CN102519920A - Ultraviolet and deep ultraviolet optical thin film element double-wavelength laser fluorescence spectrometer - Google Patents
Ultraviolet and deep ultraviolet optical thin film element double-wavelength laser fluorescence spectrometer Download PDFInfo
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- CN102519920A CN102519920A CN2011103467229A CN201110346722A CN102519920A CN 102519920 A CN102519920 A CN 102519920A CN 2011103467229 A CN2011103467229 A CN 2011103467229A CN 201110346722 A CN201110346722 A CN 201110346722A CN 102519920 A CN102519920 A CN 102519920A
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Abstract
The invention discloses an ultraviolet and deep ultraviolet optical thin film element double-wavelength laser fluorescence spectrometer, which relates to the technical field of application of an optical thin film element. The spectrometer comprises an ArF laser excitation module, a KrF laser excitation module, a sample chamber, a fluorescence detection module and an experimental synchronous control module, wherein the ArF laser excitation module and the KrF laser excitation module emit and transmit laser; the laser is emitted into the sample surface of the sample chamber to produce fluorescence; the fluorescence generated by the excitation of a sample is emitted out of the sample chamber, is transmitted to the fluorescence detection module in an incidence way to carry out spectrum light split, and is detected by a photoelectric detector to convert a fluorescence signal into an electric signal; and the electric signal is transmitted to the experimental synchronous control module. In the spectrometer, two lasers of ArF laser and KrF laser are used as laser sources, so that the sensitivity of ultraviolet and deep ultraviolet fluorescence spectrum detection is improved, and the requirements of testing of an ultraviolet and deep ultraviolet waveband optical thin film weak fluorescence spectrum can be met.
Description
Technical field
The present invention relates to the optical thin film element applied technical field, particularly ultraviolet and deep ultraviolet optics thin-film component dual-wavelength laser XRF.
Background technology
According to quantum theory, atom or molecular energy band comprise a series of discrete energy levels structure, after the material absorbing electromagnetic radiation; The ground state of atom or molecule or low-lying level electronics are excited to higher energy level; Form the atom or the molecule of excited state, the atom or the molecule that are in excited state be through the radiation transistion process, with launching identical with excitation wavelength or long wavelength's light more; Be so-called fluorescence, the principle of fluorescence phenomenon generation that Here it is.When level structure more complicated that atom or molecule comprise,, form spectrum with the fluorescence that produces different wave length.Therefore, fluorescence spectrum carries out quantitative test as a kind of intrinsic property of material through the different wave length radiation intensity that gives off after material is stimulated, i.e. fluorescent spectroscopy can accurately obtain composition, content and the status information of material.In addition because fluorescence spectrum test is in a low-down dark background, to carry out, to compare with absorption spectrum etc., the sensitivity of fluorescence spectrum test is higher.Just be based on above-mentioned factor, the fluorescence spectrum technology has become in crucial a kind of analytical technologies in field such as physics, chemistry, biology and materials.
Along with the continuous expansion of technology and demand, the research of ultraviolet and deep ultraviolet wave band optical thin film element is just becoming more and more important with application.Yet because ultraviolet and deep ultraviolet wave band are near the energy level forbidden band of most of usable medium membraneous materials; The intrinsic of membraneous material absorbs more serious; Various impurity of introducing in the process of film preparation simultaneously and defective are more serious to the influence that the influence of film also will be compared the visible waveband film, and the various defectives that especially form at the membraneous material bandtail are one of principal elements that have a strong impact on by restriction ultraviolet and deep ultraviolet optics thin-film component.Utilize the fluorescence spectrum technology to survey the various trace impurities and the defect state of ultraviolet and deep ultraviolet optics film and element internal; Be to understand the important means of estimating ultraviolet and deep ultraviolet optics film and element optical property and then groping to improve ultraviolet and film preparation of deep ultraviolet optics and treatment process in depth, have important and practical meanings.
