Measuring object and method for verifying the calibration of an x-ray fluorescence device

Abstract

The invention relates to a measuring object (100) and a method for verifying the calibration of an X-ray fluorescence device (9), wherein the measuring object (100) has a main body (110) and at least one marker (112) arranged on the main body (110). The marker is formed from a material different from the main body (110), and the marker (112) is equipped with at least one further layer (114) which emits electromagnetic radiation of different intensity (IS, IRf) when struck by X-ray radiation (RS).

Description

Technical Field

[0001] This invention relates to a measurement object and method for verifying the calibration of an X-ray fluorescence device. Background Technology

[0002] Document CN101551347B provides a calibration standard for the initial alignment of X-ray radiation points in X-ray fluorescence apparatus. This calibration standard is designed as a plate with two longitudinal slits aligned perpendicularly to each other. By moving the calibration standard on the stage of the X-ray fluorescence apparatus, the intensity of X-ray fluorescence radiation emitted in the areas of the plate and the slits is detected to align the X-ray radiation point.

[0003] Document DE 19836884C1 also discloses a method and sample assembly for determining intensity data of a measurement point in X-ray fluorescence analysis. The sample assembly consists of a surrounding material and a probe with a defined profile disposed within the surrounding material. Both the surrounding material and the probe material have the same linear attenuation coefficient for the emitted X-ray fluorescence radiation. By moving the sample assembly on the measurement stage, the intensity center of the X-ray fluorescence source and the contour of the measurement point can be determined.

[0004] An X-ray fluorescence analyzer is known from JP 2008-286554A. A camera is provided for determining the position of a sample on the measuring stage. Images of the sample's position on the measuring stage are captured and analyzed before and after the cover of the X-ray fluorescence analyzer is closed.

[0005] An X-ray fluorescence analyzer is known from document DE 10013012A1. In the preparation process for performing X-ray fluorescence analysis, the sample is positioned in an optical sample observation system, where it is irradiated with an X-ray beam. As a determining process, an image of the sample is captured, in which the brightness of material A, which is adjacent to each other and each forms a linear interface with another material B, is detected. It is then determined whether the X-ray beam irradiating the sample has partially penetrated the sample. Summary of the Invention

[0006] The object of this invention is to provide a measurement object for verifying the calibration of an X-ray fluorescence device, which enables simple and rapid verification. Another object of this invention is to provide a method for verifying the calibration of an X-ray fluorescence device, which can be performed in a simple manner.

[0007] This objective is achieved through a measurement object for verifying the calibration of an X-ray fluorescence apparatus, the measurement object comprising a body and at least one mark disposed on the body. The body is formed of a first material, and the mark disposed on or within the body is formed of a second material different from the first material. Furthermore, the measurement object is configured such that the body has a layer in at least some regions, the layer being aligned with the mark. When the layer and the mark are at least partially exposed to X-ray radiation, the layer emits or reflects electromagnetic radiation of a predetermined wavelength range, and the mark emits X-ray fluorescence radiation of a predetermined intensity. This allows the characteristic intensity of the reflected or emitted radiation from the layer and the mark, provided at least in some regions and aligned with the mark, to be detected by the layer after exposure to X-ray radiation. These intensities can be analyzed within the X-ray fluorescence apparatus.

[0008] In the data processing apparatus of an X-ray fluorescence device, it is advantageous to store reference data of various intensities for layers assigned to or aligned with markers, as well as for markers selected based on material. This reference data is compared with data determined by detectors of X-ray fluorescence emitted by the markers and by detectors (particularly optical detection devices) of electromagnetic radiation reflected or emitted by the layers. Ideally, if the detected intensities of the layers and markers match the stored reference data or intensities, it can be assumed that the X-ray source, at least one collimator or X-ray optics for guiding the X-ray beam, the detector for detecting X-ray fluorescence, and the optics for detecting the object being measured have been calibrated to the target state. This means that the object being measured can be examined simultaneously in both the light field and the X-ray field. If the intensity of radiation emitted from the layers and / or markers deviates from the predetermined intensities of the layers and markers respectively, it is necessary to readjust the X-ray fluorescence device and / or the object being measured, or its position on the measuring stage of the X-ray fluorescence device, because it has changed compared to the original calibration of the X-ray fluorescence device, for example, after delivery due to transportation or during operation due to temperature effects.

