专利摘要:
The invention relates to a method and a device for examining a sample with radiation (8) emitted by a neutron source or X-ray source (8), which is guided via at least one beam-forming unit to the sample (3) carried by a sample holder (7) According to the invention, at least one of the following components, namely radiation source (0) and / or beam-shaping unit (1, 2) and / or sample holder (7) and / or detector (5) and / or optionally a primary radiation catcher (4) arranged upstream of the detector (5), relative to at least one of the other components (0, 1, 2, 4, 5, 7) and / or with respect to a given fixed point and / or with respect to the beam path (9) with a control unit (6) via actuators (11) aligned and / or adjusted with respect to their spatial position, wherein for generating a manipulated variable delivered by the control unit (6) to the control circuits of the actuators (11) assigned to the respective components (0, 1, 2, 4, 5, 7), in particular by the detector (5) in at least one predetermined position Detector area, measured radiation intensity and / or a value derived therefrom is used.
公开号:AT513660A1
申请号:T50552/2012
申请日:2012-11-30
公开日:2014-06-15
发明作者:
申请人:Anton Paar Gmbh;
IPC主号:
专利说明:

1
The invention relates to a method according to the preamble of claim 1. Furthermore, the invention relates to a device according to the preamble of claim. 7
The elastic scattering of X-rays is used for the non-destructive structural characterization of a wide variety of sample materials. Such angle scattering measurements can be carried out both by means of X-ray radiation and in a comparable manner with neutron radiation. The invention can be realized with both types of radiation. X-ray scattering occurs when a bundle of X-rays hits an inhomogeneous, powdery, liquid and / or solid material whose structures are larger than the wavelength of X-rays used. The X-rays penetrate into the sample, the material to be examined interacts with the beam and this is scattered. This leads to characteristic interference images; the sum of the waves scattered at a certain angle is characteristic of the size and symmetry of the scattering particles.
In principle, two different scattering geometries can be used for the small-angle scattering. Either the samples are positioned at a small angle to the measuring beam, the measurement of grazing incidence is close to the critical angle of total reflection and the radiation pattern of the scattered radiation is recorded or the sample is transilluminated in transmission by the measuring beam. While the former method allows statements about the surface structure of the sample, in the transmission measurement, the nanostructure of the entire irradiated sample volume is analyzed.
Measuring devices of known and inventive type usually comprise a neutron or X-ray source with matching optics. For example, fixed X-ray tubes, rotary anodes or a synchrotron can serve as the radiation-generating sources. For beam focusing or monochromatization, for example, one-dimensional optics such as Göbel mirror or two-dimensional arrangements, for example, according to Kirkpatrick-Baez used. Both convergently focused, slightly divergent or parallelized beams may be used for the measurement. The focus of the measurement radiation may lie in the plane of the sample to be examined or in the detector plane.
In addition, the measuring beam can be further shaped or masked out by an arrangement of diaphragms and / or a collimation system in order to send a sample beam, which is as free as possible of disturbing scattered parts, for examination to the sample to be examined. After interaction with the sample, the scattering pattern is measured by means of an X-ray detector and the measured values are measured
Intensities are fed to an evaluation unit. Since only a small part of the measuring beam impinging on the sample is scattered, the unscattered portion of the measuring radiation, that is to say the primary beam, is masked out by the detector by means of a primary beam catcher so as not to damage the detector.
With different mathematical corrections to be used for the selected beam shape and scattering geometry, the real deviations from the ideal scattering experiment are corrected.
As detectors, one-dimensional detectors, e.g. Photodiode arrays, which detect the intensity distribution in a line perpendicular to the primary beam, as well as 2-dimensional arrays such as CCD cameras, image plates or X-ray films.
FIG. 1 shows the basic structure of the low-angle sweep measurement using a known classical Kratky camera, as can be seen, for example, from DE 1002138 B1.
