CN107561057B - Dual-enhancement Raman detection system with local surface plasma amplifier - Google Patents
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Abstract
The invention discloses a dual-enhancement Raman detection system with a local surface plasma amplifier, which comprises an excitation light source, an optical fiber coupler, a detection probe, the local surface plasma amplifier, a filter and a detector, wherein the excitation light source is connected with the optical fiber coupler; the local surface plasma amplifier is arranged, so that the problem that a weak Raman optical signal cannot be amplified due to spontaneous radiation noise of the amplifier is solved; the energy transfer path of the surface plasmon resonance optical amplifier is 'excitation laser' → 'local surface plasmon' → 'signal light', and when the intensity of the raman signal light is far smaller than that of the excitation laser, the signal light can obtain energy from the surface plasmon to be amplified; because the local plasma has no energy level structure, the amplifier can not generate spontaneous radiation light when being excited by laser, and can be equivalent to an ideal amplifier with extremely low noise (extremely low input signal threshold), so that the amplifier can amplify extremely weak Raman signals.
Description
Technical Field
The invention relates to the field of Raman detection, in particular to a dual-enhancement Raman detection system with a local surface plasma amplifier.
Background
As is known to those skilled in the art, light irradiated on a substance undergoes elastic scattering, in which the scattered light is of the same composition as the wavelength of the excitation light, and inelastic scattering, in which the scattered light has a composition longer and shorter than the wavelength of the excitation light, called raman effect, and the spectrum obtained is called raman spectrum. The Raman spectrum belongs to molecular vibration spectrum, is a fingerprint of substance molecules, and can be used for accurately and qualitatively identifying samples. The analysis method of Raman spectrum does not need to pretreat the sample, has simple operation and short determination time in the analysis process, is an analysis technology which can simultaneously carry out qualitative and quantitative analysis on the sample, has extremely wide application prospect, but has the defect of lower sensitivity.
Surface-enhanced Raman spectroscopy (SERS for short) is a high-sensitivity spectroscopic analysis technique developed in the 90 s of the 20 th century along with the development of nanotechnology. Like raman spectroscopy, SERS can be used to identify samples accurately and qualitatively; SERS has ultrahigh analysis sensitivity, is improved by about 6-10 orders of magnitude compared with common Raman analysis sensitivity, and can analyze research objects which are as small as single molecules and as large as cell level.
However, metal nanostructures (metal nanospheres, nanorods, nanowires, etc.) are generally used to enhance raman spectroscopy; generally, the metal nano structure only has an enhancement effect on light waves in a certain frequency domain range; the raman spectrum of the substance to be measured has a certain width, and a part of the raman frequency domain generally falls outside the range of the frequency domain that the metal nanostructure can enhance. In this case, the enhancement effect on the high-frequency raman spectrum of the substance to be measured is reduced, which puts an extremely high demand on the sensitivity of the photodetector in the subsequent optical path.
On the other hand, the typical raman characteristic peak of the substance to be measured is usually at some specific raman peak position (i.e. at different wavelengths). The traditional raman spectrum detection method is to detect a full spectrum, that is, a raman spectrum carrying information of a substance to be detected enters a raman spectrometer, so as to obtain a raman spectrum signal, and then data processing is performed to obtain information of the substance to be detected. The Raman spectrometer has the advantages of complex structure, larger volume and higher price.
In order to solve the above problems, optical amplifiers are proposed to amplify and then detect raman signal light, and the current optical amplifiers mainly include EDFAs and fiber raman amplifiers, these amplifiers have spontaneous emission noise, the lowest threshold of the input signal is about-40 dBm (100nw), while the power of the excitation light source in the actual raman spectrum detection application is generally small, and generally under 1w laser excitation, the signal intensity of raman scattered light is usually several 10pw to 1nw orders, which is much smaller than the threshold of these optical amplifiers, and amplification cannot be realized.
