CN103257134A - Method for preparing surface-enhanced Raman scattering (SERS) substrate based on capillary tube - Google Patents
Method for preparing surface-enhanced Raman scattering (SERS) substrate based on capillary tube Download PDFInfo
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Abstract
The invention provides a method for preparing a surface-enhanced Raman scattering (SERS) substrate based on a capillary tube. The method comprises the following steps of: (1), preparing a photonic crystal of a three-dimensional porous ordered SiO2 inverse opal structure in the capillary tube; and (2), loading gold nano particles in the three-dimensional porous ordered SiO2 inverse opal structure by using an in-situ reduction or electrostatic adsorption method. The photonic crystal of the inverse opal structure is in a highly-ordered porous structure, has a high specific surface area, and enables an analyte to be in full contact with the substrate; meanwhile, a good SERS enhancement effect is achieved according to the special optical property of the photonic crystal; and by using the capillary tube as the substrate of a material, according to the porosity of the inverse structure, the circulation of the analyte is facilitated, and the quick real-time detection can be realized.
Description
Technical field
The present invention relates to field of nanometer material technology, field of biological detection and Raman spectrum detection technique field, specifically is a kind of preparation method based on Surface enhanced raman spectroscopy substrate capillaceous.
Background technology
Surface enhanced raman spectroscopy (SERS) technology overcome the detection sensitivity that normal Raman spectroscopy exists low, be subject to the shortcoming that fluorescence disturbs, can on molecular level, directly provide important informations such as the surperficial molecular structure that adsorbs, state, just become a kind of study of surfaces technology of fast development.Have extensively and great application prospect in surface absorption, galvanochemistry and catalytic reaction, chemistry and biology sensor, biomedical detection and fields such as trace detection and analysis.
The preparation of SERS substrate has consequence in the SERS development, SERS effect range of application further widen the development that depends on the SERS substrate, and the preparation of SERS substrate can also provide suitable model with check SERS theory, deepens people to the understanding of SERS essence.SERS substrate preparation method is a lot, such as the electrochemical etching electrode, vacuum evaporation island film, chemogenic deposit and chemical etching method, nanometer lithographic plate printing method, metal-sol do at the bottom of the active group and the pinpoint enhanced Raman active group at the bottom of etc.Yet the Rough Metal Surface that various preparation methods obtain generally is inhomogeneous, and it is different that this surface that makes that different laser spots obtain on the surface strengthens signal.In order to overcome this shortcoming and further to improve the SERS activity, people attempt making ining all sorts of ways to prepare orderly SERS substrate.The develop rapidly of nanosecond science and technology provides the good technical support for the preparation of the orderly substrate of micro-nano level, can obtain surface relatively uniformly than large tracts of land, thereby make even, the orderly SERS substrate of preparation become possibility.
From point of practical application, as a kind of SERS substrate, it should be easy to use, is easy to preparation, has very high enhancing ability, and have repeatability.The ordered nano-structure material has very high specific surface area, can increase the touch opportunity of analyte and substrate; The orderly nano structural material of 3D not only has dispersing uniformity and the stability of height, and has a photonic crystal characteristic, can provide extra SERS enhancement effect by regulating its optical characteristics of coupling, therefore, become a focus direction of SERS substrate preparation aspect based on the SERS substrate of orderly micro-nano structure, develop ordered nano-structure technology of preparing easy and simple to handle, with low cost, become the SERS technology is applied to the problem of needing solution in the reality badly.
Summary of the invention
Technical matters:The technical problem to be solved in the present invention is to overcome the enhancing of prior art Raman to respond shortcoming inhomogeneous, apparatus expensive, a kind of method of the SERS substrate of preparation three-dimensional order in kapillary is provided, it is ingenious, with low cost to have design concept, substrate SERS strengthens effective and sample introduction advantage easily, can be used for on-the-spotly detecting in real time.
Technical scheme:Purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method based on Surface enhanced raman spectroscopy substrate capillaceous may further comprise the steps:
Step 1, in kapillary the preparation three-dimensional porous orderly SiO
2The photonic crystal of counter opal structure;
Step 2, utilize the method for in-situ reducing or Electrostatic Absorption at three-dimensional porous orderly SiO
2Counter opal structure internal burden golden nanometer particle.
