CN102633444A - Method for preparing optical window material - Google Patents
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- CN102633444A CN102633444A CN2012101209068A CN201210120906A CN102633444A CN 102633444 A CN102633444 A CN 102633444A CN 2012101209068 A CN2012101209068 A CN 2012101209068A CN 201210120906 A CN201210120906 A CN 201210120906A CN 102633444 A CN102633444 A CN 102633444A
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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 the 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, does not receive substrate sizes, shape, whether restriction such as plane.
Background technology
Sunshine is the main 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 outstanding day by day, and sunshine is when guaranteeing human daily need, and a large amount of harm rays that wherein contain have had influence on human orthobiosis gradually.Excessive solar radiation can all be brought tremendous influence to HUMAN HEALTH, article, energy-conserving and environment-protective etc.: (1) is to the influence of human body.Mainly be meant the injury that ultraviolet ray causes eyesight skin, eyesight and infrared rays.Over-exposure can make skin surface general red in ultraviolet ray, loses former flexiblely, tarnish, and skin aging, even canceration can take place.Eyes receive uviolizing for a long time, can cause cornea, retina, crystalline chain etc. impaired, visual deterioration, vertical line pain, symptom such as shed tears.High-intensity infrared rays can make tissue necrosis, protein coagulating, and the cataract that causes like short infrared, day photosensitiveness retina choroid burn etc., simultaneously, infrared rays also can aggravate UV-induced skin carcinoma.(2) to the influence of article.Article can fade under periods of direct sunlight in many indoor and the cars.Seeing through of harmful light can be caused fading, wear out etc. of article such as instrument desk, seat in indoor carpet, family property, artwork, curtain and the car.(3) to the influence of energy-conserving and environment-protective.Infrared rays has tangible heat effect, especially the near infrared part.As far as the buildings or the transportation means of 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 sunshine, when guaranteeing visible light transmissive, isolated excessive ultraviolet ray, infrared rays become an important research project.
Conventional solution to the problems described above mainly contains and uses heat reflection metal coating glass, mounts sun-proof thermal isolation film etc.But there is following shortcoming in above product: visible light permeability is poor, can not make full use of it; Reflectivity is high, and the secondary light that causes is polluted comparatively serious; Metal coating is prone to oxidation, the isolated and transparent effect of influence.By comparison, utilize functional nanomaterials to handle glass surface, the preventing ultraviolet of acquisition/near infrared light radiative material; Have characteristics such as antiradar reflectivity, high-clarity; And its making method is simple and easy, the cycle short, and material is easy to get, therefore; Utilize functional nanomaterials (like tin indium oxide because it has two isolated property of UV-light/infrared light and visible transparent property, 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 preparation preventing ultraviolet/near infrared light radiation transparent material certainly will cause extensive concern.
Alternately the 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; Like electrostatic force, Van der Waals force, coordination, close and distant water effect etc., realize that the difference in functionality material alternately grows into film in substrate.Utilize alternately stratiform self-assembling technique, select to have the nano material of specific function, can prepare multiple functional film.Than traditional film technique; Like sputtering technology, gas phase deposition technology, electron beam coating technique etc.; Advantage such as that this method has is easy to operate, the apparatus and process requirement is simple, and to size, the shape of substrate, whether the plane does not require, and is a kind of new technology that has than the great development potentiality.
Therefore, in conjunction with replacing stratiform self-assembling technique and functional nanomaterials, constructing preventing ultraviolet/infrared radiation transparent material will become the research focus.
Summary of the invention
It is a kind of based on the interactional optical window preparation methods of supramolecule that the object of the invention is to provide; 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 based on the interactional optical window preparation methods of supramolecule; It is characterized in that: alternately stratiform self-assembling technique is adopted in this invention; Its essence is that the coordination that utilizes between nanoparticle and polymer interacts; Rely on this linkage force, form stable macromolecule/nano particle laminated film, especially combine the alternately self-assembly of ultrasonic technique.
Of the present invention a kind ofly it is characterized in that,, specifically may further comprise the steps in conjunction with ultrasonic technique or spin coating and stratiform self-assembling technique alternately based on the interactional optical window preparation methods of supramolecule:
1), quartz plate or silicon chip are cleaned with washing lotion, uses washed with de-ionized water quartz plate, silicon chip again, dry up with nitrogen;
2), the substrate of gained in the step 1) is placed macromolecular solution A, leave standstill, take out the back that reaches capacity, with coordinative solvent flushing, nitrogen drying under the room temperature;
3), with step 2) in the substrate of gained place nano-particle solution B, ultrasound condition soaks down, take out the back that reaches capacity, with coordinative solvent flushing, nitrogen drying under the room temperature;
4), repeating step 2 alternately) and step 3), go up the macromolecule/nano particle laminated film of the required number of plies until the substrate surface assembling.
