CN1553219A - Preparing method for nanometer porous silica thin-membrane - Google Patents
Preparing method for nanometer porous silica thin-membrane Download PDFInfo
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- CN1553219A CN1553219A CNA2003101095335A CN200310109533A CN1553219A CN 1553219 A CN1553219 A CN 1553219A CN A2003101095335 A CNA2003101095335 A CN A2003101095335A CN 200310109533 A CN200310109533 A CN 200310109533A CN 1553219 A CN1553219 A CN 1553219A
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Abstract
The preparing method is as the follows, positive silester is used as presoma alcohol as solvent and ammonia water as well as hydrochloric acid as catalysts, they are become basic and acidic soliquid after hydrolyzation and polycondensation are carried out silica soliquid can be obtained by further polycondensation and hydrolyzation after basic silica soliquid is agitated in some acidic soliquid, a complete nanomultihole network structure which is not simply piled up can be formed by closely combining particles to be film when using acidic soliquid as coupling agent to link basic soliquid particles together.
Description
Technical field
The invention belongs to the optical thin film preparing technical field, be specifically related to a kind of preparation method with silicon dioxide optical film of nano-porous structure.
Background technology
Traditional film plating process has physical methods such as magnetron sputtering, electron beam evaporation, vacuum thermal evaporation, but be lower than 1.38 solid-state material owing to utilize current material can't obtain refractive index, the membrane structure of physical method preparation simultaneously is also comparatively single, add the process of physical method complexity and high cost, limited the widespread use of optical thin film.Sol-gel process is the chemical synthesis and preparation method of material, compare with traditional physical method have that process is simple, cost is low, controllable structure, to be suitable for various base materials, refractive index adjustable continuously and can have unique advantages aspect the preparation optical thin film to advantages such as material synthesize on molecular scale.Refractive index on a large scale in continuously adjustable optical thin film, can be used for preparing optical anti-reflective film, high film, electrochromic film, heat mirror, guide membrane etc., have broad application prospects in fields such as light laser, display system, energy-conservation, intellectual material, optical communications.The at present domestic report that does not also have about refractive index adjustable optical method for manufacturing thin film.
Summary of the invention
The object of the present invention is to provide a kind of preparation method with silicon dioxide optical film of nano-porous structure.
The preparation method of the silicon dioxide optical film that the present invention proposes, concrete steps are:
1, alkaline SiO
2The preparation of colloidal sol: with ethyl orthosilicate (TEOS), ethanol, water are raw material, and ammoniacal liquor is catalyzer.With TEOS, ammoniacal liquor, second alcohol and water at room temperature mix by following mol ratio, stir, still aging 3-7 days, form colloidal sol with white opalescence, then with colloidal sol under 60-100 ℃, backflow 6-10 hour, remove ammonia wherein, the pH value of last colloidal sol is about 7-9.Because the eliminating of catalyzer ammonia, hydrolysis and polycondensation reaction have obtained effective control, and colloidal sol is more stable.Wherein, ethyl orthosilicate: ammoniacal liquor: ethanol: water=(0.5～3): (1.0～5.0): (20～85): (0.3～0.9).
2, acid SiO
2The preparation of colloidal sol: with ethyl orthosilicate, ethanol, water are raw material, and hydrochloric acid is catalyzer.TEOS, hydrochloric acid, second alcohol and water are at room temperature mixed by following mol ratio, stir, still aging 1-2 days, become acid SiO
2Colloidal sol.Ethyl orthosilicate: hydrochloric acid: ethanol: water=(0.5～3): (1.3～5.0): (20～85): (0.1～0.95).
3, the soda acid two-step catalysis prepares silicon dioxide gel: with acid SiO
2Colloidal sol joins alkaline SiO by following mol ratio
2In the colloidal sol, mixed at room temperature, stirring and then backflow 2-6 hour, obtained the more stable SiO of performance
2Colloidal sol; Acid SiO
2Colloidal sol: alkaline SiO
2Colloidal sol=(0.01-3): 1.
