CN103698846A - Preparation method of flexible metal photonic crystal - Google Patents
Preparation method of flexible metal photonic crystal Download PDFInfo
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Abstract
The invention discloses a preparation method of flexible metal photonic crystal and belongs to the technical field of nano photonic materials and devices. The method comprises the steps of preparing a photoresist nano grating structure on a buffer layer of a buffer layer substrate, dissolving and spin-coating gold nanoparticle colloid on the surface of grating and limiting the coating gold nanoparticle colloid in a groove of the grating, performing heating processing, so as to ensure that organic ligand on gold surface is sublimed and gold nanoparticle is fused, so as to form metal photonic crystal, coating flexible substrate liquid mixed with curing agent on the metal photonic crystal, covering another buffer layer substrate, heating the metal photonic crystal to perform cross-linking polymerization, putting the metal photonic crystal into a hydrochloric acid solution or a sulfuric acid solution, so as to sufficiently dissolve the buffer layer, and cleaning obtained samples through distilled water. The method has important direct application value for developing stress and deformation sensors and novel flexible optoelectronic devices.
Description
Technical field
The invention belongs to nano-photon material and device technology field, relate to the preparation method of a kind of flexible metal photonic crystal.
Background technology
Metal photonic crystal is a kind of important form of photonic crystal, also simultaneously because the special light physics characteristics such as its plasmon become a kind of relatively independent nano-photon version.Metal photonic crystal has many-sided irreplaceable using value in photoelectron technology, sensor technology and optical engineering, and develops into important field of research of nanophotonics.This makes the technology of preparing of metal photonic crystal highlight its significance.Requirement for technology of preparing is mainly reflected in simple process, prepare that area is large, with low cost, efficiency is high, be suitable for the aspects such as batch production, thereby can provide basic technical guarantee for the through engineering approaches application of nano-photon device.
" flexibility " is an importance of nano-photon structure function always.Realize " flexibility " and not only enriched the form of fabrication technology and nano-photon structure, the more important thing is the application category of greatly having expanded the nano-devices such as photonic crystal, the application that particularly cannot use at common flat device, for development and the application of flexible device provides wide development space.The most directly, flexible device can be applicable to all kinds of stress, deformation, displacement sensing device, and can be integrated with all kinds of optics, optoelectronic system, realizes the function of its " plasmon " and " photonic crystal " device under special space and shape condition.
In currently used flexibility photonic crystal technology of preparing, nano impression is unique more ripe and technology of preparing of being widely adopted.Although this method can realize the preparation of large-area nano photon structure, exist preparation technology more complicated, in transfer process, introduce defect, cause repeatability and success ratio to reduce, and be subject to material category to affect the problems such as larger.Particularly nanometer embossing is not yet realized the preparation of metal photonic crystal.Like this, a kind of simple process is needed in the preparation of flexible photonic crystal badly, the batch technology of preparing that success ratio is high.
Up to the present also there is not the cycle of preparation in flexible substrate at the metal photonic crystal of nanometer scale.This is mainly attributed to the multiple challenges that relevant nano preparation technique relates to.
The present invention, just for the problems referred to above, has proposed a kind of technique simple, practical, and success ratio reaches cycle of 100% in the metal photonic crystal structure large area of nanometer scale, technology of preparing in batches.
Summary of the invention
It is complete, harmless at the suprabasil metal photonic crystal of the hard plates such as glass that core content of the present invention is to have realized preparation, and success ratio 100% ground is transferred to flexible substrate, as PDMS, silicone adhesive, glass cement material substrate, obtain ductility, bendability, the good plasmon nanostructured of pliability periodic array.
A kind of metal photonic crystal preparation method based on flexible substrate of the present invention, is characterized in that, comprises the following steps:
(1) on flat base, prepare cushion, obtain cushion matrix, on cushion, prepare again photoresist (PR) nanometer grating structure (as shown in Figure 1a);
(2) gold nano grain of chemosynthesis (Au NP) is formed to colloidal solution in dimethylbenzene, the dimethylbenzene colloidal solution of gold nano grain is spin-coated on to the surface of step (1) photoresist nanometer grating, under surface tension effects, gold nano grain is limited to (as shown in Figure 1 b) in grating groove;
(3) sample on the cushion matrix of being prepared by step (2) is in 200-450 ℃ of (preferably 350 ℃) muffle furnace after thermal treatment, make organic ligand distillation on gold nano grain surface, the abundant melting of gold nano grain, all enter in grating groove, and form continuous nanowires of gold (as shown in Fig. 1 c) along grating groove, on the surface of cushion matrix, successfully prepared the metal photonic crystal that Crystal structure forms;
(4) the flexible substrate liquid that is mixed with hardening agent is coated on to metal photonic crystal surface prepared by step (3), then top covers another sheet cushion matrix again, and buffering aspect is contacted with flexible substrate liquid, both sides between two cushion matrixes are supported with silicone rubber pad, to guarantee to obtain even thickness, controlled flexible substrate (as shown in Fig. 1 d and Fig. 1 e);
(5) by the sample making in step (4) 100-120 ℃ of heating, complete flexible substrate cross-linking polymerization, preferably 45 minutes-1 hour heat time;
(6) sample step (5) being obtained is placed in hydrochloric acid or sulfuric acid solution, cushion on upper and lower two matrixes is fully dissolved, flexible substrate and on the metal photonic crystal of combining closely from matrix, separate (as shown in Figure 1 f) up hill and dale;
(7) flexible device finally step (6) being obtained cleans with distilled water, removes remaining acid solution and issuable impurity, obtains independently flexible device (as shown in Figure 1 g), completes the preparation of flexible metal photonic crystal.
