CN107290056B - Raman spectrum test macro - Google Patents
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- 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
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Abstract
A kind of tunable Raman spectrum test macro, including the coupling of wide spectrum monochromatization module, optical path and output module and signal detection module, in which: wide spectrum monochromatization module, comprising: supercontinuum source, for exporting wide spectrum exciting light；Monochromatization unit, for wide spectrum exciting light to be filtered into monochromatic light；Optical path coupling and output module, for making monochromatic light exposure to sample surfaces, excitation obtains Raman signal light；Signal detection module is detected for receiving Raman signal light, obtains the Raman spectrum of sample.Monochromatization unit includes grating and the first reflecting mirror, adjusts the deflection angle of grating and the first reflecting mirror relative to supercontinuum source, and the reflection of monochromatic light of different wave length can be changed to the position of diaphragm.Wide spectrum exciting light is provided using supercontinuum source, tunable Raman spectrum of the measurable excitation light wave length and width up to 400~2400nm, there is no need to use expensive and unhandy Wavelength tunable laser, the resonance Raman spectroscopy measurement of wide scope can be conveniently realized.
Description
Technical field
The invention belongs to microspectrograph technical fields, relate more specifically to a kind of Raman spectrum test macro.
Background technique
A kind of characterization technique of the Raman spectrum as the detection material component and lattice vibration of efficient lossless, is widely used
In numerous areas such as physics, chemistry, biological medicine, material science.Resonance Raman spectroscopy technology is the base in normal Raman spectrum
On plinth, using the exciting light to resonate with sample to be tested energy level come Raman emission, the Raman signal of sample to be tested can be made to be total to
Vibration enhances several orders of magnitude.In this way, by measure Raman signal intensity change with the change of excitation wavelength curve (with
Lower abbreviation " resonance profile ") it can be obtained by the associated electrical band structure information of sample to be tested.The present gas generally used,
Ion or pumped solid state laser generally have discrete single or multiple optical maser wavelengths.Therefore test material Raman spectrum is wanted
Resonate profile, generally requires laser that cover larger wave-length coverage, large number of.In addition, will be exactly by Raman light
Spectrum resonates profile to determine the electronic band structure information of material.
Pervious Raman spectrum resonance profile is usually using tunable laser as excitation light source in three grating Ramans
It is measured on spectrometer.Tunable laser, such as ti sapphire laser or dye laser.Three grating Raman spectrometers pass through
Two-stage grating operation to filter out Rayleigh signal light well, and in visible light wave segment limit, is not needed in phase size reduction mode before making
Any trap or sideband optical filter can test the Raman signal down to 5 wave numbers using three grating Raman spectrometers.But
Due to the device efficiencies such as grating and reflecting mirror, the transmitance of the spectral signal of three grating Raman spectrometers is usually only single
The 1/10 of grating Raman spectrometer.
With the progress of science and technology, the filter of the Ramans such as notch filtering light piece and sideband optical filter for different excitation wavelengths
Mating plate is manufactured.Since Raman optical filter is up to 10 to Rayleigh signal light-6Cutoff rate so that being subtracted each other using multistage grating
Mode is unnecessary to filter Rayleigh signal light.Monochromatic light grating spectrograph combination Raman optical filter can also be used to test Raman light
Spectrum signal, and there is very high Signature penetrating rate.Therefore monochromatic light grid Raman spectrometer has become current Raman spectrum test
Mainstream equipment.
But problem is also encountered using the resonance profile of monochromatic light grid Raman spectrometer test Raman spectrum.Conventional Raman
Optical filter can make the s wave and p wave that scatter light only in a certain particular excitation Wavelength design when working normally angle more than it
Operation wavelength moving range it is different and Raman spectrum test cannot be continued to apply to.In this way, the laser of each wavelength
The sideband optical filter that must be equipped with relevant work wavelength could test Raman spectrum using monochromatic light grating spectrograph.This make using from
It is very high to test the scientific research cost of Raman spectrum resonance profile to dissipate the laser of wavelength.It is former for continuous tunable frequency-stabilized laser
It needs infinite multiple Raman optical filters that could complete the test of fine Raman spectrum resonance profile on then, and customizes off-gauge
Raman optical filter price is very expensive, and which limits monochromatic light grid Raman spectrometer answering in Raman spectrum resonance profile test
With.
Summary of the invention
Based on the above technical problem, the main purpose of the disclosure is to propose a kind of Raman spectrum test macro, for solving
At least one of certainly above technical problem.
To achieve the goals above, the present disclosure proposes a kind of Raman spectrum test macro, including wide spectrum monochromatization module,
Optical path coupling and output module and signal detection module, in which:
Wide spectrum monochromatization module, comprising:
Supercontinuum source, for exporting wide spectrum exciting light；
Monochromatization unit, for wide spectrum exciting light to be filtered into monochromatic light；
Optical path coupling and output module, for making monochromatic light exposure to sample surfaces, excitation obtains Raman signal light；
Signal detection module is detected for receiving Raman signal light, obtains the Raman spectrum of the sample.
In some embodiments of the present disclosure, above-mentioned monochromatization unit includes:
Broadband pass filter, for selecting the wide spectrum exciting light of a wavelength range；
Grating, for making the wide spectrum of a wavelength range excite the monochromatic light of optical dispersion different wave length；
Diaphragm obtains the monochromatic light for exposing to sample surfaces for filtering the monochromatic light of different wave length.
