CN108072635A - A kind of method of ingredient in analytical equipment real-time online measuring Improving Glass Manufacturing Processes using Laser induced plasma spectroscopy - Google Patents
A kind of method of ingredient in analytical equipment real-time online measuring Improving Glass Manufacturing Processes using Laser induced plasma spectroscopy Download PDFInfo
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- CN108072635A CN108072635A CN201611004497.XA CN201611004497A CN108072635A CN 108072635 A CN108072635 A CN 108072635A CN 201611004497 A CN201611004497 A CN 201611004497A CN 108072635 A CN108072635 A CN 108072635A
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- laser
- spectrum
- glass
- ingredient
- femtoseconds
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Classifications
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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
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
-
- 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
Abstract
A kind of method of ingredient in analytical equipment real-time online measuring Improving Glass Manufacturing Processes using Laser induced plasma spectroscopy, the laser that this method includes 1) laser transmitting is focused to by laser import system at the glass sample in Improving Glass Manufacturing Processes, glass sample surface to be measured is made to form plasma, generate induced with laser spectrum, 2) the induction spectrum that is generated is exported the fluorescence of generation to spectral collection subsystem by spectrum export subsystem；3) calculating, processing and analysis to collected spectrum are passed through, complete and quantitative testing qualitative to contained glass ingredient in glass sample to be measured, wherein described laser is all solid state chirped pulse amplification femto-second laser, realizes laser pulse width from femtosecond to a picosecond consecutive variations by adjusting chirp numerical value.
Description
Technical field
Laser induced plasma spectroscopy analytical equipment real-time online measuring glass production mistake is utilized the present invention relates to a kind of
The method of ingredient in journey.
Background technology
Laser-induced plasma spectroscopy (Laser Induced Plasma Spectroscopy, LIPS) is also referred to as
Make laser induced breakdown spectroscopy (Laser Induced Breakdown Spectroscopy, LIBS), be a kind of to swash
Light induces the Atomic Emission Spectral Analysis method for generating laser plasma as excitaton source, is based on laser and substance phase interaction
With physics and the elemental composition of spectroscopy and concentration analysis technology.LIPS is by by the laser beam of a branch of high-energy short pulse
It focuses on sample to be detected, and then generates high-temperature high-density and by free electron, ion and former molecular laser etc.
Gas ions, the process finally analyzed the plasma radiation spectrum.This method has the advantages that many uniquenesses, such as
Operation is easily, sample treatment is simple, detection object diversification (solid, liquid, gas, aerosol etc.), can the multielement same time-division
Analyse, be similar to non-destructive testing characteristic, can be most on detection elements periodic table element, have higher sensitivity,
Without the pure optical means contacted with sample, the ability that can be detected at a distance etc..LIPS should in the analysis detection of solid material
With the most extensively, oneself the finished product instrument through there is LIPS detection solid materials external at present occurs, and gradually commercialization with it is small-sized
Change.And it is domestic since research is started late, the development of instrument is more weak, theory that current main research contents is LIPS and
Application study, in the industrial application of glass material composition detection, there is no ready-made products.
The method of existing frequently-used measurement glass ingredient is spectrofluorimetry, and the method can apply to glass system
The composition detection of finished product.Spectrofluorimetry needs first to grind glass sample completely, and solution is made, and recycles x-ray fluorescence
Spectrometer determines the ingredient inside glass.Although this analysis method result is accurate, is generally recognized and widely used,
Since sample preparation and analytic process need the even longer time several hours, it is impossible to which real-time online obtains glass ingredient.Especially
Directly glass ingredient can not be measured in Improving Glass Manufacturing Processes by adopting said method, and when result comes out, glass product is already cold
But shape.This technology is long there are detection time, and the problem of cannot be used for the component monitoring during glass production is crossed into.
German patent DE 19537796 discloses a kind of emission spectrographic analysis method utilized based on induced with laser for making pottery
The non-destructive chemical analysis of porcelain and glass.But this method is using the laser of single pulsewidth as induced with laser light source, no genealogy of law
Influence of the analysis induced with laser light source pulse width variations of system to generation laser induced plasma effect, especially cannot preferably use
Component monitoring in glass production is crossed into.
The content of the invention
It is contemplated that overcome the prior art long there are detection time, and cannot be used for during glass production is crossed into
The technological deficiency of point monitoring is provided and ingredient in a kind of real-time online measuring Improving Glass Manufacturing Processes or glass product ingredient swashed
Photoinduction plasma spectroscopy equipment including laser, laser import system, sample to be tested room, spectrum export and is received
Collecting system, beam splitting system and spectrum acquisition system, wherein laser and spectrum acquisition system are referred to by the transmission of same impulse generator
Order control.
