• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The present invention relates to a method and a device for investigating the radiographic properties of samples (3c), wherein the x-rays scattered on a sample (3c) are recorded by a detector (5) located at a distance from the sample (3c) and evaluated with respect to the sample properties become. According to the invention, it is provided that, given a predetermined and preferably during the measurements carried out, the distance between the X-ray source (1) or the starting point (2b) of the X-ray (10) directed towards the sample (3c) and the detector (5) remains unchanged for a predetermined number of successive measurements, the distance (S1, S2) between the sample (3c) and the detector (5) is changed and set to predetermined different values.
    公开号:AT511103A4
    申请号:T377/2011
    申请日:2011-03-17
    公开日:2012-09-15
    发明作者:
    申请人:Anton Paar Gmbh；
    IPC主号:
    专利说明:

    The invention relates to a method according to the preamble of claim 1 and further a device according to the preamble of claim 8.
    The invention thus relates to a method and a device for structural characterization of samples by means of small and large or wide-angle scattering of X-radiation.
    The elastic scattering of X-rays is used for the non-destructive structural characterization of different sample materials. X-ray scattering occurs when a bundle of X-rays impinges on an inhomogeneous, powdery, liquid and / or solid material whose structures are of the order of the wavelength of the X-radiation used. The X-rays penetrate into the sample and the material to be investigated interacts with the beam, which is scattered. This leads to characteristic interference images. The distribution of the scattered waves is characteristic of the size and symmetry of the scattering particles. Scattering experiments can be carried out using X-rays as well as in a comparable way with neutron radiation.
    In principle, scattering experiments can be performed in two different geometries: (1) reflection geometry and (2) transmission geometry. The samples are either positioned at a small angle of incidence with respect to the measuring beam, the measurement is made with grazing incidence near the critical angle of total reflection and the radiation pattern of the scattered radiation is recorded (GISAXS) or the sample is transilluminated. While the former method allows statements about the surface structure of the sample, in the transmission measurement the nanostructure of the total irradiated sample volume is analyzed (SAXS). For example, fixed X-ray tubes, rotating anodes or a synchrotron can serve as the radiation-generating sources,
    The Bragg law forms in X-ray diffraction the
    Interpretation basis, we have η.λ = 2.d.sin6, where n is the order of the reflex and an integer, λ is the wavelength and Θ is half the scattering angle,
    Often, the interpretation uses the momentum transfer q, which is defined as
    Typical SAXS measurements are made with X-ray wavelengths in the
    Order of 0.1 nm and are evaluated in the scattering angle range of 0.1 to 10 °. This results in information on the size and size distribution, shape and internal structure of macromolecules, characteristic distances of partially oriented materials, pore size, etc. in the size range of 1 to 100 nm. Thus, the method covers the size range of many technologically interesting nanostructures such as m 9 • * * Λ »· 9 * 4-99 of biopolymers, liquid crystals, nanoporous materials, microemulsions, nanocomposites, etc.
    The smaller scattering angles 2Θ can be examined, the larger the structural dimensions d can be according to the Bragg equation.
    Alternatively, the evaluation of the intensities of the X-ray wide-angle scattering (WAXS) scattered over relatively large angular ranges according to the Bragg equation provides information about the smaller atomic-crystalline structures of the materials.
    In the field of nanomaterials, structural changes affect both areas simultaneously, and it is therefore desirable to study both scattered areas as simultaneously as possible.
    In radiation, smallest scattering angles have to be measured as close to the incident beam as possible.
    FIG. 1 shows the known, basic structure of a measuring arrangement for small-angle scattering measurement.
    The radiation emitted by any source 1, e.g. from a synchrotron, an X-ray tube or a rotary anode, is formed in the subsequent optics 2, which are very different arrangements of Kollimationsblöcken and / or mirrors and other optical elements, the measuring beam. Generally, line and / or point focused convergent and / or parallel monochromatic beams are used. The corrections to be used for the respective scattering geometries in order to correct the real deviations from the ideal scattering experiment are known from the prior art.
