CN103398996A - Rapid preparation method of regular triangular pyramid SERS active substrate - Google Patents
Rapid preparation method of regular triangular pyramid SERS active substrate Download PDFInfo
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- CN103398996A CN103398996A CN201310341015XA CN201310341015A CN103398996A CN 103398996 A CN103398996 A CN 103398996A CN 201310341015X A CN201310341015X A CN 201310341015XA CN 201310341015 A CN201310341015 A CN 201310341015A CN 103398996 A CN103398996 A CN 103398996A
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Abstract
Belonging to the technical field of laser Raman spectroscopy and trace drug detection, the invention in particular relates to a high sensitivity SERS (furface enhanced Raman scattering) sensor active substrate for drug detection and a preparation method thereof. The regular triangular pyramid SERS active substrate provided in the invention is a noble metal nano-pyramid array structure coated on a base chip. The noble metal material can be silver, copper and/or gold. The high sensitivity SERS sensor active substrate provided in the invention has surface enhanced Raman activity and high repetition rate, and can be used for detection of trace compounds such as drugs, explosives and the like.
Description
Technical field
The invention belongs to laser Raman spectroscopy and trace poisonous and harmful inorganic molecules detection technique field, be specifically related to a kind of sensor of high sensitivity SERS for detection of drugs active substrate and preparation method thereof; More particularly, the present invention relates to a kind of surface reinforced Raman active that has, repetition rate is high, can be used for high sensitivity SERS sensor active substrate of the detections such as trace compound such as drugs, explosive and preparation method thereof.
Background technology
As the common method of analyzing molecules vibrational spectrum, the laser raman technology be widely used in differentiating material molecular structure, analyze the field such as Surface bonding state.Yet the Ramam effect signal often very a little less than, when the concentration of tested molecule is less, or the effects on surface adsorbent is while surveying, conventional laser Raman method just seems unable to do what one wishes.Surface enhanced raman spectroscopy (SERS) effect can make the Raman scattering of molecule signal that is adsorbed on the textured metal substrate surface greatly be strengthened, therefore be used as a kind of highly sensitive surface analysis Detection Techniques, in fields such as trace analysis and qualitative detection, Surface Science, bio-science, obtained broad research.
It is simple that desirable SERS active substrate should have the preparation method, even surface roughness, the characteristics such as effective, good reproducibility that strengthen.The method for preparing the SERS substrate commonly used: the one, utilize chemistry or electrochemical method to make the surface of metal electrode roughening, obtain having the rough surface of high-specific surface area; Another kind method is the metal-sol that preparation has nanoscale, load is had the substrate of metal-sol particle as strengthening substrate.The maximum enhancing substrate of application at present is silver or golden sol particle, have stronger SERS effect, but signal reproducibility and poor stability is not easy to store.Given this, develop a kind ofly possess simultaneously simple, even surface roughness, enhancing is effective, and having the active SERS substrate of enough stability and repeatability necessary, this has great importance widening the application of SERS at aspects such as trace minute qualitative detection and unimolecule system spectrum.
Based on the explosive drugs detection instrument that laser Raman spectroscopy is sent out, its core is development and the exploitation of SERS sensor; And the gordian technique of SERS sensor is the performance of high sensitivity SERS active substrate on detecting head.The quality of this active substrate, can cause other difference of detecting concentration level even more than 10000 times, will affect greatly detection sensitivity and the performance of drugs detection system.The active substrate SERS enhancer of report is basically all 10 now
6Rank, be used for super quick detection trace drugs and also have certain difficulty.Such as national 11th Five-Year science and technology supporting project just requires will reach 100ng/ml to drugs such as the lowest detectable limit such as ketamine, KET in body fluid or urine, roughly in the 100ppb rank.This high sensor active substrate will have very big meaning to improving the sensitivity of explosive drugs SERS detection instrument.
Summary of the invention
The purpose of this invention is to provide the positive triangular pyramidal SERS of a kind of high sensitivity sensor active substrate, thereby the solution the above-mentioned problems in the prior art, this high sensitivity SERS active substrate of the present invention should have high SERS enhancing and sensitivity, tack is good, volume is little, good portability.
For achieving the above object, the present invention adopts following operation steps:
(1) polystyrene microsphere is tiled at the substrate surface individual layer.
(2) substrate surface evaporation or the sputter noble metal film modified at polystyrene.
(3) substrate is positioned in ultrasonic solution, ultrasonic processing is disposed polystyrene microsphere and is obtained the active substrate of SERS.
In the present invention, SERS active substrate used can be for being silicon chip or electro-conductive glass.
In the present invention, described precious metal film layer adopts magnetron sputtering or metal evaporation to be formed on substrate.The thickness of metallic film, to 500nm, preferably is about 200nm at 50nm.
