CN102661944A - Preparation method of surface-enhanced Raman scattering substrate of metal particle array - Google Patents
Preparation method of surface-enhanced Raman scattering substrate of metal particle array Download PDFInfo
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- CN102661944A CN102661944A CN2012101488899A CN201210148889A CN102661944A CN 102661944 A CN102661944 A CN 102661944A CN 2012101488899 A CN2012101488899 A CN 2012101488899A CN 201210148889 A CN201210148889 A CN 201210148889A CN 102661944 A CN102661944 A CN 102661944A
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Abstract
The invention provides a preparation method of a surface-enhanced Raman scattering substrate of a metal particle array. The preparation method comprises the following steps of: preparing a porous silicon nanometer wire array (PSNWA) as a substrate material through a metal-assisted chemical corrosion method; reducing metal ions in a metal salt solution to elementary substance through an impregnation-reduction method, and obtaining the surface-enhanced Raman scattering substrate after uniformly depositing the elementary substance on the surface of the PSNWA in a nanometer particle manner; and inducing a substance to be detected into an active substrate surface through an infiltration or titration method, namely carrying out Raman spectrum detection. The preparation method provided by the invention has the advantages of low cost, simple process, simplicity and convenience in operation, high sensitivity of SERS (Surface-Enhanced Raman Scattering) signals, and good repeatability; and an SERS light spectrum has very good stability and repeatability. The invention provides a molecule detection and trace quantity analysis method with high speed, high sensitivity and high reliability. The preparation method provided by the invention needs extremely less sample amount, is suitable for various liquid samples, and has wide application prospects of rapid identification of clinical biological molecules, trace quantity chemical substance detection, biological sample analysis and the like.
Description
Technical field
The invention belongs to Raman spectrum molecular detection technology field, relate to one type of preparation method with surface-enhanced Raman scattering activity substrate of with low cost, characteristics such as technology is simple, easy and simple to handle, Raman signal reinforced effects and good reproducibility.
Background technology
(Surface-enhanced Raman Scattering, SERS) since the phenomenon, SERS research has obtained develop rapidly on the coarse silver electrode surface that had been adsorbed with for the first time the pyridine molecule in 1974, to observe SERS.Utilize the SERS technology; The Raman scattering signal can be strengthened greatly when testing molecule was adsorbed on roughened metal surface; Can provide the information on the single molecules level; Have very high sensitivity, and test speed is fast, test condition is gentle, testing molecule is not had characteristics such as destructiveness, can carry out in real time simultaneously portablely, detection analysis on the spot; These all are that other analysis means is difficult to reach, and these characteristics also make the SERS spectral technique have important in theory and practice significance in scientific domains such as biology, medical science, chemistry.Because the SERS effect mainly is to be based upon on the basis of the surface plasma bulk effect that produces when noble metal nano particles receives extraneous laser radiation, be the main prerequisite that obtains good SERS signal at the bottom of the SERS active group of the noble metal nano particles that therefore obtain to have high distribution density, size is fit to.Should have at the bottom of the desirable SERS active group with low cost, technology is simple, easy and simple to handle, characteristics such as reinforced effects good, good stability, good reproducibility.Yet remain a challenge at the bottom of how preparing satisfactory active group at present; Though the metallic colloid that generally uses has good reinforced effects, its preparation process is loaded down with trivial details, the easy distinct disadvantage such as organic molecule, stability and poor reproducibility of introducing of flow process often; The substrate that utilizes modes such as plasma etching, magnetron sputtering to prepare then exists deficiencies such as preparation cost is high.Given this; Develop a kind of have simultaneously with low cost, technology is simple, easy and simple to handle; Imperative at the bottom of the SERS active group of characteristics such as the Raman signal reinforced effects is good, good stability, good reproducibility; This especially promotes it and divides the application of aspects such as analysis and unimolecule system spectrum significant at objectionable impurities trace analysises such as chemistry or biomolecule, material detection by quantitative, composition in the range of application that enlarges SERS.