[0009] Preferably, the second material is a heavy metal, such as lead. In particular, the first material is not a heavy metal.

[0010] The first material of the body may include at least one of the following materials: a) PTFE, polytetrafluoroethylene; b) PMA, polymethyl acrylate; c) PMMA, polymethyl methacrylate; d) PC, polycarbonate; e) PE, polyethylene.

[0011] Advantageously, the primary material of the body can have a relatively high purity, for example, it is free of additives, especially colorants and / or metal additives.

[0012] Compared to the labeled second material, the host first material emits relatively low X-ray fluorescence when exposed to X-ray radiation.

[0013] The layer within and / or on the body that aligns the mark, or the layer designated for the mark, can be designed as a fluorescent coating.

[0014] Preferably, the wavelength range of the layer is between 300 nm and 1100 nm (nanometers), particularly between 400 nm and 800 nm, for example, within the human visible wavelength range. This allows the user to easily perceive optically and / or detect via an image detector, such as a digital camera operating in the same or at least similar wavelength range.

[0015] Optionally, the predetermined or pre-defined wavelength range may be outside the human visible wavelength range, for example, and may be detected by a suitable digital camera, such as one having at least one image sensor with corresponding spectral sensitivity. The image sensor may be, for example, a CCD (charge-coupled device) type or a CMOS (complementary metal-oxide-semiconductor) type, or other types.

[0016] The marker may have at least two intersecting lines, particularly intersecting straight lines, which are preferably orthogonally aligned with each other. This can also facilitate and / or accelerate the alignment of the object to be measured on the measuring stage of an X-ray fluorescence apparatus with respect to the detector, particularly the optical detection device.

[0017] The mark may have at least one circle. In particular, at least two intersecting lines or at least two straight lines are arranged concentrically with the point of intersection within the circle. The advantages of a circular mark can be similar to those of an intersecting line mark.

[0018] The layer is preferably arranged inside the circle. In particular, the layer covers the entire area of ​​the circle.

[0019] The object being measured may have a sheet-like shape, wherein the thickness of the object being measured is less than at least one external dimension of the object being measured in a direction perpendicular to its thickness. For example, the thickness of the object being measured may be less than the width and height of the object being measured, or less than the width and height of the marked surface of the object being measured.

[0020] The object to be measured can be placed manually and / or automatically on the sample stage or measuring stage of the X-ray fluorescence apparatus. The sample stage can be designed as what is commonly referred to as an automated sample stage, allowing the stage surface or the object to be measured placed on the stage to be moved by an electric actuator.

[0021] The problem solved by the present invention is further addressed by a method for calibrating an X-ray fluorescence apparatus according to this application. For this purpose, a measurement object according to any of the foregoing embodiments is used. The measurement object is positioned within the X-ray fluorescence apparatus. The measurement object is then exposed to X-ray radiation at least temporarily. A first quantity is then detected, the first quantity having the intensity of electromagnetic radiation emitted by a layer on a mark of the measurement object. Furthermore, the first quantity having the intensity of electromagnetic radiation emitted by the mark of the measurement object can be detected by a detector. Subsequently, a match or difference (DS) between the first quantity detected from the layer of the measurement object and a predetermined intensity of the layer is determined, and / or a match or difference (DM) between the first quantity detected from the mark of the measurement object and a predetermined intensity of the mark of the measurement object is detected. When at least one difference (DM, DS) is determined, alignment or readjustment of the measurement object of the X-ray apparatus is performed, or readjustment of at least one detector, at least one collimator, X-ray optics, and / or the X-ray source of the X-ray fluorescence apparatus is performed. Therefore, by checking the first quantity of the layer with a detector for a predetermined wavelength range of the layer and checking the first quantity of the mark with a detector for X-ray fluorescence radiation of the mark, it is possible to simultaneously verify whether adjustment is needed and to what extent. Therefore, the operator of the X-ray fluorescence apparatus can immediately see any adjustments that may be necessary. Additionally, the operator or control system of the X-ray fluorescence apparatus can receive instructions via a display or screen indicating which components of the apparatus require realignment.

