CN103103608A - Film formed by silver nanosheets and preparation method and application of film - Google Patents

Film formed by silver nanosheets and preparation method and application of film Download PDF

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CN103103608A
CN103103608A CN2011103637484A CN201110363748A CN103103608A CN 103103608 A CN103103608 A CN 103103608A CN 2011103637484 A CN2011103637484 A CN 2011103637484A CN 201110363748 A CN201110363748 A CN 201110363748A CN 103103608 A CN103103608 A CN 103103608A
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film
silver
solution
nano silver
concentration
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朱储红
孟国文
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Hefei Institutes of Physical Science of CAS
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Hefei Institutes of Physical Science of CAS
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Abstract

The invention discloses a film formed by silver nanosheets and a preparation method and application of the film. The film is 200-500nm in thickness and is formed by covering a nanometer flat branch cluster on a conductive substrate, wherein a gap between every two nanometer flat branches in the cluster is 1-15nm; and the film is formed by connecting nanosheets with arc-shaped edges in series, wherein the thickness of each nanosheet is 10-50nm, width is 30-300nm and length is 90-150nm. The preparation method comprises the following steps of: mixing and stirring a silver nitrate water solution, a citric acid water solution and water to obtain a mixed solution, and injecting a sodium borohydride water solution into the mixed solution and stirring and aging to obtain a silver seed crystal solution; then coating the silver seed crystal solution onto the conductive substrate and then airing the conductive substrate; and then putting the conductive substrate which is coated with silver seed crystals and is used as a cathode in electrolyte consisting of the silver nitrate water solution and the citric acid water solution, and carrying out electro-deposition for 5-120 minutes under the constant current of which the current density is 0.1-1mA/cm<2> to obtain the target product. The film disclosed by the invention can be used as an SERS (Surface Enhanced Raman Scattering) active substrate to rapidly detect the content of trace rhodamine 6G or tetrachlorobiphenyl-77 attached onto the SERS active substrate.

Description

Film that Nano silver piece forms and its production and use
Technical field
The present invention relates to a kind of film and preparation method and purposes, film that especially a kind of Nano silver piece forms and its production and use.
Background technology
Have and the visibly different special performance of similar block materials based on nano level argent, people are for exploring and expand its range of application, made unremitting effort, as open day be a kind of " device of observing nano material grown by electrochemistry method and the control method thereof " mentioned in the applicant's a Chinese invention patent application Publication Specification CN 101597785A on December 9th, 2009.A kind of film and its preparation method that uses the Nano silver piece composition of said apparatus acquisition described in this specification sheets, film wherein is comprised of the Nano silver piece that is covered with on the tin indium oxide conductive substrates, the preparation method adopts electrochemical process, its electrolytic solution of selecting is that silver electrolyte, anode are that graphite flake, cathode substrate are the indium oxide tin glass that scribbles the silver crystalline substance, and the density of the constant current during electrochemical reaction is 6 μ A/cm 2, obtain final product.But, no matter be final product, or its preparation method, all exist the shortcoming part, at first, disclosed final product, Nano silver piece does not especially wherein have concrete shape characteristic and size, only know final product by the film that Nano silver piece forms, do not know whether final product has surface enhanced Raman scattering (SERS) effect; Its two, the preparation method is the composition of electrolytic solution openly, causes people will in fact impose the acquisition final product.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of film of Nano silver piece composition of the SERS of having activity for overcoming shortcoming part of the prior art.
The thin film technology method of another technical problem that the present invention will solve for providing a kind of above-mentioned Nano silver piece to form.
The present invention will solve also has a technical problem to be the purposes of the film that a kind of above-mentioned Nano silver piece is provided forms.
For solving technical problem of the present invention, the technical scheme that adopts is: the film that Nano silver piece forms comprises conductive substrates, particularly,
Be covered with the film of nanometer bar bunch composition on described conductive substrates, the thickness of described film is 200～500nm;
Gap between nanometer bar in described nanometer bar bunch is 1～15nm;
The nanometer sheet serial connection that described nanometer bar is arc by the edge consists of;
Thick 10～the 50nm of being of the sheet of described nanometer sheet, the wide 30～300nm of being of sheet, length of a film are 90～150nm, and it is the silver of face-centered cubic phase;
The described face-centered cubic plate plane of the nanometer sheet of silver formation mutually is parallel to face-centered cubic (111) face of silver mutually.