Can be applied to the fluorescence spectrum instrument of ultraviolet and deep ultraviolet optics thin-film component at present, mainly all be to adopt high-pressure discharge arc lamp, like the Xe lamp, as the light source of XRF.No matter utilize the general XRF of wide spectrum light source recited above, be to adopt Xe lamp or D
2Lamp as light source carries out ultraviolet and deep ultraviolet optics thin-film component fluorescence spectral measuring and all exists some significantly not enough.These deficiencies are wide inadequately except the work covering wavelength of XRF; For example the shortwave work lower limit of these wide spectrum light sources generally all is by the end of 200nm; Can't satisfy outside the needs of 193nm optical thin film research; Main problem is that the sensitivity of fluorescence detection is lower, can't satisfy the practical application needs.Cause the lower reason of fluorescence detection sensitivity to comprise: the very thin thickness of ultraviolet and deep ultraviolet optics film, corresponding fluorescence signal a little less than; The luminous intensity of wide spectrum light source between 200-800nm is very inhomogeneous, and especially the excitation intensity of ultraviolet below reaching about 250nm and deep ultraviolet wave band is lower, be well below the excitation intensity at visible waveband; Wide spectrum light source need carry out grating beam splitting, can cause under the less situation of the bandwidth of corresponding loss, especially spectrum of exciting light energy; Adopt grating beam splitting simultaneously, the own signal of the inadequate light source of optical filtering that grating high-order effect etc. causes can produce fluorescence signal and disturb.Above-mentioned factor is superimposed, and can seriously reduce the sensitivity of ultraviolet and deep ultraviolet wave band fluorescence detection, and then reduces ultraviolet and the Practical significance of deep ultraviolet wave band fluorescence spectrum detection in ultraviolet and deep ultraviolet optics thin film study.
Different with arc discharge wide spectrum light sources such as Xe lamps; LASER Light Source has characteristics such as monochromaticity and intensity height; Therefore adopt the light source of laser as XRF; With the detection sensitivity that greatly improves fluorescence spectrum, thereby solve the deficiency that the wide spectrum light source XRF exists, satisfy the needs of ultraviolet and deep ultraviolet optics thin film study well.Yet; Because the material level structure is many and complicated; And the not equal reason of the level structure of different materials, iff adopts the light source of the laser of single wavelength as fluorescence spectrum, can not satisfy the needs of different membraneous material tests sometimes well; Can overcome the problem that single wavelength laser light source XRF exists well through two laser, satisfy the needs of different ultraviolets and deep ultraviolet optics thin film study at entire ultraviolet and deep ultraviolet band selection suitable wavelength.
The existing ultraviolet-visible XRF that comprises wide spectrum light source, its basic structure is as shown in Figure 1, and this also is to use maximum XRFs at present.The wide spectrum light source XRF mainly comprises compositions such as wide spectrum light source, exciting light monochromator, sample chamber, emission monochromator, photodetector system.Wherein the exciting light monochromator generally is made up of chromatic dispersion grating and slit, is used for the light of wide spectrum light source different bandwidth and wavelength is separated, i.e. selective excitation wavelength and bandwidth.Emission monochromator is made up of chromatic dispersion grating and slit equally, but is used for the light of fluorescence spectrum different bandwidth and wavelength is separated, and promptly selects to survey wavelength of fluorescence and bandwidth.Photodetector system generally is made up of highly sensitive photomultiplier and corresponding circuit etc.The groundwork process of this type of XRF is to be separated by the light of exciting light monochromator with wide spectrum light source different bandwidth and wavelength; Select required excitation wavelength and bandwidth; Separate by the light of emission monochromator simultaneously different wave length in the fluorescence spectrum that produces; And survey the different wave length fluorescence intensity in the required scope successively by Photodetection system, obtain fluorescence spectrum thus.
Summary of the invention
The needs that can not satisfy different membraneous materials tests well that exist to prior art, be prone to fluorescence signal produced and disturb and problem such as luminous intensity is very inhomogeneous; The present invention provides a kind of ultraviolet and deep ultraviolet optics thin-film component dual-wavelength laser XRF, with the problem that solves technology existence now.