[0022] Preferably, when the detected intensity IS1 corresponds to a predetermined intensity IS of the layer of the object being measured within permissible limits, and when the difference DM relative to the mark is determined, it is determined that the X-ray source, at least one collimator or X-ray optics, and / or the detector for detecting X-ray fluorescence radiation must be readjusted, and the detector for electromagnetic radiation of the layer is still properly calibrated for the predetermined wavelength range. Therefore, by exposing the object being measured to X-ray radiation only once, it is possible to verify whether the optics used to detect the position of the object on the measuring stage are misaligned and / or whether the X-ray source, at least one collimator or X-ray optics, and / or the detector for detecting X-ray fluorescence needs to be readjusted.

[0023] Furthermore, preferably, when it is determined that the detected intensity IRf1 matches the predetermined intensity IRf of the mark within the tolerance range, and when the difference DS of the layer intensity is determined, it is determined that the detector used to detect electromagnetic radiation is misaligned for the predetermined wavelength range. Therefore, it can be determined that the components related to X-ray radiation and X-ray fluorescence radiation do not require readjustment, but rather that the optical detection device and / or its optical components need to be readjusted to position the object being measured on the measuring stage.

[0024] Furthermore, preferably, when determining the difference DS and difference DM after exposing the object to X-ray radiation, the object is first aligned with a detector used to detect electromagnetic radiation for a predetermined wavelength range in the first step. If a match is detected between the intensity IS1 and the predetermined intensity IS of the layer, then the determination of the marked intensity match or difference DM is performed. This method step is performed to ensure that misrepresentation is avoided if the object is not correctly positioned relative to the X-ray source and detector (especially the optical detection device). If the intensity of the layer of the object is matched and the difference DM is subsequently determined, the X-ray source, at least one collimator or X-ray optics, and / or the detector used to detect X-ray fluorescence radiation must be readjusted.

[0025] According to another advantageous embodiment of the method, when the difference DS and difference DM are determined, calibration of the measurement object on the measuring stage and the detector used to determine electromagnetic radiation is performed in the first step for a predetermined wavelength range. When the difference DS is further determined, the readjustment of the detector 12' for detecting electromagnetic radiation for the predetermined wavelength range is determined.

[0026] According to another advantageous embodiment of the method, the stage of the X-ray fluorescence apparatus can be moved outside the X-ray radiation area, and the object under test is aligned on the measuring stage using a visible beam device, particularly a laser pointer. The visible beam device is arranged adjacent to the X-ray source 10, and particularly separately from the X-ray source. The measuring stage is then moved back to the X-ray radiation area, and the determination of layer matching or difference DS and / or mark matching or difference DM is performed. If difference DS is determined, the readjustment of the detector's detection of the electromagnetic beam for a predetermined wavelength range is determined, and if difference DM is determined, the readjustment of the visible beam device (particularly the laser pointer) is determined. This allows further verification of possible readjustments of the components of the X-ray fluorescence apparatus to be performed.

[0027] Furthermore, preferably, the X-ray source is aligned with the object being measured before the object is at least temporarily exposed to X-ray radiation, and / or vice versa. On one hand, manual alignment can be provided, wherein, in particular, the position and / or orientation of the object to be measured is displayed on the display or monitor of the X-ray fluorescence apparatus. Alternatively, automatic alignment, particularly automatic alignment of the object being measured, can also be controlled. For this purpose, the controller of the X-ray fluorescence apparatus processes the data to realign the position and / or orientation of the object being measured.

