CN104949957A - Embedded type nano dot array surface enhanced Raman active substrate and preparation method thereof - Google Patents
Embedded type nano dot array surface enhanced Raman active substrate and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a novel embedded type nano dot array structure surface enhanced Raman active substrate. The substrate takes an aluminum sheet with an ordered concave pit array structure on the surface as a template and materials with SERS (Surface Enhanced Raman Scattering) performances are deposited to obtain a large-area and highly-ordered nano dot array structure embedded into a groove on the concave pit substrate. The nano dot array provided by the invention can be used for adjusting structure parameters and shapes of the embedded type nano dot array according to the size of the concave pit array, so that different influences on the Raman surface enhancing effect by different embedded type metal nano array substrates are realized. The preparation method has the advantages of simplicity in operation, no need of transferring, low cost and easiness for industrial production; the shape of the substrate is highly ordered and the Raman activity is high; and the substrate has the remarkable Raman surface enhancing effect on analytes with different concentrations and has very high detection limit.
Description
Technical field
The present invention relates to a kind of embedded nanometer lattice row surface reinforced Raman active substrate and preparation method thereof, particularly a kind of preparation method of the silver nano lattice row surface enhanced Raman active substrate based on pit template nano surface technology of preparing.
Background technology
Surface enhanced raman spectroscopy (Surface-enhanced Raman Scattering, SERS) refer to that some metals measuring and be adsorbed on special preparation are (as Precious Metals-Gold, silver), during sample on colloidal sol or admixture surface, the phenomenon that the Raman signal of binding molecule greatly strengthens, since being found from 1974, through the development of decades, develop into now a kind of ripe effective molecular vibration spectrum analysis tool, because it has very high sensitivity, the unimolecular layer being adsorbed on metal surface can be detected, the structural information of surface molecular can be provided again, in chemical products, material and life science aspect have a wide range of applications, especially the research in life science serve as more and more key player, be considered to a kind of very effective detection interfacial characteristics and intermolecular interaction, the instrument of characterizing surface molecular absorption behavior and molecular structure.Prepare a kind of stability high, strengthen effective, that detection limit is low SERS active-substrate and become key component.The method preparing SERS active-substrate conventional at present has a lot.
As: Electrochemical roughening noble metal active electrode basement, noble metal colloidal sol active substrate, the active substrate of the film activity substrate of vacuum evaporation noble metal island and chemical etching and chemogenic deposit noble metal, but the surfaceness that provides of these self assembly active substrates and regularity are difficult to the stability, homogeneity and the repeatability that control thus to have impact on binding molecule spectrum.The method of the orderly surface nano-structure of preparation that Recent study is more has the shortcomings and limitations on some Synthesis and applications.
For another example: very little with the area of beamwriter lithography and the surface nano-structure prepared by scan-probe method, productive rate is low, apparatus expensive and need to increase electric energy outward; For self-organizing growth method and nano-imprint method, the structural parameters of more difficult adjustment surface nano-structure usually.And due to its preparation procedure loaded down with trivial details, the reasons such as the high and preparation efficiency of preparation cost is low limit its development.
Anodised aluminium (Anodic Aluminum Oxide, AAO) because of its orderly, controlled nanohole array preparation process, and have superior condition for the controllability of particles size and distribution and homogeneity realizing particle in nanoparticle assembly, be widely used.Its key step comprises once oxidation, removes oxide layer, secondary oxidation, attached photoresist, removes aluminium substrate, reaming, transfer etc.Be considered to very promising nano-form technology of preparing and be subject to extensive concern, it is a kind of efficient, flexible, low cost, can prepare the method for high sensitivity, repeatably surface nano-structure SERS substrate, but the method antianode alumina formwork quality requirements is high.This basis we have proposed the method for the aluminium pit array utilizing oxidation step to obtain to prepare SERS substrate, key step is once oxidized again, except namely oxide layer obtains orderly aluminium pit array.This method not only inherits all advantages of AAO template, and overcomes the deficiency of AAO template completely, and as complex steps, transfer difficulty, AAO is frangible.This dot matrix gone out for Template preparation with aluminium pit array, without the need to removing template, making dot matrix from the pollution of solution and corrosion, thus ensure that the regularity of dot matrix.
Summary of the invention
An object of the present invention is the embedded nanometer lattice row Raman active substrate preparation method providing a kind of synthesis step succinct, may be used for the trace analysis of material and the detection of biomolecule.
Two of object of the present invention is to provide a kind of preparation method preparing the substrate of embedded nano-array surface reinforced Raman active based on pit surface nano fabrication technique.
For achieving the above object, the present invention is by the following technical solutions:
A kind of embedded nano lattice surface enhanced raman active substrate, it is characterized in that this substrate is take aluminium sheet as substrate, by nano-structured for this aluminium sheet formation aluminium pit array, in this pit array, plate the noble metal film with Surface enhanced raman spectroscopy performance, form embedded noble metal lattice structure; Centre distance between described aluminium pit array is 110 ~ 115 nm, and pit depth is 20 ~ 25 nm; The particle diameter of described noble metal dot matrix is 55 ~ 60 nm.