Patent of the present invention will adopt simple, cheap two-step approach preparation technology; It is the first metal assistant chemical burn into two steps technology of growth in situ again; Construct out one type and have large-area three-dimensional ordered structure, metallics array based SERS substrate that the SERS stability is high, realize very big enhancing and fast detecting and identification Raman signals such as chemistry or biomolecule.The reason of the following aspects has been considered in the SERS substrate that patent of the present invention is designed simultaneously.At first, utilizing the compound configuration SERS of 3 D stereo substrate to replace the substrate of two dimensional surface type is to improve the substrate specific surface, and then can greatly increase SERS " focus " density and reach the purpose that improves raman signal intensity, sensitivity; Second; Noble metal silver becomes the preferred material that present preparation has high SERS enhancing ability because of having bigger plasma resonance frequency (2.5 eV); But a very big shortcoming of argent is exactly in air, to be prone to oxidized and to cause the SERS performance to have poor time stability, and this also is that present SERS application facet is needed one of subject matter of solution badly.Employing as strengthening kernel, coats the SiO less than 5 nm with Nano silver grain on it
2Protective seam, control SiO
2Layer thickness, the electromagnetic field that makes the metallic particles kernel strengthen can affact SiO
2Test substance outside the layer can be realized the long-time stability of SERS substrate and SiO so effectively
2Have good biocompatibility and also be suitable for its application in biological field; The 3rd, Ag/SiO
2In/Si when contact, is different because of metal work function and semiconductor material Fermi level, can realize that electronics passes through SiO
2The effective transfer of medium nanometer layer between Ag-Si; And then can come very big enhanced surface plasmon resonant frequency through the carrier density that improves the metal surface; Thereby further strengthen its SERS effect, therefore adopt with metal nano material be extended to silica-based or other semiconductor base material on to design the SERS new system also be to improve SERS at present to strengthen one of effective methods; Simultaneously, crystalline silicon is one of most important base light electronic material, has into the advantage of maturity processing technique and the integrated aspect of device, selects for use crystalline silicon to prepare the SERS substrate and for further realizing biochip and solid photoelectricity integrated system possibility is provided.Harmless unmarked SERS sensor or biochip with identification molecule " fingerprint " and molecular entergy level characteristic that this patent of invention is prepared will have broad application prospects at aspects such as clinical bacteria quick identification, trace materials detection, biological sample analysises.
Summary of the invention:
In order to solve the variety of issue that the SERS technology exists in practical application; Enlarge the range of application of SERS; Especially promote its in the objectionable impurities trace analysis, material is qualitative or detection by quantitative, composition are analyzed and the application of aspects such as unimolecule system spectrum, the invention provides a kind of novel have with low cost, technology is simple, the preparation method of easy and simple to handle, characteristics such as reinforced effects good, stability and good reproducibility, the substrate of metallics array based SERS.
Technical scheme of the present invention realizes in the following manner:
The preparation method of a kind of metallics array based SERS substrate; Comprise following technical step: with resistivity is that the n of 0.001-50 Ω cm or the monocrystalline silicon piece of p type place agitated reactor, fills by the HF of massfraction 1 ~ 40%, the AgNO of 0.001 ~ 1mol/L
3And the H of massfraction 0.1% ~ 10%
2O
2The corrosive liquid of forming, the liquor capacity compactedness of agitated reactor is 40 ~ 90%, in the corrosion 1 minute ~ 2 hours down of 10 ~ 100 ℃ of temperature, can prepare required backing material porous silicon nano-wire array at the bottom of the active group after handling through above-mentioned metal assistant chemical etch.Place the precious metal salt solution of 0.001 ~ 1mol/L or the HF/0.001 of massfraction 1 ~ 40% ~ 1mol/L precious metal salt mixed solution to flood 1 second ~ 1 hour the porous silicon nano-wire array.Because the porous silicon nano-wire array has reductibility, can the precious metal ion in the solution be reduced into metal simple-substance, and with the form of nano particle on porous silicon nano-wire array surface uniform deposition.Dipping finishes that the back takes out that nature dries or at N
2In dry up, be surface-enhanced Raman scattering activity substrate based on porous silicon nano-wire array/noble metal nano particles composite structure.Introduce test substance through titration or immersion process; The solution that is about to contain test substance is titrated to active group ground surface that method for preparing goes out through pipettor or directly with in the solution that is immersed in material to be detected at the bottom of the active group 1 minute-1 hour, and substrate detects and obtain the SERS spectrum of test substance to surface-enhanced Raman scattering activity can to use Raman spectrometer.
