CN203606288U - Confocal micro-raman and laser-induced breakdown spectroscopy combined laser spectrum analysis meter - Google Patents
Confocal micro-raman and laser-induced breakdown spectroscopy combined laser spectrum analysis meter Download PDFInfo
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- CN203606288U CN203606288U CN201320817233.1U CN201320817233U CN203606288U CN 203606288 U CN203606288 U CN 203606288U CN 201320817233 U CN201320817233 U CN 201320817233U CN 203606288 U CN203606288 U CN 203606288U
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Abstract
The utility model proposes a confocal micro-raman (Raman) and laser-induced breakdown spectroscopy (LIBS) combined laser spectrum analysis meter. The analysis meter comprises a micro-raman system, a micro-LIBS system, a high-resolution microscopic imaging system, a confocal microscopic optical path, a spectrum receiving system with a time resolution function, and the like; and a white-light microscopic imaging observation mode, an automatic focus model, an LIBS spectrum work mode, a raman spectrum work mode and the like can be automatically converted. The confocal micro-raman and laser-induced breakdown spectroscopy combined laser spectrum analysis meter has significant characteristics that compact combination of Raman and LIBS is realized by using a confocal microscopy system, qualitative and quantitative analysis of substance elements and molecular structures at the same tiny position can be realized; in combination with the high-resolution imaging function, and spatial discrimination chemical analysis of the elements and the substance structures at the micrometer scale can be carried out, so as to obtain complete information about spatial distribution images and the like of chemical elements, substance structures and physical conditions of the sample.
Description
Technical field
The utility model relates to material element and analysis of the molecular structure field, especially utilizes spectrographic method testing sample same point to be done on micro-meter scale to ultimate analysis and the structure of matter analysis field of spatial discrimination.
Background technology
In recent years, Laser-induced plasma spectroscopy (be called for short LIBS) is owing to having high sensitivity, without sample pretreatment and realize the advantages such as multielement measurement, becomes a kind of new element analysis technology.There is real-time, quick, on-the-spot in situ detection and multielement and detect simultaneously, without advantages such as sample preparations, can carry out chemical analysis to variform materials such as solid, liquid, gases.LIBS spectrometer can still can not be measured sample molecule structure by measurement of species element.
Raman spectrum (Raman) can disclose organic and the molecule of dead matter and the vibration mode of crystal, and the frequency displacement information of Raman spectrometer by Raman spectrum can recognition material composition, still can not measure the element in sample.
In addition common LIBS spectral instrument needs high-octane pulsed laser, conventionally needs single pulse energy to want tens millis burnt, so that Laser Focusing produces sufficiently high energy density to sample surfaces, excited sample produces plasma.
Utility model content
The purpose of this utility model is for current laser-induced breakdown plasma light spectral technology and Raman spectral technique advantage separately, provide a kind of can measurement of species element again can measurement of species molecular structure the burnt micro-Raman of copolymerization and Laser-induced Breakdown Spectroscopy coupling laser spectral analysis instrument, this analyser shares an optical system, share a set of spectrometer, there is volume little, the advantages such as function is strong, and the energy of lasers requirement to generation LIBS spectrum and Raman spectrum is low, and micro-burnt magnitude laser instrument can meet use.
