CN101776604B - Production method of basement for enhancing raman scattering of molecule - Google Patents
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Abstract
The invention provides a production method of a basement for enhancing the raman scattering of a molecule, which comprises following steps of: (1) selecting substrate material, cleaning and hydrophilically treating; (2) producing a micro nanometer structure layer on the surface of the substrate; (3) metallizing the micro nanometer structure layer to obtain the substrate with a nanometer metal structure; (4) decorating the surface of the substrate obtained by the step (3) to obtain a surface decoration layer, wherein the surface decoration is preparation of a gas sensitivity interface or a molecule biological film or an adsorbed film or a surface activated material according to the property of the molecule to be tested to improve the property of the basement to enrich the molecule to be tested and the action for activating the basement; (5) adding the molecule to be tested on the substrate with a surface decoration layer; and (6) changing external medium environment around the substrate to improve the enhancement effect of the raman scattering of the molecule to be tested. The external medium environment around the substrate comprises circumambient environment material, or excitation wave length, or optical field distribution or magnetic field distribution. The production method can be used for high sensitivity test; and the substrate has the advantages of high controllability, consistency, repeatability, stability and the like.
Description
Technical field
The invention belongs to the micro-nano technical field, relate to a kind of substrate that strengthens Raman scattering of molecule, particularly a kind of surface plasmon resonance effect of metal Nano structure and finishing mechanism utilized realizes efficient, the high stability substrate that the molecule Raman strengthens.
Background technology
Raman scattering (RS) is a kind of scattering phenomenon of light, is photon and testing molecule interaction when monochromatic incident light, and inelastic collision occurs, and between photon and molecule, energy exchange occurs, the scattering that photon change direction of motion and frequency occur.Raman spectrum (RS) is called as the dactylogram of molecule, the characteristics of this spectrum are that bands of a spectrum are narrow, abundant information, be applied to sensing technology, have specificity high, need not preparation of samples, can provide fast, can repeat, the advantage of undamaged qualitative and quantitative analysis.But a little less than Raman scattering very, Raman spectrum is applied to Detection Techniques and has the high specific while, and sensitivity is very low.Can scattering is strengthened be the practical keys of RS Detection Techniques.
Fleischman in 1974 observes the Raman diffused light spectral intensity that is attached to textured metal micro-nano structure surface molecular and can increase substantially, and is called as Surface enhanced raman spectroscopy (Surface-enhanced Raman Scattering is called for short SERS).Primary Study shows, this is a kind of special optical enhancement effect with surface selectivity, and the Raman signal that can will be adsorbed on the metal Nano structure surface molecular strengthens several orders of magnitude singularly.The report that adopts nano metal colloidal sol to improve Raman scattering of molecule is also arranged.But at present these two kinds of methods exist all that enhancer is low, the shortcoming such as repeatability and poor stability.The experiment and theoretical research show, the surrounding environment of SERS phenomenon and testing molecule is closely related, the SERS active substrate with high enhancing ability, high stability is to utilize the enlarge-effect of SERS to realize one of key factor of high sensitivity detection.Making Raman scattering of molecule enhancing in substrate, is that the Raman scattering efficient of molecule is improved on the one hand, is to make testing molecule at utmost be gathered in substrate surface on the other hand.At present the research of Raman scattering enhancement effect only rested on the primary stage, the mechanism of generation effect is also indefinite.
Summary of the invention
the problem to be solved in the present invention is: overcome existing textured metal structural substrates, it is low that nano metal colloidal sol improves testing molecule Raman scattering efficient, detection sensitivity is low, the shortcoming of repeatability and poor stability, a kind of substrate fabrication method that strengthens Raman scattering of molecule is provided, this substrate utilizes metal micro-nanostructure local plasmon resonance body enhancement effect, adopt finishing coat, improve the external agency environment, improve simultaneously substrate enrichment testing molecule quantity and strengthened testing molecule Raman scattering efficient, realize the efficient of testing molecule Raman scattering, maximize output, satisfy the high sensitivity detection demand.