Therefore, in order to solve the above problems, a dual-enhancement raman detection system is needed, which can effectively detect weak raman signal light for a low-power excitation light source, and has a simple and compact structure, high detection accuracy, low cost, and is beneficial to popularization.
Disclosure of Invention
In view of this, the present invention aims to overcome the defects in the prior art, and provide a dual-enhancement raman detection system, which can effectively detect weak raman signal light for a low-power excitation light source, and has the advantages of simple and compact structure, high detection accuracy, low cost, and easy popularization.
The dual-enhancement Raman detection system comprises an excitation light source, an optical fiber coupler, a detection probe, a local surface plasma amplifier, a filter and a detector;
an excitation light source for generating excitation light and transmitting the excitation light to the optical fiber coupler through an optical fiber;
the optical fiber coupler is used for respectively coupling the excitation light emitted by the excitation light source and the Raman signal light generated and returned by the detection probe, and transmitting the coupled Raman signal light to the local surface plasma amplifier through an optical fiber for amplification;
the input end of the detection probe is connected with the output end of the optical fiber coupler through an optical fiber and is used for generating and collecting Raman signal light of a substance to be detected under the excitation of excitation light, and the working surface of the detection probe is provided with a first metal nano structure to realize primary Raman surface enhancement;
the local surface plasma amplifier is internally provided with a second metal nano structure for generating local plasma, and secondary Raman signal amplification is realized on the passing Raman signal light transmission energy through the local plasma;
the input end of the filter is connected with the output end of the local surface plasma amplifier and is used for filtering light with the same wavelength as the excitation light in the signals and obtaining Raman optical signals with separated wavelengths; the local surface plasma amplifier comprises a waveguide structure and a second metal nano structure arranged in the waveguide structure, wherein the interior of the waveguide structure is in a vacuum state;
and the detector is used for detecting the Raman signal light coming out of the filter and converting the Raman signal light into an electric signal for output processing.
Further, the wavelengths corresponding to the absorption spectrum of the second metal nanostructure include an excitation light wavelength and a raman signal light wavelength.
Further, the filters and the detectors are respectively arranged in a plurality of one-to-one correspondence.
Furthermore, the output end of the excitation light source is also connected with the input end of the local surface plasma amplifier through an optical fiber.
Further, the waveguide is a tubular hollow waveguide and is composed of a hollow cavity and a tubular medium reflecting layer on the periphery, the second metal nano structure is metal nano particles positioned on the inner wall of the tubular medium reflecting layer, the metal nano particles form a cylindrical shell-core structure, and the average particle diameter of the nano particles is d1The distance between the nanoparticles is g1The length of the cylindrical shell-core structure is h1D is said120-100nm, g1Is 1-10nm, h1Is 1-100 um.
Further, the waveguide is a tubular hollow waveguide and is composed of a hollow cavity and a tubular medium reflecting layer on the periphery, the second metal nano structure is a thin film which is located in the central layer and distributed along the radial direction, periodic round holes are formed in the thin film, and the diameter of each round hole is d2The distance between the edges of adjacent circular holes is g2The thickness of the film is h2D is said220-100nm, g2Is 1-10nm, h2Is 1-100 um.
Further, the waveguide is a tubular hollow waveguide and is composed of a hollow cavity and a peripheral tubular medium reflecting layer, the second metal nanostructure is a composite film which is positioned in the high-refractive-index central layer and distributed along the radial direction, the composite film comprises a base film composed of carbon nanotubes and metal nanoparticles attached to the base film, and the average particle diameter of the metal nanoparticles is d3The distance between adjacent nanoparticles is g3The thickness of the base film is h3D is said320-100nm, g3Is 1-10nm, h3Is 1-100 um.
