CN105911044A - Surface enhanced Raman spectrum substrate with nano gap and preparation method thereof - Google Patents

Surface enhanced Raman spectrum substrate with nano gap and preparation method thereof Download PDF

Info

Publication number
CN105911044A
CN105911044A CN201610262311.4A CN201610262311A CN105911044A CN 105911044 A CN105911044 A CN 105911044A CN 201610262311 A CN201610262311 A CN 201610262311A CN 105911044 A CN105911044 A CN 105911044A
Authority
CN
China
Prior art keywords
grain
nano
silver
solution
silver nano
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201610262311.4A
Other languages
Chinese (zh)
Other versions
CN105911044B (en
Inventor
佘广为
金亮亮
师文生
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Technical Institute of Physics and Chemistry of CAS
Original Assignee
Technical Institute of Physics and Chemistry of CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Technical Institute of Physics and Chemistry of CAS filed Critical Technical Institute of Physics and Chemistry of CAS
Priority to CN201610262311.4A priority Critical patent/CN105911044B/en
Publication of CN105911044A publication Critical patent/CN105911044A/en
Application granted granted Critical
Publication of CN105911044B publication Critical patent/CN105911044B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65Raman scattering
    • G01N21/658Raman scattering enhancement Raman, e.g. surface plasmons
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

Abstract

The invention discloses a surface enhanced Raman spectrum substrate with a nano gap and a preparation method thereof. The surface enhanced Raman spectrum substrate with the nanometer gap is composed of first-layer silver nanoparticles attached on a monocrystal silicon slice and having the surface loaded with gold nanoparticles and second-layer silver nanoparticles spin-coated on the first-layer silver nanoparticles. By depositing a certain size and distribution of gold nanoparticles, the nano gap is formed between the two layers of silver nanoparticles. The surface enhanced Raman spectrum substrate with the nano gap is used for detecting 4-pyridinethiol molecules in an ethanol solution, the obtained Raman spectrum signal intensity is two times that of a substrate without gold nanoparticles. The invention provides a means for preparing the nano gap to enhance the surface enhanced Raman spectrum signal, and the reference significance is provided for preparation of the high-performance surface enhanced Raman spectrum substrate.