In some embodiments of the present disclosure, above-mentioned monochromatization unit further includes the first reflecting mirror, for making different wave length
Reflection of monochromatic light to diaphragm.
In some embodiments of the present disclosure, above-mentioned grating and the first reflecting mirror are placed in the same rotatable support frame, are led to
The deflection angle of grating and the first reflecting mirror relative to supercontinuum source is overregulated, changes the reflection of monochromatic light of different wave length extremely
The position of diaphragm.
In some embodiments of the present disclosure, above-mentioned monochrome light unit further includes that at least one tunable narrow-band pass filters
Piece, each tunable narrow-band pass filter are placed in the rotatable support frame that one can adjust its position and deflection angle, are used
The monochromatic light of sample surfaces is exposed in purifying.
In some embodiments of the present disclosure, the bandpass range of above-mentioned broadband pass filter is greater than Raman spectrum resonance profile
Two times of full width at half maximum.
In some embodiments of the present disclosure, the range of working range and Raman spectrum the resonance profile of above-mentioned grating
Match.
In some embodiments of the present disclosure, above-mentioned grating includes transmission grating or reflecting grating.
In some embodiments of the present disclosure, above-mentioned optical path coupling includes: with output module
Beam splitter, for making the monochromatic light for exposing to sample surfaces be incident to microcobjective；
Microcobjective, for the monochromatic light for exposing to sample surfaces to be focused to sample surfaces, excitation obtains Raman signal
Light, and the Raman signal light of sample surfaces reflection is collected to be transmitted to beam splitter；
Condenser lens, for making the focusing of Raman signal light be incident to signal detection module.
In some embodiments of the present disclosure, above-mentioned beam splitter is placed on vertical two dimension angular adjustment frame, is irradiated for making
To the monochromatic light collimated incident of sample surfaces to microcobjective.
In some embodiments of the present disclosure, above-mentioned optical path coupling and output module further include:
At least one is tunable sideband optical filter, between microcobjective and condenser lens, for filtering out sample surfaces
The Rayleigh signal light carried when reflecting Raman signal light, obtains pure Raman signal light.
In some embodiments of the present disclosure, at least one above-mentioned tunable sideband optical filter, which is fixed on, to be arranged rotatable
On the two-dimensional vertical adjustable articulator of bracket, fine-tuned with the operating angle at least one tunable sideband optical filter.
In some embodiments of the present disclosure, above-mentioned tunable sideband optical filter is greater than the transmitance of Raman signal light etc.
In 90%；To the transmitance of Rayleigh signal light less than 10-6。
In some embodiments of the present disclosure, above-mentioned optical path coupling and output module further include:
At least one second reflecting mirror, each second reflecting mirror are placed on a vertical two dimension angular adjusting bracket, are used
In making to expose to the reflection of monochromatic light of sample surfaces to the center of beam splitter；
At least one third reflecting mirror, it is poly- for entering via beam splitter, sample surfaces reflection Raman signal light emission
Focus lens.
In some embodiments of the present disclosure, above-mentioned condenser lens is placed on three-dimensional adjustable shelf, by adjusting the three-dimensional
Adjusting bracket can make Raman signal light vernier focusing be incident to signal detection module.
In some embodiments of the present disclosure, above-mentioned signal detection module includes:
Monochromatic light grating spectrograph is detected for receiving Raman signal light, obtains the Raman spectrum of sample.
The Raman spectrum test macro that the disclosure proposes, has the advantages that
1, wide spectrum exciting light is provided using supercontinuum source, so as to provide wide swashing up to 400~2400nm wavelength
It shines, there is no need to use expensive and unhandy Wavelength tunable laser, i.e., easily selects different wave length
Monochromatic light；And since monochromatization unit uses grating and diaphragm, it is convenient to the good monochromatic light of monochromaticjty is obtained, so that output
Monochromatic half-breadth is less than 1mm；Therefore the design of wide spectrum monochromatization module is simple and practical, can be realized low cost, easy to operate,
The effects such as technical difficulty is low；
2, by adjusting the deflection angle of grating and the first reflecting mirror relative to supercontinuum source, to change different wave length
Reflection of monochromatic light to the position of diaphragm, to may make diaphragm that the monochrome for being irradiated to sample surfaces of different wave length is obtained by filtration
Light；And monochromatic light and tunable sideband optical filter are purified by the way that at least one tunable narrow-band pass filter is arranged, it can facilitate
Switching different wave length monochromatic light come carry out Raman spectrum resonance profile test, be accurately obtained sample Electron band structure
Information；
3, optical path coupling is with output module using tunable on the two-dimensional vertical adjustable articulator being placed in rotatable support frame
Sideband optical filter realizes that the optimization of its operating angle is adjusted, to reach suitable cut-off wave by changing its operating angle
Number so that most of Raman signal light all penetrates, and effectively stops Rayleigh signal light, to improve the standard of whole system test
True property.