The radiation emitted by the radiation source O is focused in a subsequent optical system 1 onto the sample 3 or the detector 5, which is located at a distance 5 from the sample 3 carried by a sample holder 7 and to which an evaluation unit 30 is connected. In front of the detector 5 there is a primary beam catcher 4. Also slightly divergent beams can be used, since the opening angle is small and sufficient intensities are available after the beam limitation. Due to the ever-present roughness of the optics and building tolerances used, the beam produced in this way is usually additionally limited according to the optics and optionally collimated in a collimator 2. Apertures used for the fine suppression of X-ray radiation always emit scattered radiation itself, which becomes very intense, especially at low angles. Therefore, a number or combination of successive apertures in the beam path is used as a rule. For example, a slot collimator comprising two blocks for masking and collimation of the measuring beam can be used as a combination of diaphragms.
When examining samples, the highest possible intensity of the measuring radiation should be directed to the sample. However, the resolution required for the respective measurement problem must also be taken into account at small angles. In addition to the manufacturing tolerances of the individual components such as collimation block, aperture, beam optics, etc., the focused X-radiation emitted by the source is also due to time-varying properties of the source and the components. For example, due to temperature effects and aging phenomena. Besides, in a modular system, changing individual components, e.g. Source, beam optics, sample holder, etc., also needs adjustments that must be as quickly as possible and comfortable for the operator.
Mechanisms for adjusting the components are known in the prior art. In DE 103 17 677, for example, the adjustment of the Primärstrahlfängers in the z-direction is represented by mechanical means. Adjustments can be made with the help of manually operated mechanical precision actuators or micrometer screws as well as, for example, spindle drives and electric stepper motors.
In order to protect the sensitive detector, the beam intensity emitted by the source can also be reduced when adjusting the system. If a reduction in the emitted intensity of the source used is not desired or possible, the reduction takes place, for example, by means of an absorber inserted between the source and the beam-focusing optics. If sensitive detectors are used whose memory image is only available by separate read-out, for example image plates, or if the radiation of the source should not be modified in intensity, an auxiliary detector can alternatively be used instead of or in front of the detector, for which, for example, photodiodes X-ray films or X-ray fluorescent screens find use.
Currently, before a measurement or between successive measurements, a user manually adjusts the individual components of a device to a suitable intensity in the detector plane in a predetermined sequence and, during the change or during each adjustment step, reads the intensities measured at the detector. These adjustment steps are described to the user in the operating manual including the required position of the image and / or intensities of the primary beam and / or scattering image at the detector. This adjustment procedure thus requires a highly trained and experienced user who manages the necessary settings manually with a sure instinct and coordinates the components in such a way that an optimal adjustment result is achieved for the respective subsequent measurement. This procedure is tedious and error-prone, the individual components can even be destroyed in case of misalignment and in case of maladjustments X-ray radiation can escape from the device into the environment.
These problems are inventively solved in a method of the type mentioned in that prior to the study of the sample at least one, preferably several, in particular all, the following components, namely radiation source and / or beam-forming unit and / or sample holder and / or detector and / or, if appropriate, a primary beam catcher arranged upstream of the detector, aligned relative to at least one of the other components and / or with respect to a fixed point and / or with respect to the beam path with a control unit via actuators and / or with respect to their spatial position, wherein for generating a manipulated variable output by the control unit to the control circuits of the actuators associated with the respective components, which is used by the detector, in particular the radiation intensity measured in at least one predetermined detector area and / or a value derived therefrom.
With the procedure according to the invention, it is possible to perform the adjustment of the device quickly and precisely, if necessary according to a predetermined program, and to initialize or prepare a following examination with high accuracy. According to the invention, the adjustment of the device according to the invention for the user is easy to handle, especially if the entire adjustment is carried out automatically via control loops and controllable components. For this purpose, the intensity occurring at the detector or determined with the intended evaluation unit and / or associated therewith and / or values derived therefrom are used in the control unit as an actuating or control variable for the individual components of the device.
It is to a plurality, preferably all, the adjustable components each equipped with at least one controllable actuator. The actuators are in communication with the control unit connected to the detector and / or the evaluation unit and are preferably controlled by the manipulated variable "intensity at the detector" or "position of the image at the detector".
