CN101655610A - Preparation method of inverse opal hydrogel photonic crystal with hybridized structure - Google Patents
Preparation method of inverse opal hydrogel photonic crystal with hybridized structure Download PDFInfo
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Abstract
The invention provides a preparation method of inverse opal hydrogel photonic crystal with hybridized structure. Polymer interpenetrating network method is adopted to prepare the crystal. The preparation method has the advantages that: the raw materials are polyacrylic acid and polyacrylamide which are available, and the preparation method includes two filling gather steps and is simple and practicable; the polyacrylic acid and polyacrylamide respectively contains carboxyl and amide functional group, thus realizing pH and solvent sense response, and not only the pattern obtained by hybridizedstructure can be converted between display state and disappeared state but also reversible transformation among multiple color states such as yellow, green and blue can be realized by controlling pH value or alcohol content in water.
Description
Technical field
The invention provides a kind of preparation method with inverse opal hydrogel photonic crystal of hybrid structure.
Background technology
Photonic crystal is a kind of periodic structure that is made of at space-alternating the material with different refractivity, and its most basic feature is to have forbidden photon band, drops on promptly that only being under an embargo in the forbidden band propagate.Because the existence of forbidden photon band, people can realize the controlling of various wavelength light obtained various new optical devices by the design forbidden band.Wherein, thus can under different environmental stimulis, regulate the propagation of the position control light of forbidden photon band significantly with the photonic crystal that hydrogel is constructed.This material is developed to various sensors, display and biomimetic material gradually.The structure of constructing hydrogel photonic crystal usually has crystal group colloid array structure, opal structural and counter opal structure, and wherein counter opal structure is because it has poriness helps quick sensing have very big advantage in hydrogel photonic crystal is used.At present, by environmental stimuli can display color stimulation-responsive gel photonic crystal (H.Fudouzi etal, Langmuir, 2003,19,9653 of pattern; K.Matsubara, Angew.Chem.Int.Ed.2007,46,1688) be developed, thereby being expected to be applied to novel photon paper/black system, this photon crystal material substitutes traditional paper/China ink and intelligent bionic material.But the multicolour pattern that this gel photonic crystal shows under environmental stimuli only has the variation of demonstration/disappearance two states, and except that above-mentioned binary states display capabilities, the exploitation that the pattern of demonstration has the photonic crystal display material of multicolour ability to transform will promote the further application of photonic crystal in field of display.To achieve these goals, people such as Y.J.Kang adopt the PS-QP2VP segmented copolymer to prepare the upper strata and have the pattern of multicolour ability to transform and double-deck salt response 1-D photon crystal (the Y.J.Kang et al that lower floor has blue background by covering plate coating and control degree of crosslinking method, Nat Mater, 2007,6,957).Although realized pattern conversion between multicolour in the document,, limited it and used widely because the material cost of using is higher and the upper layer pattern demonstration is subjected to lower floor's background influence.One of approach that solves this difficult problem is to adopt the polymer interpenetration network method.This method has been applied to the preparation (Z.B.Hu et al, Science, 1995,269,525) of double layer hybridized body hydrogel at present.The specific practice of polymer interpenetration network method is to be packed into first kind of hydrophilic polymer monomer solution, polymerization then between two tool glass sheet at regular intervals.Be immersed in after resulting first kind of thin polymer film separates between two glass sheet and carry out the secondary filling second kind of hydrophilic polymer monomer solution, film after will filling again is sandwiched in and carries out the polymerization second time between two glass sheet, this moment, the spacing of two glass sheet was greater than thin polymer film after the filling, second kind of polymer monomer is filled between this two glass sheet, separates two glass sheet after the polymerization and promptly obtains double layer hybridized body hydrogel.For inverse opal hydrogel photonic crystal, in the preparation method, also do not find to adopt the preparation method of polymer interpenetration network with hybrid structure.
Summary of the invention
The objective of the invention is to overcome the shortcoming that prior art exists, a kind of preparation method with inverse opal hydrogel photonic crystal of hybrid structure is provided, described photonic crystal has hybrid structure, the pattern that is formed by the polyacrylamide inverse opal photonic crystal and form complete inverse opal hydrogel photonic crystal film by the pattern that polyacrylamide and polyacrylic acid interpenetrating polymer network inverse opal photonic crystal form; Polyacrylamide and polyacrylic acid are water-soluble polymerss, form hydrogel by chemical crosslinking, are that the inverse opal photonic crystal of material preparation is inverse opal hydrogel photonic crystal by these water-soluble polymerss.Thereby polyacrylic acid and polyacrylamide hydrophilic gel cause variation on the gel volume to influence the grating constant of photonic crystal to ethanol water or pH sensitivity, can be the bandgap center position or the change color of the above-mentioned pattern that is formed by hybrid structure of may command by ethanol content or pH value in the regulation and control water therefore.Resulting pattern is to obtain by covering the plate photoetching process in the hybrid structure.Inverse opal photonic crystal is the inverse structure of opal photonic crystal, is to obtain by the colloidal crystal template synthetic method, is about to the opaline colloidal crystal as template, more polymerisable monomer solution is packed into opaline colloidal crystal, polymerization then.After the polymerization again selective removal opaline colloidal crystal just obtain inverse opal photonic crystal.