The technical solution adopted for the present invention to solve the technical problems is: a kind of substrate fabrication method that strengthens Raman scattering of molecule, and described substrate is comprised of decorative layer and external agency environment four parts on substrate, metal micro-nanostructure layer, surface, and it is produced as follows:
(1) select backing material, clean and do hydrophilic treatment;
(2) produce the micro-nano structure layer at substrate surface;
(3) with the metallization of micro-nano structure layer, obtain to be attached with the substrate of metal Nano structure layer;
(4) substrate surface that step (3) is obtained is modified, obtain surface decoration layer, described finishing is according to molecular property to be detected, preparation air-sensitive interface or molecular biosciences film or adsorption film or surface active material are with the ability that improves substrate enrichment testing molecule and the behavior that substrate is activated;
(5) substrate with finishing coat is added testing molecule;
(6) change substrate peripheral outer media environment, to improve testing molecule Raman scattering enhancement effect; Described substrate peripheral outer media environment comprises surrounding environment material or excitation wavelength or optical field distribution or Distribution of Magnetic Field.
Backing material in described step (1) is glass or quartzy or silicon or germanium.
Produce the micro-nano structure layer at substrate surface by nanosphere self assembly or nano-photoetching or nano impression in described step (2).
In described step (2), the characteristic dimension of micro-nano structure layer is from 20nm～900nm, and the cycle, thickness was from 10nm～500nm from 40nm～8 μ m.
The middle micro-nano structure layer that metallizes of described step (3), metallization material are gold or silver or first silver-colored rear gold or first golden rear silver-colored.
In described step (3), the arrangement mode of metal Nano structure is triangle or quadrilateral or hexagon or annular.
The mode that described step (5) passes into or drips or apply or injects is attached to substrate with finishing coat with testing molecule.
Testing molecule in described step (5) is probe gas molecule or solid molecule or fluid molecule.
The advantage that the present invention compared with prior art has is: the present invention improves Raman scattering of molecule by improving substrate to the accumulation ability of testing molecule and Raman scattering two aspects that improve molecule in substrate, take full advantage of the enlarge-effect of SERS, can realize high sensitivity detection; The present invention simultaneously has controllability, can guarantee consistance, repeatability, the stability of same batch or different batches substrate, guarantee that the method is used for the repeated and stable of Detection Techniques, solved the key technical problem that Raman spectrum is surveyed, can be widely used in the gas trace and survey or the fields such as high sensitivity solid, solution detection.
Description of drawings
Fig. 1 is a kind of structural representation that strengthens the substrate of Raman scattering of molecule of the present invention;
Fig. 2 is Raman scattering of molecule schematic diagram in the embodiment of the present invention 1;
Fig. 3 realizes the schematic diagram that Raman scattering strengthens after utilizing the plasma enhancement effect of metal micro-nanostructure in the embodiment of the present invention 1;
Fig. 4 does not carry out in the situation of finishing substrate in the embodiment of the present invention 2, the enrichment condition schematic diagram of substrate to molecule;
Fig. 5 is after in the embodiment of the present invention 3, finishing being carried out in substrate, the enrichment condition schematic diagram of substrate to molecule;
In figure: 1, base substrate, 2, metal micro-nanostructure, 3, finishing coat, 4, testing molecule, 5, Raman scattering, 6, incident laser, 7, free electron, 8, the plasma density ripple, 9, the Raman scattering after strengthening.
Embodiment
Fig. 1 is a kind of structural representation that strengthens the substrate of Raman scattering of molecule of the present invention.Substrate is comprised of decorative layer and external agency environment four parts on substrate, metal micro-nanostructure layer, surface.Wherein 1 is base substrate, and 2 is metal micro-nanostructure, and 3 is finishing coat.