Description

A kind of Raman spectrum base with nano gap and preparation method thereof
Technical field
The invention belongs to raman spectrum substrate field, relate to a kind of surface-enhanced Raman with nano gap Spectrum substrate and preparation method thereof.
Background technology
Surface enhanced raman spectroscopy (SERS) technology has high sensitivity, high-resolution, selectivity knowledge Not, can the feature such as quencher fluorescence, good stability, in fields such as Surface Science, spectroscopy, biochemistry detection There is the highest potential using value.
The application foundation of SERS technology is that development has highly sensitive active substrate.Obtain high sensitivity It is critical only that of SERS substrate in substrate, form a large amount of SERS " focus ", the office at " focus " place Territory electromagnetic field is greatly enhanced, so that the sensitivity of SERS substrate is improved.At SERS Manufacture nano gap in substrate and can produce SERS " focus ", strengthen SERS signal.People have made Standby multiple nano gap regulatable nanostructured SERS substrate, such as nanosphere, nano wire and receiving Rice cone waits (Chem.Comm., 2015,51,866-869).For obtaining higher echo signal, need to send out The nano gap SERS substrate of exhibition higher performance.Preparation has the SERS substrate of nano gap to be needed it The carrying out of the size of the metal nanoparticle on surface, pattern and spacing reasonably regulates and controls.At present, some sides Method is used to prepare the SERS substrate of nano gap, such as photoetching technique (Nano Lett., 2013,13, 1359.), template (Nanotechnology., 2013,24,185301), and with etching sacrificial layer Method (Adv.Mater., 2013,25,2678) etc..But, these methods are all subject to certain restrictions, Photolithographicallpatterned is limited by diffraction limit, and the gap that can prepare can only achieve about 10nm, and mould Plate method and the method step with etching sacrificial layer are loaded down with trivial details, preparation method very complicated.Currently, still lack The method that few a kind of fast and convenient preparation has nano gap SERS substrate.Accordingly, it is desirable to provide it is a kind of SERS substrate, this SERS substrate is highly sensitive.
Summary of the invention
First technical problem that the invention solves the problems that is to provide a kind of surface enhanced with nano gap and draws Graceful spectrum substrate.
Second technical problem that the invention solves the problems that is to provide a kind of surface enhanced with nano gap and draws The preparation method of graceful spectrum substrate.
For solving above-mentioned technical problem, the present invention adopts the following technical scheme that
A kind of SERS substrate with nano gap, including the ground floor silver of area load gold nano grain Nano-particle and the second layer silver nano-grain being spin-coated on ground floor silver nano-grain, be wherein supported on the The average diameter of the gold nano grain on one layer of silver nano-grain is 2-6nm.
The average diameter of described ground floor silver nano-grain is 50-200nm;Described second layer silver nano-grain Average diameter be 50-200nm.
In one embodiment, the average diameter of described ground floor silver nano-grain is 50-100nm.
In one embodiment, the average diameter of described second layer silver nano-grain is 50-100nm.
The preparation method of a kind of SERS substrate with nano gap, it comprises the steps:
Prepare ground floor silver nano-grain: use acetone, ethanol and distilled water to carry out ultrasonic to silicon chip successively Clean;Cleaned silicon chip is placed in silver nitrate soak in the mixed solution of Fluohydric acid., forms one layer of silver Nano-particle, by attachment silver nano-grain silicon chip in the atmosphere of noble gas, from room temperature to 160-200 DEG C, being incubated more than 20 minutes, Temperature fall is to room temperature;
Deposition gold nano grain: use ion sputtering method to deposit gold nano grain on silver nano-grain surface, The time of ion sputtering is 3-15 second (s), obtains the ground floor silver nanoparticle of area load gold nano grain Grain;
Prepare silver nano-grain dispersion soln: prepare silver nitrate solution and PVP K30 respectively (PVP-K30) solution, is added to the PVP-K30 solution prepared in silver nitrate solution, molten for mixing Liquid is heated to 155-165 DEG C, cools to room temperature, obtain being dispersed with silver nano-grain after being incubated 15-25 minute Turbid solution, with ethanol solution ultrasonic cleaning repeatedly and centrifugal after, silver nano-grain is dispersed in ethanol In solution, the silver nano-grain dispersion soln obtained;
Spin coating second layer silver nano-grain: revolve on the ground floor silver nano-grain of load gold nano grain Being coated with silver nano-grain dispersion soln, dispersion soln obtains second layer silver nano-grain after drying.