4, reflecting mirror, beam splitter, tunable sideband optical filter are all fixed on two-dimensional vertical adjustable articulator in the disclosure,
Each adjusting bracket can realize that two-dimensional directional fine-tunes.The part two-dimensional vertical adjustable articulator as in rotatable support frame,
The rotatable support frame is placed in pluggablely on the pillar for being fixed on spectrometer substrate.It is monochromatic in switching different wave length based on this
Light and when changing the cut-off sideband of tunable sideband optical filter, being capable of rapidly collimation adjustment optical path；
5, there is the Raman spectrum test macro of the disclosure low cost, exciting light and filter plate cut-off sideband to be continuously adjusted
Ability, and have many advantages, such as that easy to operate, light path arrangement is reasonable and scalability is strong.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for the resonance Raman spectroscopy test macro that one embodiment of the disclosure proposes；
Fig. 2 is the monochromatic spectrogram that wide spectrum monochromatization module is emitted in Fig. 1；
Fig. 3 is white light transmittant spectrum of the tunable sideband optical filter TLF under a certain operating angle in Fig. 1；
When Fig. 4 is the operating angle in Fig. 3, Raman spectrometer measures silicon wafer and is located at 520.6cm-1Characteristic peak Raman light
Spectrum；
Fig. 5 be using double graphene t (1+1) LG of corner measured by Raman spectrum test macro in Fig. 1 G mould (~
1580cm-1) Raman spectrum；
Fig. 6 is the Raman using the G mould of double graphene t (1+1) LG of corner measured by Raman spectrum test macro in Fig. 1
Intensity is to the resonance profile after single-layer graphene normalization.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, and reference
Attached drawing, the present invention is described in further detail.
With gradually improving for coating technique, a kind of special sideband optical filter, i.e., tunable sideband optical filter is manufactured
Out.By changing the operating angle of tunable sideband optical filter, cut-off sideband will be continuously adjusted, and in adjustment process
In, the cutoff wavelength of s wave and p wave does not have difference, allows to use in wider wave-length coverage.It, can in visible-range
The adjustable extent of sideband optical filter is tuned up to 50-100nm, adjustable range is related with operation wavelength.Single tunable sideband filter
The even several enough dye lasers of the working range of mating plate use.Therefore tunable sideband optical filter is such as applied to Raman light
Spectrum testing system can lower significantly and test Raman spectrum resonance profile using monochromatic light grid Raman spectrometer and tunable laser
Use cost.But the price of Wavelength tunable laser is very high at present or operation is very inconvenient.Therefore it is highly desirable to
Find the cost performance height for Raman spectrum resonance profile test and easy to operate tunable substitution excitation light source.
(Supercontinuum laser) has been developed as to provide as white-light spectrum in supercontinuum source
Wide unpolarized complex light, coverage area can the wide wave-length coverages up to 400~2400nm.Its total Output optical power can be to ten
Several watts, brightness are very high；Meanwhile beam divergence angle is very small, transmitting full-shape is smaller than 1mrad, and collimation is very good, can be with
Most ions or gas laser are comparable.Therefore, such Supercontinuum source can replace more light sources, such as single line
Laser, white light, superradiance wide spectrum light source (SLEDs) etc..For such a high brightness, beam divergence angle is very small to swash
Light emitting source if the monochromatic light that wavelength is continuously adjusted and stablizes output can be obtained from it, and is coupled into the monochromatic light of micro confocal
Grid Raman spectrometer, so that it may be used to test the excitation light source with broad tuning range of Raman spectrum as one.This light
Source has thousands of hours freedom from repairs service life, and the various lasers high compared to cost can be such that Raman spectrum resonance profile surveys
The use cost and technical difficulty degree of examination substantially reduce.
Therefore, how to design that a set of structure based on supercontinuum source is simple, be convenient for changing the optics member of operation wavelength
The tunable resonance Raman spectroscopy test macro that part and the tunable sideband optical filter of cooperation use is vast Raman spectrum work
Desired one of the spectral technique problem solved of person.
Therefore, the present disclosure proposes a kind of Raman spectrum test macro, including the coupling of wide spectrum monochromatization module, optical path with it is defeated
Module and signal detection module out, in which:
Wide spectrum monochromatization module, comprising:
Supercontinuum source, for exporting wide spectrum exciting light；
Monochromatization unit, for wide spectrum exciting light to be filtered into monochromatic light；
Optical path coupling and output module, for making monochromatic light exposure to sample surfaces, excitation obtains Raman signal light；
Signal detection module is detected for receiving Raman signal light, obtains the Raman spectrum of sample.
Due to providing wide spectrum exciting light using supercontinuum source, the wide excitation up to 400~2400nm wavelength can be provided
Light easily selects different wave length there is no need to use expensive and unhandy Wavelength tunable laser
Monochromatic light.
In some embodiments of the present disclosure, above-mentioned monochromatization unit includes:
Broadband pass filter, for selecting the wide spectrum exciting light of a wavelength range；
Grating, for making the wide spectrum of a wavelength range excite the monochromatic light of optical dispersion different wave length；
Diaphragm obtains the monochromatic light for exposing to sample surfaces for filtering the monochromatic light of different wave length.
Since monochromatization unit uses grating and diaphragm, it is convenient to the good monochromatic light of monochromaticjty is obtained, so that output is single
The half-breadth of coloured light is less than 1mm；Therefore the design of wide spectrum monochromatization module is simple and practical, can be realized low cost, easy to operate, skill
The effects such as art difficulty is low.
In some embodiments of the present disclosure, above-mentioned monochromatization unit further includes the first reflecting mirror, for making different wave length
Reflection of monochromatic light to diaphragm.
In some embodiments of the present disclosure, above-mentioned grating and the first reflecting mirror are placed in the same rotatable support frame, are used
In adjusting the deflection angle of grating and the first reflecting mirror relative to supercontinuum source, so that the monochromatic light for changing different wave length is anti-
It is incident upon the position of diaphragm；To may make diaphragm that the monochromatic light for being irradiated to sample surfaces of different wave length is obtained by filtration, easily
Switch the monochromatic light of different wave length to carry out Raman spectrum test.