The invention has the beneficial effects that: according to the dual-enhancement Raman detection system disclosed by the invention, the local surface plasma amplifier is arranged, so that the problem that a weak Raman optical signal cannot be amplified due to spontaneous radiation noise of the amplifier is solved. The traditional optical amplifier has a minimum input signal threshold (usually 100nw) because of spontaneous radiation of a working medium, and when 1W laser is adopted for excitation, the intensity of a Raman optical signal is about 10pw to 1nw, which is smaller than the threshold of the traditional optical amplifier, so that a weak Raman optical signal cannot be amplified; the energy transfer path of the surface plasmon resonance optical amplifier is 'excitation laser' → 'local surface plasmon' → 'signal light', and when the intensity of the raman signal light is far less than that of the excitation laser, the raman signal light can obtain energy from the surface plasmon to be amplified; because the local plasma has no energy level structure, the local plasma can not generate spontaneous radiation light when being excited by laser, and the local plasma can be equivalent to an ideal amplifier with extremely low noise (extremely low input signal threshold), so that the local plasma can amplify very weak Raman signals; the device has the advantages of simple and compact structure, high detection precision, lower cost and contribution to popularization.
Drawings
The invention is further described below with reference to the following figures and examples:
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic view of the structure of the inspection probe of the present invention;
FIG. 3 is a schematic diagram of the structure of the filter and the corresponding typical Raman characteristic peak in the present invention;
FIG. 4 is a graph of the absorption spectrum corresponding to a second metal nanostructure of the present invention;
FIG. 5 is a schematic diagram of a first structure of a localized surface plasmon amplifier in accordance with the present invention;
FIG. 6 is a schematic diagram of a second structure of a localized surface plasmon amplifier in accordance with the present invention;
FIG. 7 is a third structural diagram of a localized surface plasmon amplifier in accordance with the present invention.
Detailed Description
Fig. 1 is a schematic structural diagram of the present invention, fig. 2 is a schematic structural diagram of a detection probe in the present invention, fig. 3 is a schematic structural diagram of a filter in the present invention and a schematic structural diagram of a corresponding typical raman characteristic peak, fig. 4 is an absorption spectrum corresponding to a second metal nanostructure in the present invention, fig. 5 is a schematic structural diagram of a local surface plasmon amplifier in the present invention, fig. 6 is a schematic structural diagram of a local surface plasmon amplifier in the present invention, fig. 7 is a schematic structural diagram of a local surface plasmon amplifier in the present invention, as shown in the drawings, a dual-enhancement raman detection system in the present embodiment includes an excitation light source 1, an optical fiber coupler 2, a detection probe 3, a local surface plasmon amplifier 4, a filter 5 and a detector 6;
an excitation light source 1 for generating excitation light and transmitting the excitation light to the optical fiber coupler 2 through an optical fiber; the excitation light source 1 can be an existing low-power laser light source, and is guaranteed to be suitable for practical application and popularization; the intensity of the Raman signal is 2-3 orders of magnitude smaller than the threshold value of a common amplifier, and the adoption of a high-power excitation light source has the following disadvantages that on one hand, a continuous laser with the output power of 100-1000W is expensive and large in size, and is not suitable for being used as an instrument light source; on the other hand, the high-power laser can easily damage the sample to be detected, especially biomolecules and the like; in addition, the light source energy increases, and the noise caused by the power fluctuation of the light source increases.