Technical solution of the present utility model is:
The burnt micro-Raman of copolymerization and Laser-induced Breakdown Spectroscopy coupling laser spectral analysis instrument, comprise control system, micro-LIBS system, micro-Raman system, micro imaging system and confocal laser transmission and spectrum receiving system;
Described control system comprises programmed control all-in-one (22) and control circuit (21); Described programmed control all-in-one for accept control circuit transmit spectroscopic data and to control circuit sending controling instruction; The spectroscopic data that described control circuit sends for control time delay, receiving spectrum receiving system, and control micro-LIBS system, micro-Raman system and micro imaging system;
Described micro imaging system comprises incandescent lamp (11), lens two (12), semi-transparent semi-reflecting lens (12), beam splitter (14), imaging len (15), CCD camera (16), for placing the three-dimensional mobile platform of precision (19) of sample and being arranged on the microcobjective (18) above accurate three-dimensional mobile platform; After the focusing of the reflection of the expanding of the light scioptics two that described incandescent lamp sends, semi-transparent semi-reflecting lens, the reflection of beam splitter, microcobjective, be radiated on sample, by CCD camera, sample surfaces low-light structure and laser made a video recording in sample surfaces focal beam spot situation; The light of described sample reflection is incident to CCD camera by the expanding of microcobjective, the reflection of beam splitter, the transmission of semi-transparent semi-reflecting lens, imaging len after converging;
Described confocal laser transmission and spectrum receiving system comprise spectrometer, ICCD camera and are successively set on pin hole two (7), zero angle notch filter sheet (6), plus lens (5), the fibre-optical probe of microcobjective top, described fibre-optical probe accesses spectrometer by optical fiber, and described spectrometer output signal is sent into ICCD camera; Described ICCD camera is connected with control circuit;
Described micro-LIBS system comprises solid pulse laser (1), lens one (2), low pass filters (17); The output light of described solid pulse laser expands, produces LIBS spectrum at sample surfaces after the converging of low pass filters reflection, microcobjective through lens one;
Described micro-Raman system comprises continuous wave laser 10, is successively set on pin hole one (9) and 45 degree notch filter sheets (8) on laser instrument output light path; Described laser instrument output light produces Raman spectrum at sample surfaces after the converging of the reflection of 45 degree notch filter sheets, microcobjective;
Described low pass filters, beam splitter, 45 degree notch filter sheets are successively set between microcobjective and pin hole two from bottom to top.
Based on above-mentioned basic scheme, the utility model also does following optimization and limits and improve:
Said lens one is plano-concave lens, and its installation site meets following geometric relationship: laser beam expanding reverse extending line intersection point overlaps with this lens virtual focus, and this lens light path and microcobjective light path form the burnt light path system of empty copolymerization.
The aperture size of above-mentioned pin hole two is adjustable, and the LIBS signal after microcobjective is collected and Raman signal focus, in this pin hole position, are realized the micro-focusing-detection altogether of LIBS signal and Raman signal.
Above-mentioned continuous wave laser adopts 532nm or 785nm continuous wave laser; Described beam splitter is 20:80 beam splitter; Described solid pulse laser adopts the 1064nm YAG solid state laser of the micro-burnt magnitude pulse energy of hundreds of; Described spectrometer is for being with time-resolved CT or middle ladder ICCD spectrometer.
The utility model advantage:
1, this patent instrument comprises micro-Raman system, micro-LIBS system, high-resolution imaging system, micro-focused light passages altogether and has the spectrum receiving system etc. of time resolution function, conversion of white light micro-imaging observing pattern, autofocus mode, LIBS spectrum mode of operation, Raman spectrum mode of operation etc. automatically.When this instrument works in LIBS pattern, by solid pulse laser Emission Lasers bundle, this laser beam is focused onto testing sample surface and produces high-temperature plasma, the outside characteristic spectral line of radiation element in the cooling process of plasma, and these spectral lines are surveyed by spectrometer.Utilize the spectral line of emission of these plasmas to carry out qualitative or quantitative test to the element chemistry composition of sample.When this instrument works in Raman pattern, by continuous wave laser Emission Lasers bundle, this laser beam is focused onto testing sample same position surface, in sample surfaces transmitting Raman scattering, this raman scattering spectrum is surveyed by spectrometer, frequency displacement by Raman spectrum discloses organic and the molecule of dead matter and the vibration mode of crystal, and material composition qualitative and quantitative analysis is provided.Distinguishing feature of the present utility model is to utilize micro-confocal system to realize Raman and the compact coupling of LIBS, can realize the qualitative and quantitative analysis of same small position material element and molecule molecular structure, in conjunction with high-resolution imaging function, can on micro-meter scale, do ultimate analysis and the structure of matter analysis of spatial discrimination, obtain the complete informations such as the space distribution image of chemical element, composition and the physical condition of sample.