In some embodiments of the present disclosure, above-mentioned monochrome light unit further includes that at least one tunable narrow-band pass filters
Piece, each tunable narrow-band pass filter are placed in the rotatable support frame that one can adjust its position and deflection angle, are used
The monochromatic light of sample surfaces is exposed in purifying；To may make the test macro of the present embodiment accurately to obtain sample message.
In some embodiments of the present disclosure, the bandpass range of above-mentioned broadband pass filter is greater than Raman spectrum resonance profile
Two times of full width at half maximum.
In some embodiments of the present disclosure, the range of working range and Raman spectrum the resonance profile of above-mentioned grating
Match.
In some embodiments of the present disclosure, above-mentioned grating includes transmission grating or reflecting grating；Different grating types
Need to design different optical paths to realize the function of the present embodiment Raman spectrum test macro；Preferably, using transmission grating.
In some embodiments of the present disclosure, above-mentioned optical path coupling includes: with output module
Beam splitter, for making the monochromatic light for exposing to sample surfaces be incident to microcobjective；
Microcobjective, for the monochromatic light for exposing to sample surfaces to be focused to sample surfaces, excitation obtains Raman signal
Light, and collect the Raman signal light of sample surfaces reflection and be transmitted to beam splitter；
Condenser lens, for making the focusing of Raman signal light be incident to signal detection module.
In some embodiments of the present disclosure, above-mentioned beam splitter is placed on vertical two dimension angular adjustment frame, is irradiated for making
To the monochromatic light collimated incident of sample surfaces to microcobjective.
In some embodiments of the present disclosure, above-mentioned optical path coupling and output module further include:
At least one is tunable sideband optical filter, between microcobjective and condenser lens, for filtering out sample surfaces
The Rayleigh signal light carried when reflecting Raman signal light, obtains pure Raman signal light.
In some embodiments of the present disclosure, at least one above-mentioned tunable sideband optical filter, which is fixed on, to be arranged rotatable
On the two-dimensional vertical adjustable articulator of bracket, fine-tuned with the operating angle at least one tunable sideband optical filter.
Therefore, because optical path coupling is with output module using on the two-dimensional vertical adjustable articulator being placed in rotatable support frame
Tunable sideband optical filter realizes that the optimization of its operating angle is adjusted, to reach suitable by changing its operating angle
End wave number, so that most of Raman signal light all penetrates, and Rayleigh signal light is effectively stopped, to improve whole system survey
The accuracy of examination
In some embodiments of the present disclosure, above-mentioned tunable sideband optical filter is greater than the transmitance of Raman signal light etc.
In 90%；To the transmitance of Rayleigh signal light less than 10-6。
In some embodiments of the present disclosure, above-mentioned optical path coupling and output module further include:
At least one second reflecting mirror, each second reflecting mirror are placed on a vertical two dimension angular adjusting bracket, are used
In making to expose to the reflection of monochromatic light of sample surfaces to the center of beam splitter；
At least one third reflecting mirror, it is poly- for entering via beam splitter, sample surfaces reflection Raman signal light emission
Focus lens.
In some embodiments of the present disclosure, above-mentioned condenser lens is placed on three-dimensional adjustable shelf, by adjusting the three-dimensional
Adjusting bracket can make Raman signal light vernier focusing be incident to signal detection module.
In some embodiments of the present disclosure, above-mentioned signal detection module includes:
Monochromatic light grating spectrograph is detected for receiving Raman signal light, obtains the Raman spectrum of sample.
In some embodiments of the present disclosure, signal detection module includes monochromatic light grating spectrograph and corresponding control circuit,
It is detected for being coupled to optical path with the pure Raman signal light that output module obtains, obtains the Raman spectrum of sample SMP.Institute
Stating the monochromatic light grating spectrograph GPY in signal detection module includes slit SLT, reflecting mirror M5, reflecting mirror M6, grating GRT and detection
Device CCD, wherein the Raman signal light from slit SLT is incident on reflecting mirror MA, the signal light irradiation after reflecting mirror MA reflection
Onto grating GRT, the signal light after grating GRT dispersion is collected by reflecting mirror MB and is reflected into detector C CD and examined
It surveys.
In the disclosure, reflecting mirror, beam splitter, tunable sideband optical filter are all fixed on two-dimensional vertical adjustable articulator,
Each adjusting bracket can realize that two-dimensional directional fine-tunes.The part two-dimensional vertical adjustable articulator as in rotatable support frame,
The rotatable support frame is placed in pluggablely on the pillar for being fixed on spectrometer substrate.It is monochromatic in switching different wave length based on this
Light and when changing the cut-off sideband of tunable sideband optical filter, being capable of rapidly collimation adjustment optical path.
In addition, in some embodiments of the present disclosure, during being tested using Raman spectrum test macro, also
It is measured using a wavelength measuring apparatus via the monochromatic wavelength after diaphragm；Preferably, which can be
Fiber spectrometer or other equipment that can test excitation wavelength.