The optical fiber coupler 2 is used for respectively coupling the excitation light emitted by the excitation light source 1 and the Raman signal light generated and returned by the detection probe 3, and transmitting the coupled Raman signal light to the local surface plasma amplifier 4 through an optical fiber for amplification; the optical signals are divided and combined through the optical fiber coupler 2, and Raman signal light returned from the detection probe 3 is collected;
the input end of the detection probe 3 is connected with the output end of the optical fiber coupler 2 through an optical fiber and is used for generating and collecting Raman signal light of a substance 11 to be detected under the excitation of excitation light, and the working surface of the detection probe is provided with a first metal nano structure 7 to realize primary Raman surface enhancement; the first metal nano structure 7 can be a silver or gold nano particle structure, and the first metal nano structure 7 for attaching the substance to be detected on the working surface realizes primary Raman surface enhancement under the action of the exciting light to obtain Raman signal light amplified by a primary signal;
the local surface plasma amplifier 4 is internally provided with a second metal nano structure 8 for generating local plasma, and secondary Raman signal amplification is realized by the local plasma on the passing Raman signal light transmission energy; the second metal nanostructure 8 can be excited by the Rayleigh scattered light generated by the interaction of the excitation light with the first metal nanostructure 7 at the detection probe 3, the local surface plasmon amplifier 4 does not need a new laser light source as the excitation light, the Rayleigh scattering light (the same as the original laser wavelength) reflected by the fiber Raman probe is used as exciting light to excite surface plasma, and the energy is transferred to Raman light through surface plasma to realize secondary Raman signal amplification, because Raman scattered light is 2-3 orders of magnitude smaller than Rayleigh scattered light, the energy transfer path is "excitation laser" → "local surface plasmon" → "raman signal light", where "local surface plasmon" corresponds to an intermediate transfer link which transfers the energy of strong light (rayleigh scattered light) to weak light (raman light); because the local plasma has no energy level structure, the local plasma can not generate spontaneous radiation when being excited by laser, and the local plasma is equivalent to an ideal amplifier with extremely low noise and can amplify a very weak Raman signal; the local surface plasma amplifier 4 comprises a waveguide structure and a second metal nano structure 8 arranged in the waveguide structure, wherein the interior of the waveguide structure is in a vacuum state; the interior of the waveguide is vacuumized to ensure that no Raman scattering exists in the waveguide structure, noise interference is avoided, low-noise amplification of Raman signal light is realized, and the detection precision is further improved;
a filter 5, the input end of which is connected with the output end of the local surface plasma amplifier 4, for filtering rayleigh scattered light with the same wavelength as the excitation laser in the signal, and extracting raman scattered light within a specific wavelength (range) to form a series of raman optical signals with separated wavelengths; as shown in fig. 3, the structure of the filter can be equivalent to a single-input cascade multi-output band-pass filter, each band-pass filter only extracts the raman light with a specific wavelength and irradiates the raman light to a corresponding detector, and the light with other wavelengths can pass through the band-pass filter without loss; for a specific substance, the qualitative and quantitative analysis can be carried out only by measuring a specific spectral line without measuring all Raman spectra; thus, for different substances, different filter combinations are required to filter out a particular spectral line. Compared with the traditional Raman spectrometer, the Raman spectrometer has the advantages that the cost is greatly reduced, the size can be very small, and even one chip can be realized; it features small size, low cost and easy popularization.
A detector 6 for detecting the raman signal light from the filter 5 and converting the detected signal into an electric signal for output processing; the qualitative and quantitative analysis of the substance by the signal detected by the detector 6 is prior art and will not be described in detail here.
In this embodiment, the wavelengths corresponding to the absorption spectrum of the second metal nanostructure 8 include an excitation light wavelength and a raman signal light wavelength; as shown, i.e. the excitation light wavelength λpumpAnd raman signal light wavelength lambdasignalAre all positioned in the wave band corresponding to the absorption spectrum of the second metal nano structure 8; the energy can be smoothly transmitted to the signal light.
In this embodiment, the filters 5 and the detectors 6 are respectively provided in a plurality and in one-to-one correspondence; the passing wavelength corresponding to the single filter 5 is a typical characteristic peak corresponding to the substance, and a plurality of typical characteristic peaks of the substance are detected, so that the detection precision is improved; the substance generally has a plurality of characteristic peaks, and the qualitative and quantitative determination of the substance can be realized by analyzing the plurality of characteristic peaks.
In this embodiment, the output end of the excitation light source 1 is further connected with the input end of the local surface plasma amplifier 4 through an optical fiber; further improving the surface plasma intensity of the second metal nanometer, improving the energy transfer efficiency and being beneficial to amplifying the Raman signal light intensity.
