EP2175456A2 - Instrument d'analyse de rayons X doté d'une fenêtre d'ouverture mobile - Google Patents

Instrument d'analyse de rayons X doté d'une fenêtre d'ouverture mobile Download PDF

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Publication number
EP2175456A2
EP2175456A2 EP09000179A EP09000179A EP2175456A2 EP 2175456 A2 EP2175456 A2 EP 2175456A2 EP 09000179 A EP09000179 A EP 09000179A EP 09000179 A EP09000179 A EP 09000179A EP 2175456 A2 EP2175456 A2 EP 2175456A2
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EP
European Patent Office
Prior art keywords
ray
aperture
ray beam
window
aperture window
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
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EP09000179A
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German (de)
English (en)
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EP2175456A3 (fr
Inventor
Carsten Michaelsen
Stefanie Belgard
Jürgen Graf
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InCoaTec GmbH
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InCoaTec GmbH
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Priority to US12/461,830 priority Critical patent/US7983388B2/en
Publication of EP2175456A2 publication Critical patent/EP2175456A2/fr
Publication of EP2175456A3 publication Critical patent/EP2175456A3/fr
Withdrawn legal-status Critical Current

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    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21K—HANDLING OF 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
    • G21K1/02—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating using diaphragms, collimators
    • G21K1/04—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating using diaphragms, collimators using variable diaphragms, shutters, choppers

Definitions

  • X-ray diffraction is an efficient method for non-destructive chemical analysis of especially crystalline samples.
  • the X-ray generated by an X-ray source is directed onto a specimen via a multilayer optic, and the diffracted X-ray is analyzed by a detector.
  • multi-layer X-ray optics With multi-layer X-ray optics, monochromatization and, above all, beamforming of the X-ray beam in an X-ray analysis apparatus are performed with good efficiency.
  • the structure of the multilayer X-ray optics also determines the beam properties on the output side of the multilayer optics. Physical quantities such as the input and output convergence, the focal lengths between source and image focus, and the magnification ratio and thus also the size of the X-ray beam in the image focus must be established prior to the production of the multilayer optics.
  • multilayer X-ray optics are basically inflexible.
  • a particularly important property in X-ray diffractometry is the convergence angle ⁇ , since the resolution of a diffractometer decreases with increasing convergence angle. To adapt to changing measurement requirements convergence diaphragms have become known.
  • the DE 10 2004 052 350 A1 describes several holes of the same diameter on a rotatably mounted disc of an X-ray analyzer, with which a diaphragm function is achieved.
  • a shutter By slightly turning the disc, a shutter can be moved continuously in a first direction, and by changing to another hole on a different radius of the disc, a diaphragm can be moved in discrete steps in a second direction.
  • an X-ray analysis instrument of the aforementioned type which is characterized that the diaphragm mechanism means for stepless method of Aperture window in at least one direction transverse to the X-ray beam comprises that the aperture opening is at least as large as the cross section of the X-ray beam at the location of the aperture window, and that the path of the aperture window accessible through the aperture mechanism in the at least one direction is at least twice as large as the extent of the x-ray beam at the location of the aperture window in this direction.
  • the aperture opening With the diaphragm mechanism according to the invention, it is possible with the aperture opening with respect to the area ratio to select any portion of the X-ray beam cross section at the location of the aperture window and to supply it to a subsequent X-ray experiment.
  • the aperture opening is correspondingly proportionally overlapped with the X-ray beam cross section. If the full beam cross section is desired, the aperture opening is brought into complete overlap with the X-ray beam cross section; since the aperture opening is at least as large as the X-ray beam cross-section, the X-ray beam is in no way shaded.
  • a partial region of the X-ray cross section can be selected from two opposite sides.
  • the X-ray beam has different properties in different regions of its cross-section, so that the properties of the transmitted X-ray component can also be selected in a simple manner by means of the diaphragm mechanism according to the invention.
  • VW> AOE + RS, with VW: travel path of the aperture window; AOE: extension of the aperture opening; RS: extension of the X-ray.