Another kind of the present invention is characterized in that based on the interactional optical window preparation methods of supramolecule, may further comprise the steps:
1), with cleaning with washing lotion at the bottom of quartz plate or the silicon wafer-based, use washed with de-ionized water quartz plate, silicon chip again, dry up with nitrogen;
2), in step 1) in the substrate of gained, rotation applies macromolecular solution A, rotation applies coordinative solvent at least 2 times again; Preferred 3-5 time.
3), in step 2) in the substrate of gained, rotation coated nanoparticles solution C is carried out self-assembly, rotation applies coordinative solvent, the nanoparticle of the physical adsorption that flush away is unnecessary again;
4), repeating step 2 alternately) with step 3) repeatedly, go up the macromolecule/nano particle laminated film of the required number of plies until the substrate surface assembling, taking-up, what obtain is the optical window material.
Aforesaid method of the present invention is to carry out self-assembly in a side of substrate, perhaps carries out self-assembly respectively simultaneously in both sides.
Another kind of the present invention is characterized in that based on the interactional optical window preparation methods of supramolecule, may further comprise the steps:
1), quartz plate or silicon chip are cleaned with washing lotion, uses washed with de-ionized water quartz plate, silicon chip again, dry up with nitrogen;
2), the substrate of gained in the step 1) is placed macromolecular solution A, leave standstill, take out the back that reaches capacity, with coordinative solvent flushing, nitrogen drying under the room temperature;
3), with step 2) in the substrate of gained place nano-particle solution B, ultrasound condition soaks down, take out the back that reaches capacity, with coordinative solvent flushing, nitrogen drying under the room temperature;
4), repeating step 2 alternately) and step 3), go up the macromolecule/nano particle laminated film of the required number of plies until the 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, use washed with de-ionized water, nitrogen drying under the room temperature;
6), a side of the substrate of gained in step 5), rotation applies macromolecular solution A, rotation applies coordinative solvent at least 2 times again; Preferred 3-5 time;
7), a side of the substrate of gained in step 6), rotation coated nanoparticles solution C is carried out self-assembly, rotation applies coordinative solvent, the nanoparticle of the physical adsorption that flush away is unnecessary again;
8), repeating step 6 alternately) with step 7) repeatedly, go up the macromolecule/nano particle laminated film of the required number of plies until the substrate surface assembling, taking-up, what obtain is the optical window material;
9), through controlled step 4) and the multiplicity of step 8), can regulate the window material that obtains.Window material has the isolated effect of UV-light/infrared light.
Above-mentioned three kinds based in the interactional optical window preparation methods of supramolecule, washing lotion is the vitriol oil and hydrogen peroxide mixed solution, volume ratio is 8: 3-6: 4 all can.
Said macromolecular solution A is the polyethyleneimine: amine aqueous solution, and its concentration is 0.5-30mg/mL, preferred 1.0mg/mL, solvent for use can polymines in this area all can, for example water, ethanol etc.
Used nano-particle solution B is the tin indium oxide nano-particle solution, and its concentration is 1.0-5.0mg/mL, and solvent for use is the solvent of the routine of this area solubilized tin indium oxide nanoparticle, for example ethanol, ETHYLE ACETATE, butylacetate etc.