    The ready-made beam hits the sample 3 and the scattered intensities are detected spatially resolved with a suitable detector 5. In the prior art, one-dimensional detectors, e.g. a photodiode array which detects the intensity distribution in a line perpendicular to the primary beam, as well as the use of 2-dimensional arrays, e.g. 2D photodiode arrays, CCD cameras or Image Plates (IP).
    Limiting factors are not only the type of X-ray optics 2 used for beam conditioning prior to irradiation of the sample but also the resolution of the detector, in particular due to pixel size and cross-talk between the detector pixels, the correct sample-detector distance and the possibility of the undiffracted Primary beam by means of a beam catcher 4 in front of the detector 5 hide.
    Minimized by restrictive beam conditioning intensities lead to high recording times and excessive noise in the signal.
    The smallest angles to be resolved also depend on the extent of the incident beam and the spatial resolution of the detector used. Frequently, measuring devices in the meter range are therefore used to record evaluable scatter patterns. Because the beam always passes relatively long distances outside the sample, the measurement chambers must always be evacuated to eliminate the background scattering of the air.
    At large sample-detector intervals, the scattered intensity at the detector decreases. This can be prevented by positioning the sample closer to the detector. For geometrical reasons, a larger scattering angle range can thereby also be covered at the same time.
    DE 10 2006 029 449 B3 describes such a device with the possibility of changing the distance between sample and detector by means of a mobile detector and metal bellows sections under vacuum for the beam guidance. This membrane bellows arrangement with directly connected detector allows continuously variable sample-detector distances and allows measurements up to 0 = 40 °. However, the handling and space requirements of such a system make it impossible to use for quick and easy continuous characterization of a sample. The incident beam is generally guided in such systems as a parallel beam. N. Yagi, "simultaneous record of the SAXS / WAXS pattern which uses Shad-o-Box which added change", [online, URL: http: //www.ads-ima.co.ip/products/rad-icon /pdf/saxswaxs.pdf Nov.2011] shows the simultaneous measurement of SAXS and SWAXS using two stationary detectors, each tuned to the intensity and resolution requirements of the angular ranges. The intensity in the WAXS range is measured by fluorescence conversion into visible light. According to Rigaku JP 2009-002805, the measurement of both angular ranges takes place with the aid of two stationary detectors.
    According to AT392160B, a slit or point collimated beam is generated without parasitic reflections which allows an extremely compact structure with high intensities at all scattering angles. This enables a compact design with a sample-detector spacing in the order of <10-30 cm. This device allows with a suitable detector, a so-called imaging plate, which is arranged cylindrically symmetrical about the sample located in the center of this cylinder, the measurement of smallest scattering angles up to scattering angles &gt; 40e.
    However, this cohesive measurement of the small and wide angle range is done with the help of X-ray storage films or imaging plates, which are digitized or read by a special process in an external device. The resolution achieved here is largely determined by the readout process, generally imaging plates have the disadvantage of offline digitization of the scattering image. The possibility of cylindrically symmetrizing the storage film plays an important role in terms of measurement accuracy, since for the small spacings between sample and detector used in the SAXSess system, the distortion is caused by a planar detector surface in the wide-angle range, e.g. in the case of CCDs, play a bigger role. However, the resolution of such imaging plates is limited. Due to the lower intensity values at larger scattering angles, the interference structures appear relatively intense at small angles, while with large scattering angles the scattering intensities are still small. To measure large scattering angle ranges, extremely long IP or a combination of multiple diode arrays must be used to form a polyhedral array. With cylindrically symmetrical IP or photodiode array detectors, scattering angles up to 80 degrees can be measured.
    This would be the measurement with alternative, electronically readable detectors. However, these are not available in cylindrical symmetry and with a sufficiently large detection area. The simultaneous measurement in the SAXS-WAXS range by means of flat detectors is also limited by the necessary distance to the sample. The distance of the detector to the beam-forming unit, that is to the source, mirror or collimation block, is determined by the focus of the primary beam in the optical axis. Therefore, flat electronic detectors such as CCDs can be placed either in the small or wide angle range. The focus of the irradiated beam is in each case in the detector plane, but a complete measurement is not achieved and thus the conversion requires an opening of the measuring chamber.