Specifically, the disclosure is achieved like this, method and step are as follows:
1, suitable broadband pass filter BBF is selected, a certain wavelength model is selected from the continuous spectrum of supercontinuum source SCL
It encloses, guarantees that the working range of other optical elements in the present apparatus covers the wave-length coverage；
2, the rotatable support frame where transmission grating TG and the first reflecting mirror M1 is rotated, it is anti-to change transmission grating TG and first
Deflection angle of the mirror M1 relative to input path is penetrated, -1 grade light of the supercontinuum source SCL after transmission grating TG light splitting is changed
Bands of a spectrum reach the position on diaphragm APT.Two special tunable narrow-band pass filter TBF1 and TBF2 are adjusted to swash relative to incidence
Luminous deflection angle, to purify monochromatic light.It is filtered with monochromatic wavelength measuring device WLM measurement via the tunable narrow-band pass
The monochromatic wavelength of mating plate TBF1 and TBF2 outgoing.
3, the monochromatic light being emitted in the wide spectrum monochromatization module is incident on the second reflection by configuring the first reflecting mirror
Mirror M2, and it is reflected into beam splitter BS via the M3 in the second reflecting mirror, and then the monochromatic light after beam splitter BS reflection is via aobvious
Speck mirror OBJ focuses on the surface sample SMP.Meanwhile reflection of monochromatic light light and Raman signal light from sample SMP, via aobvious
Speck mirror OBJ is incident on beam splitter BS after collecting, then is reflected into tunable sideband optical filter TLF via third reflecting mirror M4.Root
According to incident monochromatic wavelength, rotation is located at the tunable sideband optical filter TLF in rotatable support frame, to change tunable sideband
Deflection angle of the optical filter TLF relative to optical path adjusts the cut-off sideband of tunable sideband optical filter TLF to suitable wave number.
Monochromatic reflected light (i.e. Rayleigh signal light) is filtered out and decays to only original at least 1/ by tunable sideband optical filter TLF
106, and the Raman signal light of the overwhelming majority is penetrated, and line focus lens LNS focuses the slit for entering monochromatic light grating spectrograph
It is detected after SLT for monochromatic light grating spectrograph.
4, it repeats the above steps 2,3, need to only carry out minor adjustments to the optical element in optical path, next monochrome can be carried out
The test of wavelength.
Below by way of specific embodiment, the Raman spectrum test macro proposed to the disclosure is described in detail.
Embodiment
As shown in Figure 1, present embodiment discloses a kind of surveys of the Raman spectrum of tunable resonance based on supercontinuum source
Test system, including the coupling of wide spectrum monochromatization module 10, optical path and output module 20 and signal detection module 30.
As a preferred embodiment, system is tested using the Raman spectrum of this tunable resonance based on supercontinuum source
System, the G mould Raman spectrum of test corner double graphene t (1+1) LG and single-layer graphene, the ratio for obtaining the two swash with monochromatic light
Wavelength is sent out in the Raman spectrum resonance profile of 550nm-700nm consecutive variations.
Wherein, wide spectrum monochromatization module 10 includes at least 101, wide bandpass filters of a supercontinuum source (SCL)
The reflecting mirror M1 (104) of transmission grating (TG) 103, one of piece (BBF) 102, one and diaphragm (APT) 105, the wide spectrum monochromatization mould
Block 10 is for issuing and selecting monochromatic light.It and at least further include two special 106 Hes of tunable narrow-band pass filter (TBF1)
(TBF2) 107, for purifying monochromatic light；It include optionally a monochromatic wavelength measuring device (WLM) 108, for surveying
Amount is via the monochromatic wavelength after diaphragm (APT) 105.
Preferably, the supercontinuum source (SCL) 101 in wide spectrum monochromatization module 10 uses Denmark NKT
The SuperK series super continuous spectrums of Photonics company production compose white light source EXW-12, have very wide spectral region, can
To realize the output of 400~2400nm spectrum, it is seen that optical output power is easily operated up to 1.2W, can be realized steady in a long-term
Work.
Broadband pass filter (BBF) 102, for selecting a certain wavelength from the continuous spectrum of supercontinuum source (SCL) 101
The spectrum of range, to guarantee that the working range of other optical elements in the present apparatus covers the wave-length coverage.
Preferably, the broadband pass filter (BBF) 102 in wide spectrum monochromatization module 10 has used Asahi-Spectra
The BrightLine Full of the Super Cold Filter of company super cold filter plate YSC1100 and Semrock company
The group of Spectrum Blocking single-band bandpass filter broadband pass filter FF01-632/148-25
It closes.The transmission range that broadband leads to super cold filter plate is 400~1000nm, mean transmissivity 70%, for filtering from super continuous
The wavelength that white light source (SCL) 101 is emitted is the light of 1000nm or more.The central wavelength of single tape pass filter is 632nm, transmission bands
Width is 148nm, transmissivity 93%, for from super cold filter plate transmitted through the wave that interception wavelength is 558~706nm in the light come
Section guarantees that the working range of other optical elements in the present apparatus covers the wave-length coverage.
Transmission grating (TG) 103 and reflecting mirror (M1) 104 are fixed in a rotatable support frame in wide spectrum monochromatization module,
Keep them adjustable relative to the deflection angle of input path.When transmission grating (TG) 103 and reflecting mirror (M1) 104 such as Fig. 1
When placement, -1 grade of spectral line in supercontinuum source 101 reaches diaphragm (APT) 105 by reflecting mirror (M1) 104, saturating by changing
The deflection angle of grating (TG) 103 and reflecting mirror (M1) 104 relative to incident light source is penetrated, the band for changing -1 grade of composition reaches
Monochromatic light is isolated using diaphragm (APT) 105 in position on diaphragm (APT) 105.