Used nano-particle solution C, described nano-particle solution C are zinc oxide nano-particle solution, and its concentration is 1.0-5.0mg/mL, and solvent for use is the solvent of the routine of this area solubilized zinc oxide nano-particle, for example 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 that the coordination that utilizes between nanoparticle and polymer interacts; Rely on this linkage force, form stable macromolecule/nano particle laminated film.After substrate was cleaned through the vitriol oil/hydrogen peroxide mixed solution, the surface had a large amount of hydroxyls.The substrate that has hydroxyl is immersed in the polyethyleneimine: amine aqueous solution, and polymine and substrate surface group interact, at substrate surface absorption last layer macromolecule membrane; After the tin indium oxide nano-particle solution is immersed in above-mentioned substrate; Because ultrasonic booster action; The tin indium oxide nanoparticle singly is dispersed in the solution uniformly; Utilize the coordination of tin indium oxide nanoparticle and polymine to interact,, evenly adsorb the monodispersed tin indium oxide nanoparticulate thin films of one deck on the macromolecule membrane surface of substrate; After the polymine macromolecular solution was immersed in above-mentioned substrate once more, polymine and nanoparticle generation coordination interacted, and on the nanoparticulate thin films surface of substrate, evenly adsorbed layer of polyethylene imines macromolecule membrane; Alternately soak assembling through substrate at polymine macromolecular solution and tin indium oxide nano-particle solution, can obtain uniform polymine/tin indium oxide nanoparticle laminated film at substrate surface.Clean a side of above-mentioned substrate through the vitriol oil, make the laminated film of this side be cleaned, expose a large amount of oh groups that exist of substrate surface.Adopt the spin coating package technique; In the exposed side of substrate; Through replacing coating polyethylene imines macromolecular solution and zinc oxide nano-particle solution; Be similar to the mechanism of action of polymine/tin indium oxide nanoparticle laminated film, utilize between polymer and the substrate and the coordination between polymer and the nanoparticle interacts, realize at the bottom of this side group on the constructing of polymine/zinc oxide nano-particle laminated film.Optical window material through above-mentioned a series of processes prepare when having guaranteed good visible light permeability, has the two isolated effects of excellent UV-light/near infrared light, and can regulate its isolated effect through changing alternatively stacked number of times.As a comparison; Adopt tradition to replace the stratiform assemble method in the research process and constructed polymine/tin indium oxide nanoparticle laminated film; The result shows; Adopt the polymine/tin indium oxide nanoparticle laminated film of the present invention's preparation to have the good transparency, it has significantly improved the visible region transmitance.Prepare nano thin-film than methods such as sputters, this invention equipment requirements simple, easy to operate, controllability is strong, do not receive substrate size, shape, whether limit on the plane.
The invention provides three kinds of similar methods, can select voluntarily as required.For example, first method has visible transparent property, the near infrared light that mainly isolated wavelength is shorter than the 300nm UV-light and is longer than 1400nm; Second method mainly intercepts the UV-light that wavelength is shorter than 350nm, and visible light and near infrared light are had good perviousness; The third method has combined preceding two kinds of methods, when guaranteeing the visible light highly transparent, has effectively completely cut off the near infrared light that wavelength is shorter than the 350nm UV-light and is longer than 1400nm.Appeal three kinds of methods and all have 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 the automobile industry, avoids the problems such as fading, wear out that the article long-term exposure causes under periods of direct sunlight in the car.
3, optical window material of the present invention, effectively barrier material both sides heat transmits, and reduces energy waste, can be used for environmental protection industry (epi), realizes 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, satisfies 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 does not receive shapes of substrates, size, whether limit on the plane.
Description of drawings
Fig. 1. the ultraviolet-visible-near infrared transmittance curve variation diagram of two isolated window materials of the UV-light/near infrared light of the embodiment of the invention 1 preparation and blank example.
Fig. 2. the polymine/tin indium oxide nanoparticle laminated film of the embodiment of the invention 5 preparations and Comparative Examples 1 are soaked the film laminated film ultraviolet-visible of the same race-near infrared transmittance curve variation diagram of assembling preparation.
Fig. 3. polymine/tin indium oxide nanoparticle laminated film (one-sided 10 bilayers) scanning electron microscope diagram of the embodiment of the invention 6 preparations.
Fig. 4. Comparative Examples 2 is soaked polymine/tin indium oxide nanoparticle laminated film (one-sided 10 bilayers) scanning electron microscope diagram of assembling preparation.
Fig. 5. the polymine/zinc oxide nano-particle laminated film ultraviolet-visible transmittance curve variation diagram of the embodiment of the 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 invention 8 preparations.
The practical implementation method
Below in conjunction with examples of implementation and accompanying drawing technical scheme of the present invention is done further to describe:
Blank example:
1, select substrate for use---the 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, and at room temperature with nitrogen the transparent substrates surface is dried up again.
2, isolation performance test: substrate is placed ultraviolet-visible-near infrared spectrometer, is scanning background with the air, and test substrate is the perviousness change curve in wavelength is the 200-1800nm scope, and record, and is as shown in Figure 1.
Comparative Examples 1 result shows that the transmitance of blank quartz plate in the test wavelength region is certain value basically, 93%.
