CN105241864A - Laser-induce self-assembly method for preparing high-sensitivity optical fiber SERS probe - Google Patents
Laser-induce self-assembly method for preparing high-sensitivity optical fiber SERS probe Download PDFInfo
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- CN105241864A CN105241864A CN201510692551.3A CN201510692551A CN105241864A CN 105241864 A CN105241864 A CN 105241864A CN 201510692551 A CN201510692551 A CN 201510692551A CN 105241864 A CN105241864 A CN 105241864A
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- optical fiber
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Abstract
The invention discloses a laser-induce self-assembly method for preparing a high-sensitivity optical fiber SERS probe. The method comprises the steps of conducting fusion welding on one end of an optical fiber and an output tail fiber of a laser device, and inserting the other end of the optical fiber into precious metal nano-particle sol; slowly lifting the optical fiber from the sol to be higher than the liquid level by a certain height by means of a one-dimensional precise displacement platform, so that a specific meniscus structure is formed; switching on a laser light source to enable precious metal nano-particles at the position of the meniscus to be self-assembled at the end face of the optical fiber under laser radiation, so that the optical fiber SERS probe is formed. The laser-induce self-assembly method has the advantages of being low in cost, easy to operate, short in preparation cycle, high in preparation repeatability and the like. The prepared optical fiber SERS probe has high detection sensitivity and high spectrum repeatability and has important application prospects in remote/field detection of environment pollutants, in-vivo analysis in biomedicine, real-time detection of chemical reaction process and other fields.
Description
Technical field
The present invention relates to Surface enhanced raman spectroscopy field of molecular detection, particularly relate to a kind of method that induced with laser self-assembly method prepares high sensitivity optical fiber SERS probe.
Background technology
Characteristic that Raman spectrum has " fingerprint ", can be used in the detection and indentification of various molecule.But the Raman scattering interface of molecule is very little usually, is difficult to realize high-sensitivity measurement.Surface enhanced raman spectroscopy (SurfaceEnhancedRamanScattering, SERS) spectrum utilizes the Localized field enhancement characteristic of noble metal nano structure, and (typical enhancer is 10 greatly can to strengthen the intensity of Raman signal
4-10
10magnitude), in fields such as pollutant monitoring, analytical chemistry, biomedicine, environmental sciences, there is important application.
SERS substrate is the key realizing high sensitivity Raman detection.Tradition SERS substrate is (as SiO at semiconductor (as Si) or insulator
2) substrate surface prepares various noble metal nano structure, have benefited from the physics of various maturation, chemical preparation process, such SERS substrate can provide larger SERS enhancer, but also exist in actual applications such as prepare/detect repeatability poor, be difficult to realize the problems such as long-range, original position and dangerous Site Detection.In recent years, the SERS effect of noble metal nano structure and ripe optical fiber sensing technology are combined, form optical fiber SERS probe by noble metal nano structure being prepared into optical fiber surface, a kind of possible approach is provided for solving the problem.On the one hand, optical fiber has that quality is light, pliability good, loss is little, be with the advantages such as wide, antijamming capability is strong, for long-range, the Site Detection etc. of SERS provides opportunity; On the other hand, because in SERS measurement, the whole SERS sensitizing range on optical fiber probe surface all participates in generation and the collection process of Raman, probe has good SERS and detects repeatability.So the preparations and applicatio of high sensitivity optical fiber SERS probe becomes a focus of current research.
So far, people have utilized the chemical method such as chemical modification fixation, liquid phase synthesizing method, photoinduction chemical deposition and the physical method such as physical vaporous deposition, nanolithographic method to prepare multiple optical fiber SERS probe.Normally, chemical preparation process is simple to operate, with low cost, but the nanostructured of preparation mostly is noble metal nano particles island film, and SERS enhancer is more weak (is about 10
4magnitude); And although physical preparation method can obtain larger SERS enhancer (10
6-10
8magnitude), but usually depend on valuable instrument and equipment, preparation process is complicated, consuming time and be difficult to meet functional need prepared by high flux.So the optical fiber SERS probe preparation method of Development of Novel is the key advancing optical fiber SERS probe practicalization.