Ultraviolet and deep ultraviolet optics thin-film component dual-wavelength laser XRF, this spectrometer comprises: ArF laser excitation module, KrF laser excitation module, sample chamber, fluorescence detection module and experiment synchronization control module; Said ArF laser excitation module emission and transmission ArF laser are incident to the sample chamber; Emission of KrF laser excitation module and transmission KrF laser are incident to the sample chamber; Said laser excitation optical thin film sample, the fluorescence that is produced outgoing from the sample chamber is incident to fluorescence detection module post-concentration, and converts fluorescence signal to electric signal, is sent to the experiment synchronization control module.
Beneficial effect of the present invention: the present invention adopts ArF laser and two kinds of ultraviolets of KrF laser and deep ultraviolet excitation source; Can greatly improve the sensitivity that ultraviolet and deep ultraviolet fluorescence spectrum are surveyed, overcome deficiencies such as the wide spectrum light source XRF is low in the exciting power of ultraviolet and deep ultraviolet wave band existence, noise is big, detection sensitivity is low; Through two laser, overcome the limitation of single wavelength laser light source XRF, thereby can satisfy the needs of ultraviolet and deep ultraviolet optics thin-film component hypofluorescence spectral investigation well at entire ultraviolet and deep ultraviolet band selection suitable wavelength.
Description of drawings
The structural drawing of the ultraviolet-visible XRF of Fig. 1 prior art wide spectrum light source.
The functional diagram of Fig. 2 ultraviolet of the present invention and deep ultraviolet optics thin-film component dual-wavelength laser XRF.
The structural representation of Fig. 3 ultraviolet of the present invention and deep ultraviolet optics thin-film component dual-wavelength laser XRF.
Embodiment
As shown in Figure 2, ultraviolet and deep ultraviolet optics thin-film component dual-wavelength laser XRF, this spectrometer comprises: ArF laser excitation module, KrF laser excitation module, sample chamber, fluorescence detection module and experiment synchronization control module; Emission of ArF laser excitation module and transmission ArF laser are incident to the sample chamber; Emission of KrF laser excitation module and transmission KrF laser are incident to the sample chamber; Laser excitation optical thin film sample, the fluorescence that is produced outgoing from the sample chamber is incident to the fluorescence detection module and carries out the spectrum beam split; And surveyed by photodetector; Convert fluorescence signal to electric signal, amplify, handle by data handling system afterwards by amplifier; Obtain the spectral distribution of fluorescence intensity, i.e. fluorescence spectrum.
By shown in Figure 3; In order to satisfy the needs of entire ultraviolet and deep ultraviolet wave band optical thin film element hypofluorescence spectrum test research; ArF excimer laser 20 and KrF excimer laser 30 have been selected; Be the needs that can satisfy well on the one hand, can also satisfy other simultaneously fully and be in the needs of 193nm to all the optical thin film element fluorescence spectrum tests of 300nm scope to the optical thin film element fluorescence spectrum test of these two optical maser wavelengths.On the structure; 30 two excitation sources of ArF excimer laser 20 and KrF excimer laser become 90 ° of oblique sample surfaces that are mapped on the sample clamp 40 of intersection, and excitation source all becomes 45 ° with the sample front surface, for this reason; When utilizing the different laser excitation source, sample needs Rotate 180 °.Two excitation sources of ArF laser and KrF laser have in the window entering sample chamber of corresponding bandpass filter through the sample chamber respectively; When adopting ArF excimer laser 20 excitation sources; The sample front surface is towards the direction that becomes miter angle with incident ArF PRK; ArF laser excitation reflection of light and transmission are all carried out delustring and are handled, when adopting KrF excimer laser 30 excitation sources, and sample Rotate 180 °; Its front surface is towards the direction that becomes miter angle with incident KrF PRK, and KrF laser excitation reflection of light and transmission are all carried out delustring and handled.