Embodiment 1:
1, the quartz plate substrate is immersed in the vitriol oil/hydrogen peroxide mixed solution (volume ratio is 7: 3), and scavenging period is 60min, uses washed with de-ionized water, with nitrogen the surface is dried up;
2, the quartz plate that cleans up is placed the polymine ethanolic soln, concentration is 1mg/mL, leaves standstill 10min, takes out, and with the absolute ethyl alcohol flushing, with nitrogen the surface is dried up;
3, the quartz plate with gained in the step 2 places tin indium oxide nanoparticle ethyl acetate solution, and concentration is 4mg/mL, and ultrasound condition soaks 10min down, takes out, and uses rinsed, with nitrogen the surface is dried up;
4, replace repeating step 2 and step 3 many times, repeat n time and be designated as one-sided be n+1 bilayer, n=19;
5, with a side a of the quartz plate that obtains in the vitriol oil cleaning step 4, scavenging period is 300min, uses deionized water rinsing, with nitrogen the surface is dried up;
6, a side of the quartz plate of gained in step 5, rotation coating polyethylene imines ethanolic soln, concentration is 1mg/mL; Speed of rotation is 3000 rpms, and rotational time is 30s, and rotation applies ethanol 3 times again; Speed of rotation is 3000 rpms, and rotational time is 30s.
7, a side of the quartz plate of gained in step 6, rotation applies the zinc oxide nano-particle ethanolic soln, and concentration is 4mg/mL; Speed of rotation is 3000 rpms, and rotational time is 30s, and rotation applies ethanol 3 times again; Speed of rotation is 3000 rpms, and rotational time is 30s.
8, replace repeating step 6 and step 7 many times, inferior one-sided m+1 bilayer, the m=29 of being designated as of Repeated m.
9, isolation performance test: the quartz plate substrate is placed ultraviolet-visible-near infrared spectrometer; With the air is scanning background, and after test procedure 5 finished back and step 8 end respectively, substrate is the transmitance change curve in wavelength 200-1800nm scope; And record, as shown in Figure 2.
Embodiment 1 test result shows that after step 5 finished, a side was coated with the quartz plate substrate of polymine/tin indium oxide nanoparticle laminated film, and in its wavelength 400-1000nm scope, visible light transmissivity maintains about 90%; In the 200-400nm scope, begin uv transmittance from 325nm and begin obvious decline, until about 200nm, reaching 0%; In the 1000-1800nm scope, increase with wavelength, transmitance presents progressively downtrending, and is behind 1600nm, basicly stable about 25%.After step 8 finishes; One side is coated with polymine/tin indium oxide nanoparticle laminated film, and opposite side is coated with the quartz plate substrate of polymine/zinc oxide nano-particle laminated film, in its wavelength 400-1000nm scope; Visible light transmissivity maintains 83-90%, is higher than 85% basically; In the 200-400nm scope, begin uv transmittance from 380nm and begin to descend, and sharply drop to 23% at the 350nm place, 290nm reduces to 10% in the place, reaches 0% about 240nm; In the 1000-1800nm scope, increase with wavelength, transmitance presents progressively downtrending, and is behind 1600nm, basicly stable about 20%.
Blank example, embodiment 1 show; This invention has effectively completely cut off the UV-light of wavelength below 350nm; Transmitance is lower than 25%, isolated effect is higher than 75%, and the near infrared light of wavelength more than 1000nm, about the above transmitance of 1600nm is stabilized in 20%, isolated effect is near 80%.For the visible light of wavelength at 400-800nm, the transparency has effectively been kept in this invention, and transmitance is higher than 85% basically between 83-90%.
Embodiment 2:
1, the quartz plate substrate is immersed in the vitriol oil/hydrogen peroxide mixed solution (volume ratio is 7: 3), and scavenging period is 60min, uses washed with de-ionized water, with nitrogen the surface is dried up;
2, the quartz plate that cleans up is placed the polymine ethanolic soln, concentration is 1mg/mL, leaves standstill 10min, takes out, and with the absolute ethyl alcohol flushing, with nitrogen the surface is dried up;
3, the quartz plate with gained in the step 2 places tin indium oxide nanoparticle ethyl acetate solution, and concentration is 4mg/mL, and ultrasound condition soaks 10min down, takes out, and uses rinsed, with nitrogen the surface is dried up;
4, replace repeating step 2 and step 3 many times, repeat n time and be designated as one-sided be n+1 bilayer, n=19,39,59;
5, with a side a of the quartz plate that obtains in the vitriol oil cleaning step 4, scavenging period is 300min, uses deionized water rinsing, with nitrogen the surface is dried up;
6, a side of the quartz plate of gained in step 5, rotation coating polyethylene imines ethanolic soln, concentration is 1mg/mL; Speed of rotation is 3000 rpms, and rotational time is 30s, and rotation applies ethanol 3 times again; Speed of rotation is 3000 rpms, and rotational time is 30s.
