CN105004706A - Surface enhanced Raman scattering active substrate and production method thereof - Google Patents
Surface enhanced Raman scattering active substrate and production method thereof Download PDFInfo
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Abstract
The invention provides a high-responsibility surface enhanced Raman scattering active substrate and a production method thereof. The active substrate comprises an III-V semiconductor substrate with a porous gully surface and Au nanoparticles distributed on the III-V semiconductor substrate. The method comprises the following steps: etching the surface of a substrate to form a rough surface; and depositing the Au nanoparticles on the surface of the substrate with a porous gully surface through an electrochemical deposition technology. The production method has the advantages of simplicity, low cost and easy realization; and the surface enhanced Raman scattering active substrate produced through the method has no nanoparticle agglomeration phenomenon, and has very high electric field intensity, long photo-induced carrier life and high Raman signal intensity, so the surface enhanced Raman scattering active substrate has high reuse rate and detection sensitivity, thereby the surface enhanced Raman scattering active substrate can be used in ultralow molecular concentration SERS detection, and can be widely used.
Description
Technical field
The present invention relates to nano surface science, galvanochemistry, bio-science and laser raman detection technique field, be specifically related to the preparation method of a kind of high-responsivity surface-enhanced Raman scattering activity substrate.
Background technology
Surface enhanced raman spectroscopy (Surface-enhanced Raman scattering, SERS) spectrum, owing to possessing high sensitivity, the structural information of material can be studied on a molecular scale and realize monomolecular detection, becoming the surface light spectral technology that has future.Wherein based on the material of noble silver, gold, copper and alkaline metal, there is higher SERS active, and the strongest with the enhancing ability of silver, and gold, copper take second place; Meanwhile, the activity of SERS substrate is to a great extent to size, the shape of metal nanoparticle and support that substrate surface topography is relevant.Therefore, in order to prepare the substrate of high SERS performance, for the regulation and control of metal nanoparticle and to supporting that the selection of backing material and finishing are quite necessary.
Along with the development of nano science and nanosecond science and technology, develop the method for a lot of synthesis difformity, size metallic nano particle, such as chemical reduction method, chemical method of substitution, photoreduction, thermal decomposition and ultrasonic decomposition method etc.The simplest and most popular method is chemical reduction method.Chemical reduction method refers to the process in the solution metal salt back being become metal nanoparticle, and reductive agent comprises sodium citrate, NaBH
4, oxygen, ethanol etc.Some surfactants, the Chang Zuowei protective agents such as such as CTAB, PVP, SDS are added into control pattern and size in reaction, and prevent coagulation and the oxidation of particle.But, for at present, it is not generally very desirable for strengthening effect and repeat usage by these methods Raman active substrate obtained based on Au, and the metal-sol method acquisition substrate adopted has the most excellent SERS performance, but result of study shows, obtain nano particle to be by this method easy to agglomeration occurs, make its substrate performance extremely unstable.
Summary of the invention
For solving the problem existing for above-mentioned prior art, the object of the present invention is to provide a kind of preparation method of surface-enhanced Raman scattering activity substrate, the method utilizes electrochemical deposition method having the substrate surface deposition Au nano particle of rough surface, without nanoparticle agglomerates phenomenon in the surface-enhanced Raman scattering activity substrate making it prepare, not only increase accuracy of detection, also improve recycling rate of waterused simultaneously.
To achieve these goals, the preparation method of a kind of surface-enhanced Raman scattering activity substrate provided by the invention, preparation comprises III-V semiconductor base with rough surface and the surface-enhanced Raman scattering activity substrate being distributed in described suprabasil Au nano particle, comprise step: etching processing is carried out to substrate surface, form coarse surface; By electrochemical deposition method, there is the substrate surface deposition Au nano particle of rough surface.
Preferably, above-mentioned steps specifically comprises:
A) etching processing is carried out to substrate surface, form coarse surface;
B) by electrochemical deposition method, there is the substrate surface deposition Au nano particle of rough surface.
Preferably, described etching processing comprises in galvanochemistry or Optical Electro-Chemistry a kind of.
Preferably, the electrolytic solution in described step b is the HAuCl of 1 ~ 15mM/L
4solution.
Preferably, the electrochemical deposition method in described step b is a kind of for following in peace voltammetry or instant potential method.
Correspondingly, the invention also discloses a kind of SERS substrate adopting said method to prepare, comprise III-V semiconductor base with surface, porous gully and be distributed in described suprabasil Au nano particle.
Preferably, the diameter of described Au nano particle is less than 25nm.
Preferably, described Au grain spacing is less than 10nm.
Preferably, described III-V semiconductor base is porous gully shape.