Be close-packed arrays between the further improvement of the film that forms as Nano silver piece, described nanometer bar bunch; Described conductive substrates is conductive glass, or conductive rubber, or metal.
For solving another technical problem of the present invention, another technical scheme that adopts is: the thin film technology method that above-mentioned Nano silver piece forms comprises electrodip process, and particularly completing steps is as follows:
Step 1, be first that the silver nitrate aqueous solution of 8～12g/L, aqueous citric acid solution and the water that concentration is 6～8g/L are 1.8～2.2: 0.9～1.1 according to volume ratio with concentration: 96～100 ratio stirs 2min at least after mixing, obtain mixed solution, with concentration be again the sodium borohydride aqueous solution of 0.7～0.9g/L be injected into stir at least 10min in mixed solution after, aging 20h at least under room temperature, obtain the young brilliant solution of silver, wherein, silver nitrate aqueous solution and the volume ratio between sodium borohydride aqueous solution in the young brilliant solution of silver is 0.9～1.1: 0.9～1.1;
Step 2, after first being coated on the young brilliant solution of silver on conductive substrates, be placed in the moisture that evaporates solution under 35～45 ℃, obtain being covered with on it young brilliant conductive substrates of silver, being placed in electrolytic solution as negative electrode, graphite flake as anode with being covered with the young brilliant conductive substrates of silver on it again, is 0.1～1mA/cm in current density 2Continuous current under galvanic deposit 5～120min, wherein, electrolytic solution is that concentration is that silver nitrate aqueous solution and the concentration of 1～16g/L is the mixed solution of the aqueous citric acid solution of 4～72g/L, makes the film that Nano silver piece forms.
As the thin film technology further improvements in methods that Nano silver piece forms, described water is deionized water, or distilled water; Describedly be applied to spin coating, or spraying, or dipping; Described conductive substrates is conductive glass, or conductive rubber, or metal; The described film that the Nano silver piece that makes is formed re-uses argon gas after with washed with de-ionized water and dries up.
For solving the technical problem that also has of the present invention, the technical scheme that also has that adopts is: the purposes of the film that above-mentioned Nano silver piece forms is,
The film that Nano silver piece is formed is as the active substrate of surface enhanced Raman scattering, the rhodamine 6G (R6G) that uses the burnt Raman spectrometer of copolymerization to measure to adhere on it or the content of tetrachloro biphenyl-77 (PCB-77).
The further improvement of the purposes of the film that forms as Nano silver piece, the optical maser wavelength of the burnt Raman spectrometer of described copolymerization is that 532nm, output rating are 9～13mW, be 1～60s the integral time during measurement.
Beneficial effect with respect to prior art is, one, use respectively scanning electron microscope, transmission electron microscope, X-ray diffractometer and ultraviolet-visible-near infrared spectrometer to characterize to the target product that makes, by characterization result as can be known, target product is the film that is overlying on substrate; Wherein, the thickness of film is 200～500nm, and it bunch is comprised of compact arranged nanometer bar each other.Gap between nanometer bar in nanometer bar bunch is 1～15nm, and the nanometer sheet serial connection that the nanometer bar is arc by the edge consists of.Thick 10～the 50nm of being of the sheet of nanometer sheet, the wide 30～300nm of being of sheet, length of a film are 90～150nm, and it is the silver of face-centered cubic phase, and the face-centered cubic plate plane of the nanometer sheet of silver formation mutually is parallel to face-centered cubic (111) face of silver mutually.Substrate is conductive substrates, and it is conductive glass, or conductive rubber, or metal.Target product is that the 381nm place has a plasma resonance absorption peak at wavelength, and is that the 532nm place also has stronger photoabsorption at wavelength, has demonstrated that when using excitation wavelength as 532nm, it has the performance of stronger SERS active substrate.Its two, the target product that contains trace rhodamine 6G or tetrachloro biphenyl-77 is characterized it with the burnt Raman spectrometer of copolymerization, by its result as can be known, when the concentration of rhodamine 6G is low to moderate 10 -15The concentration of mol/L or tetrachloro biphenyl-77 is low to moderate 10 -6During mol/L, target product still can show it effectively.When sign contained the target product of trace rhodamine 6G, exciting light wavelength was that 532nm, power are that 1mW, integral time are 1s.When sign contained the target product of trace tetrachloro biphenyl-77, exciting light wavelength was that 532nm, power are that 1mW, integral time are 60s.They are three years old, preparation method's science, effective, both prepared the film of the Nano silver piece composition with stronger SERS active substrate structure, after making again the target product that makes focus on together the Raman spectrometer cooperation, possessed the function of environment toxic pollutant rhodamine 6G and tetrachloro biphenyl-77 being carried out quick trace detection, the advantage that cost of manufacture is cheap, be easy to suitability for industrialized production has also been arranged.