To achieve the above object, the technical solution taken in the present invention is as follows：
According to the present invention, a kind of utilization Laser induced plasma spectroscopy analytical equipment real-time online measuring glass is provided to give birth to
The method of ingredient during production, the equipment include pulse laser, laser import system, spectrum export and collection system, light splitting
System and spectrum acquisition system, wherein, spectrum export and collection system include spectrum export subsystem and spectral collection subsystem,
With, wherein pulse laser and spectrum acquisition system by same impulse generator send instruction control, laser transmitting laser lead to
Too drastic smooth import system is focused at sample, and sample surfaces is made to form plasma, generation induced with laser spectrum and pass through spectrum
Export subsystem exports generated fluorescence to spectral collection subsystem, passes through calculating, processing and the analysis to collecting spectrum
To carry out qualitative and quantitative testing to contained element in sample, wherein the laser is all solid state chirped pulse amplification femtosecond
Laser is (that is, by the use of all solid state chirped pulse amplification femto-second laser as Laser induced plasma spectroscopy analytical equipment
Light source), laser pulse width is realized from femtosecond to a picosecond consecutive variations by adjusting chirp numerical value,
This method includes：
1) laser of laser transmitting is focused to by laser import system at the glass sample in Improving Glass Manufacturing Processes,
Glass sample surface to be measured is made to form plasma, generates induced with laser spectrum, 2) the induction spectrum generated is led by spectrum
Go out subsystem to export the fluorescence of generation to spectral collection subsystem；3) by the calculating, processing and analysis to collected spectrum,
Complete and quantitative testing qualitative to contained glass ingredient in glass sample to be measured.
It is preferred that using all solid state chirped pulse amplification femto-second laser as from 500 femtoseconds to 100 picoseconds of consecutive variations
Ultra-short pulse laser light source.
It is preferred that in all solid state chirped pulse amplification femto-second laser, same transmission volume holography grating is both used as broadening
Device is used as compressor reducer again.Wherein stretcher is the seed source of a femtosecond pulsewidth (such as 150-220 femtoseconds, such as 180 femtoseconds)
Beam broadening is then put to a picosecond pulsewidth (such as 15-25 picoseconds, such as 20 picoseconds) by magneto optic isolator injection regeneration
Big device；Laser beam is reciprocal (such as 60-200 times, preferably 80-150 times, such as from about 100 times) back and forth in regenerative amplifier, pulse
Then energy gradual magnification projects regenerative amplifier to maximum by magneto optic isolator；The process being emitted from regenerative amplifier
The laser beam of energy amplification compresses laser pulse width from picosecond pulsewidth (such as 15-25 picoseconds, such as 20 picoseconds) by compressor reducer
Return the femtosecond pulsewidth (such as 350-650 femtoseconds；Such as 500 femtoseconds, i.e. most short pulse duration is 500 femtoseconds), by adjusting chirp
Numerical value realizes the laser pulse width from femtosecond to a picosecond consecutive variations.
It is preferred that laser caused by all solid state chirped pulse amplification femto-second laser (induced with laser light source) is flown from 500
Second to 100 picoseconds of consecutive variations ultra-short pulse laser (light source).
It is preferred that the laser of laser import system is focused to adjustable focal length mode.In addition, be designed as can for spectral collection subsystem
Focalize system.
Inventor has developed a set of chirped pulse amplification total solids femto-second laser for above equipment.Schematic diagram is as schemed
Shown in 2.Femtosecond seed source can use commercial product, such as come from Austrian HIGH Q companies, the femtosecond laser arteries and veins of generation
Wide 180 femtosecond, repetition rate 90MHz, mean power 90mW.In order to save space, same transmission volume holography grating is used as
Stretcher is used as compressor reducer again.Stretcher is the seed source beam broadening of a femtosecond pulsewidth (such as 180 femtoseconds) to one
Picosecond pulsewidth (such as 20 picoseconds), then injects regenerative amplifier by magneto optic isolator.Laser beam is in regenerative amplifier
Reciprocal (for example, about 100 times) back and forth, then single pulse energy gradual magnification to maximum projects regeneration by magneto optic isolator and puts
Big device.The laser beam by energy amplification being emitted from regenerative amplifier is by compressor reducer laser pulse width from picosecond pulsewidth
(such as 20 picoseconds) femtosecond pulsewidth described in compression and back (such as 500 femtoseconds, i.e. most short pulse duration is 500 femtoseconds), by adjusting Zhou
Numerical value sing to realize laser pulse width from femtosecond to a picosecond consecutive variations.
The present invention is set using chirped pulse amplification total solids femto-second laser as Laser induced plasma spectroscopy analysis
Standby induction light source realizes laser pulse width from femtosecond to a picosecond consecutive variations, for real-time by adjusting chirp numerical value
The ingredient of glass in on-line checking Improving Glass Manufacturing Processes.