According to the invention, the individual components can be adjusted automatically according to an adjustment program contained in the control and / or evaluation unit, wherein the entire adjustment process is advantageously carried out step by step automatically for the individual components.
Even with Einjustierung of only one of the components of the device according to the invention with the proposed control unit, it comes to a simplification and specification of the adjustment process. The radiation intensity used as a manipulated variable is very sensitive to a non-exact adjustment and it is thus possible to quickly obtain an optimum value for the proper or required adjustment of the respective component. The Einjustierung of one or more components can be made in a predetermined order of Justierschritten or adapted to the particular problem.
The advantage is that no user-dependent adjustment steps and / or settings are required. Due to the automatic adjustment, absolute positions or adjustment intensities can be reproducibly restored; this guarantees the comparability of the measurements in the case of serial tests, for example on nanoparticles.
It is advantageous if the individual components, if necessary independently of one another, are adjusted to a predetermined starting position before carrying out a measurement, or are in a defined starting position where the values of this output adjustment corresponding to the position and / or orientation of the components are used as initial values for the adjustment be used. , Thus, the starting position of the adjustment process is clearly specified and serves as the basis for the following special Einjustierung.
It is expedient here if the radiation intensity determined at the detector and / or values derived therefrom are compared with stored desired values and the individual components are adjusted or adjusted with the actuators depending on the comparison, and / or if the individual components are adjusted during the adjustment the radiation intensity measured at least one predetermined detector area is approximated to a predetermined value, in particular a maximum, and / or that the signal-to-noise ratio and / or the absolute intensity in the integral two-dimensional image at the detector and / or the values derived from the measured radiation intensity Intensity of individual intensity maxima in the scattering image and / or, in particular when using a one-dimensional detector, which is moved over the measured angular range, local intensity maxima are determined or used.
The measured intensities or any values derived therefrom can be used directly to determine the manipulated variables for the actuators, as long as these values have a significant dependence on the respective position and / or orientation of the respective component.
In order to obtain the greatest possible variety of adjustment options for the adjustment and to take into account all types of components to be adjusted, it can be provided that the components for adjustment with respect to their spatial position in the direction of the beam path and / or adjusted in a plane perpendicular thereto and / or in their Adjusted alignment with respect to the axis of the beam path, in particular rotated about the axis of the beam path and / or tilted with respect to this axis.
To increase the precision of Einjustierung can be provided that the incident on the detector X-ray radiation for the determination of the manipulated variables is measured at a plurality of different detector areas, wherein optionally integrated over predetermined detector ranges of the course of the radiation intensity. 6/24 6
A device of the aforementioned type is inventively characterized in that for alignment and / or position adjustment of the components, namely radiation source and / or beam-forming unit and / or beam-limiting unit and / or sample holder and / or detector and / or optionally a primary detector upstream of the detector , at least one component, preferably a number or each of the components, in each case connected to at least one, in particular each with at least one own actuator and adjustable, which is acted upon by control unit with control signals, wherein the control unit an input for at least one predetermined Detector range of the detector has detected measured values of the radiation intensities and / or values derived therefrom and created in response to these measured values, the control signals. , The structure of the device allows a quick, accurate and secure adjustment of the components. By program default misalignments can be excluded from the house. For safety reasons, the adjusting movements of the actuators can also be preset limits. It is possible to adjust the individual components independently of one another precisely step by step or in a defined sequence.
A simple and rapid adjustment of the device is obtained if the control unit has an input for the adjustment actual values corresponding to the respective orientation and / or position of the components, these actual values either being stored in memories or being determinable with measuring units connected to the control unit or provided by the actuators or are removable from these and / or the control unit (6) comprises a comparator with which the measured values of the radiation intensity determined in predetermined detector areas are comparable with the adjustment actual values stored and / or determined for the individual components.
In the einzujustierenden components, it is advantageous if they are designed to be adjustable in all spatial directions, in particular it is expedient if the beam-forming optics and / or the beam-limiting optics and the radiation source with its respective actuator in the three spatial dimensions relative to each other and / or displaceable about the optical axis or the beam path rotatable and / or tiltable and are driven adjustable.