The preparation method of described a kind of surface-enhanced Raman scattering activity substrate based on porous silicon nano-wire array/noble metal nano particles composite structure, it is characterized in that: the precious metal salt that uses in the stain process is AgNO
3Or HAuCl
4
The application of described a kind of surface-enhanced Raman scattering activity substrate based on porous silicon nano-wire array/noble metal nano particles composite structure; It is characterized in that: said substrate can be used for the chemical molecular of unknown kind, unknown concentration or biomolecule are carried out detection by quantitative; Utilize " finger-print " characteristic of Raman signal characteristic peak to confirm the kind of solution, utilize the quantitative relationship curve of setting up between intensity and the known standard substance solution concentration of Raman signal characteristic peak to confirm the concentration of solution to be measured.
The application of described a kind of surface-enhanced Raman scattering activity substrate based on porous silicon nano-wire array/noble metal nano particles composite structure is characterized in that: can detectable concentration between 10
-2～10
-16The chemical substance of the mol/L order of magnitude or living matter, chemical substance comprise agricultural chemicals, food additives, halogenated hydrocarbons, colorant, and living matter comprises protein, enzyme, bacterium, virus, nucleosides.
Description of drawings:
Fig. 1: the microcosmic synoptic diagram of a kind of metallics array based SERS substrate.
1. monocrystalline substrate
2. porous silicon nano-wire array
3. porous silicon nano wire
4. noble metal nano particles
Embodiment:
Following illustrative example and some further explanations.
Embodiment one:
(1) is that the n of 2 Ω cm or the monocrystalline silicon piece of p type place agitated reactor with resistivity, fills by the HF of massfraction 10%, the AgNO of 0.005mol/L
3And the H of massfraction 0.5%
2O
2The corrosive liquid of forming, the liquor capacity compactedness of agitated reactor is 80%, corrodes 15 minutes down for 50 ℃ in temperature, can prepare the required backing material porous silicon nano-wire array of substrate after handling through above-mentioned metal assistant chemical etch;
(2) the porous silicon nano-wire array is placed the AgNO of 0.01mol/L
3Dipping is 2 minutes in the solution, and taking-up is used N after cleaning
2Dry up, promptly obtain the substrate of metallics array based SERS;
(3) rhodamine 6G solution is dripped to substrate surface with the mode of hanging drop, put into Raman spectrometer analysis, detectability can be low to moderate 10
-16Mol/L.
Embodiment two:
(1) is that the monocrystalline silicon piece of n type (111) orientation of 0.001 Ω cm places agitated reactor with resistivity, fills by the HF of massfraction 1%, the AgNO of 0.001mol/L
3And the H of massfraction 0.1%
2O
2The corrosive liquid of forming, the liquor capacity compactedness of agitated reactor is 40%, corrodes 2 hours down for 10 ℃ in temperature, can prepare the required backing material porous silicon nano-wire array of substrate after handling through above-mentioned metal assistant chemical etch;
(2) the porous silicon nano-wire array is placed the HF and the 1mol/L AgNO of massfraction 40%
3Dipping takes out nature after 1 second and dries in the mixed solution, promptly obtains the substrate of metallics array based SERS;
(3) agricultural chemicals thiram (Thiram) solution is dripped to substrate surface with the mode of hanging drop, put into Raman spectrometer analysis, detectability can be low to moderate 10
-12Mol/L.
