxide Nanocomposites film, its transmittance curve presents unimodal variation between test zone, there is obvious absorption visible region, maximum transmission is in left and right, 800nm place, along with the increase of n, 800nm place transmitance is respectively 85%, 72%, 60%, and 400nm place transmitance is respectively 50%, 25%, 8%; When n=9, wavelength is shorter than the UV-light of 260nm is isolated completely, and the near infrared light transmitance that wavelength is longer than 1400nm reaches stationary value, is 10% left and right; When n=19, wavelength is shorter than the UV-light of 300nm is isolated completely, and the near infrared light that wavelength is longer than 1350nm is completely cut off completely; When n=29, wavelength is shorter than the UV-light of 330nm isolates completely, and the near infrared light that wavelength is longer than 1220nm is completely cut off completely.
Blank example, comparative example 1 demonstration, tradition is soaked polymine/tin indium oxide Nanocomposites film that alternately prepared by stratiform self-assembling method, have outstanding isolated ultraviolet/near infrared performance, but visible light permeability is extremely low, and impact is applied.
Comparative example 2
1, at the bottom of silicon wafer-based, immerse in the vitriol oil/hydrogen peroxide mixed solution (volume ratio is 7: 3), scavenging period is 60min, and at room temperature water cleans, and with nitrogen, surface is dried up.
2, the quartz plate cleaning up is placed in to polymine ethanolic soln, concentration is 1mg/mL, and standing 10min takes out, and with dehydrated alcohol, rinses, and flush time is 1min, with nitrogen, surface is dried up.
3, the quartz plate of gained in step 2 is placed in to tin indium oxide nanoparticle ethyl acetate solution, concentration is 4mg/mL, soaks 10min, takes out, and by ethyl acetate rinse, flush time is 1min, with nitrogen, surface is dried up.
4, replace repeating step 2 and step 3 many times, repeating to be designated as for n time one-sided is n+1 bilayer, n=0,9.
5, internal structure test: use field emission scanning electron microscope to observe the internal structure of the laminated film of silicon wafer-based basal surface covering, and record, as shown in Figure 4.
Comparative example 2 test results show, traditional immersion replaces in polymine/tin indium oxide Nanocomposites film that stratiform self-assembling method obtains, and tin indium oxide nanoparticle exists with coacervate form in a large number, and internal structure is loose, there is a large amount of holes, loose.
Blank example, embodiment 5 and 6, comparative example 1 and 2 test results show, than traditional immersion, replace stratiform self-assembling method, the ultrasonic subsidiary conditions that this invention is introduced have effectively increased the order degree that nanoparticle is arranged, improved the internal structure regularity of film, and then when guaranteeing isolated UV-light/near infrared light, significantly improved the visible region perviousness of film.
Embodiment 7
1, quartz plate substrate is immersed in the vitriol oil/hydrogen peroxide mixed solution (volume ratio is 7: 3), and scavenging period is 60min, and at room temperature water cleans, and with nitrogen, surface is dried up.
2, quartz plate is placed on rotation sol evenning machine, at one side a rotary coating polymine ethanolic soln, concentration is 1mg/mL, speed of rotation is 3000 rpms, and rotational time is 30s, then rotary coating ethanol 3 times, speed of rotation is 3000 rpms, and rotational time is 30s.
3, a side of gained quartz plate in step 2, rotary coating zinc oxide nano-particle ethanolic soln, concentration is 4mg/mL, speed of rotation is 3000 rpms, and rotational time is 30s, then rotary coating ethanol 3 times, speed of rotation is 3000 rpms, and rotational time is 30s.
4, replace repeating step 2 and step 3 many times, it is m+1 bilayer, m=4,9,14,19,24,29 that every Repeated m time is designated as one-sided.
5, isolation performance test: substrate is placed in to ultraviolet-visible-near infrared spectrometer, take air as scanning background, and test substrate is at wavelength 200-800nm scope internal absorbance change curve, and within the scope of 200-1800nm transmitance change curve, and record, as shown in Figure 5.