Beneficial effect:
The preparation method of surface-enhanced Raman scattering activity substrate provided by the invention, utilize electrochemical deposition method having the substrate surface deposition Au nano particle of rough surface, not only method is simple, with low cost, is easy to realize; And, without nanoparticle agglomerates phenomenon in the surface-enhanced Raman scattering activity substrate prepared by the method, and there is higher electric field intensity and photo-generated carrier life-span and higher Raman signal intensity, thus make it have higher recycling rate of waterused and detection sensitivity, and then may be used for, in ultra-low molecular concentration SERS detection, making it have wider usable range.
Accompanying drawing explanation
The structural representation of the surface-enhanced Raman scattering activity substrate that Fig. 1 provides for the embodiment of the present invention 1,2,3.
The structural representation of the surface-enhanced Raman scattering activity substrate that Fig. 2 provides for the embodiment of the present invention 4.
The SEM figure with the structure GaN-based end, porous gully that Fig. 3 provides for the embodiment of the present invention 3, wherein Fig. 3 a is that the SEM at the bottom of GaN base with porous gully structure schemes; Fig. 3 b is the enlarged drawing of Fig. 3 a.
The SEM figure of the surface-enhanced Raman scattering activity substrate that Fig. 4 provides for the embodiment of the present invention 3, wherein, Fig. 4 a is the SEM figure at the gully place of surface-enhanced Raman scattering activity substrate; Fig. 4 b is the SEM figure at the poroid place of surface-enhanced Raman scattering activity substrate.
Embodiment
In order to set forth technical characterstic of the present invention and structure better, be described in detail below in conjunction with the preferred embodiments of the present invention and accompanying drawing thereof.
For convenience of explanation, in the examples below, we are to be described at the bottom of GaN base, and certainly, in other embodiments, substrate also can be other III-V semiconductor materials.
Embodiment 1
A) Optical Electro-Chemistry etching processing is carried out to the surface at the bottom of GaN base: clean at the bottom of this GaN base with acetone, ethanol and deionized water successively, to immerse in the dilute sulfuric acid of 0.5M/L at the bottom of GaN base, and add bias voltage and the ultraviolet source of 3V, anode etching 15min.Certainly, in other embodiments, also can immerse as the acid solutions such as hydrofluorite etch.By washed with de-ionized water after etching, to material is thus formed at the bottom of the GaN base with porous gully shape 110.
B) adopt cyclic voltammetry, at GaN base basal surface deposition Au nano particle 120, prepare the SERS active-substrate based on Au-GaN: with the HAuCl of 1mM/L
4add NaCl (or the KNO of 1M/L
3or KCl) as electrolyte, adopt cyclic voltammetry, at GaN base basal surface deposition Au nano particle 120.In a kind of preferred embodiment, scanning voltage scope is-2.0-0.5V, sweep speed 50mV/s, and the scanning number of turns is 5.Deposit rear taking-up washed with de-ionized water, thus obtain surface-enhanced Raman scattering activity substrate as shown in Figure 1.
Be less than 25nm by the diameter of the Au nano particle 120 in the SERS active-substrate that this legal system is standby, Au grain spacing is from being less than 10nm, and its SERS active-substrate is 10 to the limit of rhodamine 6G detectable concentration
-16m/L.
Embodiment 2
A) Optical Electro-Chemistry etching processing is carried out to the surface at the bottom of GaN base: clean at the bottom of this GaN base with acetone, ethanol and deionized water successively, then dry up with nitrogen; Immerse at the bottom of GaN base in the dilute sulfuric acid of 0.5M/L, and add bias voltage and the ultraviolet source of 5V, anode etching 45min; By washed with de-ionized water after etching, and dry up with nitrogen, to material is thus formed at the bottom of the GaN base with porous gully shape 110.
B) adopt cyclic voltammetry, at GaN base basal surface deposition Au nano particle 120, prepare the SERS active-substrate based on Au-GaN: with the HAuCl of 1mM/L
4add NaCl (or the KNO of 0.5M/L
3) as electrolyte, adopt cyclic voltammetry, at GaN base basal surface deposition Au nano particle 120.In a kind of preferred embodiment, scanning voltage scope is-2.0-0.5V, sweep speed 50mV/s, and the scanning number of turns is 20.Deposit rear taking-up washed with de-ionized water, just obtain SERS substrate as shown in Figure 1.