Depending on the nature and structure of the individual components, the orientation and position play an important role and it can be provided that for the adjustment of the beam-forming and / or beam-shaping optics these optics in the form of in 7/24
Formed and / or einkippbaren or adjustable with respect to their slit width apertures are formed, and / or that the sample holder and / or sample and / or the Primärstrahlenfänger of one in a plane perpendicular to the beam path in the beam path and / or inserted from one in the Beam path tiltable carrier unit are worn and / or the mutual distance between the radiation source and sample holder and / or detector and / or the distance between the sample holder and detector with the actuators associated with these components is adjustable depending on the measured value of the radiation intensity and / or a value derived therefrom.
In the following the invention will be explained, for example, with reference to the drawings. The drawings show some examples of possible adjustments.
Fig. 2 shows schematically the structure of a device according to the invention.
Fig. 3 and 3a show adjustable collimator or aperture units, with which a limitation or collimation of the radiation can be made. Fig. 3b shows an adjustable optics. Fig. 4 shows an optic with sliding panels. Fig. 5 and 6 show a einjustierbaren with actuators sample holder. Fig. 7 shows an adjustable primary ray trap.
Fig. 2 shows the basic structure and the essential components of an X-ray examination apparatus according to the invention, with which the method according to the invention can be carried out. This device is based on the device of FIG. 1, supplemented with a control unit 6 with the actuators 11 for the individual components 0, 01, 1, 2, 4, 5, 7 are controllable. Each component may also be associated with a plurality of actuators 11, e.g. Adjust the component in a different spatial direction. In a simple embodiment, an actuator 11 can adjust a displaceable along the x-y plane arrangement with a holder for the component to be adjusted.
When examining samples 3, the highest possible intensity of the measuring radiation should usually be directed to the sample 3, although the resolution required for the respective measuring problem also has to be considered at small angles. Thus, high demands are placed on the adjustment.
It is also important to determine the actual position of the components.
The actual position of the respective component can be determined at any time by suitable position detecting means, e.g. Position sensors or the position of the actuators 11 themselves, detected or obtained, in particular when the actuators 11, the position and / or orientation of the component to the control unit 6 and / or the evaluation unit 30 feedback. However, the position determination can also be carried out 8/24 8 starting from a rest position without absolute determination of the position, since the relative position of the components plays a role here.
The control of the actuators 11 is advantageously carried out by means of evaluation of the recorded at the detector 5 intensity and / or intensity distribution, comparison of the obtained intensity measured value with a for optimal adjustment position, preferably in the evaluation unit 30, predetermined value and subsequent movement of the respective component. Suitable control algorithms are specified. The respective component is moved with the actuator 11 until the intensity and / or intensity distribution measured at the detector 5 coincides with the predetermined value or is approximated as best as possible.
Preferably, a CCD array or a photodiode array or other position-sensitive detectors are used as the detector 5, which support the adjustment by the recording of spatially resolved images optionally in conjunction with an image recognition software. As a detector, a point-shaped detector can be used which is moved along the primary beam.