In this embodiment, the waveguide structure has a refractive index of n1 Hollow cavity 9 and refractive index n of 12The hollow waveguide is composed of a tubular reflecting cladding layer 10 with the thickness larger than 1, and the second metal nano structure 8 is a metal nano particle positioned on the inner wall of the tubular medium reflecting layer 10And the metal nanoparticles form a cylindrical shell-core structure, the average particle diameter of the nanoparticles is d1The distance between the nanoparticles is g1The length of the cylindrical shell-core structure is h1D is said120-100nm, g1Is 1-10nm, h1Is 1-100 um. The inside of the shell-core structure is gold or silver noble metal nano particles, and the outer surface of the shell-core structure is coated with a layer of oxidation resistant film with the thickness of several nanometers, so that the metal nano particles can be protected from being oxidized for a long time and high Raman enhancement activity can be kept; the shell-core structure can be manufactured by a chemical synthesis method, and the size of metal nano particles and the thickness of a protective film can be changed and ensured by adjusting the time of chemical reaction and the formula of a solution; in addition, an atomic layer coating instrument can be used for coating a protective layer on the purchased finished metal nanoparticles to realize the core-shell structure.
In another embodiment, the waveguide structure is composed of a refractive index n1 Hollow cavity 9 and refractive index n of 12The hollow waveguide is composed of a tubular reflecting cladding 10 larger than 1, the second metal nano structure 8 is a film which is positioned in the hollow cavity 9 and distributed along the radial direction, periodic round holes are formed in the film, and the diameter of each round hole is d2The distance between the edges of adjacent circular holes is g2The thickness of the film is h2D is said220-100nm, g2Is 1-10nm, h2Is 1-100 um; the metal nanostructures 8 may be processed using existing nano-processing methods to ensure their accuracy; specifically, the process assurance such as "nanoimprint", "nanolithography", or Focused Ion Beam (FIB) direct writing may be employed. The second metal nanostructure 8 may also be directly grown by a material chemical method, and different geometric dimensions may be obtained by adjusting the growth process parameters, so as to ensure the parameter accuracy of the metal nanostructure 8.
In another embodiment, the waveguide structure is composed of a refractive index n1 Hollow cavity 9 and refractive index n of 12A hollow waveguide composed of a tubular reflective cladding 10 larger than 1, the second metal nanostructure 8 is a composite film radially distributed in the hollow cavity 9, and the composite film comprises carbon nano-particlesA base film of tubes 12 and metal nanoparticles attached to the base film, the metal nanoparticles having an average particle diameter d3The distance between adjacent nanoparticles is g3The thickness of the base film is h3D is said320-100nm, g3Is 1-10nm, h3Is 1-100 um. The second metal nanostructure 8 is manufactured by the following steps: in the first step, the carbon nanotubes 12 are grown by Chemical Vapor Deposition (CVD); secondly, preparing the carbon nano tube 12 into a suspension, and preparing the carbon nano tube base film by adopting a vacuum filtration method, a titration drying method or a centrifugal machine spin coating method; thirdly, preparing chemical silver sol or gold sol, coating the chemical silver sol or gold sol on the carbon nano tube base film, and drying to form the second metal nano structure 8; or sputtering a layer of noble metal film on the carbon nano tube base film, and then growing into the metal nano particles by adopting a high-temperature annealing method. In the three steps, a large number of process tests are required to determine process parameters so as to ensure the manufacturing accuracy of the geometric parameters of the second metal nanostructure 8.