In the present invention, the diameter of polystyrene microsphere is 50-500nm, preferably is about 100nm.
In the present invention, ultrasonic solution can, for absolute ethyl alcohol or phenixin, be preferably ethanol solution.
The SERS active substrate preparation method that the present invention proposes, simple to operate, favorable reproducibility, reduced the consumption of reagent and sample, reduced the time of sample preparation and detection, have portable, economical, fast, efficiently, characteristics accurately, have a good application prospect at aspects such as trace analysis, qualitative detection.
Description of drawings
Fig. 1. be high-amplification-factor scanning electron microscope (SEM) the pattern photo of SERS active substrate noble metal nano cone array structure of the present invention.
Fig. 2. be the present invention take the 10nM isonicotinic acid as probe molecule, relatively (A) is adsorbed on nanocone volume array structural substrates, (B) Raman spectrum of silicon base.Exciting light is 532nm, and firing time is 5s.
Specific embodiments
Embodiment 1
The 200nm polystyrene microsphere is tiled at Si substrate surface individual layer, gold thin film at the hot evaporation 100nm of substrate surface that modifies through polystyrene, subsequently substrate is positioned in the absolute ethyl alcohol ultrasonic solution, processing in ultrasonic 2 minutes is disposed polystyrene microsphere and is obtained the active substrate of SERS.
Embodiment 2
The 100nm polystyrene microsphere is tiled at electro-conductive glass substrate surface individual layer, silver-colored film at the hot evaporation 100nm of substrate surface that modifies through polystyrene, subsequently substrate is positioned in the absolute ethyl alcohol ultrasonic solution, processing in ultrasonic 2 minutes is disposed polystyrene microsphere and is obtained the active substrate of SERS.
Embodiment 3
The 300nm polystyrene microsphere is tiled at electro-conductive glass substrate surface individual layer, copper film at the hot evaporation 200nm of substrate surface that modifies through polystyrene, subsequently substrate is positioned in the phenixin ultrasonic solution, processing in ultrasonic 2 minutes is disposed polystyrene microsphere and is obtained the active substrate of SERS.
Claims (8)
1. fast preparation method with the active substrate of positive triangular pyramidal SERS, described positive triangular pyramidal SERS active substrate is to be coated in on-chip noble metal nano cone array structure, described precious metal material be silver-colored, copper and/or gold.
2., by the active substrate of positive triangular pyramidal SERS claimed in claim 1, it is characterized in that, its making step is as follows:
(1) polystyrene microsphere is tiled at the substrate surface individual layer;
(2) substrate surface evaporation or the sputter noble metal film modified at polystyrene;
(3) substrate is positioned in ultrasonic solution, ultrasonic processing is disposed polystyrene microsphere and is obtained the active substrate of SERS.
3. press the fast preparation method of the active substrate of the described positive triangular pyramidal SERS of claim 1 or 2, it is characterized in that, in described noble metal nano cone array structure, nanometer cone root diameter (RD) is about 100-500nm, cone needle point diameter is 10-20nm, and the nanocone body length is 50-1000nm.
4., by the fast preparation method of the active substrate of the described positive triangular pyramidal SERS of claim 1 or 2, it is characterized in that, the thickness of described precious metal film layer is that 100nm is to 1000nm.
5., by the fast preparation method of the active substrate of the described positive triangular pyramidal SERS of claim 1 or 2, it is characterized in that, described precious metal film layer adopts magnetron sputtering or metal evaporation to be formed on substrate.
6., by the fast preparation method of the active substrate of the described positive triangular pyramidal SERS of claim 1 or 2, it is characterized in that, substrate can be silicon chip or electro-conductive glass.
7., by the fast preparation method of the active substrate of the described positive triangular pyramidal SERS of claim 1 or 2, it is characterized in that, the diameter of polystyrene microsphere is 50-500nm.