4, the preparation of silicon dioxide optical film: adopt dip-coating method or spin-coating method on glass or monocrystal silicon substrate, to prepare SiO
2Film.Pull rate is 7～30cm/min; Rotational speed is 1000～4000r/min.
5, the thermal treatment of film: silica membrane was heated 45-90 minute down at 80-120 ℃.
Utilize the present invention can prepare individual layer, double-layer reflection-decreasing rete, or preparation is used for the sol-gel broadband silicon dioxide antireflecting film of solar thermal collector etc.
The present invention controls the refractive index of film by the voidage in the soda acid two-step catalysis reaction control film.Acid SiO
2SiO in the colloidal sol
2Cluster is network of fibers shape structure, and it plates the film refractive index height, alkaline SiO
2SiO in the colloidal sol
2Cluster is porous prilled structure, and its institute's film refractive index that plates is low, with acid SiO
2Colloidal sol and alkaline SiO
2Colloidal sol is entrained in together by different proportion, can obtain the film of different refractivity.Among the present invention, the hole size of film is controlled at several nanometers to tens nanometers, little more a lot of than common optical wavelength, so film is a uniform dielectric concerning common light wave, its macroscopic reflectance and volume density (hole ratio) are closely related, can regulate its refractive index continuously by the hole ratio of stepless control film.The present invention adopts sol-gelatin plating method, and this method is at room temperature carried out, and thickness is controlled easily, and membranous layer ingredient is even.And sol-gel process to prepare optical thin film equipment needed thereby investment little, be converted into suitability for industrialized production easily.
Description of drawings
Fig. 1 is film refractive index and relation diagram sour, alkaline colloidal sol molar ratio.When not adding acidic sol, alkaline SiO
2The refractive index of film is low to be about 1.18, along with acid SiO
2The refractive index of the adding film of colloidal sol increases sharply, as: when acidic sol: when alkaline colloidal sol mol ratio is 0.1, the refractive index of film is 1.23, and when this ratio rises to 0.8, refractive index rapidly increases to 1.35, when ratio was increased to 1.0, it is just relatively milder that refractive index increases, when pure acidic sol 1.43.Realized like this refractive index 1.18～1.43 adjustable continuously.
Fig. 2 is the different product structures under different acid, the base catalyst reaction.
Fig. 3 is silica membrane surface microscopic topographic diagram.
Embodiment
The invention will be further described below by embodiment, but this invention is not limited in the following examples.
Embodiment 1: with ethyl orthosilicate (TEOS analyze pure), ethanol (adopt anhydrous, analyze pure), water is raw material, and ammoniacal liquor is catalyzer.At first with ethyl orthosilicate, ammoniacal liquor, ethanol and deionized water in room temperature with certain molar ratio (1: 2.0: 35: 0.3) mix, stir, ethyl orthosilicate and water issue unboiled water in the ammonia-catalyzed effect and separate reaction, between the hydroxyl that forms in the hydrolysis reaction polycondensation reaction takes place simultaneously, at room temperature still aging 3 days, form colloidal sol with white opalescence, then colloidal sol was refluxed 8 hours at 80 ℃, remove ammonia wherein, make alkaline SiO
2Colloidal sol.With TEOS, hydrochloric acid (pH=1), ethanol and deionized water with 1: 2.3: 38: 0.245 mixed in molar ratio, stir, at room temperature still aging 1.5 days, make acid SiO
2Colloidal sol.With acid SiO
2Colloidal sol joins alkaline SiO with 2.5: 1.0 mol ratios
2In the colloidal sol, mixed at room temperature, stirring, and then refluxed 3 hours, obtained the more stable SiO of performance
2Colloidal sol.Be lower than in relative humidity and adopt dip-coating method on the K9 film substrate, to prepare SiO in 60% the cleaning ambient
2Film.Pull rate is 12cm/min; Rotational speed is 1500r/min.At last film was heated 1 hour gained silica membrane refractive index 1.41 (optical wavelength 632.8nm place) down at 100 ℃.
