EP1953537A1 - Dispositif pour détecter ou guider des rayons x utilisant une optique pour rayons x - Google Patents

Dispositif pour détecter ou guider des rayons x utilisant une optique pour rayons x Download PDF

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Publication number
EP1953537A1
EP1953537A1 EP07001978A EP07001978A EP1953537A1 EP 1953537 A1 EP1953537 A1 EP 1953537A1 EP 07001978 A EP07001978 A EP 07001978A EP 07001978 A EP07001978 A EP 07001978A EP 1953537 A1 EP1953537 A1 EP 1953537A1
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Prior art keywords
ray
radiation
sample
optical elements
optics
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EP07001978A
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German (de)
English (en)
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Josef Dr. Kemmer
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    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21K—TECHNIQUES FOR HANDLING PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
    • G21K1/00—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating
    • G21K1/06—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating using diffraction, refraction or reflection, e.g. monochromators
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21K—TECHNIQUES FOR HANDLING PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
    • G21K2201/00—Arrangements for handling radiation or particles
    • G21K2201/06—Arrangements for handling radiation or particles using diffractive, refractive or reflecting elements
    • G21K2201/064—Arrangements for handling radiation or particles using diffractive, refractive or reflecting elements having a curved surface

Definitions

  • the invention relates to a device for detecting and / or guiding X-ray radiation and uses thereof in e.g. analytical and medical applications. Furthermore, the invention relates to the use and the arrangement of X-ray optical systems in the field of analytical or spectroscopic and medical applications. Furthermore, the invention relates to radiation sources and the combination of one or more such radiation sources with one or more optical systems and sensors for measuring the radiation. As sensors, semiconductor detectors such as e.g. Silicon drift detectors (SDDs) or PIN diodes.
  • SDDs Silicon drift detectors
  • PIN diodes PIN diodes
  • X-ray optical systems in particular lens systems and waveguides, which are composed of a large number of glass capillaries (or special X-ray mirrors) are known and have been produced successfully for several years (eg IfG Institute for Scientific Instruments GmbH, Rudower Clice 29/3, D -12489 Berlin Germany). It uses the principle of total reflection of X-rays on the inner surfaces of treated glass capillaries or X-ray mirrors, which means that X-rays can be both focused and forwarded over long distances almost lossless. Since the refractive indices for X-radiation in glass are very close to 1, the rays must impinge on the surface at a very shallow angle in order to be reflected at all.
  • Such lens systems are outstandingly suitable for collimating the diverging X-ray light emanating from an X-ray tube or toward a tiny point focus and thus achieve local amplification of X-rays up to a factor of 500 and even higher at the sample.
  • the intensity and energy distribution of this fluorescence radiation is used to perform a non-destructive quantitative analysis of the irradiated sample. This is possible because each element of the periodic table has a so-called characteristic fluorescence radiation in the X-ray region, which is excited by the primary radiation and can be used for the quantitative analysis of the material composition of the sample.
  • the x-ray optical properties of the abovementioned capillary lens systems depend on the design and the type of capillaries.
  • Lens systems available that reflect the X-ray of a point source back to a point-like focus.
  • the dimensions, in particular the length of these lens systems can be varied within wide limits.
  • half-lenses which generate a parallel X-ray beam from a diverging beam or, in the inverse of the beam path, concentrate a parallel beam into a focus.
  • the X-ray lenses are used to focus the intensity of weak X-ray sources on a sample and thus to strengthen. This has mainly economic reasons, since weak X-ray sources have smaller dimensions, are simpler and safer to operate and are significantly less expensive to buy.
  • the object of the invention is to provide new applications for X-ray optical systems.
  • the invention provides an apparatus for detecting X-radiation, according to the subject-matter of claim 1.
  • Another aspect of the invention is directed to an apparatus for conducting x-radiation, according to the subject-matter of claim 19.
  • Further aspects of the invention relate to uses of said devices in the field of X-ray fluorescence analysis, X-ray analysis, medical technology, quality assurance and / or production monitoring.
  • Fig. 1 a first embodiment of a device for detecting X-ray radiation with a capillary lens system, which serves to detect the divergent X-radiation from a fluorescence excited sample in a larger solid angle and to focus on the X-ray detector.