Embodiment 1
In TNT gas trace was surveyed, method for making of the present invention was:
(1) selecting K9 glass is base substrate, the washing lotion of putting into concentration 90%～98% concentrated sulphuric acid and oxydol H 2SO4: 30%H2O22～be made at 4: 1 is heated to 80 ℃～120 ℃ and soaked 30～60 minutes, to remove impurity, then repeatedly rinse, put into the solution NH3 that ammoniacal liquor, hydrogen peroxide and water are made into: H2O2: H2O/1: ultrasound wave was processed 20～60 minutes in 1: 5 again, take out again substrate and repeatedly rinse use, preserve, in order to using;
(2) design the triangle metal nanostructured that hexagon is arranged, structural metallic materials is gold, characteristic dimension 100nm, and cycle 500nm, thickness 10nm, the plasma resonance frequency of this structure is about 420nm.Adopt the method for nano impression to produce metal micro-nanostructure 2 on base substrate 1;
(3) method by gold evaporation metallizes micro-nano structure, obtains to be attached with the substrate of nm of gold structure;
(4) substrate surface is modified, and formation can be carried out to the TNT vapour molecule decorative layer of selective adsorption.Concrete ways is as follows: with certain herbaceous plants with big flowers mercaptan (CH3 (CH2) 9SH of substrate at concentration 1mM, soaked 24 hours 1-DT), by-HS group 1-DT will be at the individual layer of the metal surface of substrate self assembly formation ordered arrangement, this individual layer will effectively adsorb TNT, and with the confinement of TNT molecule in the Electromagnetic enhancement scope.Micro-concentrations 1mg/ml cetomacrogol 1000 chloroformic solution (PEG100) is covered the substrate surface film forming, and at 80 ℃ of oven dry 1h, allow solvent evaporates remove, formation can be carried out to the TNT vapour molecule gas sensing layer of selective adsorption;
(5) additional testing molecule, be placed in vacuum environment with this substrate, passes into gas to be measured, and gas molecule is enriched in the decorative layer 3 of substrate surface;
(6) introduce the incident laser 6 irradiation substrate surfaces that wavelength is 442nm, in the laser excitation metal nanoparticle, free electron 7, surface plasmon resonance phenomenon (LSPR) occurs in substrate, produce plasma density ripple 8, gas molecule to be measured 4 Raman scatterings that are in field intensity are strengthened greatly, as shown in Figure 9.Adopt spectrometer to survey.
Embodiment 2
In sucrose solution is surveyed, realize the making of substrate by following steps
(1) to select silicon be substrate, clean and do hydrophilic treatment.
(2) produce Triangle-Profile at substrate surface by the nanosphere self assembly, characteristic dimension 50nm, the nanostructured of cycle 300nm.
(3) method of passing through magnetron sputtering is with nanostructured metal, and then first sputter last layer argent changes target sputter last layer metallic gold, obtains to be attached with 50nm gold, the substrate of the nanometer metal structure of the double-level-metal of the thick silver of 20nm.
(4) if this substrate directly is positioned in solution to be measured, survey, substrate to Adsorbed molecular effect to be measured as shown in Figure 4.This substrate surface is added one deck molecular biosciences film 3, and activate: with octane mercaptan (1-octanethiol, 1-OT) prepare the solution of 1mM with the 11-Mercaptoundecanoic acid (11-MUA) that contains sulfydryl in ethanol, the ratio of 3: 1 by volume is made into activating reagent, substrate is dipped in activated solution 4 ℃ hatched 18 hours, make metal watch wear the reactive group of carboxyl, increase the accumulation ability to testing molecule, as shown in Figure 5.
(5) substrate is placed in solution to be measured, and then changes its refractive index by improving the electric-field intensity distribution in solution or improving solution concentration, to improve testing molecule Raman scattering enhancement effect.
In charcoal is surveyed apart from viral powder, realize the making of substrate by following steps
(1) to select germanium be backing material, clean and do hydrophilic treatment;
(2) adopt nano impression to produce characteristic dimension 800nm at substrate surface, cycles 3 μ m, the nanostructured layers that quadrilateral is arranged;
(3) with the metallization of micro-nano structure layer, then first sputter last layer metallic gold changes target sputter last layer argent, obtains to be attached with 300nm gold, the substrate of the nanometer metal structure of the double-level-metal of the thick silver of 100nm;
(4) substrate surface that step (3) is obtained is modified, and obtains surface decoration layer, and the preparation adsorption film improves the ability of substrate enrichment testing molecule, and substrate is activated;
(5) adopt the method for coating to add testing molecule to the substrate with finishing coat;
(6) strengthen the distribution of light intensity distribution of substrate peripheral outer media environment, to improve testing molecule Raman scattering enhancement effect.
Embodiment 4
In viral solution is surveyed, realize the making of substrate by following steps
(1) select melt quartzy for backing material, clean and do hydrophilic treatment;
(2) utilize nanoimprinting technology to produce the micro-nano structure layer at substrate surface, the micro-nano structure layer is annular arrangement, characteristic dimension 20nm, the structure of cycle 40nm.
