CN106018378A - Method for preparing surface-enhanced Raman scattering active substrate by utilizing sintering technology - Google Patents
Method for preparing surface-enhanced Raman scattering active substrate by utilizing sintering technology Download PDFInfo
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- CN106018378A CN106018378A CN201610309855.1A CN201610309855A CN106018378A CN 106018378 A CN106018378 A CN 106018378A CN 201610309855 A CN201610309855 A CN 201610309855A CN 106018378 A CN106018378 A CN 106018378A
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- raman scattering
- enhanced raman
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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
Abstract
The invention discloses a method for preparing a surface-enhanced Raman scattering active substrate by utilizing a sintering technology. The method includes the following steps that 1, a substrate is coated with a layer of conductive silver ink; 2, the infiltrated substrate is sintered at the temperature of 160-230 degrees for 30-50 minutes, and then natural cooling is performed to reach room temperature, namely the surface-enhanced Raman scattering active substrate can be obtained. Compared with the prior art, the method has the following advantages that the method comprehensively utilizes the sintering technology and a surface microstructure of a substrate material to prepare nano silver, a silver-plated layer with a specific micro-nano structure is prepared on the surface of the substrate, especially filter paper, and the SERS active substrate stable and reliable in performance is obtained and can be used for trace detection of nano materials on the aspects of science, biology, environmentology and the like. Preparation is performed by utilizing the sintering technology, the process is simple, complex chemical equipment is not needed, the production costs are low, and the output rate is high.
Description
Technical field
The present invention relates to a kind of method utilizing sintering technology to prepare surface-enhanced Raman scattering activity substrate.
Background technology
Surface enhanced raman spectroscopy (Surface-Enhanced Raman Scattering, it is called for short SERS) it is the phenomenon that absorption molecule on metallic nanostructured surface is excited by the plasma resonance that metal surface occurs and the Raman scattering intensities that causes strengthens, since Fleischmann observes surface enhanced raman spectroscopy first in coarse silver electrode surface, the mechanism of SERS and applied research have obtained a large amount of concern.As a kind of high efficiency technical detecting Raman signal, SERS has a wide range of applications in the field such as chemical analysis, biomedicine, environment and safety.Research shows, the enhancer of SERS signal is typically up to 106 - 1011, mainly affected by characterization of adsorption between roughness of the substrate and substrate and molecular detection.The preparation of SERS active-substrate is always of paramount importance link in this technology.Preparing at present the method for SERS substrate, mainly to have metal nanoparticle sol solution, metal nanoparticle self assembly, nanolithographic and template to prepare etc. several.But these methods are more complicated, take time and effort, and output is low.
In actual applications, it is desirable to base material can not only provide stable Raman enhancing signal, and low cost, easily preparation and convenient use.Filter paper is cheap as one, flexible and environment-friendly materials, is widely used in analytical chemistry and the field such as biomedical.In recent years, it is developed multiple method and is prepared for papery SERS active-substrate material, the method such as including inkjet technology, infiltration, silk screen printing and vapour deposition, the Chen Yuanyuan of such as Hunan University develops filter paper SERS immuno analytical method [Chen Yuanyuan in its Master's thesis, SERS immuno analytical method research on paper, Master's thesis, 2012, Hunan University].When methods such as using inkjet technology, infiltration and silk screen printing prepares papery SERS active-substrate, the suspension of nano metal particles the most all can be used.But, the suspension of nano metal particles is typically not easy to preserve, and standing time, slightly length was susceptible to agglomeration, affected quality.And process that laboratory prepares nano metal particles is more complicated.