Above-mentioned noble metal is: gold, silver or copper.
Prepare a method for above-mentioned embedded nano lattice surface enhanced raman active substrate, steps of the method are:
A. the pre-service of aluminium substrate: by high-purity aluminium flake of 99.999% ultrasonic cleaning 30 min in acetone, 450 ~ 550 DEG C of annealing 5 h under nitrogen protection, then, in the ethanol of temperature 0 DEG C and the mixed liquor of perchloric acid, under 600 mA constant current conditions, electrochemical polish is carried out;
B. will carry out nano-structured through pretreated aluminium substrate surface, remove the aluminium substrate material that the pre-structure of the unordered aluminium oxide of surperficial one deck obtains having pit array; Its concrete steps are: carry out first time anodized under 45 V constant voltages after, and the time is 7 ~ 12 h; Then under temperature 60 C condition, in the mixed liquor of massfraction 6% phosphoric acid and 1.8% chromic acid, 10 h are soaked;
C. by the aluminium substrate of step b gained noble metal film on its plated surface, noble metal is assembled, and obtains embedded nanometer lattice row, and its concrete steps are: aluminium substrate is placed in evaporating and coating equipment, and vacuum tightness is 8 × 10
-4under Pa, evaporation rate 1.4 ~ 1.6 nm/s condition, evaporation precious metal powder thickness is 8 ~ 12nm;
D. the above-mentioned sample obtained is immersed in the molecular solution with Raman active, soak 30 min, nitrogen dries up.
Above-mentioned nano-structured method can be: anodizing, photoetching technique method, nanometer embossing method or reactive ion etching method.
The method of the pre-structural sheet of above-mentioned removing substrate is with acid, nitration mixture or caustic corrosion solution or removes with physical separation methods.
Above-mentioned the molecular solution rhodamine 6G with Raman active, crystal violet or glucose etc. have very high activity.
Advantage of the present invention and effect are: the present invention compared with prior art, has the following advantages:
1) preparation method preparing metallic nanostructured surface enhancing Raman active substrate provided by the invention, preparation process is extremely simple, and this embedded nanostructured has natural substrate, the analysis thing for variable concentrations has significant surface Raman enhancement effect.
2) preparation method of the surface reinforced Raman active substrate of embedded nano-dot matrix structure provided by the invention, these metal dots arrays are with the mode land embedded inside each pit, and this structure to a certain degree can protect the effective constituent of SERS substrate.
3) preparation method of the surface reinforced Raman active substrate of embedded nano-dot matrix provided by the invention, while realizing the surface nano-structure of preparation based on different substrates and metal material large area high-sequential.Only need the very thin precious metal material of evaporation (being about 10 nm) to have cost low, be easy to industrial advantage.
Accompanying drawing explanation
Fig. 1 is experiment flow figure of the present invention.
Fig. 2 is the orderly pit array aluminium substrate template SEM(Scanning Electron Microscope prepared in the present invention) figure.
Fig. 3 is the SEM figure utilizing the silver nano lattice of aluminium pit Template preparation to arrange in the present invention.
Fig. 4 utilizes the silver nano lattice array structure of Template preparation to variable concentrations (1 × 10 in the present invention
-8m, 1 × 10
-9m, 1 × 10
-10m, 1 × 10
-11m) rhodamine 6G probe molecule test signal Raman spectrogram.
Embodiment
Embodiment 1: the present embodiment with through anodic oxidation and after removing oxide layer with the aluminium substrate of orderly pit array structure for template, prepare large-area ordered, homogeneous Ag nano-dot matrix array structure, and with 1 × 10
-7the rhodamine (rhodamine 6G, R6G) of M is probe molecule, carries out the test of Surface Raman Spectra.Concrete steps are:
1) first by aluminium flake acetone ultrasonic cleaning 30 min of thick for 0.2 mm 99.999%, under nitrogen protection, 450 ~ 550 DEG C of annealing 5 h, take out for subsequent use;
2) 1 is taken out) aluminium flake that process is placed in the ethanol of temperature 0 DEG C and the mixed liquor (volume ratio 1:9) of perchloric acid, and electrochemical polish about 5 min under constant current (600 mA) condition, obtains aluminium flake for subsequent use;
3) by pretreated aluminium flake for subsequent use in 0.3M oxalic acid 45V voltage, be oxidized 8-12 h at 2 DEG C;
4) take out, put into the mixed solution that volume ratio is the 1.8w% chromic acid of 1:1 and the phosphoric acid of 6w%, at the temperature of 60 DEG C, corrode 10 h; After repeatedly rinsing with deionized water, dry, obtain the aluminium substrate with pit array structure, for subsequent use, as shown in Figure 2, this aluminium substrate can as the native substrate of nanostructured.
