CN202854037U - Integration laser-induced intensified plasma spectrum acquisition system - Google Patents
Integration laser-induced intensified plasma spectrum acquisition system Download PDFInfo
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Abstract
The utility model relates to an integration laser-induced intensified plasma spectrum acquisition system, belonging to the field of laser plasma spectrum detection. The integration laser-induced intensified plasma spectrum acquisition system comprises a pulse laser, a light beam raiser, a spectrometer, a range limiting ring, a high-voltage discharge electrode, an ICCD (Intensified Charge Coupled Device) camera, a focusing lens, a sample room, a reflector, an adjustable fiber optics receiving system, a sample to be tested, a three-dimensional electronic control translation platform, an imaging CCD (Charge Coupled Device), a gas flowmeter and a gas pressure gauge. The integration laser-induced intensified plasma spectrum acquisition system provided by the utility model completes the acquisition of different LIBS (Laser-induced Breakdown Spectroscopy) signals through the control on an environment in a small independent sealing space and synchronous control and realizes integration; and a high-voltage discharge intensified and ring range limitation intensified LIBS system integrating functions of spectrum acquisition, dynamic image analysis and the like realizes more accurate measurement through control on environment stress and shielding gas around the sample, and the operation is quick and convenient. The system is beneficial to industrial production and application.
Description
Technical field
The utility model relates to a kind of integrated laser and induces enhancing plasma spectrometry acquisition system, belongs to the spectrum of laser plasma detection field.
Background technology
At present, Laser-induced Breakdown Spectroscopy (Laser-Induced Breakdown Spectroscopy, LIBS) detection technique is rapid as a kind of atomic emission spectrum technical development, by adopting high-resolution spectrometer, the LIBS technology can realize that the multielement of solid, liquid, powder and gaseous matter detects online, and, can under rugged surroundings, carry out in real time.The LIBS technology can realize concentration or content analysis to element in the sample by amalyzing substances plasma spectrometry intensity data, thereby realize the qualitative and quantitative analysis of material, have fast, need not sample preparation, loss is minimum and multielement such as detects simultaneously at the advantage.The LIBS technology can be applicable to the numerous areas such as chemical industry, detection of poison gas, ature of coal on-line measurement, nuclear industry, medical science.Wherein in the application that succeeded aspect gemstone testing and some the industrial on-line monitorings.
Because the induced with laser material produces in the process of plasma, matrix effect is large, the laser light scattering background interference is large, plasma emission spectral line theoretical system is incomplete, in the practical application, LIBS detects and exists sensitivity lower, detection limit even higher than traditional spectral technique, and quantitatively detect the problems such as difficult, limited development and the application of this technology.The result of most LIBS also rests on the laboratory.A lot of systems can not satisfy the needs of industrialization on-the-spot test.From the angle of scientific research, in many research about LIBS, explore the laser induced plasma mechanism of production, the intensity of enhancing substance characteristic signal and reduction LIBS detection limit are the primary study directions of LIBS technology.Angle from industrialization and the marketization.The practical integrated LIBS detection system that has than high s/n ratio and lower detection limit is the target that pursue in enterprise and market.
In order to improve the intensity of LIBS detectable signal, all done some more typical systems both at home and abroad and improved and research.As adopt the double-pulse laser shooting techniques, and two pulse actions that namely utilize be separated by several nanoseconds or several delicate times are to the same position of material, and this technology can improve signal intensity and detection sensitivity.Also there are a lot of reports in the LIBS system that utilizes effluve to strengthen, patent report is also arranged on monopulse LIBS basis, adds second high electric field pulse and strengthens laser induced plasma atomic radiation intensity.Yet, for the detection of Cucumber element, no matter be complicated double-pulse system or the LIBS system of the enhancing of discharging etc., sensitivity still need improve.Above result has promoted the development of LIBS system effectively, but major part rests on experimental stage.Especially in the result of the research and development of industrialization all-in-one seldom.
The utility model content
The purpose of this utility model is to rest on laboratory stage in order to solve prior art, can't satisfy the demand of industrialization on-the-spot test, has proposed a kind of integrated laser and has induced enhancing plasma spectrometry acquisition system.
The utility model purpose is achieved through the following technical solutions.
