CN110296974A - Quantitative LIBS laser system and quantitative approach - Google Patents
Quantitative LIBS laser system and quantitative approach Download PDFInfo
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- CN110296974A CN110296974A CN201910639175.XA CN201910639175A CN110296974A CN 110296974 A CN110296974 A CN 110296974A CN 201910639175 A CN201910639175 A CN 201910639175A CN 110296974 A CN110296974 A CN 110296974A
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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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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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
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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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N2021/0106—General arrangement of respective parts
- G01N2021/0112—Apparatus in one mechanical, optical or electronic block
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Abstract
The present invention relates to a kind of quantitative LIBS laser system and quantitative approach, belong to laser induced breakdown spectroscopy (LIBS) technical field, including laser and spectroscopic analysis system；It is characterized by: the laser that laser generates, which passes sequentially through to enter after beam expanding lens, light velocity adjustment module, semi-transparent partly returns mirror；The semi-transparent reflected light path for partly returning mirror is equipped with laser condensing lens A, and the semi-transparent transmitted light path for partly returning mirror is equipped with laser condensing lens B, and the output light path of laser condensing lens A is equipped with CCD light combination eyeglass A, and the output light path of laser condensing lens B is equipped with CCD light combination eyeglass B；Spectroscopic analysis system includes spectroscopic analysis system A and spectroscopic analysis system B；Spectroscopic analysis system A obtains the spectral information of unknown sample to be tested by sampling mirror A；The spectroscopic analysis system B obtains the spectral information of known sample to be tested by sampling mirror B；CCD camera passes sequentially through microscope, CCD light combination eyeglass A acquires the information of unknown sample to be tested.
Description
Technical field
The invention belongs to laser induced breakdown spectroscopy (LIBS) technical fields, and in particular to a kind of quantitative LIBS laser system
And quantitative approach.
Background technique
Laser induced breakdown spectroscopy (Laser Induced Breakdown Spectroscopy, LIBS), which has, not to be needed
Preparation of samples, multielement detect simultaneously, measuring speed is fast, can long-range non-cpntact measurement, system structure composition it is simple etc. many excellent
Point.Since Laser Energy Change, the serious, poor repeatability of system signal fluctuation etc. have seriously affected LIBS quantitative measurment and extensive
Using.Therefore, design and develop a kind of higher quantitative LIBS laser system of precision and quantitative approach seem it is particularly important.
Summary of the invention
The present invention is to solve technical problem present in well-known technique and provide a kind of quantitative LIBS laser system and quantitative
Method, the present invention acquires while analyzing unknown sample to be tested and known standard sample by same optical path, simultaneously, by spectral line knot
Fruit carries out differential ratio pair, reduces the error of optical path and acquisition, can accurately realize the quantitative detection to unknown sample.
The first object of the present invention is to provide a kind of quantitative LIBS laser system, including laser (1) and spectrum analysis system
System；The laser that above-mentioned laser (1) generates passes sequentially through beam expanding lens (4), light velocity adjustment module (5) partly returns mirror into semi-transparent afterwards
(3)；It is provided with laser condensing lens A (6-1) on the above-mentioned semi-transparent reflected light path for partly returning mirror (3), semi-transparent partly returns mirror (3) above-mentioned
Transmitted light path on be provided with laser condensing lens B (6-2), be provided with CCD on the output light path of the laser condensing lens A (6-1)
Light combination eyeglass A (7-1) is provided with CCD light combination eyeglass B (7-2) on the output light path of above-mentioned laser condensing lens B (6-2)；Also wrap
It includes:
For detecting the energy detection photodiode A (8-1) of laser energy on CCD light combination eyeglass A (7-1)；
For detecting the energy detection photodiode B (8-2) of laser energy on CCD light combination eyeglass B (7-2)；
For carrying the XYZ D translation platform A (12-1) of unknown sample to be tested (11)；
For carrying the XYZ D translation platform B (12-2) of known sample to be tested (15)；
The spectroscopic analysis system includes spectroscopic analysis system A (14-1) and spectroscopic analysis system B (14-2)；
The spectroscopic analysis system A (14-1) obtains the spectrum letter of unknown sample to be tested (11) by sampling mirror A (13-1)
Breath；The spectroscopic analysis system B (14-2) obtains the spectral information of known sample to be tested (15) by sampling mirror B (13-2)；CCD
Video camera (10) passes sequentially through microscope (9), CCD light combination eyeglass A (7-1) acquires the information of unknown sample to be tested (11).