The method for adjusting the components in a small and / or wide angle measuring device starts advantageously after installation of the desired components in a modular system or in a fixed system without change options with an adjustment of the radiation source 0 and the beam-forming optics 1. Depending on the used Optics are either the radiation source 0 and / or the beam-focusing optics 1, eg Mirror, Göbel mirror, 2-D optics, 3-D optics od. Like., Aligned relative to each other, so that the highest possible intensity primary beam is formed and this is then passed through the other components of this device. According to the invention, this first step, at least when changing the radiation source 0 and / or the focusing optics 1, can be automated by turning and / or tilting the optics 1 or adjusting the radiation source 0 in the plane perpendicular to the z-axis of the device with the actuators 11. The z-axis usually corresponds to the course of the beam path 9. This step can be controlled with the control unit 6. For adjusting the radiation source 0 and the beam-forming optical system 1, the collimating or beam-limiting optical system 2 is usually removed. This is done either manually by expanding the collimator and aperture comprehensive beam-limiting optics 2, sample holder 7, primary beam catcher 4 or automated according to the invention by moving these components with the actuator 11 in a position that does not limit the measuring beam. Here, an absorber 01 is usually used, which can also be brought into position with an actuator. 9/24 9
When adjusting the beam-limiting optics 2, e.g. Slot collimators in the form of blocks or individual Strahlbegrenzungskomponenten, the Primärstrahlfänger 4 is moved from its measuring position with an actuator and there is an adjustment of the Kollimationselements by tilting the same relative to the z-axis of the camera with its actuator 11th
The aperture elements or collimation elements of the optics 2 can be arranged in a housing or on a mount by means of mounting as well as the other components and can be mounted with actuators 11, e.g. be moved in the form of servomotors, linear motors and / or magnetic drives.
FIG. 3 shows the arrangement of two collimation blocks B1 and B2 located on a carrier 31 which delimit the beam and the primary beam trapper 12. The components collimation blocks B1 and B2 and primary beam catcher 12 can be combined in a housing or frame to form a unit or beam-limiting optics 2 summarized and carried by the carrier 31. This unit can be tilted with the actuator 11 during adjustment relative to the optical axis. This can be done either by tilting the entire optics 2 or by tilting the remaining components, radiation source 0, optics 1, beam catcher 4 and detector 5 bearing frame in which these components along the optical axis 9, that is parallel to the z-direction, are arranged stationary, since it only depends on the relative position and orientation of the individual components to each other. This adjustment takes place automatically as the change of the aperture position with the driven by the control unit 6 actuators eleventh
3a shows a beam-limiting optical system 2, which comprises two tiltable collimation blocks B1 and B2 as well as an adjustable inlet diaphragm 32 and adjustable outlet diaphragms 7a, 7b, 7c and 7d. The tilting and the adjustment of the aperture can be done with servomotors 11, which are indicated here, as well as in the remaining figures. Fig. 3b shows a lens 2 which is adjustable with servomotors 11 via spindle drives 13a, 13b and 13c in all directions and tiltable about all spindle axes.
In order to obtain a simplified adjustment, the optics 2 with an actuator 11 can also be moved along the y-axis in order to adapt the height of the diaphragm to the actual primary beam, separately with an actuator 11, a rotation about the z-axis, to adjust the position of the collimated beam in the xy plane. An adjustment of the adjustable elements of a Kollimationselements can be done by means of a displacement of the aperture with an actuator 11 along the x-axis and adjustment of the diaphragm gap.
As shown in FIG. 4, panels 7a and 7b of an optical system 2 can be slidably mounted on a rail parallel to the x-direction. It can with the 10/24 10
Actuators 11, the distance between the apertures 7a and 7b and thus the gap width S1 can be changed. The actuators 11 drive the spindles 23a and 23b, on which the two panels 7a and 7b are mounted. In addition, the position of the gap can also be shifted along the x-axis. This serves to adjust the gap relative to the beam path 9 of the primary beam through the slot collimation blocks B1 and B2. The collimation blocks B1, B2 or the entire beam-limiting optics can be adjusted by rotation about the z-axis and rotation about the x-axis with appropriate servomotors 11.
If the adjustment, for example, with actuators 11 having stepper motors and spindle drives, the stepper motors can be driven by the evaluation unit 30 and / or control unit 6 with control pulses until the desired position of the aperture 7a, 7b with respect to the slot collimation blocks B1 and B2 is reached.
The gap width S1 can be calculated, for example, starting from the open or closed end position of the shutters 7a, 7b by counting the motor steps and known advance of the spindles 23a, 23b in the control unit 6 and / or evaluation unit 30. Alternatively, the distance of the two diaphragms 7a, 7b with a suitable length measuring system, e.g. optical displacement sensor or distance measuring device to be determined.