  • the at least one direction, in which the aperture window can be moved steplessly and over at least twice the beam extent extends from the source-near to the source-distant portion of the X-ray beam cross section.
  • particularly relevant properties of the transmitted X-ray beam can be influenced.
  • the diaphragm mechanism comprises means for continuously moving the aperture window in two independent directions transverse to the X-ray beam, and that the respective path of the aperture window accessible by the shutter mechanism in each of the independent directions is at least twice as large as the extent of the x-ray beam at the location of the aperture window in the respective independent direction.
  • the diaphragm mechanism in the design with two independent traversing directions allows an even larger, almost arbitrary selection of a contiguous subsection of the cross section of an X-ray beam.
  • the aperture opening which is at least as large as the extent of the x-ray beam, is brought into overlap with the x-ray beam only to the extent that the cross-section of the x-ray beam is to enter the subsequent x-ray experiment (typically the irradiation of a sample).
  • the aperture window In most positions of the aperture window, therefore, only part of the aperture opening is irradiated by X-ray radiation, and the remaining part of the aperture opening is illumi- nated.
  • the aperture window Around the aperture opening, the aperture window has a sufficiently wide shading frame from which the portion of the x-ray radiation that does not pass through the aperture opening is completely shadowed.
  • the entire X-ray beam can pass through the aperture window, since the aperture (if appropriate after setting the window size, if this is adjustable) is greater than or at least equal to the extent of the X-ray beam at the location of the aperture window.
  • the trajectory of the aperture window in the embodiment with two independent traversing directions is sufficiently large so that each point on the edge of the aperture stop can be overlapped with any point on the edge of the X-ray beam cross section (at the aperture window location).
  • a partial region of the beam cross section of the X-ray beam can be selected from any direction.
  • AOE extension of the aperture opening.
  • the area of the selected (transmitted) portion of the X-ray beam cross section is also infinitely variable.
  • this subarea can be selected arbitrarily between 0% and 100% of the X-ray beam cross-section with an area fraction. Note that for this stepless selection of the subregion, a fixed, unchangeable aperture size can be maintained.
  • the selection of a specific subarea of an X-ray beam is carried out in particular to improve the data quality in an X-ray diffractometric measurement, in particular a signal-to-noise ratio.
  • the selection of an optimal subarea can in particular by means of ray tracing methods taking into account the properties of the (multilayer) X-ray optics in a simulation, in particular wherein the distribution of the X-ray flux density over the cross section of the X-ray beam is calculated, and the effects of selecting different subregions of the cross section for the intensity distribution in a detection level is determined.
  • the at least one direction or the two independent directions are preferably at least approximately perpendicular to the propagation direction of the X-ray beam; Preferably, the two independent directions are still at least approximately perpendicular to each other.
  • the "location of the aperture window" refers to the position with respect to the propagation direction of the X-ray beam.
  • the size of the aperture opening is not adjustable.
  • An aperture window with fixed aperture opening has a particularly simple and therefore cost-effective design.
  • the size of the aperture opening is adjustable, wherein the aperture opening is adjustable to a size which is at least as large as the cross section of the X-ray beam at the location of the aperture window.
  • Other selectable sizes of the aperture window are then typically smaller than the cross-section of the x-ray beam.
  • there is an even greater freedom in the selection of the portion of the cross section of the X-ray beam In particular, subregions in the interior of the cross section (ie subregions without edge portion) can be selected.
  • the diaphragm mechanism is arranged on the output side of the X-ray optics.
  • the aperture window has a square aperture opening
  • that the X-ray beam at the location of the aperture stop has an approximately square cross section, wherein the side edges of the square aperture opening and the square cross section of the X-ray beam are oriented parallel to each other, and that at least one direction in which the aperture window is movable, along a diagonal of the square aperture opening is oriented.
  • the beam quality often varies particularly greatly toward the corner regions of a square X-ray beam cross section, and the above device of the travel paths makes these corner regions particularly easily accessible.