Further, be provided between the laser (1) and beam expanding lens (4) adjustment optical path total reflection mirror A (2-1) and
Total reflection mirror B (2-2).
Further, semi-transparent partly return is provided with being all-trans for adjustment optical path between mirror (3) and laser condensing lens A (6-1)
Penetrate mirror C (2-3).
Further, being provided with the total reflection mirror of adjustment optical path between the microscope (9) and CCD light combination eyeglass A (7-1)
D(2-4)。
It is further: the parameter of the laser (1) are as follows: wavelength is 1064nm, and repetition is 1Hz, and energy is greater than 200mj,
Pulsewidth is less than 10ns, and tune Q mode is actively Q-switched, and hot spot focal diameter is less than 0.1；The type of cooling is air-cooled, data test RSD
Less than 10%.
The second object of the present invention is to provide a kind of quantitative approach of quantitative LIBS laser system, includes the following steps:
S1, laser generate laser it is semi-transparent partly return mirror after be divided into first via laser and the second road laser；
S2, first via laser reflection enter focus lamp B, using CCD light combination eyeglass B, focus on known standard sample table
Face, the Laser Plasma Emission Spectrum signal of generation are coupled in optical fiber by sampling mirror B, are transmitted to spectroscopic analysis system B,
The light splitting and detection for completing spectrum obtain known standard sample spectral line；
Second road laser is transmitted into total reflection mirror C, and the laser that is all-trans enters focus lamp A, poly- using CCD light combination eyeglass A
Coke arrives unknown sample to be tested surface, and the Laser Plasma Emission Spectrum signal of generation is coupled in optical fiber by sampling mirror A, passes
Spectroscopic analysis system A is transported to, the light splitting and detection of spectrum are completed, obtains unknown sample to be tested spectral line；Unknown sample to be tested is composed
Line and software standard library compare, and obtain element category；
S3, above-mentioned known standard sample spectral line is compared with unknown sample to be tested spectral line, is data scaling specifically:
If known standard sample is that spectral line peak value line wavelength is consistent with unknown sample to be tested, for same substance, root
According to content formula: z=(a/b) c, in which: z is constituent content required by unknown sample, and a is the unknown sample element spectral line intensity, b
For the known standard sample element spectral line intensity, c is the known standard sample constituent content, finds out containing for unknown sample each element
Amount；
If known standard sample and it is unknown to sample be that spectral line peak value is inconsistent, for different material；By with java standard library
Comparison obtains element category, in the same band, according to y=(m/n) x+d；Wherein: y is constituent content required by unknown sample, m
For the unknown sample element spectral line intensity, n is known standard sample reference element the intensity of spectral line, and x is known this yuan of standard sample
Cellulose content, d are constant.
