CN1296700C - Mineral material infrared fluorescent light analysis method - Google Patents
Mineral material infrared fluorescent light analysis method Download PDFInfo
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- CN1296700C CN1296700C CNB2003101254327A CN200310125432A CN1296700C CN 1296700 C CN1296700 C CN 1296700C CN B2003101254327 A CNB2003101254327 A CN B2003101254327A CN 200310125432 A CN200310125432 A CN 200310125432A CN 1296700 C CN1296700 C CN 1296700C
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Abstract
The present invention relates to a method for analyzing and identifying the characteristics of trace elements, defects, growth conditions, processes, etc. of samples of mineral substances, material, etc., particularly a method for analyzing infrared fluorescence of material of mineral substances, etc. The present invention is characterized in that a near ultraviolet-infrared light source whose wavelength is slightly shorter than the wavelength of the peak of a fluorescence spectrum to be analyzed is radiated on samples of mineral substances, material, etc. to be analyzed on a sample table in a surface, thread, point or beam expanding mode, and infrared fluorescence is excited; then the infrared fluorescence is converged on an entrance window of an optical splitter; a photoelectric detector is arranged in the position of an exit window of the optical splitter to carry out photoelectric conversion; electrical signals converted from the fluorescence are converted into digital signals in an analog-to-digital conversion mode, and then the digital signals are input into a computer by interfaces; the computer draws a wavelength-intensity curve, namely a fluorescence spectrum; the peak shape, the peak position and the intensity of the fluorescence spectrum (mainly the infrared part) are analyzed to obtain the sample information of the mineral material, etc. The present invention has the characteristics of multiple analyzable varieties of samples of mineral substances, material, etc., wide analyzable wavelength range, high fluorescence excitation efficiency, low cost, etc.
Description
Technical field
The present invention relates to a kind of mineral and material sample be carried out the method that characteristics such as trace element, defective are analyzed and differentiated, specifically, be to mineral, jewel, artificial lens or other method natural or artificial material carries out Infrared fluorescence test analysis and similar sample discriminating.
Background technology
Fluorescence analysis method is an ancient analytical technology, it is generally acknowledged that producing the long visible light of wavelength with short some sample of rayed of blue light, purple light or ultraviolet light equiwavelength is exactly fluorescence, fluorescence color, wavelength and intensity can response sample kind, trace element, defective and distribution thereof, widespread use biology, medical science, organic chemical industry, agricultural, food, jewel, learn, field such as archaeology, criminal investigation.Corresponding instrument mainly contains Ultraluminescence lamp viewer, fluorescent microscope, cathodeluminescence instrument etc.Fluorescence analysis method has generalization tendency in recent years, and as the cathode-luminescence that excites with high-power electron beam, the XRF of excitation of X-rays etc., the fluorescence that is excited is visible light not necessarily also, and can be X ray, ultraviolet light, infrared light etc.As (natural science fund projects: " invisible cathode-luminescence analysis of micron order mineral and GEOLOGICAL APPLICATION ", Yang Yong etc.) such as negative electrode ultra-violet light-emitting micro-zone analysis instrument.But concrete Infrared fluorescence analytical approach yet there are no report as a kind of special mineral, material analysis method and instrument.Present Infrared fluorescence is used and also only is confined to biological and medical application (much need carry out processing such as Infrared fluorescence coloring agent or contrast preparation to sample), anti-forgery ink and evaluation, military with infrared laser fluorescence warning (textile) coating, fluorescent dye method oil analysis etc.Analyzing related patent with Infrared fluorescence has: gradient field fluorescence correlation spectrometer (application number: 01142027.8) be used for the analysing biomolecules associated sample; Multifunctional molecular radar (application number: 01136671.0) be used for the biological cell associated sample; Portable inspection of document instrument (ZL95220975.6) is used for the authenticating document true and false; (application number: 93121606.0) this method mainly is to sneak into fluorescent material in sample to the method for evaluation liquid petroleum product, and the analysis of fluorescence feature is inferred the oil plant quality again.In a word, the principal feature of present fluorescent method is: the wavelength of the fluorescence of being analyzed is visible light (except the XRF); Some need add suitable reagent; Be used for organic sample more; Exciting (illumination) light source is indigo plant, purple, ultraviolet light, X ray, cathode ray.
Summary of the invention
The object of the present invention is to provide the expansion of a kind of sample analysis expanded range, analyzable wavelength coverage, mineral material Infrared fluorescence analytic approach that cost is low.