Excimer laser is used for the light source that the optical thin film sample damage is tested usefulness, selects the product with higher-wattage and high-energy stability for use, and its output facula size is 10mm * 5mm, and the corresponding angle of divergence is 2mrad * 1mrad.The ArF excimer laser is selected the Compax 200-193nm of relevant company for use, and the KrF excimer laser is selected the Compax 200-248nm of relevant company for use.ArF excimer laser 20 has all adopted the control corresponding optical element with KrF excimer laser 30, comprises shutter 21,31, automatically controlled variable attenuator 22,32, collimator and extender mirror system 23,33.In reality test, can be as required, select ArF laser excitation separately, select KrF laser excitation and select two kinds of excitation light source excites equal excitation modes respectively separately; Excimer laser emission laser; Through shutter 21,31, be incident to automatically controlled variable attenuator 22,32, by the laser behind automatically controlled variable attenuator 22, the 32 adjusting power; Be incident to collimator and extender mirror system 23,33; Make 2: 1 incident light of length breadth ratio become 1: 1 emergent light of length breadth ratio, be incident to the sample chamber, its realization is to realize automatically through the experiment synchronization control module.In said mechanism, the mechanical structure that shutter 21,31 adopts pulse signal to trigger carries an electric controller, and this electric controller externally triggering of signal is opened shutter down; Automatically controlled variable attenuator 22,32 adopts the quarter wave plate of an automatically controlled anglec of rotation to realize; The automatically controlled variable attenuator 22 of ArF laser adopts the quarter wave plate of the 193nm wavelength of an automatically controlled anglec of rotation to realize, the automatically controlled variable attenuator 32 of KrF laser adopts the quarter wave plate of the 248nm wavelength of an automatically controlled anglec of rotation to realize.Collimator and extender mirror system 23,33 is a spherical mirror and two anamorphic systems that plano-convex cylindrical mirror telescopic system is formed; This anamorphic system is to becoming 1: 1 square hot spot with 2: 1 the typical output facula of length breadth ratio of excimer laser; The operating distance of whole mirror group is about 600mm; The operation wavelength of the first collimator and extender mirror system 23 is 193nm, and the operation wavelength of the second collimator and extender mirror system 23 is 248nm.
Exciting light gets into the sample chamber; Sample chamber wire chamber 41 is made up of the Al material that inside surface has carried out the black coating processing, on the incident direction of ArF excimer laser 20 and KrF excimer laser 30 excitation sources, opening is arranged, and the bandpass filter sealing of 193nm and 248nm is arranged respectively; The reflection of excitation source and transmission absorb with attenuator 42 respectively; Centre bit at exit facet is equipped with an opening, is used to collect the fluorescence that is produced, and collected fluorescence gets into the fluorescence detection module.
In order to realize the detection of Ultraluminescence spectrum a little less than the optical thin film element; At first need utilize a fluorescence focusing system 50 that beam dump is focused on emission monochromator 51; Separate with the light of emission monochromator then different wave length in the fluorescence spectrum; Get into Photodetection system 52 at last, change fluorescence signal into electric signal, and further amplify and signal extraction by photodetector.Fluorescence focusing system 50 adopts the fluorescence signal of being made up of object lens and field lens to collect optical system, adopts this system, can increase the visual field of collection system, is that focused beam is more even simultaneously.Emission monochromator 51 comprises a diffraction grating level time optical filter wheel, entrance slit, concave grating, a cover concave grating and rotates step-scan mechanism, and exit slit; The optical filter that three different-wavebands are arranged respectively above the diffraction grating level time optical filter wheel; The incisure density of concave grating is 1200 lines/cm, and the central task wavelength is 500nm; Concave grating rotate step-scan mechanism by a precision stepper motor, accurate screw mandrel, and a rotation platform form.Entrance slit and exit slit are automatically controlled mechanical type slit.The beam split of 51 pairs of fluorescence spectrums of emission monochromator mainly is the rotation step-scan mechanism through automatically controlled control concave grating base; Change the incident angle of fluorescence to concave grating; Make the fluorescence spectrum after the concave grating chromatic dispersion launches,, obtain the fluorescence of different wave length successively through exit slit.In order to overcome the high-order effect of diffraction grating, need the percent of pass mating plate to filter high order diffraction fluorescence interference signal.Photodetection system 52 is made up of with signal processing circuit board the sensitive photomultiplier that strengthens of a ultraviolet, corresponding signal amplification.The sensitive photomultiplier that strengthens of ultraviolet can be selected 7852 type photomultipliers of shore pine company for use.