The sample 3, which is arranged on or received by an arbitrary sample holder 7, can be adjusted in position, for which purpose the sample holder 7 is initially set to the position intended for it. Different sample holders, e.g. Exchangeable cells, cuvettes, capillary holders, etc., are provided. Sample holders 7 for grazing incidence measurements can also be used. With the actuators 11, the sample holder 7 and the sample 3 relative to the beam path 9 rotational movements, tilting and grid movements are granted to allow spatially resolved investigations.
A change system may be provided for guiding, fixing and installing the sample holder 7 and guide pins, snaps, screw u. Like., Which bring the respective sample 3 in a defined starting position with respect to the sample holder 7.
Optionally, the sample holder 7 can be equipped with a non-contact sensor or chip, which optionally also provides calibration data of the sample holder and can be automatically detected. These data can be used as position and orientation measurements to align the respective sample holder 7 with the 11/24 11
To bring actuators 11 movable in all directions and also rotatably arranged sample holder 7 in the appropriate position.
Fig. 5 shows such an arrangement with actuators 11, which drive the associated spindles 32a, 32b and 32c for translation of the sample 3 in the y-direction, translation in the z-direction and translation in the x-direction. At the same time tilting of the sample holder 7 about the z-axis by an actuator 11 is possible. The control of the movements of the actuators 11 can be done by means of predetermined number of steps with a pulse generator.
If a moveable detector 5 is used in the system, the desired scattering angle range to be measured can optionally be effected by selecting the distance S between the sample 3 and the detector 5. The adjustment of the distance between the sample 3 and the detector 5 can be automated by moving the sample 3 or the sample holder 7 on a sample table and / or moving the detector 5 to the correct position with the actuators 11 as specified. Thus, a fully automatic measurement with different angular ranges by changing the distance between the sample 3 and detector 5 and subsequent automation-supported evaluation of the recorded spectra and standardization of the measurements can be made to each other.
FIG. 6 shows an adjustable sample holder 7 on a table 37 which can be moved in the z-direction, wherein the actuator 11 drives a spindle 36 and thus moves the sample table 37 along the z-axis. Thus, the distance between the sample 3 and the detector 5 can be changed and the sample 3 can be displaced along the optical axis 9. The sample table 37 may be an integral part of the sample holder 7 or part of a removable sample holder. Even a completely modular design is possible.
The primary beam catcher 4 must be able to hide a slit-shaped primary beam when the diaphragm gap is open. Primary beam catcher 4 for a slot-collimated beam of different stroke length and a point-collimated beam can be arranged interchangeably in a Flalterung.
To fully automate the device, automated exchange of different primary beam traps 4, 4 ', 4 " be provided by means of actuated by actuators 11 changing device 15, that is, the respective Primärstrahlfänger 4 is movable with an actuator 11 with a spindle drive 36 in or out of the beam path 9. At 18, the frame of the device is designated, which can support the components and the actuators.
Alternatively, a multi-part design of a Primärstrahlfängers 4 can be realized. At least one primary beam catcher 4 is available for adjustment in a plane perpendicular to the beam path 9. The chosen 12/24 12
Beam catcher 4 is brought by means of an actuator 11 optionally from below into its position in the measurement plane and brought with the measured intensity at the detector 5 with the primary beam in the y direction to cover. If necessary, the orientation of the beam catcher 4 relative to the position of the gap on the detector 5 in the x-y plane must be adjusted by rotating about the z-axis with an actuator 11 here. Preferably, the beam catcher 4 is introduced into the beam path 9 from below in the x-y plane. Each Primärstrahlfänger 4 has a separate feed in the y-direction as shown in Fig. 7 for the Primärstrahlfänger 4, which is adjustable with an actuator 11 with a spindle 36.
The entire adjustment can be automated, for example by selecting the manipulated variable in steps or by specifying absolute values. The control is advantageously carried out e.g. over "smallest detectable scattering angle " or the " desired intensity at the detector " or a " desired " Resolution.
