CN102879379A - Method for preparing broken-line type inclined silver nanorod array surface enhanced Raman substrate - Google Patents
Method for preparing broken-line type inclined silver nanorod array surface enhanced Raman substrate Download PDFInfo
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- CN102879379A CN102879379A CN2012103482399A CN201210348239A CN102879379A CN 102879379 A CN102879379 A CN 102879379A CN 2012103482399 A CN2012103482399 A CN 2012103482399A CN 201210348239 A CN201210348239 A CN 201210348239A CN 102879379 A CN102879379 A CN 102879379A
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Abstract
The invention discloses a method for preparing a broken-line type inclined silver nanorod array surface enhanced Raman substrate, which belongs to the technical field of a surface enhanced Raman effect. In the invention, an electron beam evaporation film plating machine is utilized, silver is adopted as a target, the broken-line type inclined silver nanorod array with the number of inflection points of 1 to 7 obliquely grows on a silicon-based substrate or a glass-based substrate under the temperature of 200 to 260K, and the broken-line type inclined silver nanorod array surface enhanced Raman substrate is obtained; and then a rhodamine 6G as a detection molecule is utilized for calibrating the surface enhanced Roman capacity of the obtained broken-line type inclined silver nanorod array surface enhanced Raman substrate. The enhanced Roman capacity of the obtained broken-line type inclined silver nanorod array surface enhanced Raman substrate obtained by the invention is obviously stronger than that of a straight-line type inclined silver nanorod array surface enhanced Raman substrate, and is especially stronger when the number of inflection points is 3, 4 or 5; and the method provided by the invention is simple and fast, and is low in cost and high in sensitivity.
Description
Technical field
The invention belongs to the surface-enhanced Raman effects technical field, particularly the oblique excellent array surface of a kind of broken line type silver nanoparticle strengthens the preparation method of Raman substrate.
Background technology
At present, the method for the detection persistence organic poison of generally acknowledging in the world mainly is the high resolving power GC-MS(gas chromatography-mass spectrography), and the method has unique selectivity and higher sensitivity to the analysis of trace, ultratrace organic contaminant.But, the chromatographia method need to have complicated sample pretreatment process, requirement has accurate instrument, good experimental situation and well-trained operating personnel, and the standard items of using for the preparation of quantitative and qualitative analysis, and these have brought difficulty all for the application of the method.
Surface-enhanced Raman effects is used for the trace detection of chemistry, biomolecule, has highly sensitive, the advantages such as detection time is short, expense is low, nondestructive analysis.The oblique excellent array of silver nanoparticle is a kind of efficient surface enhanced Raman substrate, and the surface-enhanced Raman effects that how further to improve the oblique excellent array of silver nanoparticle becomes heat subject.
Summary of the invention
The purpose of this invention is to provide the preparation method that the oblique excellent array surface of a kind of broken line type silver nanoparticle strengthens the Raman substrate.
The preparation method that the oblique excellent array surface of described broken line type silver nanoparticle strengthens the Raman substrate is as follows:
Use the electron beam evaporation deposition machine, adopt silver as target, under the temperature of 200 ~ 260K, at silicon base or the substrate of glass good oblique excellent array of broken line type silver nanoparticle of growth discreteness that tilts, obtain the oblique excellent array surface of broken line type silver nanoparticle and strengthen the Raman substrate; Then use rhodamine 6G to demarcate the surface-enhanced Raman performance that the oblique excellent array surface of the broken line type silver nanoparticle that obtains strengthens the Raman substrate as detection molecules.
Specifically, method of the present invention may further comprise the steps:
(1) with silicon base or substrate of glass with acetone, alcohol, one by one ultrasonic cleaning of deionized water, then dry;
(2) will be fixed on the sample stage of electron beam evaporation deposition machine through the pretreated substrate of step (1);
(3) adopting argent is target, and electron beam evaporation deposition machine chamber is evacuated to 3 * 10
-5～8 * 10
-5The high vacuum of Pa;
(4) use liquid nitrogen that the sample stage temperature is reduced to 200 ~ 260K;
(5) adjust electron beam incident angle to 75～85 degree, and make sample stage static, placing substrate on the sample stage tiltedly rod of growth silver nanoparticle that tilts; Specimen rotating holder 180 degree, the silver nanoparticle that continues to be coated with equal length is rod tiltedly;
(6) repeating step (5), finally being coated with the formation total length in substrate is 300 ~ 2000nm, the flex point number is the oblique excellent array of the broken line type silver nanoparticle of N; Wherein, to count the scope of N be the integer of 1≤N≤7 to described flex point.
