CN105004706B - Surface-enhanced Raman scattering activity substrate and preparation method thereof - Google Patents
Surface-enhanced Raman scattering activity substrate and preparation method thereof Download PDFInfo
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Abstract
Surface-enhanced Raman scattering activity substrate of a kind of high-responsivity provided by the invention and preparation method thereof, preparing includes the surface-enhanced Raman scattering activity substrate of the Au nano particles of III V semiconductor bases and distribution with porous gully surface on the substrate, including step：Processing is performed etching to substrate surface, forms coarse surface；Au nano particles are deposited in the substrate surface with porous gully structure by electrochemical deposition method.Not only method is simple for the preparation method, of low cost, it is easy to accomplish；And, without nanoparticle agglomerates phenomenon in the surface-enhanced Raman scattering activity substrate prepared by this method, and with very high electric field strength and photo-generated carrier service life and higher Raman signal intensity, so as to make it have higher recycling rate of waterused and detection sensitivity, and then can be used in ultra-low molecular concentration SERS detections, make it have wider use scope.
Description
Technical field
The present invention relates to nano surface science, electrochemistry, bioscience and LR laser raman detection technique fields, specifically relate to
And a kind of preparation method of high-responsivity surface-enhanced Raman scattering activity substrate.
Background technology
Surface enhanced Raman scattering (Surface-enhanced Raman scattering, SERS) spectrum, due to possessing
High sensitivity can study the structural information of substance and realize to monomolecular detection, become a pole on a molecular scale
Has the surface spectrum technology of future.Substance wherein based on noble silver, gold, copper and alkali metal has higher SERS activity,
And it is most strong with the enhancing ability of silver, gold, copper take second place；Meanwhile SERS substrates activity largely with metal nanoparticle
Size, shape and support substrate surface topography are related.Therefore, in order to prepare the substrate of high SERS performances, for metal nano
The regulation and control of particle and to support substrate material selection and surface modification be quite it is necessary to.
With the development of nano science and nanosecond science and technology, many synthesis different shapes, size metallic nano particle are developed
Method, such as chemical reduction method, chemical substitute method, photoreduction, thermal decomposition and ultrasonic decomposition method etc..Most simple and use
Widest method is chemical reduction method.Chemical reduction method refers to the mistake that metal salt is reduced into metal nanoparticle in the solution
Journey, reducing agent include sodium citrate, NaBH4, oxygen, ethyl alcohol etc..Some surfactants, such as CTAB, PVP, SDS etc. often make
It is added into for protective agent in reaction to control pattern and size, and prevents coagulation and the oxidation of particle.However, for current,
It is generally less desirable by Raman active substrate enhancing effect of these methods acquisition based on Au and repeat usage, and adopt
Metal-sol method, which obtains substrate, has most excellent SERS performances, however result of study shows to obtain by this method
Nano particle is easy to that agglomeration occurs so that its substrate performance is extremely unstable.
The content of the invention
To solve the problems of above-mentioned prior art, it is an object of the invention to provide a kind of surface-enhanced Ramans to dissipate
The preparation method of active substrate is penetrated, this method deposits Au nanometers using electrochemical deposition method in the substrate surface with rough surface
Particle makes to not only increase inspection without nanoparticle agglomerates phenomenon in the surface-enhanced Raman scattering activity substrate that it is prepared
Precision is surveyed, while also improves recycling rate of waterused.
To achieve these goals, the preparation method of a kind of surface-enhanced Raman scattering activity substrate provided by the invention,
Preparing includes the surface enhanced of the Au nano particles of III-V semiconductor base and distribution with rough surface on the substrate
Raman scattering active substrate, including step：Processing is performed etching to substrate surface, forms coarse surface；It is sunk by electrochemistry
Area method deposits Au nano particles in the substrate surface with rough surface.
Preferably, above-mentioned steps specifically include：
A) processing is performed etching to substrate surface, forms coarse surface；
B) Au nano particles are deposited in the substrate surface with rough surface by electrochemical deposition method.
Preferably, the etching processing includes a kind of in electrochemistry or optical electro-chemistry.