However, a program present in the control unit 6 and / or in the evaluation unit 30 can also provide the user with completely defined measurement programs for, for example, standard characterization of samples. In this case, the automated sequence of several different calibration routines with measurement and subsequent joint evaluation of structural data, for example of nanoparticles over several orders of magnitude, can also take place, as will be explained in more detail below:
Selection of automatic measuring program "Characterization of isotropic nanoparticles with anisotropic internal crystalline structure" Adjustment routine 1 Automatic procedure Sample holder, Adjusting slit collimator and 2D optics to max. Gap length and minimum height, automatic adjustment Primary beam tracer measurement 1 recording isotropic small angle dispersion with minimal qmin adjustment routine 2 Adjust slit collimator and 2D optics to minimum gap length (resolution anisotorpe structure and greater height), adjust primary beam capture measurement 2 recording isotropic / anisotropic small angle dispersion adjustment routine 3 Adjust slit collimator and 2D optics method of sample to greater distance. Measurement 3 Recording wide - angle scattering Automation - supported evaluation and presentation of results 13/24 13
The zero positions from the adjustment can be stored in the memory unit, e.g. the control unit 6, are deposited; From this, different measuring profiles can be derived.
From the automatic adjustment, the zero position or the starting values and the positions for the different profiles are stored in the program and during the actual measurement on a sample when the threshold value is undershot, routines can be carried out automatically. Thus, for example, the measuring beam intensity can be increased and a better evaluable image can be achieved. Thus, even with differing samples without prior knowledge of the expected scatter intensities an evaluable image can be achieved.
It is noted that units for determining the actual actual position and / or orientation of the individual components 0, 1, 2, 4, 5, 7 are not shown in the drawing. Measurement signals relating to this can be obtained with measuring devices of various types which measure the components or are also obtained by the actuators 11 themselves whose respective positioning position can be regarded as a measurement of the position and / or orientation of the respective component.
As a fixed point for an adjustment can advantageously be the position of the radiation source 0 or the sample 3 are used. 14/24
权利要求:
Claims (11)
[1]
1. A method for examining a sample with radiation (8) emitted by a neutron or X-ray source (0), which has at least one beam-forming unit, preferably a beam-forming optical system (1) and / or a beam-limiting optical system (2), to the sample (3) carried by a sample holder (7) and detected by a detector (5) and evaluated in an evaluation unit (30), characterized in that before starting the examination of the sample at least one, preferably several, in particular all the following components, namely radiation source (0) and / or beam-shaping unit (1, 2) and / or sample holder (7) and / or detector (5) and / or optionally a primary radiation trap (4) arranged upstream of the detector (5), Relative to at least one of the other components (0, 1,2,4, 5, 7) and / or with respect to a predetermined fixed point and / or with respect to the beam path (9) with a control unit (6) via Stellan geared (11) and / or adjusted with respect to their spatial position, wherein for the preparation of one of the control unit (6) to the control circuits of the respective components (0, 1, 2, 4, 5, 7) associated actuators (11) delivered manipulated variable, which is used by the detector (5), in particular the radiation intensity measured in at least one predetermined detector area, and / or a value derived therefrom.
[2]
2. The method according to claim 1, characterized in that the individual components (0, 1, 2, 4, 5, 7), optionally independently, are adjusted before performing a measurement in a predetermined starting position, or are in a defined starting position wherein the values of this output adjustment corresponding to the position and / or orientation of the components are used as initial values for the adjustment.
[3]
3. The method according to claim 1 or 2, characterized in that the detector (5) detected radiation intensity and / or values derived therefrom compared with stored setpoint values and depending on the comparison, the individual components (0, 1,2, 4, 5, 7) with the actuators (11) can be adjusted or adjusted.
[4]
4. The method according to any one of claims 1 to 3, characterized in that during the Einjustierung of the individual components (0, 1, 2, 4, 5, 7) measured in the at least one predetermined detector area radiation intensity a predetermined value, in particular a maximum , is approximated, and / or that as of the measured radiation intensity! derived values the signal-to-noise ratio 15/24 2 and / or the absolute intensity in the integral, two-dimensional image at the detector (5) and / or the intensity of individual intensity maxima in the scattering image and / or, in particular when using a one-dimensional detector (5) , which is moved over the measured angular range, local intensity maxima are determined or used.