Be less than 25nm by the diameter of the acquisition Au nano particle 120 of the method, grain spacing is less than 10nm, and its SERS active-substrate is 10 to the limit of rhodamine 6G detectable concentration
-16m/L
Embodiment 3
A) electrochemical etching process is carried out to the surface at the bottom of GaN base: clean at the bottom of this GaN base with acetone, ethanol and deionized water successively; Substrate is immersed ionic liquid 1-butyl-3-methyl imidazolium perchlorate, and add bias voltage 3V, reaction 40min, anode etching is carried out at the bottom of GaN base, by washed with de-ionized water after etching, to material is thus formed at the bottom of the GaN base with porous gully shape 110, its SEM figure consults Fig. 3.
B) adopt cyclic voltammetry, at GaN base basal surface deposition Au nano particle 120, prepare the SERS active-substrate based on Au-GaN: with the HAuCl of 1mM/L
4add NaCl (or the KNO of 0.5M/L
3) as electrolyte, adopt cyclic voltammetry, at GaN base basal surface deposition Au nano particle 120.In a kind of preferred embodiment, scanning voltage scope is-2.0-0.5V, sweep speed 50mV/s, and the scanning number of turns is 15.Deposit rear taking-up washed with de-ionized water, just obtain SERS substrate as shown in Figure 1.Consult Fig. 4, for the SEM of the SERS active-substrate prepared by the method is schemed, as can be seen from the figure, the Au nano particle at the bottom of GaN base not only has less size, and its diameter is less than 25nm, and it is evenly distributed, and grain spacing is less than 10nm.
Embodiment 4
A) electrochemical etching process is carried out to the surface at the bottom of GaN base: clean at the bottom of this GaN base with acetone, ethanol and deionized water successively; Ionic liquid 1-butyl-3-methyl imidazolium perchlorate is immersed by the bottom of the GaN base cleaned up, and adding bias voltage 5V, reaction 60min, carries out anode etching at the bottom of this GaN base, by washed with de-ionized water after etching, material is thus formed at the bottom of the GaN base with porous gully shape.
B) adopt chronoptentiometry, at GaN base basal surface deposition Au nano particle, prepare the SERS active-substrate based on Au-GaN: with the HAuCl of 12.5mM/L
4with 15g/L polyvinylpyrrolidone as electrolyte, adopt chronoptentiometry, at GaN base basal surface deposition Au nano particle.In a kind of preferred embodiment, cathode current is 0.225mA, and sedimentation time is 30min, thus obtains the gold grain structure of class sea urchin shape.Deposit rear taking-up washed with de-ionized water, thus obtain SERS active-substrate.
Au nano-particle diameter in SERS active-substrate prepared by the present embodiment is less than 25nm, and its SERS active-substrate is 10 to the limit of rhodamine 6G detectable concentration
-16m/L.
Embodiment 5
A) Optical Electro-Chemistry etching processing is carried out to the surface at the bottom of GaN base: clean at the bottom of GaN base with acetone, ethanol and deionized water successively; Immerse at the bottom of the GaN base cleaned up in the dilute sulfuric acid of 0.5M/L, and add bias voltage and the ultraviolet source of 6V, anode etching 45min; By washed with de-ionized water after etching, material is thus formed at the bottom of the GaN base with porous gully structure.
B) adopt chronoptentiometry, at GaN base basal surface deposition Au nano particle, prepare the SERS active-substrate based on Au-GaN: with the HAuCl of 12.5mM/L
4with 15g/L polyvinylpyrrolidone as electrolyte, adopt chronoptentiometry, at GaN base basal surface deposition Au nano particle.In a kind of preferred embodiment, cathode current is 0.225mA, and sedimentation time is 70min, thus obtains the gold grain structure of class sea urchin shape.Deposit rear taking-up washed with de-ionized water, and dried up with nitrogen and just obtain SERS active-substrate.
Au nano-particle diameter in SERS active-substrate prepared by the present embodiment is less than 25nm, and Au nano particle spacing is less than 10nm, and its SERS active-substrate is 10 to the limit of rhodamine 6G detectable concentration
-16m/L.
In sum, the preparation method of surface-enhanced Raman scattering activity substrate provided by the invention, utilize electrochemical deposition method having the substrate surface deposition Au nano particle of rough surface, not only method is simple, with low cost, is easy to realize; And, without nanoparticle agglomerates phenomenon in the surface-enhanced Raman scattering activity substrate prepared by the method, and there is higher electric field intensity and photo-generated carrier life-span and higher Raman signal intensity, thus make it have higher recycling rate of waterused and detection sensitivity, and then may be used for, in ultra-low molecular concentration SERS detection, making it have wider usable range.