The whole test system of controlling computer 50 realizes integrated control by LabView software.
Signal delay generator 51 is used for the synchro control of all electric control gears, and minimum delay time is differentiated 1ns, pulsewidth 10ns-5ms, and maximum 40s time delay, but external trigger, the way of output is that TTL and CMOS are optional.
Fill N
2Protection pipeline 24 is made up of the Al material that inside surface has carried out handling, and its concrete size is decided according to the physical size of ArF laser excitation module.Fill N
2Gas shiled pipeline 24 has turnover N
2Two openings of gas, N
2The gas inlet port is positioned at the protection pipeline near ArF excimer laser 20 1 sides, its opening vertical optical path, N
2The gas outlet is positioned at collimating and beam expanding system one side; In non-test process; Two openings can seal, and at ArF excimer laser 20 incident ends and the first collimator and extender mirror system, 23 exit ends a deep ultraviolet fused quartz diaphragm are installed respectively, are used for the ArF light beam and pass through.
Claims (8)
1. ultraviolet and deep ultraviolet optics thin-film component dual-wavelength laser XRF is characterized in that this spectrometer comprises: ArF laser excitation module, KrF laser excitation module, sample chamber, fluorescence detection module and experiment synchronization control module; Said ArF laser excitation module emission and transmission ArF laser are incident to the sample chamber; Emission of KrF laser excitation module and transmission KrF laser are incident to the sample chamber; Said laser excitation optical thin film sample produces fluorescence outgoing from the sample chamber, is incident to fluorescence detection module post-concentration, and converts fluorescence signal to electric signal, is sent to the experiment synchronization control module.
2. ultraviolet as claimed in claim 1 and deep ultraviolet optics thin-film component dual-wavelength laser XRF is characterized in that said experiment synchronization control module comprises: controlling computer (10) and signal delay generator (11); Said controlling computer (10) control signal delay generator (11) is to the specific parameter signal of each module emission.
3. ultraviolet as claimed in claim 1 and deep ultraviolet optics thin-film component dual-wavelength laser XRF; It is characterized in that said ArF laser excitation module comprises: ArF excimer laser (20), first shutter (21), the first automatically controlled variable attenuator (22), the first collimator and extender mirror system (23) and fill N
2Gas shiled pipeline (24); Said ArF excimer laser (20) emission ArF laser; Through first shutter (21); Be incident to the first automatically controlled variable attenuator (22), the laser by behind the first automatically controlled variable attenuator (22) the adjusting power is incident to the first collimator and extender mirror system (23); Make 2: 1 incident light of length breadth ratio become 1: 1 emergent light of length breadth ratio, get into the sample chamber and be incident to sample surfaces; The said N2 of filling gas shiled pipeline (24) fills N
2Gas also protects ArF laser excitation module not disturbed by external environmental.
4. ultraviolet as claimed in claim 3 and deep ultraviolet optics thin-film component dual-wavelength laser XRF is characterized in that the said N that fills
2Gas shiled pipeline (24) is provided with aperture in ArF laser excitation module and corresponding position, sample chamber, at ArF excimer laser (20) the incident end and first collimator and extender mirror system (23) exit end diaphragm is installed respectively.
5. ultraviolet as claimed in claim 1 and deep ultraviolet optics thin-film component dual-wavelength laser XRF; It is characterized in that said KrF laser excitation module comprises: KrF excimer laser (30), second shutter (31), the second automatically controlled variable attenuator (32) and the second collimator and extender mirror system (33); Said KrF excimer laser (30) emission KrF laser; Through second shutter (31); Be incident to the second automatically controlled variable attenuator (32), the laser by behind the second automatically controlled variable attenuator (32) the adjusting power is incident to the second collimator and extender mirror system (33); Make 2: 1 incident light of length breadth ratio become 1: 1 emergent light of length breadth ratio, get into the sample chamber and be incident to sample surfaces.