    The systems described can generally be equipped with a wide variety of sample holders and measuring cells in order to characterize a wide variety of samples. For SAXS measurement systems, for example, capillary holders for liquids, sample holders for solids, paste cells for viscous samples, flow cells for the automatic measurement and characterization of reactions of liquid samples are available as well as a so-called VarioStage for the positioning and orientation of solid samples. With this sample holder, the sample can be rotated in the beam, tilted and screened to perform spatially resolved investigations. A humidity cell for powder and film samples in a climate chamber is available, as is an autosampler for automatically loading the capillary holders via a slide rail system. In all these cases, the assumed measurement position with respect to the incident beam remains approximately the same, movements of the sample with the sample are perpendicular to the sample
    Sliding rail system are used only for adjustment and small variation of the measuring range on the sample.
    Since the Chrp arrays for the electronic detectors are flat plates, and several arranged similar detectors are also too expensive and expensive for standard applications in the industry, a replacement of the imaging plates by compact electronic detectors is not easily possible. In addition, there is also the problem here that each detector has its own characteristic and the necessary corrections and standardizations practically do not lead to a consistently evaluable image.
    The aim of the invention is to design a device of the type mentioned above such that measurements can be carried out with any desired detectors, as are known from the prior art, both in the small angle measuring range and in the wide or wide angle measuring range. It should be in the desired scattering angle range of 0 degrees to angles greater than 40 degrees or in the pulse transfer range from 0 to 28 / nm overlapping scatter images result. In addition, larger scattering angle ranges with smallest possible and only slightly bent IP or photodiode array detectors up to 80 degrees should be possible. It is assumed that the Kleinwinkelstreubereich in the range of 0 degrees to about 10 degrees and the large angle scattering range of about 10 degrees to 50 degrees or 80 degrees given slightly curved detector surface.
    To achieve this object, the invention provided in a method of the type mentioned, the features specified in the characterizing part of claim 1. Thus, apart from a simple modification of the distance between the sample and the detector, it is achieved that measurements of the small-angle scattering range and measurements of the large-angle scattering range can be made alternately in the course of measurements without great conversion difficulties on one and the same sample. The characteristic of the detector remains unchanged and thus the measurement results from the two scattering angle ranges can be evaluated and combined immediately. The position of the detector with respect to the X-ray beam is not changed. It is much easier to adjust the sample along the X-ray beam than to move a much more massive and complex detector for its adjustment. Furthermore, it is also possible to move the sample along the X-ray beam very accurately or to adjust, whereas this adjustment for a detector brings considerable losses in the measurement accuracy with it. Apart from that, the retooling of a detector takes much longer than the adjustment or displacement of a sample, so that measurements in which a rapid succession of measurements of the small-angle scattering range and the large-angle scattering range should take place are not possible.
    According to the invention it is now possible to adjust the sample, wherein the sample is left in the X-ray beam or in the optical axis of the device, while the sample is moved with an adjusting device in a different distance with respect to the detector. There is no need to interrupt the vacuum. At most, the image processing and the scaling must be adjusted and a continuous scattering pattern is obtained without having to re-adjust the measuring beam and the detector.
    It is advantageous if the distance between the sample and the detector remains unchanged and the distance between the X-ray source and the starting point of the sample-directed X-ray and the detector is unchanged and preferably unchanged during the measurements made, and the distance between the sample and the detector is varied for a predetermined number of successive measurements can be set to predetermined different values. This makes it possible to specify the desired distances for certain examinations, which are then approached with the sample or into which the sample is brought to carry out the desired scattering angle measurement.
    It is possible that for changing the distance, a continuous displacement of the sample in or against the direction of the X-ray beam in the predetermined measuring position is made, or that the sample is displaced by the sample in at least two along the X-ray beam at different distances from Detector lying test recordings is used. In the first possibility, the sample may be mounted on an adjusting device which adjusts the sample along the X-ray beam in a continuous, in particular rapid, movement between the two predetermined distances from the detector. It is also possible that, manually or with a gripping device, the sample is transferred from one of the sample receptacles to the other sample receptacle, which sample recordings are located at a defined, predetermined distance from the detector.
