CN104422681A - Raman spectrometer - Google Patents
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- CN104422681A CN104422681A CN201310393168.9A CN201310393168A CN104422681A CN 104422681 A CN104422681 A CN 104422681A CN 201310393168 A CN201310393168 A CN 201310393168A CN 104422681 A CN104422681 A CN 104422681A
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Abstract
The invention relates to a raman spectrometer, which can be used for accurately qualitatively and half quantitatively analyzing a sample. The raman spectrometer comprises a laser, a raman signal acquisition device, a transmittance-type grating spectrometer, a plasma filter plate, a laser attenuation plate and a soleplate, wherein all the parts are fixed on the soleplate. The laser, the raman signal acquisition device and the transmittance-type grating spectrometer are fixed on a floor, and the raman spectrometer adopts transmittance-type coaxial optical-path design, so that the confocal measurement can be realized. The raman spectrometer has advantages of high light throughput, good spectral resolution, good stability and the like. The raman spectrometer is applicable to various excitation light sources of ultraviolet light, visible light, near-infrared light and the like.
Description
Technical field
The present invention relates to a kind of Raman spectrometer, as a kind of analytical instrument, can be analyzed by the composition of the Raman spectrum of collected specimens to material.
Background technology
Raman spectrum is called as molecular fingerprint spectrum, can analyze fast and accurately sample.Raman spectrum is widely used, and can be applied to food, safety, material evidence, mineral, environment, chemistry, and material is biological, multiple field such as ocean.Sample type comprises the variforms such as solid, powder, liquid, gas, interface, colloid.Current, the importance of Raman spectrum is gradually by everybody understanding, and its application is also more and more extensive.
The principle of Raman spectrum is: a photon and a molecule interact, if the energy of molecule absorption photon transits to high level from the low-lying level of vibration or rotary state, so according to law of conservation of energy, the energy that the energy level transition of the energy of photon loss and the vibration of molecule or rotation needs is equal, photon loses energy after vibration frequency changes, by the Changing Pattern that Raman spectrometer record photon frequency occurs, be Raman spectrum.
Raman spectrum is a kind of very weak signal, and its intensity is less than 10 of excitation source intensity
-8, in order to obtain the measured Raman spectrum of matter, require Raman spectrometer collection Raman spectrum efficiency and transmit Raman spectrum efficiency high, background noise is low and undesired signal is few.
There is the Raman spectrometer of three types in the market: one is three grades of Raman spectrometers (patent No.s 98113710.5), reflection ellipsoidal mirror or lens are used to gather Raman signal, the interference of the parasitic light that front two-stage spectrometer adopts addition or phase size reduction mode filtering Rayleigh scattering etc. to produce, afterbody spectrometer carries out record and the output of Raman spectrum.Three grades of Raman spectrometers are applied widely, multiple excitation source can be used to carry out exciting and do not need to change optical element, be applicable to deep ultraviolet, ultraviolet, visible, the excitation source of the multiple wave band such as near infrared, especially adopts reflection ellipsoidal mirror (patent No. 98113709.1) to collect Raman signal in ultraviolet region, collecting efficiency can be improved, the impact of color difference eliminating.But it is large that three grating Raman spectrometers also have volume, and Raman signal transfer efficiency is low, debugging and the shortcoming such as difficult in maintenance.The second is the Confocal laser-scanning microscopy instrument of use for laboratory, microscope is adopted to gather Raman signal, with the interference of optical filter filtering parasitic light, copolymerization Jiao can be realized and measure, there is small volume, gather and transfer efficiency advantages of higher, but the microscope volume gathered is comparatively large, and cost is high, and Confocal laser-scanning microscopy instrument weight is larger, high to environmental requirement, be inconvenient to carry.The third is fiber Raman spectrometer, adopts optical fiber to collect Raman signal, adopts Raman optical filter filtering parasitic light, has volume little, be easy to carry, can the advantage such as remote measurement.But Optical Fiber Transmission efficiency is low, is not suitable for ultraviolet band, common focusing function cannot be realized.