A kind of preparation method with inverse opal hydrogel photonic crystal of hybrid structure comprises the steps:
(1) earlier the monodispersed silicon dioxide microsphere of homogeneous is dispersed in the ethanol, be configured to the solution that massfraction is a 0.5%-4% concentration, again this solution is poured in the clean container, at last the vertical liquid level of clean substrate is inserted in the above-mentioned container that monodisperse silica microspheres solution is housed, be positioned in the airtight environment that week age makes silicon dioxide microsphere deposit to substrate surface under room temperature, form the opaline colloidal crystal at substrate surface; Described substrate is glass or silicon chip; Described silicon dioxide microsphere sphere diameter is 180nm-300nm;
(2) the vertical liquid level of substrate that the surface that obtains in the step (1) is formed the opaline colloidal crystal immerses 3min in the polyacrylic acid monomers solution, the polyacrylic acid monomers solution concentration is 1M-5M, containing massfraction in the polyacrylic acid monomers solution is the crosslinking chemical N of 1%-10%, N '-methylene-bisacrylamide and massfraction are 3% light trigger 1-hydroxy cyclohexyl phenylketone, polyacrylic acid monomers solution is packed in the hole of opaline colloidal crystal, then, another is clean microslide covers its surface formation by this substrate, the sandwich structure that opaline colloidal crystal and microslide form; And then plate is covered in photoetching covered above the microslide, polyacrylic acid monomers is carried out uv photopolymerization 1min, and ultraviolet wavelength is 365nm, after the polymerization, to go up layer photoetching and cover the plate removal, remove unpolymerized polyacrylic acid monomers solution between microslide and the substrate with deionized water rinsing;
(3) this sandwich structure after step (2) processing is immersed in the polyacrylamide monomer solution, filled polypropylene amide monomer 12h, described polyacrylamide monomer solution concentration is 1M-5M, the polyacrylamide monomer solution contains the crosslinking chemical N that massfraction is 1-10%, N '-methylene-bisacrylamide and massfraction are 0.5% light trigger 1-hydroxy cyclohexyl phenylketone, take out the uv photopolymerization 15min that this sandwich structure carries out the polyacrylamide amine monomers, ultraviolet wavelength is 365nm, after the polymerization, it is 24h in 10% the silicon dioxide etching liquid hydrofluorite that resulting this sandwich structure is immersed massfraction, remove silicon dioxide opaline colloidal crystal, microslide separates the resulting film in back with substrate be the inverse opal hydrogel photonic crystal with hybrid structure.Concrete structure as shown in Figure 1.
Beneficial effect: compared with the prior art, the present invention adopts the preparation of polymer interpenetration network method to have the inverse opal hydrogel photonic crystal of hybrid structure.This preparation method's advantage is that raw material is that polyacrylic acid and polyacrylamide are cheap and easy to get, and the preparation method uses and fills polymerization procedure twice, and is simple; Polyacrylic acid and polyacrylamide contain carboxyl respectively and the acid amides functional group can be realized pH and solvent sensing response, not only can between demonstration and disappearance two states, change by ethanol content in control pH value or the water by the pattern that hybrid structure obtained, but also can realize that pattern is between the multicolour state as from the redness to the yellow, green, blue reversible transformation.
Description of drawings
Fig. 1 is the inverse opal hydrogel photonic crystal basic structure synoptic diagram with hybrid structure.Among the figure, 1 is the counter opal polyacrylamide; 2 is counter opal polyacrylamide/polyacrylic acid interpenetrating polymer network.