2, the utility model adopts incandescent lamp to illuminate sample, utilizes ccd image to process and determines the focal plane of sample to microcobjective, and in micro-meter scale high resolving power, sample surfaces is carried out to imaging.
3, the utility model LIBS system, Raman system, spectrum collection system all adopt laser co-focusing optical system, and incandescent lamp, CCD, diaphragm one, diaphragm two are by microcobjective copolymerization Jiao.Adopt same light path collection system respectively the spectrum of two kinds of phenomenons to be collected, analyzed, on micro-meter scale, do ultimate analysis and the structure of matter analysis of spatial discrimination, obtain the complete informations such as the space distribution image of chemical element, composition and the physical condition of sample.
4, the utility model adopts confocal system, so the requirement of laser energy energy is reduced, micro-burnt magnitude laser instrument can meet use.
Accompanying drawing explanation
Fig. 1 is the structure principle chart of the utility model analyser; Wherein: 1-1064nm solid pulse laser; 2-lens one (extender lens group); 3a-ICCD; 3b-spectrometer; 4a-fibre-optical probe; 4b-optical fiber; 5-plus lens; 6-zero angle notch filter sheet; 7-pin hole two (diaphragm two); 8-45 degree 532nm notch filter sheets; 9-pin hole one (diaphragm one); 10-532nm continuous wave laser; 11-incandescent lamp; 12-lens two; 13-semi-transparent semi-reflecting lens; 14-beam splitter; 15-imaging len; 16-CCD camera; 17-low pass filters; 18-microcobjective; 19-accurate three-dimensional mobile platform; 20-test sample, 21-control circuit, 22-programmed control all-in-one.
Fig. 2 is the utility model method implementing procedure figure.
Fig. 3 is the defeated schematic diagram of LIBS analysis result of an embodiment of the utility model.
Fig. 4 is the Raman analysis result output schematic diagram of an embodiment of the utility model.
Embodiment
The micro-Raman of laser co-focusing and LIBS coupling spectroanalysis instrument, this instrument comprises micro-LIBS system, micro-Raman system, micro imaging system and confocal laser transmission and spectrum receiving system.
This device adopts incandescent lamp to illuminate sample, utilizes ccd image to process and determines the focal plane of sample to microcobjective, and in micro-meter scale high resolving power, sample surfaces is carried out to imaging.
This device adopts 532nm or 785nm continuous laser as Raman excitation source.
This device adopts 1064nm pulse laser as LIBS excitation source.
As shown in Figure 1 and Figure 2, workflow of the present utility model is as follows:
Opening program control all-in-one 22, opens incandescent lamp 11, regulates microcobjective 18 and accurate three-dimensional to move platform 19, until sample stops when imaging clearly is visible on CCD16 regulating, closes incandescent lamp 11.Start 532nm laser instrument 10, laser is reflected by 45 degree 532nm notch filter sheets 8 by pin hole 1 is rear, converge to sample surfaces through microcobjective and produce Raman spectrum, the spectrum producing passes through microcobjective, Yan Yuan returns on road after 20:80 beam splitter 14 20% light reflection and enters CCD and carry out moment picture collection, after 80% light transmission by after co-focusing imaging through needle passing hole 27, then by 6 filtering again of zero angle 532nm notch filter sheet, finally enter fibre-optical probe 4 by plus lens 5, regulate relative delay to start ICCD spectrometer 3a and gather incident light spectrum, carry out the analysis of molecular structure, close subsequently 532nm laser instrument, open 1064nm laser instrument 1, laser is low pass filtering sheet reflection after by extender lens group 2 and enters microcobjective and converge to sample surfaces and produce LIBS spectrum, the spectrum producing passes through microcobjective, Yan Yuan returns on road after 20:80 beam splitter 14 20% light reflection and enters CCD and carry out picture collection, after 80% light transmission by after co-focusing imaging through needle passing hole two, then enter fibre-optical probe by plus lens, regulate relative delay to start ICCD spectrometer and gather incident light spectrum, sample element is analyzed, finally obtain the analysis result of sample element and structure.