The present invention utilizes the capillary siphoning effect determinand solution to be sucked in the kapillary of above-mentioned load gold nano particle, the above-mentioned kapillary that is adsorbed with liquid to be measured is parallel or place under the Raman spectrometer perpendicular to the exciting light direction and to detect, focusing beats in the zone that possesses the SERS effect laser, detects the signal of determinand then.
Step 1 described in kapillary the preparation three-dimensional porous orderly SiO
2Counter opal structure is by with PS colloidal solution and SiO
2Colloidal solution mixes for 25:1～30:1 by volume, wherein in the PS colloidal solution diameter of colloidal particle between 197nm～326nm, SiO
2The diameter of colloidal particle is 3 ~ 10nm in the colloidal solution, mixed liquor is sucked kapillary carry out common assembling, treats after the water evaporates that high-temperature calcination removes the PS template and obtain.
The described utilization of step 2 utilizes the method for in-situ reducing at three-dimensional porous orderly SiO
2Counter opal structure internal burden golden nanometer particle is by with HAuCl
4The mixed liquor of solution and reductive agent places kapillary the water-bath heating simultaneously slowly by kapillary, reaches the purpose of in-situ reducing golden nanometer particle in inverse opal photonic crystal.
Described reductive agent is that percent concentration is 1% trisodium citrate aqueous solution, described HAuCl
4The percent concentration of solution is 0.01%, described HAuCl
4The volume ratio of solution and trisodium citrate aqueous solution is: 100:0.25～100:2.5.
The described electrostatic adsorption of step 2 is at three-dimensional porous orderly SiO
2Counter opal structure internal burden golden nanometer particle is by at SiO
2Counter opal structure finishing amino utilizes amino coordination to make golden nanometer particle be adsorbed on SiO
2The surface obtains.
Beneficial effect:With traditional SERS substrate comparatively speaking, this is bearing basement with the kapillary, the SERS substrate in conjunction with the ordered structure preparation of photonic crystal has the following advantages:
(1) sample introduction is convenient, detection speed is fast: traditional SERS substrate all is based on the plane and constructs, object solution to be measured need be dripped in substrate with other instruments when practical operation, wait to do the back and detect under Raman spectrum, process is loaded down with trivial details and be inconvenient to carry.The above-mentioned non-productive operation that does not need other instruments based on SERS substrate capillaceous fully, utilize syphonic effect capillaceous just can be directly object to be measured to be sucked kapillary SERS substrate inside, the poriness of counter opal structure also is conducive to analyte and is combined the abundant contact of focus with SERS.
(2) substrate homogeneity is good: the photonic crystal of counter opal structure is a kind of porous structure of high-sequential, has very high specific surface area, can improve dispersion degree and the stability of the golden nanometer particle of load, and then guarantees the homogeneity of substrate; Silicon dioxide this material itself can not detect to produce and disturb SERS simultaneously.
(3) enhancing is effective: the enhancing effect of SERS and pattern and the interparticle distance of particle have substantial connection, yet, when interparticle distance is in several nanometer range, though can produce extremely strong electromagnetic field strengthens, but also because of the touch opportunity that reduces to reduce greatly focus in analyte and the planar S ERS substrate of spacing, thereby reduce to strengthen effect, and uses kapillary to make that as substrate analyte is limited in circulating in the pipeline, increased it and be combined the initiative that focus contacts with SERS.In addition, by regulating the size of antistructure, utilize the photonic band gap character of photonic crystal uniqueness can obtain extra SERS humidification.
(4) extensibility height: be substrate with this micro-fluidic pipeline of kapillary, can be integrated with micro-fluidic chips such as sample pre-service, separation and Extraction easily, promoted microminiaturization and the robotization of analytic system;
Description of drawings
Fig. 1 is the technical scheme synoptic diagram that the present invention is based on Surface enhanced raman spectroscopy substrate preparation method capillaceous.
Fig. 2 is SiO in the kapillary
2The scanning electron microscope of photonic crystal with inverse opal structure (SEM) figure, wherein A: kapillary is blocked the back clap the SiO that penetrates from the cross section
2The sem photograph of photonic crystal with inverse opal structure; B: to the partial enlarged drawing of figure A.