Embodiment 7 absorbancy change curve test results show, surface is with the quartz plate of polymine/tin indium oxide Nanocomposites film, visible region is completely without absorbing, at wavelength within the scope of 360-350nm, absorbancy is undergone mutation, sharply rises, and be characteristic absorbance, wavelength is shorter than after 340nm, and absorbancy shortens and slowly rises gradually with wavelength.Along with the increase of m value, the absorbance at its 340nm place is respectively 0.16,0.25,0.35,0.43,0.52,0.60, presents the linear growth trend of absorbancy to double-deck number.According to absorbancy defined formula: absorbancy=-lg (transmitance), derivation obtains, and the ultraviolet region transmitance of this quartz plate increases with double-deck number, presents progressively downtrending.
Embodiment 7 transmitance change curve test results show, the surperficial quartz plate with polymine/tin indium oxide Nanocomposites film, and visible region transmitance maintains more than 85% substantially.At wavelength, within the scope of 360-350nm, transmitance sharply declines, and wavelength is shorter than after 340nm, and permeability is with the wavelength slow decreasing that shortens.Along with the increase of m value, the transmitance value at its 340nm place presents progressively downtrending.
Blank example, embodiment 7 test results demonstrations, this invention can, by regulating the alternating growth number of plies of polymine polymer and zinc oxide nano-particle, reach the ability that regulates its isolated ultraviolet, and visible light permeability not had to larger impact.
Blank example, embodiment 4,5,7 test results show, polymine/zinc oxide nano-particle laminated film is than polymine/tin indium oxide nanoparticulate thin films, at ultraviolet region, have higher isolation performance, isolated wave band is longer, improves isolation performance.
Embodiment 8
1, at the bottom of silicon wafer-based, immerse in the vitriol oil/hydrogen peroxide mixed solution (volume ratio is 7: 3), scavenging period is 60min, and at room temperature water cleans, and with nitrogen, surface is dried up.
2, silicon chip is placed on rotation sol evenning machine, at one side a rotary coating polymine ethanolic soln, concentration is 1mg/mL, speed of rotation is 3000 rpms, and rotational time is 30s, then rotary coating ethanol 3 times, speed of rotation is 3000 rpms, and rotational time is 30s.
3, a side of gained silicon chip in step 2, rotary coating zinc oxide nano-particle ethanolic soln, concentration is 4mg/mL, speed of rotation is 3000 rpms, and rotational time is 30s, then rotary coating ethanol 3 times, speed of rotation is 3000 rpms, and rotational time is 30s.
4, replace repeating step 2 and step 3 many times, it is m+1 bilayer, m=0,29 that every Repeated m time is designated as one-sided.
5, internal structure test: use field emission scanning electron microscope to observe the internal structure of the laminated film of silicon wafer-based basal surface covering, and record, as shown in Figure 6.
Embodiment 8 test results demonstrations, in polymine/zinc oxide nano-particle laminated film that this invention obtains, zinc oxide nano-particle exists with single discrete form, tightly packed, and internal structure is regular, even, fine and close.
Claims (6)
1. the preparation method based on the interactional optical window material of supramolecule, is characterized in that, in conjunction with ultrasonic technique or spin coating and stratiform self-assembling technique alternately, specifically comprises the following steps:
1), quartz plate or silicon chip are cleaned by washing lotion, then use washed with de-ionized water quartz plate, silicon chip, with nitrogen, dry up;
2), the substrate of gained in step 1) is placed in to macromolecular solution A, standing, after reaching capacity, take out, with coordinative solvent, rinse nitrogen drying under room temperature;
3), by step 2) in the substrate of gained be placed in nano-particle solution B, under ultrasound condition, soak, after reaching capacity, take out, with coordinative solvent, rinse nitrogen drying under room temperature;
4), repeating step 2 alternately) and step 3), until the macromolecule/nano particle laminated film of the upper required number of plies of substrate surface assembling;
Washing lotion is the vitriol oil and hydrogen peroxide mixed solution, and volume ratio is 8:3-6:4;
Described macromolecular solution A is polyethyleneimine: amine aqueous solution, and nano-particle solution B used is tin indium oxide nano-particle solution.