Described substrate and be the oblique excellent array surface of broken line type silver nanoparticle at the oblique excellent array of broken line type silver nanoparticle that substrate prepares and strengthen the Raman substrate.
The detection method of the surface-enhanced Raman performance of the oblique excellent array surface enhancing Raman of the broken line type silver nanoparticle of preparation substrate is as follows:
(1) will put into concentration with the substrate of the oblique excellent array surface enhancing Raman of the broken line type silver nanoparticle of said method preparation is 10
-6Mol/L rhodamine 6G solution soaked 30 minutes;
(2) take out the oblique excellent array surface of broken line type silver nanoparticle and strengthen the Raman substrate, brush with nitrogen stream, make the water volatilization;
(3) put into Raman spectrometer with strengthening the Raman substrate with the oblique excellent array surface of the broken line type silver nanoparticle of trace rhodamine 6G in the step (2), selecting wavelength is the light source of 514nm or 633nm, and the 3mW energy is set, and carries out the measurement of Raman spectrum.
Beneficial effect of the present invention is:
By making the oblique excellent array of silver nanoparticle form fold-line-shaped (integers of the several 1≤N of flex point≤7), obtain the surface-enhanced Raman performance and be better than the oblique excellent array surface enhancing Raman of the broken line type silver nanoparticle substrate that the oblique excellent array surface of linear pattern silver nanoparticle strengthens the Raman substrate.The method is simple, quick, cost is low, highly sensitive.
Description of drawings
Fig. 1 is the stereoscan photograph that the oblique excellent array surface of the broken line type silver nanoparticle of the different flex point numbers of preparation in the embodiment of the invention 1 strengthens the Raman substrate;
Fig. 2 is the electron beam evaporation deposition machine schematic diagram that the oblique excellent array surface of the preparation broken line type silver nanoparticle used of the present invention strengthens the Raman substrate;
Among the figure: the 1st, substrate; The 2nd, the oblique excellent array of broken line type silver nanoparticle of deposition; The 3rd, the incident angle of electron beam; The 4th, the solid-state part of silver-colored evaporation source; The 5th, silver-colored evaporation source melt portions; The 6th, electron beam; The 7th, sample stage.
Fig. 3 is the surface-enhanced Raman the performance test results that the oblique excellent array surface of the broken line type silver nanoparticle of the embodiment of the invention 1 preparation strengthens the Raman substrate.
Embodiment
The present invention will be further described below in conjunction with accompanying drawing and specific embodiment:
The present invention is the inclination growing method of utilizing temperature control, and plated metal silver on silicon base or substrate of glass obtains the oblique excellent array surface of broken line type silver nanoparticle and strengthens the Raman substrate; Then the aqueous solution by rhodamine 6G characterizes the surface-enhanced Raman performance that the oblique excellent array surface of broken line type silver nanoparticle strengthens the Raman substrate; Find when flex point is counted the integer of N position 1≤N≤7, the oblique excellent array surface of broken line type silver nanoparticle strengthens the Raman substrate and is improved than the surface-enhanced Raman effects that the oblique excellent array surface of linear pattern silver nanoparticle strengthens the Raman substrate.