Summary of the invention
The invention provides a kind of Raman spectrometer, comprise laser instrument, fixed base plate, Raman signal harvester and transmission-type grating spectrometer, Raman signal harvester and transmission-type grating spectrometer are all fixed on base plate;
Raman signal harvester comprises the hollow tube-shape container of two end openings, and two openends in cylindrical container are respectively equipped with object lens, condenser lens, and object lens and condenser lens are arranged with optical axis, are provided with optical filter in the cylindrical container between object lens and condenser lens; Through hole is offered on the side wall surface of cylindrical container, as incidence hole, the exciting light that laser instrument sends enters in cylindrical container by incidence hole, optical filter surface is reflexed to through the catoptron be provided with in cylindrical container, object lens are reflexed to again by optical filter, focus on testing sample by object lens, all to be collected and optical filter filters through object lens by the exciting light of the Raman signal of testing sample scattering, Rayleigh signal and reflection, the light of reflection and the Rayleigh signal of scattering are by filtering, and Raman signal arrives condenser lens through optical filter and focuses on;
Transmission-type grating spectrometer comprises entrance slit, collimation lens, grating, condenser lens, catoptron, photoelectric conversion device, housing, it is characterized in that: the slit being provided with through side wall surface in the sidewall of housing, as entrance slit, light enters in the housing of spectrometer through entrance slit, becoming with entrance slit is the diverging light of radiation center, diverging light becomes directional light through focal plane at the collimation lens at slit place and arrives optical grating diffraction face, through optical grating diffraction, the optical diffraction of different wave length is to different directions, diffraction light through condenser lens focus on after again through reflector alignment light path reflect focalization on the light sensitive component of photoelectric conversion device, form Raman spectrum to carry out recording and/or exporting.
Technical scheme: plasma optical filter can be installed between laser instrument and Raman signal harvester, laser attenuation sheet and laser instrument, plasma optical filter and laser attenuation sheet be all installed on fixed base plate;
The light that laser instrument sends enters in the cylindrical container of Raman signal harvester by the incidence hole of Raman signal harvester;
The geometric center of the optical filter of Raman signal harvester is in the optical axis of object lens and condenser lens;
In Raman signal harvester, the angle between the optical axis of the optical axis of optical filter and object lens and condenser lens is less than 10 degree;
Exciting light is reflexed to the center of optical filter by the catoptron of Raman signal harvester, and catoptron is not on the optical axis of object lens and condenser lens, do not affect the transmission of light between object lens and optical filter;
The laser that catoptron reflection comes by the optical filter of Raman signal harvester reflexes to object lens along the optical axis of object lens;
In Raman signal harvester, can increase between optical filter and condenser lens and be provided with the second optical filter to optimize the filtration result of Rayleigh signal and reflected light, the optical axis included angle degree of being less than of optical filter optical axis angle and condenser lens.
The collimation lens of transmission-type grating spectrometer be placed on entrance slit be the position of focal plane and entrance slit center on the optical axis of collimation lens;
The grating placement location of transmission-type grating spectrometer should make its groove direction vertical with the optical axis of incident parallel light, and parallel with the slit direction of entrance slit, and the angle of placing should make the diffraction efficiency of incident parallel light reach best;
Transmission-type grating spectrometer, the position that condenser lens is placed should make its optical axis vertical with grating line direction, and its focus and the center superposition of diffracted light in optical grating diffraction face;
Transmission-type grating spectrometer, the position that catoptron and photoelectric conversion device are placed and angle, should make the light of the different wave length focused on through condenser lens all focus on the photovoltaic sensing element surface of photoelectric conversion device;
Transmission-type grating spectrometer, the sidewall that photoelectric conversion device is fixed on housing keeps stable; Transmission-type grating spectrometer uses airtight lucifuge shell to enter to stop parasitic light; It is the position of focal plane that collimation lens is placed on entrance slit;
Transmission-type grating spectrometer, photoelectric conversion device is charge-coupled image sensor or photomultiplier.If charge-coupled image sensor, then the placement direction of photoelectric conversion device should make the pixel orientation of photovoltaic sensing element and grating line direction perpendicular or parallel.
