CN104374751B - Device based on conllinear LIBS crop nutrient quick detection - Google Patents
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- 238000001514 detection method Methods 0.000 title claims abstract description 34
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- 238000002536 laser-induced breakdown spectroscopy Methods 0.000 title claims abstract description 17
- 230000003595 spectral effect Effects 0.000 claims abstract description 34
- 239000007787 solid Substances 0.000 claims abstract description 21
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 230000003287 optical effect Effects 0.000 claims abstract description 8
- 238000012545 processing Methods 0.000 claims abstract description 5
- 238000013499 data model Methods 0.000 claims abstract description 4
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- 101000694017 Homo sapiens Sodium channel protein type 5 subunit alpha Proteins 0.000 claims description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
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- 229910052698 phosphorus Inorganic materials 0.000 description 3
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- 229910052724 xenon Inorganic materials 0.000 description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 3
- 241000931526 Acer campestre Species 0.000 description 2
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a kind of device based on conllinear LIBS crop nutrient quick detection, including the Double-impulse solid laser for producing coaxial double-pulse laser, the repetition rate 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 beam laser is 200~2000ns；Energy attenuator, light path have been sequentially arranged along the optical axis of the Double-impulse solid laser to climb system and sample stage, plasma has been produced in sample surfaces by the climb laser vertical impact of system exit of light path；Also include signal acquisition and processing system, the characteristic spectral line that collection plasma cooling sends, and be input into the data model for establishing, calculate the content of nutrient.The present invention realizes the quick detection of crop nutrient, with simple to operate, the features such as low cost, the characteristics of effectively overcome traditional detection method detection time long, complex operation, it is to avoid pollution of the chemical reagent to environment.
Description
Technical field
It is more particularly to a kind of to be made based on conllinear LIBS the present invention relates to crop nutrient detection technique
The device of thing nutrient quick detection.
Background technology
Crop nutrient (nitrogen, phosphorus, potassium etc.) is closely related with the upgrowth situation and yield of crop.Nitrogen, phosphorus, potassium are to make
The big main nutrient elements of thing three.Nitrogen is the constituent of pigment, can promote photosynthesis of plant, increases crop yield；Phosphorus is to make
The component of thing multiple compounds, has material impact to crop quality；Potassium can promote crop photosynthesis, and crop resists for enhancing
Inverse property.The upgrowth situation that crop nutrient information is conducive to understanding crop is obtained, the nutritional deficiency situation according to crop realizes early stage
Quantitative fertilization.At present, the detection method of crop nutrient mainly has triumphant formula nitriding, Du Mashi combustion methods, colorimetric method, flame
Combustion method etc..However, these method complex operation, high costs, it usually needs a large amount of chemical reagent of consumption simultaneously cause environmental pollution,
The requirement of field-crop nutritional information quick obtaining cannot be met.
Laser induced breakdown spectrograph (Laser-Induced Breakdown Spectroscopy, LIBS) utilizes pulse
Laser-produced plasma ablation simultaneously excites material in sample (normally solid), and obtained by spectrometer excite etc. from
The spectrum that daughter atom is launched, the element constituent in sample is recognized with this, and then can carry out the identification of material, divide
Class, qualitative and quantitative analysis.The technology can quickly realize long-range, micro- damage to sample unit without being pre-processed to sample
Plain (especially metallic element) is detected, can be used for the detection of solid, gas, fluid sample.In recent years, laser-induced breakdown
Spectral technique quickly grows, and is widely used in multiple fields, such as heavy metal analysis in biomedicine, archaeology, environmental monitoring, water
And explosive detection etc..
Using LIBS energy quick obtaining crop nutritional information, be advantageously implemented agriculture precision,
Intelligentize and informatization.However, due to LIBS amount of analysis very little, matrix effect has obvious to analysis result
Influence.Therefore generally need to carry out repeatability of the sample preparation compressing tablet to ensure detection for crop sample.
The content of the invention
The invention provides a kind of crop nutrient device for fast detecting, realize based on LIBS pair
Crop compressing tablet nutrient quick detection, can simultaneously meet the detection of Different Crop laser spectrum, convenient with system fading margin, into
This is low, and detection is quick, the features such as micro- damage.
