CN105954251A - Surface enhanced Raman scattering substrate and manufacturing method thereof - Google Patents

Surface enhanced Raman scattering substrate and manufacturing method thereof Download PDF

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Publication number
CN105954251A
CN105954251A CN201610215076.5A CN201610215076A CN105954251A CN 105954251 A CN105954251 A CN 105954251A CN 201610215076 A CN201610215076 A CN 201610215076A CN 105954251 A CN105954251 A CN 105954251A
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substrate
raman scattering
enhanced raman
surface enhanced
gold nano
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CN201610215076.5A
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宋春元
汪联辉
笪炳涛
魏玉涵
张海婷
丛兴
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Nanjing Post and Telecommunication University
Nanjing University of Posts and Telecommunications
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Nanjing Post and Telecommunication University
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65—Raman scattering
    • G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons

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  • Health & Medical Sciences (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

The invention discloses a surface enhanced Raman scattering (SERS) substrate and a manufacturing method thereof. The method comprises: immersing a substrate in a first cleaning solution, a second cleaning solution and a third cleaning solution while performing ultrasonic treatment, respectively; immersing the obtained substrate in an ethanol solution of an amino silylating agent, an aqueous solution of sodium 4-styrene sulfonate and an aqueous solution of poly(diallyldimethylammonium chloride) for modification; and co-culturing a gold nano-particle sol and the obtained substrate subjected to multiple electric charge modification, and manufacturing the SERS active gold nano-particle film solid substrate through physical deposition and electrostatic interaction. The manufacturing method of the SERS substrate is simple and easy to operate and low in equipment requirements, and enables an SERS substrate with large area to be made. The manufactured SERS substrate has excellent performance, and has certain application prospects with respect to biochemical detection.