The preferred PDMS of flexible substrate described above, silicone adhesive, glass cement material substrate.The material of cushion is the materials such as the metal that is dissolved in hydrochloric acid or sulfuric acid, metal oxide, and can be by technological process preparations such as hot evaporation, magnetron sputtering, pulsed laser depositions on flat plate substrate, preferably ITO layer.
Above-mentioned matrix adopting is insoluble to the solution such as hydrochloric acid, sulfuric acid and can stands the transparent material of 450 ℃ of following heat treatment process, as glass, quartz.
There is dentate metal nanoparticle material on the surface that is applicable to be insoluble to hydrochloric acid or sulfuric acid that gold nano grain described above replaces with other.
Preferred: upper and lower two on-chip ITO layers are used as cushion, the silicone rubber pad that is 1mm with thickness is therebetween isolated, and controls thickness and the depth of parallelism of final flexible substrate.Device integral body is completed to cross-linking polymerization for 50-60 minute as for heating in the baking oven of 100 ℃.After cooling, in the hydrochloric acid of 20%-30%, soak 2 hours, realize peeling off of glass substrate and PDMS, thereby realize metal photonic crystal to the transfer printing on PDMS.Flexible metal photonic crystal device is cleaned in deionized water, remove other impurity of residual hydrochloric acid and surface attachment, after being dried under room temperature, complete the preparation of device.
Metal photonic crystal structure on ito glass substrate can adopt the preparation method of the various nano-photon structures such as solwution method, hot vapour deposition method, reactive ion beam dry corrosion method.It is the restriction that in the present invention, preparation method is not subject to photonic crystal preparation method.
Utilize insoluble in hydrochloric acid and sulfuric acid of nano-photon structure that in Waveguide coupling metal photonic crystal, noble metal and dielectric material (ducting layer and template grating material) form, and ducting layer material-indium tin-oxide (ITO) good dissolution characteristics therein, and good pliability and the stability of the dimethyl silicone polymer after cross-linked polymeric (PDMS), realized the complete transfer printing of metal photonic crystal from ito glass hard substrate to PDMS, its success ratio can reach 100%.Thereby obtained flexible metal photon crystal device.This device is for exploitation stress, changing sensor, and novel flexible optoelectronic device has important direct application value.
Advantageous feature of the present invention:
(1) the present invention has realized the preparation of metal photonic crystal in flexible substrate, and its core technology is to realize the complete transfer printing of metal photonic crystal from glass substrate to PDMS.In fact, this technology is not subject to metal photonic crystal preparation method's restriction.
(2) preparation method is easy, easily capable, and without expensive equipment, complicated technological process, the material of special expensive, accurate controlling and technical ability, preparation process is efficient.
(3) utilize the soluble characteristic of cushion metal oxide in hydrochloric acid and sulfuric acid, realize the completely harmless transfer printing of metal photonic crystal from hard ito glass flat plate substrate to PDMS flexible substrate, the success ratio of transfer printing process reaches 100%.
(4) size of flexible substrate and thickness can arbitrarily be controlled as required, do not affect the transfer printing process of metal photonic crystal.
(5) be applicable to the transfer printing of metal photon structure and the preparation of flexible device of attainable any period, size, be not subject to the impact of metal photon structure shape, dimension.
Accompanying drawing explanation
The preparing technique process process schematic diagram of Fig. 1, the metal photonic crystal based on flexible substrate;
Photo in kind and the diffraction pattern thereof of Fig. 2, flexible metal photon crystal device;
A:PDMS flexible substrate; B: metal photonic crystal and the diffraction pattern under white light thereof.