The optical axis coincidence of the collimation lens of the object lens of Raman signal harvester and condenser lens and described transmission-type grating spectrometer.
Beneficial effect: adopt backward scattering mode to gather Raman signal, collecting efficiency is high; Laser instrument, small-size multifunction Raman signal harvester, transmission-type grating spectrometer, plasma optical filter, laser attenuation sheet is fixed on same base plate, good stability; Small-size multifunction Raman signal harvester and transmission-type grating spectrometer are fixed together, and adopt the coaxial light path design of transmission-type, reach the effect of copolymerization Jiao; Lens adopt achromat group, reduce the impact of aberration and astigmatism, improve spectral resolution; Be applicable to the Raman spectrum test of fixing excitation wavelength, comprise ultraviolet, visible, the test of the Raman spectrum of near-infrared band.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is structure principle chart of the present invention.
Fig. 2 is structural representation of the present invention.
Fig. 3 is the structural representation of the Raman signal harvester in the present invention.
Fig. 4 is the structural representation of the transmission-type grating spectrometer in the present invention
Fig. 5 is embody rule example of the present invention: adamantine Raman spectrogram.
1. laser instruments in figure, 2. plasma optical filter, 3. laser power attenuator, 4. incidence hole, 5. Raman signal harvester, 6. object lens, 7. sample, 8. entrance slit, 9. transmission-type grating spectrometer, 10.CCD, 11. fixed base plates.
4. incidence holes in Fig. 3,5-2. small reflector, 5-3. optical filter, 6. object lens, 5-5. condenser lens, 5-6. crust of the device, 7. sample.
8. entrance slits in Fig. 4,9-2. collimation lens, 9-3. grating, 9-4. condenser lens, 9-5. catoptron, 9-6. photoelectric conversion device, 9-7. photoelectric conversion device induction chip, 9-8. slit fixed board, 10.CCD, 9-10. housing.
Embodiment
In FIG, a kind of Raman spectrometer, comprises laser instrument 1, plasma optical filter 2, laser power attenuator 3, incidence hole 4, Raman signal harvester 5, object lens 6, sample 7, entrance slit 8, transmission-type grating spectrometer 9, CCD10, fixed base plate 11.Laser instrument 1, plasma optical filter 2, laser power attenuator 3, Raman signal harvester 5, transmission-type grating spectrometer 9 is all fixed on base plate.
In figure 3, Raman signal harvester 5, comprise the hollow tube-shape container 5-6 of two end openings, two openends in cylindrical container 5-6 are respectively equipped with object lens 6, condenser lens 5-5, object lens 6 and condenser lens 5-5 are arranged with optical axis, are provided with optical filter 5-3 in the cylindrical container between object lens 6 and condenser lens 5-5, through hole is offered on the side wall surface of cylindrical container 5-6, be between object lens 4 and optical filter 3 as incidence hole 4(), the laser that laser instrument sends enters in cylindrical container 5-6 by incidence hole 4, be between object lens 4 and optical filter 3 through the catoptron 5(be provided with in cylindrical container 5-6)-2 reflex to optical filter 5-3 surface, object lens 6 are reflexed to again by optical filter 5-3, focus on testing sample 7 by object lens 6, by the Raman signal of testing sample 7 scattering, the exciting light of Rayleigh signal and reflection all filters through object lens 6 collection and optical filter 5-3, the light of reflection and the Rayleigh signal of scattering are by filtering, Raman signal arrives condenser lens 5-5 through optical filter 5-3 and focuses on the entrance slit 8 of transmission-type grating spectrometer 9.
