CN105300956A - Preparation method for Raman enhancement substrate - Google Patents
Preparation method for Raman enhancement substrate Download PDFInfo
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- CN105300956A CN105300956A CN201510686767.9A CN201510686767A CN105300956A CN 105300956 A CN105300956 A CN 105300956A CN 201510686767 A CN201510686767 A CN 201510686767A CN 105300956 A CN105300956 A CN 105300956A
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Abstract
The invention provides a preparation method for a Raman enhancement substrate. By the utilization of magnetron sputtering, a zinc nanometer film of a certain thickness is prepared; a silver nitrate-cetyl trimethyl ammonium bromide (CTAB) mixed solution of a certain concentration is prepared; a prepared zinc nanometer film glass sheet is placed into the mixed solution for certain time and then taken out; the substrate which is taken out is washed several times with alcohol and deionized water until CTAB is completely washed away. The preparation method is simple in technology, easy to control and good in repeatability and has commercial value.
Description
Technical field
The invention belongs to materials chemistry technology and detect analysis field, relating to a kind of preparation method with the substrate of Raman enhancing effect.
Background technology
Raman scattering spectrum, because it is to the specificity at molecule and chemical bond oscillations peak, becomes a powerful molecular detection technology.Due to the scattering xsect that Raman scattering is very little, Raman scattering is a very weak process, and is unfavorable for the qualitative analysis of micro substance.Can scattering be made to strengthen be the practical keys of raman scattering spectrum Detection Techniques.Fleischman in 1974 observes the Raman diffused light spectral intensity being attached to textured metal micro-nano structure surface molecular and can increase substantially, and is called as Surface enhanced raman spectroscopy (Surface-enhancedRamanScattering is called for short SERS).Surface enhanced raman spectroscopy (SERS) is that one has surface optionally enhancement effect, the Raman signal of the molecule being adsorbed on material surface can be amplified several order of magnitude, can reach overdelicate detection in the fields such as analysis, environment and catalysis.
Surface Raman enhancement substrate generally uses the noble metals such as silver, gold, copper as coarse metal surface.
A lot, these methods mainly comprise the self assembly of metal nanoparticle to the current bibliographical information about surface Raman enhancement substrate preparation method, reactive ion etching (RIE), electron beam lithography (EBL) and nanosphere etching etc.But all there is multiple shortcoming in current method.Nano particle is poor from group leader's repeatability, RIE and EBL cost is higher, and preparation difficulty.Strengthen for substrate for practical Raman, the repeatability of substrate, the sensitivity of detection and the cost of preparation are all the factors needing to consider.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides the preparation method that a kind of Raman strengthens substrate, there is good sensitivity, and preparation technology is simple, reproducible, can large area preparation.
Raman strengthens a preparation method for substrate, it is characterized in that, comprises following steps:
(1) magnetron sputtering is utilized to prepare certain thickness zinc nano thin-film in substrate of glass;
(2) finite concentration silver nitrate-cetyl trimethyl ammonium bromide (CTAB) mixed solution is prepared;
(3) the zinc nano thin-film glass sheet prepared by step (1) is inserted certain hour in the mixed solution described in step (2), take out;
(4) by take out substrate alcohol and deionized water rinsing repeatedly, clean CTAB.
In step (1), described zinc nano film thickness is 50-100nm.
In step (2), described mixed solution, silver nitrate concentration and CTAB concentration are 2:1, and wherein silver nitrate is 0.01M-0.1M.
In step (3), described certain hour is 10s-60s.
In step (4), described flushing repeatedly, at least alternately by alcohol and washed with de-ionized water 10 times.
The present invention utilizes simple displacement reaction, the silver nano-grain of certain dispersion is formed on zinc nano thin-film surface, size and the distribution of silver nano-grain can be controlled easily by reaction time, reaction density, zinc nano film thickness, there is good Raman-enhancing energy, technique is simple, easy to control, reproducible, there is commercial value.
Accompanying drawing explanation
The SEM figure of Fig. 1 nanometer Ag substrate prepared by embodiment 1.
Nanometer Ag substrate can figure to the Raman-enhancing of glycerine prepared by embodiment 1-4 for Fig. 2.
Embodiment
Embodiment 1:
Utilize magnetron sputtering to prepare the thick zinc nano thin-film of 50nm in substrate of glass, configuration 0.01M silver nitrate and 0.005MCTAB mixed solution, inserts prepared mixed solution 60s by the Nano-Zinc base of preparation, takes out, by alcohol and washed with de-ionized water 10 times.Fig. 1 is that prepared substrate SEM schemes.
Embodiment 2:
Utilize magnetron sputtering to prepare the thick zinc nano thin-film of 100nm in substrate of glass, configuration 0.03M silver nitrate and 0.015MCTAB mixed solution, inserts prepared mixed solution 30s by the Nano-Zinc base of preparation, takes out, by alcohol and washed with de-ionized water 10 times.