Embodiment
(1) earlier the monodispersed silicon dioxide microsphere of homogeneous is dispersed in the ethanol, be configured to the solution that massfraction is 4% concentration, again this solution is poured in the clean container, at last the vertical liquid level of clean substrate is inserted in the above-mentioned container that monodisperse silica microspheres solution is housed, be positioned in the airtight environment that week age makes silicon dioxide microsphere deposit to substrate surface under room temperature, form the opaline colloidal crystal at substrate surface; Described substrate is glass or silicon chip; Described silicon dioxide microsphere sphere diameter is 180nm;
(2) the vertical liquid level of substrate that the surface that obtains in the step (1) is formed the opaline colloidal crystal immerses 3min in the polyacrylic acid monomers solution, the polyacrylic acid monomers solution concentration is 5M, contain massfraction in the polyacrylic acid monomers solution and be 10% crosslinking chemical N, N '-methylene-bisacrylamide and massfraction are 3% light trigger 1-hydroxy cyclohexyl phenylketone, polyacrylic acid monomers solution is packed in the hole of opaline colloidal crystal, then, another is clean microslide covers its surface formation by this substrate, the sandwich structure that opaline colloidal crystal and microslide form; And then plate is covered in photoetching covered above the microslide, polyacrylic acid monomers is carried out the 1min uv photopolymerization, and ultraviolet wavelength is 365nm, after the polymerization, to go up layer photoetching and cover the plate removal, remove unpolymerized polyacrylic acid monomers solution between microslide and the substrate with deionized water rinsing;
(3) this sandwich structure after step (2) processing is immersed in the polyacrylamide monomer solution, filled polypropylene amide monomer 12h, described polyacrylamide monomer solution concentration is 5M, it is 10% crosslinking chemical N that the polyacrylamide monomer solution contains massfraction, N '-methylene-bisacrylamide and massfraction are 0.5% light trigger 1-hydroxy cyclohexyl phenylketone, take out the 15min uv photopolymerization that this sandwich structure carries out the polyacrylamide amine monomers, ultraviolet wavelength is 365nm, after the polymerization, it is that 24h removes silicon dioxide opaline colloidal crystal in 10% the silicon dioxide etching liquid hydrofluorite that resulting this sandwich structure is immersed massfraction, and microslide separates the resulting film in back with substrate be the inverse opal hydrogel photonic crystal with hybrid structure.
(1) earlier the monodispersed silicon dioxide microsphere of homogeneous is dispersed in the ethanol, be configured to the solution that massfraction is 1% concentration, again this solution is poured in the clean container, at last the vertical liquid level of clean substrate is inserted in the above-mentioned container that monodisperse silica microspheres solution is housed, be positioned in the airtight environment that week age makes silicon dioxide microsphere deposit to substrate surface under room temperature, form the opaline colloidal crystal at substrate surface; Described substrate is glass or silicon chip; Described silicon dioxide microsphere sphere diameter is 232nm;
(2) the vertical liquid level of substrate that the surface that obtains in the step (1) is formed the opaline colloidal crystal immerses 3min in the polyacrylic acid monomers solution, the polyacrylic acid monomers solution concentration is 4M, contain massfraction in the polyacrylic acid monomers solution and be 5% crosslinking chemical N, N '-methylene-bisacrylamide and massfraction are 3% light trigger 1-hydroxy cyclohexyl phenylketone, polyacrylic acid monomers solution is packed in the hole of opaline colloidal crystal, then, another is clean microslide covers its surface formation by this substrate, the sandwich structure that opaline colloidal crystal and microslide form; And then plate is covered in photoetching covered above the microslide, polyacrylic acid monomers is carried out the 1min uv photopolymerization, and ultraviolet wavelength is 365nm, after the polymerization, to go up layer photoetching and cover the plate removal, remove unpolymerized polyacrylic acid monomers solution between microslide and the substrate with deionized water rinsing;
(3) this sandwich structure after step (2) processing is immersed in the polyacrylamide monomer solution, filled polypropylene amide monomer 12h, described polyacrylamide monomer solution concentration is 4M, it is 5% crosslinking chemical N that the polyacrylamide monomer solution contains massfraction, N '-methylene-bisacrylamide and massfraction are 0.5% light trigger 1-hydroxy cyclohexyl phenylketone, take out the 15min uv photopolymerization that this sandwich structure carries out the polyacrylamide amine monomers, ultraviolet wavelength is 365nm, after the polymerization, it is that 24h removes silicon dioxide opaline colloidal crystal in 10% the silicon dioxide etching liquid hydrofluorite that resulting this sandwich structure is immersed massfraction, and microslide separates the resulting film in back with substrate be the inverse opal hydrogel photonic crystal with hybrid structure.