Preferably, the electrolyte in the step b is the HAuCl of 1~15mM/L4Solution.
Preferably, the electrochemical deposition method in the step b is a kind of in peace voltammetry or instant potentiometry to follow.
Correspondingly, it is porous including including having the invention also discloses a kind of SERS substrates prepared using the above method
The Au nano particles of III-V semiconductor base and distribution on gully surface on the substrate.
Preferably, the diameter of the Au nano particles is less than 25nm.
Preferably, the Au grain spacings are less than 10nm.
Preferably, III-V semiconductor base is porous gully shape.
Advantageous effect：
The preparation method of surface-enhanced Raman scattering activity substrate provided by the invention, using electrochemical deposition method with
The substrate surface deposition Au nano particles of rough surface, not only method is simple, of low cost, it is easy to accomplish；Moreover, pass through the party
Without nanoparticle agglomerates phenomenon in surface-enhanced Raman scattering activity substrate prepared by method, and with higher electric field strength and light
Raw carrier lifetime and higher Raman signal intensity, so as to make it have higher recycling rate of waterused and detection sensitivity, into
And it can be used in ultra-low molecular concentration SERS detections, making it have wider use scope.
Description of the drawings
Fig. 1 is the structure diagram for the surface-enhanced Raman scattering activity substrate that the embodiment of the present invention 1,2,3 provides.
Fig. 2 is the structure diagram for the surface-enhanced Raman scattering activity substrate that the embodiment of the present invention 4 provides.
Fig. 3 be the embodiment of the present invention 3 provide with the structure GaN-based bottom in porous gully SEM figure, wherein Fig. 3 a for
The SEM figures at the GaN base bottom of porous gully structure；Fig. 3 b are the enlarged drawing of Fig. 3 a.
Fig. 4 is the SEM figures for the surface-enhanced Raman scattering activity substrate that the embodiment of the present invention 3 provides, wherein, Fig. 4 a are table
SEM figures at the gully of face enhancing Raman scattering active substrate；Fig. 4 b are the poroid place of surface-enhanced Raman scattering activity substrate
SEM figure.
Specific embodiment
In order to preferably illustrate the technical characterstic of the present invention and structure, below in conjunction with the preferred embodiment of the present invention and its attached
Figure is described in detail.
For convenience of description, in the examples below, we illustrate by taking GaN base bottom as an example, certainly, in other realities
It applies in example, substrate or other III-V semi-conducting materials.
Embodiment 1
A) optical electro-chemistry etching processing is carried out to the surface at GaN base bottom：By the GaN base bottom successively with acetone, ethyl alcohol and
Deionized water is cleaned, and GaN base bottom is immersed in the dilute sulfuric acid of 0.5M/L, and is added in the bias and ultraviolet source of 3V, anode
Etch 15min.Certainly, in other embodiments, such as hydrofluoric acid acid solution can also be immersed to perform etching.After etching
It is cleaned with deionized water, material is thus formed the GaN base bottoms 110 with porous gully shape.
B) using cyclic voltammetry, in GaN base bottom surface deposition Au nano particles 120, the SERS based on Au-GaN is prepared
Active substrate：With the HAuCl of 1mM/L4In addition NaCl (or the KNO of 1M/L3Or KCl) as electrolyte, using cyclic voltammetry,
In GaN base bottom surface deposition Au nano particles 120.In a kind of preferred embodiment, scanning voltage scope is -2.0-0.5V,
Sweep speed 50mV/s, the scanning number of turns are 5.Taking-up is cleaned with deionized water after the completion of deposition, so as to obtain as shown in Figure 1
Surface-enhanced Raman scattering activity substrate.
The diameter of Au nano particles 120 in the SERS active-substrate prepared by the method is less than 25nm, Au grain spacings
From less than 10nm, 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 GaN base bottom：By the GaN base bottom successively with acetone, ethyl alcohol and
Deionized water is cleaned, and is then dried up with nitrogen；GaN base bottom is immersed in the dilute sulfuric acid of 0.5M/L, and add in the bias of 5V
And ultraviolet source, anode etching 45min；It is cleaned with deionized water after etching, and is dried up with nitrogen, material is thus formed tools
There is the GaN base bottom 110 of porous gully shape.