Integrated laser of the present utility model is induced and is strengthened the plasma spectrum acquisition system, comprises pulsed laser, light beam lifter, spectrometer, confinement ring, high-voltage discharging electrode, ICCD camera, condenser lens, sample chamber, catoptron, adjustable fiber optics receiving system, testing sample, three-dimensional electronic control translation stage, imaging CCD, gas flow meter, gas gauge;
Annexation: the ICCD camera is positioned over loam cake place, sample chamber; Imaging CCD, catoptron, condenser lens are placed successively, and are integral straight line with sample spot, and imaging CCD, incidence reflection mirror, condenser lens are positioned on the sample chamber and cover; The bottom, sample chamber has air intake opening, and top has the gas outlet, and gas is full of whole sample chamber when guaranteeing to fill protection gas; Gas flow meter is installed in the air intake opening place, is used for the control gas flow, and gas gauge is installed in optional position on the sample chamber, can carry out the measurement of Laser induced plasma spectroscopy under different buffer gass and the pressure environment; The side, sample chamber has view window, and there is dismountable lid at the view window place, but by view window direct viewing inner case, and be convenient for changing sample; Miniature three-dimensional adjustment rack one end is fixed on the internal side wall of sample chamber, and the other end is used for fixing the fibre-optical probe of spectrometer; The D translation platform is fixed in the bottom of casing, and sample is positioned over D translation platform top, by the movement of D translation platform, can realize repeatedly exciting the sample diverse location; The confinement ring is placed on sample top, and the confinement ring does not directly contact with sample, and the confinement ring is fixed on the internal side wall of sample chamber by support, and simultaneously confinement endless belt has handle, can debug in advance the position of confinement ring; After high-voltage discharging electrode passes the confinement ring, the corresponding placement, namely two high-voltage discharging electrodes become 180 ° of angles, and high-voltage discharging electrode is fixed on the internal side wall of sample chamber by support; Pulsed laser passes through the light beam lifter with laser directive sample; Computing machine induces enhancing plasma spectrum acquisition system to be connected with integrated laser, is used for gathering and showing data.
Described adjustable fiber optics receiving system comprises miniature three-dimensional adjusting bracket and optical fiber end lenticule.
The material of described confinement ring is electrically non-conductive material, is preferably teflon, and the diameter of confinement ring is 2-6mm.
Described high-voltage discharging electrode is spherical cylindrical electrode for the tip.
The fiber optics receiving system of described spectrometer is equipped with polaroid, and this polaroid is used for the selective reception of emission spectrum polarization.
The course of work is: pulsed laser is launched a bundle of pulsed laser, after light velocity lifter promotes, get on the catoptron of top, sample chamber after, by condenser lens, impinge perpendicularly on and produce laser induced plasma in the confinement ring; Because sample surfaces and confinement ring close together, plasma outwards expand rapidly in the space of confinement ring; Part electronics and ion enter between the high-voltage discharging electrode that has charged, and are excited once again under the effect of high-voltage discharging electrode voltage, thereby have produced stronger plasma spark, and this spark is limited in again in the confinement ring; Therefore, the signal intensity of material plasma light has obtained enhancing; Utilize adjustable fiber optics receiving system, maximization receives luminescent spectrum, and obtains on computers the real time spectrum demonstration; The ICCD of top, sample chamber takes synchronously and excites the rear different laser plasma plume wing constantly, carries out computer picture and shows, analyzes excited state; According to the realtime graphic that CCD gathers, judge the situation that excites the position; Utilize the movement of D translation platform, the diverse location that can exchange sample surfaces for excites, separately the spectra re-recorded data; But the also different position of continuous agitation, and gather associated picture and spectrum; The spectroscopic data and the plasma view data that collect are analyzed, and the comparison of element original spectrum, qualitative and quantitative analysis provided.
Beneficial effect
1, integrated laser of the present utility model is induced and is strengthened the plasma spectrum acquisition system, utilize the control of environment in the less independent sealed space and the collection that synchro control is finished Different L IBS signal, realized integrated, integrated spectra collection, the LIBS system that the effluve of the functions such as dynamic image analysis strengthens, the ring confinement strengthens synchronously utilizes the control of sample ambient pressure and protection gas to realize measuring more accurately; Efficient and convenient.Be conducive to suitability for industrialized production and application.