7, a side of the quartz plate of gained in step 6, rotation applies the zinc oxide nano-particle ethanolic soln, and concentration is 4mg/mL; Speed of rotation is 3000 rpms, and rotational time is 30s, and rotation applies ethanol 3 times again; Speed of rotation is 3000 rpms, and rotational time is 30s.
8, alternately repeating step 6 and step 7 many times, Repeated m time are designated as one-sided be m+1 bilayer, m=29.
9, isolation performance test: the quartz plate substrate is placed ultraviolet-visible-near infrared spectrometer, is scanning background with the air, and after test procedure 5 finished back and step 8 end respectively, substrate transmitance in wavelength 200-1800nm scope changed, and record.
Embodiment 2 test results show, are accompanied by the increase of polymine/tin indium oxide nanoparticle laminated film number of plies, and the transparency of resultant product changes little; The isolated effect of near infrared significantly strengthens, and drops to 0% gradually by 20%; The isolated effect of ultraviolet region also strengthens to some extent, but effect and not obvious, this mainly be since the isolated wavelength of the ultraviolet of zinc oxide than tin indium oxide longer due to.
Embodiment 3:
1, the quartz plate substrate is immersed in the vitriol oil/hydrogen peroxide mixed solution (volume ratio is 7: 3), and scavenging period is 60min, uses washed with de-ionized water, with nitrogen the surface is dried up;
2, the quartz plate that cleans up is placed the polymine ethanolic soln, concentration is 1mg/mL, leaves standstill 10min, takes out, and with the absolute ethyl alcohol flushing, with nitrogen the surface is dried up;
3, the quartz plate with gained in the step 2 places tin indium oxide nanoparticle ethyl acetate solution, and concentration is 4mg/mL, and ultrasound condition soaks 10min down, takes out, and uses rinsed, with nitrogen the surface is dried up;
4, replace repeating step 2 and step 3 many times, repeat n time and be designated as one-sided be n+1 bilayer, n=19;
5, with a side a of the quartz plate that obtains in the vitriol oil cleaning step 4, scavenging period is 300min, uses deionized water rinsing, with nitrogen the surface is dried up;
6, a side of the quartz plate of gained in step 5, rotation coating polyethylene imines ethanolic soln, concentration is 1mg/mL; Speed of rotation is 3000 rpms, and rotational time is 30s, and rotation applies ethanol 3 times again; Speed of rotation is 3000 rpms, and rotational time is 30s.
7, a side of the quartz plate of gained in step 6, rotation applies the zinc oxide nano-particle ethanolic soln, and concentration is 4mg/mL; Speed of rotation is 3000 rpms, and rotational time is 30s, and rotation applies ethanol 3 times again; Speed of rotation is 3000 rpms, and rotational time is 30s.
8, alternately repeating step 6 and step 7 many times, Repeated m time are designated as one-sided be m+1 bilayer, m=4,9,14.
9, isolation performance test: the quartz plate substrate is placed ultraviolet-visible-near infrared spectrometer, is scanning background with the air, and after test procedure 5 finished back and step 8 end respectively, substrate transmitance in wavelength 200-800nm scope changed, 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 resultant product transparency changes little; The isolated effect of ultraviolet region strengthens significantly, and the isolated effect of ultraviolet that is mainly reflected in the beginning of 350nm place improves constantly.
Blank example, embodiment 1-3 test result show that the optical window material of this invention preparation has isolated property of excellent UV-light/near infrared light and good visible transparent property, and its UV-light/near infrared light general layout effect has controllability.
Embodiment 4:
1, the 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 the surface is dried up.
2, the quartz plate that cleans up is placed the polymine ethanolic soln, concentration is 1mg/mL, leaves standstill 10min, takes out, and with the absolute ethyl alcohol flushing, with nitrogen the surface is dried up.
3, the quartz plate with gained in the step 2 places tin indium oxide nanoparticle ethyl acetate solution, and concentration is 4mg/mL, and ultrasound condition soaks 10min down, takes out, and uses rinsed, with nitrogen the surface is dried up.
4, replace repeating step 2 and step 3 many times, repeat n time and be designated as one-sided be n+1 bilayer, n=0-7.
5, isolation performance test: substrate is placed ultraviolet-visible-near infrared spectrometer, is scanning background with the air, and test substrate changes at wavelength 200-800nm scope internal absorbance, and record.
Embodiment 4 test results show; The surface has the quartz plate of polymine/tin indium oxide nanoparticle laminated film; Visible region does not have absorption, and the ultraviolet region absorption peak is in the 200-325nm wavelength region, and 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 the 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, the 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 the surface is dried up.