This device LIBS system, Raman system, spectrum collection system all adopt laser co-focusing optical system, and incandescent lamp, CCD, diaphragm one, diaphragm two are by microcobjective copolymerization Jiao.Adopt same light path collection system respectively the spectrum of two kinds of phenomenons to be collected, analyzed, on micro-meter scale, do ultimate analysis and the structure of matter analysis of spatial discrimination, obtain the complete informations such as the space distribution image of chemical element, composition and the physical condition of sample.
Claims (4)
1. the burnt micro-Raman of copolymerization and Laser-induced Breakdown Spectroscopy coupling laser spectral analysis instrument, comprises control system, micro-LIBS system, micro-Raman system, micro imaging system and confocal laser transmission and spectrum receiving system;
Described control system comprises programmed control all-in-one (22) and control circuit (21); Described programmed control all-in-one for accept control circuit transmit spectroscopic data and to control circuit sending controling instruction; The spectroscopic data that described control circuit sends for control time delay, receiving spectrum receiving system, and control micro-LIBS system, micro-Raman system and micro imaging system;
Described micro imaging system comprises incandescent lamp (11), lens two (12), semi-transparent semi-reflecting lens (12), beam splitter (14), imaging len (15), CCD camera (16), for placing the three-dimensional mobile platform of precision (19) of sample and being arranged on the microcobjective (18) above accurate three-dimensional mobile platform; After the focusing of the reflection of the expanding of the light scioptics two that described incandescent lamp sends, semi-transparent semi-reflecting lens, the reflection of beam splitter, microcobjective, be radiated on sample, by CCD camera, sample surfaces low-light structure and laser made a video recording in sample surfaces focal beam spot situation; The light of described sample reflection is incident to CCD camera by the expanding of microcobjective, the reflection of beam splitter, the transmission of semi-transparent semi-reflecting lens, imaging len after converging;
Described confocal laser transmission and spectrum receiving system comprise spectrometer, ICCD camera and are successively set on pin hole two (7), zero angle notch filter sheet (6), plus lens (5), the fibre-optical probe of microcobjective top, described fibre-optical probe accesses spectrometer by optical fiber, and described spectrometer output signal is sent into ICCD camera; Described ICCD camera is connected with control circuit;
Described micro-LIBS system comprises solid pulse laser (1), lens one (2), low pass filters (17); The output light of described solid pulse laser expands, produces LIBS spectrum at sample surfaces after the converging of low pass filters reflection, microcobjective through lens one;
Described micro-Raman system comprises continuous wave laser 10, is successively set on pin hole one (9) and 45 degree notch filter sheets (8) on laser instrument output light path; Described laser instrument output light produces Raman spectrum at sample surfaces after the converging of the reflection of 45 degree notch filter sheets, microcobjective;
Described low pass filters, beam splitter, 45 degree notch filter sheets are successively set between microcobjective and pin hole two from bottom to top.
2. the burnt micro-Raman of copolymerization and Laser-induced Breakdown Spectroscopy coupling laser spectral analysis instrument according to claim 1, it is characterized in that: described lens one are plano-concave lens, its installation site meets following geometric relationship: laser beam expanding reverse extending line intersection point overlaps with this lens virtual focus, and this lens light path and microcobjective light path form the burnt light path system of empty copolymerization.
3. according to the burnt micro-Raman of copolymerization described in claim 1 or 2 and Laser-induced Breakdown Spectroscopy coupling laser spectral analysis instrument, it is characterized in that: the aperture size of described pin hole two is adjustable, LIBS signal after microcobjective is collected and Raman signal focus, in this pin hole position, are realized the micro-focusing-detection altogether of LIBS signal and Raman signal.