B) using cyclic voltammetry, in GaN base bottom surface deposition Au nano particles 120, the SERS based on Au-GaN is prepared
Active substrate：With the HAuCl of 1mM/L4In addition NaCl (or the KNO of 0.5M/L3) as electrolyte, using cyclic voltammetry,
GaN base bottom surface deposition Au nano particles 120.In a kind of preferred embodiment, scanning voltage scope is -2.0-0.5V, is swept
Rate 50mV/s is retouched, the scanning number of turns is 20.Taking-up is cleaned with deionized water after the completion of deposition, has just been obtained as shown in Figure 1
SERS substrates.
25nm is less than by the diameter for obtaining Au nano particles 120 of this method, grain spacing is less than 10nm, and SERS lives
Property substrate be 10 to the limit of rhodamine 6G detectable concentration-16M/L
Embodiment 3
A) electrochemical etching processing is carried out to the surface at GaN base bottom：The GaN base bottom with acetone, ethyl alcohol and is gone successively
Ionized water is cleaned；Substrate is immersed into ionic liquid 1-butyl-3-methyl imidazolium perchlorate, and adds in bias 3V, reaction
40min carries out GaN base bottom anode etching, is cleaned after etching with deionized water, material is thus formed with porous gully
The GaN base bottom 110 of shape, SEM figures are refering to Fig. 3.
B) using cyclic voltammetry, in GaN base bottom surface deposition Au nano particles 120, the SERS based on Au-GaN is prepared
Active substrate：With the HAuCl of 1mM/L4In addition NaCl (or the KNO of 0.5M/L3) as electrolyte, using cyclic voltammetry,
GaN base bottom surface deposition Au nano particles 120.In a kind of preferred embodiment, scanning voltage scope is -2.0-0.5V, is swept
Rate 50mV/s is retouched, the scanning number of turns is 15.Taking-up is cleaned with deionized water after the completion of deposition, has just been obtained as shown in Figure 1
SERS substrates.Refering to Fig. 4, the SEM of the SERS active-substrate to be prepared by this method schemes, it can be seen from the figure that GaN
Au nano particles in substrate not only have smaller size, and diameter is less than 25nm, and it is evenly distributed, and grain spacing is small
In 10nm.
Embodiment 4
A) electrochemical etching processing is carried out to the surface at GaN base bottom：The GaN base bottom with acetone, ethyl alcohol and is gone successively
Ionized water is cleaned；Ionic liquid 1-butyl-3-methyl imidazolium perchlorate is immersed at the GaN base bottom cleaned up, and is added
Enter and bias 5V, react 60min, anode etching is carried out to the GaN base bottom, is cleaned after etching with deionized water, thus shape
Into the GaN base bottom 210 with porous gully shape.
B) using chronoptentiometry, in GaN base bottom surface deposition Au nano particles 220, the SERS based on Au-GaN is prepared
Active substrate：With the HAuCl of 12.5mM/L4With 15g/L polyvinylpyrrolidones as electrolyte, using chronoptentiometry,
GaN base bottom surface deposition Au nano particles 220.In a kind of preferred embodiment, cathode current 0.225mA, sedimentation time
For 30min, so as to obtain the gold grain structure of class sea urchin shape.Taking-up is cleaned with deionized water after the completion of deposition, so as to obtain
SERS active-substrate.
220 diameter of Au nano particles in SERS active-substrate prepared by the present embodiment is less than 25nm, SERS activity
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 GaN base bottom：GaN base bottom with acetone, ethyl alcohol and is gone successively
Ionized water is cleaned；The GaN base bottom cleaned up is immersed in the dilute sulfuric acid of 0.5M/L, and add in the bias and ultraviolet light of 6V
Source, anode etching 45min；It is cleaned after etching with deionized water, material is thus formed the GaN bases with porous gully structure
Bottom.
