CN109554666B - A kind of preparation method of conical fiber SERS probe - Google Patents
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
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Abstract
The invention discloses a kind of preparation methods of conical fiber SERS probe, are related to Surface Enhanced Raman Scattering Spectrum field.The preparation method includes: the optical fiber conical surface that noble metal nano film is plated on to conical fiber structure；Using laser coupled unit, couple femtosecond laser in the conical fiber for being coated with noble metal nano film；The femtosecond laser transmitted in conical fiber structure interacts with the noble metal nano film for being plated on the optical fiber conical surface, the laser energy of noble metal nano film absorption femtosecond laser is simultaneously converted to self heat, noble metal nano film experience insulation high-temperature annealing process, to form the noble metal nano particles of dispersion in the optical fiber conical surface, the preparation of optical fiber SERS probe is realized.Femtosecond laser preparation method provided by the present invention is able to solve the problem of existing continuous light prepares the photo-thermal accumulation or damage that face when optical fiber SERS probe；And transmitted by coupling femtosecond laser in optical fiber, solve the problems, such as that existing femtosecond laser technology is difficult to prepare conical fiber SERS probe.
Description
Technical field
The present invention relates to Surface Enhanced Raman Scattering Spectrum fields, more particularly to a kind of system of conical fiber SERS probe
Preparation Method.
Background technique
It is logical that optical fiber surface, which enhances Raman scattering (surface enhanced Raman scattering, SERS) probe,
It crosses and prepares noble metal nano structure or particle in optical fiber surface and formed, SERS spectra technology is mutually tied with optical fiber sensing technology
It closes, there is Raman detection high sensitivity, reproducible, strong antijamming capability, low in cost and long-range, in-situ Raman detection etc.
Advantage shows important application prospect in fields such as biomedicine, life science, chemical reaction monitorings.
The preparation of optical fiber SERS probe is the key that realize highly sensitive detection.Currently, induced with laser method is to prepare optical fiber
A kind of common method of SERS probe.For example, Jilin University Xu Weiqing, Tsinghua University Yang Chang happiness etc. has developed laser-induced chemical
Sedimentation (Langmuir, 2008,24:4394；Langmuir,2011,27:4623；CN200910135729), by by laser
It is coupled in optical fiber, is transmitted in the reaction solution containing reducing agent and soluble precious-metal salt through optical fiber, utilizes induced with laser
Redox reaction can realize noble metal nano particles in the deposition of fiber end face, to form optical fiber SERS probe.Due to
The laser used in this method is continuous laser, and when carrying out probe preparation, there are light thermal buildup issue, Yi Yinqi nano particles
Between reunion and damage；And the nanoparticle size being prepared is larger, pattern is not easy to control, to influence SERS enhancing effect
Fruit.
A kind of induced with laser self-assembly method is disclosed in patent of invention CN201510692551, by by laser through optical fiber coupling
Merging is transmitted in noble metal nano particles colloidal sol, utilizes the photo-thermal effect and electromagnetism phase of noble metal nano particles under induced with laser
Interaction, can be in the assembling of optical fiber conical surface realization pattern, the more uniform noble metal nano particles of size.Although this method can be compared with
Big degree solves the problems, such as the pattern of optical fiber conical surface noble metal nano particles, dimensional homogeneity, but due to equally using continuous laser
It is irradiated, it will be apparent that heat accumulation and thermal diffusion still will lead to the reunion between noble metal nano particles and even damage.