Description

Surface enhanced Raman scattering substrate and preparation method thereof
Technical field
The present invention relates to Raman scattering substrate preparation field, be specifically related to a kind of surface enhanced Raman scattering substrate and system thereof Preparation Method.
Background technology
Surface enhanced raman spectroscopy (SERS) analyzes detection means as one a three below obvious advantage: (1) Gao Ling The enhancer of sensitivity: SERS is the highest can reach 1014-1015, it is possible to achieve Single Molecule Detection.(2) high selectivity: SERS Can only strengthen target molecule or group in complex system, obtain the Fingerprint information of target molecule.(3) testing conditions temperature With: SERS spectrum may be used for water solution system, and the physical aspect of sample is unrestricted.
In order to SERS should be had enhancing ability as a kind of routine, online analytical tool, prepared SERS substrate Strong and homogeneity is good, easily prepared and storage, the feature such as easy to use.Owing to having optical property and the nanoscale of uniqueness Rough surface, the nanostructured such as gold, silver, copper has good SERS activity;And along with the day of nano material preparation technology Benefit is ripe, and the highly controllable metal nanoparticle of size and dimension can be prepared out by multiple method.Therefore, Utilizing nanotechnology to prepare SERS active-substrate is the important development direction that current SERS studies.
The substrate of solid-state SERS because be provided simultaneously with efficient SERS enhancement effect and well spectrum repeatability become and grind Study carefully focus.At present the method for preparation solid substrate mainly has: self-assembly method, template, electron beam lithography, ion beam lithography and Growth in situ etc..As a example by self-assembly method, owing to membrane formation mechanism restricts, the spacing between particle is bigger than normal, it is difficult to formation is enriched Nano-scale particle gap, thus SERS strengthens limited performance.Electron beam lithography and ion beam lithography can obtain SERS effect Excellent enhancing substrate, but equipment cost is high, and fabrication cycle is long.It is convenient that growth in situ method has self-assembling method economy Advantage, and SERS performance is outstanding compared with self-assembling method, but repeatability is difficult to ensure that.Therefore, how by simple, economical Method prepares that enhancing ability is strong and homogeneity good, easily prepared and storage, SERS substrate easy to use remains one has Problem to be solved.
Summary of the invention
For the deficiencies in the prior art, the present invention provides a kind of surface enhanced raman spectroscopy (SERS) substrate and preparation side thereof Method, it is possible to prepare on the premise of simple economy that enhancing ability is strong and homogeneity good, easily prepared and storage, easy to use SERS substrate.
The technical scheme that the present invention takes is as follows:
The preparation method of a kind of surface enhanced Raman scattering substrate, comprises the following steps:
1) substrate is immersed successively in the first cleanout fluid, the second cleanout fluid and the 3rd cleanout fluid, respectively supersound process；
2) it is water-soluble that the substrate after step 1) being processed immerses Aminosilylation reagent alcohol solution, 4-styrene sulfonic acid fat sodium successively Liquid and diallyl dimethyl ammoniumchloride aqueous solution are modified；
3) substrate is co-cultured with gold nano-particle colloid, after 4-25 DEG C stands growth 12-15 h, remove gold nano grain glue Body, dries；
4) repeat step 3) 1 ~ 3 time, obtain surface enhanced Raman scattering substrate.
First cleanout fluid described in step 1) is ethanol, and the second cleanout fluid is acetone, and the 3rd cleanout fluid is ultra-pure water.Described The volume fraction of the first cleanout fluid ethanol is 99.7%, and the volume fraction of described second cleanout fluid acetone is 99.5%, described The three ultrapure resistivity of waters of cleanout fluid are 18.2 M Ω cm.
Supersound process 15-20 min in step 1).
Step 2) described Aminosilylation reagent is 3-aminopropyl triethoxysilane, the mass fraction of solution is 5%- 9.8%；The mass fraction of described 4-styrene sulfonic acid fat sodium solution is 3%-5%, diallyl dimethyl ammoniumchloride solution Mass fraction be 2%-5%.
Overnight (more than 8h) is processed, at 4-styrene sulfonic acid fat sodium solution with poly-in Aminosilylation reagent alcohol solution Diallyldimethylammonium chloride solution processes more than 1.5.
Described gold nano grain be shaped as flower-shaped or polyhedron, the size of gold nano grain be 402 ± 13 nm or 142±16 nm。