As the further embodiment of beneficial effect, the one, be preferably close-packed arrays between nanometer bar bunch, be beneficial to the higher SERS of acquisition active.The 2nd, conductive substrates is preferably conductive glass, or conductive rubber, or metal, except conductive substrates is had larger choice, preparation technology is more easily implemented and flexibly.The 3rd, water is preferably deionized water, or distilled water, has avoided the introducing of impurity, has guaranteed the quality of mixed solution.The 4th, apply and be preferably spin coating, or spraying, or dipping, can not only guarantee the young brilliant quality of silver, also easy to implement.The 5th, the film that the Nano silver piece that makes is formed preferably dries up with re-using argon gas after washed with de-ionized water, has guaranteed purity and the quality of target product.
Description of drawings
Below in conjunction with accompanying drawing, optimal way of the present invention is described in further detail.
Fig. 1 uses respectively one of result that scanning electron microscope (SEM) and transmission electron microscope (TEM) characterize to the target product that makes.Wherein, Fig. 1 a, Fig. 1 b, Fig. 1 c and Fig. 1 d are the SEM photo, and Fig. 1 b wherein is the enlarged photograph of rectangular area in Fig. 1 a, and Fig. 1 c is the enlarged photograph of rectangular area in Fig. 1 b, Fig. 1 d is the SEM photo in target product cross section, can be known pattern and the size of target product by these SEM photos; Fig. 1 e and Fig. 1 f are the TEM photo, and the illustration in Fig. 1 e lower right corner is the selected area electron diffraction pattern in its rectangular area, and Fig. 1 f is the high-resolution TEM photo of Fig. 1 e.
Fig. 2 uses respectively one of result that X-ray diffraction (XRD) instrument and ultraviolet-visible-near infrared spectrometer characterize to the target product that makes.Wherein, Fig. 2 a is the XRD spectra of target product, the curve of spectrogram middle and upper part is that the curve of bottom is the XRD figure spectrum of tin indium oxide (ITO) glass as the tin indium oxide (ITO) of one of conductive glass of conductive substrates the XRD figure spectrum that is covered with the film of nanometer bar bunch composition on glass; Fig. 2 b is the ultraviolet-visible-near-infrared absorption spectrum of target product.
Fig. 3 is one of result that respectively rhodamine 6G and the burnt Raman spectrometer of target product use copolymerization that contains the trace rhodamine 6G is characterized.Wherein, the curve I in Fig. 3 a is that standard Raman line, curve II and the curve III of R6G film are that the concentration that target product contains R6G is respectively 10 -11Mol/L and 10 -15SERS spectral line during mol/L, the time of integration is 3s; Fig. 3 b is is 10 from the concentration that contains R6G -6The SERS spectral line of choosing at random 6 points on the target product of mol/L and measuring, the time of integration is 2s.
Fig. 4 is one of result that respectively tetrachloro biphenyl-77 and the burnt Raman spectrometer of target product use copolymerization that contains trace tetrachloro biphenyl-77 is characterized.Curve 1 in spectrogram is respectively 10 for the standard Raman line of PCB-77 powder, curve 2～4 for the concentration that target product contains PCB-77 -4Mol/L, 10 -6Mol/L and 3 * 10 -7SERS spectral line during mol/L, the time of integration is 60s.
Embodiment
At first buy from market or make with ordinary method:
Silver nitrate aqueous solution; Aqueous citric acid solution; Deionized water and distilled water as water; Sodium borohydride aqueous solution; Conductive glass, conductive rubber and metal as conductive substrates.
Then,
Embodiment 1
The concrete steps of preparation are:
Step 1 is first that the silver nitrate aqueous solution of 8g/L, aqueous citric acid solution and the water that concentration is 6g/L are the rear 2min of stirring of ratio mixing of 1.8: 1.1: 96 according to volume ratio with concentration; Wherein, water is deionized water, obtains mixed solution.With concentration be again the sodium borohydride aqueous solution of 0.7g/L be injected into stir 10min in mixed solution after, aging 20h under room temperature obtains the young brilliant solution of silver; Wherein, silver nitrate aqueous solution and the volume ratio between sodium borohydride aqueous solution in the young brilliant solution of silver is 1.1: 0.9.