Embodiment three:
(1) is that the monocrystalline silicon piece of p type (100) orientation of 50 Ω cm places agitated reactor with resistivity, fills by the HF of massfraction 40%, the AgNO of 1mol/L
3And the H of massfraction 10%
2O
2The corrosive liquid of forming, the liquor capacity compactedness of agitated reactor is 90%, corrodes 1 minute down for 100 ℃ in temperature, can prepare the required backing material porous silicon nano-wire array of substrate after handling through above-mentioned metal assistant chemical etch;
(2) the porous silicon nano-wire array is placed the HAuCl of 0.0001mol/L
4Dipping took out and cleans the back at N in 1 hour in the solution
2In dry up, promptly obtain the substrate of metallics array based SERS;
(3) substrate is immersed in the rhodamine 6G solution 1 hour, dries after the taking-up, put into Raman spectrometer analysis, detectability can be low to moderate 10
-12Mol/L.
Claims (4)
1. the preparation method of metallics array based SERS substrate is characterized in that, may further comprise the steps:
(1) is that the n of 0.001-50 Ω cm or the monocrystalline silicon piece of p type place agitated reactor with resistivity, fills by the HF of massfraction 1 ~ 40%, the AgNO of 0.001 ~ 1mol/L
3And the H of massfraction 0.1% ~ 10%
2O
2The corrosive liquid of forming, the liquor capacity compactedness of agitated reactor is 40 ~ 90%, corrodes 1 minute ~ 2 hours down for 10 ~ 100 ℃ in temperature, can prepare the required backing material porous silicon nano-wire array of substrate after handling through above-mentioned metal assistant chemical etch;
(2) place the precious metal salt solution of 0.0001 ~ 1mol/L or the HF/0.0001 of massfraction 1 ~ 40% ~ 1mol/L precious metal salt mixed solution dipping to take out nature after 1 second ~ 1 hour the porous silicon nano-wire array and dry, or at N
2In dry up, promptly obtain the substrate of metallics array based SERS.
2. the preparation method of a kind of metallics array based SERS as claimed in claim 1 substrate, it is characterized in that: the precious metal salt that uses in the dip process is AgNO
3Or HAuCl
4
3. the application of a kind of metallics array based SERS according to claim 1 substrate; It is characterized in that: said substrate is used for the chemical molecular of unknown kind, unknown concentration or biomolecule are carried out detection by quantitative; Utilize " finger-print " characteristic of Raman signal characteristic peak to confirm the kind of solution, utilize the quantitative relationship curve of setting up between intensity and the known standard substance solution concentration of Raman signal characteristic peak to confirm the concentration of solution to be measured.
4. the application of a kind of metallics array based SERS according to claim 1 substrate, it is characterized in that: detectable concentration is between 10
-2～10
-16The chemical substance of the mol/L order of magnitude or living matter, chemical substance comprise agricultural chemicals, food additives, halogenated hydrocarbons, colorant, and living matter comprises protein, enzyme, bacterium, virus, nucleosides.
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| CN102976266A (en) * | 2012-12-03 | 2013-03-20 | 东南大学 | Surface enhanced Raman scattering tag based on gold and silver nanowire array and preparation method thereof |
| CN103149194A (en) * | 2013-02-28 | 2013-06-12 | 西安交通大学 | Method for preparing surface-enhanced Raman scattering (SERS) matrix |
| CN103258718A (en) * | 2013-05-16 | 2013-08-21 | 华北电力大学 | Method for preparing crater-type porous silicon structure based on LSP effect |
| CN103342337A (en) * | 2013-07-11 | 2013-10-09 | 昆明理工大学 | Method for preparing mesoporous silicon nanowire by metal nanoparticle auxiliary etching method |
| CN103569961A (en) * | 2013-11-20 | 2014-02-12 | 中国科学院理化技术研究所 | Preparation method for silver nanoparticle chain under inducement of silicon nanowire |
| CN103884685A (en) * | 2014-04-10 | 2014-06-25 | 新疆大学 | Au-PSM (Phase Shift Mask) substrate as well as preparation method and application thereof |
| RU2524453C2 (en) * | 2012-10-19 | 2014-07-27 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Московский государственный университет имени М.В. Ломоносова" (МГУ) | Sensitive element of sensor for molecular analysis |
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Application publication date: 20120912 |