    The inventive method is particularly simple if it is provided that the radiation and measurement geometry is kept unchanged during a displacement of the sample and / or during the displacement of the sample, this is left in its position on or with respect to the axis of the X-ray. Thus, a modification of the measurement setup is not required; it is merely the sample spent from one layer to another, the two layers are known and predetermined with respect to their distance from the detector. In both layers, the sample is exposed in a predetermined manner by the X-ray and provides a radiation pattern imaged on the detector. • * * * * * * ~ 7 * * * * * t ·
    It can be provided that the X-rays scattered during the large-angle scattering are imaged onto the detector in the case of a test location of the sample near the detector, and the X-rays scattered in the case of a small-angle scattering are recorded in a test position of the sample remote from the detector. In the situation of the sample, in which the detector of the large-angle scattering range is mapped, can also be provided that the small-angle scattering is hidden, if for longer shots the
    Small angle dispersion would affect the recorded image unfavorable.
    The procedure according to the invention is particularly suitable for receiving scattered X-rays with a plate-shaped CCD sensor. Such CCD sensors are einjustierbar only with great effort and an adjustment of such sensors along the axis of the X-ray beam or the optical axis of the measuring arrangement requires a lot of effort and is tedious.
    A device of the type mentioned is characterized by the features cited in the characterizing part of claim 8. This device allows a rapid change of samples for recording small angle scattering and large angle scattering and is simple.
    In the following the invention will be explained in more detail with reference to the drawing, for example. Fig. 2 shows schematically the structure of a device in which the sample can be moved along the X-ray beam. Fig. 3 shows an embodiment of a device in which the sample can be adjusted along the X-ray beam in different predetermined receiving positions.
    Fig. 2 shows a schematic view of a device according to the invention for investigating the radiographic properties of a sample 3c, which is arranged on a sample holder 3a. The X-ray radiation emanating from an X-ray source 1 is focused in an X-ray mirror 2 a onto the plane of a detector 5. The beam width is set with a collimation block 2b. Of course, it is also possible that a parallel x-ray beam or other beam geometries are used. It is also the formation of a dot or stroke focus possible. The mirror 2a and the collimation block 2b are adjustable with respect to the X-ray source 1 and the detector 5, whereby the guidance of the X-ray beam 10 is independent of the sample position. The position of the sample 3c can now be changed along the X-ray beam 10 with respect to the detector 5. For this purpose, a displacement or adjustment of the sample carrier 7a takes place relative to the X-ray beam 10 along the optical axis of the device. The sample 3c is for this purpose mounted on a sample holder 3a, which is in particular releasably connected to a spindle nut 7a, which can be moved along the X-ray beam 10 by means of a stepping motor 8 which drives a screw spindle 7. The sample 3 c is thus continuously adjustable along the optical axis or the X-ray beam 10. A position measurement can take place, for example, via a defined starting position and counting of the turning steps of the spindle in or counterclockwise and multiplication by the step angle. For determining the position measuring devices can also be provided which determine the distance between the detector 5 and the sample 3c, for example potentiometers, incremental displacement transducers, inductive displacement transducers, dial gauges, etc. Similarly, the distance between the spindle nut 7 and a predetermined reference position can be measured , In particular, the determination of the distance between the sample 3c and the detector 5 refers to the detector plane.
    It is also possible to provide other Verstetleinrichtungen or feed devices instead of a spindle. For example, mechanical linear feed devices may be provided parallel to the optical axis, wherein the sample is adjusted by means of linear motors or rack and pinion gear.
    As soon as the stepping motor 8 rotates the spindle 7, the spindle nut 7a is displaced along the X-ray beam 10 and the sample 3c is moved along the optical axis of the device in the direction of the detector 5 or away from it. The distance S1 between the sample 3c and the detector 5 shown in FIG. 2 corresponds to a relatively large distance and the position P corresponds in practice to the distance to the image of the small-angle scattering region. The distance S2, in which the sample 3c is arranged in the position P ', corresponds to the large-angle scattering region, wherein for reasons of intensity, the center-beam and / or the small-angle scattering region can be masked out by means of a shield 4.
    It is also possible to take pictures during the movement of the sample 3c, whereby a continuous change of the recorded scattering angle pattern can be recorded by the detector 5 on the basis of the different changing distances of the sample 3c. The movement of the sample 3c is controlled by means of a control unit 6, which can also carry out the evaluation of the detector signals. In this case, a recording of the values of the distances as well as the scattering measured values determined by the detector 5 takes place.