China Patent Publication No. is that the Patent Publication of CN102321402A discloses a kind of high agranular type transparent electrical ink and preparation method thereof.This disclosure of the invention is a kind of can low-temperature sintering, the agranular type electrically conducting transparent ink and preparation method thereof of good stability.Agranular type conductive ink is mainly made up of with organic silver salts organic amine, organic amine and other solvent after such as ethanol is mixed homogeneously, need to be added appropriate organic silver salts, can be prepared by conductive ink after it is completely dissolved dispersion during preparation.This conductive ink can form pattern or wet film by printing or coating method, and organic silver part therein can be reduced to Argent grain in heat treatment process subsequently and form conductive pattern or conductive film.The preparation method technique that this invention proposes is simple, and reaction condition is gentle, and the response time is short, and preparation cost is low.But this patent of invention is only applied to printing technology prepares the fields such as micro-nano circuit.
China Patent Publication No. is patent of invention disclosure SERS active-substrate disclosing a kind of flexible erasable of CN104849258A and preparation method thereof.The SERS substrate that this invention proposes, including flexible support layers and metal nano film attached thereto.Its flexible support layers has the flexible material of loose structure, including the organic film material such as polyacrylamide, polyvinyl alcohol.The metal nano film being coated in flexible support layers mainly includes gold, silver, copper and mickel, needs through surface moditied processing.Surface enhanced Raman substrate prepared by this invention can realize the organic chemicals to solid material surface, the especially quick detection to 2，4，6-trinitrotoluene.This invention needs the organic film using the preparation of cryodesiccated method to have loose structure, simultaneously need to certain chemical technology prepares nano metal solution, relative complex.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of method utilizing sintering technology to prepare surface-enhanced Raman scattering activity substrate.
The present invention is achieved by the following technical solutions:
A kind of method utilizing sintering technology to prepare surface-enhanced Raman scattering activity substrate, comprises the steps:
(1) on matrix, one layer of conductive silver ink is coated；
(2) matrix after infiltration is sintered 30-50 minute at a temperature of 160-230 °, then naturally cool to room temperature, can be prepared by surface-enhanced Raman scattering activity substrate.
As the preferred implementation of said method, described matrix is filter paper, have the paper of surface roughness, through surface micro-nano process silica-based in one of which.
Preferred implementation as said method, described step (2) is particularly as follows: hang in the temperature control electric oven after preheating by the matrix after infiltration, sinter 30-50 minute at a temperature of 160-230 °, it is then shut off temperature control electric oven, naturally cool to room temperature, can be prepared by surface-enhanced Raman scattering activity substrate.
As the preferred implementation of said method, in described step (2), the matrix after infiltration is sintered 30 minutes at a temperature of 160 °.
As the preferred implementation of said method, described step (1) is carried out as follows: use dropper sampling method to coat conductive silver ink on the subregion of matrix.
As the preferred implementation of said method, described step (1) is carried out as follows: using soaking method to be immersed by matrix in conductive silver ink and stands 1-5 minute, being covered with conductive silver ink water so that being all coated with on full wafer matrix.
As the preferred implementation of said method, described matrix is quantitative filter paper the most at a slow speed.
The present invention has the advantage that compared to existing technology
A kind of method utilizing sintering technology to prepare surface-enhanced Raman scattering activity substrate that the present invention provides, the Surface Microstructure of comprehensive utilization sintering technology and matrix material prepares the advantage of nanometer silver, there is the silver coating of specific micro-nano structure in the preparation of matrix especially its surface, obtain SERS active-substrate stable and reliable for performance, can be used for the trace detection of the aspects such as nanometer material science, biology and environmentology.And utilizing sintering technology to prepare, technique is simple, it is not necessary to complicated chemical device, and production cost is low, and output capacity is high；It is suitable on the multiple material surface with micro-nano structure preparing SERS active-substrate simultaneously, has wide range of applications.
Accompanying drawing explanation
Fig. 1 is a scanning electron microscope (SEM) photograph of the SERS active-substrate in the embodiment of the present invention one.
Fig. 2 is another scanning electron microscope (SEM) photograph of the SERS active-substrate in the embodiment of the present invention one.
Fig. 3 is in the SERS active-substrate in the embodiment of the present invention one, and concentration is the SERS spectra of the R6G transmitting of 5pM.
Fig. 4 is the graph of a relation between the SERS intensity in the embodiment of the present invention one and R6G solution concentration.