Fig. 3 is the interior SiO of kapillary with in-situ reducing method load gold nano particle
2The scanning electron microscope of photonic crystal with inverse opal structure (SEM) figure, wherein, A: with the SiO behind the less golden nanometer particle of particle diameter in the local reduction way load
2The sem photograph of photonic crystal with inverse opal structure; B: to the partial enlarged drawing of figure A; C: with the SiO behind the golden nanometer particle that particle diameter is bigger in the local reduction way load
2The sem photograph of photonic crystal with inverse opal structure; D: to the partial enlarged drawing of figure C.
Fig. 4 is the Raman spectrogram with the Electrostatic Absorption method load gold nano particle creatinine solution that substrate records as SERS.
Fig. 5 is the Raman spectrogram with the in-situ reducing method load gold nano structure 4-ATP that substrate records as SERS and R6G.
Embodiment
The present invention is further illustrated below in conjunction with accompanying drawing.
Shown in Fig. 1, may further comprise the steps based on Surface enhanced raman spectroscopy substrate preparation method capillaceous: the first step: the method with assembling altogether in kapillary prepares solid SiO
2Photonic crystal with inverse opal structure; Second step: again to SiO in the kapillary
2Photonic crystal with inverse opal structure carries out surface amination and modifies; The 3rd step: gold nano structure in the method load of use Electrostatic Absorption or in-situ reducing.
Fig. 2 is SiO in the kapillary
2The scanning electron microscope of photonic crystal with inverse opal structure (SEM) figure.
It is made up of A, B two parts, wherein, and A: kapillary is blocked the back clap the SiO that penetrates from the cross section
2The sem photograph of photonic crystal with inverse opal structure; B: to the partial enlarged drawing of figure A, the three-dimensional order counter opal of visible preparation is the hexagonal closs packing structure.
Fig. 3 is the interior SiO of the kapillary of load gold nano particle
2The scanning electron microscope of photonic crystal with inverse opal structure (SEM) figure.It is by in A, B, C, the D four part groups, wherein, and A: with the SiO behind the less golden nanometer particle of particle diameter in the local reduction way load
2The sem photograph of photonic crystal with inverse opal structure; B: to the partial enlarged drawing of figure A, the visible less golden nanometer particle of particle diameter is adsorbed on the antistructure surface comparatively equably; C: with the SiO behind the golden nanometer particle that particle diameter is bigger in the local reduction way load
2The sem photograph of photonic crystal with inverse opal structure; D: to the partial enlarged drawing of figure C, the visible bigger golden nanometer particle of particle diameter comparatively is evenly distributed in the antistructure cavity.
The invention will be further described below in conjunction with embodiment, but the present invention is not limited to following embodiment.
Embodiment 1
At first, with diameter be the less SiO of particle diameter that the bigger PS colloidal particle of the particle diameter of 197nm～326nm and diameter are 3 ~ 10nm
2Colloidal particle carries out the common assembling in kapillary, through 550
oThe C high-temperature calcination is removed the PS template, obtains solid SiO in the kapillary
2Photonic crystal with inverse opal structure; Then, it is carried out surface amination handle, make its surperficial positively charged.With syringe pump with mean grain size be the aurosol of 60nm slowly by kapillary, by the coordination between amino and the gold atom, golden nanometer particle is adsorbed in the kapillary in the photonic crystal with inverse opal structure.
The SERS substrate that obtains with this kind method, with creatinine (the metabolic product of muscle, a kind of main biochemical substances composition in the urine) as detection molecules, it is 40-130mg/dL that its detectability can reach the normal creatinine content of 30mg/dL(human body), as can be seen from Figure 4, be the Raman spectrometer of 785nm when the aqueous solution of variable concentrations creatinine is detected with excitation wavelength, along with the reduction of creatine concentration, its signal intensity also weakens thereupon.Be followed successively by the Raman signal of the creatinine aqueous solution of 150 mg/dL, 120 mg/dL, 90 mg/dL, 60 mg/dL, 30 mg/dL concentration among the figure from top to bottom.