Step 2 after first being coated on the young brilliant solution of silver on conductive substrates, is placed in the moisture that evaporates solution under 35 ℃; Wherein, be applied to spin coating (or spraying, or dipping), conductive substrates is conductive glass, obtains being covered with on it young brilliant conductive substrates of silver.Being placed in electrolytic solution as negative electrode, graphite flake as anode with being covered with the young brilliant conductive substrates of silver on it again, is 0.1mA/cm in current density 2Continuous current under galvanic deposit 120min; Wherein, electrolytic solution is that concentration is that silver nitrate aqueous solution and the concentration of 1g/L is the mixed solution of the aqueous citric acid solution of 72g/L, make be similar to shown in Figure 1, and the film that forms of the Nano silver piece as shown in the curve in Fig. 2.
Embodiment 2
The concrete steps of preparation are:
Step 1 is first that the silver nitrate aqueous solution of 9g/L, aqueous citric acid solution and the water that concentration is 6.5g/L are the rear 3min of stirring of ratio mixing of 1.9: 1.05: 97 according to volume ratio with concentration; Wherein, water is deionized water, obtains mixed solution.With concentration be again the sodium borohydride aqueous solution of 0.75g/L be injected into stir 11min in mixed solution after, aging 20.5h under room temperature obtains the young brilliant solution of silver; Wherein, silver nitrate aqueous solution and the volume ratio between sodium borohydride aqueous solution in the young brilliant solution of silver is 1.05: 0.95.
Step 2 after first being coated on the young brilliant solution of silver on conductive substrates, is placed in the moisture that evaporates solution under 38 ℃; Wherein, be applied to spin coating (or spraying, or dipping), conductive substrates is conductive glass, obtains being covered with on it young brilliant conductive substrates of silver.Being placed in electrolytic solution as negative electrode, graphite flake as anode with being covered with the young brilliant conductive substrates of silver on it again, is 0.3mA/cm in current density 2Continuous current under galvanic deposit 65min; Wherein, electrolytic solution is that concentration is that silver nitrate aqueous solution and the concentration of 4g/L is the mixed solution of the aqueous citric acid solution of 55g/L, make be similar to shown in Figure 1, and the film that forms of the Nano silver piece as shown in the curve in Fig. 2.
Embodiment 3
The concrete steps of preparation are:
Step 1 is first that the silver nitrate aqueous solution of 10g/L, aqueous citric acid solution and the water that concentration is 7g/L are the rear 4min of stirring of ratio mixing of 2: 1: 98 according to volume ratio with concentration; Wherein, water is deionized water, obtains mixed solution.With concentration be again the sodium borohydride aqueous solution of 0.8g/L be injected into stir 12min in mixed solution after, aging 21h under room temperature obtains the young brilliant solution of silver; Wherein, silver nitrate aqueous solution and the volume ratio between sodium borohydride aqueous solution in the young brilliant solution of silver is 1: 1.
Step 2 after first being coated on the young brilliant solution of silver on conductive substrates, is placed in the moisture that evaporates solution under 40 ℃; Wherein, be applied to spin coating (or spraying, or dipping), conductive substrates is conductive glass, obtains being covered with on it young brilliant conductive substrates of silver.Being placed in electrolytic solution as negative electrode, graphite flake as anode with being covered with the young brilliant conductive substrates of silver on it again, is 0.6mA/cm in current density 2Continuous current under galvanic deposit 60min; Wherein, electrolytic solution is that concentration is that silver nitrate aqueous solution and the concentration of 8g/L is the mixed solution of the aqueous citric acid solution of 38g/L, make as shown in Figure 1, and the film that forms of the Nano silver piece as shown in the curve in Fig. 2.
Embodiment 4
The concrete steps of preparation are:
Step 1 is first that the silver nitrate aqueous solution of 11g/L, aqueous citric acid solution and the water that concentration is 7.5g/L are the rear 5min of stirring of ratio mixing of 2.1: 0.95: 99 according to volume ratio with concentration; Wherein, water is deionized water, obtains mixed solution.With concentration be again the sodium borohydride aqueous solution of 0.85g/L be injected into stir 13min in mixed solution after, aging 21.5h under room temperature obtains the young brilliant solution of silver; Wherein, silver nitrate aqueous solution and the volume ratio between sodium borohydride aqueous solution in the young brilliant solution of silver is 0.95: 1.05.