Embodiment 3
(1) earlier the monodispersed silicon dioxide microsphere of homogeneous is dispersed in the ethanol, be configured to the solution that massfraction is 0.5% concentration, again this solution is poured in the clean container, at last the vertical liquid level of clean substrate is inserted in the above-mentioned container that monodisperse silica microspheres solution is housed, be positioned in the airtight environment that week age makes silicon dioxide microsphere deposit to substrate surface under room temperature, form the opaline colloidal crystal at substrate surface; Described substrate is glass or silicon chip; Described silicon dioxide microsphere sphere diameter is 300nm;
(2) the vertical liquid level of substrate that the surface that obtains in the step (1) is formed the opaline colloidal crystal immerses 3min in the polyacrylic acid monomers solution, the polyacrylic acid monomers solution concentration is 1M, contain massfraction in the polyacrylic acid monomers solution and be 1% crosslinking chemical N, N '-methylene-bisacrylamide and 3% light trigger 1-hydroxy cyclohexyl phenylketone, polyacrylic acid monomers solution is packed in the hole of opaline colloidal crystal, then, another is clean microslide covers the sandwich structure that its surface formation is formed by this substrate, opaline colloidal crystal and microslide; And then plate is covered in photoetching covered above the microslide, polyacrylic acid monomers is carried out the 1min uv photopolymerization, and ultraviolet wavelength is 365nm, after the polymerization, to go up layer photoetching and cover the plate removal, remove unpolymerized polyacrylic acid monomers solution between microslide and the substrate with deionized water rinsing;
(3) with being immersed in the polyacrylamide monomer solution after step (2) processing, filled polypropylene amide monomer 12h, described polyacrylamide monomer solution concentration is 1M, it is 1% crosslinking chemical N that the polyacrylamide monomer solution contains massfraction, N '-methylene-bisacrylamide and massfraction are 0.5% light trigger 1-hydroxy cyclohexyl phenylketone, take out the 15min uv photopolymerization that this sandwich structure carries out the polyacrylamide amine monomers, ultraviolet wavelength is 365nm, after the polymerization, it is that 24h removes silicon dioxide opaline colloidal crystal in 10% the silicon dioxide etching liquid hydrofluorite that resulting this sandwich structure is immersed massfraction, and microslide separates the resulting film in back with substrate be the inverse opal hydrogel photonic crystal with hybrid structure.
Claims (1)
1, a kind of preparation method with inverse opal hydrogel photonic crystal of hybrid structure is characterized in that step is as follows:
(1) earlier the monodispersed silicon dioxide microsphere of homogeneous is dispersed in the ethanol, be configured to the solution that massfraction is a 0.5%-4% concentration, again this solution is poured in the clean container, at last the vertical liquid level of clean substrate is inserted in the above-mentioned container that monodisperse silica microspheres solution is housed, be positioned in the airtight environment that week age makes silicon dioxide microsphere deposit to substrate surface under room temperature, form the opaline colloidal crystal at substrate surface; Described substrate is glass or silicon chip; Described silicon dioxide microsphere sphere diameter is 180nm-300nm;
(2) the vertical liquid level of substrate that the surface that obtains in the step (1) is formed the opaline colloidal crystal immerses 3min in the polyacrylic acid monomers solution, the polyacrylic acid monomers solution concentration is 1M-5M, containing massfraction in the polyacrylic acid monomers solution is the crosslinking chemical N of 1%-10%, N '-methylene-bisacrylamide and massfraction are 3% light trigger 1-hydroxy cyclohexyl phenylketone, polyacrylic acid monomers solution is packed in the hole of opaline colloidal crystal, then, another is clean microslide covers its surface formation by this substrate, the sandwich structure that opaline colloidal crystal and microslide form; And then plate is covered in photoetching covered above the microslide, polyacrylic acid monomers is carried out uv photopolymerization 1min, and ultraviolet wavelength is 365nm, after the polymerization, to go up layer photoetching and cover the plate removal, remove unpolymerized polyacrylic acid monomers solution between microslide and the substrate with deionized water rinsing;
(3) this sandwich structure after step (2) processing is immersed in the polyacrylamide monomer solution, filled polypropylene amide monomer 12h, described polyacrylamide monomer solution concentration is 1M-5M, the polyacrylamide monomer solution contains the crosslinking chemical N that massfraction is 1-10%, N '-methylene-bisacrylamide and massfraction are 0.5% light trigger 1-hydroxy cyclohexyl phenylketone, take out the uv photopolymerization 15min that this sandwich structure carries out the polyacrylamide amine monomers, ultraviolet wavelength is 365nm, after the polymerization, it is 24h in 10% the silicon dioxide etching liquid hydrofluorite that resulting this sandwich structure is immersed massfraction, remove silicon dioxide opaline colloidal crystal, microslide separates the resulting film in back with substrate be the inverse opal hydrogel photonic crystal with hybrid structure.
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