Embodiment 2
At first, with diameter be the less SiO of particle diameter that the bigger PS colloidal particle of the particle diameter of 197nm～326nm and diameter are 3 ~ 10nm
2Colloidal particle carries out the common assembling in kapillary, through 550
oThe C high-temperature calcination is removed the PS template, obtains solid SiO in the kapillary
2Photonic crystal with inverse opal structure, and it is carried out surface amination handle.Then, kapillary one end is linked to each other with the syringe that reactant liquor is housed by the Teflon flexible pipe, the other end puts the Teflon flexible pipe reactant liquor is derived, and capillary monolithic is placed water-bath, keeps 80
oC constant temperature.Reactant liquor is by HAuCl
4Solution and reductive agent trisodium citrate aqueous solution mix by a certain percentage.In the course of reaction, use peristaltic pump that reactant liquor is slowly passed through inverse opal photonic crystal in the kapillary with the speed of 10uL/min, carry out the growth in situ of gold nano structure.Fig. 3 A and B are with 0.01%HAuCl
4Solution and 1% trisodium citrate aqueous solution 100:2.5 by volume mix as reactant liquor, the SEM photo of the substrate of the load gold nano structure that obtains, and the gold nano physical dimension of visible load is less, and mean grain size is below 50nm; Fig. 3 C and D are with 0.01%HAuCl
4Solution and 1% trisodium citrate aqueous solution 100:0.25 by volume mix as reactant liquor, the SEM photo of the substrate of the load gold nano structure that obtains, and the gold nano physical dimension of visible load is bigger, and mean grain size is more than 100nm.
SERS substrate with Fig. 3 C and D correspondence, with 4-ATP(chemistry p-aminophenyl thiophenol by name) and R6G(chemistry rhodamine 6G by name) as detection molecules, respectively the ethanolic solution of 4-ATP and the aqueous solution of R6G have been carried out Raman signal detection, Fig. 5 is the result who respectively 4-ATP, R6G and mixed liquor thereof is detected, concrete operation method is that determinand solution is directly sucked in the kapillary, detects with the 785nm exciting light under Raman spectrometer.The result shows that its SERS signal is stronger, can detect two kinds of speciality simultaneously, shows at the bottom of this kind SERS active group to have applicability widely.
Claims (5)
1. the preparation method based on Surface enhanced raman spectroscopy substrate capillaceous is characterized in that, may further comprise the steps:
Step 1, in kapillary the preparation three-dimensional porous orderly SiO
2Photonic crystal with inverse opal structure;
Step 2, utilize the method for in-situ reducing or Electrostatic Absorption at three-dimensional porous orderly SiO
2Counter opal structure internal burden golden nanometer particle.
2. the preparation method of Surface enhanced raman spectroscopy substrate according to claim 1 is characterized in that: step 1 described in kapillary the three-dimensional porous orderly SiO of preparation
2Photonic crystal with inverse opal structure is by being that 5% PS colloidal solution and massfraction are 30% SiO with massfraction
2Colloidal solution mixes for 25:1～30:1 by volume, wherein in the PS colloidal solution diameter of colloidal particle between 197nm～326nm, SiO
2The diameter of colloidal particle sucks kapillary with mixed liquor and carries out common assembling at 3～10nm in the colloidal solution, treats after the water evaporates that high-temperature calcination removes the PS template and obtain.
3. the preparation method of Surface enhanced raman spectroscopy substrate according to claim 1, it is characterized in that: the method for the described in-situ reducing of step 2 is: by with HAuCl
4The mixed liquor of solution and reductive agent places kapillary the water-bath heating simultaneously slowly by kapillary, reaches the purpose of in-situ reducing golden nanometer particle in photonic crystal with inverse opal structure.
4. the preparation method of Surface enhanced raman spectroscopy substrate according to claim 3, it is characterized in that: described reductive agent is that percent concentration is 1% trisodium citrate aqueous solution, described HAuCl
4The percent concentration of solution is 0.01%, described HAuCl
4The volume ratio of solution and trisodium citrate aqueous solution is: 100:0.25～100:2.5.
5. the preparation method of Surface enhanced raman spectroscopy substrate according to claim 1 is characterized in that: the method for the described Electrostatic Absorption of step 2 is by at SiO
2Counter opal structure finishing amino utilizes amino coordination to make golden nanometer particle be adsorbed on SiO
2The surface obtains.