  • the at least one direction runs along the diagonal of the X-ray cross section, along which the source-near to the source-distant portion of the X-ray beam is passed. With two independent traversing directions, these typically run on the two diagonals of the square X-ray cross section.
  • an embodiment which is characterized in that the X-ray optics are arranged in a gas-tight optical housing and the diaphragm mechanism in a gas-tight diaphragm housing, wherein the two housings are evacuated or are flooded with a protective gas, or that the X-ray optics and the diaphragm mechanism are arranged in a common, gas-tight housing, wherein the common housing is evacuated or flooded with a protective gas.
  • the protective gas can reduce corrosion and soiling on the surfaces of the X-ray optics and the diaphragm mechanism as well as the air absorption.
  • the means for continuous movement of the aperture window comprise at least one micrometer screw and / or at least one fine-threaded bolt. These agents have proven themselves in practice.
  • the micrometer screw is particularly suitable for a direction to be adjusted frequently.
  • the diaphragm mechanism has a holder for a replaceable aperture window element, and that the holder can be moved by the means for stepless movement of the aperture window.
  • An X-ray analysis instrument can be used, in particular in X-ray diffractometry, to select a portion of the X-ray beam to direct reflection separation by means of the aperture opening of the aperture window and to direct it to a sample.
  • the selection of the proportion (or partial area) is targeted and at the same time particularly simple and flexible.
  • the scope of the present invention also includes the use of a diaphragm mechanism comprising an aperture window with an aperture opening for selecting a portion of an X-ray beam, wherein the X-ray beam is emitted by an X-ray source and imaged onto a sample by X-ray optics, in particular a multi-layer X-ray mirror in particular wherein this use takes place with an X-ray analysis instrument according to the invention, characterized in that for adjusting, in particular reducing, the focus size of the X-ray beam at the location of the sample by means of the aperture opening of the aperture window, a proportion of the X-ray beam remote from the X-ray optics is selected.
  • a source-remote portion of an X-ray beam can give better data quality, in particular a better signal-to-background ratio in X-ray experiments, especially in X-ray diffraction experiments on smaller samples compared to the total X-ray beam at the sample location.
  • scattering in air, sample holder or other parts of the X-ray analysis instrument can be reduced by an optimized focus size.
  • the selected, distant portion of the X-ray beam extends with its cross-sectional area at the location of the aperture window in the case of a single reflection on the X-ray optics (such as a Göbelspiegel) according to the invention to a maximum of the center line of the cross section of the entire X-ray beam, said center line, the X-ray beam at the location of the aperture window divided into a (with respect to the reflection at the X-ray optics) near the source and a source distant half, each with the same area proportions.
  • a double reflection on the X-ray optics (such as a Monteloptik) according to the invention extends the selected, distant source portion of the X-ray to a maximum of the two centerlines of the cross section of the entire X-ray beam, said center lines of the X-ray at the location of the aperture window in each case (with respect the respective reflection on the X-ray optics) divide source-near and source-distant half, each with the same area proportion; with others Words, the selected, distant from the source portion of the X-ray is then in that area (typically "quarter") of the X-ray cross section, with respect to which both reflections are attributable to the X-ray optics of the source distant side.
  • the off-center portion of the X-ray comprises, in the case of a single reflection, 50% or less, and preferably 40% or less, of the cross-sectional area of the entire X-ray.
  • the off-center portion of the X-ray beam typically comprises 25% or less, and preferably 20% or less, of the cross-sectional area of the entire X-ray beam.
  • the focus size of the X-ray beam at the location of the sample is set to the size of the sample.
  • the signal-to-background ratio can be optimized.
  • the adjustment of the focus size is effected in particular by the relative positioning of the aperture opening to the X-ray beam with respect to source proximity and source distance (ie transversely to the propagation direction of the X-ray beam), whereby the focus size at the sample location can be adjusted even if the size of the aperture opening or the same area of the selected beam cross section is invariable ,
  • the selected portion of the X-ray beam distant from the source has a below-average mean photon flux density compared to the rest of the X-ray beam.