8 × 10
-4under Pa, evaporation rate 1.4 ~ 1.6 nm/s condition, evaporation silver powder thickness is 10 nm.After taking-up, obtain the silver nano lattice array structure that in substrate as shown in Figure 3, large area arrangement is orderly, structure and morphology is homogeneous.This structure has easily transfer and constitutionally stable feature.
6) the above-mentioned sample obtained being dipped in concentration is 1 × 10
-7take out after 30 min in the solution of M rhodamine 6G, nitrogen dries up, and tests with confocal laser micro-Raman spectroscopy.Fig. 3 utilizes the silver nano lattice array structure of Template preparation to variable concentrations (1 × 10 in the present invention
-8m, 1 × 10
-9m, 1 × 10
-10m, 1 × 10
-11m) rhodamine 6G probe molecule test Raman signal spectrogram.
Can see that this SERS signal based on the silver nano lattice array structure substrate aluminium substrate strengthens effect from Fig. 3 very good, be especially 1 × 10 when probe molecule rhodamine 6G concentration is low to moderate
-10base Raman signal still highly significant during M, its enhancer can reach 3.74 × 10
10.This is far away higher than the large-area SERS substrate of template synthesis of bibliographical information.Illustrate that substrate surface Raman signal prepared by the present invention strengthens significantly, and detection limit is low.
Claims (6)
1. an embedded nano lattice surface enhanced raman active substrate, it is characterized in that this substrate is take aluminium sheet as substrate, by nano-structured for this aluminium sheet formation aluminium pit array, in this pit array, plate the noble metal film with Surface enhanced raman spectroscopy performance, form embedded noble metal lattice structure; Centre distance between described aluminium pit array is 110 ~ 115 nm, and pit depth is 20 ~ 25 nm; The particle diameter of described noble metal dot matrix is 55 ~ 60 nm.
2. embedded nanometer lattice row surface reinforced Raman active according to claim 1 substrate, is characterized in that described noble metal is: gold, silver or copper.
3. prepare a method for embedded nano lattice surface enhanced raman active substrate according to claim 1 and 2, steps of the method are:
A. the pre-service of aluminium substrate: by high-purity aluminium flake of 99.999% ultrasonic cleaning 30 min in acetone, 450 ~ 550 DEG C of annealing 5 h under nitrogen protection, then, in the ethanol of temperature 0 DEG C and the mixed liquor of perchloric acid, under 600 mA constant current conditions, electrochemical polish is carried out;
B. will carry out nano-structured through pretreated aluminium substrate surface, remove the aluminium substrate material that the pre-structure of the unordered aluminium oxide of surperficial one deck obtains having pit array; Its concrete steps are: carry out first time anodized under 45 V constant voltages after, and the time is 7 ~ 12 h; Then under temperature 60 C condition, in the mixed liquor of massfraction 6% phosphoric acid and 1.8% chromic acid, 10 h are soaked;
C. by the aluminium substrate of step b gained noble metal film on its plated surface, noble metal is assembled, and obtains embedded nanometer lattice row, and its concrete steps are: aluminium substrate is placed in evaporating and coating equipment, and vacuum tightness is 8 × 10
-4under Pa, evaporation rate 1.4 ~ 1.6 nm/s condition, evaporation precious metal powder thickness is 8 ~ 12nm;
D. the above-mentioned sample obtained is immersed in the molecular solution with Raman active, soak 30 min, nitrogen dries up.
4. the preparation method of embedded nano lattice surface enhanced raman active substrate according to claim 3, is characterized in that described nano-structured method can be: anodizing, photoetching technique method, nanometer embossing method or reactive ion etching method.
5., according to the preparation method of the embedded nano lattice surface enhanced raman active substrate described in claim 3, it is characterized in that the method for the pre-structural sheet of described removing substrate is with acid, nitration mixture or caustic corrosion solution or removes with physical separation methods.
6. the preparation method of embedded nano lattice surface enhanced raman active substrate according to claim 3, is characterized in that this substrate has very high activity to described the molecular solution rhodamine 6G with Raman active, crystal violet or glucose etc.
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| CN106995930A (en) * | 2016-01-22 | 2017-08-01 | 陕西师范大学 | Aluminium oxide nano pin and its preparation method and application with hole composite array structure |
| CN107290326A (en) * | 2016-04-12 | 2017-10-24 | 中国科学院苏州纳米技术与纳米仿生研究所 | Chip device and preparation method thereof |
| CN107561051A (en) * | 2016-07-01 | 2018-01-09 | 清华大学 | A kind of molecular vehicle for Single Molecule Detection |
| CN107576648A (en) * | 2017-09-14 | 2018-01-12 | 电子科技大学 | A kind of preparation method of Raman enhancing substrate |
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