In recent years, it has been proposed that a kind of method (such as Optics for preparing SERS substrate using femtosecond laser revulsion
Letters, 2010,35:2937, Sensors andActuators B, 2018,272:485).By in precious metal salt solution
Femtosecond laser is focused to the optical fiber conical surface on substrate by bottom holding plane substrate (such as Si, SiO2, PMMA), and is aided with quickly
Laser scanning can realize that noble metal nano particles are precipitated in the substrate optical fiber conical surface using the multiphoton -effect that femtosecond laser induces,
To form SERS substrate；The method of this femtosecond laser processing can effectively avoid photo-thermal diffusion and accumulation, be conducive to be formed smaller
Size, the noble metal nano structure of greater density distribution, improve SERS detection sensitivity.But space-focusing coupling in this method
It closes and the working method that quickly scans is not particularly suited for the heavy of noble metal nano particles on curved surface (such as the optical fiber conical surface, side)
Product；In addition, the multiphoton -effect that femtosecond laser induces in precious metal salt solution belongs to nonlinear optical effect, the list of required laser
Pulse energy is higher, it usually needs uses amplifying stage, increases preparation cost.To sum up, existing conical fiber SERS probe preparation is deposited
Photo-thermal accumulation or damage problem and femtosecond laser processing method in the preparation of such as continuous light are difficult to prepare conical fiber
The problem of SERS probe.
Summary of the invention
The purpose of the present invention is to provide a kind of conical fiber SERS probe preparation methods, to solve existing continuous light preparation
The photo-thermal accumulation faced when optical fiber SERS probe or damage problem and existing femtosecond laser processing method are difficult to prepare conical fiber
The problem of SERS probe.
To achieve the above object, the present invention provides following schemes:
A kind of preparation method of conical fiber SERS probe, comprising:
Noble metal nano film is plated on to the optical fiber conical surface of conical fiber structure；Using laser coupled unit, femtosecond is swashed
It is optically coupled in the conical fiber for being coated with the noble metal nano film, forms conical fiber SERS probe；The conical fiber
The femtosecond laser transmitted in structure interacts with the noble metal nano film for being plated on the optical fiber conical surface, described expensive
Metal nanometer thin film absorbs the laser energy of the femtosecond laser and is converted to self heat, the noble metal nano film experience
It is insulated high-temperature annealing process, to form the noble metal nano particles of dispersion in the optical fiber conical surface, realizes the system of optical fiber SERS probe
It is standby.
Optionally, the thicknesses of layers of the noble metal nano film is less than 20nm.
Optionally, described to utilize laser coupled unit, it couples femtosecond laser to and is coated with the noble metal nano film
In conical fiber, formed before conical fiber SERS probe, further includes:
Adjust the power and repetition rate of the femtosecond laser.
Optionally, the fiber optic materials of the conical fiber structure be common silica fibre material, polymer light fiber material or
Ti:Sapphire laser fiber optic materials；The optical fiber type of the conical fiber structure is single mode optical fiber, multimode fibre or D-type optical fiber.
Optionally, layers of chrome, the thickness of the layers of chrome are coated between the noble metal nano film and the optical fiber conical surface
For 1nm, the layers of chrome is used to increase the adhesive force of the noble metal nano film Yu the optical fiber conical surface.
Optionally, the material of the noble metal nano film is the metal material with larger surface plasma resonance characteristic
Material, the ingredient of the metal material are gold, silver, platinum or copper.
Optionally, the laser coupled unit determines that the femtosecond swashs according to the different output interfaces of the femtosecond laser
Coupled modes between light and the conical fiber structure；The coupled modes include spatial coupling and the direct coupling of optical fiber
Conjunction mode.
Optionally, the preparation method of the conical fiber structure includes fused biconical taper method and HF etch.
Optionally, the plated film mode of the noble metal nano film includes vacuum magnetic-control sputtering method and thermal evaporation plated film
Method.
The specific embodiment provided according to the present invention, the invention discloses following technical effects: the present invention provides one kind
The preparation method of conical fiber SERS probe, using on the femtosecond laser and the optical fiber conical surface transmitted in conical fiber structure
Noble metal nano film directly intercouples effect, forms optical fiber SERS probe, effectively overcomes traditional continuous laser expensive when inducing
The photo-thermal of metal Nano structure accumulates or the problems such as photothermal injury, is conducive to improve SERS detection sensitivity；Simultaneously as being omitted
The step of noble metal nano particles is precipitated in precious metal salt solution under Multiphoton Absorbtion effect, is not necessarily to very high single laser pulse energy
Amount solves in current femtosecond laser processing since space-focusing and quick scanning work mode are difficult to realize conical fiber SERS
The difficulty of probe preparation, reduces preparation cost, has application value.