2, the quartz plate that cleans up is placed the polymine ethanolic soln, concentration is 1mg/mL, leaves standstill 10min, takes out, and with the absolute ethyl alcohol flushing, with nitrogen the surface is dried up.
3, the quartz plate with gained in the step 2 places tin indium oxide nanoparticle ethyl acetate solution, and concentration is 4mg/mL, and ultrasound condition soaks 10min down, takes out, and uses rinsed, with nitrogen the surface is dried up.
4, replace repeating step 2 and step 3 many times, repeat n time and be designated as one-sided be n+1 bilayer, n=9,19,29.
5, isolation performance test: substrate is placed ultraviolet-visible-near infrared spectrometer, is scanning background with the air, and test substrate is the perviousness change curve in wavelength is the 200-1800nm scope, and record, and is as shown in Figure 2.
Embodiment 5 test results show that the surface has the quartz plate of polymine/tin indium oxide nanoparticle laminated film, and visible region does not have obvious absorption, but with the increase of n, average visible light transmissivity progressively reduces, and is respectively 92%, 88%, 85%; It is isolated that ultraviolet takes place in the 200-325nm wavelength region, and 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; It is isolated that near infrared takes place in the 1000-1800nm wavelength region, and transmitance reaches stationary value after wavelength is longer than 1600nm, and along with the increase of n, 1600nm place transmitance is respectively about 15%, 5%, 1%, presents the rising tendency of isolated effect to double-deck number.
Blank example, embodiment 4-5 show; Polymine/tin indium oxide nanoparticle the laminated film of this invention preparation; Can be through 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 bigger influence.
Embodiment 6
1, immerse in the vitriol oil/hydrogen peroxide mixed solution (volume ratio is 7: 3) at the bottom of the silicon wafer-based, scavenging period is 60min, and at room temperature water cleans, and with nitrogen the surface is dried up.
2, the quartz plate that cleans up is placed the polymine ethanolic soln, concentration is 1mg/mL, leaves standstill 10min, takes out, and with the absolute ethyl alcohol flushing, with nitrogen the surface is dried up.
3, the quartz plate with gained in the step 2 places tin indium oxide nanoparticle ethyl acetate solution, and concentration is 4mg/mL, and ultrasound condition soaks 10min down, takes out, and uses rinsed, with nitrogen the surface is dried up.
4, replace repeating step 2 and step 3 many times, repeat n time and be designated as one-sided be 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 show that in the polymine that this invention obtains/tin indium oxide nanoparticle laminated film, the tin indium oxide nanoparticle exists with monodisperse particles shape form, and internal structure is even, regular, fine and close.
Comparative Examples 1
1, the 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 the surface is dried up.
2, the quartz plate that cleans up is placed the polymine ethanolic soln, concentration is 1mg/mL, leaves standstill 10min, takes out, and with the absolute ethyl alcohol flushing, with nitrogen the surface is dried up.
3, the quartz plate with gained in the step 2 places tin indium oxide nanoparticle ethyl acetate solution, and concentration is 4mg/mL, soaks 10min, takes out, and uses rinsed, with nitrogen the surface is dried up.
4, replace repeating step 2 and step 3 many times, repeat n time and be designated as one-sided be n+1 bilayer, n=9,19,29.
5, isolation performance test: substrate is placed ultraviolet-visible-near infrared spectrometer, is scanning background with the air, and test substrate is the perviousness change curve in wavelength is the 200-1800nm scope, and record, and is as shown in Figure 2.
Comparative Examples 1 test result shows; The surface has the quartz plate of polymine/tin indium oxide nanoparticle laminated film, and its transmittance curve presents unimodal variation between the test zone, and visible region has obvious absorption; Maximum transmission is about the 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 fully, and the near infrared light transmitance that wavelength is longer than 1400nm reaches stationary value, is about 10%; When n=19, wavelength is shorter than the UV-light of 300nm is isolated fully, and wavelength is longer than the near infrared light of 1350nm by isolated fully; When n=29, wavelength is shorter than the UV-light of 330nm isolates fully, and wavelength is longer than the near infrared light of 1220nm by isolated fully.
Blank example, Comparative Examples 1 show that tradition is soaked the alternately polymine/tin indium oxide nanoparticle laminated film of stratiform self-assembling method preparation, have outstanding isolated ultraviolet/near infrared performance, but visible light permeability is extremely low, and influence is used.
Comparative Examples 2
1, immerse in the vitriol oil/hydrogen peroxide mixed solution (volume ratio is 7: 3) at the bottom of the silicon wafer-based, scavenging period is 60min, and at room temperature water cleans, and with nitrogen the surface is dried up.