Embodiment 1:
(1) with the one by one ultrasonic cleaning and drying of silicon base 1 usefulness acetone, alcohol, deionized water;
(2) will be fixed on the sample stage 7 of electron beam evaporation deposition machine through the pretreated silicon base 1 of step (1);
(3) adopting argent is target, and the chamber of electron beam evaporation deposition machine is evacuated to 3 * 10
-5The high vacuum of Pa;
(4) use liquid nitrogen that the sample stage temperature is reduced to 200 ~ 260K;
(5) adjust incident angle 3 to 80 degree of electron beam 6, and make sample stage 7 static, placing silicon base 1 on the sample stage 7 tiltedly rod of growth silver nanoparticle that tilts; Specimen rotating holder 180 degree, the silver nanoparticle that continues to be coated with equal length is rod tiltedly;
(6) repeating step (5), finally being coated with the formation total length in substrate is 300 ~ 2000nm, the flex point number is the oblique excellent array of the broken line type silver nanoparticle of N; The described oblique excellent array of broken line type silver nanoparticle for preparing in substrate is the oblique excellent array surface of broken line type silver nanoparticle and strengthens the Raman substrate.
The stereoscan photograph of the oblique excellent array of broken line type silver nanoparticle of the different flex point numbers that prepare as shown in Figure 1; The numerical value of N representative is the tiltedly flex point number of rod of fold-line-shaped silver nanoparticle among the figure.
The surface-enhanced Raman performance that the oblique excellent array surface of the broken line type silver nanoparticle of preparation strengthens the Raman substrate adopts following method to detect:
(1) rhodamine 6G is water-soluble, be made into 10
-6Then the solution of mol/L strengthen the Raman substrate with the oblique excellent array surface of the broken line type silver nanoparticle that makes and soaked 30 minutes in the rhodamine 6G solution for preparing;
(2) take out the oblique excellent array surface of broken line type silver nanoparticle and strengthen the Raman substrate, brush with the substrate of the oblique excellent array surface enhancing Raman of the broken line type silver nanoparticle of rhodamine 6G with nitrogen stream, make the water volatilization;
(3) put into Raman spectrometer with strengthening the Raman substrate with the oblique excellent array surface of the broken line type silver nanoparticle of trace rhodamine 6G in the step (2), selecting wavelength is the light source of 633nm, and the 3mW energy is set, carry out the measurement of Raman spectrum, to characterize the surface-enhanced Raman performance of substrate;
The result who measures as shown in Figure 3; As seen from Figure 3, when the scope of counting N when flex point was the integer of 1≤N≤7, it is strong that the surface-enhanced Raman performance that the oblique excellent array surface of broken line type silver nanoparticle strengthens the Raman substrate all strengthens the Raman substrate than the oblique excellent array surface of linear pattern (N=0) silver nanoparticle; When N was the integer of 1≤N≤4, the surface-enhanced Raman performance that the oblique excellent array surface of broken line type silver nanoparticle strengthens the Raman substrate raise gradually; When but the value of counting N when flex point was 5,6,7, the surface-enhanced Raman performance that the oblique excellent array surface of broken line type silver nanoparticle strengthens the Raman substrate reduced gradually.
Claims (4)
1. the preparation method of the oblique excellent array surface enhancing Raman of broken line type silver nanoparticle substrate is characterized in that, described method may further comprise the steps:
(1) with substrate acetone, alcohol, one by one ultrasonic cleaning of deionized water, then dries;
(2) will be fixed on the sample stage of electron beam evaporation deposition machine through the pretreated substrate of step (1);
(3) adopting argent is target; Electron beam evaporation deposition machine chamber is evacuated to 3 * 10
-5～8 * 10
-5The high vacuum of Pa;
(4) the sample stage temperature is reduced to 200 ~ 260K;
(5) adjust electron beam incident angle to 75～85 degree, and make sample stage static, placing substrate on the sample stage tiltedly rod of growth silver nanoparticle that tilts; Specimen rotating holder 180 degree, the silver nanoparticle that continues to be coated with equal length is rod tiltedly;
(6) repeating step (5), finally being coated with the formation total length in substrate is 300 ~ 2000nm, the flex point number is the oblique excellent array of the broken line type silver nanoparticle of N;
Described substrate and be the oblique excellent array surface of broken line type silver nanoparticle at the oblique excellent array of broken line type silver nanoparticle that substrate prepares and strengthen the Raman substrate.
2. method according to claim 1 is characterized in that, described substrate is silicon base or substrate of glass.
3. method according to claim 1 is characterized in that, uses liquid nitrogen that the sample stage temperature is reduced to 200 ~ 260K.