Embodiment 2: with ethyl orthosilicate (TEOS analyzes pure), absolute ethyl alcohol (analyzing pure), water is raw material, and ammoniacal liquor is catalyzer.At first with ethyl orthosilicate, ammoniacal liquor, ethanol and deionized water with certain molar ratio (0.5: 1.5: 25: 0.3) mix, stir at room temperature still aging 5 days, formation has the colloidal sol of white opalescence, then colloidal sol was refluxed 7 hours at 90 ℃, remove ammonia wherein, make alkaline SiO
2Colloidal sol.With TEOS, hydrochloric acid (pH=1), ethanol and deionized water with 0.6: 2.0: 26: 0.145 mixed in molar ratio, stir, at room temperature still aging 1 day, become acid SiO
2Colloidal sol.With acid SiO
2Colloidal sol joins alkaline SiO with 2.0: 1.0 mol ratios
2In the colloidal sol, mixed at room temperature, stirring and then refluxed 4.5 hours have obtained the more stable SiO of performance
2Colloidal sol.Be lower than in relative humidity and adopt dip-coating method on the K9 film substrate, to prepare SiO in 60% the cleaning ambient
2Film.Pull rate is 20cm/min; Rotational speed is 1000～r/min.At last film was heated 50 minutes gained silica membrane refractive index 1.38 (optical wavelength 632.8nm place) down at 90 ℃.
Embodiment 3: with ethyl orthosilicate (TEOS analyzes pure), absolute ethyl alcohol (analyzing pure), water is raw material, and ammoniacal liquor is catalyzer.At first with ethyl orthosilicate, ammoniacal liquor, ethanol and deionized water with certain molar ratio (1: 2.0: 45: 0.3) mix, stir at room temperature still aging 7 days, formation has the colloidal sol of white opalescence, then colloidal sol was refluxed 8 hours at 110 ℃, remove ammonia wherein, make alkaline SiO
2Colloidal sol.With TEOS, hydrochloric acid (pH=1), ethanol and deionized water with 0.7: 2.1: 28: 0.165 mixed in molar ratio, stir, at room temperature still aging 2 days, become acid SiO
2Colloidal sol.With acid SiO
2Colloidal sol joins alkaline SiO with 1.0: 1.0 mol ratios
2In the colloidal sol, mixed at room temperature, stirring and then refluxed 4 hours have obtained the more stable SiO of performance
2Colloidal sol.Be lower than in relative humidity and adopt dip-coating method on the K9 film substrate, to prepare SiO in 60% the cleaning ambient
2Film.Pull rate is 21cm/min; Rotational speed is 3500r/min.Last film heated 45 minutes gained silica membrane refractive index 1.35 (optical wavelength 632.8nm place) down at 120 ℃.
Embodiment 4: with ethyl orthosilicate (TEOS analyzes pure), absolute ethyl alcohol (analyzing pure), water is raw material, and ammoniacal liquor is catalyzer.At first with ethyl orthosilicate, ammoniacal liquor, ethanol and deionized water with certain molar ratio (2.0: 3.0: 65: 0.6) mix, stir at room temperature still aging 7 days, formation has the colloidal sol of white opalescence, then colloidal sol was refluxed 6 hours at 100 ℃, remove ammonia wherein, make alkaline SiO
2Colloidal sol.With TEOS, hydrochloric acid (pH=1), ethanol and deionized water with 2.0: 4.0: 78: 0.7 mixed in molar ratio, stir, at room temperature still aging 1 day, become acid SiO
2Colloidal sol.With acid SiO
2Colloidal sol joins alkaline SiO with 0.25: 1.0 mol ratio
2In the colloidal sol, mixed at room temperature, stirring and then refluxed 6 hours have obtained the more stable SiO of performance
2Colloidal sol.Be lower than in relative humidity and adopt dip-coating method on the K9 film substrate, to prepare SiO in 60% the cleaning ambient
2Film.Pull rate is 7cm/min; Rotational speed is 1000r/min.Last film heated 1 hour gained silica membrane refractive index 1.27 (optical wavelength 632.8nm place) down at 85 ℃.