2, integrated laser of the present utility model is induced and is strengthened the plasma spectrum acquisition system, in the middle of the high electric field pulse electrode, add a confinement loop configuration, greatly improve the detection signal strength of LIBS, thereby further reduced the detection limit of material element, improved spectral detection sensitivity.Can be used better in fields such as coal industry, smelting industries.
3, integrated laser of the present utility model is induced and is strengthened the plasma spectrum acquisition system, can obtain the time resolved spectroscopy image of high-resolution laser induced plasma by ICCD, analyze the mechanism of laser and material, laser plasma interactions, carry out the detection of material and take isoionic state, optimize better signal acquiring system.
Description of drawings
Fig. 1 is that integrated laser of the present utility model is induced the synoptic diagram that strengthens the plasma spectrum acquisition system;
Fig. 2 is the synoptic diagram that ICCD obtains the plasma spectrometry image device;
Fig. 3 sample induced with laser strengthens plasma spectrometry part effect synoptic diagram.
Wherein, 1-confinement ring, 2-high-voltage discharging electrode, 3-ICCD camera, 4-condenser lens, 5-sample chamber, 6-catoptron, the adjustable fiber optics receiving system of 7-, 8-testing sample, 9-D translation platform, 10-imaging CCD, 11-gas flow meter, 12-gas gauge.
Embodiment
Below in conjunction with embodiment content of the present utility model is further described.
Embodiment
Integrated laser is induced and is strengthened the plasma spectrum acquisition system, comprises the adjustable fiber optics receiving system 7 of fibre-optical probe, testing sample 8, D translation platform 9, imaging CCD10, gas flow meter 11, the gas gauge 12 of pulsed laser, light beam lifter, spectrometer, confinement ring 1, high-voltage discharging electrode 2, ICCD camera 3, condenser lens 4, sample chamber 5, catoptron 6, spectrometer;
Annexation: ICCD camera 3 is positioned over 5 loam cake places, sample chamber; Imaging CCD10, catoptron 6, condenser lens 4 are placed successively, and place in line with sample spot, and imaging CCD10, incidence reflection mirror 6, condenser lens 4 are positioned on the sample chamber 5 and cover; 5 bottoms, sample chamber have air intake opening, and top has the gas outlet, guarantee that gas is full of whole sample chamber 5; Gas flow meter 11 is installed in the air intake opening place, and for detection of gas flow, gas gauge 12 is installed in optional position on the sample chamber 5, can carry out the measurement of Laser induced plasma spectroscopy under different buffer gass and the pressure environment; 5 sides, sample chamber have view window, and there is dismountable lid at the view window place, but by view window direct viewing response situation, and be convenient for changing sample; Miniature three-dimensional adjustment rack one end is fixed on 5 internal side wall of sample chamber, and the other end is used for fixing the fibre-optical probe of spectrometer; D translation platform 9 is fixed in the bottom of casing, and sample is positioned over D translation platform 9 tops, by the movement of D translation platform 9, can realize repeatedly exciting the sample diverse location; Confinement ring 1 is placed on sample top, and confinement ring 1 does not directly contact with sample, and confinement ring 1 is fixed on 5 internal side wall of sample chamber by support, and simultaneously confinement ring 1 can have been debugged the position of confinement ring 1 in advance with handle; After high-voltage discharging electrode 2 passes confinement ring 1, the corresponding placement, i.e. 2 one-tenth 180 ° of angles of two high-voltage discharging electrodes, high-voltage discharging electrode 2 is fixed on 5 internal side wall of sample chamber by support; Pulsed laser passes through the light beam lifter with laser directive sample; Computing machine induces enhancing plasma spectrum acquisition system to be connected with integrated laser, is used for gathering and showing data.
The material of described confinement ring 1 is teflon, and the diameter of confinement ring 1 is 6mm.
Described high-voltage discharging electrode 2 is spherical cylindrical electrode for the tip.
The fiber optics receiving system of described spectrometer is equipped with polaroid, the reception that this polaroid can the filtering parasitic light, the signal to noise ratio (S/N ratio) that the enhanced spectrum signal receives.