The electron micrograph image of Fig. 3, the metal photonic crystal of preparation on ito glass;
Fig. 4, be transferred to the electron micrograph image of the metal photonic crystal on PDMS;
Fig. 5, be transferred to the atomic force microscopy image of the metal photonic crystal on PDMS;
The stretching sensing experiment of Fig. 6, flexible metal photonic crystal;
A: be prepared in the metal photonic crystal in PDMS flexible substrate, B: fixed support, C: translation stage, D: the white light source of collimation, E: condenser lens, F: collimation lens, G: fiber spectrometer fibre-optical probe, H: fiber spectrometer;
The definition of Fig. 7, flexible metal photonic crystal deformation transducing signal amplitude (A);
The test result of Fig. 8, the stretching of flexible metal photonic crystal and return curve.
Embodiment:
The present invention is further illustrated in conjunction with the embodiments, but the present invention is not limited to following examples.Embodiment 1: the preparation of flexible metal photonic crystal.
(1) be coated with on the glass substrate of 200nm indium tin oxide (ITO) film, with 2000rpm rotating speed spin coating S1805 photoresist.
(2) adopt the He-Cd laser that wavelength is 325nm in S1805 photoresist film, to carry out interference lithography.By participating in that angle between two bundle laser of interference lithography controls, be 48 degree, take the cycle that guarantees to make photoresist grating is 400nm.Adopting optical shutter to control the time shutter is 20s.Then 6s develops in developer solution.With distilled water, clean 30s afterwards.Sample after cleaning is dried at 120 ℃ in baking oven, obtain photoresist grating structure.
(3) colloidal solution of the chemosynthesis gold nano grain that is 100mg/ml by concentration in dimethylbenzene is spin-coated on the surface of photoresist grating with the rotating speed of 2000rpm.
(4) sample making in (2) is heated at 350 ℃ 20 minutes in muffle furnace, obtain preparation in the on-chip metal photonic crystal structure of ito glass.
(5) PDMS and hardening agent are removed to wherein bubble with vacuum pump after the ratio mixing with 10:1.
(6) on the metal photonic crystal obtaining, place thickness and be about after the silicon rubber isolating pad of 1mm in (4), PDMS is cast in to metal photonic crystal surface.
(7) another sheet ito glass is placed on above the metal photonic crystal that scribbles PDMS, and makes ito thin film towards PDMS.And top ito glass is supported on silicone rubber pad.
(8) sample in (7) is positioned in baking oven and is heated 50 minutes at 100 ℃, complete the cross-linking polymerization of PDMS, become transparent pliable and tough substrate.
(9) approximately 30 milliliters of the aqueous hydrochloric acid solutions that configuration concentration is 25%, and be placed in 50 ml beakers.
(10) sample in step (8) is immersed in hydrochloric acid solution, in beaker bottom static approximately 2 hours, make upper and lower two-layer ito thin film fully be dissolved in hydrochloric acid.PDMS and the metal photonic crystal film of combining closely thereon naturally peel off from upper and lower two glass substrates.
(11) by obtaining the metal photonic crystal being transferred on PDMS in (10), with clear water, clean up, natural drying after, can obtain flexible metal photon crystal device.
(12) flexible metal photonic crystal shows very strong stretching, bending toughness.Fig. 2 has provided the photo of the flexible metal photonic crystal being bent under effect of stress.
Embodiment 2: the microstructure test of flexible metal photonic crystal.
(1) adopt the microstructure of the metal photonic crystal of preparation in Nova NanoSEM type scanning electron microscopy measurement example 1 step 4, as shown in Figure 3.The cycle of metal photonic crystal is about 400nm, the nanowires of gold of periodic arrangement, consists of.The mean breadth of nanowires of gold is about 165nm.Between nanowires of gold, remain a part of gold nano grain, its diameter is all less than 70nm.
(2) adopt the desk-top electron scanning micrometering of FEI Phenom to be transferred to the metal photonic crystal structure on PDMS.Because PDMS substrate is non-conductive, cannot complete high-resolution electronic micrometering, can not adopt the testing tool adopting in step (1).Test result as shown in Figure 4.Due to what now measure, be the bottom surface of preparation metal photonic crystal on ito glass in step (1), and between nanowires of gold, have photoresist, the SEM image in Fig. 4 does not observe the gold nano grain structure between nanowires of gold.
(3) adopt the atomic force microscope that is integrated in Witec SNOM system to test the atomic force microscopy image of metal photonic crystal in flexible substrate, test result as shown in Figure 5.Test result shows, the depth of modulation of the metal photonic crystal in flexible substrate is about 18nm.
Embodiment 3: the stretching realization of flexible metal photonic crystal and tensile deformation sensor experiment thereof.
