CN204214779U - Based on the device that conllinear Laser-induced Breakdown Spectroscopy crop alimentary element detects fast - Google Patents
Based on the device that conllinear Laser-induced Breakdown Spectroscopy crop alimentary element detects fast Download PDFInfo
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- CN204214779U CN204214779U CN201420688747.6U CN201420688747U CN204214779U CN 204214779 U CN204214779 U CN 204214779U CN 201420688747 U CN201420688747 U CN 201420688747U CN 204214779 U CN204214779 U CN 204214779U
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/718—Laser microanalysis, i.e. with formation of sample plasma
Abstract
The utility model discloses a kind of device detected fast based on conllinear Laser-induced Breakdown Spectroscopy crop alimentary element, comprise the Double-impulse solid laser for generation of coaxial double-pulse laser, the repetition frequency of Double-impulse solid laser is 1 ~ 10Hz, the energy of laser 532nm is 80 ~ 200mJ, the energy of laser 1064nm is 80 ~ 300mJ, and the interval time between two bundle laser is 200 ~ 2000ns; Optical axis along described Double-impulse solid laser is furnished with energy attenuator successively, light path climbs system and sample stage, by light path climb system exit laser vertical impact sample surfaces produce plasma; Also comprise signal acquisition and processing system, gather plasma and cool the characteristic spectral line sent, and input the data model established, calculate the content of nutrient.The utility model achieves the quick detection of crop alimentary element, has simple to operate, the features such as cost is low.Effectively overcome the feature of traditional detection method length detection time, complicated operation, avoid the pollution of chemical reagent to environment.
Description
Technical field
The utility model relates to crop alimentary Element detection technology, particularly a kind of device detected fast based on conllinear Laser-induced Breakdown Spectroscopy crop alimentary element.
Background technology
Upgrowth situation and the output of crop alimentary element (nitrogen, phosphorus, potassium etc.) and crop are closely related.Nitrogen, phosphorus, potassium are the large main nutrient elements of crop three.Nitrogen is the constituent of pigment, can promote photosynthesis of plant, increases crop yield; Phosphorus is the component of crop multiple compounds, has material impact to crop quality; Potassium can promote crop photosynthesis, strengthens crop anti-adversity.Obtain the upgrowth situation that crop alimentary element information is conducive to understanding crop, the nutritional deficiency situation according to crop realizes early stage quantitative fertilization.At present, the detection method of crop alimentary element mainly contains triumphant formula nitriding, Du Mashi combustion method, colourimetry, flame combustion process etc.But these method complicated operations, cost are high, usually need consume a large amount of chemical reagent and cause environmental pollution, the requirement of field-crop nutritional information quick obtaining cannot be met.
Laser induced breakdown spectrograph (Laser-Induced Breakdown Spectroscopy, LIBS) plasma ablation utilizing pulse laser to produce material in excited sample (being generally solid), and obtain by spectrometer the spectrum that activated plasma atom launches, identify the element constituent in sample with this, and then the identification of material, classification, qualitative and quantitative test can be carried out.This technology, without the need to carrying out pre-service to sample, can realize long-range, micro-damage fast and detect sample element (especially metallic element), can be used for the detection of solid, gas, fluid sample.In recent years, LIBS development rapidly, is widely used in multiple field, as heavy metal analysis and explosive detection etc. in biomedicine, archaeology, environmental monitoring, water.
Application LIBS energy quick obtaining crop alimentary information, is conducive to realizing agriculture precision, intelligentize and informatization.But because Laser-induced Breakdown Spectroscopy amount of analysis is very little, matrix effect has obvious impact to analysis result.Therefore crop sample is needed usually to the repeatability carrying out sample preparation compressing tablet to ensure detecting.
Utility model content
The utility model provides a kind of crop alimentary element device for fast detecting, achieves and detects fast crop compressing tablet nutrient based on Laser-induced Breakdown Spectroscopy, can meet the detection of Different Crop laser spectrum simultaneously, there is system fading margin convenient, cost is low, detects fast, the features such as micro-damage.