Preferably, the transmission grating (TG) 103 in the wide spectrum monochromatization module has used Ibsen Fused
Silica Transmission Gratings VIS-1379-911, service band are 400~800nm, and grating resolution is
1379mm-1。
Two special tunable narrow-band pass filters (TBF1) 106 and (TBF2) 107 in wide spectrum monochromatization module 10 are used
Stray light is filtered, the monochromatic purpose of purifying is reached.
Preferably, two special 106 Hes of tunable narrow-band pass filter (TBF1) in wide spectrum monochromatization module 10
(TBF2) 107 Semrock company has been usedTunable bandpass filter tunable narrow-band pass
Optical filter TBP01-561/14 (tunable center wavelength range 501.5nm~561.0nm, bandwidth 14nm), TBP01-617/14 (can
Adjust central wavelength range 550nm~617nm, bandwidth 13nm), TBP01-628/14 (tunable center wavelength range 561nm~
627nm, bandwidth 14nm), TBP01-697/13 (tunable center wavelength range 618.5nm~697.0nm, bandwidth 13nm),
TBP01-704/13 (tunable center wavelength range 627.7nm~703.8nm, bandwidth 13nm), need to carry out group according to actual needs
It closes.By suitably adjusting its deflection angle relative to input path, change the central wavelength of tunable narrow-band pass filter, benefit
With the intersection of the band logical wave band of two tunable narrow-band pass filters, reach the monochromatic purpose of purifying.
Further, two special tunable narrow-band pass filters (TBF1) 106 and (TBF2) 107 are respectively placed in one and can revolve
Turn on bracket, can position to tunable narrow-band pass filter and deflection angle fine-tune.
Optical path coupling includes at least two second reflecting mirrors (M2) 201 and (M3) 202, beam splitter (BS) with output module 20
203, microcobjective (OBJ) 204, third reflecting mirror (M4) 205, tunable sideband optical filter (TLF) 206 and condenser lens
(LNS) 207, the monochromatic light for obtaining the wide spectrum monochromatization module is reflected by two reflecting mirrors (M2) 201, (M3) 202
To the center of beam splitter (BS) 203, homogeneous beam is oriented to microcobjective (OBJ) 204 again by beam splitter (BS) 203, through micro- object
Mirror (OBJ) 204 focuses on sample (SMP) and is irradiated to it, and allows reflected light (the i.e. Rayleigh of (SMP) after irradiating sample
Signal light) and Raman signal light through microcobjective (OBJ) 204 collection after retroeflection to the center of beam splitter (BS) 203, process is adjustable
Humorous sideband optical filter (TLF) 206 obtains pure Raman signal light, and then is converged to by condenser lens (LNS) 207 subsequent
Signal detection module.
Preferably, in optical path coupling and output module 20, the second reflecting mirror (M2) 201, (M3) 202 and third reflecting mirror
(M4) it 205 is both secured on two-dimensional vertical adjustable articulator, keeps their angle two dimension adjustable；Adjust the second reflecting mirror (M3)
202 allow homogeneous beam to be incident on the center of beam splitter (BS) 203.
Preferably, in optical path coupling and output module 20, beam splitter (BS) 203 and tunable sideband optical filter (TLF)
206 are respectively arranged on two-dimensional vertical adjustable articulator in a manner of pluggable, so as to its position and deflection angle progress
It is accurate to adjust.
Further, the reflectivity of beam splitter (BS) 203 be 50%, transmissivity 50%.The two dimension of beam splitter (BS) 203
Vertically adjustable section frame further includes adjusting screw thread, can position to the optical filter supported on two-dimensional vertical adjustable articulator and angle into
Row further fine-tunes.
Preferably, tunable sideband optical filter (TLF) 206 uses the VersaChrome of Semrock company
EdgeTM(adjustable sideband wave is a length of by tunable longpass filter is tunable long wave sideband optical filter TLP01-628
561nm~628nm) and TLP01-704 (the adjustable a length of 628nm~704nm of sideband wave), transmitance > 90%.Its two dimension is perpendicular
Straight adjustable articulator is fixed in a rotatable support frame, which is placed in the pillar for being fixed on spectrometer substrate pluggablely
On, can position to tunable sideband optical filter (TLF) 206 and deflection angle further fine-tuned.
Preferably, optical path coupling is with output module 20, microcobjective (OBJ) 204 has used 100 times of micro- objects of Lycra
Mirror (numerical aperture NA=0.9), the monochromatic spot diameter for reaching sample SMP is 1~2 μ 2.
Preferably, condenser lens (LNS) 207 is placed on D translation adjusting bracket, adjusted by adjusting D translation
Three translation shafts of frame can not only be adjusted up the position of condenser lens 207 in two-dimensional vertical side, additionally it is possible in optical axis direction
The position for adjusting plus lens 207 enables Raman signal light accurate incident and slit that is focusing on signal detection module 30
(SLT) 301, so that signal detection module is detected.
Monochromatic light grating spectrograph in signal detection module 30 include the 301, the 4th reflecting mirror (M5) 302 of slit (SLT),
5th reflecting mirror (M6) 303, grating (GRT) 304 and detector (CCD) 305, wherein coming from the Raman signal of slit (SLT) 301
Light is incident on the 4th reflecting mirror (M5) 302, and the signal light after the reflection of the 4th reflecting mirror (M5) 302 is irradiated to grating (GRT) 304
On, the signal light after 304 dispersion of grating (GRT) is collected by the 5th reflecting mirror (M6) 303 and is reflected into detector (CCD)
305 are detected.