It should be noted that, in this article, the such as relational terms of first and second grades and so on is only used for an entity or operation to separate with another entity or operational zone, and not necessarily requires or imply the relation that there is any this reality between these entities or operation or sequentially.And, term " comprises ", " comprising " or its any other variant are intended to contain comprising of nonexcludability, thus make to comprise the process of a series of key element, method, article or equipment and not only comprise those key elements, but also comprise other key elements clearly do not listed, or also comprise by the intrinsic key element of this process, method, article or equipment.When not more restrictions, the key element limited by statement " comprising ... ", and be not precluded within process, method, article or the equipment comprising described key element and also there is other identical element.
Although the present invention is described in detail with reference to its exemplary embodiment and shows, but will be understood by those skilled in the art that, when not departing from the spirit and scope of the present invention be defined by the claims, the various changes of form and details can be carried out to it.
Claims (9)
1. a preparation method for surface-enhanced Raman scattering activity substrate, is characterized in that, preparation comprises III-V semiconductor base with surface, porous gully and the surface-enhanced Raman scattering activity substrate being distributed in described suprabasil Au nano particle.
2. preparation method according to claim 1, is characterized in that, specifically comprises step:
A) etching processing is carried out to substrate surface, form coarse surface;
B) by electrochemical deposition method, there is the substrate surface deposition Au nano particle of rough surface.
3. preparation method according to claim 2, is characterized in that, the etching processing in described step a comprises in galvanochemistry or Optical Electro-Chemistry a kind of.
4. preparation method according to claim 2, is characterized in that, the electrolytic solution in described step b is the HAuCl of 1 ~ 15mM/L
4solution.
5. preparation method according to claim 2, is characterized in that, the electrochemical deposition method in described step b is a kind of in cyclic voltammetry or instant potential method.
6. a SERS substrate, is characterized in that, this substrate comprises III-V semiconductor base with surface, porous gully and is distributed in described suprabasil Au nano particle.
7. SERS substrate according to claim 6, is characterized in that the diameter of described Au nano particle is less than 25nm.
8. SERS substrate according to claim 6, is characterized in that described Au grain spacing is from being less than 10nm.
9. SERS substrate according to claim 6, is characterized in that described III-V semiconductor base is porous gully shape.
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| CN107290326A (en) * | 2016-04-12 | 2017-10-24 | 中国科学院苏州纳米技术与纳米仿生研究所 | Chip device and preparation method thereof |
| CN107337176A (en) * | 2017-06-16 | 2017-11-10 | 中国科学院苏州纳米技术与纳米仿生研究所 | surface enhanced Raman scattering substrate and its preparation technology |
| CN107522410A (en) * | 2017-09-11 | 2017-12-29 | 中国科学技术大学 | A kind of distinguishable CdTe thin film of surface vibration pattern and preparation method thereof and application |
| CN108950632A (en) * | 2018-07-31 | 2018-12-07 | 北京航空航天大学 | The preparation method of SERS substrate based on making active materials for use in secondary electrochemical sedimentation |
| CN110412012A (en) * | 2019-08-06 | 2019-11-05 | 长春工业大学 | For photodetector surfaces and the real-time characterization method and system in situ at interface |
| CN110714184A (en) * | 2019-09-29 | 2020-01-21 | 山东大学 | Surface enhanced Raman scattering substrate based on porous gallium nitride and preparation method thereof |
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| CN107290326A (en) * | 2016-04-12 | 2017-10-24 | 中国科学院苏州纳米技术与纳米仿生研究所 | Chip device and preparation method thereof |
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| CN107337176A (en) * | 2017-06-16 | 2017-11-10 | 中国科学院苏州纳米技术与纳米仿生研究所 | surface enhanced Raman scattering substrate and its preparation technology |
| CN107522410A (en) * | 2017-09-11 | 2017-12-29 | 中国科学技术大学 | A kind of distinguishable CdTe thin film of surface vibration pattern and preparation method thereof and application |
| CN108950632A (en) * | 2018-07-31 | 2018-12-07 | 北京航空航天大学 | The preparation method of SERS substrate based on making active materials for use in secondary electrochemical sedimentation |
| CN108950632B (en) * | 2018-07-31 | 2020-05-22 | 北京航空航天大学 | Preparation method of SERS substrate based on secondary electrochemical deposition method |
| US11237306B2 (en) | 2019-01-23 | 2022-02-01 | National Tsing Hua University | Method of fabricating optical substrate |
| CN110412012A (en) * | 2019-08-06 | 2019-11-05 | 长春工业大学 | For photodetector surfaces and the real-time characterization method and system in situ at interface |
| CN110412012B (en) * | 2019-08-06 | 2021-11-02 | 长春工业大学 | In-situ real-time characterization method and system for surface and interface of photoelectric detector |
| CN110714184A (en) * | 2019-09-29 | 2020-01-21 | 山东大学 | Surface enhanced Raman scattering substrate based on porous gallium nitride and preparation method thereof |
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