This example describes three ways of implementing the second metallic nanostructures 8, which can be used either alone or in combination to implement the localized surface plasmon amplifier of the present invention.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (7)
1. A dual-enhancement Raman detection system with a local surface plasma amplifier is characterized in that: the device comprises an excitation light source, an optical fiber coupler, a detection probe, a local surface plasma amplifier, a filter and a detector;
an excitation light source for generating excitation light and transmitting the excitation light to the optical fiber coupler through an optical fiber;
the optical fiber coupler is used for respectively coupling the excitation light emitted by the excitation light source and the Raman signal light generated and returned by the detection probe, and transmitting the coupled Raman signal light to the local surface plasma amplifier through an optical fiber for amplification;
the input end of the detection probe is connected with the output end of the optical fiber coupler through an optical fiber and is used for generating and collecting Raman signal light of a substance to be detected under the excitation of excitation light, and the working surface of the detection probe is provided with a first metal nano structure to realize primary Raman surface enhancement;
the local surface plasma amplifier is internally provided with a second metal nano structure for generating local plasma, and secondary Raman signal amplification is realized on the passing Raman signal light transmission energy through the local plasma; the local surface plasma amplifier comprises a waveguide structure and a second metal nano structure arranged in the waveguide structure, wherein the interior of the waveguide structure is in a vacuum state;
the input end of the filter is connected with the output end of the local surface plasma amplifier and is used for filtering light with the same wavelength as the excitation light in the signals and obtaining Raman optical signals with separated wavelengths;
and the detector is used for detecting the Raman signal light coming out of the filter and converting the Raman signal light into an electric signal for output processing.
2. The dual enhanced raman detection system according to claim 1, wherein: the absorption spectrum of the second metal nanostructure includes an excitation light wavelength and a raman signal light wavelength.
3. The dual enhanced raman detection system according to claim 2, wherein: the filters and the detectors are respectively arranged in a plurality of one-to-one correspondence.
4. The dual enhanced raman detection system according to claim 1, wherein: the output end of the excitation light source is also connected with the input end of the local surface plasma amplifier through an optical fiber.
5. The dual enhanced raman detection system according to claim 1, wherein: the waveguide is a tubular hollow waveguide and consists of a hollow cavity and a tubular medium reflecting layer on the periphery, the second metal nano structure is metal nano particles positioned on the inner wall of the tubular medium reflecting layer, the metal nano particles form a cylindrical shell-core structure, and the average particle diameter of the nano particles is d1The distance between the nanoparticles is g1The length of the cylindrical shell-core structure is h1D is said120-100nm, g1Is 1-10nm, h1Is 1-100 um.
6. The dual enhanced raman detection system according to claim 1, wherein: the waveguide is a tubular hollow waveguide and consists of a hollow cavity and a peripheral tubular medium reflecting layer, the second metal nano structure is a film which is positioned in the central layer and radially distributed, periodic round holes are formed in the film, and the diameter of each round hole is d2The distance between the edges of adjacent circular holes is g2The thickness of the film is h2D is said220-100nm, g2Is 1-10nm, h2Is 1-100 um.
7. The dual enhanced raman detection system according to claim 1, wherein: the waveguide is a tubular hollow waveguide and consists of a hollow cavity and a peripheral tubular medium reflecting layer, the second metal nano structure is a composite film which is positioned in the high-refractive-index central layer and is distributed along the radial direction, the composite film comprises a base film consisting of carbon nano tubes and metal nano particles attached to the base film, and the average particle diameter of the metal nano particles is d3The distance between adjacent nanoparticles is g3The thickness of the base film is h3D is said320-100nm, g3Is 1-10nm, h3Is 1-100 um.
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| CN108593624B (en) * | 2018-04-13 | 2021-03-19 | 东南大学 | Multi-wavelength metal plasma resonance structure with enhanced selectivity and preparation method thereof |
| CN109781709B (en) * | 2019-03-19 | 2021-06-01 | 重庆大学 | Optical amplification Raman spectrum detection system based on waveguide structure |
| CN111505474B (en) * | 2020-04-24 | 2021-11-02 | 中国科学院长春光学精密机械与物理研究所 | CO2Laser amplifier upper energy level service life testing device and method |
| TWI750718B (en) * | 2020-07-03 | 2021-12-21 | 國立中興大學 | Signal enhancement structure and manufacturing method thereof |
| CN113418902B (en) * | 2021-03-23 | 2023-10-13 | 重庆大学 | On-chip Raman detection system |
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