  • an improvement of the reflection separation or the signal-to-background ratio is possible, compared with, for example, the use of a source-proximate portion with regularly larger average Flux density than the rest (or in the whole) X-ray.
  • the average flux density in a selected portion of the x-ray beam is determined over the total (integrated) photon flux in the selected portion divided by the cross-sectional area of the selected portion; the same applies to the rest of the x-ray beam.
  • a variant of use is also preferred in which the aperture window is positioned so that no X-ray radiation passes through part of the aperture opening of the aperture window. In other words, only part of the aperture opening is held in the X-ray beam (or overlapped with the X-ray beam). As a result, a portion of an X-ray beam cross-section, which is smaller than the aperture opening, can be selected for transmission with little effort even with a large aperture opening.
  • the aperture window is arranged in the X-ray beam between the X-ray optics and the sample.
  • the invention relates to an X-ray analysis instrument, in particular an X-ray diffractometer, having an X-ray source, an X-ray optics, in particular a multi-layer X-ray mirror, and a variable diaphragm mechanism.
  • Multilayer X-ray optics and their applications in X-ray diffractometry are known, for example, from US Pat DE 198 33 524 A1 for so-called Göbelspiegel, and from the US 6,041,099 known for Montelapt (also called Monteloptiken).
  • engineered multi-layer systems are used to generate X-rays Monochromatize, parallelize or focus applications in X-ray analysis.
  • the mirror is parabolic, elliptical in shape to provide a focused beam.
  • the multilayers must vary along the mirror in their "d-spacing" to satisfy the Bragg relationship for a single wavelength (eg, Cu-K alpha radiation) at each position of the mirror.
  • the mathematical course of this layer thickness variation is known from earlier work (Laterally d-spacing graded multilayers, see eg M. Schuster et al., Proc. SPIE 3767, 1999, pp. 183-198 ).
  • Fig. 1 shows by way of example the essential geometric parameters of a focusing (elliptical) GöbelLites.
  • Fig.1 shows a GöbelLite with the length L, the distance f1 to the source SC, and the distance f2 to the image focus IM and with the semi-axes a and b.
  • ⁇ is the light collection angle and ⁇ is the convergence (or divergence) of the useful beam.
  • the field of application of the mirrors described in this invention is X-ray diffractometry, with typical photon energies> 5000 eV. Under these conditions, the Bragg angles ⁇ for typical Göbelspiegel in the range of less degrees, so that b «a applies. Therefore, f1 'is approximately equal to f1, and f2' is approximately equal to f2.
  • the ratio f2 / f1 is called the magnification ratio of the optics.
  • Monteloptiken consist essentially of two Göbelaptn, which are mounted vertically to each other. While Göbel mirrors only parallelize or focus the X-ray in one dimension, Montel mirrors effect parallelization or focusing in two dimensions.
  • a disadvantage of these X-ray mirrors is that the beam properties on the output side of the mirrors are determined by the design of the optics.
  • physical variables such as the Ninververgenz, the focal lengths between the source and image focus, the magnification and thus the size of the X-ray image focus before manufacturing.
  • the quantities f1, f2, a, b, ⁇ , L must be determined before production and can not be subsequently varied.
  • a change to the requirements makes the costly and costly production of a new mirror type necessary. This makes the use inflexible for different sample requirements. Other sample requirements must be performed under suboptimal conditions, or require the change of optics, which is expensive and requires significant modification and costly adjustment of the system.
  • a subsequent bending of the mirror to another form is out of the question, since in this case, the coating would have to be changed to fulfill the Bragg condition, which is subsequently no longer possible in the rule.
  • An essential ray property is the convergence ⁇ , since the resolution of the diffractometer decreases with increasing ⁇ : The separation of closely adjacent diffraction reflections of the sample requires a not too large ⁇ . If the sample requires a higher resolution, the mirror must be changed.
  • DE 10 2004 052 350 A1 essentially describes a Nipkow disk or alternatively movable belts. Manufacturing these components with the required quality is difficult and their physical dimensions are quite large. An integration in the protection of optics usually evacuated or flushable with inert gas shielded beam path does not seem possible.