A kind of device based on conllinear LIBS crop nutrient quick detection, including for producing altogether
The Double-impulse solid laser of axle double-pulse laser, the repetition rate of described Double-impulse solid laser is 1~10Hz, laser
The energy of 532nm is 80~200mJ, and the energy of laser 1064nm is 80~300mJ, and the interval time between two beam laser is
200~2000ns；Energy attenuator, light path are sequentially arranged along the optical axis of the Double-impulse solid laser to climb system and sample
Sample platform, by light path climb system exit laser vertical impact sample surfaces produce plasma；Also include signal acquisition and
Processing system, the characteristic spectral line that collection plasma cooling sends, and the data model for establishing is input into, calculate nutrient
Content.
Preferably, described signal acquisition and processing system includes：Optical fiber collection system, for collecting plasma cooling
The characteristic spectral line for sending；Beam splitting system, for carrying out light splitting to characteristic spectral line；ICCD detectors, for by the light of beam splitting system
Signal is converted to electric signal；Computer, according to the data model that described electric signal, input are established, calculates nutrient
Content.
Preferably, described beam splitting system is echelle spectrometer.
Echelle spectrometer is the spectrometer using echelle grating as dispersion element, without by raster scanning one
Secondary property obtains full modal data, is avoided that conventional spectrograph multichannel head and the tail section Bonding Problem.Echelle spectrometer inside nothing
Mechanical part, stability is higher, and resolution ratio can reach 0.08nm, can meet spectral line light splitting requirement.
Preferably, described light path climbs system by the first speculum, the second speculum and the 3rd reflection that are sequentially arranged
Microscope group is into second speculum is located at the surface of the first speculum, and the 3rd speculum is located at the surface of sample stage.
The light path system of climbing is mainly used in lifting light path, and laser will be converted into and vertically propagate in the horizontal direction.
Can be prevented effectively from rising laser positions using the light path system of climbing causes the laser factors of instability.Laser is from directly over sample
Impact sample surfaces, are conducive to effectively exciting for plasma, it is ensured that plasma is uniformly and symmetrically distributed.
Preferably, the first described speculum, the second speculum and the 3rd speculum use 1 inch of double frequency Nd：YAG swashs
Light reflection mirror, the reflectivity at 532nm, 1064nm is more than 98%.
Because the optical maser wavelength of Double-impulse solid laser is 532nm and 1064nm, to reduce laser energy in light path system
The loss of system, it is ensured that the effective rate of utilization of laser energy, described speculum uses double frequency Nd：YAG laser mirrors, its
Reflectivity at 532nm, 1064nm is more than 98%.
Preferably, described sample stage includes electric displacement platform, the lifting being movably arranged on electric displacement platform with four-degree-of-freedom
Plate and the objective table being slidably fitted on electric displacement platform；The lifter plate is provided with transparent constraint window, laser light constraint window
Sample is impacted after mouthful；Restraining plate is provided with below the lifter plate, the restraining plate is placed in the surface of sample, is distributed on restraining plate
Constrained chamber, the constraint chamber is used to constrain the plasma of sample excitation.
Sample stage limits enhanced line intensity by space, and energy plasma is laterally and row constraint, and root are entered in longitudinal direction
Constraint space size adjustment the intensity of spectral line is adjusted according to different sample requirements, the intensity of spectral line enhancing scope is 2~10 times.Constraint window
Mouth is mainly used in plasma and longitudinally enters row constraint, and has to the characteristic spectral line that incident laser and plasma are produced preferable
Transmissivity.The transverse direction that restraining plate is mainly used in plasma enters row constraint, and characteristic spectral line is carried out constraint propagation, improves
Spectral line collection efficiency and the intensity of spectral line.
Preferably, described lifter plate is provided with light-transmitting opening, is coated with light-passing board at the light-transmitting opening, the light-transmitting opening with it is saturating
The described constraint window of tabula rasa composition.
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 more than 90%,
Energy threshold is more than 10J/cm2.Line enhancement effect suffers restraints influence of the window with a distance from sample.By properties of samples and institute
The element spectral line intensity to be detected is different, and constraint window of the invention can be moved in vertical direction, as needed regulation spectrum
Line strength.It is to ensure that laser effectively excites effective collection with characteristic spectral line, light-passing board is saturating to optical maser wavelength and characteristic spectral line
The rate of mistake should be greater than 90%.Meanwhile, to prevent laser from being caused damage to poly (methyl methacrylate) plate, its energy threshold should be greater than 10J/cm2。
The invention has the advantages that：
(1) parameter of energy quick regulation instrument, realizes the optimization of optimum detection parameter；
(2) quick detection of crop nutrient is realized, with simple to operate, the features such as low cost.Effectively overcome
Traditional detection method detection time is long, complex operation the characteristics of, it is to avoid pollution of the chemical reagent to environment.