In the diagram, a kind of transmission-type grating spectrometer 9, comprise entrance slit 8, collimation lens 9-2, grating 9-3, condenser lens 9-4, catoptron 9-5, CCD10, housing 9-10, the slit of through side wall surface is provided with in the sidewall of housing 9-10, as entrance slit 9-1, Raman signal enters in the housing 9-10 of spectrometer through entrance slit 8, the diverging light that to become with slit 8 be radiation center, diverging light becomes directional light through focal plane at the collimation lens 9-2 at slit 8 place and arrives grating 9-3 diffraction surfaces, through grating 9-3 diffraction, the optical diffraction of different wave length is to different directions, diffraction light adjusts light path reflect focalization on the light sensitive component 9-7 of CCD10 through catoptron 9-5 again after condenser lens 9-4 focuses on, form Raman spectrum to carry out recording and/or exporting.
The geometric center of the optical filter 5-3 of Raman signal harvester 5 is in the optical axis of object lens 6 and condenser lens 5-5;
Angle between the optical axis of the optical filter 5-3 of Raman signal harvester 5 and the optical axis of object lens 6 and condenser lens 5-5 is less than 10 degree, the efficiency of optical filter 5-3 reflects laser is greater than 90%, the efficiency about 99.99% of filtering interference signals, Raman signal transmitance is greater than 80%;
The catoptron 5-2 of Raman signal harvester 5 reflects the laser light to the center of optical filter 5-3, and catoptron is not on the optical axis of object lens 6 and condenser lens 5-5, do not affect the transmission of light between object lens 6 and optical filter 5-3.
Catoptron 5-2 is reflected the laser that comes and reflexes to object lens 6 along the optical axis of object lens 6 by the optical filter 5-3 of Raman signal harvester 5, makes the use of object lens 6 reach common optical axis effect.
On Raman signal harvester 5, the outside (namely away from the side of hollow tube-shape container 5-6) of condenser lens 5-5 side is provided with transmission-type grating spectrometer 9, and Raman signal is focused on the entrance slit 8 of transmission-type grating spectrometer 9 by condenser lens 5-5.
Collimation lens 9-2 is placed on entrance slit 8 for focal plane, and focus is on the center of entrance slit 8, makes collimation lens 9-2 reach common optical axis effect, reduces the impact of aberration and aberration;
Grating 9-3 placement location makes its groove direction vertical with the optical axis of incident parallel light, and parallel with the slit direction of entrance slit 8, and the angle that grating 9-3 places makes the diffraction efficiency of incident parallel light reach best;
The position that condenser lens 9-4 places makes its optical axis vertical with grating 9-3 groove direction, and its focus and diffracted light are at the center superposition of grating 9-3 diffraction surfaces, condenser lens 9-4 is made to reach common optical axis effect, reduce the impact of aberration and aberration, after line focus lens 9-4, the light of Same Wavelength diffraction light focuses on same point, and Raman light is divided into Raman spectrum;
The position that catoptron 9-5 and CCD10 places and angle, make the Raman spectrum of the different wave length focused on through condenser lens 9-4 all focus on the surface of the photoelectric conversion device induction chip 9-7 of CCD10, record and export Raman spectrum;
In the embodiment depicted in figure 2, the pixel of the photoelectric conversion device induction chip 9-7 of CCD10 is 2048 × 512, and the Width of photoelectric conversion device induction chip 9-7 is parallel with grating 3 groove direction, and length direction is vertical with grating 3 groove direction;
Can increase between the optical filter 5-3 of Raman signal harvester 5 and condenser lens 5-5 and be provided with the second optical filter to optimize the filtration result of Rayleigh signal and reflected light, the optical axis included angle of optical filter optical axis angle and condenser lens 5-5 is less than 10 degree.
In the embodiment shown in fig. 5, record adamantine Raman spectrum, in figure, horizontal ordinate is Raman frequency shift, experiment condition is: excitation wavelength, 355 nanometer lasers, and entrance slit width is 20 microns, grating be 2400 quarter lines per millimeter grating, CCD pixel size is 14 microns × 14 microns.