Embodiment 3:
Utilize magnetron sputtering to prepare the thick zinc nano thin-film of 80nm in substrate of glass, configuration 0.05M silver nitrate and 0.025MCTAB mixed solution, inserts prepared mixed solution 20s by the Nano-Zinc base of preparation, takes out, by alcohol and washed with de-ionized water 10 times.
Embodiment 4:
Utilize magnetron sputtering to prepare the thick zinc nano thin-film of 80nm in substrate of glass, configuration 0.1M silver nitrate and 0.05MCTAB mixed solution, inserts prepared mixed solution 10s by the Nano-Zinc base of preparation, takes out, by alcohol and washed with de-ionized water 10 times.
Raman the various embodiments described above prepared strengthens substrate and is used for 10
-6the Raman signal test of the glycerite of M, as shown in Figure 2, result shows that prepared base has glycerine Raman signal and obviously strengthens effect test result.
Claims (5)
1. Raman strengthens a preparation method for substrate, it is characterized in that, comprises following steps:
(1) magnetron sputtering is utilized to prepare certain thickness zinc nano thin-film in substrate of glass;
(2) finite concentration silver nitrate-cetyl trimethyl ammonium bromide (CTAB) mixed solution is prepared;
(3) the zinc nano thin-film glass sheet prepared by step (1) is inserted certain hour in the mixed solution described in step (2), take out;
(4) by take out substrate alcohol and deionized water rinsing repeatedly, clean CTAB.
2. a kind of Raman according to claim 1 strengthens the preparation method of substrate, and it is characterized in that, in step (1), described zinc nano film thickness is 50-100nm.
3. a kind of Raman according to claim 1 strengthens the preparation method of substrate, and it is characterized in that, in step (2), described mixed solution, silver nitrate concentration and CTAB concentration are 2:1, and wherein silver nitrate is 0.01M-0.1M.
4. a kind of Raman according to claim 1 strengthens the preparation method of substrate, and it is characterized in that, in step (3), described certain hour is 10s-60s.
5. a kind of Raman according to claim 1 strengthens the preparation method of substrate, it is characterized in that, in step (4), described flushing repeatedly, at least alternately by alcohol and washed with de-ionized water 10 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510686767.9A CN105300956A (en) | 2015-10-22 | 2015-10-22 | Preparation method for Raman enhancement substrate |
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| CN201510686767.9A CN105300956A (en) | 2015-10-22 | 2015-10-22 | Preparation method for Raman enhancement substrate |
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| CN105300956A true CN105300956A (en) | 2016-02-03 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105755431A (en) * | 2016-04-25 | 2016-07-13 | 上海交通大学 | Preparation method for synthesizing gold nanoparticle-coated SERS substrate on basis of replacement method |
| CN108318472A (en) * | 2017-12-28 | 2018-07-24 | 肇庆市华师大光电产业研究院 | A kind of preparation method for the surface enhanced Raman scattering substrate that high sensitivity is quickly analyzed |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005077362A (en) * | 2003-09-03 | 2005-03-24 | Keio Gijuku | Method for creating surface strengthening raman scattering active substrate |
| CN102634780A (en) * | 2012-04-23 | 2012-08-15 | 山东大学 | Method for covering silver nanoparticle aggregate on solid substrate material |
| CN103074627A (en) * | 2013-01-17 | 2013-05-01 | 中国科学院微电子研究所 | Method for preparing compound semiconductor sensitive membrane based on replacement reaction-thermal oxidation method |
| CN204405548U (en) * | 2014-12-26 | 2015-06-17 | 中国农业科学院农产品加工研究所 | A kind of portable SERS detects dull and stereotyped |
-
2015
- 2015-10-22 CN CN201510686767.9A patent/CN105300956A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005077362A (en) * | 2003-09-03 | 2005-03-24 | Keio Gijuku | Method for creating surface strengthening raman scattering active substrate |
| CN102634780A (en) * | 2012-04-23 | 2012-08-15 | 山东大学 | Method for covering silver nanoparticle aggregate on solid substrate material |
| CN103074627A (en) * | 2013-01-17 | 2013-05-01 | 中国科学院微电子研究所 | Method for preparing compound semiconductor sensitive membrane based on replacement reaction-thermal oxidation method |
| CN204405548U (en) * | 2014-12-26 | 2015-06-17 | 中国农业科学院农产品加工研究所 | A kind of portable SERS detects dull and stereotyped |
Non-Patent Citations (1)
| Title |
|---|
| 杨衡: "新型表面增强拉曼散射基底的制备及相关机理研究", 《中国博士学位论文全文数据库 工程科技I辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105755431A (en) * | 2016-04-25 | 2016-07-13 | 上海交通大学 | Preparation method for synthesizing gold nanoparticle-coated SERS substrate on basis of replacement method |
| CN108318472A (en) * | 2017-12-28 | 2018-07-24 | 肇庆市华师大光电产业研究院 | A kind of preparation method for the surface enhanced Raman scattering substrate that high sensitivity is quickly analyzed |
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Application publication date: 20160203 |