Embodiment 5: preparation double-layer reflection-decreasing rete.Acidic sol: the film (refractive index is 1.20) that the component of alkaline colloidal sol=0.06 forms constitutes with the film (refractive index is 1.43) that pure acidic sol forms.Film layer structure is: air/alkaline film/acid film/substrate.Double-deck variable refractivity film cording has good wide band antireflective effect, makes that the average reflectance of K9 substrate of glass is the (400nm～760nm), and reflectivity curve is more smooth that 8.70% is reduced to 0.44%.
Embodiment 6: preparation is used for the sol-gel broadband silicon dioxide antireflecting film of solar thermal collector.Acidic sol: the film (refractive index is 1.20) that the component of alkaline colloidal sol=0.06 forms constitutes with the film (refractive index is 1.43) that pure acidic sol forms.Film layer structure is: air/alkaline film/acid film/glass.In 300～2500nm wave band, be respectively 1.43 and 1.20 monofilm for refractive index, average reflectance is about 5.20% and 2.60%, and refractive index is 1.43 and 1.20 duplicatures of forming, average reflectance is about 1.50%, and these reflectivity all are starkly lower than not plated film sample (average reflectance is 6.90%); Wherein the reflectance curve of duplicature has the reflectivity lower than monofilm, and the wave band of antiradar reflectivity is wideer than the monofilm.
Claims (3)
1. the preparation method of a nano-stephanoporate silicon dioxide optical thin film is characterized in that specifically may further comprise the steps:
(1) alkaline SiO
2The preparation of colloidal sol: with ethyl orthosilicate, ethanol, water are raw material, and ammoniacal liquor is catalyzer, with ethyl orthosilicate, ammoniacal liquor, second alcohol and water at room temperature mix by following mol ratio, stir, still aging 3-7 days, form colloidal sol with white opalescence, then with colloidal sol under 60-100 ℃, backflow 6-10 hour, remove ammonia wherein, the pH value of last colloidal sol is 7-9; Wherein, ethyl orthosilicate: ammoniacal liquor: ethanol: water=(0.5～3): (1.0～5.0): (20～85): (0.3～0.9);
(2) acid SiO
2The preparation of colloidal sol: with ethyl orthosilicate, ethanol, water are raw material, and hydrochloric acid is catalyzer.Ethyl orthosilicate, hydrochloric acid, second alcohol and water are at room temperature mixed by following mol ratio, stir, still aging 1-2 days, become acid SiO
2Colloidal sol; Ethyl orthosilicate: hydrochloric acid: ethanol: water=(0.5～3): (1.3～5.0): (20～85): (0.1～0.95);
(3) the soda acid two-step catalysis prepares silicon dioxide gel: with acid SiO
2Colloidal sol joins alkaline SiO by following mol ratio
2In the colloidal sol, mixed at room temperature, stirring and then backflow 2-6 hour, obtain SiO
2Colloidal sol, acid SiO
2Colloidal sol: alkaline SiO
2Colloidal sol=(0.01-3): 1;
(4) preparation of silicon dioxide optical film: adopt dip-coating method or spin-coating method on the K9 substrate of glass, to prepare SiO
2Film, pull rate are 7～30cm/min; Rotational speed is 1000～4000r/min;
(5) thermal treatment of film: film heated 45-90 minute down at 80-120 ℃.
2, nano-stephanoporate silicon dioxide optical thin film according to claim 1 is characterized in that the application of double-layer reflection-decreasing rete.
3, nano-stephanoporate silicon dioxide optical thin film according to claim 1 is characterized in that the application of the sol-gel broadband silicon dioxide antireflecting film of solar thermal collector.
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