B) using chronoptentiometry, Au nano particles are deposited in GaN base bottom surface, prepare the SERS activity based on Au-GaN
Substrate：With the HAuCl of 12.5mM/L4With 15g/L polyvinylpyrrolidones as electrolyte, using chronoptentiometry, in GaN base
Bottom surface deposits Au nano particles.In a kind of preferred embodiment, cathode current 0.225mA, sedimentation time 70min,
So as to obtain the gold grain structure of class sea urchin shape.Taking-up is cleaned with deionized water after the completion of deposition, and is just obtained with nitrogen drying
SERS active-substrate.
Au nano-particle diameters in SERS active-substrate prepared by the present embodiment are less than 25nm, Au nano particle spacing
From less than 10nm, SERS active-substrate is 10 to the limit of rhodamine 6G detectable concentration-16M/L。
In conclusion the preparation method of surface-enhanced Raman scattering activity substrate provided by the invention, is sunk using electrochemistry
Area method deposits Au nano particles in the substrate surface with rough surface, and not only method is simple, of low cost, it is easy to accomplish；And
And without nanoparticle agglomerates phenomenon in the surface-enhanced Raman scattering activity substrate prepared by this method, and with higher
Electric field strength and photo-generated carrier service life and higher Raman signal intensity, so as to make it have higher recycling rate of waterused and inspection
Sensitivity is surveyed, and then can be used in ultra-low molecular concentration SERS detections, makes it have wider use scope.
It should be noted that herein, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any this actual relation or order.Moreover, term " comprising ", "comprising" or its any other variant are intended to
Non-exclusive inclusion, so that process, method, article or equipment including a series of elements not only will including those
Element, but also including other elements that are not explicitly listed or further include as this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that
Also there are other identical elements in process, method, article or equipment including the element.
Although the present invention is described in detail and shows with reference to its exemplary embodiment, the common skill of this field
Art personnel it should be understood that in the case where not departing from the spirit and scope of the present invention being defined by the claims, can to its into
The various changes of row form and details.
Claims (5)
1. a kind of preparation method of surface-enhanced Raman scattering activity substrate, which is characterized in that the preparation method includes step：
A) processing is performed etching to the surface of III-V semiconductor base, to form porous gully surface, so as to form coarse table
Face；
B) Au nano particles, institute are deposited on the surface of III-V semiconductor base with rough surface by electrochemical deposition method
The diameter for stating Au nano particles is less than 25nm, and distance is less than 10nm between the Au nano particles.
2. preparation method according to claim 1, which is characterized in that the etching processing in the step a includes electrochemistry
It is or a kind of in optical electro-chemistry.
3. preparation method according to claim 1, which is characterized in that the electrolyte in the step b is 1~15mM/L's
HAuCl4Solution.
4. preparation method according to claim 1, which is characterized in that the electrochemical deposition method in the step b is Xun Huan
It is a kind of in voltammetry or chronoptentiometry.
5. a kind of SERS substrates, which is characterized in that the substrate includes III-V semiconductor base with porous gully surface and leads to
Cross the Au nano particles of electrochemical deposition method deposition on the substrate；The diameter of the Au nano particles is less than 25nm；It is described
Distance is less than 10nm between Au nano particles.
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| CN107290326B (en) * | 2016-04-12 | 2020-07-17 | 中国科学院苏州纳米技术与纳米仿生研究所 | Chip device and manufacturing method thereof |
| CN106179542A (en) * | 2016-07-11 | 2016-12-07 | 上海理工大学 | Porous gold mercury ion detecting Fluorescence chip preparation method and Fluorescence chip purposes |
| CN107337176B (en) * | 2017-06-16 | 2019-12-27 | 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 preparation process thereof |
| CN107522410B (en) * | 2017-09-11 | 2020-05-05 | 中国科学技术大学 | CdTe film with distinguishable surface vibration mode and preparation method and application thereof |
| 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 |
| TWI687677B (en) | 2019-01-23 | 2020-03-11 | 國立清華大學 | Optical substrate and method of fabricating the same |
| 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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