A kind of device detected fast based on conllinear Laser-induced Breakdown Spectroscopy crop alimentary element, comprise the Double-impulse solid laser for generation of coaxial double-pulse laser, the repetition frequency of described Double-impulse solid laser is 1 ~ 10Hz, the energy of laser 532nm is 80 ~ 200mJ, the energy of laser 1064nm is 80 ~ 300mJ, and the interval time between two bundle laser is 200 ~ 2000ns; Optical axis along described Double-impulse solid laser is furnished with energy attenuator successively, light path climbs system and sample stage, by light path climb system exit laser vertical impact sample surfaces produce plasma; Also comprise signal acquisition and processing system, gather plasma and cool the characteristic spectral line sent, and input the data model established, calculate the content of nutrient.
Preferably, described signal acquisition and processing system comprises: optical fiber collection system, cools for collecting plasma the characteristic spectral line sent; Beam splitting system, for carrying out light splitting to characteristic spectral line; ICCD detector, for being converted to electric signal by the light signal of beam splitting system; Computing machine, according to described electric signal, inputs the data model established, calculates the content of nutrient.
Preferably, described beam splitting system is echelle spectrometer.
Echelle spectrometer is the spectrometer using echelle grating as dispersion element, disposablely can obtain full modal data without the need to raster scanning, can avoid conventional spectrograph hyperchannel head and the tail section Bonding Problem.Echelle spectrometer inner inorganic tool part, stability is higher, and resolution can reach 0.08nm, can meet spectral line light splitting requirement.
Preferably, described light path system of climbing is made up of the first catoptron arranged successively, the second catoptron and the 3rd catoptron, and described second catoptron is positioned at directly over the first catoptron, and the 3rd catoptron is positioned at directly over sample stage.
The light path system of climbing is mainly used in lifting light path, and will in the horizontal direction laser conversion for vertically to propagate.The application light path system of climbing effectively can be avoided raising laser positions and cause the laser factors of instability.Laser impacts sample surfaces directly over sample, is conducive to effectively exciting of plasma, ensures that plasma uniformity is symmetrical.
Preferably, the first described catoptron, the second catoptron and the 3rd catoptron all adopt 1 inch of double frequency Nd:YAG laser mirror, and the reflectivity at 532nm, 1064nm place is more than 98%.
Optical maser wavelength due to Double-impulse solid laser is 532nm and 1064nm, for reducing the loss of laser energy at light path system, ensure the effective rate of utilization of laser energy, described catoptron all adopts double frequency Nd:YAG laser mirror, and its reflectivity at 532nm, 1064nm place is more than 98%.
Preferably, described sample stage comprises the electric displacement platform with four-degree-of-freedom, the objective table being movably arranged on the lifter plate on electric displacement platform and being slidably fitted on electric displacement platform; Described lifter plate is provided with transparent constraint window, impacts sample after laser light constraint window; The below of described lifter plate is provided with restraining plate, and this restraining plate is placed in directly over sample, and restraining plate is distributed with constraint chamber, this constraint chamber is for retraining the plasma of sample excitation.
Sample stage, by space constraint enhanced line intensity, can laterally and longitudinally retrain by plasma, and regulates constraint space size adjustment line strength according to different sample requirement, and it is 2 ~ 10 times that line strength strengthens scope.Constraint window is mainly used in plasma and longitudinally retrains, and has good transmissivity to the characteristic spectral line of incident laser and plasma generation.The transverse direction that restraining plate is mainly used in plasma retrains, and makes characteristic spectral line carry out constraint propagation, improves spectral line collection efficiency and line strength.
Preferably, described lifter plate is provided with printing opacity mouth, and this printing opacity mouth place is coated with light-passing board, the constraint window described in described printing opacity mouth and light-passing board form.