Claims (10)
1. a Raman spectrometer, comprise laser instrument (1), fixed base plate (11), Raman signal harvester (5) and transmission-type grating spectrometer (9), is characterized in that: described Raman signal harvester (5) and transmission-type grating spectrometer (9) are all fixed on fixed base plate;
Described Raman signal harvester (5) comprises the hollow tube-shape container (5-6) of two end openings, two openends in cylindrical container (5-6) are respectively equipped with object lens (6), condenser lens (5-5), object lens (6) and condenser lens (5-5) are arranged with optical axis, are provided with optical filter (5-3) in the cylindrical container (5-6) between object lens (6) and condenser lens (5-5), through hole is offered on the side wall surface of cylindrical container (5-6), as incidence hole (4), the exciting light that laser instrument (1) sends enters in cylindrical container (5-6) by incidence hole (4), optical filter (5-3) surface is reflexed to through the catoptron (5-2) be provided with in cylindrical container (5-6), object lens (6) are reflexed to again by optical filter (5-3), focus on testing sample (7) by object lens (6), by the Raman signal of testing sample (7) scattering, the exciting light of Rayleigh signal and reflection is all collected and optical filter (5-3) optical filtering through object lens (6), the light of reflection and the Rayleigh signal of scattering are by filtering, Raman signal arrives condenser lens (5-5) through optical filter (5-3) and focuses on,
Described transmission-type grating spectrometer (9) comprises entrance slit (8), collimation lens (9-2), grating (9-3), condenser lens (9-4), catoptron (9-5), photoelectric conversion device (9-6), housing (9-10), the slit of through side wall surface is provided with in the sidewall of housing (9-10), as entrance slit (8), the outside of upper condenser lens (5-5) side of Raman signal harvester (5) is provided with transmission-type grating spectrometer (9), the light that Raman signal focuses on by condenser lens (5-5) enters in the housing (9-10) of spectrometer through entrance slit (8), the diverging light that to become with entrance slit (8) be radiation center, diverging light becomes directional light through focal plane at the collimation lens (9-2) at entrance slit (8) place and arrives grating (9-3) diffraction surfaces, through grating (9-3) diffraction, the optical diffraction of different wave length is to different directions, diffraction light adjusts light path reflect focalization on the light sensitive component (9-7) of photoelectric conversion device (9-6) through catoptron (9-5) again after condenser lens (9-4) focuses on, form Raman spectrum to carry out recording and/or exporting.
2. Raman spectrometer according to claim 1, is characterized in that: can be provided with plasma optical filter (2), laser attenuation sheet (3) between laser instrument (1) and Raman signal harvester (5) successively; And laser instrument (1), plasma optical filter (2) and laser attenuation sheet (3) are all installed on fixed base plate (11).
3. Raman spectrometer according to claim 1, is characterized in that: described Raman signal harvester (5), and the geometric center of optical filter (5-3) is in the optical axis of object lens (6) and condenser lens (5-5);
Described Raman signal harvester (5), the laser that catoptron (5-2) reflection comes by optical filter (5-3) reflexes to object lens (6) along the optical axis of object lens (6).
4. the Raman spectrometer according to claim 1 or 3, is characterized in that: described Raman signal harvester (5), and the angle between the optical axis of optical filter (5-3) and the optical axis of object lens (6) and condenser lens (5-5) is less than 10 degree.
5. Raman spectrometer according to claim 1, it is characterized in that: described Raman signal harvester (5), exciting light is reflexed to the center of optical filter (5-3) by catoptron (5-2), and catoptron (5-2) is not on the optical axis of object lens (6) and condenser lens (5-5), do not affect the transmission of light between object lens (6) and optical filter (5-3).
6. Raman spectrometer according to claim 1, it is characterized in that: described Raman signal harvester (5), can increase between optical filter (5-3) and condenser lens (5-5) and be provided with the second optical filter to optimize the filtration result of Rayleigh signal and reflected light, the optical axis included angle of optical filter optical axis angle and condenser lens (5) is less than 10 degree.