(3) sample stage limits enhanced line intensity by space, and energy plasma is laterally and row constraint is entered in longitudinal direction, carries
Spectral line collection efficiency high and the intensity of spectral line；It is avoided that and excites particle to cover sample surfaces again；And smooth sample surfaces, make sample
Product keep constant so as to improve detection repeatability to the distance of condenser lens.
Brief description of the drawings
Fig. 1 is the structure drawing of device of crop nutrient quick detection；
Fig. 2 is the structure chart of sample stage；
Fig. 3 is the top view of sample stage in Fig. 2.
Specific embodiment
As shown in figure 1, a kind of device based on conllinear LIBS crop nutrient quick detection, including
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 is coaxially exported, and (2) 532nm is coaxially exported,
(3) the different axle outputs of different axle output (4) 1064nm, the 532nm of 1064nm.Double-impulse solid laser 1 can be by 2 pulse 1064nm
Solid state laser, frequency-doubling crystal and conjunction beam optical path are realized.The repetition rate of Double-impulse solid laser 1 is 1-10Hz, and energy is
80-200mJ (@532nm), 80-300mJ (@1064nm), the interval time between two beam laser are 200~2000ns.
The control Double-impulse solid laser 1 of delay time generator 2 adjusts Q triggered times, xenon lamp to open triggered time and ICCD spies
Survey the gate duration of device.Delay time generator sets Double-impulse solid laser and adjusts the triggered time of Q signal to be triggered in xenon lamp signal
150 ± 20 μ s afterwards.The opening time that controls of optimization detector is 1.5 μ s after the second road laser Q-switching switch triggering time.
Energy attenuator 3 is made up of the beam splitter 32 of half-wave plate 31 and first.Laser energy real-time monitoring system 4 includes thermoelectricity
Probe pulse 42, the second beam splitter 41, USB connecting lines and computer 13.
Light path system 5 of climbing is made up of the first speculum 52, the second speculum 51 and the 3rd speculum 53, the first speculum
52nd, the second speculum 51 and the 3rd speculum 53 select 1 inch of double frequency Nd：YAG laser mirrors, it is anti-at 532nm, 1064nm
Rate is penetrated more than 98%.
Optical fiber collection system 10 is made up of light collector and optical fiber.Sample surface imaging system 11 is used to monitor laser impact
Position, including CCD camera 114, imaging lens 113, the 3rd beam splitter 112, LED light source for illuminating 111.
Detector 6 is ICCD detectors.Spectrometer 7 is echelle spectrometer.
Condenser lens 9 be installed on along optical axis direction have regulation the free degree Lens mounting carrier along, for adjust sample with
The distance of lens, so as to control impact to the laser parameter on sample.Condenser lens selects N-BK7, plates V-arrangement film, its
Reflectivity at 532nm, 1064nm is less than 0.25%.
As shown in Figures 2 and 3, sample stage 8 include gear rack elevating bar 901, gear slider 902, right angle pinboard 903, etc.
Plasma confinement window 904, cylindrical guide 905, plasma confinement plate 906, V-type sliding block 907 combines electric displacement platform 909, pull bar
910, constrain chamber 911.Combination electric displacement platform 909 is using four-degree-of-freedom (x, y, z, w) combination electric displacement platform, including 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 installed at group
Close on electric displacement platform 909, gear slider 902 is engaged with gear rack elevating bar 901, can vertically be moved up and down.Right angle pinboard
903 are secured by bolts on gear slider 902, and plane is provided with the light-transmitting opening of rectangle, and light-transmitting opening edge is provided with support level, thoroughly
Light is intraoral to be provided with light-passing board, forms plasma confinement window 904.Cylindrical guide 905 be fixed on combination electric displacement platform 909, wait from
Daughter restraining plate 906 can be slided up and down along cylindrical guide 905.Cylindrical guide 905 and gear rack elevating bar 901 are connected by bolts
In on combination electric displacement platform 909.Combination electric displacement platform 909 is provided with V-groove, and V-type sliding block 907 can be left along V-groove under the effect of pull bar 910
Right slip, pull bar 910 is threadably secured in V-type sliding block 907.Sample 908 places V-type sliding block 907 (equivalent to objective table)
On, laser is impacted down from above, and by plasma confinement window 904, and by plasma confinement plate 906, impact is arrived
Sample surfaces, excite plasma, and cooling sends characteristic spectral line and 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 more than 90%, energy threshold
More than 10J/cm2.Plasma confinement window 904 is mainly used in plasma and longitudinally enters row constraint, and to incident laser with
The characteristic spectral line that plasma is produced has preferable transmissivity.N-BK7 is a kind of common optical glass, can be passed through
The light of 350nm~2000nm wave bands, the transmissivity of its laser is more than 90%, and energy threshold is more than 10J/cm2.Therefore plasma
Constraint window 904 the selection of material is N-BK7, and thickness is 1~3m.Plasma confinement window 904 can be acted in gear slider 902
Under vertically move.Line enhancement effect suffers restraints influence of the window with a distance from sample.Due to properties of samples and
The element spectral line intensity to be detected is different, and plasma confinement window 904 of the invention can be moved in vertical direction, root
According to need adjust the intensity of spectral line.