In one embodiment, described silicon chip is monocrystalline silicon piece, monocrystalline silicon piece each ultrasonic cleaning time It it is 10 minutes.
It is 10-100 second (s) that described silicon chip is placed in silver nitrate with the time of immersion in the mixed solution of Fluohydric acid..
Soaking in the mixed solution of silicon chip, the concentration of silver nitrate is 3-10mmol/L, and the concentration of Fluohydric acid. is 4.5-5.0mol/L.In one embodiment, soaking in the mixed solution of silicon chip, the concentration of silver nitrate is 5mmol/L, the concentration of Fluohydric acid. is 4.8mol/L.Due to the Si--H bond reduction to silver ion, Silicon chip surface forms one layer of silver nano-grain.
In one embodiment, in the step preparing ground floor silver nano-grain, silver nanoparticle will be adhered to The silicon chip of granule, in the atmosphere of noble gas, was warmed up to 180 DEG C with 30 minutes from room temperature (about 20 DEG C), After being incubated 20 minutes, Temperature fall is to room temperature.
In another embodiment, in the step preparing ground floor silver nano-grain, attachment silver is received The silicon chip of rice grain, in the atmosphere of noble gas, was warmed up to 180 DEG C with 60 minutes from room temperature (about 20 DEG C), After being incubated 40 minutes, Temperature fall is to room temperature.
The time of the step intermediate ion sputtering of deposition gold nano grain is 5-8 second (s).
Preparing in the step of silver nano-grain dispersion soln, the solvent of preparation silver nitrate solution is ethylene glycol. The concentration of silver nitrate solution is 0.05-0.15mol/L, in one embodiment, and the concentration of silver nitrate solution For 0.1mol/L.
Preparing in the step of silver nano-grain dispersion soln, the solvent of preparation PVP-K30 solution is ethylene glycol. The concentration of PVP-K30 solution is 0.05-0.15mol/L, in one embodiment, and PVP-K30 solution Concentration is 0.1mol/L.
Preparing in the step of silver nano-grain dispersion soln, the PVP-K30 solution prepared is added drop-wise to acutely In silver nitrate solution under stirring.
In one embodiment, prepare in the step of silver nano-grain dispersion soln, PVP-K30 solution Move in autoclave with silver nitrate solution mixed solution and seal, put into and Muffle furnace is heated to 160 DEG C, insulation After 20 minutes, Temperature fall is to room temperature, obtains being dispersed with the turbid solution of silver nano-grain.
In one embodiment, use sol evenning machine that silver nano-grain dispersion soln is spin-coated on load Jenner On the ground floor silver nano-grain of rice grain, i.e. obtain the surface enhanced raman spectroscopy with nano gap Substrate.Sol evenning machine rotating speed is 4000-6000rev/min, it is preferable that sol evenning machine rotating speed is 5000rev/min.
The preparation method of the present invention obtains SERS by introducing gold nano grain in two-layer silver nano-grain Substrate, gold nano grain makes to be formed between two-layer silver nano-grain nano gap, thus SERS is greatly improved The sensitivity of substrate.
Beneficial effects of the present invention is as follows:
Compared with art methods, the invention provides one have nano gap SERS substrate and Preparation method, by load gold nano grain on ground floor silver nano-grain so that ground floor silver nanoparticle The nano gap regulated and controled by size of nanometer gold grain is formed between granule and second layer silver nano-grain, To the SERS substrate with nano gap.
Accompanying drawing explanation
Below in conjunction with the accompanying drawings the detailed description of the invention of the present invention is described in further detail.
Fig. 1 illustrates that the present invention prepares the schematic flow sheet with nano gap SERS substrate.
Fig. 2 illustrates the SEM figure of the silver nano-grain being attached on monocrystalline silicon piece obtained in embodiment 1 Sheet.
Fig. 3 illustrates TEM picture (a) and the area load Jenner sputtering gold nano grain in embodiment 1 TEM picture (b) of the silver nano-grain of rice grain.
Fig. 4 illustrates the SEM picture of the SERS substrate obtained in embodiment 1.
Fig. 5 illustrates the SEM picture of the SERS substrate obtained in comparative example 1.
Fig. 6 illustrates the SERS of the 4-mercaptopyridine molecular solution of gained sample test 1mM in embodiment 1 Spectrogram, ground floor silver nano-grain (a), the ground floor silver nano-grain of area load gold nano grain (b), spin coating second layer silver nano-grain (c) on ground floor silver nano-grain, and prepared SERS Substrate (d).
Fig. 7 illustrates TEM picture (a) and the ground floor silver nanoparticle sputtering gold nano grain in embodiment 2 TEM picture (b) after particle surface sputtering gold nano grain.