    Advantageously, before the measurement, the determination of the distances for the measurements to be made of the two scattering angle ranges. It is quite possible to define only subareas of the two scattering angle ranges and not to imaged on the detector 5 too small and too large boundary regions of the scattering or of the respective region.
    An alternative procedure is shown in FIG. Here, defined measurement positions or positions P, P 'are predetermined by test recordings 9a, 9b into which the sample carriers 3b of the sample 3c can be inserted into .fwdarw.I * .k. The measurement positions P, P 'are at a distance S1 or S2 from the detector 5 and from the detector plane, respectively, so that an exactly reproducible adjustment of the samples 3c with respect to the detector 5 is possible. Precisely machined guides for the sample carriers 3b, which ensure exact positioning of the sample 3c with respect to the detector 5, can be provided on the receptacles 9a, 9b.
    It is also possible to make the displacement of the sample carrier 3b by means of an automatically functioning device, for example a robot, and to provide detection systems which detect the storage of a sample 3c in the position P or in the position P '.
    It can also be provided that adapters 9a, 9b can be attached to the sample holders, which holders can accommodate different sample carriers 3b. It is also possible to form the sample carriers 3b in the form of flow cells or controlled atmosphere cells. The selection of sample carriers is in principle arbitrary.
    It is possible to make arbitrary embodiments of the measuring device according to the invention, as they are known in the prior art in diversity, a limitation is the possibility to spend the sample in different distances to the detector 5, not. Rather, it is possible that a change between the measuring positions P, P 'can be made automatically by the control unit 6. A sample adjustment is therefore possible without interrupting a vacuum.
    With the intended detector 5, different angular ranges can thus be measured in immediately successive measurements and a recalibration of the detector is eliminated since only the distance between the sample 3c and the detector 5 is adjusted.
    The advantages achieved in the device according to the invention are independent of whether a focused X-ray beam 10 or a parallel X-ray beam 10 is used.
    权利要求:
    Claims (10)
    [1]
    1. Method for investigating the radiographic properties of samples (3c), wherein the x-rays scattered on a sample (3c) are recorded by a detector (5) located at a distance from the sample (3c) and evaluated with respect to the sample properties, characterized in that, for a predetermined and preferably during the measurements made, the distance between the X-ray source (1) or the starting point (2b) of the X-ray (10) directed towards the sample (3c) and the detector (5) is maintained for a predetermined number of consecutive times following measurements, the distance (S1, S2) between the sample (3c) and the detector (5) is changed and set to predetermined different values.
    [2]
    2. The method according to claim 1, characterized in that the distance (S1, S2) is set to values for which the small-angle scattering range and / or the large or wide-angle scattering range are imaged on the detector (5).
    [3]
    3. The method according to claim 1 or 2, characterized in that for changing the distance, a continuous displacement of the sample (3c) in or against the direction of the X-ray beam (10) in the predetermined measuring position (P, P ') is made.
    [4]
    4. The method according to any one of claims 1 to 3, characterized in that the sample (3c) is displaced by the sample in at least two along the X-ray beam (10) at different distances (S1, S2) from the detector (5) lying test recordings (9b) is used.
    [5]
    5. The method according to any one of claims 1 to 4, characterized in that the radiation and measurement geometry is kept unchanged during a displacement of the sample (3c) and / or during the displacement of the sample (3c) these in their position on the or with respect to the axis of the X-ray beam (10).
    [6]
    6. The method according to any one of claims 1 to 5, characterized in that the detector (5) at a detector-near test position (P ') of the sample (3c) scattered in the large-angle scattering X-rays and at a remote detection position (P) of the sample (3c) depicting X - rays scattered in a small angle spread,. ·. ** 11
    [7]
    7. The method according to any one of claims 1 to 6, characterized in that the scattered X-rays are received by a plate-shaped CCD sensor (5) or a curved imaging plate or a diode detector.