Wherein, light-passing board is poly (methyl methacrylate) plate, and the selection of material is N-BK7, and thickness is 1 ~ 5mm, and transmitance is greater than 90%, and energy threshold is greater than 10J/cm
2.Line enhancement effect suffers restraints the impact of window from sample distance.Because properties of samples is different with the element spectral line intensity that will detect, constraint window of the present utility model can move in the vertical direction, regulates line strength as required.For ensureing that laser effectively excites the effective collection with characteristic spectral line, the transmitance of light-passing board to optical maser wavelength and characteristic spectral line should be greater than 90%.Meanwhile, for preventing laser from causing damage to poly (methyl methacrylate) plate, its energy threshold should be greater than 10J/cm
2.
The beneficial effect that the utility model has is:
(1) parameter of energy quick adjustment instrument, realizes the optimization of optimum detection parameter;
(2) achieve the quick detection of crop alimentary element, have simple to operate, the features such as cost is low.Effectively overcome the feature of traditional detection method length detection time, complicated operation, avoid the pollution of chemical reagent to environment.
(3) sample stage is by space constraint enhanced line intensity, laterally and longitudinally can retrain by plasma, improves spectral line collection efficiency and line strength; Can avoid exciting particle again to cover sample surfaces; And smooth sample surfaces, make sample remain unchanged to the distance of condenser lens thus improve detection repeatability.
Accompanying drawing explanation
Fig. 1 is the structure drawing of device that crop alimentary element detects fast;
Fig. 2 is the structural drawing of sample stage;
Fig. 3 is the vertical view of sample stage in Fig. 2.
Embodiment
As shown in Figure 1, based on the device that conllinear Laser-induced Breakdown Spectroscopy crop alimentary element detects fast, comprise Double-impulse solid laser 1, delay time generator 2, energy attenuator 3, laser energy real-time monitoring system 4, light path is climbed system 5, detector 6, spectrometer 7, sample stage 8, condenser lens 9, optical fiber collection system 10 and sample surface imaging system 11.
Double-impulse solid laser 1 has 4 kinds of working methods: (1) 1064nm coaxially exports, and (2) 532nm coaxially exports, and the different axle of (3) 1064nm exports the different axle of (4) 1064nm, 532nm and exports.Double-impulse solid laser 1 can be realized by 2 monopulse 1064nm solid state lasers, frequency-doubling crystal and conjunction beam optical paths.The repetition frequency of Double-impulse solid laser 1 is 1-10Hz, and energy is 80-200mJ (@532nm), 80-300mJ (@1064nm), and the interval time between two bundle laser is 200 ~ 2000ns.
Delay time generator 2 controls the gate duration that Double-impulse solid laser 1 adjusts the Q triggered time, xenon lamp opens triggered time and ICCD detector.Delay time generator arranges Double-impulse solid laser and adjusts the triggered time of Q signal 150 ± 20 μ s after xenon lamp signal triggers.Optimize control opening time of detector be the second road laser Q-switching switch triggering time after 1.5 μ s.
Energy attenuator 3 is made up of half-wave plate 31 and the first beam splitter 32.Laser energy real-time monitoring system 4 comprises thermoelectric pulse probe the 42, second beam splitter 41, USB connecting line and computing machine 13.
Light path system 5 of climbing is made up of the first catoptron 52, second catoptron 51 and the 3rd catoptron 53,1 inch of double frequency Nd:YAG laser mirror selected by first catoptron 52, second catoptron 51 and the 3rd catoptron 53, and the reflectivity at 532nm, 1064nm place is more than 98%.
Optical fiber collection system 10 is made up of light collector and optical fiber.Sample surface imaging system 11, for monitoring laser impact position, comprises CCD camera 114, imaging lens 113, the 3rd beam splitter 112, LED light source for illuminating 111.
Detector 6 is ICCD detector.Spectrometer 7 is echelle spectrometer.
Condenser lens 9 is installed on to be had in the Lens mounting carrier regulating degree of freedom along optical axis direction, for regulating the distance of sample and lens, thus controls impact to the laser parameter on sample.N-BK7 selected by condenser lens, and plating V-arrangement film, it is less than 0.25% at the reflectivity at 532nm, 1064nm place.