Fig. 8 illustrates the TEM picture sputtering gold nano grain in embodiment 3.
Fig. 9 illustrates the SEM picture of the ground floor silver nano-grain obtained in embodiment 4.
Figure 10 illustrates the SEM picture of the ground floor silver nano-grain obtained in embodiment 5.
Detailed description of the invention
In order to be illustrated more clearly that the present invention, below in conjunction with preferred embodiments and drawings, the present invention is done into one The explanation of step.Parts similar in accompanying drawing are indicated with identical reference.Those skilled in the art Should be appreciated that following specifically described content is illustrative and be not restrictive, should not limit with this Protection scope of the present invention.
Embodiment 1: preparation has the SERS substrate of nano gap
Prepare ground floor silver nano-grain: use acetone, ethanol, distilled water that monocrystalline silicon piece is carried out successively Ultrasonic cleaning, each ultrasonic cleaning time is 10 minutes.Cleaned silicon chip is placed in silver nitrate and hydrogen fluorine Soaking 10 seconds in the mixed solution of acid, wherein in mixed solution, the concentration of silver nitrate is 5mmol/L, hydrogen fluorine The concentration of acid is 4.8mol/L.Wherein to the obtained silver nano-grain on silicon chip in pure argon atmosphere Middle being warmed up to 160 DEG C with 30 minutes from room temperature (about 20 DEG C), after being incubated 20 minutes, Temperature fall arrives Room temperature, obtains the ground floor silver nano-grain being attached on monocrystalline silicon piece, SEM picture as in figure 2 it is shown, The average diameter of gained silver nano-grain is 50nm.
Deposition gold nano grain: use ion sputtering method ground floor silver nano-grain area load Jenner Rice grain, sputtering pressure is 10pa, and sputtering current is 10mA, and sputtering time is 5s, the Jenner of sputtering TEM picture such as Fig. 3 a of the ground floor silver nano-grain of rice grain and load gold nano grain and Fig. 3 b institute Showing, the average diameter of gained gold nano grain is 2.5nm.
Prepare silver nano-grain dispersion soln: making spent glycol as solvent, preparation 10ml concentration is respectively The silver nitrate solution of 0.1mol/L and PVP-K30 solution.The PVP-K30 solution prepared is added drop-wise to play In silver nitrate solution under strong stirring, then mixed solution is moved in autoclave and seal, put into horse Not being heated to 160 DEG C in stove, after being incubated 20 minutes, Temperature fall is to room temperature, obtains being dispersed with silver nanoparticle The turbid solution of grain, after ethanol solution ultrasonic cleaning being repeatedly centrifuged, silver nano-grain is dispersed in ethanol In solution, the silver nano-grain dispersion soln obtained.
Spin coating second layer silver nano-grain: use sol evenning machine that silver nano-grain dispersion soln is spin-coated on preparation Sputtering have on the ground floor silver nano-grain of gold nano grain, sol evenning machine rotating speed is 5000rev/min, Dispersion soln obtains second layer silver nano-grain after drying.The average diameter of second layer nano-particle is 100nm.The table of nano gap it is made up of ground floor silver nano-grain, second layer silver nano-grain and gold grain Face strengthens raman spectrum substrate, and SEM picture is as shown in Figure 4.
Comparative example 1: preparation has SERS substrate
Prepare ground floor silver nano-grain: use acetone, ethanol, distilled water that monocrystalline silicon piece is carried out successively Ultrasonic cleaning, each ultrasonic cleaning time is 10 minutes.Cleaned silicon chip is placed in silver nitrate and hydrogen fluorine Soaking 10 seconds in the mixed solution of acid, wherein in mixed solution, the concentration of silver nitrate is 5mmol/L, hydrogen fluorine The concentration of acid is 4.8mol/L.Wherein to the obtained silver nano-grain on silicon chip in pure argon atmosphere In, it was warmed up to 180 DEG C with 30 minutes from room temperature (about 20 DEG C), after being incubated 20 minutes, Temperature fall To room temperature, obtain the ground floor silver nano-grain being attached on monocrystalline silicon piece, SEM picture as in figure 2 it is shown, The average diameter of gained silver nano-grain is 50nm.
Prepare silver nano-grain dispersion soln: making spent glycol as solvent, preparation 10ml concentration is respectively The silver nitrate solution of 0.1mol/L and PVP K30 solution.The PVP K30 solution prepared is added drop-wise to play In silver nitrate solution under strong stirring, then mixed solution is moved in autoclave and seal, put into horse Not being heated to 160 DEG C in stove, after being incubated 20 minutes, Temperature fall is to room temperature, obtains being dispersed with silver nanoparticle The turbid solution of grain, after ethanol solution ultrasonic cleaning being repeatedly centrifuged, silver nano-grain is dispersed in ethanol In solution, the silver nano-grain dispersion soln obtained.