Detailed description of the invention
It in order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, below will be to institute in embodiment
Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only some implementations of the invention
Example, for those of ordinary skill in the art, without any creative labor, can also be according to these attached drawings
Obtain other attached drawings.
Fig. 1 is the preparation method flow chart of conical fiber SERS probe provided by the present invention；
Fig. 2 is conical fiber SERS probe preparation facilities structural schematic diagram provided by the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
The object of the present invention is to provide a kind of preparation methods of conical fiber SERS probe, to solve existing continuous light preparation
The photo-thermal accumulation faced when optical fiber SERS probe or damage problem and existing femtosecond laser processing method are difficult to prepare conical fiber
The problem of SERS probe.
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing and specific real
Applying mode, the present invention is described in further detail.
As shown in Figure 1, the present invention provides a kind of preparation methods of conical fiber SERS probe, based on as shown in Figure 2
Preparation facilities.
Step 101: noble metal nano film is plated on to the optical fiber conical surface of conical fiber structure；The taper of the optical fiber conical surface
It can be a variety of geometries such as single cone, bipyramid, combination tapered.
Step 102: utilizing laser coupled unit, couple femtosecond laser to the taper for being coated with the noble metal nano film
In optical fiber structure, conical fiber SERS probe is formed.
The present invention prepares conical fiber structure using a variety of methods such as fused biconical taper method, HF etch；On the optical fiber conical surface
Noble metal nano film is plated, thicknesses of layers is from several nanometers to 20 nanometer；Open femtosecond laser light source 1, the femtosecond laser light
Source issues femtosecond laser, and the femtosecond laser passes through laser coupled unit 2, realizes the femtosecond laser and the conical fiber
Efficient, stable coupling between SERS probe；By modes such as the power of adjusting femtosecond laser light source and repetition rates, in femtosecond
Under the insulation high-temperature annealing process of laser, noble metal nano film is converted into the noble metal nano particles of dispersion, to realize cone
The preparation of shape optical fiber SERS probe.
In practical applications, the thicknesses of layers of the noble metal nano film is less than 20nm.
In practical applications, described to utilize laser coupled unit, it couples femtosecond laser to and is coated with the noble metal nano
In the conical fiber of film, formed before conical fiber SERS probe, further includes:
Adjust the power and repetition rate of the femtosecond laser.
In practical applications, the fiber optic materials of the conical fiber structure are common silica fibre material, polymer optical fiber
Material or Ti:Sapphire laser fiber optic materials；The optical fiber type of the conical fiber structure is single mode optical fiber, multimode fibre or D-type optical fiber.
In practical applications, layers of chrome, the layers of chrome are coated between the noble metal nano film and the optical fiber conical surface
Thickness be 1nm, the layers of chrome is used to increase the adhesive force of the noble metal nano film Yu the optical fiber conical surface.
In practical applications, the material of the noble metal nano film is with larger surface plasma resonance characteristic
Metal material, the ingredient of the metal material are gold, silver, platinum or copper.
In practical applications, the laser coupled unit is according to the different output interfaces of the femtosecond laser, determine described in
Coupled modes between femtosecond laser and the conical fiber structure；The coupled modes include spatial coupling and optical fiber
Direct coupling system.
In practical applications, the preparation method of the conical fiber structure includes fused biconical taper method and HF etch.
In practical applications, the plated film mode of the noble metal nano film includes vacuum magnetic-control sputtering method and thermal evaporation
Coating method.
The present invention prepares optical fiber SERS probe using femtosecond laser revulsion, effectively overcomes traditional continuous laser expensive when inducing
The photo-thermal of metal Nano structure accumulates or the problems such as photothermal injury；Meanwhile this method is easy to operate, can be formed in the optical fiber conical surface
The noble metal nano particles that small size, greater density are distributed are conducive to improve SERS detection sensitivity.