Signal acquisition and the analytic process of the Raman spectrum of the present embodiment the following steps are included:
Step 1, the suitable broadband pass filter (BBF) 102 of selection, from the continuous spectrum of supercontinuum source (SCL) 101
A certain wave-length coverage is selected, guarantees that the working range of other optical elements in the present apparatus covers the wave-length coverage.
Rotatable support frame where step 2, rotation transmission grating (TG) 103 and the first reflecting mirror (M1) 104, changes transmission
The deflection angle of grating (TG) 103 and the first reflecting mirror (M1) 104 relative to input path changes supercontinuum source (SCL)
101-1 grade of band after the light splitting of transmission grating (TG) 103 reaches the position on diaphragm (APT) 105.Adjustment two is special can
Narrow-band pass filter (TBF1) 106 and deflection angle of (TBF2) 107 relative to incident exciting light are tuned, to purify monochromatic light.
Gone out with the measurement of monochromatic wavelength measuring device (WLM) 108 via tunable narrow-band pass filter (TBF1) 106 and (TBF2) 107
The monochromatic wavelength penetrated.
The monochromatic light being emitted in wide spectrum monochromatization module is incident on the by configuration the first reflecting mirror (M1) 103 by step 3
Two-mirror (M2) 201 is reflected into beam splitter (BS) 203 through the second reflecting mirror (M3) 202, and then anti-through beam splitter (BS) 203
Monochromatic light after penetrating focuses on the surface sample SMP via microcobjective (OBJ) 204.Meanwhile microcobjective (OBJ) 204 is collected and
Enter after being collected from the reflection of monochromatic light light (i.e. Rayleigh signal light) and Raman signal light of sample SMP via microcobjective (OBJ) 204
It is mapped to beam splitter (BS) 203, then is reflected into tunable sideband optical filter (TLF) 206 via third reflecting mirror (M4) 205.According to
Incident monochromatic wavelength, rotation is located at the tunable sideband optical filter (TLF) 206 in rotatable support frame, tunable to change
Deflection angle of the sideband optical filter (TLF) 206 relative to optical path adjusts the cut-off sideband of tunable sideband optical filter (TLF) 206
To suitable wave number.Monochromatic reflected light (i.e. Rayleigh signal light) is filtered out and is decayed by tunable sideband optical filter (TLF) 206
To only original at least 1/106, and the Raman signal light of the overwhelming majority is penetrated, and line focus lens (LNS) 207 focus
It is detected after into the slit (SLT) 301 of monochromatic light grating spectrograph for monochromatic light grating spectrograph.
Step 4, repeat the above steps (2), (3), only need to carry out minor adjustments to the optical element in optical path, can carry out
The test of next monochrome wavelength.
Using the Raman spectrum test macro of the present embodiment, the double graphenes of corner and mono-layer graphite of (1 layer+1 layer) are tested
The G mould Raman spectrum of alkene, has used 100 times of Lycra microcobjectives, 600 ruling gratings, and 100 μ meters of spectrometer input slit width.
The wavelength for being illustrated in figure 2 the outgoing of wide spectrum monochromatization module is the monochromatic spectrogram of 619.5nm, it is seen that
The monochromatic half-breadth is less than 0.5nm, it is seen that has extraordinary monochromaticjty.As shown in Figure 3 and Figure 4, it is filtered for tunable sideband
White light transmittant spectrum of the mating plate (TLF) 206 under a certain deflection angle is located at the silicon wafer that Raman spectrometer measures at this time
520.6cm-1Characteristic peak Raman spectrum, it is seen that the tunable sideband optical filter (TLF) 206 can end to 200cm-1,
200cm-1Above spectrum is without obvious spurious signal.As shown in figure 5, for the present embodiment Raman spectrum test macro measure turn
The double graphenes in angle are located at 1580cm-1G mould Raman spectrum.Because the intensity of Raman signal is related with laser power, it is total to
Vibration intensity spectrum needs to carry out normalizing to excitation light power.In this embodiment, it is located at 1580cm with single-layer graphene G mould-1G
Mould raman scattering intensity carries out normalizing.As shown in fig. 6, for the corner that measures of Raman spectrum test macro double graphenes of the present embodiment
Positioned at 1580cm-1The pass that changes relative to the raman scattering intensity of single-layer graphene G mould relative to monochromatic excitation light of G mould raman scattering intensity
System composes with monochromatic light excitation wavelength in the strength of resonance of 550nm~700nm to obtain the double graphenes of corner.
Above example example illustrates that the Raman spectrum test macro of disclosure design can not only obtain what wavelength was continuously adjusted
Stablize the monochromatic light of output, and the feature adjustable using the cut-off sideband of tunable sideband optical filter, surveys strength of resonance spectrum
Amount is achieved in commercialized monochromatic light grid Raman spectrometer, and design it is simple and practical, it is easy to operate, light path arrangement is reasonable
It is strong with scalability.The disclosure can make up commercialized Raman spectrometer and be unable to satisfy the technology of strength of resonance spectrometry not
Foot pushes application of the confocal micro Raman spectrum in investigation of materials.
Particular embodiments described above has carried out further in detail the purpose of the present invention, technical scheme and beneficial effects
Describe in detail bright, it should be understood that the above is only a specific embodiment of the present invention, is not intended to restrict the invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in protection of the invention
Within the scope of.