Summary of the invention
The object of the invention is exactly the defect in order to make up prior art, provides a kind of novel induced with laser self-assembly method to prepare the method for high sensitivity optical fiber SERS probe.
The present invention is achieved by the following technical solutions:
Induced with laser self-assembly method prepares a method for high sensitivity optical fiber SERS probe, comprises following step:
(1) optical fiber one end and laser instrument are exported tail optical fiber welding, the other end inserts previously prepared good noble metal nano particles colloidal sol;
(2) after optical fiber and colloidal sol complete wetting, utilize one-dimensional precise displacement platform to be carried by optical fibre slow to liquid level upper surface, under surface tension of liquid, form meniscus structure;
(3) open LASER Light Source, under the irradiation of induced laser, the noble metal nano particles at meniscus place, in fiber end face self assembly arrangement, forms optical fiber SERS probe.
Described optical fiber is silica fibre or polymer optical fiber or Ti∶Sapphire laser optical fiber.
Described induced laser transfers to fiber end face by coupling fiber and carries out probe preparation.
Described noble metal nano particles colloidal sol is distributed in alcohol, hydrosolvent by the gold, silver noble metal nano particles having specific dimensions/pattern, have larger Localized field enhancement of chemosynthesis in advance to be formed.
Under laser irradiation, the thermal effect of nano particle causes the localized hyperthermia at meniscus place, and then cause the local rapid evaporation of liquid, simultaneously, under surface tension of liquid effect, the liquid of meniscus place evaporation can be supplemented in time by sol solution, greatly adds the concentration of meniscus place noble metal nano particles, thus makes more noble metal nano particles participate in the self assembling process at meniscus place.
Under laser irradiation, between adjacent metal nano particle, show as electromagnetic attraction, thus the spacing of nano particle may be reduced further, form cluster structure, to provide larger Localized field enhancement, and then realize the high-sensitivity detection of Raman molecular.
Advantage of the present invention is:
One, the present invention utilize the self assembly of meniscus place noble metal nano particles under induced with laser to realize the preparation of optical fiber SERS probe, and the method is with low cost, simple to operate, manufacturing cycle is short;
Its two, the optical fiber SERS probe that the present invention prepares can provide the high Localized field enhancement factor, and all participates in exciting of SERS and collection process due to whole sensitizing range, and spectral measurement is reproducible;
Its three, the present invention can realize the repetition controlled synthesis of probe;
Its four, the present invention highly sensitive optical fiber SERS probe, be particularly useful for environmental contaminants long-range/Site Detection, biomedical in-vivo analysis, chemical reaction process the field such as to detect in real time.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that induced with laser self-assembly method prepares optical fiber SERS probe.
Fig. 2 is the scanning electron microscope (SEM) photograph of the optical fiber SERS probe prepared.
Fig. 3 is that the optical fiber SERS probe of preparation is to typical Raman molecular
pthe testing result of-ATP.
Fig. 4 is that the optical fiber SERS probe of preparation is to the testing result of residues of pesticides MP.
Fig. 5 is the five optical fibers SERS probe pair that induced with laser self-assembly method repeats to prepare
pthe spectral detection result of-ATP.
Embodiment
As shown in Figure 1, a kind of induced with laser self-assembly method prepares the method for high sensitivity optical fiber SERS probe, comprises following step:
(1) optical fiber 2 one end and laser instrument 1 are exported tail optical fiber welding, the other end inserts previously prepared good noble metal nano particles colloidal sol 4;
(2) after optical fiber 2 with colloidal sol complete wetting, utilize one-dimensional precise displacement platform 3 slowly to carry to liquid level upper surface by optical fiber 2, under surface tension of liquid, form meniscus structure 5;
(3) open LASER Light Source, under the irradiation of induced laser, the noble metal nano particles at meniscus 5 place, in optical fiber 2 end face self assembly arrangement, forms optical fiber SERS probe.
Described optical fiber 2 can be the multiple low-loss transmission optical fiber such as silica fibre, polymer optical fiber, Ti∶Sapphire laser optical fiber.
Described induced laser 1 carries out probe preparation by optical fiber 2 coupled transfer to fiber end face.
Described noble metal nano particles colloidal sol 4 is distributed in alcohol, water equal solvent by the noble metal nano particles such as the gold, silver having specific dimensions/pattern, have larger Localized field enhancement of chemosynthesis in advance to be formed.
Structural representation of the present invention as shown in Figure 1, induced with laser self-assembly method prepares high sensitivity optical fiber SERS probe, comprises the narrow band laser 1 of the 785nm that optical fiber pigtail exports, multimode silica fibre 2, one-dimensional precise displacement platform 3 and pre-synthesis Ag-nanocube alcohol colloidal sol 4.Fibre core and cladding diameter are respectively 200um and 220um, numerical aperture NA=0.22; The pre-synthesis Ag-nanocube size in laboratory is about 60nm, is dissolved in alcohol and obtains the Ag-nanocube alcoholic solution that mass concentration is 1mg/ml, for the preparation of probe.In concrete enforcement, after the both ends of the surface cutting process of multimode silica fibre, by its one end and the welding of laser instrument tail optical fiber, the other end inserts in Ag-nanocube alcohol colloidal sol; Then utilize one-dimensional precise translation stage slowly to be mentioned from colloidal sol by optical fiber, until higher than liquid level 0.45mm, form meniscus structure as shown in Figure 1; Now, open induced laser, due to the thermal effect of noble metal nano particles, the temperature at meniscus place significantly raises, and causes the rapid evaporation of meniscus place solution.In experiment, the container inner wall that we are containing colloidal sol observes a large amount of droplets.Under surface tension of liquid, the liquid of meniscus place rapid evaporation constantly can be supplemented by the sol solution of surrounding, thus causes fiber end face place noble metal nano particles concentration greatly to increase.Meanwhile, in laser irradiation after the match, between noble metal nano particles, show as electromagnetic attraction, be beneficial to nano particle and be self-assembled into cluster structure at fiber end face.Experimental result shows, induced with laser power, induction time etc. have larger impact to probe preparation.The experiment condition optimized, namely induced laser power is 70mW, induction time is when being 60s, and the surface topography of optical fiber SERS probe as shown in Figure 2.Due to the flat-top mode profile of multimode optical fiber, noble metal nano particles distributes at fiber end face approaches uniformity; Under induced with laser, a large amount of Ag-nanocube is adsorbed on fiber end face; And partial enlarged drawing can find out that particle becomes the cluster of class chain to arrange, and is formed numerous " focus ", is beneficial to highly sensitive SERS spectral detection.
In order to verify the effect of optical fiber SERS probe prepared by the method, the above-mentioned optical fiber SERS probe for preparing is inserted conventional Raman molecular p-Mercaptoaniline (
p-aminothiophenol,
p-ATP) and residues of pesticides parathion-methyl (Methylparathion, MP) aqueous solution in, utilize the SERS spectral results that Portable Raman spectrometer measurement obtains as shown in Figure 3, Figure 4.In spectrum test, employing must reach Tyke Portable Raman spectrometer Raman-Mini, and excitation wavelength is 785nm, and power is 50mW, spectrum integral time 2s.As seen from the figure, the optical fiber SERS probe pair prepared of the method
pthe detection sensitivity of-ATP and MP reaches 10 respectively
-9m and 10
-7m.That is, even if adopt the portable Raman spectrometer that sensitivity is lower, the SERS detection sensitivity of optical fiber SERS probe prepared by the inventive method is still higher, can be comparable in conjunction with the detection sensitivity of large-scale Confocal laser-scanning microscopy instrument with the current utilization tradition SERS substrate reported.Secondly, if accurately control the experiment conditions such as room temperature, concentrations of nanoparticles, induced laser power, induced with laser time, the optical fiber SERS probe that the method prepares has good repeatability.Fig. 5 provide repeat under the same conditions prepare five optical fibers SERS probe to 10
-7m
pthe spectral detection result of-ATP.Visible, five spectral lines almost overlap, and the relative standard deviation (RSD) at each Raman peaks place is all less than 10%, thus show that induced with laser self-assembly method of the present invention is prepared high sensitivity optical fiber SERS probe and had good preparation repeatability.
Obviously, those skilled in the art can prepare high sensitivity optical fiber SERS probe to induced with laser self-assembly method of the present invention and carries out various change and modification and do not depart from the spirit and scope of the present invention.Therefore, if any amendment and modification belong within the scope of the claims in the present invention and equivalent technologies thereof, then the present invention is also intended to comprise these change and modification.
Claims (4)
1. induced with laser self-assembly method prepares a method for high sensitivity optical fiber SERS probe, it is characterized in that: comprise following step:
(1) optical fiber one end and laser instrument are exported tail optical fiber welding, the other end inserts previously prepared good noble metal nano particles colloidal sol;
(2) after optical fiber and colloidal sol complete wetting, utilize one-dimensional precise displacement platform to be carried by optical fibre slow to liquid level upper surface, under surface tension of liquid, form meniscus structure;
(3) open LASER Light Source, under the irradiation of induced laser, the noble metal nano particles at meniscus place, in fiber end face self assembly arrangement, forms optical fiber SERS probe.
2. induced with laser self-assembly method according to claim 1 prepares the method for high sensitivity optical fiber SERS probe, it is characterized in that: described optical fiber is silica fibre or polymer optical fiber or Ti∶Sapphire laser optical fiber.
3. induced with laser self-assembly method according to claim 1 prepares the method for high sensitivity optical fiber SERS probe, it is characterized in that: described induced laser transfers to fiber end face by coupling fiber and carries out probe preparation.
4. induced with laser self-assembly method according to claim 1 prepares the method for high sensitivity optical fiber SERS probe, it is characterized in that: described noble metal nano particles colloidal sol is distributed in alcohol, hydrosolvent by the gold, silver noble metal nano particles having specific dimensions/pattern, have larger Localized field enhancement of chemosynthesis in advance to be formed.
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Cited By (12)
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| CN105758838A (en) * | 2016-04-11 | 2016-07-13 | 北京大学 | Method and device for detecting and selecting laser-induce enhanced Raman spectrum in liquid |
| CN106744663A (en) * | 2017-02-28 | 2017-05-31 | 西北工业大学 | The method that Localized field enhancement focus induction self-assembly method prepares silver-colored micro- flower |
| CN107478640A (en) * | 2017-08-04 | 2017-12-15 | 中国科学院合肥物质科学研究院 | A kind of enhanced Portable Raman spectrometer of optical fiber probe |
| CN108333166A (en) * | 2018-02-09 | 2018-07-27 | 上海理工大学 | The surface enhanced Raman scattering substrate and preparation method of induced with laser |
| CN109520990A (en) * | 2018-09-29 | 2019-03-26 | 东莞理工学院 | The method that one step czochralski method of induced with laser prepares conical fiber SERS probe |
| CN109520991A (en) * | 2018-09-29 | 2019-03-26 | 东莞理工学院 | A kind of preparation method of functionization coffee ring pattern optical fiber SERS probe |
| CN109612970A (en) * | 2018-11-23 | 2019-04-12 | 山西大学 | A kind of method and device enhancing gold nanosphere fluorescence intensity |
| CN109813349A (en) * | 2019-02-27 | 2019-05-28 | 华南理工大学 | A kind of composite optical fiber device and preparation and application detecting light, electricity and chemical signal |
| CN109884026A (en) * | 2019-01-21 | 2019-06-14 | 东莞理工学院 | A kind of liquid phase in-situ SERS detection method |
| CN110108693A (en) * | 2019-04-26 | 2019-08-09 | 安徽建筑大学 | A kind of glue envelope Ag nano particle spheroiding efficient uniform SERS substrate preparation method |
| CN110146482A (en) * | 2019-05-13 | 2019-08-20 | 上海大学 | A kind of novel near-field raman scattering detection device |
| CN114346235A (en) * | 2022-01-17 | 2022-04-15 | 华东师范大学重庆研究院 | Self-assembled spherical-hexagonal gold nanoparticle assembly and preparation method thereof |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105758838A (en) * | 2016-04-11 | 2016-07-13 | 北京大学 | Method and device for detecting and selecting laser-induce enhanced Raman spectrum in liquid |
| CN105758838B (en) * | 2016-04-11 | 2018-08-10 | 北京大学 | The detection of induced with laser enhancing Raman spectrum and method for separating and its device in liquid |
| CN106744663A (en) * | 2017-02-28 | 2017-05-31 | 西北工业大学 | The method that Localized field enhancement focus induction self-assembly method prepares silver-colored micro- flower |
| CN107478640A (en) * | 2017-08-04 | 2017-12-15 | 中国科学院合肥物质科学研究院 | A kind of enhanced Portable Raman spectrometer of optical fiber probe |
| CN108333166A (en) * | 2018-02-09 | 2018-07-27 | 上海理工大学 | The surface enhanced Raman scattering substrate and preparation method of induced with laser |
| CN109520990A (en) * | 2018-09-29 | 2019-03-26 | 东莞理工学院 | The method that one step czochralski method of induced with laser prepares conical fiber SERS probe |
| CN109520991A (en) * | 2018-09-29 | 2019-03-26 | 东莞理工学院 | A kind of preparation method of functionization coffee ring pattern optical fiber SERS probe |
| CN109520990B (en) * | 2018-09-29 | 2021-07-27 | 东莞理工学院 | Method for preparing tapered optical fiber SERS (surface enhanced Raman Scattering) probe by laser-induced one-step pulling method |
| CN109612970B (en) * | 2018-11-23 | 2021-07-02 | 山西大学 | Method and device for enhancing fluorescence intensity of gold nanospheres |
| CN109612970A (en) * | 2018-11-23 | 2019-04-12 | 山西大学 | A kind of method and device enhancing gold nanosphere fluorescence intensity |
| CN109884026A (en) * | 2019-01-21 | 2019-06-14 | 东莞理工学院 | A kind of liquid phase in-situ SERS detection method |
| CN109813349A (en) * | 2019-02-27 | 2019-05-28 | 华南理工大学 | A kind of composite optical fiber device and preparation and application detecting light, electricity and chemical signal |
| CN110108693A (en) * | 2019-04-26 | 2019-08-09 | 安徽建筑大学 | A kind of glue envelope Ag nano particle spheroiding efficient uniform SERS substrate preparation method |
| CN110108693B (en) * | 2019-04-26 | 2021-07-13 | 安徽建筑大学 | Preparation method of colloid-sealed Ag nano-particle spherical efficient uniform SERS substrate |
| CN110146482A (en) * | 2019-05-13 | 2019-08-20 | 上海大学 | A kind of novel near-field raman scattering detection device |
| CN114346235A (en) * | 2022-01-17 | 2022-04-15 | 华东师范大学重庆研究院 | Self-assembled spherical-hexagonal gold nanoparticle assembly and preparation method thereof |
| CN114346235B (en) * | 2022-01-17 | 2024-01-26 | 华东师范大学重庆研究院 | Self-assembled spherical-hexagonal gold nanoparticle assembly and preparation method thereof |
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