Step 2 after first being coated on the young brilliant solution of silver on conductive substrates, is placed in the moisture that evaporates solution under 43 ℃; Wherein, be applied to spin coating (or spraying, or dipping), conductive substrates is conductive glass, obtains being covered with on it young brilliant conductive substrates of silver.Being placed in electrolytic solution as negative electrode, graphite flake as anode with being covered with the young brilliant conductive substrates of silver on it again, is 0.8mA/cm in current density 2Continuous current under galvanic deposit 35min; Wherein, electrolytic solution is that concentration is that silver nitrate aqueous solution and the concentration of 12g/L is the mixed solution of the aqueous citric acid solution of 21g/L, make be similar to shown in Figure 1, and the film that forms of the Nano silver piece as shown in the curve in Fig. 2.
Embodiment 5
The concrete steps of preparation are:
Step 1 is first that the silver nitrate aqueous solution of 12g/L, aqueous citric acid solution and the water that concentration is 8g/L are the rear 6min of stirring of ratio mixing of 2.2: 0.9: 100 according to volume ratio with concentration; Wherein, water is deionized water, obtains mixed solution.With concentration be again the sodium borohydride aqueous solution of 0.9g/L be injected into stir 14min in mixed solution after, aging 22h under room temperature obtains the young brilliant solution of silver; Wherein, silver nitrate aqueous solution and the volume ratio between sodium borohydride aqueous solution in the young brilliant solution of silver is 0.9: 1.1.
Step 2 after first being coated on the young brilliant solution of silver on conductive substrates, is placed in the moisture that evaporates solution under 45 ℃; Wherein, be applied to spin coating (or spraying, or dipping), conductive substrates is conductive glass, obtains being covered with on it young brilliant conductive substrates of silver.Being placed in electrolytic solution as negative electrode, graphite flake as anode with being covered with the young brilliant conductive substrates of silver on it again, is 1mA/cm in current density 2Continuous current under galvanic deposit 5min; Wherein, electrolytic solution is that concentration is that silver nitrate aqueous solution and the concentration of 16g/L is the mixed solution of the aqueous citric acid solution of 4g/L, make be similar to shown in Figure 1, and the film that forms of the Nano silver piece as shown in the curve in Fig. 2.
Select respectively again deionized water or distilled water as water, conductive glass or conductive rubber or metal as conductive substrates, repeat above-described embodiment 1～5, made equally as or be similar to shown in Figure 1, and the film that forms of the Nano silver piece as shown in the curve in Fig. 2.
If further improve purity and the quality of target product, the film that can form the Nano silver piece that makes re-uses argon gas after with washed with de-ionized water and dries up.
The purposes of the film that Nano silver piece forms is,
The film that Nano silver piece is formed is as the active substrate of surface enhanced Raman scattering, the rhodamine 6G that uses the burnt Raman spectrometer of copolymerization to measure to adhere on it or the content of tetrachloro biphenyl-77; Wherein, the optical maser wavelength of the burnt Raman spectrometer of copolymerization is that 532nm, output rating are 9～13mW, and be 1～60s the integral time during measurement.
Obviously, those skilled in the art's film that can form Nano silver piece of the present invention and its production and use carries out various changes and modification and does not break away from the spirit and scope of the present invention.Like this, if of the present invention these are revised and within modification belongs to the scope of claim of the present invention and equivalent technologies thereof, the present invention also is intended to comprise these changes and modification interior.

Claims (10)

1. the film that Nano silver piece forms, comprise conductive substrates, it is characterized in that:
Be covered with the film of nanometer bar bunch composition on described conductive substrates, the thickness of described film is 200～500nm;
Gap between nanometer bar in described nanometer bar bunch is 1～15nm;
The nanometer sheet serial connection that described nanometer bar is arc by the edge consists of;
Thick 10～the 50nm of being of the sheet of described nanometer sheet, the wide 30～300nm of being of sheet, length of a film are 90～150nm, and it is the silver of face-centered cubic phase;
The described face-centered cubic plate plane of the nanometer sheet of silver formation mutually is parallel to face-centered cubic (111) face of silver mutually.