To achieve these goals, technical scheme of the present invention is: mineral material Infrared fluorescence analytic approach, it is characterized in that: the light source of choosing wavelength and be near ultraviolet-infrared is with face, line or point mode irradiation are placed on the mineral material sample to be analyzed on the sample stage, inspire Infrared fluorescence, Infrared fluorescence is converged on the incidence window of optical splitter, the place is provided with photodetector at optical splitter outgoing window, carry out opto-electronic conversion, the electric signal analog to digital conversion that Infrared fluorescence is converted to becomes digital signal, through interface input computing machine, computer drawing wavelength-intensity curve, it is fluorescence spectrum, peak shape to fluorescence spectrum, peak position, the mineral material sample message is obtained in intensive analysis; Also the brightness of the electric signal modulation display after the opto-electronic conversion can be carried out the Infrared fluorescence image and show, or the relative sample position of analog-to-digital digital signal is generated the fluorescence digital image; Or directly or by microscope take pictures carrying out face scanning illumination (contain and expand Shu Zhaoming) time with infrared negative.Adopt methods such as standard specimen contrast, similar sample contrast to analyze, some sample shows different spectrum signatures or fluoroscopic image and has just reached purpose.
The present invention expands to the Infrared fluorescence wave band with (ultraviolet-) visible fluorescence analysis of samples such as mineral, material, expand the fluorescence information scope significantly, but expanded the kind of analytic sample, remedying existing fluorescence analysis method obtains fluorescence information and is only limited to visible light, but assaying or material sample kind are limited, defectives such as Ultraluminescence detection instrument complex structure, ultraviolet-visible fluorescence excitation difficulty.Can be used in growth ring band structure, trace element and distribution, defective and distribution, the crystal of opaque, translucent and transparent mineral and synthetic crystal analysis such as the molecules align degree of order, crystal growth condition, later stage experience, crystal secondary enlargement, recrystallization process, generation of minerals relation and jewel identifies.Also may be used for Quality Detection such as seed, agricultural product, food, beverage, industrial chemicals.
(1) expands the mineral samplers scope that to carry out fluorescence analysis.Conventional fluorescence analysis method can only be analyzed the partially transparent mineral crystal, as adamas etc.Infrared fluorescence may be analyzed some opaque metals and semimetal mineral.As Fig. 3, the 4th, the Infrared fluorescence collection of illustrative plates of sample segment.
(2) expanded range of information.The analyst coverage of general fluorescence analysis is 0.4-0.7 μ m, and the analyst coverage of Infrared fluorescence can the wide 0.4-25 of reaching μ m or wideer (the above near ultraviolet scope of 180nm also can be analyzed).
(3) scanning by computer drives sample stage or control excitation beam can realize the analysis of sample point, line, surface fluorescent characteristics.
(4) but the time response of irradiation analytic sample fluorescence of control excitaton source.
(5) because near ultraviolet-infrared light absorbs lessly in air, and instrument system does not need vacuum equipment to keep vacuum, system's operation and cost are lower, make things convenient for.
(6) because light source, infrared eye costs such as infrared laser are lower than ultraviolet source and ultraviolet detector, instrument cost can be lower like this.
Description of drawings
Each wavelength small semiconductor laser of Fig. 1 or led light source wiring layout
Fig. 2 is to be the fluorescence analysis synoptic diagram of light source with small semiconductor laser and LED
Fig. 3 is an abrasive material emery near infrared light spectrogram
Fig. 4 is certain Doped GaAs sample Infrared fluorescence spectrogram
Embodiment
Mineral material Infrared fluorescence analytic approach, its concrete steps are as follows:
1). choose near ultraviolet, visible and infrared light supply, as select the LED device of the light emitting diode of the small semiconductor laser of various wavelength, various wavelength, wavelength is respectively: 460-470,470-480,500-510,520-530,585-593,600-610, equiwavelengths such as 620-635,650,680,850,880,940nm are as excitation source; The light source 1 of each wavelength is installed on the rotatable disk 2 by the wavelength order, and disk can rotate around axle 3, and by register pin 4 location.
2). with the method for test, attempt light with several wavelength, as 400nm, 800nm, 1200nm, 1600nm left and right sides equiwavelength's optical excitation sample, the short-wavelength limit λ of the wavelength of fluorescence that emphasis is to be analyzed is determined in the position that preliminary observation institute excited fluorescent spike is grown
L, then the most effective excitaton source wavelength is about λ
L-10 to λ
L-100nm, the method for available experiment obtains maximum excitation wavelength accurately, makes the fluorescence that is inspired the most outstanding.