4. method according to claim 1 is characterized in that, the scope that described flex point is counted N is the integer of 1≤N≤7.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104181143A (en) * | 2014-08-08 | 2014-12-03 | 清华大学 | High-stability surface-enhanced Raman substrate and preparation method thereof |
| CN104404512A (en) * | 2014-10-10 | 2015-03-11 | 清华大学 | High-stability recyclable surface-enhanced Raman substrate and preparation method |
| CN108680556A (en) * | 2018-05-14 | 2018-10-19 | 清华大学 | A kind of silver aluminium solid solution nanorod surfaces enhancing Raman substrate and preparation method thereof |
| CN108707867A (en) * | 2018-04-25 | 2018-10-26 | 清华大学 | A kind of Surface enhanced Raman scattering substrate and preparation method thereof |
| CN109916877A (en) * | 2019-03-25 | 2019-06-21 | 中国工程物理研究院材料研究所 | A kind of flexible surface enhancing Raman scattering substrate and its preparation, detection method |
| CN111218653A (en) * | 2020-01-14 | 2020-06-02 | 江苏师范大学 | Surface-enhanced Raman scattering substrate of spatially folded silver nanorods and preparation method thereof |
| CN111398245A (en) * | 2020-04-13 | 2020-07-10 | 清华大学 | Periodically arranged handrail type surface enhanced Raman substrate and preparation method thereof |
| CN111443072A (en) * | 2020-04-30 | 2020-07-24 | 苏州翊清环境科技有限公司 | Raman chip for virus detection, preparation method and virus rapid detection method |
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| CN101398382A (en) * | 2008-10-23 | 2009-04-01 | 清华大学 | Method for rapidly detecting trace amount pentachlorinated biphenyl |
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Patent Citations (1)
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| CN101398382A (en) * | 2008-10-23 | 2009-04-01 | 清华大学 | Method for rapidly detecting trace amount pentachlorinated biphenyl |
Non-Patent Citations (1)
| Title |
|---|
| QIN ZHOU ET.AL: "Enhanced surface-enhanced Raman Scattering performance by folding silver nanorods", 《APPLIED PHYSICS LETTERS》, 12 March 2012 (2012-03-12) * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104181143A (en) * | 2014-08-08 | 2014-12-03 | 清华大学 | High-stability surface-enhanced Raman substrate and preparation method thereof |
| CN104404512A (en) * | 2014-10-10 | 2015-03-11 | 清华大学 | High-stability recyclable surface-enhanced Raman substrate and preparation method |
| CN108707867A (en) * | 2018-04-25 | 2018-10-26 | 清华大学 | A kind of Surface enhanced Raman scattering substrate and preparation method thereof |
| CN108680556A (en) * | 2018-05-14 | 2018-10-19 | 清华大学 | A kind of silver aluminium solid solution nanorod surfaces enhancing Raman substrate and preparation method thereof |
| CN109916877A (en) * | 2019-03-25 | 2019-06-21 | 中国工程物理研究院材料研究所 | A kind of flexible surface enhancing Raman scattering substrate and its preparation, detection method |
| CN111218653A (en) * | 2020-01-14 | 2020-06-02 | 江苏师范大学 | Surface-enhanced Raman scattering substrate of spatially folded silver nanorods and preparation method thereof |
| CN111218653B (en) * | 2020-01-14 | 2022-03-11 | 江苏师范大学 | Surface-enhanced Raman scattering substrate of spatially folded silver nanorods and preparation method thereof |
| CN111398245A (en) * | 2020-04-13 | 2020-07-10 | 清华大学 | Periodically arranged handrail type surface enhanced Raman substrate and preparation method thereof |
| CN111443072A (en) * | 2020-04-30 | 2020-07-24 | 苏州翊清环境科技有限公司 | Raman chip for virus detection, preparation method and virus rapid detection method |
| CN111443072B (en) * | 2020-04-30 | 2023-12-22 | 苏州翊清环境科技有限公司 | Raman chip for virus detection, preparation method and virus rapid detection method |
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Application publication date: 20130116 |