(1) adopt the flexible photonic crystal tension test platform build voluntarily, its device schematic diagram as shown in Figure 6, is separately fixed at two independently on accurate translation stage by the two ends of the PDMS substrate of flexible metal photonic crystal.Mobile two translation stages, make its centre position in meter full scale respectively, and by additional certain primary stress on PDMS substrate, to ensure that substrate is evened up.Except draw direction, substrate is without other direction shape strain and stress.
(2) wideband white light source is focused on and is radiated at the metal photonic crystal on PDMS substrate, and transmitted light is accepted by the probe of fiber spectrometer, to measure transmitted spectrum.
(3) first gather the transmitted spectrum of flexible metal photonic crystal under primary stress, be denoted as I
0(λ, Δ=0), and by its spectrum as a setting.
(4) utilize one of them translation stage to increase deformation quantity D, a transmitted spectrum of every increase by 100 μ m records, I
s(λ, Δ) is until deformation quantity reaches 1mm.Complete stretching implementation procedure.Calculate tensile deformation spectrum-log
10[I
s(λ, Δ)/I
0(λ, Δ=0)].
(5) move the translation stage regulating in (4), reduce gradually deformation quantity, often reduce a transmitted spectrum I of 100 μ m records
r(λ, Δ) is 0 until deformation quantity is replied.Complete reply experimentation.Calculate deformation recovery spectrum-log
10[I
r(λ, Δ)/I
0(λ, Δ=0)].
(6) measure respectively the transducing signal amplitude that stretches and reply corresponding different deformation in experiment.The definition of sensor signal amplitude as shown in Figure 7.Draw stretching and the return curve of sensor, as shown in Figure 8." A " represents transducing signal amplitude, and " D " represents deformation quantity." ■ " represents stretching experiment curve.
represent to reply empirical curve.
Claims (7)
1. the metal photonic crystal preparation method based on flexible substrate, is characterized in that, comprises the following steps:
(1) on flat base, prepare cushion, obtain cushion matrix, on cushion, prepare again photoresist (PR) nanometer grating structure;
(2) gold nano grain of chemosynthesis (Au NP) is formed to colloidal solution in dimethylbenzene, the dimethylbenzene colloidal solution of gold nano grain is spin-coated on to the surface of step (1) photoresist nanometer grating, under surface tension effects, gold nano grain is limited in grating groove;
(3) sample on the cushion matrix of being prepared by step (2) is in 200-450 ℃ of muffle furnace after thermal treatment, make organic ligand distillation on gold nano grain surface, the abundant melting of gold nano grain, all enter in grating groove, and form continuous nanowires of gold along grating groove, on the surface of cushion matrix, successfully prepared the metal photonic crystal that Crystal structure forms;
(4) the flexible substrate liquid that is mixed with hardening agent is coated on to metal photonic crystal surface prepared by step (3), then top covers another sheet cushion matrix again, and buffering aspect is contacted with flexible substrate liquid, both sides between two cushion matrixes are supported with silicone rubber pad, to guarantee to obtain even thickness, controlled flexible substrate;
(5) by the sample making in step (4) 100-120 ℃ of heating, complete flexible substrate cross-linking polymerization;
(6) sample step (5) being obtained is placed in hydrochloric acid or sulfuric acid solution, and the cushion on upper and lower two matrixes is fully dissolved, flexible substrate and on the metal photonic crystal of combining closely from matrix, separate up hill and dale;
(7) flexible device finally step (6) being obtained cleans with distilled water, removes remaining acid solution and issuable impurity, obtains independently flexible device, completes the preparation of flexible metal photonic crystal;
Matrix adopting is insoluble to the solution such as hydrochloric acid, sulfuric acid and can stands the transparent material of 450 ℃ of following heat treatment process; The material of cushion is metal, the metal oxide materials that is dissolved in hydrochloric acid or sulfuric acid, and can be by hot evaporation, magnetron sputtering or the preparation of pulse laser deposition process process on flat base.
2. according to the method for claim 1, it is characterized in that the preferred PDMS of flexible substrate, silicone adhesive, glass cement material substrate.
3. according to the method for claim 1, it is characterized in that, cushion is ITO layer.
4. according to the method for claim 1, it is characterized in that, flat base is glass or quartz.
5. according to the method for claim 1, it is characterized in that, the heat treatment temperature of step (2) is 350 ℃.
6. according to the method for claim 1, it is characterized in that, the time that step (5) adds thermal response is 45 minutes-1 hour.
7. according to the method for claim 1, it is characterized in that, there is dentate metal nanoparticle material on the surface that is applicable to be insoluble to hydrochloric acid or sulfuric acid that gold nano grain replaces with other.
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