  • Fig. 2 a second embodiment: a similar structure as Fig. 1 However, wherein the X-ray from the sample is converted by a so-called half-lens into a parallel beam.
  • a parallel x-ray beam can be generated and directed to a more distant x-ray detector and measured.
  • Fig. 3 a third embodiment: two of the half-lenses, one parallelizes the X-rays and the other focuses the parallelized radiation. In between there is a container that is evacuated or filled with a medium of low absorption.
  • FIG. 4 A fourth exemplary embodiment: a conductor for X-ray light with the aid of which the radiation can be guided over greater distances without great losses. This device can also be used for the application according to the invention.
  • Fig. 5 An embodiment of a possible structure of an X-ray source, an X-ray optics between the X-ray source and the sample, the sample, the X-ray optics between the sample and the X-ray detector and the X-ray detector, which is mounted on a housing.
  • Fig. 6 a photograph of an X-ray spectrometer KETEK GMBH, Kunststoff, which can be used in an embodiment of the invention.
  • Fig. 1 illustrates in detail a first embodiment with a capillary lens system which serves to detect the divergent X-ray radiation from a fluorescence excited sample in a larger solid angle and to focus on the X-ray detector, so as to achieve a gain effect up to 500 and higher.
  • a capillary lens system which serves to detect the divergent X-ray radiation from a fluorescence excited sample in a larger solid angle and to focus on the X-ray detector, so as to achieve a gain effect up to 500 and higher.
  • Like reference numerals in the figures indicate the same or similar parts in the embodiments.
  • the X-ray optical system is not used to amplify the intensity of the primary X-ray source, but is used to focus or amplify the emanating from the irradiated sample secondary or fluorescent radiation and thus lossless as possible to supply an X-ray detector in larger Distance from the sample can be located.
  • X-ray optics in X-ray spectroscopy have in common that the X-ray detector is in the immediate vicinity of the sample to be examined and the X-ray optical systems not according to the invention serve to those of the Probe incoming secondary radiation over a longer distance away from the sample to the X-ray detector.
  • the x-ray detector is as close as possible to the sample in order to record and register as much secondary radiation as possible over a large solid angle.
  • the X-ray detectors must be cooled to temperatures between 0 ° C and -50 ° C. So there are additional cooling devices on cold fingers or heatpipes required to reach the necessary temperatures at the X-ray detector.
  • X-ray detector and sample are often installed in special measuring chambers, which are evacuated during the measurement or filled with gas. This is especially true for use in electron microscopes.
  • Inventive embodiments are characterized in an extremely advantageous manner by the fact that the use of the X-ray optics between the sample and the X-ray detector, the X-ray detector no longer needs to be placed in the immediate vicinity of the sample, but can even be installed outside the measuring chamber. When used in electron microscopes can be eliminated by the backscattered and the detector striking the electrons caused background.
  • the X-ray detector with the entire cooling and amplifier technology can be accommodated in a separate housing outside the evacuated measuring chamber.
  • the measuring chambers can be downsized and the cooling technology can be greatly simplified since no more cold fingers are needed.
  • the standard cold fingers made of copper have the disadvantages that they are heavy and, depending on the diameter of the finger lead to a loss of heat of about 0.5 to 1 degree C per cm length of the finger. With finger lengths of several 10 cm, this loss must be compensated for by correspondingly greater (multi-stage) cooling, which requires additional technical effort and additional costs.
  • the cooling element Peltier cooler / Thermo Electrical Cooler: TEC
  • TEC Thermo Electrical Cooler
  • this advantage can be exploited in small, battery-powered handsets, as a reduction of the leakage current by a factor of two for silicon detectors, e.g. SDDs (Silicon Drift Detector) and PIN diodes allows a temperature increase of the X-ray detector by about 7 degrees, without deteriorating its properties. Due to the reduced cooling capacity, a longer operating time of the batteries can thus be achieved. Alternatively, an X-ray detector with a higher leakage current can be cooled lower, thus reducing the leakage current and improving the quality of the X-ray detector.
  • SDDs Silicon Drift Detector
  • PIN diodes allows a temperature increase of the X-ray detector by about 7 degrees, without deteriorating its properties. Due to the reduced cooling capacity, a longer operating time of the batteries can thus be achieved.
  • an X-ray detector with a higher leakage current can be cooled lower, thus reducing the leakage current and improving the quality of the X-ray detector.
  • An additional advantage of an arrangement of X-ray optics between the sample and the X-ray detector in embodiments according to the invention is furthermore that different X-ray optics can be mounted on the same X-ray detector as required by the application, thereby not only achieving high flexibility in the use of the customer, but also in the production of the detector systems, the mechanical structure can be simplified and less execution models are required.