As shown in Figures 2 and 3, sample stage 8 comprises gear rack elevating bar 901, gear slider 902, right angle card extender 903, plasma confinement window 904, cylindrical guide 905, plasma confinement plate 906, V-type slide block 907, combined electrical moving stage 909, pull bar 910, constraint chamber 911.Combined electrical moving stage 909 adopts four-degree-of-freedom (x, y, z, w) combined electrical moving stage, comprises three single-degree-of-freedoms (x, y and z) pulse electric displacement platform and rotary freedom (w) electric rotary table.Gear rack elevating bar 901 is vertically arranged in combined electrical moving stage 909, and gear slider 902 engages with gear rack elevating bar 901, can be lower mobile in the vertical direction.Right angle card extender 903 is secured by bolts on gear slider 902, and plane is provided with the printing opacity mouth of rectangle, and printing opacity mouth edge is provided with support level, is provided with light-passing board in printing opacity mouth, forms plasma confinement window 904.Cylindrical guide 905 is fixed on combined electrical moving stage 909, and plasma confinement plate 906 can slide up and down along cylindrical guide 905.Cylindrical guide 905 and gear rack elevating bar 901 all by bolt-connection in combined electrical moving stage 909.Combined electrical moving stage 909 has V-type groove, and V-type slide block 907 can horizontally slip along V-type groove under pull bar 910 acts on, and pull bar 910 is by being screwed in V-type slide block 907.Sample 908 is placed on V-type slide block 907 (being equivalent to objective table), laser impacts downwards from top, by plasma confinement window 904, and through plasma confinement plate 906, impact is to sample surfaces, activated plasma, cooling sends characteristic spectral line and is collected by optical fiber collection system 10.
The material of plasma confinement window 904 is N-BK7, and thickness is 1 ~ 5mm, and transmitance is greater than 90%, and energy threshold is greater than 10J/cm
2.Plasma confinement window 904 is mainly used in plasma and longitudinally retrains, and has good transmissivity to the characteristic spectral line of incident laser and plasma generation.N-BK7 is a kind of common optical glass, can through the light of 350nm ~ 2000nm wave band, and the transmissivity of its laser is greater than 90%, and energy threshold is greater than 10J/cm
2.Therefore plasma confinement window 904 the selection of material is N-BK7, and thickness is 1 ~ 3m.Plasma confinement window 904 vertically can move under gear slider 902 acts on.Line enhancement effect suffers restraints the impact of window from sample distance.Because properties of samples is different with the element spectral line intensity that will detect, plasma confinement window 904 of the present utility model can move in the vertical direction, regulates line strength as required.
In the present embodiment, the material of plasma confinement plate 906 is the aluminium sheet of chromium plating, and thickness is 1mm, and be evenly distributed with conical constraint chamber 911 in the middle of it, upper conical surface diameter and lower conical surface diameter are 2mm and 3mm respectively.With combined electrical moving stage 909, the spacing in constraint chamber 911 should plan that displacement is consistent.The transverse direction that plasma restraining plate 6 is mainly used in plasma retrains, and makes characteristic spectral line carry out constraint propagation, improves spectral line collection efficiency and line strength, and it is 2 ~ 10 times that line strength strengthens scope.In the constraint chamber 911 of aluminium sheet, carry out chromium plating, make inner chamber have higher reflectivity, make characteristic spectral line constraint propagation, improve spectral line collection efficiency.Constraint chamber adopts conical structure, and due to the structure that it is up-small and down-big, the structure compared with column type better can obtain plasma and retrain.In addition, when plasma is from taper shape constraint chamber injection, because its space constraint strengthens, its electron density and movement velocity all can be enhanced, therefore advantageously in the enhancing of spectral line signal.With combined electrical moving stage 909, the spacing in the constraint chamber of plasma confinement plate 906 of the present utility model plans that displacement is consistent, can be applicable to the working method of Laser-induced Breakdown Spectroscopy Surface scan.The utility model using plasma restraining plate 906 covers sample surfaces, is conducive to smooth sample surfaces and improves detection repeatability, avoid exciting other region to be measured of particle contamination simultaneously.When testing sample is the surface irregularity samples such as fresh blade, its region to be measured and lens distance there are differences, and then affect the laser parameter that laser arrives sample.The detection stability of Laser-induced Breakdown Spectroscopy and the laser parameter in region to be detected closely bound up, therefore smooth sample surfaces be conducive to fixed laser parameter improve detect repeatability.In addition, the up-small and down-big conical structure of plasma confinement plate 906 is conducive to farthest avoiding exciting particle contamination by a upper surveyed area, ensures that institute's detected object is the element in region to be detected.