  • the aperture In US 7,245,699 B2 the aperture always consists of a fixed and a movable part. The moving part blocks in the design of the US 7,245,699 B2 always only the source distant part of the reflected by the optics Radiation; this proportion is loud US 7,245,699 B2 less efficient than the near-source fraction.
  • the aim of the present invention is to broaden the uses of X-ray optics by using an improved, very compact shutter mechanism and thus to improve the data quality of X-ray diffractometers in general.
  • the present invention proposes an X-ray analysis instrument, in particular an X-ray diffractometer, having an X-ray optics and a diaphragm mechanism consisting of one or more apertures which can be moved continuously in at least one direction, and preferably in two independent directions, perpendicular to the optical axis , And whose travel paths are at least twice as large as the X-ray beam emerging from the X-ray optics, so that any conceivable proportion of the X-ray beam emerging from the X-ray optics can be selected to illuminate the sample.
  • at least one fully open position should be achievable with the aperture mechanism.
  • the diaphragm mechanism is preferably mounted on the output side of the X-ray optics.
  • the construction according to the invention is easy to operate over the prior art, of compact design and therefore cost can be produced, but allows a significant flexibility in the applications of X-ray optics and extremely simple and reproducible handling. It can even in existing, evacuatable optics housing, eg accordingly DE 10 2006 015933 B3 to be fully integrated. This will be explained in more detail below.
  • a ray tracing program has been developed, which has been optimized for X-ray optics. Comparisons with experiments showed that this ray tracing program makes excellent, accurate predictions.
  • Fig. 2 shows the ray tracing specific intensity profile of a 150 mm long multi-layer MontelLites. High intensity areas are dark, and areas of low intensity are bright. Out Fig. 2 It can be seen that the square beam profile is not homogeneously filled with intensity, but in the upper left corner is particularly dark (and thus rich in intensity).
  • the intense beam area in the upper left corner of Fig. 2 was reflected twice each from a near-source portion of the Monteladors, and the lower-intensity beam area bottom right was reflected twice each of a source distant portion of the Monteladors.
  • the cross section of the X-ray beam can be divided by the two dashed lines center lines M1 and M2 in each case in terms of area in a near-source and a source distant half with respect to each of the two reflections. From the quadrant on the top left, a source (with respect to both reflections) near the source of the X-ray beam can be selected, and from the quadrant at the bottom right one can select a source (with respect to both reflections).
  • the travel path of the diaphragm must be at least twice as large as the X-ray beam emerging from the X-ray optics.
  • the ray tracing calculations used a square aperture (aperture window 2) as in the FIGS. 3 to 5 sketched stepwise in either direction A or direction B, and then the beam properties were determined; the particular beam characteristics are in the FIGS. 6 to 8 shown.
  • the directions A and B are equal to each other, and thus in the context of the invention, the direction pair A / B together only one traversing direction (traversing) of the aperture window 2 across the X-ray beam corresponds.
  • Travel A corresponds in its effect according to the prior art US 7,245,699 B2 ; Travel path B is in the training after the US 7,245,699 B2 not possible or not provided, since here the supposedly less efficient beam component is.
  • the iris is fully opened along the x-axis.
  • Example optics is the beam size in focus with fully open aperture about 0.2 mm.
  • the beam becomes larger in the direction A in the method, and smaller in the method in the direction B. It is thus possible to vary the beam size and to adjust the sample size by choosing the direction of travel. This is very interesting for applications in single-crystal diffractometry for the structure determination of proteins and small organic molecules, where the samples often have a size in the range 0.1-0.3 mm.
  • the direction of travel of the diaphragm one can set the best beam size, in which only the sample is illuminated.
  • the sample is smaller than 0.2 mm, then rays which do not hit the sample and which only lead to air scattering and thus generate a raised background in the diffraction measurement can be avoided. If the sample is greater than 0.2 mm, the beam can be increased by travel direction A, so that the sample is homogeneously illuminated, which is also advantageous for the measurement.