(3) with the metallization of micro-nano structure layer, obtain to be attached with the substrate of metal Nano structure layer, structural thickness is 50nm;
(4) substrate surface that step (3) is obtained is modified, and obtains the molecular biosciences film, with the ability that improves substrate enrichment testing molecule and the behavior that substrate is activated;
(5) substrate with finishing coat is added testing molecule;
(6) change substrate peripheral outer media environment, substrate is placed in nitrogen chamber (it is namely a kind of method that changes substrate peripheral outer media environment that substrate is placed in nitrogen chamber), improve testing molecule Raman scattering enhancement effect.
Embodiment 5
In the toxin detection of gas, realize the making of substrate by following steps
(1) to select zinc selenide be backing material, clean and do hydrophilic treatment;
(2) adopt nanoimprinting technology to produce the micro-nano structure layer that hexagon is arranged at substrate surface, characteristic dimension is 900nm, and the cycle is 8 μ m;
(3) method that adopts chemical silvering obtains to be attached with the substrate of metal Nano structure layer with the metallization of micro-nano structure layer, and structural thickness is 500nm;
(4) substrate that step (3) is obtained prepares adsorption film, with the ability that improves substrate enrichment testing molecule and the behavior that substrate is activated;
(5) substrate with finishing coat is added testing molecule;
(6) improve substrate peripheral outer magnetic field distribution, to improve testing molecule Raman scattering enhancement effect.
In a word, the present invention is according to the difference of detected object, and by selecting the substrate of different materials, the optimal design underlying structure makes Raman scattering of molecule obtain maximum the enhancing; By substrate surface is modified, change simultaneously the external agency environment, realize testing molecule farthest enrichment in substrate.Can be used for high sensitivity detection, this substrate simultaneously has controllability, consistance, repeatability, stable advantages of higher.
Claims (1)
1. substrate fabrication method that strengthens Raman scattering of molecule in TNT gas trace is surveyed, it is characterized in that: making step is as follows:
(1) selecting K9 glass is base substrate, puts into concentration 90%～98% concentrated sulphuric acid H
2SO
4With 30% oxydol H
2O
2Be heated to 80 ℃～120 ℃ in the washing lotion that is made into and soaked 30～60 minutes, wherein, H
2SO
4: H
2O
2Proportioning is 2～4:1, to remove impurity, then repeatedly rinses, then puts into the solution NH that ammoniacal liquor, hydrogen peroxide and water are made into
3: H
2O
2: H
2In O/1:1:5, ultrasound wave was processed 20～60 minutes, then took out substrate and repeatedly rinse, and preserved, in order to using;
(2) design the triangle metal nanostructured that hexagon is arranged, the metal Nano structure material is gold, characteristic dimension 100nm, and cycle 500nm, thickness 10nm, the plasma resonance frequency of this structure is about 420Hz; Adopt the method for nano impression to produce metal micro-nanostructure on base substrate;
(3) method by gold evaporation metallizes micro-nano structure, obtains to be attached with the substrate of nm of gold structure;
(4) substrate surface is modified, and formation can be carried out the decorative layer of selective adsorption to TNT gas, and concrete ways is as follows: with substrate at the 1-of concentration 1mM decyl mercaptan (CH
3(CH
2)
9SH, 1-DT) in soaked 24 hours, will form the individual layer of ordered arrangement in the self assembly of the metal surface of substrate by-HS group 1-DT, this individual layer will effectively adsorb TNT gas, and with the confinement of TNT gas in the Electromagnetic enhancement scope; The cetomacrogol 1000 chloroformic solution that is 1mg/ml with micro-concentrations covers the substrate surface film forming, and at 80 ℃ of oven dry 1h, allows solvent evaporates remove, and formation can be carried out to TNT gas the gas sensing layer of selective adsorption;
(5) additional testing molecule, be placed in vacuum environment with this substrate, passes into gas to be measured, and gas molecule is enriched in the decorative layer of substrate surface;
(6) introduce the incident laser irradiation substrate surface that wavelength is 442nm, free electron in the laser excitation metal nanoparticle, surface plasmon resonance phenomenon (LSPR) occurs in substrate, produce the plasma density ripple, the gas molecule Raman scattering to be measured that is in field intensity is strengthened greatly.
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