V-type slide block 907 can move along V-type groove under pull bar 910 acts on, and adopts this V-type sliding block guide track structure, avoids raising the troublesome operation such as plasma confinement window mouth and plasma restraining plate.Connection between plasma confinement plate 906 and cylindrical guide 905 is stressed joint, and plasma confinement plate 906 can not freely glide under gravity.
During the work of this sample stage, it is corresponding with the position of top laser that control combination electric displacement platform 909 makes the pyramid type of plasma confinement plate 906 retrain chamber 911, and the work step-length arranging combined electrical moving stage 909 is conical constraint chamber neighbor distance or multiple.Coaxial double-pulse laser is through light path system, and line focus lens are propagated downwards from top, through plasma confinement window 904, and through conical constraint chamber impact sample.Its laser transmittance of plasma confinement window 904 is greater than 90%, and energy threshold is greater than 10J/cm
2.Plasma cooling sends characteristic spectral line and is collected by the optical fiber collection system 10 of top.The number of times of required impact can be selected in each position according to actual requirement, moved carry out multiple positions spectra collection after completing a position by combined electrical moving stage 909.When without plasma confinement window 904 and plasma confinement plate 906, the plasma inspired is free excited state; After limiting the plasma excited, the density of plasma increases, and plasma temperature raises, and enhances line strength of excited atom.
Delay time generator 2 controls Q-switch triggered time and the xenon lamp unlatching triggered time of Double-impulse solid laser 1.Under delay time generator 2 controls, Double-impulse solid laser 1 produces coaxial 532nm (1064nm) double-pulse laser.Laser is decayed through energy attenuator 3 pairs of laser energies.Control from beam splitter 32 energy out by rotating half-wave plate 31.After decay, laser is respectively through the first catoptron 52 and the second catoptron 51, then changes light path through the 3rd catoptron 53, propagates downwards.Laser focuses on impact sample surfaces through condenser lens 9, produces plasma.The characteristic spectral line that plasma cooling produces is collected through optical fiber collection system 10, through spectrometer 7 light splitting, be finally converted into electric signal by the photomultiplier on detector 6, be connected on computing machine 12 by USB, by the model database established, calculate crop alimentary constituent content.
Inventive point of the present utility model only relates to light path design and apparatus structure, and after acquisition characteristics spectral line information, the existing technology of computer utility, can calculate the content of crop alimentary element, does not relate to the improvement in software and computing method.
The foregoing is only better implementation example of the present utility model, be not limited to the utility model, all within the utility model spirit and principle, any amendment done, equivalent replacement, improvement etc., all should be included within protection domain of the present utility model.
Claims (7)
1. the device detected fast based on conllinear Laser-induced Breakdown Spectroscopy crop alimentary element, it is characterized in that, comprise the Double-impulse solid laser for generation of coaxial double-pulse laser, the repetition frequency of described Double-impulse solid laser is 1 ~ 10Hz, the energy of laser 532nm is 80 ~ 200mJ, the energy of laser 1064nm is 80 ~ 300mJ, and the interval time between two bundle laser is 200 ~ 2000ns;
Optical axis along described Double-impulse solid laser is furnished with energy attenuator successively, light path climbs system and sample stage, by light path climb system exit laser vertical impact sample surfaces produce plasma;
Also comprise signal acquisition and processing system, gather plasma and cool the characteristic spectral line sent, and input the data model established, calculate the content of nutrient.