  • Fig. 7 shows that the direction of travel A is advantageous if the divergence is to be reduced, while the flow (photons / sec) should remain as high as possible.
  • Fig. 8 shows that the direction of travel B is advantageous if the flux density (photons / sec / mm 2 ) should remain as high as possible.
  • the FIGS. 6 to 8 can be used simultaneously as calibration curves when moving the aperture. All three curves intentionally contain the flow as the x or y axis, but not the travel of the orifice.
  • the exact position of the X-ray in space may not be known exactly, and may change as a result of readjusting the optics or other circumstances.
  • the flow on the output side of the diaphragm can be measured very easily, eg with a photodiode. So if you move the aperture, for example, in direction A, until the river is halved, so you can with the FIGS. 6 to 8 Immediately read the resulting beam size, divergence, and flux density. Conversely, to set a particular divergence, one can see how far one has to reduce the flow.
  • traversing directions A and B shown diagonally through the square beam In addition to the traversing directions A and B shown diagonally through the square beam, of course, other beam cross sections, traversing directions (or travel direction pairs) and positionings of the diaphragm are possible.
  • a diaphragm mechanism BM constructed on the basis of the calculations (see Figures 9 and 10 ) for an inventive X-ray analysis instrument is arranged in a diaphragm housing 1 with optional loading window 7 and optional vacuum connection 4, wherein the diaphragm mechanism BM is equipped with a diaphragm (ie an aperture window 2 with aperture 3) and an adjustment mechanism with two actuators (here Micrometer screw 5 and fine thread bolt 6).
  • the optics is rotated by 45 degrees, so that the square beam profile and thus also the square aperture 3 are on the top. Under these conditions, the diagonal movements of the FIGS. 3 to 5 to horizontal or vertical movements.
  • FIG. 11 shows the central adjustment mechanism with diaphragm holder (holder) 11, not yet mounted in the housing.
  • the aperture can be moved by two adjustments perpendicular to the beam direction in the X direction and in the Y direction. It is in the embodiment shown in the X direction via a micrometer screw 5 and in the Y direction by a fine thread bolt 6 adjustable, see.
  • Fig. 12 The aperture is mounted in a mounted on two axles 12 holder 11, which with two springs 13 against the micrometer screw 5 is pressed. Thus, an automatic reset of the aperture (or the aperture window 2) is ensured in this direction.
  • the suspension of the adjustment mechanism, cf. Fig. 11 Via two guide pins 14 and rotatably mounted in the aperture housing fine thread bolt 6; Thus, an entire frame 15 of the adjusting mechanism can be moved, cf. Fig. 12 ,
  • the movement of the aperture in the X and Y direction could also be done by means of other adjustment mechanisms, such as two micrometer screws, two simple screws, slots with screws, etc.
  • a version with only a micrometer and a fine-threaded bolt is advantageous if the aperture only should be aligned once in height on a standing on the point square beam, while the adjustment to hide unwanted beam portions should be mostly horizontal.
  • FIGS. 13 and 14 In this case, an aperture window element 16, in which the aperture opening is formed, is held exchangeably in a holder 11. In FIG. 14 a removed aperture window element 16 is shown in front of the associated holder 11.
  • apertures with holes can be used.
  • a preferred design uses a standing on the top square.
  • Another type is in the FIGS. 15a and 15b shown rectangle panel, in which the aspect ratios and the size can be adjusted, in particular with two L-shaped Apert concentrate scholaren 18 a, 18 b.
  • a variable iris diaphragm can also be realized in this way.
  • the diaphragm housing 1 can, for example, in front of or behind an optical housing 17, for example DE 10 2006 015933 B3 be mounted, cf. Fig. 16 which can be evacuated via the vacuum connection 4 located in the cover housing 1.
  • the diaphragm can be operated in vacuum or purged with inert gas, which prevents intensity losses of the beam and protects the optics from corrosion.
  • the device is very compact.
  • the beam then leaves the housing 1 through a beryllium window 7 located in the diaphragm housing 1.