Spin coating second layer silver nano-grain: use sol evenning machine that silver nano-grain dispersion soln is spin-coated on preparation Sputtering have on the ground floor silver nano-grain of gold nano grain, sol evenning machine rotating speed is 5000rev/min, Dispersion soln obtains second layer silver nano-grain after drying.The average diameter of second layer nano-particle is 100nm.Raman spectrum substrate is constituted, as right by ground floor silver nano-grain and second layer silver nano-grain According to, SEM picture is as shown in Figure 5.
The raman spectral signal test of embodiment 2:SERS substrate
SERS substrate raman spectral signal intensity prepared by comparative example 1 and comparative example 1.Specifically Method of testing is as follows:
4-mercaptopyridine molecule is dissolved in ethanol, and wherein the concentration of 4-mercaptopyridine molecule is 1mmol/L. Substrate immersion in ethanol solution 1 hour, after taking-up, of alcohol flushing, then makes after drying up with nitrogen Raman spectrum detects.4-mercaptopyridine can be existed by sulfydryl and suprabasil silver atoms generation chemical reaction Silver surface forms 4-mercaptopyridine monolayer.As shown in Figure 6, experimental result shows gained SERS spectrogram Show: in the detection to the 4-mercaptopyridine molecule of same molar concentration, the SERS substrate of embodiment 1 Higher raman spectral signal intensity is shown than the substrate of comparative example 1.
Embodiment 3: preparation has the SERS substrate of nano gap
The method preparing ground floor silver nano-grain is same as in Example 1.The method of deposition gold nano grain Same as in Example 1, wherein sputtering time is 3s, the gold nano grain of sputtering and sputtering gold nano grain To ground floor silver nano-grain TEM picture as shown in figs. 7 a and 7b, gained gold nano grain flat The most a diameter of 2nm.The method preparing silver nano-grain dispersion soln is same as in Example 1.Spin coating second The embodiment of the method 1 of layer silver nano-grain is identical.
Embodiment 4: preparation has the SERS substrate of nano gap
The method preparing ground floor silver nano-grain is same as in Example 1.The method of deposition gold nano grain Same as in Example 1, wherein sputtering time is 15s, the TEM picture of the gold nano grain of sputtering such as figure Shown in 8, the average diameter of gained gold nano grain is 6nm.The method preparing silver nano-grain dispersion soln Same as in Example 1.The embodiment of the method 1 of spin coating second layer silver nano-grain is identical.
Embodiment 5: preparation has the SERS substrate of nano gap
The method preparing ground floor silver nano-grain is same as in Example 1, and wherein silicon chip is at silver nitrate solution It is 40s with the soak time in the mixed solution of Fluohydric acid., the ground floor silver nano-grain SEM figure of preparation Sheet is as it is shown in figure 9, the average diameter of gained silver nano-grain is 100nm.The side of deposition gold nano grain Method is same as in Example 1.The method preparing silver nano-grain dispersion soln is same as in Example 1.Spin coating The embodiment of the method 1 of second layer silver nano-grain is identical.
Embodiment 6: preparation has the SERS substrate of nano gap
The method preparing ground floor silver nano-grain is same as in Example 1, and wherein silicon chip is at silver nitrate solution It is 100s with the soak time in the mixed solution of Fluohydric acid., the ground floor silver nano-grain SEM figure of preparation As shown in Figure 10, the average diameter of gained silver nano-grain is 200nm to sheet.The side of deposition gold nano grain Method is same as in Example 1.The method preparing silver nano-grain dispersion soln is same as in Example 1.Spin coating The embodiment of the method 1 of second layer silver nano-grain is identical.
The raman spectral signal test of embodiment 7:SERS substrate
The SERS substrate of embodiment 3-6 being detected, detection method is with embodiment 2, and result display is real Execute the raman spectral signal of the SERS substrate of example 3-6 and the raman spectral signal of embodiment 1SERS substrate Essentially identical.
Obviously, the above embodiment of the present invention is only for clearly demonstrating example of the present invention, and It is not the restriction to embodiments of the present invention, for those of ordinary skill in the field, Can also make other changes in different forms on the basis of described above, here cannot be to all Embodiment give exhaustive, every belong to the obvious change that technical scheme extended out Change or change the row still in protection scope of the present invention.