The course of work is: place on the sample stage of a briquette sample in volume 300mm * 300mm * 400mm sample chamber 5, place the polytetrafluoroethylene ring of electroded internal diameter size 6mm on the sample, and fixing handle is fixed on sidewall together, it is positioned on the position about the 0.2mm of sample surfaces top.The position of regulating ring, so that 5 tops, sample chamber overlap with the center of ring substantially by the laser spot center after the condenser lens 4, high-voltage discharging electrode 2 is placed at the two ends of ring, electrode connects peripheral charge-discharge circuit.Sparking electrode is spherical cylindrical electrode for the tip, and two sparking electrode spacings are about 4mm, and charge and discharge capacitance is 6nF, and the constant-voltage of direct supply is at 15kV.Electrode discharge is to exist in the middle of two electrodes under the condition of laser induced plasma to realize.In the experimentation, ring maintains static with electrode.After sealing is good, at first deflates and be filled with argon gas to the 1000mbar, laser instrument adopts the Nd:YAG pulsed laser, and optical maser wavelength is 532nm, and pulsewidth is 5ns, maximum Output of laser energy 130mJ@532nm.During actual measurement, the employing energy is that the laser of 90mJ carries out excited sample generation plasma spectrometry, uses D translation platform 9 mobile examples, chooses difference and carries out different spectra collections.Start computer control software, make laser instrument, spectrometer, ICCD, sample stage enter numerically controlled duty.Laser instrument is launched a bundle of pulsed laser, after light velocity lifter promotes, get on the catoptron 6 of 5 tops, sample chamber after, by condenser lens 4, impinge perpendicularly on confinement ring 1 interior generation laser induced plasma; Because sample surfaces and confinement ring 1 close together, plasma outwards expand rapidly in the space of confinement ring 1; Part electronics and ion enter between the high-voltage discharging electrode 2 that has charged, and are excited once again under the effect of high-voltage discharging electrode 2 voltages, thereby have produced stronger plasma spark, and this spark is limited in again in the confinement ring 1; Therefore, the signal intensity of material plasma light has obtained enhancing; Utilize adjustable fiber optics receiving system 7, fiber spectrometer can be maximized receive luminescent spectrum, the investigative range of spectrometer is 180nm-950nm, and resolution is less than 0.1nm, and minimum gate-width integration setup times is 1ms, postpones adjustable.And obtain on computers real time spectrum and show; The ICCD camera 3 of 5 tops, sample chamber adopts the external trigger pattern, as shown in Figure 2, resolution is 1024 * 256, it is 2ns that minimum arranges gate-width, the high-definition picture of realizing laser induced plasma assistant and sample ablation situation shows, ICCD takes the laser plasma plume wing of different time state, carries out computer picture and shows, analyzes excited state; According to the realtime graphic of 3,000,000 pixel CCD camera collections, judge the situation that excites the position; Utilize the movement of the three-D electric translation stage of 5 microns of degrees of regulation, another point that can exchange sample surfaces for excites, separately the spectra re-recorded data; But the also different position of continuous agitation, and gather associated picture and spectrum; The spectroscopic data and the plasma view data that collect are analyzed, and the comparison of element original spectrum.The triggering of described pulsed laser and spectrometer, ICCD gathers, and carries out synchro control, and spectrometer and ICCD gather spectrum and can set time delay, can effectively avoid noise signal.
Compare the spectrogram that traditional single-pulse laser induced breakdown spectroscopy obtains, the novel all-in-one induced with laser that adopts the utility model to provide strengthens the plasma spectrum acquisition system, can obtain stronger plasma light spectrogram, spectral line is discrete more clear, and baseline is very flat.As illustrate gained spectrogram shown in Figure 3.
In a word, in the low situation of single-pulse laser induced breakdown spectroscopy detection sensitivity, the novel all-in-one induced with laser that the utility model provides strengthens the plasma spectrum acquisition system, can produce the signal of enhancing, and the system integration degree is high, simple to operate.Be convenient to carrying and be used for different occasions, good stability.This system has good using value in the context of detection of material element.