In the present embodiment, the material of plasma confinement plate 906 is the aluminium sheet of chromium plating, and thickness is 1mm, uniform in the middle of it
Cone constraint chamber 911 is furnished with, upper conical surface diameter and lower conical surface diameter are respectively 2mm and 3mm.Distance should between constraint chamber 911
It is consistent with the combination planning displacement of electric displacement platform 909.The transverse direction that plasma restraining plate 6 is mainly used in plasma enters row constraint,
And characteristic spectral line is carried out constraint propagation, and spectral line collection efficiency and the intensity of spectral line are improved, the intensity of spectral line enhancing scope is 2~10
Times.Chromium plating is carried out in the constraint chamber 911 of aluminium sheet, makes inner chamber that there is reflectivity higher, make characteristic spectral line constraint propagation, improved
Spectral line collection efficiency.Constraint chamber uses conical structure, and due to its up-small and down-big structure, the structure compared with cylindrical type can be more preferably
Obtain plasma and enter row constraint.In addition, when plasma is projected from cone constraint chamber, because its space constraint is increased,
Its electron density can be strengthened with movement velocity, therefore advantageously in the enhancing of spectral line signal.Plasma of the invention
Distance is consistent with the combination planning displacement of electric displacement platform 909 between the constraint chamber of body restraining plate 906, can be suitably used for laser-induced breakdown
The working method of spectrum Surface scan.Using plasma restraining plate 906 of the present invention covers sample surfaces, is conducive to smooth sample table
Detection repeatability is improved in face, while avoiding exciting other regions to be measured of particle contamination.When testing sample is the surfaces such as fresh blade
During out-of-flatness sample, its region to be measured has differences with lens distance, and then influences laser to reach the laser parameter of sample.Laser
The detection stability of induced breakdown spectroscopy is closely bound up with the laser parameter in region to be detected, therefore smooth sample surfaces are conducive to
Fixed laser parameter improves the repeatability of detection.Additionally, the up-small and down-big conical structure of plasma confinement plate 906 is conducive to
Farthest avoid exciting particle contamination by a upper detection zone, it is ensured that institute's detection object is the element in region to be detected.
V-type sliding block 907 can be moved under the effect of pull bar 910 along V-groove, using this V-type sliding block guide track structure, it is to avoid be raised
The troublesome operation such as plasma confinement window mouthful and plasma restraining plate.Company between plasma confinement plate 906 and cylindrical guide 905
It is connected in be close to and connects, plasma confinement plate 906 can not freely glides under gravity.
When this sample stage works, control combination electric displacement platform 909 makes the pyramid type of plasma confinement plate 906 constrain chamber 911
Position with top laser is corresponding, and the work step-length for setting combination electric displacement platform 909 is cone constraint chamber neighbor distance or again
Number.Coaxial double-pulse laser is propagated down from above by light path system, line focus lens, through plasma confinement window
904, and by cone constraint chamber impact sample.Its laser transmittance of plasma confinement window 904 is more than 90%, energy
Threshold value is more than 10J/cm2.Plasma cooling sends characteristic spectral line and is collected by the optical fiber collection system 10 of top.Each position can
According to actual requirement selection needed for impact number of times, when complete a position after by combine electric displacement platform 909 movement carry out it is many
Individual position spectra collection.When without plasma confinement window 904 and during plasma confinement plate 906, the plasma for inspiring
It is free excited state；After the plasma to exciting is limited, the density of plasma increases, plasma temperature liter
Height, enhances the intensity of spectral line of excited atom.
The Q-switch triggered time of the control Double-impulse solid laser 1 of delay time generator 2 and xenon lamp open the triggered time.