The present invention is direct by the noble metal nano particles film using the femtosecond laser and the optical fiber conical surface transmitted in optical fiber
The method for interacting and forming optical fiber SERS probe efficiently solves in the processing of current femtosecond laser due to space-focusing and fast
Fast scanning work mode is difficult to realize the difficulty of conical fiber SERS probe preparation.
Compared with femtosecond laser preparation SERS FLOOR method of the tradition based on Multiphoton Absorbtion effect, the present invention proposes benefit
The mechanism of dispersion noble metal nano particles is formed under high annealing with noble metal nano film to prepare optical fiber SERS probe, pole
The big energy for reducing required femtosecond laser when preparation, conducive to cost is reduced.
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with other
The difference of embodiment, the same or similar parts in each embodiment may refer to each other.
Used herein a specific example illustrates the principle and implementation of the invention, and above embodiments are said
It is bright to be merely used to help understand method and its core concept of the invention；At the same time, for those skilled in the art, foundation
Thought of the invention, there will be changes in the specific implementation manner and application range.In conclusion the content of the present specification is not
It is interpreted as limitation of the present invention.
Claims (9)
1. a kind of preparation method of conical fiber SERS probe characterized by comprising
Noble metal nano film is plated on to the optical fiber conical surface of conical fiber structure；
It using laser coupled unit, couples femtosecond laser in the conical fiber for being coated with the noble metal nano film, is formed
Conical fiber SERS probe；The femtosecond laser transmitted in the conical fiber structure and your gold for being plated on the optical fiber conical surface
Belong to nano thin-film to interact, the laser energy of femtosecond laser described in the noble metal nano film absorption is simultaneously converted to certainly
Body heat, the noble metal nano film experience insulation high-temperature annealing process, to form the noble metal of dispersion in the optical fiber conical surface
Nano particle realizes the preparation of optical fiber SERS probe.
2. the preparation method of conical fiber SERS probe according to claim 1, which is characterized in that the noble metal nano
The thicknesses of layers of film is less than 20nm.
3. the preparation method of conical fiber SERS probe according to claim 1, which is characterized in that described to utilize laser coupling
Unit is closed, is coupled femtosecond laser in the conical fiber for being coated with the noble metal nano film, conical fiber SERS is formed and visits
Before needle, further includes:
Adjust the power and repetition rate of the femtosecond laser.
4. the preparation method of conical fiber SERS probe according to claim 1, which is characterized in that the conical fiber knot
The fiber optic materials of structure are common silica fibre material, polymer light fiber material or Ti:Sapphire laser fiber optic materials；The conical fiber knot
The optical fiber type of structure is single mode optical fiber, multimode fibre or D-type optical fiber.
5. the preparation method of conical fiber SERS probe according to claim 1, which is characterized in that the noble metal nano
Layers of chrome is coated between film and the optical fiber conical surface, the thickness of the layers of chrome is 1nm, and the layers of chrome is for your gold to be increased
Belong to the adhesive force of nano thin-film and the optical fiber conical surface.
6. the preparation method of conical fiber SERS probe according to claim 1, which is characterized in that the noble metal nano
The material of film is the metal material with larger surface plasma resonance characteristic, the ingredient of the metal material be gold, silver,
Platinum or copper.
7. the preparation method of conical fiber SERS probe according to claim 1, which is characterized in that the laser coupled list
Member determines the coupling between the femtosecond laser and the conical fiber structure according to the different output interfaces of the femtosecond laser
Mode；The coupled modes include spatial coupling and Direct couple mode.
8. the preparation method of conical fiber SERS probe according to claim 1, which is characterized in that the conical fiber knot
The preparation method of structure includes fused biconical taper method and HF etch.
9. the preparation method of conical fiber SERS probe according to claim 1, which is characterized in that the noble metal nano
The plated film mode of film includes vacuum magnetic-control sputtering method and thermal evaporation coating method.
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