Claims (4)
1. integrated laser is induced and is strengthened the plasma spectrometry acquisition system, it is characterized in that: comprise pulsed laser, light beam lifter, spectrometer, confinement ring (1), high-voltage discharging electrode (2), ICCD camera (3), condenser lens (4), sample chamber (5), catoptron (6), adjustable fiber optics receiving system (7), testing sample (8), three-dimensional electronic control translation stage, imaging CCD (10), gas flow meter (11), gas gauge (12); ICCD camera (3) is positioned over loam cake place, sample chamber (5); Imaging CCD (10), catoptron (6), condenser lens (4) are placed successively, and being integral straight line with sample spot, imaging CCD (10), incidence reflection mirror (6), condenser lens (4) are positioned on the sample chamber (5) and cover; Bottom, sample chamber (5) has air intake opening, and top has the gas outlet, and gas is full of whole sample chamber (5) when guaranteeing to fill protection gas; Gas flow meter (11) is installed in the air intake opening place, be used for the control gas flow, gas gauge (12) is installed in upper optional position, sample chamber (5), can carry out the measurement of Laser induced plasma spectroscopy under different buffer gass and the pressure environment; Side, sample chamber (5) has view window, and there is dismountable lid at the view window place, but by view window direct viewing inner case, and be convenient for changing sample; Miniature three-dimensional adjustment rack one end is fixed on the internal side wall of sample chamber (5), and the other end is used for fixing the fibre-optical probe of spectrometer; D translation platform (9) is fixed in the bottom of casing, and sample is positioned over D translation platform (9) top, by the movement of D translation platform (9), can realize repeatedly exciting the sample diverse location; Confinement ring (1) is placed on sample top, confinement ring (1) does not directly contact with sample, confinement ring (1) is fixed on the internal side wall of sample chamber (5) by support, and confinement ring (1) has been debugged the position of confinement ring (1) with handle simultaneously; After high-voltage discharging electrode (2) passes confinement ring (1), the corresponding placement, namely two high-voltage discharging electrodes (2) become 180 ° of angles, and high-voltage discharging electrode (2) is fixed on the internal side wall of sample chamber (5) by support; Pulsed laser passes through the light beam lifter with laser directive sample; Computing machine induces enhancing plasma spectrum acquisition system to be connected with integrated laser, is used for gathering and showing data; Pulsed laser is launched a bundle of pulsed laser, after the catoptron (6) of getting to top, sample chamber (5) after the lifting of light velocity lifter is upper, by condenser lens (4), impinges perpendicularly on and produces laser induced plasma in the confinement ring (1); Because sample surfaces and confinement ring (1) close together, plasma outwards expand rapidly in the space of confinement ring (1); Part electronics and ion enter between the high-voltage discharging electrode (2) that has charged, under the effect of high-voltage discharging electrode (2) voltage, be excited once again, thereby produced stronger plasma spark, this spark is limited in again in the confinement ring (1); Therefore, the signal intensity of material plasma light has obtained enhancing; Utilize adjustable fiber optics receiving system (7), maximization receives luminescent spectrum, and obtains on computers the real time spectrum demonstration; The ICCD of top, sample chamber (5) takes synchronously and excites the rear different laser plasma plume wing constantly, carries out computer picture and shows, analyzes excited state; According to the realtime graphic that CCD gathers, judge the situation that excites the position; Utilize the movement of D translation platform (9), the diverse location that can exchange sample surfaces for excites, separately the spectra re-recorded data; But the also different position of continuous agitation, and gather associated picture and spectrum; The spectroscopic data and the plasma view data that collect are analyzed, and the comparison of element original spectrum, qualitative and quantitative analysis provided.
2. integrated laser as claimed in claim 1 is induced and is strengthened the plasma spectrometry acquisition system, and it is characterized in that: described adjustable fiber optics receiving system (7) comprises miniature three-dimensional adjusting bracket and optical fiber end lenticule.
3. integrated laser as claimed in claim 1 is induced and strengthened the plasma spectrometry acquisition system, it is characterized in that: described high-voltage discharging electrode (2) is spherical cylindrical electrode for the tip.
4. integrated laser as claimed in claim 1 is induced and is strengthened the plasma spectrometry acquisition system, and it is characterized in that: adjustable fiber optics receiving system of described spectrometer is equipped with polaroid, and this polaroid is used for the selective reception of emission spectrum polarization.
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| CN102841078A (en) * | 2012-09-10 | 2012-12-26 | 北京宝瑞光电科技有限公司 | Integrated laser-induced enhanced plasma spectrum acquisition system |
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