7. Raman spectrometer according to claim 1, it is characterized in that: described transmission-type grating spectrometer (9), collimation lens (9-2) be placed on entrance slit (9-1) position that is focal plane and entrance slit (9-1) center on the optical axis of collimation lens (9-2);
Described transmission-type grating spectrometer (9), grating (9-3) placement location should make its groove direction vertical with the optical axis of incident parallel light, and parallel with the slit direction of entrance slit (9-1), and the angle of placing should make the diffraction efficiency of incident parallel light reach best;
Described transmission-type grating spectrometer (9), the position that condenser lens (9-4) is placed should make its optical axis vertical with grating (9-3) groove direction, and its focus and diffracted light are at the center superposition of grating (9-3) diffraction surfaces;
Described transmission-type grating spectrometer (9), the position that catoptron (9-5) and photoelectric conversion device (9-6) are placed and angle, should make the light of the different wave length focused on through condenser lens (9-4) all focus on photovoltaic sensing element (9-7) surface of photoelectric conversion device (9-6).
8. Raman spectrometer according to claim 1, is characterized in that: described transmission-type grating spectrometer (9), the sidewall that photoelectric conversion device (9-6) is fixed on housing (9-10) keeps stable; Transmission-type grating spectrometer (9) uses airtight lucifuge shell (9-10) to stop parasitic light to enter; It is the position of focal plane that collimation lens is placed on entrance slit.
9. Raman spectrometer according to claim 1, is characterized in that: described transmission-type grating spectrometer (9), and photoelectric conversion device (9-6) is charge-coupled device (CCD) or photomultiplier;
If charge-coupled device (CCD), then the placement direction of photoelectric conversion device (9-6) should make the pixel orientation of photovoltaic sensing element (9-7) and grating (9-3) groove direction perpendicular or parallel.
10. Raman spectrometer according to claim 1, is characterized in that: the object lens (6) of described Raman signal harvester (5), the optical axis coincidence of the collimation lens (9-2) of condenser lens (5-5) and described transmission-type grating spectrometer (9).
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| CN106645082A (en) * | 2016-11-03 | 2017-05-10 | 北京信息科技大学 | Gating optical fiber Raman spectrometer based on laser ranging automatic focusing |
| CN106645082B (en) * | 2016-11-03 | 2020-12-11 | 北京信息科技大学 | Gated fiber Raman spectrometer based on automatic focusing of laser ranging |
| CN106841166A (en) * | 2017-03-24 | 2017-06-13 | 北京极光仪器科技有限公司 | Cuboid Portable Raman spectrometer based on concave grating |
| CN108007570A (en) * | 2017-11-28 | 2018-05-08 | 北京云端光科技术有限公司 | Spectrometer and spectral detection system |
| CN108181294A (en) * | 2018-01-05 | 2018-06-19 | 厦门大学 | Raman spectrometer light path system |
| CN108181294B (en) * | 2018-01-05 | 2023-11-07 | 厦门大学 | Raman spectrometer optical path system |
| 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 |
| CN109115340A (en) * | 2018-09-06 | 2019-01-01 | 马浩臣 | A kind of spectrometer |
| CN109580582A (en) * | 2018-12-12 | 2019-04-05 | 哈尔滨工业大学（威海） | A kind of laser Raman spectrometer based on compound Amici Prism group |
| CN109580582B (en) * | 2018-12-12 | 2021-06-22 | 哈尔滨工业大学（威海） | Laser Raman spectrometer based on composite Amisy prism group |
| CN109975210A (en) * | 2019-04-28 | 2019-07-05 | 重庆冠雁科技有限公司 | A kind of bare engine module of handheld Raman spectrometer |
| CN111141722A (en) * | 2020-02-19 | 2020-05-12 | 吴玉珍 | Laser Raman spectrometer |
| CN111175282A (en) * | 2020-02-24 | 2020-05-19 | 江苏师范大学 | Raman spectrometer based on objective signal acquisition |
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