4. the burnt micro-Raman of copolymerization and Laser-induced Breakdown Spectroscopy coupling laser spectral analysis instrument according to claim 3, is characterized in that: described continuous wave laser adopts 532nm or 785nm continuous wave laser; Described beam splitter is 20:80 beam splitter; Described solid pulse laser adopts the 1064nm YAG solid state laser of the micro-burnt magnitude pulse energy of hundreds of; Described spectrometer is for being with time-resolved CT or middle ladder ICCD spectrometer.
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| CN103743718A (en) * | 2013-12-11 | 2014-04-23 | 中国科学院西安光学精密机械研究所 | Laser spectrum analyzer combining confocal micro-Raman spectrometer with laser-induced breakdown spectrometer |
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| CN104677884A (en) * | 2015-03-17 | 2015-06-03 | 北京理工大学 | High-spatial-resolution laser spectral-pupil differential confocal mass spectrum microscopic imaging method and device |
| CN105067568A (en) * | 2015-07-16 | 2015-11-18 | 河南科技大学 | Automatic focusing laser-induced breakdown spectroscopy detection system and detection method thereof |
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- 2013-12-11 CN CN201320817233.1U patent/CN203606288U/en not_active Withdrawn - After Issue
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| CN103743718B (en) * | 2013-12-11 | 2015-12-23 | 中国科学院西安光学精密机械研究所 | The burnt microscopic Raman of copolymerization and Laser-induced Breakdown Spectroscopy coupling laser spectral analysis instrument |
| CN103743718A (en) * | 2013-12-11 | 2014-04-23 | 中国科学院西安光学精密机械研究所 | Laser spectrum analyzer combining confocal micro-Raman spectrometer with laser-induced breakdown spectrometer |
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| CN105067568A (en) * | 2015-07-16 | 2015-11-18 | 河南科技大学 | Automatic focusing laser-induced breakdown spectroscopy detection system and detection method thereof |
| CN105067568B (en) * | 2015-07-16 | 2017-10-20 | 河南科技大学 | Automatic focusing LIBS detecting system and its detection method |
| CN105588640A (en) * | 2016-03-08 | 2016-05-18 | 中国科学院半导体研究所 | Multifunctional microscopic confocal spectrometer |
| CN105737986B (en) * | 2016-03-08 | 2019-02-01 | 中国科学院半导体研究所 | Multi-functional micro confocal spectrometer |
| CN105588640B (en) * | 2016-03-08 | 2017-10-03 | 中国科学院半导体研究所 | Multi-functional micro confocal spectrometer |
| CN105737986A (en) * | 2016-03-08 | 2016-07-06 | 中国科学院半导体研究所 | Multifunctional microscopic confocal spectrometer |
| CN106596511A (en) * | 2016-12-27 | 2017-04-26 | 南京先进激光技术研究院 | Reflection type coaxial structure laser-induced breakdown spectroscopy analysis device |
| CN107820567A (en) * | 2017-08-03 | 2018-03-20 | 深圳前海达闼云端智能科技有限公司 | Raman detection method, apparatus and storage medium |
| CN107820567B (en) * | 2017-08-03 | 2022-08-09 | 北京云端光科技术有限公司 | Raman detection method, device and storage medium |
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| CN108717057A (en) * | 2018-05-31 | 2018-10-30 | 中央民族大学 | A kind of portable surface enhancing Raman spectrometer and its measurement method |
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| CN110231332A (en) * | 2019-07-03 | 2019-09-13 | 榆林学院 | The coherent anti-stokes raman scattering spectral device and method simplified using super steep filter plate |
| CN110231332B (en) * | 2019-07-03 | 2022-01-11 | 榆林学院 | Coherent anti-Stokes Raman scattering spectrum device and method simplified by utilizing super-steep filter plate |
| CN111880072A (en) * | 2020-08-21 | 2020-11-03 | 天津大学 | Method for characterizing 4H-SiC electrical properties by Raman spectrum based on photon-generated carrier effect |
| 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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| AV01 | Patent right actively abandoned |
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| C25 | Abandonment of patent right or utility model to avoid double patenting |