2, the quartz plate that cleans up is placed the polymine ethanolic soln, concentration is 1mg/mL, leaves standstill 10min, takes out, and with the absolute ethyl alcohol flushing, flush time is 1min, with nitrogen the surface is dried up.
3, the quartz plate with gained in the step 2 places tin indium oxide nanoparticle ethyl acetate solution, and concentration is 4mg/mL, soaks 10min, takes out, and uses rinsed, and flush time is 1min, with nitrogen the surface is dried up.
4, replace repeating step 2 and step 3 many times, repeat n time and be designated as one-sided be 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 Examples 2 test results show; Traditional immersion replaces in polymine/tin indium oxide nanoparticle laminated film that the stratiform self-assembling method obtains, and the tin indium oxide nanoparticle exists with the 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 Examples 1 and 2 test results show; Replace the stratiform self-assembling method than traditional immersion; The ultrasonic subsidiary conditions that this invention is introduced have effectively increased the order degree that nanoparticle is arranged; Improve 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, the 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 the surface is dried up.
2, quartz plate is placed on the rotation sol evenning machine, at one of which side a rotation coating polyethylene imines ethanolic soln, concentration is 1mg/mL; Speed of rotation is 3000 rpms, and rotational time is 30s, and rotation applies ethanol 3 times again; Speed of rotation is 3000 rpms, and rotational time is 30s.
3, a side of gained quartz plate in step 2, rotation applies the zinc oxide nano-particle ethanolic soln, and concentration is 4mg/mL; Speed of rotation is 3000 rpms, and rotational time is 30s, and rotation applies ethanol 3 times again; Speed of rotation is 3000 rpms, and rotational time is 30s.
4, alternately repeating step 2 and step 3 many times, every Repeated m time are designated as one-sided be m+1 bilayer, m=4,9,14,19,24,29.
5, isolation performance test: substrate is placed ultraviolet-visible-near infrared spectrometer; With the air is scanning background, and test substrate is at wavelength 200-800nm scope internal absorbance change curve, and in the 200-1800nm scope transmitance change curve; And record, as shown in Figure 5.
Embodiment 7 absorbancy change curve test results show that the surface has the quartz plate of polymine/tin indium oxide nanoparticle laminated film, and visible region does not have absorption fully; At wavelength in the 360-350nm scope; Absorbancy is undergone mutation, and sharply rises, and is characteristic absorbance; After wavelength was shorter than 340nm, absorbancy shortened with wavelength and slowly rises gradually.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 the 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 that the surface has the quartz plate of polymine/tin indium oxide nanoparticle laminated film, and the visible region transmitance maintains more than 85% basically.In the 360-350nm scope, transmitance sharply descends at wavelength, and after wavelength was shorter than 340nm, permeability shortened with wavelength and slowly descends.Along with the increase of m value, the transmitance value at its 340nm place presents progressively downtrending.
Blank example, embodiment 7 test results show that this invention can reach the ability of regulating its isolated ultraviolet, and visible light permeability is not had bigger influence through regulating the alternating growth number of plies of polymine polymer and zinc oxide nano-particle.
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; Have higher isolation performance at ultraviolet region, isolated wave band is longer, improves isolation performance.
Embodiment 8
1, immerse in the vitriol oil/hydrogen peroxide mixed solution (volume ratio is 7: 3) at the bottom of the silicon wafer-based, scavenging period is 60min, and at room temperature water cleans, and with nitrogen the surface is dried up.
2, silicon chip is placed on the rotation sol evenning machine, at one of which side a rotation coating polyethylene imines ethanolic soln, concentration is 1mg/mL; Speed of rotation is 3000 rpms, and rotational time is 30s, and rotation applies ethanol 3 times again; Speed of rotation is 3000 rpms, and rotational time is 30s.
3, a side of gained silicon chip in step 2, rotation applies the zinc oxide nano-particle ethanolic soln, and concentration is 4mg/mL; Speed of rotation is 3000 rpms, and rotational time is 30s, and rotation applies ethanol 3 times again; Speed of rotation is 3000 rpms, and rotational time is 30s.
4, alternately repeating step 2 and step 3 many times, every Repeated m time are designated as one-sided be m+1 bilayer, m=0,29.
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 show that in the polymine that this invention obtains/zinc oxide nano-particle laminated film, zinc oxide nano-particle exists with single discrete form, and is tightly packed, and internal structure is regular, even, fine and close.