2. according to the method for claim 1, it is characterized in that, described macromolecular solution A, its concentration is 0.5-30mg/mL, nano-particle solution B used, its concentration is 1.0-5.0mg/mL.
3. the preparation method based on the interactional optical window material of supramolecule, is characterized in that, comprises the following steps:
1), will at the bottom of quartz plate or silicon wafer-based, by washing lotion, clean, then use washed with de-ionized water quartz plate, silicon chip, with nitrogen, dry up;
2), in step 1) in the substrate of gained, rotary coating macromolecular solution A, then rotary coating coordinative solvent at least 2 times;
3), in step 2) in the substrate of gained, rotary coating nano-particle solution C carries out self-assembly, then rotary coating coordinative solvent, washes away the nanoparticle of unnecessary physical adsorption;
4), repeating step 2 alternately) and step 3) repeatedly, until the macromolecule/nano particle laminated film of the upper required number of plies of substrate surface assembling, taking-up, what obtain is optical window material;
Washing lotion is the vitriol oil and hydrogen peroxide mixed solution, and volume ratio is 8:3-6:4;
Described macromolecular solution A is polyethyleneimine: amine aqueous solution, and described nano-particle solution C is zinc oxide nano-particle solution;
Aforesaid method, is to carry out self-assembly in a side of substrate, or in both sides, carries out self-assembly respectively simultaneously.
4. according to the method for claim 3, it is characterized in that, described its concentration of macromolecular solution A is 0.5-30mg/mL; Its concentration of described nano-particle solution C is 1.0-5.0mg/mL.
5. the preparation method based on the interactional optical window material of supramolecule, is characterized in that, comprises the following steps:
1), quartz plate or silicon chip are cleaned by washing lotion, then use washed with de-ionized water quartz plate, silicon chip, with nitrogen, dry up;
2), the substrate of gained in step 1) is placed in to macromolecular solution A, standing, after reaching capacity, take out, with coordinative solvent, rinse nitrogen drying under room temperature;
3), by step 2) in the substrate of gained be placed in nano-particle solution B, under ultrasound condition, soak, after reaching capacity, take out, with coordinative solvent, rinse nitrogen drying under room temperature;
4), repeating step 2 alternately) and step 3), until the macromolecule/nano particle laminated film of the upper required number of plies of substrate surface assembling;
5), with vitriol oil cleaning step 4) in a side a of the substrate that obtains, wash the laminated film of assembling, by washed with de-ionized water, nitrogen drying under room temperature;
6), in step 5) in a side of substrate of gained, rotary coating macromolecular solution A, then rotary coating coordinative solvent at least 2 times;
7), in step 6) in a side of substrate of gained, rotary coating nano-particle solution C carries out self-assembly, then rotary coating coordinative solvent, washes away the nanoparticle of unnecessary physical adsorption;
8), repeating step 6 alternately) and step 7) repeatedly, until the macromolecule/nano particle laminated film of the upper required number of plies of substrate surface assembling, taking-up, what obtain is optical window material;
9), by controlling step 4) and step 8) multiplicity, adjusting obtains obtains optical window material;
Washing lotion is the vitriol oil and hydrogen peroxide mixed solution, and volume ratio is 8:3-6:4;
Described macromolecular solution A is polyethyleneimine: amine aqueous solution; Nano-particle solution B used is tin indium oxide nano-particle solution; Described nano-particle solution C is zinc oxide nano-particle solution.
6. according to the method for claim 5, it is characterized in that, described its concentration of macromolecular solution A is 0.5-30mg/mL; Nano-particle solution B concentration used is 1.0-5.0mg/mL; Described nano-particle solution C concentration is 1.0-5.0mg/mL.
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