2. the film that forms of Nano silver piece according to claim 1 is characterized in that being close-packed arrays between nanometer bar bunch.
3. the film of Nano silver piece composition according to claim 1, is characterized in that conductive substrates is conductive glass, or conductive rubber, or metal.
4. the thin film technology method that the described Nano silver piece of claim 1 forms, comprise electrodip process, it is characterized in that completing steps is as follows:
Step 1, be first that the silver nitrate aqueous solution of 8～12g/L, aqueous citric acid solution and the water that concentration is 6～8g/L are 1.8～2.2: 0.9～1.1 according to volume ratio with concentration: 96～100 ratio stirs 2min at least after mixing, obtain mixed solution, with concentration be again the sodium borohydride aqueous solution of 0.7～0.9g/L be injected into stir at least 10min in mixed solution after, aging 20h at least under room temperature, obtain the young brilliant solution of silver, wherein, silver nitrate aqueous solution and the volume ratio between sodium borohydride aqueous solution in the young brilliant solution of silver is 0.9～1.1: 0.9～1.1;
Step 2, after first being coated on the young brilliant solution of silver on conductive substrates, be placed in the moisture that evaporates solution under 35～45 ℃, obtain being covered with on it young brilliant conductive substrates of silver, being placed in electrolytic solution as negative electrode, graphite flake as anode with being covered with the young brilliant conductive substrates of silver on it again, is 0.1～1mA/cm in current density 2Continuous current under galvanic deposit 5～120min, wherein, electrolytic solution is that concentration is that silver nitrate aqueous solution and the concentration of 1～16g/L is the mixed solution of the aqueous citric acid solution of 4～72g/L, makes the film that Nano silver piece forms.
5. the thin film technology method of Nano silver piece composition according to claim 4, is characterized in that water is deionized water, or distilled water.
6. the thin film technology method of Nano silver piece composition according to claim 4, is characterized in that being applied to spin coating, or spraying, or dipping.
7. the thin film technology method of Nano silver piece composition according to claim 4, is characterized in that conductive substrates is conductive glass, or conductive rubber, or metal.
8. the thin film technology method that forms of Nano silver piece according to claim 4 is characterized in that re-using argon gas after film that the Nano silver piece that makes is formed is with washed with de-ionized water dries up.
9. the purposes of the film that forms of the described Nano silver piece of a claim 1 is characterized in that:
The film that Nano silver piece is formed is as the active substrate of surface enhanced Raman scattering, the rhodamine 6G that uses the burnt Raman spectrometer of copolymerization to measure to adhere on it or the content of tetrachloro biphenyl-77.
10. the purposes of the film of Nano silver piece composition according to claim 9, is characterized in that the optical maser wavelength of the burnt Raman spectrometer of copolymerization is that 532nm, output rating are 9～13mW, and be 1～60s the integral time during measurement.
CN2011103637484A 2011-11-09 2011-11-09 Film formed by silver nanosheets and preparation method and application of film Pending CN103103608A (en)

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CN103264166A (en) * 2013-06-07 2013-08-28 北京科技大学 Preparation method of self-assembled silver ball SERS (Surface Enhanced Raman Scattering) base with controllable silver nano sheet thickness
CN103616366A (en) * 2013-11-20 2014-03-05 中国科学院合肥物质科学研究院 Method capable of quantitatively detecting surface enhanced Raman spectroscopy (SERS) of polychlorinated biphenyl
CN103641065A (en) * 2013-11-29 2014-03-19 中国科学院合肥物质科学研究院 SERS substrate based on basil seed surface network structure and preparation method and usage of SERS substrate
CN103789807A (en) * 2014-01-06 2014-05-14 中国科学院合肥物质科学研究院 Nano tube array consisting of noble metal nano structure units, preparation method for nano tube array and application of nano tube array in organic molecule detection
CN105174194A (en) * 2015-08-06 2015-12-23 中国科学院合肥物质科学研究院 Gold micro-nano structure array and preparation method as well as application thereof
CN106077697A (en) * 2016-06-13 2016-11-09 合肥国轩高科动力能源有限公司 Preparation method and application of silver nano flower cluster/silver micron sheet with hierarchical structure
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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
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
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CN103641065A (en) * 2013-11-29 2014-03-19 中国科学院合肥物质科学研究院 SERS substrate based on basil seed surface network structure and preparation method and usage of SERS substrate
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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
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