The advantages and positive effects of the present invention are:
Same laser is divided into two-way laser by semi-transparent semi-reflecting lens first by the present invention, then sample known to laser irradiation all the way
Product generate a spectral line, and in addition laser irradiation unknown sample generates a spectral line all the way, the spectral line finally generated with known sample
The spectral line generated with unknown sample compares, and the content of unknown sample is extrapolated by the content of known sample.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the preferred embodiment of the present invention；
Specific embodiment
In order to further understand the content, features and effects of the present invention, the following examples are hereby given, and cooperate attached drawing
Detailed description are as follows:
As shown in Figure 1, a kind of quantitative LIBS laser system, including laser 1 and spectroscopic analysis system；Above-mentioned laser 1
The laser of generation, which passes sequentially through to enter after beam expanding lens 4, light velocity adjustment module 5, semi-transparent partly returns mirror 3；In the above-mentioned semi-transparent mirror 3 of partly returning
It is provided with laser condensing lens A6-1 on reflected light path, is provided with laser condensing lens on the above-mentioned semi-transparent transmitted light path for partly returning mirror 3
B6-2 is provided with CCD light combination eyeglass A7-1 on the output light path of the laser condensing lens A6-1, above-mentioned laser condensing lens B6-2's
CCD light combination eyeglass B7-2 is provided on output light path；Further include:
For detecting the energy detection photodiode A8-1 of laser energy on CCD light combination eyeglass A7-1；
For detecting the energy detection photodiode B8-2 of laser energy on CCD light combination eyeglass B7-2；
For carrying the XYZ D translation platform A12-1 of unknown sample to be tested 11；
For carrying the XYZ D translation platform B12-2 of known sample to be tested 15；
The spectroscopic analysis system includes spectroscopic analysis system A14-1 and spectroscopic analysis system B14-2；
The spectroscopic analysis system A14-1 obtains the spectral information of unknown sample to be tested 11 by sampling mirror A13-1；It is described
Spectroscopic analysis system B14-2 obtains the spectral information of known sample to be tested 15 by sampling mirror B13-2；CCD camera 10 is successively
The information of unknown sample to be tested 11 is acquired by microscope 9, CCD light combination eyeglass A7-1.
Preferably, in order to reduce volume and space: being provided with adjustment optical path between the laser 1 and beam expanding lens 4 and use
Total reflection mirror A2-1 and total reflection mirror B2-2.
It is described it is semi-transparent partly return be provided between mirror 3 and laser condensing lens A6-1 adjustment optical path total reflection mirror C2-3.
The total reflection mirror D2-4 of adjustment optical path is provided between the microscope 9 and CCD light combination eyeglass A7-1.
The parameter of the laser 1 are as follows: wavelength is 1064nm, and repetition is 1Hz, and energy is greater than 200mj, and pulsewidth is less than
10ns, tune Q mode are actively Q-switched, and hot spot focal diameter is less than 0.1；The type of cooling be it is air-cooled, data test RSD is less than 10%.
The working principle of above preferred embodiment are as follows:
The laser that laser 1 generates is by total reflection mirror A2-1, vertically into total reflection mirror B2-2, then passes through beam expanding lens
4, light beam adjustment module 5 (can be by adjusting laser indicator) partly returns mirror 3 into semi-transparent, and the semi-transparent mirror 3 that partly returns realizes that two-way is average
Light splitting (+50% transmission of 50% reflection)；First via laser reflection enters focus lamp B6-2, using CCD light combination eyeglass B7-2, gathers
Coke arrives known 15 surface of standard sample, and the Laser Plasma Emission Spectrum signal of generation is coupled to optical fiber by sampling mirror B13-2
It is interior, it is transmitted to spectroscopic analysis system B14-2, completes the light splitting and detection of spectrum, obtains known standard sample spectral line.Energy detection
Laser energy can be monitored in real time by feux rouges light combination eyeglass 3 in diode B8-2；If laser energy is not that test is required, can
To adjust laser parameter, reach requirement.
Second road laser is transmitted into total reflection mirror C2-3, and the laser that is all-trans enters focus lamp A6-1, using CCD light combination mirror
Piece A7-1 focuses on unknown 11 surface of sample to be tested, the Laser Plasma Emission Spectrum signal of generation, by sampling mirror A13-1 coupling
It is bonded in optical fiber, is transmitted to spectroscopic analysis system A14-1, complete the light splitting and detection of spectrum, obtain unknown sample to be tested spectral line.
It is compared with software standard library, obtains element category；Energy detection diode A8-1 can be supervised in real time by CCD light combination eyeglass A7-1
Survey laser energy；If laser energy is not that test is required, adjustable laser parameter reaches requirement.Unknown sample difference
By total reflection mirror D2-4, zoom mirror (microscope 9), into CCD camera 10 (transmitting data to computer by USB3.0 line),
Computer can acquire its image in real time, by adjusting XYZ D translation platform, the point for the sample analyzed required for determining.