Claims (10)

1. a SERS substrate with nano gap, it is characterised in that include area load gold nano The ground floor silver nano-grain of granule and the second layer silver nanoparticle being spin-coated on ground floor silver nano-grain Grain, the average diameter of the gold nano grain being wherein supported on ground floor silver nano-grain is 2-6nm.
2. SERS substrate as claimed in claim 1, it is characterised in that described ground floor silver nanoparticle The average diameter of grain is 50-200nm, it is preferable that the average diameter of described ground floor silver nano-grain is 50-100nm。
3. SERS substrate as claimed in claim 1, it is characterised in that described second layer silver nanoparticle The average diameter of grain is 50-200nm, it is preferable that the average diameter of described second layer silver nano-grain is 50-100nm。
4. the preparation method of SERS substrate as claimed in claim 1, it is characterised in that include as follows Step:
Prepare ground floor silver nano-grain: use acetone, ethanol and distilled water to carry out ultrasonic to silicon chip successively Clean;Cleaned silicon chip is placed in silver nitrate soak in the mixed solution of Fluohydric acid., forms one layer of silver Nano-particle, by attachment silver nano-grain silicon chip in the atmosphere of noble gas, from room temperature to 160-200 DEG C, being incubated more than 20 minutes, Temperature fall is to room temperature;
Deposition gold nano grain: use ion sputtering method to deposit gold nano grain on silver nano-grain surface, The time of ion sputtering is 3-15 second (s), obtains the ground floor silver nanoparticle of area load gold nano grain Grain;
Prepare silver nano-grain dispersion soln: prepare silver nitrate solution and PVP K30 respectively (PVP-K30) solution, is added to the PVP-K30 solution prepared in silver nitrate solution, molten for mixing Liquid is heated to 155-165 DEG C, cools to room temperature, obtain being dispersed with silver nano-grain after being incubated 15-25 minute Turbid solution, with ethanol solution ultrasonic cleaning repeatedly and centrifugal after, silver nano-grain is dispersed in ethanol In solution, the silver nano-grain dispersion soln obtained;
Spin coating second layer silver nano-grain: revolve on the ground floor silver nano-grain of load gold nano grain Being coated with silver nano-grain dispersion soln, dispersion soln obtains second layer silver nano-grain after drying.
5. preparation method as claimed in claim 4, it is characterised in that described silicon chip be placed in silver nitrate with The time soaked in the mixed solution of Fluohydric acid. is the 10-100 second.
6. preparation method as claimed in claim 4, it is characterised in that soak in the mixed solution of silicon chip, The concentration of silver nitrate is 3-10mmol/L, and the concentration of Fluohydric acid. is 4.5-5.0mol/L, it is preferable that soak In the mixed solution of silicon chip, the concentration of silver nitrate is 5mmol/L, and the concentration of Fluohydric acid. is 4.8mol/L.
7. preparation method as claimed in claim 4, it is characterised in that the step of deposition gold nano grain The time of intermediate ion sputtering is 5-8 second (s).
8. preparation method as claimed in claim 4, it is characterised in that prepare silver nano-grain dispersion molten In the step of liquid, the solvent of preparation silver nitrate solution is ethylene glycol;The concentration of silver nitrate solution is 0.05-0.15mol/L;Preferably, the concentration of silver nitrate solution is 0.1mol/L.
9. preparation method as claimed in claim 4, it is characterised in that prepare silver nano-grain dispersion molten In the step of liquid, the solvent of preparation PVP-K30 solution is ethylene glycol;The concentration of PVP-K30 solution is 0.05-0.15mol/L;Preferably, the concentration of PVP-K30 solution is 0.1mol/L.
10. preparation method as claimed in claim 4, it is characterised in that prepare silver nano-grain dispersion In the step of solution, the PVP-K30 solution prepared is added drop-wise to the silver nitrate solution under the state that is stirred vigorously In.
CN201610262311.4A 2016-04-25 2016-04-25 A kind of Raman spectrum base and preparation method thereof with nano gap Active CN105911044B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610262311.4A CN105911044B (en) 2016-04-25 2016-04-25 A kind of Raman spectrum base and preparation method thereof with nano gap