Described gold nano-particle colloid is adopted and is prepared with the following method: by gold chloride (HAuCl4) and cetyl front three Ammonium chloride (CTAC) mix and blend, is subsequently adding ascorbic acid (AA) stirring, stands growth, obtain gold nano-particle colloid.
Described substrate is silicon chip or sheet glass.
The surface enhanced Raman scattering substrate that described preparation method prepares.
The principle that the present invention uses is as follows: physical deposition combines Electrostatic Absorption, repeatedly surface charge and modifies, and Multiple depositions becomes Film.
Beneficial effect
Compared with existing, present invention have the advantage that
First, the present invention need not introduce complexity, the micro-nano processing method of high cost, such as oxygen rie, ion beam etching Deng the micro-nano technology technique high to equipment dependency degree, reduce the requirement to Preparation equipment；Meanwhile, the physics of gold nano grain Being deposited as spontaneously forming, it is only necessary to control basic external environment condition, process is simple and easy to do, significantly simplifies SERS substrate and prepares Technological process, low for equipment requirements, effectively reduce cost, be more beneficial for the promotion and application of the SERS substrate prepared, can Realizing large area and prepare SERS substrate, prepared SERS substrate is functional, has certain utilization prospect in terms of biochemistry detection.
Secondly, the present invention is modified and membrane formation times by regulation and control substrate surface electric charge, it is possible to realize substrate surface Jenner The controllable that rice grain density and SERS strengthen, it is thus achieved that optimum preparation process, is reducing cost, is obtaining while Simplified flowsheet Obtain the SERS substrate of function admirable.
Accompanying drawing explanation
Fig. 1 is the preparation method flow chart of surface enhanced Raman scattering substrate of the present invention；
Fig. 2 is the scanning that embodiment of the present invention 1.2.3 silicon chip substrate surface flower-shaped gold nano grain film strengthens Raman scattering substrate Electron micrograph, wherein (a) embodiment 1 substrate surface gold nano grain scattergram, (b) embodiment 2 substrate surface Jenner Rice grain pattern；(c) embodiment 3 substrate surface gold nano grain pattern；Enlargement ratio is 400；
Fig. 3 is that Raman molecular 4-mercaptobenzoic acid (4-MBA) scans on the surface enhanced Raman scattering substrate of embodiment 1.2.3 The SERS spectra obtained；
Fig. 4 is the scanning electron that the embodiment of the present invention 3 silicon chip substrate surface flower-shaped gold nano grain film strengthens Raman scattering substrate Microphotograph, gold nano grain size is 402 ± 13 nm, wherein (a) substrate surface gold nano grain scattergram (times magnification Rate is 5K), (b) substrate surface gold nano grain pattern (enlargement ratio is 50K)；
Fig. 5 is the scanning of polyhedron gold nano grain film surface enhanced Raman scattering substrate on the embodiment of the present invention 4 silicon chip substrate Electron micrograph, gold nano grain size is 142 ± 16 nm, and wherein (a) substrate surface gold nano grain scattergram (is put Big multiplying power is 10K), (b) substrate surface gold nano grain pattern (enlargement ratio is 100K)；
Fig. 6 is the electron scanning micrograph of the embodiment of the present invention 5 surface enhanced Raman scattering substrate, gold nano grain size It is 402 ± 13 nm, wherein (a) substrate surface gold nano grain scattergram (enlargement ratio is 5K), (b) substrate surface gold nano Granule-morphology (enlargement ratio is 50K).
Detailed description of the invention
Material agents etc. used in following embodiment, if no special instructions, is all from commercial sources.Ethanol volume integral Number is 99.7%, and the volume fraction of acetone is 99.5%, prepares 9.8wt% Aminosilylation reagent alcohol solution, 3 wt%4- Styrene sulfonic acid fat sodium water solution (PSS), 2 wt% diallyl dimethyl ammoniumchloride aqueous solution (PDDA), by original molten Liquid with corresponding solvent dilution to the mass fraction specified.
Embodiment 1
A kind of surface enhanced Raman scattering substrate, utilizes physical deposition on the substrate through over cleaning and surface charge moditied processing With electrostatic interaction assemble nanometer particle membrane, described substrate is silicon chip, and the material of described film layer is gold nano grain.
The physical deposition method of above-mentioned surface enhanced raman spectroscopy (SERS) substrate, comprises the following steps:
Step 1, volume fraction 99.7% ethanol is the first cleanout fluid, and volume fraction 99.5% acetone is the second cleanout fluid, resistivity Be 18.2 M Ω cm ultra-pure waters be the 3rd cleanout fluid.