  • devices having a plurality of identical or different lens systems can be realized which, depending on the problem, can also be advantageously used simultaneously.
  • combinations of X-ray optical systems are possible both for the known primary radiation and for the secondary radiation emanating from the sample, or in the case of absorption measurements, the transmission radiation. It may also be advantageous to simultaneously use a plurality of X-ray optical systems and a plurality of X-ray detectors. Such applications are conceivable in X-ray structure analysis.
  • X-ray optics When using the X-ray optics in the primary radiation to increase the intensity of weak X-ray sources, a possibly occurring change in the primary X-ray spectrum is irrelevant. Such a change of the secondary spectrum by the However, X-ray optics has the disadvantage that it can lead to distortions in the energy distribution of the secondary radiation and thus errors in the based on the evaluation of the spectrum quantitative analysis.
  • adjustable X-ray optics for the conduction of X-radiation, comprising a chain of X-ray optical elements, wherein the X-ray optical elements are arranged in a beam path one behind the other.
  • the mean propagation directions of two X-ray optical elements must be at an angle to each other, which is selected so that the condition of the total reflection of the X-radiation over the course of the X-ray optical elements is fulfilled.
  • the X-ray optical elements can be flexibly and / or flexibly coupled to one another in such a way that the angle between the central propagation directions can be varied to such an extent that the condition of the total reflection of the X-radiation remains fulfilled over the course of the X-ray optical elements.
  • adjustable X-ray optics is the use according to the invention of flexible X-ray mirrors or curved or flexible capillaries and capillary bundles made of suitable material, which are optionally provided in the interior with one or more layers of very thin metal layers on which the total reflection of the X-radiation takes place.
  • X-rays can not only be guided straight out and focused, but also be changed in their direction of propagation, in particular follow the directions of propagation of curved capillaries.
  • the inventive use of such curved capillaries has extraordinary constructive advantages, since obviously both the X-ray sources and the X-ray detectors no longer have to be arranged on a straight line connecting the sample. In particular, for use in electron microscopes and small measuring chambers or handheld devices, these advantages can come to full advantage.
  • curvilinear or bendable X-ray capillary optics is of exceptional importance for medical applications, as the X-ray light can be confined in a small space to the areas of the human body where it is needed.
  • An example of this is the treatment of skin tumors, which can also be performed by linear X-ray optics.
  • a curved or flexible capillary optics represents a great simplification.
  • bent or flexible X-ray optics for endoscopic treatments or in the local irradiation of internal organs.
  • it represents a huge step forward in the treatment of tumors in the intestinal area, even if small tumor colonies from the inside of the intestine can be specifically treated with X-ray therapy.
  • An advantage of the bent or flexible X-ray optics, which can not be overestimated, is that the entire X-ray source with the power supply, etc., are outside the body, are not affected by the intervention, and only the X-ray optics needs to be cleaned or replaced.
  • Such arrangements can be advantageously combined with existing endoscopes, so that a faster use in medical technology is to be expected. It is also possible to use the capillaries of the X-ray optics at least partially as light guides in order to illuminate the areas to be examined or to visualize and locate them via suitable optical systems.
  • X-ray examinations are playing an increasingly important role in measurement and testing technology as well as in the monitoring of current production processes. Examples include the error-free contacting of chips in microelectronics or the inspection of welds in piping systems.
  • X-rays are usually used as the primary radiation for exciting the X-ray fluorescence radiation of a sample, but the excitation of the fluorescence radiation is also possible with other sources such as electrons or ionizing radiation such as electrons, protons or alpha particles etc. or radioactive sources.
  • sources such as electrons or ionizing radiation such as electrons, protons or alpha particles etc. or radioactive sources.
  • fluorescent radiation which can be used in addition to the figure serving backscattered electrons for an element mapping.
  • the method of analysis in electron microscopes is often referred to as EDX analysis (energy dispersive x-ray analysis).
  • the analysis with the aid of protons is used in a method known as PIXE (proton induced x-ray emission).