Detailed description of the invention
Elaborating embodiments of the invention below, the present embodiment is implemented under premised on technical solution of the present invention, gives detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment one
Present embodiment discloses a kind of method utilizing sintering technology to prepare surface-enhanced Raman scattering activity substrate, comprise the steps:
(1) on matrix, one layer of conductive silver ink is coated, the conductive silver ink used in the present embodiment is the SC-100 conductive silver ink that Kunshan Hisense Electronics Co., Ltd. produces, what matrix was selected is quantitative filter paper the most at a slow speed, except of course that beyond quantitative filter paper the most at a slow speed, can also select other have the paper of surface roughness or through surface micro-nano process silica-based, coating method is: using soaking method to be immersed by matrix in conductive silver ink and stands 1 minute, being covered with conductive silver ink water so that being all coated with on full wafer matrix；
(2) matrix after infiltration is hung in the temperature control electric oven after preheating, sinter 30 minutes at a temperature of 160, be then shut off temperature control electric oven, naturally cool to room temperature, can be prepared by surface-enhanced Raman scattering activity substrate.
Being scanned analyzing to the SERS active-substrate surface that the present embodiment prepares with scanning electron microscope (SEM), the scanning electron microscope (SEM) photograph of the SERS active-substrate obtained is as shown in Figure 1 and Figure 2.From Fig. 1, Fig. 2 it can be seen that silver coating surface has substantial amounts of micro-nano microstructure.The coarse surface texture of this micro-nano is the essential condition producing SERS signal.
Rhodamine 6G (R6G) is dissolved in ethanol solution, is prepared as certain density R6G solution.Liquid getting device is used to be dropped in above-mentioned prepared SERS active-substrate by the 10 microlitre R6G solution that concentration is 5pM.Then Raman based on the iHR550 spectrogrph test system built according to laboratory, under the laser excitation that laser light wavelength is 532 nanometers, measures the SERS spectra that on SERS active-substrate surface, R6G launches, and the SERS spectra recorded is as shown in Figure 3.Change the concentration of R6G solution further, test the corresponding relation of raman spectrum strength and R6G solution concentration, as shown in Figure 4.Test result shows, the detectable limit of SERS active-substrate prepared by this embodiment up to limting concentration be 10-12M。
Embodiment two
Present embodiment discloses a kind of method utilizing sintering technology to prepare surface-enhanced Raman scattering activity substrate, comprise the steps:
(1) on matrix, one layer of conductive silver ink is coated, described matrix is filter paper, have the paper of surface roughness, through surface micro-nano process silica-based in one of which, coating method is: coat conductive silver ink on the subregion of matrix by dropper sampling method；
(2) matrix after infiltration is hung in the temperature control electric oven after preheating, sinter 40 minutes at a temperature of 230 °, be then shut off temperature control electric oven, naturally cool to room temperature, can be prepared by surface-enhanced Raman scattering activity substrate.
Embodiment three
Present embodiment discloses a kind of method utilizing sintering technology to prepare surface-enhanced Raman scattering activity substrate, comprise the steps:
(1) on matrix, one layer of conductive silver ink is coated, described matrix is filter paper, have the paper of surface roughness, through surface micro-nano process silica-based in one of which, coating method is: using soaking method to be immersed by matrix in conductive silver ink and stands 5 minutes, being covered with conductive silver ink water so that being all coated with on full wafer matrix；
(2) matrix after infiltration is hung in the temperature control electric oven after preheating, sinter 50 minutes at a temperature of 190 °, be then shut off temperature control electric oven, naturally cool to room temperature, can be prepared by surface-enhanced Raman scattering activity substrate.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all any amendment, equivalent and improvement etc. made within the spirit and principles in the present invention, should be included within the scope of the present invention.
Claims (7)
1. one kind utilizes the method that sintering technology prepares surface-enhanced Raman scattering activity substrate, it is characterised in that comprise the steps:
(1) on matrix, one layer of conductive silver ink is coated；
(2) matrix after infiltration is sintered 30-50 minute at a temperature of 160-230 °, then naturally cool to room temperature, can be prepared by surface-enhanced Raman scattering activity substrate.