  • the operating direction of the micrometer screw 5 can be changed by installing the adjusting mechanism in a different orientation and mounting the micrometer screw 5 on the opposite side. This facilitates the practical use in left- and right-sided system solutions.
  • the hole not used by the micrometer screw is provided with a blanking plug 8.
  • a crystal of a defined size and with known lattice constants was mounted at a fixed distance from the source and the detector on an X-ray diffractometer (Smart Apex-11, Bruker AXS).
  • the crystal had a long cell axis, which showed a tendency to reflections at the selected detector spacing.
  • the crystal was oriented so that the closely adjacent reflections of the long cell axis were clearly visible on the detector.
  • FIGS. 17a and 17b show two diffraction patterns on a small thaumatin crystal, once with an approximately 0.25 mm large beam ( Fig. 17a ), and once with a beam of about 0.12 mm ( Fig. 17b ).
  • the photon flux in the case of the smaller beam was only a fraction of the total flux, the result was a much better diffraction pattern, ie much better data. This is essentially because the smaller beam essentially hits only the sample, while the larger beam additionally hits a portion of the sample holder and the surrounding air and excites scattering. This scattering leads to a raised background, which covers the diffraction reflexes.
  • the Fig. 18a schematically shows an inventive Röntgenanalysisinstrument, here a Röntgendiffratometer 21.
  • an X-ray beam 23 is emitted, which is from an X-ray optics 24, here a Göbel mirror, reflected and thereby focused.
  • an aperture window 2 is arranged with an aperture 3 in the X-ray beam 23.
  • the aperture window 2 is part of a diaphragm mechanism, and can be moved continuously in two independent directions x and y perpendicular to the propagation direction of the x-ray beam 23.
  • the y-direction is perpendicular to the plane of the drawing, and in the region of the aperture window 2, the z-direction is parallel to the propagation direction of the x-ray radiation.
  • stepless movement of the aperture window 2 means not shown in detail, such as a micrometer screw and a fine-threaded bolt, are formed in the aperture mechanism.
  • RS x At the location (with respect to the z-direction) of the aperture 2 in the x direction has the X-ray beam 23 an extension RS x and the aperture 2 has an extension AOE x in the x-direction.
  • RS x ⁇ AOE x (in the exemplary embodiment shown, RS x is slightly smaller than AOE x ); The same applies to the corresponding quantities in the y-direction.
  • the aperture window 2 is used to a first portion of the X-ray beam 23, namely a in Fig. 18 upper portion of the X-ray beam 23, through the aperture 3 to pass (see transmitted X-ray partial beam or portion 26), and a second (in Fig. 18a lower) portion of the X-ray beam 23.
  • the transmitted partial beam 26 was at the x-ray optics 24 at a farther from the x-ray source 22, in the FIG. 18a
  • the right-most region of the X-ray optics 24 is reflected, and is therefore referred to as a source distant portion of the X-ray beam 23.
  • Radiation diffracted by the sample 27 can be registered by means of a detector 28; the detector 28 is here movable on a circular arc around the sample 27.
  • FIG. 18b For example, the relationships in the cross-section 32 of the X-ray beam at the location (ie, the z-position) of the aperture window of FIG Fig. 18a illustrated in more detail.
  • the substantially circular cross-section 32 is divided by the center line M into two parts (or halves) QNH, QFH with the same surface area.
  • the in Fig. 18b The right-hand part QNH ("near-source half") was reflected closer to the source of the X-ray optics than the one in Fig. 18b left part QFH ("source far half").
  • a partial beam 26 is selected by overlapping with the cross section 32 of the X-ray beam. In order to select a source distant partial beam (portion) 26, while the aperture opening 3 is advanced to at most the center line M; in Fig. 18b the aperture 3 is not fully advanced to the center line M.
  • a source-remote portion of an X-ray beam is selected, as a result of which improved reflection separations and improved signal-to-background ratios can be achieved.
  • any other beam components of the X-ray beam for example a portion close to the source, can also be selected, depending on the requirements of the particular X-ray experiment.