  • Radioactive sources are widely used in handheld devices and planetary exploration because they are smaller in size and do not require electrical power.
  • Fig. 1 shows this an apparatus for detecting X-ray radiation with an X-ray optical lens 1, which is between a by a primary radiation source (not shown), such as X-ray source, electron beam source, ionizing radiation source, radioactive sources, etc., irradiated sample 2 and an X-ray detector 4.
  • a primary radiation source such as X-ray source, electron beam source, ionizing radiation source, radioactive sources, etc.
  • divergent radiation 3a is emitted. This is secondary or fluorescent radiation, to which the sample 2 is excited by the primary radiation.
  • the lens 1 collects the diverging radiation 3a via an opening with the diameter d1 and produces over a length L behind an opening with the diameter d2 focused radiation 3b at the X-ray detector 4.
  • the distance of the sample 2 to the lens 1 is denoted by f P , the Distance of the lens 1 to the X-ray detector 4 with f D.
  • Fig.2 shows an apparatus for detecting X-ray radiation with an X-ray optical half-lens 5, which is at the beginning of a by a primary radiation source (not shown) irradiated sample 2 beginning and bridging distance L, and one end of a container 7, the evacuated or with a medium of low attenuation is filled and that extends over part of the distance L to be bridged.
  • divergent radiation 3a is emitted.
  • the half-lens 5 collects the divergent radiation 3 a via an opening with the diameter d1 and generates a parallel beam 3c, which covers part of the distance L in the container 7.
  • Parallel radiation in the sense of the exemplary embodiments means that individual rays propagate in imaginary or concrete parallel, straight or curved channels of width ⁇ , where ⁇ is smaller by a multiple than the length of the channels. Focusing in the sense of the embodiments means that a beam of a certain width is bundled to a smaller width.
  • Fig. 3 shows a further variant with the half-lens 5 and the container 7 in the arrangement with sample 2, as in Fig. 2 and a further to the half-lens 5 exactly adjusted half-lens 6 in front of an X-ray detector 4.
  • the other terms and functions correspond to the descriptions Fig. 2 and Fig. 3 , If samples have different geometries, the container 7 can also be made variable in length along the distance L b .
  • the X-ray detector 4 can also be mounted without the half-lens 6 behind the container 7.
  • a straight capillary 8 as shown in FIG Fig. 4 is shown closer, for bridging a distance L between the sample 2 and X-ray detector 4 are attached. If the capillary 8 is preferably bent, then a propagation direction of X-radiation can be influenced as long as the condition of total reflection remains satisfied. It is also possible to use several capillaries in parallel as capillary bundles.
  • the capillary 8 can be made elastically deformable or permanently bent.
  • a plurality of capillaries may be arranged in a chain in the beam path one behind the other;
  • a single capillary can also be understood as a chain of shorter capillaries, which are arranged directly behind one another in the beam path.
  • capillary bundles can also be used indirectly and / or be arranged directly behind one another. If the X-ray radiation (3a, 3b, 3c) is to be both focused and guided, X-ray optical elements such as lenses 1, half lenses 5, 6, containers 7, which are evacuated or filled with a medium of low attenuation, and / or capillaries 8 can also be used be combined in the beam path one behind the other in a chain.
  • the individual x-ray optical elements (1; 5; 6; 7; 8) can be movable relative to one another.
  • Each of the X-ray optical elements (1; 5; 6; 7; 8) carries X-radiation (3a; 3b; 3c) along a mean propagation direction which is the mean propagation direction of the sum of the X-ray propagation direction vectors (3a; 3b; 3c) at the output of an X-ray optical system Elements (1; 5; 6; 7; 8) corresponds.
  • Fig. 5 shows the schematic structure of an embodiment of an X-ray spectrometer according to the invention for use in the RFA, wherein a first X-ray optical element 10 serves to focus the primary radiation of the X-ray source 9 to the sample 2.
  • a second X-ray optical element 11 detects the secondary fluorescence radiation emanating from the sample 2 and, according to the invention, images it onto an X-ray detector 4, with the aid of which the spectral analysis is carried out.
  • the distance of the X-ray detector 4 from the sample 2 can be varied within wide limits. Since the cold finger is eliminated, the X-ray detector 4 can be mounted directly on a housing 12 of the X-ray spectrometer, which contains an electronics and is used for heat dissipation.
  • Fig. 6 shows a photograph of an AXAS X - ray spectrometer KETEK GMBH, Kunststoff, which is for the embodiment of the Fig. 5 suitable is.
  • the thermoelectrically cooled X-ray detector is connected via a longer copper rod as a heat conductor to the housing, which serves for heat dissipation and in which the electronics is located.
  • the copper rod is replaced by a suitable X-ray optics, which makes it possible to integrate the cooled X-ray detector directly in the AXAS housing and thus to achieve, among other advantages, in particular an improvement or a reduction of the required cooling capacity.