3). it is luminous that the light source of maximum excitation wavelength is rotated in place back energized 5, focusing of light process or beam expander 6, photoscanner 7, shine on the mineral material sample (as abrasive material emery) 8, mineral material sample (as abrasive material emery) 8 is fixed on the multidimensional sample stage 9, and drivings of each dimension of sample stage 9 can be the electronic of computing machine 10 controls or manually; Institute's excited fluorescent enters monochromator 11, changes electric signal into by photodetector 12, through AD converter 13 input computing machines 10, composes scanning analysis or the analysis of standing wave changqiang degree by computing machine 10 controls in the analysis again; Keep photoscanner 7, sample stage 9 motionless sample 8 point analysiss of realizing in the analysis, photoscanner 7 or sample stage 9 one-dimensional scannings can carry out sample 8 line analysises, and photoscanner 7 or sample stage 9 two dimensions scan simultaneously can carry out sample 8 surface analysises; Computer drawing wavelength-intensity curve, i.e. fluorescence spectrum, the mineral material sample message can be analyzed or obtain to contrast standard specimen spectrum or similar peak shape, peak position, the strength characteristic of waiting to distinguish the fluorescence spectrum of sample.Adopt methods analysts such as standard specimen contrast, similar sample contrast, spectrum and fluoroscopic image mutation analysis, fluoroscopic image signature analysis; Sample analysis method is general fluorescence analysis method.
Near infrared light spectrogram when as shown in Figure 3, the mineral material sample is certain abrasive material emery.
As shown in Figure 4, sample is certain Doped GaAs sample Infrared fluorescence spectrogram.(annotate: GaAs is a kind of synthetic semiconductor crystal material)
Details:
(1) chooses excitation source
1. choose the principle of excitation wavelength
The excitation source of choosing certain wavelength is crucial.Method and the principle chosen are: earlier with the method for test, attempt with several wavelength light (as 400nm, 800nm, 1200nm, about 1600nm etc.) excited sample, the wavelength short-wavelength limit λ of emphasis fluorescence to be analyzed is determined in the position that preliminary observation institute excited fluorescent spike is long
L, then the most effective excitaton source wavelength is about λ
L-10 to λ
L-100nm, the method for available experiment obtains maximum excitation wavelength accurately, makes institute's excited fluorescent the most outstanding.
2. choose the kind of light source
Best light source is wavelengthtunable Visible-to-Near InfaRed laser instrument (or combination of many sublasers), and its advantage is that brightness is big, the launching efficiency height, and focal length and beam flying are convenient, can carry out micro-zone analysis and light beam face, line, spot scan analysis.Shortcoming is that cost height, wavelength regulation scope are little.
Light source can also select common continuous radiation light source and atomic lamp etc., as: SiC, W silk lamp, iodine-tungsten lamp, high-pressure sodium lamp, deuterium lamp, sodium vapor lamp, blackbody radiation source or the like, principle are strong, the working stabilities of high brightness, visible-infrared light composition.The light of therefrom choosing specific wavelength is to select the light of the wavelength that needs with color filter (sheet) or monochromator (grating, prism etc.) as the method for excitaton source.Advantage is that wavelength coverage is wide, wavelength is easy to adjust, cost is low, and shortcoming is that brightness is low after selecting the light of certain wavelength, the fluorescence that inspires a little less than.
Resultant effect light source selection scheme preferably is a light emitting diode (LED) of selecting the small semiconductor laser of various wavelength and various wavelength as the LED device of series (materials such as InGaN and AlGaInP) such as luminous stronger HF18, HF19, HF30, and wavelength is respectively: 460-470,470-480,500-510,520-530,585-593,600-610, equiwavelengths such as 620-635,650,680,850,880,940nm are as excitation source.
Choose light emitting diode, the concrete device of miniature devices such as semiconductor laser tube during as excitation source be as shown in Figure 2: with the light source 1 of each wavelength (according to the operation instruction of semiconductor laser and LED, install current-limiting resistance, the power supply adapter 17 of divider resistance etc., and fix contact electrode 16, luminous by luminotron 18, see as Fig. 1) be installed on the rotatable disk 2 by the wavelength order, disk can be around axle 3 rotations, and by register pin 4 location, it is luminous that the light source of a wavelength is rotated in place back energized 5, exciting light 14 is through focusing on or beam expander 6 (commodity), photoscanner 7 (commodity), shine on the sample 8, sample 8 is fixed on multidimensional (X, Y, Z, the R rotation, T inclination etc., also can be reduced to 1 dimension) on the sample stage 9 (commodity), driving of each dimension can be the electronic of computing machine 10 controls (drive software and hardware commodity are all arranged) or manually.Institute's excited fluorescent 15 enters monochromator 11 (commodity), change electric signal into by photodetector 12 (commodity), through AD converter 13 (commodity) input computing machine 10 (commodity), compose scanning analysis or standing wave changqiang degree analysis (control and analysis software and hardware all have commodity) by computing machine 10 controls in the analysis again.Keep photoscanner 7, sample stage 9 motionless sample 8 point analysiss of realizing in the analysis; Photoscanner 7 or sample stage 9 one-dimensional scannings can carry out sample 8 line analysises, and photoscanner 7 or sample stage 9 two dimensions scan simultaneously can carry out sample 8 surface analysises.