8., by the fast preparation method of the active substrate of the described positive triangular pyramidal SERS of claim 1 or 2, it is characterized in that, ultrasonic solution can be absolute ethyl alcohol or phenixin.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104849259A (en) * | 2015-06-05 | 2015-08-19 | 中物院成都科学技术发展中心 | Preparation method of flexible surface enhanced Raman substrate |
| WO2016015599A1 (en) * | 2014-07-27 | 2016-02-04 | 北京工业大学 | Fast preparation method for large area monocrystalline silicon substrate with surface-enhanced raman spectrum |
| CN106048537A (en) * | 2016-06-22 | 2016-10-26 | 天津大学 | Method for preparing SERS substrate by combining colloidal sphere self-assembly with ion-sputtering coating |
| CN107064107A (en) * | 2017-04-11 | 2017-08-18 | 中山大学 | Super hydrophobic surface enhancing Raman substrate prepared by a kind of utilization silicon nanometer dielectric material and preparation method thereof |
| CN108344690A (en) * | 2018-01-03 | 2018-07-31 | 东南大学 | SERS substrates based on microfluidic mixer device prepare and detection integral method |
| CN109748238A (en) * | 2017-11-08 | 2019-05-14 | 厦门大学 | A kind of large area, the preparation method of uniform nanometer dimerization volume array |
| CN109856116A (en) * | 2019-02-28 | 2019-06-07 | 吉林大学 | A kind of classifying nano cone array and preparation method thereof using the chemical reaction of Surface enhanced Raman scattering in-situ monitoring |
| CN110146485A (en) * | 2019-05-23 | 2019-08-20 | 中国科学院合肥物质科学研究院 | Golden Triangle pit array material and its preparation method and application |
| CN111426675A (en) * | 2020-03-31 | 2020-07-17 | 江苏海尔森检测技术服务有限公司 | Detection method of dioxin compound |
| CN113702352A (en) * | 2021-08-25 | 2021-11-26 | 山东智微检测科技有限公司 | SERS detection chip suitable for gas-phase erosive toxicant and preparation method thereof |
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| JP2006349463A (en) * | 2005-06-15 | 2006-12-28 | Canon Inc | Surface reinforcing raman spectroscopic analyzing jig and its manufacturing method |
| CN102628808A (en) * | 2012-04-13 | 2012-08-08 | 中国科学院光电技术研究所 | Preparation method and application method of high-sensitivity and high-stability surface-enhanced Raman chip |
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Patent Citations (2)
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| JP2006349463A (en) * | 2005-06-15 | 2006-12-28 | Canon Inc | Surface reinforcing raman spectroscopic analyzing jig and its manufacturing method |
| CN102628808A (en) * | 2012-04-13 | 2012-08-08 | 中国科学院光电技术研究所 | Preparation method and application method of high-sensitivity and high-stability surface-enhanced Raman chip |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016015599A1 (en) * | 2014-07-27 | 2016-02-04 | 北京工业大学 | Fast preparation method for large area monocrystalline silicon substrate with surface-enhanced raman spectrum |
| CN104849259B (en) * | 2015-06-05 | 2018-02-23 | 中物院成都科学技术发展中心 | A kind of preparation method of flexible surface enhancing Raman substrate |
| CN104849259A (en) * | 2015-06-05 | 2015-08-19 | 中物院成都科学技术发展中心 | Preparation method of flexible surface enhanced Raman substrate |
| CN106048537A (en) * | 2016-06-22 | 2016-10-26 | 天津大学 | Method for preparing SERS substrate by combining colloidal sphere self-assembly with ion-sputtering coating |
| CN107064107B (en) * | 2017-04-11 | 2019-11-19 | 中山大学 | A kind of super hydrophobic surface enhancing Raman substrate and preparation method thereof using the preparation of silicon nanometer dielectric material |
| CN107064107A (en) * | 2017-04-11 | 2017-08-18 | 中山大学 | Super hydrophobic surface enhancing Raman substrate prepared by a kind of utilization silicon nanometer dielectric material and preparation method thereof |
| CN109748238A (en) * | 2017-11-08 | 2019-05-14 | 厦门大学 | A kind of large area, the preparation method of uniform nanometer dimerization volume array |
| CN109748238B (en) * | 2017-11-08 | 2020-03-17 | 厦门大学 | Preparation method of large-area and uniform nano dimer array |
| CN108344690A (en) * | 2018-01-03 | 2018-07-31 | 东南大学 | SERS substrates based on microfluidic mixer device prepare and detection integral method |
| CN108344690B (en) * | 2018-01-03 | 2021-01-26 | 东南大学 | Preparation and detection integrated method of SERS substrate based on micro-flow mixer |
| CN109856116A (en) * | 2019-02-28 | 2019-06-07 | 吉林大学 | A kind of classifying nano cone array and preparation method thereof using the chemical reaction of Surface enhanced Raman scattering in-situ monitoring |
| CN109856116B (en) * | 2019-02-28 | 2021-06-29 | 吉林大学 | Hierarchical nanocone array for in-situ monitoring of chemical reaction by using surface enhanced Raman scattering and preparation method thereof |
| CN110146485A (en) * | 2019-05-23 | 2019-08-20 | 中国科学院合肥物质科学研究院 | Golden Triangle pit array material and its preparation method and application |
| CN111426675A (en) * | 2020-03-31 | 2020-07-17 | 江苏海尔森检测技术服务有限公司 | Detection method of dioxin compound |
| CN113702352A (en) * | 2021-08-25 | 2021-11-26 | 山东智微检测科技有限公司 | SERS detection chip suitable for gas-phase erosive toxicant and preparation method thereof |
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Application publication date: 20131120 |