Advantageous effect of the invention
It benefit of the invention is that can be with quick the reason for obtaining glass ingredient, such benefit can be generated of real-time online just
It is that the present invention exports laser using existing nanosecond laser and focuses on generation laser induced plasma to glass detection sample
Optical signal simultaneously utilizes the Laser induced plasma spectroscopy analytical equipment of the present invention to the light of laser induced plasma optical signal
Spectrum analysis accurately determines glass ingredient.
The spectrum generated using glass sample analyzes laser by Laser induced plasma spectroscopy analytical equipment of the present invention
The spectral information of focus point can accurately determine glass ingredient in real time.Utilize invented Laser induced plasma spectroscopy
Analytical equipment realizes real-time online measuring glass ingredient or real-time online measuring finished glass article in Improving Glass Manufacturing Processes
Ingredient.
Description of the drawings
Fig. 1 is present device schematic diagram.
Fig. 2 is laser schematic diagram of the present invention.
In fig. 1：
10 be induced with laser light source；
20 be echelle spectrometer；
30 be focusing system；
11 be laser；
12 be scala media grating spectrograph；
13 be integrated delay detection system；
14 for test point apart from dynamic monitoring system；
15 be feedback regulation control system；
16 monitor regulating system for beam quality；
17 turn back system for light beam；
18 be sample to be tested.
In fig. 2：
1 is femtosecond laser oscillator, 180 femtosecond of femtosecond laser pulsewidth of generation, repetition rate 90MHz, mean power
90mW；
2 be stretcher；
3 be regenerative amplifier；
4 be compressor reducer；
5 be scanning element；
6 be plasma spectroscopy unit；
7 Brewster polarizers (Brewster Polatizer)；
8 pumps (pump).
Fig. 3 is the spectrum observed using equipment real-time online set forth in the present invention detection glass, it can be seen that member
The spectral line of plain silicon.
Specific embodiment
It is further illustrated the present invention below in conjunction with attached drawing.
The application provides a kind of Laser induced plasma spectroscopy analytical equipment, including laser, laser import system, light
Spectrum export and collection system, beam splitting system and spectrum acquisition system, wherein laser and spectrum acquisition system are sent out by same pulse
Raw device sends instruction control, and laser transmitting laser is focused to by import system at sample, and sample surfaces is made to form plasma
Body, generation induced with laser spectrum and pass through guiding system by generate fluorescence export to spectral collection system, by collect spectrum
Calculating, processing and analysis qualitative and quantitative testing is carried out to contained element in sample, wherein being put using all solid state chirped pulse
Big light source of the femto-second laser as Laser induced plasma spectroscopy analytical equipment, laser is realized by adjusting chirp numerical value
Pulsewidth is from femtosecond to a picosecond consecutive variations.
The laser is using the same transmission volume holography grating of a set of chirped pulse amplification total solids femto-second laser
As stretcher 2 again as compressor reducer 4.Stretcher 2 is the seed source beam broadening of a femtosecond pulsewidth (such as 180 femtoseconds)
To a picosecond pulsewidth (such as 20 picoseconds), regenerative amplifier 3 is then injected by magneto optic isolator.Laser beam is put in regeneration
Reciprocal (for example, about 100 times) back and forth in big device 3, then single pulse energy gradual magnification to maximum is penetrated by magneto optic isolator
Go out regenerative amplifier.The laser beam by energy amplification being emitted from regenerative amplifier 3 is by compressor reducer 4 laser pulse width from skin
Second grade pulsewidth (such as 20 picoseconds) femtosecond pulsewidth described in compression and back (such as 500 femtoseconds, i.e. most short pulse duration is 500 femtoseconds), leads to
Chirp numerical value is overregulated to realize laser pulse width from femtosecond to a picosecond consecutive variations.
The Laser induced plasma spectroscopy analytical equipment for the new observation steel samples ingredient that the application proposes, feature
It is the pulse laser of 10 to 20 nanoseconds not common caused by induced with laser light source, but from 500 femtoseconds to 100 picoseconds of companies
The ultra-short pulse laser light source of continuous variation can effectively explore the ultra-short pulse laser of distinct pulse widths as produced by induction light source
Plasma signal effect.Using above equipment detect Improving Glass Manufacturing Processes in ingredient or glass product ingredient method
Comprise the following steps：
1) laser of laser transmitting is focused to by laser import system at the glass sample in Improving Glass Manufacturing Processes,
Glass sample surface to be measured is made to form plasma, generates induced with laser spectrum, 2) the induction spectrum generated is led by spectrum
Go out subsystem to export the fluorescence of generation to spectral collection subsystem；3) by the calculating, processing and analysis to collected spectrum,
Complete and quantitative testing qualitative to contained glass ingredient in glass sample to be measured.