(2) control of exciting light
1. exciting light size Control: if need macroscopical mean fluorecence situation of analytic sample, (method that expands bundle is the conventional method in the common geometrical optics can to expand bundle to exciting light, as lens combination or the reverse use of telescope etc.), if need the situation of analytic sample microcell to focus on to exciting light.The straightforward procedure of focal length is common geometrical optics method of focusing, adds the method on light hurdle etc. as lens combination.
2. the scan control of excitation beam.If need of the distribution of analytic sample fluorescent characteristics, can be undertaken by the scan mode of control bundle along straight line or plane.Method for scanning is that adopting existing is beam flying element (commodity), as: galvanometer, multiple surface rotating mirror, acousto-optic or electrooptical deflection mirror etc.
(3) sample stage and control
1. volume and weight design sample platform per sample, adjusting and computer control that sample stage should be carried out X, Y, Z three directions drive, and preferably there is sample stage to horizontally rotate the function precision optics platform product of reference optical instrument plant (can directly choose in most cases or), this spinfunction is conveniently to examine under a microscope and seek tiny area to be analyzed earlier, behind latched position and the Rotate 180 degree selected analytic target is placed on the shot point of exciting light.
2. X, Y, Z computer drives, driving step-length and speed can select.Be used for being provided with easily analysis position, and realize sample spot, line or the surface analysis of sample stage type of drive.
(4) fluorescence spectrophotometer and detection
1. fluorescence is assembled on monochromator (or on other beam splitter) incidence window, regulated incidence window and outgoing window, the grating of choosing corresponding wavelength or prism, adjust its direction (can by computer control) carries out corresponding wave band to fluorescence scanning analysis by the method for adjustment of general monochromator.
2. the photodetector (the visible or infrared photoelectric detector spare as PbS, photomultiplier, snowslide photosensitive tube, pyroelectricity, thermal reactor etc.) of corresponding wave band is set at optical splitter outgoing window place, carries out opto-electronic conversion.If weak output signal also needs to adopt feeble signal analytical equipments (commodity are arranged) such as photon counter or lock-in amplifier.
Change in fluorescence curve when 3. detection is controlled quick optical excitation and ended optical excitation fast with methods such as fine light, fast gate light.
(5) fluorescence signal is handled
1. the electric signal analog to digital conversion that fluorescence is converted to becomes digital signal, through interface input computing machine.Computing machine is drawn wavelength-intensity curve, i.e. fluorescence spectrum by its corresponding wavelength.To peak shape, peak position, the intensive analysis of fluorescence spectrum, obtain sample message.
2. the electric signal that fluorescence is converted to is to registering instrument Y direction modulation drafting spectral curve.
3. the electric signal that fluorescence is converted to is modulated display brightness, obtains fluoroscopic image.Or generate the corresponding necessarily digital phosphor image of wavelength channel according to correspondence position after the analog to digital conversion.
(6) other analysis mode
1. with the brightness of the direct modulation display of electric signal after the opto-electronic conversion, the Infrared fluorescence image carried out in the scanning of photoscanning signal modulation display show.
The coordinate of 2. analog-to-digital digital signal and counter sample position generates the fluorescence digital image.
3. carry out face scanning illumination when (contain and expand Shu Zhaoming) directly or by microscope with the take pictures fluoroscopic image of sample of infrared negative.
Claims (3)
1. mineral material Infrared fluorescence analytic approach, it is characterized in that: choosing wavelength is that near ultraviolet-infrared light supply is with face, line or point mode irradiation are placed on the mineral material sample to be analyzed on the sample stage, inspire Infrared fluorescence, Infrared fluorescence is converged on the incidence window of optical splitter, the place is provided with photodetector at optical splitter outgoing window, carry out opto-electronic conversion, the electric signal analog to digital conversion that Infrared fluorescence is converted to becomes digital signal, through interface input computing machine, computer drawing wavelength-intensity curve, be fluorescence spectrum, to the peak shape of fluorescence spectrum, peak position, the mineral material sample message is obtained in intensive analysis; Or with the brightness of the direct modulation display of electric signal after the opto-electronic conversion, the Infrared fluorescence image carried out in the scanning of photoscanning signal modulation display show; Or the coordinate of analog-to-digital digital signal and counter sample position generated the fluorescence digital image; Or directly or by microscope carry out sample analysis carrying out face when illumination scanning with the take pictures fluoroscopic image of sample of infrared negative.