Step 2, preparation mass fraction is the Aminosilylation reagent alcohol solution of 9.8%, and mass fraction is the 4-benzene of 3% Vinyl sulfonic acid fat sodium water solution, mass fraction is the diallyl dimethyl ammoniumchloride aqueous solution of 2%, is used by original solution Corresponding solvent dilution is to the mass fraction specified；The solute of described Aminosilylation reagent alcohol solution is 3-aminopropyl Triethoxysilane.
Step 3, measuring 5 mL molar concentrations is 10 mM gold chloride (HAuCl4), 50 mL molar concentration 200 mM hexadecanes Base trimethyl ammonium chloride (CTAC), mix and blend 2 min, add 2.5 mL molar concentrations 0.3 M ascorbic acid (AA) and stir 2 Min, stands growth 3 h, obtains flower-shaped gold nano-particle colloid at 25 DEG C, gold nano grain size is 402 ± 13 nm；By institute Obtain colloid and be concentrated into 3 mL；
Step 4, immerses in the first cleanout fluid, the second cleanout fluid and the 3rd cleanout fluid successively by substrate, respectively ultrasonic 15-20 min；
Step 5, immerses Aminosilylation reagent alcohol solution, 4-styrene sulfonic acid fat successively by the substrate after step 4 processes Sodium water solution and diallyl dimethyl ammoniumchloride aqueous solution are modified, wherein in Aminosilylation reagent alcohol solution Submergence is no less than 8h, processes 1.5h respectively at 4-styrene sulfonic acid fat sodium solution and diallyl dimethyl ammoniumchloride solution.
20 μ L gold nano-particle colloid are co-cultured in wet box by step 6 with substrate, wetter box is put into standing in 4 DEG C Remove gold nano particle colloidal sols with liquid rifle after growing 15 h, baking oven is dried to obtain surface enhanced Raman scattering substrate.
Embodiment 2
The present embodiment step 1-5 is identical with embodiment 1, and step 7 repeats the operation of step 6, particularly as follows:
20 μ L gold nano-particle colloid are co-cultured in wet box by step 6 with substrate, wetter box is put into standing growth in 4 DEG C Remove gold nano particle colloidal sols with liquid rifle after 15 h, baking oven is dried.
Step 7, co-cultures the substrate that 20 μ L gold nano-particle colloid and step 6 are dried in wet box, then is put by wet box Remove gold nano particle colloidal sols with liquid rifle after entering 4 DEG C stand growth 15 h, baking oven is dried to obtain surface enhanced raman spectroscopy base The end.
Embodiment 3
The present embodiment step 1-6 is identical with embodiment 2, and step 7 repeats the operation twice of step 6.
Embodiment 1 ~ 3 respectively film forming once, the surface enhanced raman spectroscopy for preparing for three times of film forming twice and film forming Substrate, electron scanning micrograph is as in figure 2 it is shown, from figure 2 it can be seen that membrane formation times difference can regulate and control SERS increasing Strong and gold nano grain density, by changing membrane formation times, it is possible to realize substrate surface gold nano grain density and SERS increasing Strong controllable, on the premise of limited contact area and gold nano particle colloidal sols, the film forming of single does not ensures that all Region have uniform film of nanoparticles to be formed, the operation of repeated deposition can well solve this problem.
Raman molecular 4-mercaptobenzoic acid (4-MBA) scans on the surface enhanced Raman scattering substrate of embodiment 1.2.3 The SERS spectra figure obtained is as it is shown on figure 3, along with the increase of membrane formation times, film aspect is long-pending to be increased, and thickness increases, and grain spacing becomes Little, these SERS that can effectively improve substrate strengthen performance.
Embodiment 4
Step 1.2, step 4-6 is identical with embodiment 1, and difference is step 3, and measuring 5 mL molar concentrations is 10 mM gold chlorides (HAuCl4), 50 mL molar concentrations 200 mM hexadecyltrimethylammonium chloride (CTAC), mix and blend 2 min, add 0.5 ML gold seeds, adds 2.5 ml molar concentrations 0.3 M ascorbic acid (AA) and stirs 2 min, stands growth 3 h, obtain at 25 DEG C Polyhedral gold nano-particle colloid, gold nano grain size is 142 ± 16 nm；Gained colloid is concentrated into 3 mL；
Step 7 repeats the operation twice of step 6.
The enhancing performance of flower-shaped gold nano-particle colloid is better than polyhedral gold nano-particle colloid, and this is by granulated Looks determine, flower-shaped structure is due to its petal design, and granule self has and preferably strengthens performance, this example demonstrates that the present invention Method can be general to different morphologies granule, and application surface is wider.
Embodiment 5
Step 1-6 is with embodiment 1, and substrate used is sheet glass, and step 7 repeats the operation twice of step 6.