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)
EP07001978A 2007-01-30 2007-01-30 Dispositif pour détecter ou guider des rayons x utilisant une optique pour rayons x Withdrawn EP1953537A1 (fr)

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EP07001978A EP1953537A1 (fr) 2007-01-30 2007-01-30 Dispositif pour détecter ou guider des rayons x utilisant une optique pour rayons x

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102009009602A1 (de) * 2008-10-27 2010-04-29 Ifg - Institute For Scientific Instruments Gmbh Spektralauflösende elektronische Röntgenkamera
DE102013209104A1 (de) * 2013-05-16 2014-11-20 Carl Zeiss Microscopy Gmbh Vorrichtung und Verfahren zur spektroskopischen Analyse
CN113109374A (zh) * 2021-03-30 2021-07-13 中国科学院合肥物质科学研究院 一种长光路能量色散x-射线衍射装置
CN115389538A (zh) * 2022-08-09 2022-11-25 深圳市埃芯半导体科技有限公司 X射线分析装置及方法

Citations (7)

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Publication number Priority date Publication date Assignee Title
DE4408057A1 (de) * 1994-03-07 1995-09-14 Ifg Inst Fuer Geraetebau Gmbh Verfahren und Vorrichtung zur Röntgenfluoreszenzspektroskopie
WO1995031815A1 (fr) * 1994-05-11 1995-11-23 The Regents Of The University Of Colorado Systeme optique de miroirs spheriques pour rayons x rasants
EP0723272A1 (fr) * 1994-07-08 1996-07-24 Muradin Abubekirovich Kumakhov Procede de guidage de faisceaux de particules neutres et chargees et son dispositif de mise en uvre
EP1107293A1 (fr) * 1999-05-28 2001-06-13 Mitsubishi Denki Kabushiki Kaisha Appareil d'exposition aux rayons x, procede d'exposition aux rayons x, masque a rayons x, appareil a rayonnement synchrotron, procede de rayonnement par synchrotron et dispositif a semi-conducteur
EP1170755A1 (fr) * 1999-10-18 2002-01-09 Muradin Abubekirovich Kumakhov Lentille integrale destine a un flux de particules hautes energies, procede de fabrication des lentilles de l'invention et utilisation desdites lentilles dans des dispositifs d'analyse, des dispositifs de traitement par rayonnements et de lithographie
WO2002103710A2 (fr) * 2001-06-19 2002-12-27 X-Ray Optical Systems, Inc. Systeme de spectrometre x dispersif en longueur d'onde avec optique de focalisation pour l'excitation et monochromateur pour la collecte
WO2003081222A1 (fr) * 2002-03-19 2003-10-02 X-Ray Optical Systems, Inc. Criblage de banque combinatoire au moyen d'analyse par rayons x