  • a source-distant beam component of the X-ray beam can also be selected with a conventional diaphragm, in particular a diaphragm with a smaller size than the beam cross-section or a mobility of less than twice the beam extension.
  • FIGS. 19a to 19c illustrate the movability of an aperture window 2 according to the invention in a plane perpendicular to the propagation direction (in this case z-direction) of an x-ray beam, typically on the output side (behind) of a multi-layer x-ray optics.
  • the aperture window 2 can be moved in two independent (and here also orthogonal) directions x and y via a travel path corresponding to twice the extent of the x-ray beam cross section in the respective direction; According to the invention, however, only one traversing direction (for example only the traversability in the x-direction shown) can be provided, or the traversing possibility in a second direction (approximately the y-direction) can be less than twice the extent of the x-ray beam in the second direction over a travel distance be reduced and serve only a fine adjustment of the aperture window.
  • the aperture window 2 comprises a shading frame 31 and a (here) rectangular aperture 3.
  • the aperture 3 has in the x-direction the extent AOE x , and in the y-direction the extent AOEy.
  • the X-ray beam has in the embodiment shown at the location of the aperture window 2 (unshaded) an oval cross section 32 with an extension RS x in the x direction and RS y in the y direction.
  • the aperture opening 3 is at least as large as the cross section 32 of the X-ray beam, ie, the cross-section 32 of the X-ray beam is completely within the aperture opening 3 (in the fully open position).
  • Fig. 19b illustrates the mobility of the aperture window 2 in the x direction.
  • the aperture window 2 can be displaced in the positive x direction at least to the extent that the aperture 3 no longer overlaps the cross section 32 of the x-ray beam.
  • the travel path VW x of the aperture window 2 (indicated for the lower edge of the aperture 3) in the x-direction in the embodiment shown is at least twice as large as the extent x of the x-ray in the x-direction.
  • Fig. 19c illustrates the mobility of the aperture window 2 in the y-direction.
  • the aperture window 2 can in turn be displaced in the positive y-direction, at least to the extent that the aperture 3 no longer overlaps the cross-section 32 of the x-ray beam.
  • the travel path VWy of the aperture window 2 (indicated for the left edge of the aperture 3) in the y direction in the embodiment shown is at least twice as large as the extent RS y of the x-ray beam in the y direction.
  • the aperture 3 in the two independent spatial directions x and y can at least be moved out of the cross section 32 of the x-ray beam, a marginal portion of the cross section 32 can be selected for overlapping with the aperture 3 from each approaching direction and fed to a subsequent x-ray experiment , The remaining portion of the cross section 32 is then blocked by the shading frame 31.
  • the area fraction of the selected subregion can also be selected steplessly in the two directions x and y, in particular in order to optimize photon flux, photon flux density and / or beam divergence in the subsequent x-ray analysis experiment due to the infinitely variable mobility of the aperture window 2.
  • the entire X-ray beam in the fully opened traveling position of the aperture window 2 can be supplied to the following experiment.
  • the size of the aperture opening of the aperture window may also be adjustable, in particular reducible, and preferably infinitely variable, by the aperture mechanism, so that non-border portions of the cross section of the x-ray beam can also be selected (cf. Fig. 15a and Fig. 15b ).
  • the present invention allows the greatest possible freedom in the selection of a subarea of an X-ray cross-section for an X-ray analysis experiment.

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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)
EP09000179A 2008-10-08 2009-01-09 Instrument d'analyse de rayons X doté d'une fenêtre d'ouverture mobile Withdrawn EP2175456A3 (fr)

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DE102008050851A DE102008050851B4 (de) 2008-10-08 2008-10-08 Röntgenanalyseinstrument mit verfahrbarem Aperturfenster

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JP5931394B2 (ja) * 2011-10-07 2016-06-08 株式会社東芝 Ｘ線診断装置及び線量分布データ生成方法
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US7983388B2 (en) 2011-07-19
DE102008050851B4 (de) 2010-11-11
US20100086104A1 (en) 2010-04-08

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