A kind of method utilizing sintering technology to prepare surface-enhanced Raman scattering activity substrate, it is characterised in that described matrix is filter paper, have the paper of surface roughness, through surface micro-nano process silica-based in one of which.
A kind of method utilizing sintering technology to prepare surface-enhanced Raman scattering activity substrate, it is characterized in that, described step (2) is particularly as follows: hang in the temperature control electric oven after preheating by the matrix after infiltration, sinter 30-50 minute at a temperature of 160-230 °, it is then shut off temperature control electric oven, naturally cool to room temperature, can be prepared by surface-enhanced Raman scattering activity substrate.
A kind of method utilizing sintering technology to prepare surface-enhanced Raman scattering activity substrate, it is characterised in that in described step (2), sinters the matrix after infiltration 30 minutes at a temperature of 160 °.
A kind of method utilizing sintering technology to prepare surface-enhanced Raman scattering activity substrate, it is characterised in that described step (1) is carried out as follows: use dropper sampling method to coat conductive silver ink on the subregion of matrix.
A kind of method utilizing sintering technology to prepare surface-enhanced Raman scattering activity substrate, it is characterized in that, described step (1) is carried out as follows: using soaking method to be immersed by matrix in conductive silver ink and stands 1-5 minute, being covered with conductive silver ink water so that being all coated with on full wafer matrix.
A kind of method utilizing sintering technology to prepare surface-enhanced Raman scattering activity substrate, it is characterised in that described matrix is quantitative filter paper the most at a slow speed.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110441284A (en) * | 2019-07-23 | 2019-11-12 | 海南大学 | The preparation method and products obtained therefrom of a kind of Surface enhanced Raman scattering chip can be used for trace detection and application |
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| CN102321402A (en) * | 2011-08-16 | 2012-01-18 | 天津大学 | Agranular transparent conductive ink and its preparation method |
| US20120300203A1 (en) * | 2011-05-27 | 2012-11-29 | Som Tyagi | Flexible sers substrates with filtering capabilities |
| CN103048304A (en) * | 2012-12-07 | 2013-04-17 | 江苏大学 | Preparation method of recyclable surface-enhanced Raman-spectrum active substrate |
| CN103115912A (en) * | 2013-01-23 | 2013-05-22 | 中国科学院合肥物质科学研究院 | Surface enhanced raman spectrum printing test paper for field test and preparation method thereof |
| CN102408094B (en) * | 2011-11-11 | 2014-04-09 | 华东理工大学 | Preparation method for highly repetitive surface enhanced Raman spectrum (SERS) active substrate |
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- 2016-05-11 CN CN201610309855.1A patent/CN106018378A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120300203A1 (en) * | 2011-05-27 | 2012-11-29 | Som Tyagi | Flexible sers substrates with filtering capabilities |
| CN102321402A (en) * | 2011-08-16 | 2012-01-18 | 天津大学 | Agranular transparent conductive ink and its preparation method |
| CN102408094B (en) * | 2011-11-11 | 2014-04-09 | 华东理工大学 | Preparation method for highly repetitive surface enhanced Raman spectrum (SERS) active substrate |
| CN103048304A (en) * | 2012-12-07 | 2013-04-17 | 江苏大学 | Preparation method of recyclable surface-enhanced Raman-spectrum active substrate |
| CN103115912A (en) * | 2013-01-23 | 2013-05-22 | 中国科学院合肥物质科学研究院 | Surface enhanced raman spectrum printing test paper for field test and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110441284A (en) * | 2019-07-23 | 2019-11-12 | 海南大学 | The preparation method and products obtained therefrom of a kind of Surface enhanced Raman scattering chip can be used for trace detection and application |
| CN110441284B (en) * | 2019-07-23 | 2022-02-15 | 海南大学 | Preparation method of surface-enhanced Raman scattering chip for trace detection, obtained product and application |
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