    [8]
    8. An apparatus for examining the radiographic properties of samples (3c) with an X-ray source (1), which apparatus comprises a sample carrier (3b) for holding the sample (3c) and a detector (5) which is at a fixed distance from the X-ray source (10) or from the starting point (2) of the directed to the sample (3c) X-ray beam (10), wherein the of the sample (3c) scattered X-rays of the distance (S1, S2) to the sample (3c) located Detector (5) are recorded and the signals obtained are evaluated with respect to sample properties, characterized in that - an adjusting unit (8) is provided, with which the sample (3c) parallel to the axis of the X-ray beam (10) in a near-inspection test position (P '. ), in which on the detector (5) of the small-angle scattering range is shown, and in a remote detector test position (P) is movable, in which the detector (5) of the Groliwinkelstreubereich and gefäfa If the small-angle scattering region is also imaged, or - that receptacles (9a, 9b) for the sample (3c) are located along at least two spaced-apart locations (P, P ') along the axis of the x-ray beam (10) (3c) in the detector-like image (9b) is imaged onto the detector (5) of the small-angle scattering region and, when the sample (3c) is arranged in the detector (9a) remote from the detector, the grille angle scattering region and optionally also the small-angle scattering region is imaged onto the detector (5) ,
    [9]
    9. Apparatus according to claim 8, characterized in that the adjusting unit (8) on a spindle (7) adjustably mounted sample carrier (7a), wherein the spindle (7) of a control or stepping motor (8) rotatable and thus the Sample carrier (7a) along the axis of the X-ray beam (10) is adjustable.
    [10]
    10. Apparatus according to claim 8 or 9, characterized in that the detector (5) is a CCD, IP or diode array sensor. Vienna, March 17, 2011
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    同族专利:
    公开号 | 公开日
    WO2012122577A1|2012-09-20|
    AT511103B1|2012-09-15|
    US20140098940A1|2014-04-10|
    DE112012001274A5|2013-12-19|
    US9329143B2|2016-05-03|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    EP1477796A2|2003-05-05|2004-11-17|Bruker AXS, Inc.|Small angle x-ray scattering system with vertical beam for simplified analysis of liquid samples|
    SU1562808A1|1987-07-17|1990-05-07|Всесоюзный Научно-Исследовательский Институт Молекулярной Биологии|Small-angle x-ray diffractometer|
    AT392160B|1989-09-14|1991-02-11|Otto Dipl Ing Dr Kratky|Diaphragm arrangement for the low-scatter, single-sided, linear limitation of an X-ray beam|
    JP2003215068A|2002-01-29|2003-07-30|Sumitomo Chem Co Ltd|X-ray measurement method|
    DE102006029449B3|2006-06-21|2007-09-06|Hahn-Meitner-Institut Berlin Gmbh|Small angle scattering measuring device for analysis of nanostructure of sample, has channel formed by sections that are lowered in gap of optical bank inside of frame, where frame has guide for balancing trigonometric length variation|
    JP5116014B2|2007-06-21|2013-01-09|株式会社リガク|Small-angle wide-angle X-ray measurement system|
    JP5237186B2|2009-04-30|2013-07-17|株式会社リガク|X-ray scattering measuring apparatus and X-ray scattering measuring method|AT513660B1|2012-11-30|2014-09-15|Anton Paar Gmbh|Method and device for examining samples|
    US10359376B2|2016-07-20|2019-07-23|Malvern Panalytical B.V.|Sample holder for X-ray analysis|
    EP3605074A4|2017-03-30|2021-03-10|Rigaku Corporation|X-ray analysis assistance device and x-ray analysis device|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    ATA377/2011A|AT511103B1|2011-03-17|2011-03-17|METHOD AND DEVICE FOR STUDYING THE X-RAY PROPERTIES OF SAMPLES|ATA377/2011A| AT511103B1|2011-03-17|2011-03-17|METHOD AND DEVICE FOR STUDYING THE X-RAY PROPERTIES OF SAMPLES|
    US14/004,999| US9329143B2|2011-03-17|2012-03-12|Method and apparatus for investigating the X-ray radiographic properties of samples|
    DE112012001274T| DE112012001274A5|2011-03-17|2012-03-12|Method and device for investigating the radiographic properties of samples|
    PCT/AT2012/000059| WO2012122577A1|2011-03-17|2012-03-12|Method and apparatus for investigating the x-ray radiographic properties of samples|
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