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610262311.4A CN105911044B (en) 2016-04-25 2016-04-25 A kind of Raman spectrum base and preparation method thereof with nano gap

Publications (2)

Publication Number Publication Date
CN105911044A true CN105911044A (en) 2016-08-31
CN105911044B CN105911044B (en) 2019-02-15

Family

ID=56752860

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610262311.4A Active CN105911044B (en) 2016-04-25 2016-04-25 A kind of Raman spectrum base and preparation method thereof with nano gap

Country Status (1)

Country Link
CN (1) CN105911044B (en)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106872440A (en) * 2017-02-28 2017-06-20 中国科学院合肥物质科学研究院 Portable multi-function soil nutrient tacheometer based on SERS
CN107462565A (en) * 2017-07-21 2017-12-12 山东师范大学 Silver-colored gyrus/graphene/golden film D S ERS substrates and preparation 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
CN108535234A (en) * 2018-01-17 2018-09-14 天津大学 Human body IgG Protein Detection SERS substrates based on modified by silver nanoparticles
CN108562567A (en) * 2018-01-17 2018-09-21 天津大学 Human body IgG Protein Detection SERS substrates based on gold nano particle modification
CN108663387A (en) * 2018-05-16 2018-10-16 国家纳米科学中心 A kind of method that wet etching prepares nano particle TEM sample
CN110702660A (en) * 2019-10-09 2020-01-17 天津工业大学 Novel nano gold film anti-counterfeiting method based on surface enhanced Raman spectroscopy
JP2021512331A (en) * 2017-12-14 2021-05-13 サフトラ フォトニクス,スポロツノスト エス ルチェニム オメゼニム Nano-optical plasmon chips for detecting substances or molecules in the environment, food, and biological systems
CN114018897A (en) * 2021-10-21 2022-02-08 云南省产品质量监督检验研究院 Preparation method of silicon-based SERS substrate based on double-layer silver nanostructure

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020142480A1 (en) * 2001-01-26 2002-10-03 Surromed, Inc. Surface-enhanced spectroscopy-active sandwich nanoparticles
US20070229817A1 (en) * 2003-05-27 2007-10-04 Hong Wang Light scattering device having multi-layer micro structure
CN103575721A (en) * 2013-11-07 2014-02-12 无锡英普林纳米科技有限公司 Multilayer structure surface enhanced Raman scattering base and preparation method thereof
CN103842785A (en) * 2011-05-13 2014-06-04 李�浩 Sers substrates
CN104707992A (en) * 2014-12-01 2015-06-17 中国科学院合肥物质科学研究院 Preparation method for superstructure Au/Ag@Al2O3@Ag nanosphere array and SERS performance of superstructure Au/Ag@Al2O3@Ag nanosphere array

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020142480A1 (en) * 2001-01-26 2002-10-03 Surromed, Inc. Surface-enhanced spectroscopy-active sandwich nanoparticles
US20070229817A1 (en) * 2003-05-27 2007-10-04 Hong Wang Light scattering device having multi-layer micro structure
CN103842785A (en) * 2011-05-13 2014-06-04 李�浩 Sers substrates
CN103575721A (en) * 2013-11-07 2014-02-12 无锡英普林纳米科技有限公司 Multilayer structure surface enhanced Raman scattering base and preparation method thereof
CN104707992A (en) * 2014-12-01 2015-06-17 中国科学院合肥物质科学研究院 Preparation method for superstructure Au/Ag@Al2O3@Ag nanosphere array and SERS performance of superstructure Au/Ag@Al2O3@Ag nanosphere array

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
HAIBIN TANG: "Hexagonally arranged arrays of urchin-like Ag hemispheres decorated with Ag nanoparticles for suface-enhanced Raman scattering substrates", 《NANO RESEARCH》 *
HAIBIN TANG等: "Urchin-like Au-nanoparticals@Ag-nanohemisphere arrays as active SERS-substrate for recognition of PCBs", 《RSC ADVANCED》 *
YUAN ZHAO等: "Highly sensitive surface-enhanced Raman scattering based on multi-dimensional palsmonic coupling in Au-", 《CHEMCOMM》 *
ZHULIN HUANG等: "Improved SERS Performance from Au Nanopillar Arrays by Abridging the pillar Tip Spacing by Ag Sputtering", 《ADVANCED MATERIALS》 *