2. mineral material Infrared fluorescence analytic approach according to claim 1, it is characterized in that its concrete steps are as follows: 1). choose near ultraviolet-infrared light supply, the light source (1) of each wavelength is installed on the rotatable disk (2) by the wavelength order, disk can rotate around axle (3), and is located by register pin (4);
2). adopt the method for using test earlier, attempt the light with several wavelength, the wavelength of fluorescence short-wavelength limit λ that emphasis is to be analyzed is determined in the position of the wavelength at preliminary observation institute excited fluorescent spectrum peak
L, then the most effective excitaton source wavelength is λ
L-10 to λ
L-100nm obtains maximum excitation wavelength accurately with the method for testing in this interval, makes fluorescence to be analyzed the most outstanding;
3). it is luminous that the light source of maximum excitation wavelength is rotated in place back energized (5), focusing of light process or beam expander (6), photoscanner (7), shine on the mineral material sample (8), mineral material sample (8) is fixed on the multidimensional sample stage (9), and driving of each dimension of sample stage (9) is the electronic of computing machine (10) control or manually; Institute's excited fluorescent enters monochromator (11), changes electric signal into by photodetector (12), through AD converter (13) input computing machine (10), composes scanning analysis or the analysis of standing wave changqiang degree by computing machine (10) control again; Keep photoscanner (7), the motionless realization sample of sample stage (9) (8) point analysis in the analysis, photoscanner (7) or sample stage (9) one-dimensional scanning carry out sample (8) line analysis, and photoscanner (7) or sample stage (9) two dimension scan simultaneously carries out sample (8) surface analysis; Computer drawing wavelength-intensity curve, promptly fluorescence spectrum to peak shape, peak position, the intensive analysis of fluorescence spectrum, obtains the mineral material sample message.
3. mineral material Infrared fluorescence analytic approach according to claim 2 is characterized in that described near ultraviolet-infrared light supply is the small semiconductor laser of various wavelength, the LED device of various wavelength.
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| CN105004673B (en) * | 2015-08-24 | 2018-10-19 | 北京雪迪龙科技股份有限公司 | A kind of infrared spectrum sampling platform and infrared spectrum detecting system |
| CN106971162A (en) * | 2017-03-28 | 2017-07-21 | 合肥科的星测控科技有限公司 | A kind of material analyzing system based on laser technology |
| CN107831116B (en) * | 2017-11-29 | 2023-09-05 | 苏州蛟视智能科技有限公司 | Self-adaptive imaging device and method |
| CN111272725A (en) * | 2020-04-03 | 2020-06-12 | 吴建明 | Hazardous article on-site detector based on fluorescence spectrum analysis |
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| US4541438A (en) * | 1983-06-02 | 1985-09-17 | The Johns Hopkins University | Localization of cancerous tissue by monitoring infrared fluorescence emitted by intravenously injected porphyrin tumor-specific markers excited by long wavelength light |
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| CN1336541A (en) * | 2001-09-07 | 2002-02-20 | 清华大学 | Gradient field fluorescence correlation spectrometer |
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| EP1342768A1 (en) * | 2000-11-22 | 2003-09-10 | Tokushu Paper Manufacturing Co. Ltd | Particles emitting fluorescence by irradiation of infrared ray and forgery preventing paper using the same |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4541438A (en) * | 1983-06-02 | 1985-09-17 | The Johns Hopkins University | Localization of cancerous tissue by monitoring infrared fluorescence emitted by intravenously injected porphyrin tumor-specific markers excited by long wavelength light |
| WO1993021530A1 (en) * | 1992-04-10 | 1993-10-28 | Messerschmitt-Bölkow-Blohm Gmbh | PROCESS AND DEVICE FOR INCREASING THE SENSITIVITY AND SELECTIVITY OF IMMUNO-ASSAYS, MOLECULE-RECEPTOR, DNA-COMPLEMENTARY DNA and FOREIGN MOLECULE-HOST MOLECULE INTERACTION ASSAYS |
| EP1342768A1 (en) * | 2000-11-22 | 2003-09-10 | Tokushu Paper Manufacturing Co. Ltd | Particles emitting fluorescence by irradiation of infrared ray and forgery preventing paper using the same |
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