Claims (10)

1. the preparation method of a surface enhanced Raman scattering substrate, it is characterised in that comprise the following steps:
1) substrate is immersed successively in the first cleanout fluid, the second cleanout fluid and the 3rd cleanout fluid, respectively supersound process；
2) it is water-soluble that the substrate after step 1) being processed immerses Aminosilylation reagent alcohol solution, 4-styrene sulfonic acid fat sodium successively Liquid and diallyl dimethyl ammoniumchloride aqueous solution are modified；
3) substrate is co-cultured with gold nano-particle colloid, after 4-25 DEG C stands growth 12-15 h, remove gold nano grain glue Body, dries；
4) repeat step 3) 1 ~ 3 time, obtain surface enhanced Raman scattering substrate.
The preparation method of surface enhanced Raman scattering substrate the most according to claim 1, it is characterised in that institute in step 1) Stating the first cleanout fluid is ethanol, and the second cleanout fluid is acetone, and the 3rd cleanout fluid is ultra-pure water.
The preparation method of surface enhanced Raman scattering substrate the most according to claim 1, it is characterised in that super in step 1) Sonication 15-20 min.
The preparation method of surface enhanced Raman scattering substrate the most according to claim 1, it is characterised in that step 2) described Aminosilylation reagent is 3-aminopropyl triethoxysilane, and the mass fraction of solution is 5%-9.8%.
The preparation method of surface enhanced Raman scattering substrate the most according to claim 1, it is characterised in that step 2) described The mass fraction of 4-styrene sulfonic acid fat sodium solution is 3%-5%, the mass fraction of diallyl dimethyl ammoniumchloride solution For 2%-5%.
The preparation method of surface enhanced Raman scattering substrate the most according to claim 1, it is characterised in that described gold nano Granule be shaped as flower-shaped or polyhedron.
The preparation method of surface enhanced Raman scattering substrate the most according to claim 1, it is characterised in that institute in step 3) State gold nano-particle colloid to adopt and prepare with the following method: by gold chloride and hexadecyltrimethylammonium chloride mix and blend, It is subsequently adding ascorbic acid stirring, stands growth, obtain gold nano-particle colloid.
The preparation method of surface enhanced Raman scattering substrate the most according to claim 2, it is characterised in that described first clear The volume fraction of washing liquid ethanol is 99.7%, and the volume fraction of described second cleanout fluid acetone is 99.5%, and the described 3rd cleans The ultrapure resistivity of water of liquid is 18.2 M Ω cm.
9. the surface enhanced Raman scattering substrate that in claim 1 to 8, preparation method described in any one prepares.
Surface enhanced Raman scattering substrate the most according to claim 9, it is characterised in that described gold nano grain big Little is 402 ± 13 nm or 142 ± 16 nm.
CN201610215076.5A 2016-04-07 2016-04-07 Surface enhanced Raman scattering substrate and manufacturing method thereof Pending CN105954251A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107057257A (en) * 2017-04-20 2017-08-18 合肥学院 A kind of surface enhanced Raman scattering substrate of pH response types template assemblies, preparation method and the method using the substrate detection molecules
CN107328750A (en) * 2017-06-19 2017-11-07 吉林大学 A kind of high activity, surface enhanced Raman scattering substrate of high homogeneity and preparation method thereof
CN107884386A (en) * 2017-11-16 2018-04-06 东南大学 A kind of acetylcholine detection method based on SERS
CN108526487A (en) * 2018-06-09 2018-09-14 山东大学 A kind of preparation method of macro-size closs packing gold nano grain monofilm
CN109365831A (en) * 2018-12-19 2019-02-22 上海纳米技术及应用国家工程研究中心有限公司 The preparation method of new infrared photodetection substrate based on tip deposition Pd/Ag gold nano double cone structure
CN112441752A (en) * 2020-11-09 2021-03-05 杭州苏铂科技有限公司 Surface-enhanced Raman scattering substrate and preparation method thereof
CN113203726A (en) * 2021-05-11 2021-08-03 江苏大学 Preparation method of surface-enhanced Raman substrate for rapidly detecting fluorene in haze particles

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104807802A (en) * 2015-04-03 2015-07-29 南京邮电大学 Surface enhanced raman scattering base and in-situ growth method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104807802A (en) * 2015-04-03 2015-07-29 南京邮电大学 Surface enhanced raman scattering base and in-situ growth method thereof

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107057257A (en) * 2017-04-20 2017-08-18 合肥学院 A kind of surface enhanced Raman scattering substrate of pH response types template assemblies, preparation method and the method using the substrate detection molecules
CN107328750A (en) * 2017-06-19 2017-11-07 吉林大学 A kind of high activity, surface enhanced Raman scattering substrate of high homogeneity and preparation method thereof
CN107328750B (en) * 2017-06-19 2020-02-04 吉林大学 High-activity high-uniformity surface enhanced Raman scattering substrate and preparation method thereof
CN107884386A (en) * 2017-11-16 2018-04-06 东南大学 A kind of acetylcholine detection method based on SERS
CN107884386B (en) * 2017-11-16 2020-02-18 东南大学 Acetylcholine detection method based on surface enhanced Raman spectroscopy
CN108526487A (en) * 2018-06-09 2018-09-14 山东大学 A kind of preparation method of macro-size closs packing gold nano grain monofilm
CN108526487B (en) * 2018-06-09 2019-07-30 山东大学 A kind of preparation method of macro-size closs packing gold nano grain monofilm
CN109365831A (en) * 2018-12-19 2019-02-22 上海纳米技术及应用国家工程研究中心有限公司 The preparation method of new infrared photodetection substrate based on tip deposition Pd/Ag gold nano double cone structure
CN112441752A (en) * 2020-11-09 2021-03-05 杭州苏铂科技有限公司 Surface-enhanced Raman scattering substrate and preparation method thereof
CN113203726A (en) * 2021-05-11 2021-08-03 江苏大学 Preparation method of surface-enhanced Raman substrate for rapidly detecting fluorene in haze particles

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