Claims (12)
1. a kind of Raman spectrum test macro, including the coupling of wide spectrum monochromatization module, optical path and output module and signal detection mould
Block, in which:
Wide spectrum monochromatization module, comprising:
Supercontinuum source, for exporting wide spectrum exciting light, the wave-length coverage of the wide spectrum exciting light is 400 ~ 2400nm；
Monochromatization unit, for the wide spectrum exciting light to be filtered into monochromatic light, wherein the monochromatization unit includes:
Broadband pass filter, for selecting the wide spectrum exciting light of a wavelength range；
Grating, for making the wide spectrum of a wavelength range excite the monochromatic light of optical dispersion different wave length；
Diaphragm obtains the monochromatic light for exposing to sample surfaces for filtering the monochromatic light of the different wave length；
First reflecting mirror, for making the reflection of monochromatic light of the different wave length to the diaphragm；
At least one tunable narrow-band pass filter, each described tunable narrow-band pass filter, which is placed in one, can adjust it
In the rotatable support frame of position and deflection angle, for purifying the monochromatic light for exposing to sample surfaces；
Optical path coupling and output module, for making the monochromatic light exposure to sample surfaces, excitation obtains Raman signal light；
Signal detection module is detected for receiving the Raman signal light, obtains the Raman spectrum of the sample.
2. Raman spectrum test macro as described in claim 1, wherein the grating and the first reflecting mirror be placed in it is same can
On runing rest, by adjusting the deflection angle of the grating and the first reflecting mirror relative to the supercontinuum source, change
The reflection of monochromatic light of the different wave length is to the position of diaphragm.
3. Raman spectrum test macro as described in claim 1, wherein the bandpass range of the broadband pass filter is greater than institute
Two times for stating Raman spectrum resonance profile full width at half maximum；The model of the working range of the grating and Raman spectrum resonance profile
Enclose matching.
4. Raman spectrum test macro as described in claim 1, wherein the grating includes transmission grating or reflecting grating.
5. Raman spectrum test macro as described in claim 1, wherein the optical path, which is coupled with output module, includes:
Beam splitter, for making the monochromatic light for exposing to sample surfaces be incident to microcobjective；
Microcobjective, for the monochromatic light for exposing to sample surfaces to be focused to sample surfaces, excitation obtains Raman signal
Light, and the Raman signal light of sample surfaces reflection is collected to be transmitted to beam splitter；
Condenser lens, for making the Raman signal light focusing be incident to the signal detection module.
6. Raman spectrum test macro as claimed in claim 5, wherein the beam splitter is placed in vertical two dimension angular adjustment frame
On, for making the monochromatic light collimated incident for exposing to sample surfaces to the microcobjective.
7. Raman spectrum test macro as claimed in claim 5, wherein the optical path coupling and output module further include:
At least one is tunable sideband optical filter, between the microcobjective and condenser lens, for filtering out sample surfaces
The Rayleigh signal light carried when reflecting Raman signal light, obtains pure Raman signal light.
8. Raman spectrum test macro as claimed in claim 7, wherein at least one described tunable sideband optical filter is fixed
In on the two-dimensional vertical adjustable articulator that rotatable support frame is arranged in, with the work at least one tunable sideband optical filter
Angle is fine-tuned.
9. Raman spectrum test macro as claimed in claim 7, wherein the tunable sideband optical filter believes the Raman
The transmitance of number light is more than or equal to 90%；To the transmitance of the Rayleigh signal light less than 10-6。
10. Raman spectrum test macro as claimed in claim 5, wherein the optical path coupling and output module further include:
At least one second reflecting mirror, each described second reflecting mirror are placed on a vertical two dimension angular adjusting bracket, are used
In make the reflection of monochromatic light for exposing to sample surfaces to the center of the beam splitter；
At least one third reflecting mirror, for making via the beam splitter, sample surfaces reflection Raman signal light emission enter institute
State condenser lens.
11. Raman spectrum test macro as claimed in claim 5, wherein the condenser lens is placed on three-dimensional adjustable shelf,
By adjusting the three-dimensional adjustable shelf, Raman signal light vernier focusing can be made to be incident to the signal detection module.
12. Raman spectrum test macro as described in claim 1, wherein the signal detection module includes:
Monochromatic light grating spectrograph is detected for receiving the Raman signal light, obtains the Raman spectrum of the sample.
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| CN107807432A (en) * | 2017-12-13 | 2018-03-16 | 奥谱天成（厦门）光电有限公司 | A kind of microscopic Raman light path coupler |
| EP3743699A1 (en) | 2018-01-23 | 2020-12-02 | Danmarks Tekniske Universitet | An apparatus for carrying out raman spectroscopy |
| CN108169211A (en) * | 2018-02-12 | 2018-06-15 | 上海出入境检验检疫局动植物与食品检验检疫技术中心 | A kind of Raman spectrum enhances measuring system |
| CN109632717A (en) * | 2018-12-29 | 2019-04-16 | 深圳奥比中光科技有限公司 | Diffusing reflection rate detection device and method |
| CN109799222A (en) * | 2019-01-17 | 2019-05-24 | 华东师范大学 | A kind of image-pickup method of Raman face battle array EO-1 hyperion |
| WO2020255034A1 (en) * | 2019-06-20 | 2020-12-24 | National Research Council Of Canada | Broadband raman excitation spectroscopy with structured excitation profiles |
| CN114636543B (en) * | 2020-12-15 | 2022-12-27 | 中国科学院大连化学物理研究所 | Optical filter spectrum detection device |
| CN113030063A (en) * | 2021-03-31 | 2021-06-25 | 厦门大学 | Small-sized needle tip enhanced Raman spectrum measuring device and detection method thereof |
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