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106872440A (en) * 2017-02-28 2017-06-20 中国科学院合肥物质科学研究院 Portable multi-function soil nutrient tacheometer based on SERS
CN106872440B (en) * 2017-02-28 2020-11-13 中国科学院合肥物质科学研究院 Portable multifunctional soil nutrient tachymeter based on surface enhanced Raman spectroscopy
CN107462565A (en) * 2017-07-21 2017-12-12 山东师范大学 Silver-colored gyrus/graphene/golden film D S ERS substrates and preparation method
JP2021512331A (en) * 2017-12-14 2021-05-13 サフトラ フォトニクス,スポロツノスト エス ルチェニム オメゼニム Nano-optical plasmon chips for detecting substances or molecules in the environment, food, and biological systems
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
CN108535234A (en) * 2018-01-17 2018-09-14 天津大学 Human body IgG Protein Detection SERS substrates based on modified by silver nanoparticles
CN108562567A (en) * 2018-01-17 2018-09-21 天津大学 Human body IgG Protein Detection SERS substrates based on gold nano particle modification
CN108663387A (en) * 2018-05-16 2018-10-16 国家纳米科学中心 A kind of method that wet etching prepares nano particle TEM sample
CN110702660A (en) * 2019-10-09 2020-01-17 天津工业大学 Novel nano gold film anti-counterfeiting method based on surface enhanced Raman spectroscopy
CN114018897A (en) * 2021-10-21 2022-02-08 云南省产品质量监督检验研究院 Preparation method of silicon-based SERS substrate based on double-layer silver nanostructure

Also Published As

Publication number Publication date
CN105911044B (en) 2019-02-15

Similar Documents

Publication Publication Date Title
CN105911044A (en) Surface enhanced Raman spectrum substrate with nano gap and preparation method thereof
Galopin et al. Silicon nanowires coated with silver nanostructures as ultrasensitive interfaces for surface-enhanced Raman spectroscopy
CN101832933B (en) Method for enhancing Raman spectrum by using shell isolated nano particles
Alessandri Enhancing Raman scattering without plasmons: unprecedented sensitivity achieved by TiO2 shell-based resonators
US9040158B2 (en) Generic approach for synthesizing asymmetric nanoparticles and nanoassemblies
Zhang et al. Graphene oxide-wrapped flower-like sliver particles for surface-enhanced Raman spectroscopy and their applications in polychlorinated biphenyls detection
Wang et al. Effect of silver nanoplates on Raman spectra of p-aminothiophenol assembled on smooth macroscopic gold and silver surface
Aldeanueva‐Potel et al. Spiked Gold Beads as Substrates for Single‐Particle SERS
Li et al. Cyclic electroplating and stripping of silver on Au@ SiO 2 core/shell nanoparticles for sensitive and recyclable substrate of surface-enhanced Raman scattering
Yi et al. Facile preparation of Au/Ag bimetallic hollow nanospheres and its application in surface-enhanced Raman scattering
Wang et al. Highly ordered Au-Ag alloy arrays with tunable morphologies for surface enhanced Raman spectroscopy
CN104692827B (en) A kind of Ag nanometers of preparation method of ball array of Ag SiO2
Osorio-Román et al. Plasmon enhanced fluorescence with aggregated shell-isolated nanoparticles
CN103990812A (en) Method for preparing surface enhanced Raman substrate
Kim et al. Co-reduced Ag/Pd bimetallic nanoparticles: Surface enrichment of Pd revealed by Raman spectroscopy
CN102253027A (en) Surface-enhanced Raman scattering active substrate based on star-shaped gold nanoparticles and preparation method thereof
CN105866098B (en) A kind of Cu2Compound micro particles surface-enhanced Raman scattering activity substrate of O-Au and preparation method thereof
CN108333168A (en) A kind of enhancing Raman detection method using satellite structure
Xue et al. A facile method to prepare a series of SiO2@ Au core/shell structured nanoparticles
Long et al. Preparation of stable core–shell dye adsorbent Ag-coated silica nanospheres as a highly active surfaced-enhanced Raman scattering substrate for detection of Rhodamine 6G
CN108318473A (en) A kind of surface-enhanced Raman scattering activity substrate and its preparation method and application
CN104568895B (en) surface-enhanced Raman scattering probe and its manufacturing method
Wei et al. Electrostatic assembly of CTAB-capped silver nanoparticles along predefined λ-DNA template
Zhao et al. Surface-enhanced Raman scattering-active plasmonic metal nanoparticle-persistent luminescence material composite films for multiple illegal dye detection
Zhang et al. Layer-by-layer assembled gold nanoparticle films on amine-terminated substrates

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant