CN112782268A - SERS micro-cavity structure based on hollow optical fiber inner wall and laser processing method thereof - Google Patents
SERS micro-cavity structure based on hollow optical fiber inner wall and laser processing method thereof Download PDFInfo
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Abstract
An SERS microcavity structure based on the inner wall of a hollow optical fiber and a laser processing method thereof belong to the technical field of plasmon nanophotonics and sensors. The laser processing method of the three-dimensional plasmon nanometer structure distributed on the inner wall of the hollow optical fiber is provided, the process is automatically controlled and efficient, and the novel SERS detection substrate can be prepared in batches by laser direct writing processing. The hollow optical fiber SERS substrate greatly improves the three-dimensional feedback and collection of SERS detection signals.
Description
Technical Field
The invention belongs to the technical field of plasmon nanophotonics and sensors. A laser processing method of three-dimensional plasmon nanometer structures distributed on the inner wall of a hollow optical fiber is provided, and the method is used for realizing high-sensitivity SERS sensing and trace detection technologies.
Background
The metal plasmon micro-nano structure is widely applied to various fields due to the excellent optical response characteristic. The micro-nano structure enables the optical field to be localized in the range of the nano scale around the metal nano structure, breaks through the diffraction limit of the traditional optics and enables the nano-scale light control to be possible. Based on this, a super-resolution excitation and imaging method using a surface plasmon interference field on a metal nanowire as an excitation source was developed, which has an optical resolution that breaks through the diffraction limit because the period of the surface plasmon interference fringes is much smaller than the wavelength of the excitation light. The electromagnetic field at the surface of the metal nanostructure can be greatly enhanced, thereby facilitating the interaction of light with the substance. If the light field is localized in the nanoparticle gap with small distance, the light field is Enhanced, so that a molecular Raman signal to be detected in the gap is Enhanced by more than ten orders of magnitude, and the metal plasmon micro-nano structure with the property is also called SERS (surface Enhanced Raman Scattering) structure, so that the metal plasmon micro-nano structure has very obvious advantages and wide application in the aspect of micro-content substance detection.
The preparation of the metal plasmon micro-nano structure comprising the SERS substrate is a precondition and a basis for the research and application of plasmon photophysics, and the research of the preparation technology capable of meeting different requirements has very important significance for promoting the development of nano photonics research. At present, there are many well-developed preparation methods of metal plasmon micro-nano structures, including physical methods of material reduction from top to bottom, such as electron beam etching, focused ion beam processing, laser interference ablation direct writing, nano imprinting, self-assembly processing, interference lithography combined with photoreduction, and the like; there is also a chemical synthesis method of constructing a structure from the bottom "from the bottom up", such as reducing a metal complex in a dilute solution to prepare a metal cutin dispersion, and the preparation of various metal plasmon micro-nano structures can be realized by the chemical synthesis method.
In various fields, the SERS device prepared by the above preparation method is mainly based on a planar substrate or a substrate with a more complex three-dimensional structure, for example, a two-dimensional inverted pyramid-shaped metal groove array is prepared by using a method of combining electron beam lithography with etching sputtering. Because the concentration of molecules in a liquid sample is low and the molecules are not easy to migrate, the direct SERS detection of the liquid sample is always a difficult problem. More importantly, the depth or thickness of the liquid is typically on the order of millimeters or even centimeters, while the interaction distance for the SERS effect is on the order of 100 nm. The preparation and application of the metal plasmon micro-nano structure based on the hollow optical fiber are also a hotspot of research, and the hollow optical fiber has great advantages in the aspects of conducting an optical field and allowing liquid to flow. In the hollow optical fiber, not only the optical field is localized in the micro-nano scale, but also a large amount of liquid substances are localized in the scale, thereby greatly improving the interaction between the light and the substances. ResearchersThe plasmon nanometer photonic devices are prepared by combining the plasmon micro-nano structures and the hollow optical fibers, and have good performance. Shanthil et al convert Ag @ SiO with silica shells of varying thickness (2-25 nm)2The nano particles (Ag-60 nm) are assembled on the inner wall of the hollow optical fiber, the length of the hollow optical fiber assembled with the nano particles exceeds 2cm, and the coverage is continuous and uniform. The particle density of the inner surface of the device plays a decisive role in enhancing Raman signals, and when the particle density is 30Ag @ SiO2/μm2When bound to the inner wall of a hollow core fiber, multiple hot spots are created. The detection of various substances such as polyaromatic hydrocarbon (pyrene), amino acid (tryptophan), protein (bovine serum albumin) and the like shows that Ag @ SiO is prepared2Hollow-core optical fibers of plasmonic micro-nano structures have wide applicability to the detection of molecules (m.shanthil, et al.acs Applied Materials Interfaces 9, 19470-.
Nevertheless, it is still a challenge to construct a large-area and continuous and uniform plasmon micro-nano structure on the inner wall of the hollow optical fiber, and various mature methods such as electron beam exposure, interference lithography and the like cannot be effectively combined with the hollow optical fiber substrate to prepare the continuous and uniform micro-nano structure in a long length.
Disclosure of Invention
Based on the research background and the technical problem, the invention provides a three-dimensional plasmon nano-structure laser processing method distributed on the inner wall of a hollow optical fiber, which is used for realizing a novel SERS detection technology. The method has the advantages of laser direct-writing processing of the high-sensitivity SERS detector, automatic control and efficient and batch preparation of the technological process, high-quality, continuous and uniform processing of the SERS structure, accurate and controllable structure parameters, and three-dimensional feedback and collection of SERS detection signals.
The preparation method for the plasmon micro-nano structure is characterized by being capable of realizing automatic processing control of three-dimensional SERS on the inner wall of a hollow optical fiber, being adjustable in parameters, realizing coaxial rotation of the front end and the rear end of the optical fiber by connection of flexible materials and limitation of double concentric holes in a rigid plate, and ensuring uniformity of laser processing.
The novel SERS detection structure is characterized in that the structure is distributed on the inner wall of a hollow optical fiber in a three-dimensional mode, a light field and a large amount of liquid are localized in the micro-nano scale of the hollow optical fiber, and high SERS detection sensitivity is achieved.
In order to achieve the above effects, the present invention is realized by the following steps:
the preparation device for the SERS microcavity structure is characterized by comprising a motor (1), a flexible connecting pipe (2), a hollow optical fiber (3) and a rigid plate (4), wherein a particle film formed by metal nanoparticles is adsorbed on the inner wall of the hollow optical fiber (1); the motor is coaxially connected with one end of the hollow optical fiber through a flexible material; the two rigid plates are parallel and opposite, the rigid plates are provided with limiting holes (5), the hollow optical fiber (3) penetrates through the two limiting holes (5), and the limiting holes (5) have the functions of supporting and limiting the hollow optical fiber; the laser is vertically focused on the outer wall of the hollow optical fiber; the motor can directly advance and rotate, the hollow optical fiber is driven by the motor to directly advance and rotate through the motor, and the limiting hole enables the hollow optical fiber and the motor to rotate coaxially. The process can be automatically controlled, and the processing is efficient.
The flexible material connecting the motor and the hollow core optical fiber may be a rubber tube, an adhesive tape, a string, preferably a rubber tube.
The rigid plate is selected from iron plate, aluminum plate, plastic plate, etc. The hollow optical fiber is vertical to the rigid plate.
The diameter of the hole on the rigid plate is larger than that of the outer wall of the hollow optical fiber, and is 1-2 times of the diameter of the outer wall of the hollow optical fiber and not 1 time.
The metal nano particle colloidal solution can be filled in the fiber core of the hollow optical fiber, and a metal nano particle multilayer film can be formed on the inner wall of the hollow optical fiber through the pretreatment process.
The bridging characteristic of 3-aminopropyl trimethoxy silane (APTMS) molecules is utilized to adsorb metal nanoparticles on the inner wall of the hollow optical fiber.
In the laser processing process, a cylindrical lens is used for generating an elliptical light spot, the elliptical light spot is parallel to the long axis of the optical fiber at the focus, and the uniform LSPR structure is generated by maximally processing a local area.
A uniform and long three-dimensional LSPR structure can be prepared on the inner wall of the hollow optical fiber.
By controlling the laser power and the straight advancing and rotating speeds of the hollow optical fiber, plasmon micro-nano structures with different surface morphologies can be processed.
Advantageous features of the invention
1. The SERS structure with three-dimensional distribution can be constructed on the inner wall of the hollow optical fiber.
2. The motor and the hollow optical fiber are connected by the flexible material, and the front end and the rear end of the hollow optical fiber can coaxially rotate by the limitation of the limiting hole.
3. By automatically controlling the straight advance and the rotation of the hollow optical fiber, the high-efficiency, large-area and uniform preparation of the plasmon micro-nano structure can be realized.
4. Raman signals are efficiently fed back and collected, and the SERS detection sensitivity is very high.
Drawings
FIG. 1 is a 3D view of a spacing device for controlling the linear movement of a hollow core optical fiber.
Fig. 2 is a top view of the device.
The device comprises a motor 1, a flexible connecting pipe 2, a hollow optical fiber 3 and a rigid plate 4.
Fig. 3 is a front sectional view of the device.
The device comprises a motor 1, a flexible connecting pipe 2, a hollow optical fiber 3, a rigid plate 4 and a limiting hole 5.
Fig. 4 is a right side view of the device. Wherein, 3-hollow optical fiber, 4-rigid plate and 5-limiting hole.
FIG. 5 is a schematic diagram showing the operation of the apparatus and the laser irradiation method.
Wherein, a (double-headed straight arrow): path of motor straight going, B (unidirectional straight arrow): laser irradiation direction for machining, C (double-sided circular arc arrow): direction of rotation of motor and hollow core optical fiber
FIG. 6 is an SEM photograph of an SERS structure attached to the inner wall of a hollow fiber after laser processing.
FIG. 7 shows the Raman spectra of different rhodamine 6G ethanol solutions measured by using a hollow-core optical fiber with SERS structure
Detailed Description
The present invention will be further described with reference to examples, but the present invention is not limited to the following examples.
Example 1: preparation of multilayer gold nanoparticle film on inner wall of hollow optical fiber tube
(1) Preparing a hollow optical fiber with the inner diameter of 600nm and the length of 10cm for later use;
(2) soaking the hollow optical fiber in NaOH aqueous solution for 30min, and then washing with deionized water for 2-3 times;
(3) preparing an APTMS methanol solution with the concentration of 5%;
(4) soaking the hollow-core optical fiber in an APTMS methanol solution for 2h, then washing the hollow-core optical fiber for 2-3 times by using methanol, and removing APTMS molecules which are not bonded on the inner wall of the hollow-core optical fiber;
(5) preparing gold nanoparticle powder with diameter of 2-5nm by using a Brust two-phase method;
(6) dissolving the prepared gold nanoparticle powder in xylene to prepare a gold nanoparticle colloidal solution with the concentration of 100 mg/mL;
(7) sucking the gold nanoparticle colloidal solution into the core of the hollow optical fiber by using capillary force, discharging the colloidal solution by using gravity, and repeating the process for 3-4 times;
(8) setting the temperature of the heating plate to 210 ℃, and placing the hollow optical fiber filled with the gold nanoparticle colloidal solution on the heating plate;
(9) and removing the gold nanoparticles which are not adsorbed on the inner wall of the hollow optical fiber when the solvent is volatilized, wherein the inner wall of the hollow optical fiber is adsorbed with a plurality of layers of compact gold nanoparticles.
Example 2: preparation of hollow optical fiber tube inner wall LSPR structure
(1) Connecting a hollow optical fiber with a silver nanoparticle silver multilayer film adsorbed on the inner wall by using a rubber tube, coaxially inserting the hollow optical fiber into two plastic plate holes which are oppositely fixed in position to limit the hollow optical fiber, wherein the two holes are on the same horizontal line with the motor rotating shaft;
(2) a 532nm continuous laser is used, the power of the laser is set to be 400mW, and the elliptical major axis of a laser spot is focused on the outer wall of the optical fiber in parallel through the focusing of a cylindrical lens (the major axis of the laser spot is 1cm, and the minor axis of the laser spot is 200 mu m);
(3) the motor was given a rotational speed of 360 °/s and a linear speed of 0.5 mm/s.
(4) And simultaneously turning on a rotation and straight-moving controller of the motor, starting laser processing, and finally preparing the hollow optical fiber with the length of 5cm and the inner wall attached with the LSPR structure, wherein the LSPR structure of the inner wall is shown in figure 6.
Example 3: hollow-core optical fiber with LSPR structure on inner wall for liquid Raman detection
Respectively placing hollow-core optical fibers with gold nanoparticle LSPR structures on the inner walls at different concentrations of 10-7-10-2In the environment of mol/L rhodamine 6G alcohol solution, a 785nm excitation light source is used for exciting Raman signals, the output power of the excitation light is 200mW, and the integration time is 1 s. The enhanced Raman spectrum of the obtained rhodamine 6G alcoholic solution is shown in FIG. 7. With the concentration of the rhodamine 6G ethanol solution decreasing, as shown in curves (1) (2) (3) (4) (5) (6) in FIG. 7, the Raman enhancement signal of the rhodamine 6G measured by the hollow-core fiber with the gold nanoparticle LSPR structure prepared on the inner wall gradually decreases. The lower concentration capable of detecting rhodamine 6G ethanol solution is 10-7mol/L。
Claims (8)
1. The preparation device for the SERS microcavity structure is characterized by comprising a motor (1), a flexible connecting pipe (2), a hollow optical fiber (3) and a rigid plate (4), wherein a particle film formed by metal nanoparticles is adsorbed on the inner wall of the hollow optical fiber (1); the motor is coaxially connected with one end of the hollow optical fiber through a flexible material; the two rigid plates are parallel and opposite, the rigid plates are provided with limiting holes (5), the hollow optical fiber (3) penetrates through the two limiting holes (5), and the limiting holes (5) have the functions of supporting and limiting the hollow optical fiber; the laser is vertically focused on the outer wall of the hollow optical fiber; the motor can directly advance and rotatory, and the straight advance of motor drives hollow fiber directly to advance and rotatory with the rotation, and spacing hole makes hollow fiber and the coaxial core of motor rotate, SERS microcavity structure for the SERS microcavity structure based on hollow fiber inner wall.
2. The apparatus of claim 1, wherein the flexible connection tube connecting the motor and the hollow fiber is a rubber tube or is replaced by an adhesive tape or string.
3. The apparatus of claim 1, wherein the rigid plate is selected from the group consisting of an iron plate, an aluminum plate, and a plastic plate; the hollow optical fiber is vertical to the rigid plate.
4. The apparatus of claim 1, wherein the diameter of the limiting hole in the rigid plate is larger than the diameter of the outer wall of the hollow-core fiber, and is 1-2 times but not 1 time the diameter of the outer wall of the hollow-core fiber.
5. The method for preparing the SERS microcavity structure by using the device according to any one of claims 1 to 4, wherein a metal nanoparticle colloidal solution is filled in a core of a hollow-core optical fiber, and a metal nanoparticle multilayer film is formed on the inner wall of the hollow-core optical fiber through a pretreatment process; adsorbing metal nanoparticles on the inner wall of a hollow optical fiber by using the bridging characteristic of 3-Aminopropyltrimethoxysilane (APTMS) molecules;
in the laser processing process, a cylindrical lens is used for generating an elliptical light spot, the elliptical light spot is parallel to the long axis of the optical fiber at the focus, and the local area is processed to the maximum extent to generate an even SERS structure.
6. The method of claim 5, wherein a uniform and relatively long length volumetric SERS structure is fabricated on the inner wall of the hollow core fiber.
7. The method as claimed in claim 5, wherein the plasmonic micro-nano structures of different surface morphologies are processed by automatically controlling the laser power, the speed of the hollow core fiber's straight and rotational.
8. The SERS microcavity structure based on the inner wall of the hollow-core optical fiber is characterized in that three-dimensional SERS is arranged on the inner wall of the hollow-core optical fiber.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040150818A1 (en) * | 1999-05-17 | 2004-08-05 | Armstrong Robert L. | Optical devices and methods employing nanoparticles, microcavities, and semicontinuous metal films |
| CN1815197A (en) * | 2006-02-24 | 2006-08-09 | 清华大学 | Photon crystal optical-fiber probe sensor based on nano grain surface increasing Raman spectrum |
| WO2008062634A1 (en) * | 2006-11-22 | 2008-05-29 | Nano Craft Technologies Co. | Three-dimensional microstructure, method for manufacturing the microstructure, and apparatus for manufacturing the microstructure |
| WO2011037533A1 (en) * | 2009-09-25 | 2011-03-31 | Nanexa Ab | Sers device |
| US20130171667A1 (en) * | 2010-06-09 | 2013-07-04 | Agency For Science, Technology And Research | Photonic crystal fiber sensor |
| US20190262949A1 (en) * | 2016-08-04 | 2019-08-29 | Spi Lasers Uk Limited | Apparatus and Method For Laser Processing A Material |
| CN112179889A (en) * | 2020-09-15 | 2021-01-05 | 北京工业大学 | Optical feedback device and method based on hollow fiber SERS detection |
| CN215449094U (en) * | 2021-01-13 | 2022-01-07 | 北京工业大学 | Preparation device for SERS microcavity structure |
-
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- 2021-01-13 CN CN202110045821.7A patent/CN112782268A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040150818A1 (en) * | 1999-05-17 | 2004-08-05 | Armstrong Robert L. | Optical devices and methods employing nanoparticles, microcavities, and semicontinuous metal films |
| CN1815197A (en) * | 2006-02-24 | 2006-08-09 | 清华大学 | Photon crystal optical-fiber probe sensor based on nano grain surface increasing Raman spectrum |
| WO2008062634A1 (en) * | 2006-11-22 | 2008-05-29 | Nano Craft Technologies Co. | Three-dimensional microstructure, method for manufacturing the microstructure, and apparatus for manufacturing the microstructure |
| WO2011037533A1 (en) * | 2009-09-25 | 2011-03-31 | Nanexa Ab | Sers device |
| US20130171667A1 (en) * | 2010-06-09 | 2013-07-04 | Agency For Science, Technology And Research | Photonic crystal fiber sensor |
| US20190262949A1 (en) * | 2016-08-04 | 2019-08-29 | Spi Lasers Uk Limited | Apparatus and Method For Laser Processing A Material |
| CN112179889A (en) * | 2020-09-15 | 2021-01-05 | 北京工业大学 | Optical feedback device and method based on hollow fiber SERS detection |
| CN215449094U (en) * | 2021-01-13 | 2022-01-07 | 北京工业大学 | Preparation device for SERS microcavity structure |
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