[5]
5. The method according to any one of claims 1 to 4, characterized in that the components (0, 1, 2, 4, 5, 7) for adjustment with respect to their spatial position in the direction of the beam path (9) and / or in a plane perpendicular adjusted and / or adjusted in their orientation with respect to the axis of the beam path (9), in particular rotated about the axis of the beam path (9) and / or tilted with respect to this axis.
[6]
6. The method according to any one of claims 1 to 5, characterized in that the detector (5) incident X-ray radiation for the determination of the manipulated variables is measured at a plurality of different detector areas, wherein optionally integrated over predetermined detector areas of the course of the radiation intensity.
[7]
7. An apparatus for radiographic examination of samples, comprising a neutron or X-ray source (0), at least one beam-forming unit, preferably at least one beam-forming optics (1) and / or a beam-limiting optics (2), one between the radiation source (0) and a sample holder (7) arranged in a detector (5), wherein the detector (5) is optionally preceded by a primary radiation trap (4), characterized in that for alignment and / or position adjustment of the components, namely radiation source (0) and / or beam-forming unit ( 1) and / or beam-limiting unit (2) and / or sample holder (7) and / or detector (5) and / or optionally a detector (5) upstream Primärstrahlenfänger (4), at least one component, preferably a number or each of Components, each with at least one, in particular in each case with at least one own, actuator (11) is connected and adjustable, of a Steuereinhei The control unit (6) has an input for measured values of the radiation intensities determined at at least one predetermined detector area of the detector (5) and / or values derived therefrom and generates the actuating signals as a function of these measured values.
[8]
8. The device according to claim 7, characterized in that the control unit (6) has an input for the respective orientation and / or position of the components (0, 1, 16/24 3 2, 4, 5, 7) corresponding adjustment actual values wherein these actual values are either stored in memories or can be determined with measuring units connected to the control unit (6) or provided by the actuators (11) or can be removed therefrom.
[9]
9. Apparatus according to claim 7 or 8, characterized in that the control unit (6) comprises a comparator with which the determined in predetermined detector areas measured values of the radiation intensity with for the individual components (0, 1, 2, 4, 5, 7) stored and / or determined calibration actual values are comparable.
[10]
10. The method according to any one of claims 7 to 9, characterized in that the beam-forming optical system (1) and / or the beam-limiting optics (2) and the radiation source (0) with their respective actuator (11) in the three spatial dimensions relative to each other and / or about the optical axis or the beam path (9) rotatably mounted and / or tiltable and are driven adjustable.
[11]
11. Device according to one of claims 7 to 10, characterized in that for Einjustierung the beam-forming and / or beam-shaping optics (1, 2), these optics (1, 2) in the form of in the beam path (9) and / or einkippbaren or with respect to their gap width adjustable aperture are formed, and / or that the sample holder (7) and / or sample 3 and / or the Primärstrahlenfänger (4) of a in a plane perpendicular to the beam path (9) in the beam path (9) insertable and / or carried by a carrier unit which can be tilted into the beam path and / or the mutual distance between the radiation source (0) and sample holder (7) and / or detector (5) and / or the distance between sample holder (7) and detector (5) with the actuators associated with these components (11) is adjustable depending on the measured value of the radiation intensity and / or a value derived therefrom. 17/24
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法律状态:
优先权:
申请号 | 申请日 | 专利标题
ATA50552/2012A|AT513660B1|2012-11-30|2012-11-30|Method and device for examining samples|ATA50552/2012A| AT513660B1|2012-11-30|2012-11-30|Method and device for examining samples|
DE102013112736.3A| DE102013112736A1|2012-11-30|2013-11-19|Method and device for examining samples|
JP2013249271A| JP2014109579A|2012-11-30|2013-12-02|Method and device for examining sample with beam emitted from neutron or x-ray beam source|
US14/093,873| US9562865B2|2012-11-30|2013-12-02|Method and apparatus for analysis of samples|
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