Above-mentioned optimal technical scheme measures comparison with the second road unknown sample using standard sample known to the first via is quantitative
Method is data scaling, by result differential ratio pair, realizes the error for eliminating optical path and acquisition.
If known standard sample is that spectral line peak value line wavelength is consistent with unknown sample to be tested, for same substance.It can
According to content formula: z=(a/b) c, in which: z is constituent content required by unknown sample, and a is that the unknown sample element spectral line is strong
Degree, b are the known standard sample element spectral line intensity, and c is the known standard sample constituent content, find out unknown sample each element
Content.In order to improve accuracy, it can test 100 times, be averaged as final result.
If known standard sample and it is unknown to sample be that spectral line peak value is inconsistent, for different material；By with java standard library
Comparison, then know element category.In the same band, such as 200-400nm, according to y=(m/n) x+d；Wherein: y is unknown sample
Constituent content required by product, m are the unknown sample element spectral line intensity, and n is known standard sample (in the wave band) reference element spectrum
Line intensity, x are the known standard sample constituent content, and d is constant.In order to improve accuracy, it can test 100 times, be averaged
Value is final result.
The above is only the preferred embodiments of the present invention, and is not intended to limit the present invention in any form,
Any simple modification made to the above embodiment according to the technical essence of the invention, equivalent variations and modification, belong to
In the range of technical solution of the present invention.
Claims (6)
1. a kind of quantitative LIBS laser system, including laser (1) and spectroscopic analysis system；It is characterized by:
The laser that above-mentioned laser (1) generates passes sequentially through beam expanding lens (4), light velocity adjustment module (5) partly returns mirror into semi-transparent afterwards
(3)；It is provided with laser condensing lens A (6-1) on the above-mentioned semi-transparent reflected light path for partly returning mirror (3), semi-transparent partly returns mirror (3) above-mentioned
Transmitted light path on be provided with laser condensing lens B (6-2), be provided with CCD on the output light path of the laser condensing lens A (6-1)
Light combination eyeglass A (7-1) is provided with CCD light combination eyeglass B (7-2) on the output light path of above-mentioned laser condensing lens B (6-2)；Also wrap
It includes:
For detecting the energy detection photodiode A (8-1) of laser energy on CCD light combination eyeglass A (7-1)；
For detecting the energy detection photodiode B (8-2) of laser energy on CCD light combination eyeglass B (7-2)；
For carrying the XYZ D translation platform A (12-1) of unknown sample to be tested (11)；
For carrying the XYZ D translation platform B (12-2) of known sample to be tested (15)；
The spectroscopic analysis system includes spectroscopic analysis system A (14-1) and spectroscopic analysis system B (14-2)；
The spectroscopic analysis system A (14-1) obtains the spectral information of unknown sample to be tested (11) by sampling mirror A (13-1)；Institute
State the spectral information that spectroscopic analysis system B (14-2) obtains known sample to be tested (15) by sampling mirror B (13-2)；CCD camera shooting
Machine (10) passes sequentially through microscope (9), CCD light combination eyeglass A (7-1) acquires the information of unknown sample to be tested (11).
2. quantitative LIBS laser system according to claim 1, it is characterised in that: the laser (1) and beam expanding lens (4)
Between be provided with adjustment optical path total reflection mirror A (2-1) and total reflection mirror B (2-2).
3. quantitative LIBS laser system according to claim 1, it is characterised in that: described semi-transparent partly to return mirror (3) and laser
The total reflection mirror C (2-3) of adjustment optical path is provided between focus lamp A (6-1).
4. quantitative LIBS laser system according to claim 1, it is characterised in that: the microscope (9) and CCD light combination mirror
The total reflection mirror D (2-4) of adjustment optical path is provided between piece A (7-1).