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Cited By (9)
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| CN104101630A (en) * | 2014-07-24 | 2014-10-15 | 南京大学 | Method for preparing nano-porous structure based on nano-particle self-assembly and application thereof |
| CN104226387A (en) * | 2014-09-01 | 2014-12-24 | 中国科学院合肥物质科学研究院 | Microflow device based on surface enhanced Raman scattering (SERS) effect and preparation method and application of microflow device |
| CN106153599A (en) * | 2015-04-22 | 2016-11-23 | 吴世法 | One has, without receptor nano titania metal film Raman chip and manufacture method |
| CN106546533A (en) * | 2015-09-20 | 2017-03-29 | 简佩蓉 | A kind of use full aperture angle parabolic lens collects the equipment of Surface Enhanced Raman Scattering Spectrum |
| CN107132212A (en) * | 2017-06-09 | 2017-09-05 | 天津大学 | The preparation method of the SERS senser element with side effect based on photonic crystal |
| CN108344713A (en) * | 2018-02-06 | 2018-07-31 | 军事科学院军事医学研究院环境医学与作业医学研究所 | Photonic crystal sensor material and its preparation method and application |
| CN110068564A (en) * | 2019-04-10 | 2019-07-30 | 东南大学 | A kind of dioxide photon crystal capillary and its preparation and application |
| CN110118765A (en) * | 2018-02-05 | 2019-08-13 | 武汉大学 | A kind of preparation of SERS substrate and its application in terms of cancer detection |
| CN111122537A (en) * | 2019-12-23 | 2020-05-08 | 中国科学院合肥物质科学研究院 | Surface-enhanced Raman spectroscopy substrate based on transmission-type capillary with open side wall and preparation method and application thereof |
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| CN104101630A (en) * | 2014-07-24 | 2014-10-15 | 南京大学 | Method for preparing nano-porous structure based on nano-particle self-assembly and application thereof |
| CN104226387A (en) * | 2014-09-01 | 2014-12-24 | 中国科学院合肥物质科学研究院 | Microflow device based on surface enhanced Raman scattering (SERS) effect and preparation method and application of microflow device |
| CN106153599B (en) * | 2015-04-22 | 2019-12-10 | 大连世佩达光谱智能检测科技有限公司 | receptor-containing and receptor-free titanium dioxide nano metal film Raman chip and manufacturing method thereof |
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| CN106546533B (en) * | 2015-09-20 | 2019-12-10 | 大连世佩达光谱智能检测科技有限公司 | Equipment for collecting surface enhanced Raman scattering spectrum by using full-aperture angle parabolic mirror |
| CN106546533A (en) * | 2015-09-20 | 2017-03-29 | 简佩蓉 | A kind of use full aperture angle parabolic lens collects the equipment of Surface Enhanced Raman Scattering Spectrum |
| CN107132212A (en) * | 2017-06-09 | 2017-09-05 | 天津大学 | The preparation method of the SERS senser element with side effect based on photonic crystal |
| CN107132212B (en) * | 2017-06-09 | 2020-07-10 | 天津大学 | Preparation method of surface-enhanced Raman scattering sensor |
| CN110118765A (en) * | 2018-02-05 | 2019-08-13 | 武汉大学 | A kind of preparation of SERS substrate and its application in terms of cancer detection |
| CN108344713A (en) * | 2018-02-06 | 2018-07-31 | 军事科学院军事医学研究院环境医学与作业医学研究所 | Photonic crystal sensor material and its preparation method and application |
| CN110068564A (en) * | 2019-04-10 | 2019-07-30 | 东南大学 | A kind of dioxide photon crystal capillary and its preparation and application |
| CN111122537A (en) * | 2019-12-23 | 2020-05-08 | 中国科学院合肥物质科学研究院 | Surface-enhanced Raman spectroscopy substrate based on transmission-type capillary with open side wall and preparation method and application thereof |
| CN111122537B (en) * | 2019-12-23 | 2022-09-13 | 中国科学院合肥物质科学研究院 | Surface-enhanced Raman spectrum substrate based on transmission-type capillary with open side wall and preparation method and application thereof |
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Application publication date: 20130821 |