Claims (9)
1. one kind based on the interactional optical window preparation methods of supramolecule, it is characterized in that, in conjunction with ultrasonic technique or spin coating and stratiform self-assembling technique alternately, specifically may further comprise the steps:
1), quartz plate or silicon chip are cleaned with washing lotion, uses washed with de-ionized water quartz plate, silicon chip again, dry up with nitrogen;
2), the substrate of gained in the step 1) is placed macromolecular solution A, leave standstill, take out the back that reaches capacity, with coordinative solvent flushing, nitrogen drying under the room temperature;
3), with step 2) in the substrate of gained place nano-particle solution B, ultrasound condition soaks down, take out the back that reaches capacity, with coordinative solvent flushing, nitrogen drying under the room temperature;
4), repeating step 2 alternately) and step 3), go up the macromolecule/nano particle laminated film of the required number of plies until the substrate surface assembling;
Said macromolecular solution A is the polyethyleneimine: amine aqueous solution, and used nano-particle solution B is the tin indium oxide nano-particle solution.
2. according to the method for claim 1, it is characterized in that, said macromolecular solution A, its concentration is 0.5-30mg/mL, used nano-particle solution B, its concentration is 1.0-5.0mg/mL.
3. according to the method for claim 1, it is characterized in that washing lotion is the vitriol oil and hydrogen peroxide mixed solution, volume ratio is 8: 3-6: 4 all can.
4. one kind based on the interactional optical window preparation methods of supramolecule, it is characterized in that, may further comprise the steps:
1), with cleaning with washing lotion at the bottom of quartz plate or the silicon wafer-based, use washed with de-ionized water quartz plate, silicon chip again, dry up with nitrogen;
2), in step 1) in the substrate of gained, rotation applies macromolecular solution A, rotation applies coordinative solvent at least 2 times again;
3), in step 2) in the substrate of gained, rotation coated nanoparticles solution C is carried out self-assembly, rotation applies coordinative solvent, the nanoparticle of the physical adsorption that flush away is unnecessary again;
4), repeating step 2 alternately) with step 3) repeatedly, go up the macromolecule/nano particle laminated film of the required number of plies until the substrate surface assembling, taking-up, what obtain is the optical window material;
Said macromolecular solution A is the polyethyleneimine: amine aqueous solution, and described nano-particle solution C is a zinc oxide nano-particle solution;
Aforesaid method is to carry out self-assembly in a side of substrate, perhaps carries out self-assembly respectively simultaneously in both sides.
5. according to the method for claim 4, it is characterized in that said 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.
6. according to the method for claim 4, it is characterized in that washing lotion is the vitriol oil and hydrogen peroxide mixed solution, volume ratio is 8: 3-6: 4 all can.
7. one kind based on the interactional optical window preparation methods of supramolecule, it is characterized in that, may further comprise the steps:
1), quartz plate or silicon chip are cleaned with washing lotion, uses washed with de-ionized water quartz plate, silicon chip again, dry up with nitrogen;
2), the substrate of gained in the step 1) is placed macromolecular solution A, leave standstill, take out the back that reaches capacity, with coordinative solvent flushing, nitrogen drying under the room temperature;
3), with step 2) in the substrate of gained place nano-particle solution B, ultrasound condition soaks down, take out the back that reaches capacity, with coordinative solvent flushing, nitrogen drying under the room temperature;
4), repeating step 2 alternately) and step 3), go up the macromolecule/nano particle laminated film of the required number of plies until the 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, use washed with de-ionized water, nitrogen drying under the room temperature;
6), a side of the substrate of gained in step 5), rotation applies macromolecular solution A, rotation applies coordinative solvent at least 2 times again;
7), a side of the substrate of gained in step 6), rotation coated nanoparticles solution C is carried out self-assembly, rotation applies coordinative solvent, the nanoparticle of the physical adsorption that flush away is unnecessary again;
8), repeating step 6 alternately) with step 7) repeatedly, go up the macromolecule/nano particle laminated film of the required number of plies until the substrate surface assembling, taking-up, what obtain is the optical window material;
9), through controlled step 4) with the multiplicity of step 8), adjusting obtains obtains the optical window material;
Said macromolecular solution A is the polyethyleneimine: amine aqueous solution; Used nano-particle solution B is the tin indium oxide nano-particle solution; Described nano-particle solution C is a zinc oxide nano-particle solution.
8. according to the method for claim 1, it is characterized in that said its concentration of macromolecular solution A is 0.5-30mg/mL; Used nano-particle solution B concentration is 1.0-5.0mg/mL; Described nano-particle solution C concentration is 1.0-5.0mg/mL.
9. washing lotion is the vitriol oil and hydrogen peroxide mixed solution, and volume ratio is 8: 3-6: 4 all can.
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