5. quantitative LIBS laser system according to claim 1-4, it is characterised in that: the laser (1)
Parameter are as follows: wavelength is 1064nm, and repetition is 1Hz, and energy is greater than 200mj, and pulsewidth is less than 10ns, and tune Q mode is actively Q-switched, light
Spot focal diameter is less than 0.1；The type of cooling be it is air-cooled, data test RSD is less than 10%.
6. a kind of quantitative approach based on quantitative LIBS laser system described in claim 5, it is characterised in that: including walking as follows
It is rapid:
S1, laser generate laser it is semi-transparent partly return mirror after be divided into first via laser and the second road laser；
S2, first via laser reflection enter focus lamp B, using CCD light combination eyeglass B, focus on known standard sample surface, produce
Raw Laser Plasma Emission Spectrum signal is coupled in optical fiber by sampling mirror B, is transmitted to spectroscopic analysis system B, completes light
The light splitting and detection of spectrum obtain known standard sample spectral line；
Second road laser is transmitted into total reflection mirror C, and the laser that is all-trans enters focus lamp A, focuses on using CCD light combination eyeglass A
Unknown sample to be tested surface, the Laser Plasma Emission Spectrum signal of generation are coupled in optical fiber by sampling mirror A, are transmitted to
Spectroscopic analysis system A completes the light splitting and detection of spectrum, obtains unknown sample to be tested spectral line；By unknown sample to be tested spectral line with
The comparison of software standard library, obtains element category；
S3, above-mentioned known standard sample spectral line is compared with unknown sample to be tested spectral line, is data scaling specifically:
If known standard sample is that spectral line peak value line wavelength is consistent with unknown sample to be tested, for same substance, according to containing
Measure formula: z=(a/b) c, in which: z is constituent content required by unknown sample, and a is the unknown sample element spectral line intensity, and b is
Know the standard sample element spectral line intensity, c is the known standard sample constituent content, finds out the content of unknown sample each element；
If known standard sample and it is unknown to sample be that spectral line peak value is inconsistent, for different material；By being compared with java standard library,
Element category is obtained, in the same band, according to y=(m/n) x+d；Wherein: y is constituent content required by unknown sample, and m is not
Know the sample element spectral line intensity, n is known standard sample reference element the intensity of spectral line, and x is that the known standard sample element contains
Amount, d is constant.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111855643A (en) * | 2020-07-21 | 2020-10-30 | 华谱智能科技(天津)有限公司 | LIBS soil detection method, system and equipment for realizing self-adaptive spectral line balance |
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| CN102262075A (en) * | 2011-07-26 | 2011-11-30 | 清华大学 | Method for measuring elemental concentration through laser-induced breakdown spectroscopy based on spectrophotometry |
| CN102830096A (en) * | 2012-08-29 | 2012-12-19 | 国电燃料有限公司 | Method for measuring element concentration and correcting error based on artificial neural network |
| CN109781711A (en) * | 2019-02-21 | 2019-05-21 | 华中科技大学 | A kind of laser induced breakdown spectroscopy quantitative analysis method based on the calibration of single standard specimen |
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2019
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| CN1338623A (en) * | 2001-10-12 | 2002-03-06 | 周向前 | Miniature biochemical analyzer using dual-spectrum detection |
| CN101196471A (en) * | 2007-12-21 | 2008-06-11 | 中国科学院上海技术物理研究所 | Soil heavy metal pollution quantification detecting system and detecting method |
| CN102262075A (en) * | 2011-07-26 | 2011-11-30 | 清华大学 | Method for measuring elemental concentration through laser-induced breakdown spectroscopy based on spectrophotometry |
| CN102830096A (en) * | 2012-08-29 | 2012-12-19 | 国电燃料有限公司 | Method for measuring element concentration and correcting error based on artificial neural network |
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| CN111855643A (en) * | 2020-07-21 | 2020-10-30 | 华谱智能科技(天津)有限公司 | LIBS soil detection method, system and equipment for realizing self-adaptive spectral line balance |
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