Inventor has built experimental provision and has carried out experimental verification according to the present invention, is existed using equipment set forth in the present invention
The spectrum observed in laboratory glass, experiment results are as shown in Figure 3, it can be seen that the spectral line of elemental silicon.
Claims (6)
1. a kind of side of ingredient in analytical equipment real-time online measuring Improving Glass Manufacturing Processes using Laser induced plasma spectroscopy
Method, the equipment include pulse laser, laser import system, spectrum export and collection system, beam splitting system and spectrum acquisition system
System, wherein, spectrum export and collection system include spectrum export subsystem and spectral collection subsystem and, wherein pulse laser
Device and spectrum acquisition system send instruction control by same impulse generator, and laser transmitting laser is gathered by laser import system
At coke to sample, sample surfaces is made to form plasma, generation induced with laser spectrum and will be produced by spectrum export subsystem
Raw fluorescence is exported to spectral collection subsystem, by calculating, processing and the analysis to collecting spectrum so as to contained in sample
Element carries out qualitative and quantitative testing, wherein the laser is all solid state chirped pulse amplification femto-second laser, passes through adjusting
Chirp numerical value realizes laser pulse width from femtosecond to a picosecond consecutive variations,
This method includes：
1) laser of laser transmitting is focused to by laser import system at the glass sample in Improving Glass Manufacturing Processes, makes to treat
Survey glass sample surface and form plasma, generate induced with laser spectrum, 2) the induction spectrum generated passes through spectrum export
System exports the fluorescence of generation to spectral collection subsystem；3) by the calculating, processing and analysis to collected spectrum, complete
And quantitative testing qualitative to contained glass ingredient in glass sample to be measured.
2. according to the method described in claim 1, wherein all solid state chirped pulse amplification femto-second laser be used as from 500 femtoseconds to
The ultra-short pulse laser light source of 100 picoseconds of consecutive variations.
3. according to the method described in claim 1, wherein in all solid state chirped pulse amplification femto-second laser, same transmission
Volume holographic grating had not only been used as stretcher but also as compressor reducer.
4. according to the method described in claim 3, wherein stretcher a femtosecond pulsewidth (such as 150-220 femtoseconds, such as
180 femtoseconds) seed source beam broadening to picosecond pulsewidth (such as 15-25 picoseconds, such as 20 picoseconds), then pass through magneto-optic
Isolator injects regenerative amplifier；Laser beam is reciprocal (such as 60-200 times, such as from about 100 times) back and forth in regenerative amplifier, single
Then pulse energy gradual magnification projects regenerative amplifier to maximum by magneto optic isolator；It is emitted from regenerative amplifier
Laser beam by energy amplification is by compressor reducer laser pulse width from picosecond pulsewidth (such as 15-25 picoseconds, such as 20 picoseconds)
Femtosecond pulsewidth described in compression and back (such as 350-6500 femtoseconds；Such as 500 femtoseconds, i.e. most short pulse duration is 500 femtoseconds), pass through adjusting
Chirp numerical value realizes the laser pulse width from femtosecond to a picosecond consecutive variations.
5. according to the described method of any one of claim 1-4, wherein all solid state chirped pulse amplification femto-second laser is produced
Raw laser is the ultra-short pulse laser from 500 femtoseconds to 100 picoseconds of consecutive variations.
6. according to the described method of any one of claim 1-4, the laser of wherein laser import system is focused to adjustable focal length
Mode and spectral collection subsystem are designed as adjustable focal length system.
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| CN201611004497.XA CN108072635A (en) | 2016-11-15 | 2016-11-15 | A kind of method of ingredient in analytical equipment real-time online measuring Improving Glass Manufacturing Processes using Laser induced plasma spectroscopy |
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| CN201611004497.XA CN108072635A (en) | 2016-11-15 | 2016-11-15 | A kind of method of ingredient in analytical equipment real-time online measuring Improving Glass Manufacturing Processes using Laser induced plasma spectroscopy |
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Cited By (2)
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| CN109521000A (en) * | 2019-01-24 | 2019-03-26 | 中国工程物理研究院流体物理研究所 | Grating beam splitting formula while multiple spot laser induced breakdown spectroscopy measuring system and method |
| CN111239090A (en) * | 2020-02-13 | 2020-06-05 | 华东师范大学重庆研究院 | Method and system for measuring single-pulse laser-induced transient molecular fluorescence spectrum |
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| CN103884689A (en) * | 2014-01-04 | 2014-06-25 | 青岛大学 | Laser induced single droplet breakdown detection method and device |
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