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4408057A1 (de) * 1994-03-07 1995-09-14 Ifg Inst Fuer Geraetebau Gmbh Verfahren und Vorrichtung zur Röntgenfluoreszenzspektroskopie
WO1995031815A1 (fr) * 1994-05-11 1995-11-23 The Regents Of The University Of Colorado Systeme optique de miroirs spheriques pour rayons x rasants
EP0723272A1 (fr) * 1994-07-08 1996-07-24 Muradin Abubekirovich Kumakhov Procede de guidage de faisceaux de particules neutres et chargees et son dispositif de mise en uvre
EP1107293A1 (fr) * 1999-05-28 2001-06-13 Mitsubishi Denki Kabushiki Kaisha Appareil d'exposition aux rayons x, procede d'exposition aux rayons x, masque a rayons x, appareil a rayonnement synchrotron, procede de rayonnement par synchrotron et dispositif a semi-conducteur
EP1170755A1 (fr) * 1999-10-18 2002-01-09 Muradin Abubekirovich Kumakhov Lentille integrale destine a un flux de particules hautes energies, procede de fabrication des lentilles de l'invention et utilisation desdites lentilles dans des dispositifs d'analyse, des dispositifs de traitement par rayonnements et de lithographie
US20030209677A1 (en) * 1999-10-18 2003-11-13 Kumakhov Muradin Abubekirovich Integral lens for high energy particle flow, method for producing such lenses and use thereof in analysis devices and devices for radiation therapy and lithography
WO2002103710A2 (fr) * 2001-06-19 2002-12-27 X-Ray Optical Systems, Inc. Systeme de spectrometre x dispersif en longueur d'onde avec optique de focalisation pour l'excitation et monochromateur pour la collecte
WO2003081222A1 (fr) * 2002-03-19 2003-10-02 X-Ray Optical Systems, Inc. Criblage de banque combinatoire au moyen d'analyse par rayons x

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102009009602A1 (de) * 2008-10-27 2010-04-29 Ifg - Institute For Scientific Instruments Gmbh Spektralauflösende elektronische Röntgenkamera
WO2010049409A1 (fr) 2008-10-27 2010-05-06 Ifg - Institute For Scientific Instruments Gmbh Caméra radiographique électronique à résolution spectrale
EP2934001A1 (fr) 2008-10-27 2015-10-21 IFG - Institute For Scientific Instruments GmbH Caméra électronique à rayons x à résolution spectrale
US9407836B2 (en) 2008-10-27 2016-08-02 Pnsensor Gmbh Electronic x-ray camera with spectral resolution
DE102013209104A1 (de) * 2013-05-16 2014-11-20 Carl Zeiss Microscopy Gmbh Vorrichtung und Verfahren zur spektroskopischen Analyse
US9927361B2 (en) 2013-05-16 2018-03-27 Carl Zeiss Microscopy Gmbh Devices and methods for spectroscopic analysis
US10436712B2 (en) 2013-05-16 2019-10-08 Carl Zeiss Microscopy Gmbh Devices and methods for spectroscopic analysis
CN113109374A (zh) * 2021-03-30 2021-07-13 中国科学院合肥物质科学研究院 一种长光路能量色散x-射线衍射装置
CN115389538A (zh) * 2022-08-09 2022-11-25 深圳市埃芯半导体科技有限公司 X射线分析装置及方法
CN115389538B (zh) * 2022-08-09 2023-12-29 深圳市埃芯半导体科技有限公司 X射线分析装置及方法

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