6. ultraviolet as claimed in claim 1 and deep ultraviolet optics thin-film component dual-wavelength laser XRF is characterized in that said sample chamber is made up of sample clamp (40), metallic cavity (41) and attenuator (42); Said sample clamp (40) is positioned over the centerline of ArF laser and KrF laser cross angle; Said attenuator (42) is used for absorbing the light of the reflection and the transmission of excitation source, and it is peripheral that said metallic cavity (41) constitutes the sample chamber, opens hole, three places in laser incident and outgoing place.
7. ultraviolet as claimed in claim 6 and deep ultraviolet optics thin-film component dual-wavelength laser XRF is characterized in that, said sample clamp (40) can carry out the rotation of 180 degree around its base.
8. ultraviolet as claimed in claim 1 and deep ultraviolet optics thin-film component dual-wavelength laser XRF is characterized in that said fluorescence detection module comprises: fluorescence focusing system (50), emission monochromator (51) and photodetector (52); The fluorescence entering fluorescence focusing system (50) that sample is excited and is produced; After assembling, get into emission monochromator (51); By emission monochromator (51) incident fluorescence is carried out beam split, the monochromatic light that is produced gets into photodetector (52), and said photodetector (52) converts light signal to electric signal.
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| CN108982463A (en) * | 2018-09-20 | 2018-12-11 | 韩山师范学院 | One kind being used for Solid surface fluorescence detecting instrument and its detection method |
| CN111380847A (en) * | 2020-03-31 | 2020-07-07 | 深圳大学 | Thin film double-sided fluorescent signal detection device and detection method |
| CN111948187A (en) * | 2020-09-18 | 2020-11-17 | 南开大学 | Device and method for detecting free radicals |
| CN114336264A (en) * | 2021-03-19 | 2022-04-12 | 武汉仟目激光有限公司 | Laser detection method based on dual-wavelength laser |
| CN114689525A (en) * | 2022-04-15 | 2022-07-01 | 中国科学院半导体研究所 | Deep ultraviolet light modulation reflection spectrometer and application thereof |
| CN116539599A (en) * | 2023-07-04 | 2023-08-04 | 科美诊断技术股份有限公司 | Photo-excitation chemiluminescence detection device, control method and photo-excitation chemiluminescence analyzer |
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| CN108982463B (en) * | 2018-09-20 | 2023-10-03 | 韩山师范学院 | Solid surface fluorescence detection instrument and detection method thereof |
| CN111380847A (en) * | 2020-03-31 | 2020-07-07 | 深圳大学 | Thin film double-sided fluorescent signal detection device and detection method |
| CN111380847B (en) * | 2020-03-31 | 2023-08-18 | 深圳大学 | Film double-sided fluorescence signal detection device and detection method |
| CN111948187A (en) * | 2020-09-18 | 2020-11-17 | 南开大学 | Device and method for detecting free radicals |
| CN114336264A (en) * | 2021-03-19 | 2022-04-12 | 武汉仟目激光有限公司 | Laser detection method based on dual-wavelength laser |
| CN114689525A (en) * | 2022-04-15 | 2022-07-01 | 中国科学院半导体研究所 | Deep ultraviolet light modulation reflection spectrometer and application thereof |
| CN114689525B (en) * | 2022-04-15 | 2023-03-10 | 中国科学院半导体研究所 | Deep ultraviolet light modulation reflection spectrometer and application thereof |
| CN116539599A (en) * | 2023-07-04 | 2023-08-04 | 科美诊断技术股份有限公司 | Photo-excitation chemiluminescence detection device, control method and photo-excitation chemiluminescence analyzer |
| CN116539599B (en) * | 2023-07-04 | 2024-03-26 | 科美诊断技术股份有限公司 | Photo-excitation chemiluminescence detection device, control method and photo-excitation chemiluminescence analyzer |
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Application publication date: 20120627 |