2. the device detected fast based on conllinear Laser-induced Breakdown Spectroscopy crop alimentary element as claimed in claim 1, it is characterized in that, described signal acquisition and processing system comprises:
Optical fiber collection system, cools for collecting plasma the characteristic spectral line sent;
Beam splitting system, for carrying out light splitting to characteristic spectral line;
ICCD detector, for being converted to electric signal by the light signal of beam splitting system;
Computing machine, according to described electric signal, inputs the data model established, calculates the content of nutrient.
3. the device detected fast based on conllinear Laser-induced Breakdown Spectroscopy crop alimentary element as claimed in claim 2, it is characterized in that, described beam splitting system is echelle spectrometer.
4. the device detected fast based on conllinear Laser-induced Breakdown Spectroscopy crop alimentary element as claimed in claim 1, it is characterized in that, described light path system of climbing is made up of the first catoptron arranged successively, the second catoptron and the 3rd catoptron, described second catoptron is positioned at directly over the first catoptron, and the 3rd catoptron is positioned at directly over sample stage.
5. the device detected fast based on conllinear Laser-induced Breakdown Spectroscopy crop alimentary element as claimed in claim 4, it is characterized in that, the first described catoptron, the second catoptron and the 3rd catoptron all adopt 1 inch of double frequency Nd:YAG laser mirror, and the reflectivity at 532nm, 1064nm place is more than 98%.
6. the device detected fast based on conllinear Laser-induced Breakdown Spectroscopy crop alimentary element as claimed in claim 1, it is characterized in that, described sample stage comprises the electric displacement platform with four-degree-of-freedom, the objective table being movably arranged on the lifter plate on electric displacement platform and being slidably fitted on electric displacement platform;
Described lifter plate is provided with transparent constraint window, impacts sample after laser light constraint window;
The below of described lifter plate is provided with restraining plate, and this restraining plate is placed in directly over sample, and restraining plate is distributed with constraint chamber, this constraint chamber is for retraining the plasma of sample excitation.
7. the device detected fast based on conllinear Laser-induced Breakdown Spectroscopy crop alimentary element as claimed in claim 6, it is characterized in that, described lifter plate is provided with printing opacity mouth, and this printing opacity mouth place is coated with light-passing board, the constraint window described in described printing opacity mouth and light-passing board form.
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| CN201420688747.6U CN204214779U (en) | 2014-11-17 | 2014-11-17 | Based on the device that conllinear Laser-induced Breakdown Spectroscopy crop alimentary element detects fast |
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| CN201420688747.6U CN204214779U (en) | 2014-11-17 | 2014-11-17 | Based on the device that conllinear Laser-induced Breakdown Spectroscopy crop alimentary element detects fast |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104374751A (en) * | 2014-11-17 | 2015-02-25 | 浙江大学 | Device for rapidly detecting nutrient elements of crops based on collinear laser-induced breakdown spectroscopy |
| CN113331235A (en) * | 2021-07-05 | 2021-09-03 | 吉林省长春皓月清真肉业股份有限公司 | Slaughtering device |
| US11635386B2 (en) | 2020-11-25 | 2023-04-25 | King Fahd University Of Petroleum And Minerals | Quantification of the micronutrient profile in Moringa oleifera tree leaves using calibration free laser induced breakdown spectroscopy |
-
2014
- 2014-11-17 CN CN201420688747.6U patent/CN204214779U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104374751A (en) * | 2014-11-17 | 2015-02-25 | 浙江大学 | Device for rapidly detecting nutrient elements of crops based on collinear laser-induced breakdown spectroscopy |
| CN104374751B (en) * | 2014-11-17 | 2017-06-20 | 浙江大学 | Device based on conllinear LIBS crop nutrient quick detection |
| US11635386B2 (en) | 2020-11-25 | 2023-04-25 | King Fahd University Of Petroleum And Minerals | Quantification of the micronutrient profile in Moringa oleifera tree leaves using calibration free laser induced breakdown spectroscopy |
| CN113331235A (en) * | 2021-07-05 | 2021-09-03 | 吉林省长春皓月清真肉业股份有限公司 | Slaughtering device |
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