Under the control of delay time generator 2, Double-impulse solid laser 1 produces coaxial 532nm (1064nm) double-pulse laser.Laser passes through
Energy attenuator 3 decays to laser energy.By rotating the energy that half-wave plate 31 controls from beam splitter 32 out.After decay
Laser changes light path respectively through the first speculum 52 and the second speculum 51, then by the 3rd speculum 53, propagates downwards.Swash
Light focuses on impact sample surfaces by condenser lens 9, produces plasma.The characteristic spectral line that plasma cooling is produced is through optical fiber
Collection system 10 is collected, and by the light splitting of spectrometer 7, is finally converted into electric signal by the photomultiplier on detector 6, is passed through
USB is connected on computer 12, by the model database for establishing, calculates crop nutritive element content.
The foregoing is only preferable implementation example of the invention, be not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (6)
1. a kind of device based on conllinear LIBS crop nutrient quick detection, it is characterised in that including
Double-impulse solid laser for producing coaxial double-pulse laser, the repetition rate of described Double-impulse solid laser is 1
The energy of~10Hz, laser 532nm is 80~200mJ, and the energy of laser 1064nm is 80~300mJ, between two beam laser
Interval time is 200~2000ns；
Energy attenuator, light path are sequentially arranged along the optical axis of the Double-impulse solid laser to climb system and sample stage, by
Light path climb system exit laser vertical impact sample surfaces produce plasma；
Described sample stage includes the electric displacement platform with four-degree-of-freedom, the lifter plate being movably arranged on electric displacement platform and is slidably matched
Objective table on electric displacement platform；The lifter plate is provided with transparent constraint window, and sample is impacted after laser light constraint window；
Restraining plate is provided with below the lifter plate, the restraining plate is placed in the surface of sample, Constrained chamber is distributed on restraining plate, this is about
Beam chamber is used to constrain the plasma of sample excitation；
Described constraint chamber is cone constraint chamber, and upper conical surface diameter and lower conical surface diameter are respectively 2mm and 3mm, and constraint chamber
Inwall chromium plating；
Also include signal acquisition and processing system, the characteristic spectral line that collection plasma cooling sends, and be input into the number for establishing
According to model, the content of nutrient is calculated.
2. the device of conllinear LIBS crop nutrient quick detection is based on as claimed in claim 1, its
It is characterised by, described signal acquisition and processing system includes：
Optical fiber collection system, for collecting the characteristic spectral line that plasma cooling sends；
Beam splitting system, for carrying out light splitting to characteristic spectral line；
ICCD detectors, for the optical signal of beam splitting system to be converted into electric signal；
Computer, according to the data model that described electric signal, input are established, calculates the content of nutrient.
3. the device of conllinear LIBS crop nutrient quick detection is based on as claimed in claim 2, its
It is characterised by, described beam splitting system is echelle spectrometer.
4. the device of conllinear LIBS crop nutrient quick detection is based on as claimed in claim 1, its
Be characterised by, described light path climb system by the first speculum, the second speculum and the 3rd speculum group that are sequentially arranged into,
Second speculum is located at the surface of the first speculum, and the 3rd speculum is located at the surface of sample stage.
5. the device of conllinear LIBS crop nutrient quick detection is based on as claimed in claim 4, its
It is characterised by, described the first speculum, the second speculum and the 3rd speculum use 1 inch of double frequency Nd：YAG laser reflections
Mirror, the reflectivity at 532nm, 1064nm is more than 98%.
6. the device of conllinear LIBS crop nutrient quick detection is based on as claimed in claim 1, its
It is characterised by, described lifter plate is provided with light-transmitting opening, light-passing board, the light-transmitting opening and light-passing board group is coated with the light-transmitting opening
Into described constraint window.
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| CN105699338B (en) * | 2016-01-22 | 2019-02-05 | 清华大学 | The LIBS system of micro heavy detection based on plasma confinement chamber |
| CN107764794A (en) * | 2017-11-21 | 2018-03-06 | 江西农业大学 | Utilize the device of tunable resonance LIBS detection pork heavy metal distribution |
| CN109324026A (en) * | 2018-10-16 | 2019-02-12 | 浙江大学 | It is copolymerized two area's fluorescence lifetime micro imaging system of burnt near-infrared |
| CN112629670B (en) * | 2020-12-28 | 2021-09-24 | 上海交通大学 | High-frequency dynamic flame temperature measuring method and system |
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