[0028] Automatic alignment can be based on, for example, digital image or video data streams captured by a digital camera or camcorder.

[0029] Preferably, pattern recognition methods can be used to determine the markings of the measurement object on the digital image or in the video data stream, and if necessary, to determine and / or influence the relative alignment of the X-ray source and the measurement object, thereby improving the accuracy of the alignment.

[0030] If a difference in DS or DM is detected, further processing steps can preferably be performed to characterize the difference. The processing arrangement includes: changing the arrangement and / or alignment of the object being measured relative to the X-ray source; repeatedly detecting at least temporary exposure of the object to X-ray radiation and electromagnetic radiation emitted by at least one component of the object (particularly layers and markers) due to the X-ray exposure; and determining a change in a first quantity based on the detected electromagnetic radiation, and optionally, changing the arrangement and / or alignment of the object relative to the X-ray source again based on the change in the first quantity. In this way, the position and / or alignment of the X-ray source and its associated detectors and other optical devices can be determined first.

[0031] To determine the position and / or orientation of an X-ray source relative to a measurement object, the following steps can be performed: determining multiple values ​​of electromagnetic radiation emitted by at least one component of the measurement object due to the object's exposure to X-ray radiation; each of at least two of these values ​​being associated with a different arrangement and / or alignment of the measurement object relative to the X-ray source; and determining information characterizing the alignment (e.g., misalignment) and / or arrangement of the X-ray source relative to the measurement object via at least two of these values, using at least one vector (e.g., an error vector). This enables computational corrections or practical alterations to the setup of at least one component of an X-ray fluorescence apparatus.

[0032] Preferably, a first quantity (or intensity IS1) of the layer of the object being measured is detected by at least one digital image, wherein a digital camera can be used to determine at least one first quantity.

[0033] Preferably, the method includes: changing the arrangement and / or alignment of the object to be measured relative to the X-ray source; repeatedly detecting at least temporary exposure of the object to X-ray radiation and electromagnetic radiation emitted by at least one component of the object (particularly layers and markings) due to the exposure of the object to X-ray radiation, said detection being detected by at least one digital image; and determining a change in a first quantity based on the detected digital image, and again changing the arrangement and / or alignment of the object to be measured relative to the X-ray source based on the change in the first quantity. Misalignment between the X-ray source and the object to be measured can be determined by differences between a first digital image, a second digital image, or other digital images, and a vector can be determined, particularly an error vector for correction, or it can be determined whether the change has resulted in the desired alignment, rather than the aforementioned deviation.

[0034] The method may further include sending information characterizing the alignment and / or arrangement of the X-ray source relative to the object being measured to at least one drive unit to change the arrangement and / or alignment of the object being measured relative to the X-ray source. This enables, for example, closed-loop control of the arrangement and / or alignment of the object being measured relative to the X-ray source.

[0035] Optionally or additionally, the method may further include: informing the user about the alignment and / or arrangement of the X-ray source relative to the object being measured by outputting information on the display of the X-ray fluorescence apparatus. This allows for manual adjustment of the alignment and / or arrangement, or allows the user to be informed of the current alignment and / or arrangement.

[0036] Preferably, the following steps may be performed: a) providing a measurement object for X-ray fluorescence analysis; b) enabling the X-ray source to be effectively and / or precisely aligned and / or positioned relative to the measurement object, and / or vice versa; c) ensuring that the optical field of view that can be captured by a camera (e.g., a digital camera) corresponds to the area that can be exposed to X-ray radiation from the X-ray source (“X-ray field”), the X-ray source being independent of any components that may be present in the beam path of the X-ray radiation, such as components that change the beam, such as collimators (K), filters, and apertures; d) checking the alignment and / or positioning of the X-ray source relative to the measurement object; e) assisting the user in orienting and / or positioning the X-ray source relative to the measurement object, and / or vice versa; f) selecting a collimator and / or another field-shaping element to be positioned in the beam path of the X-ray radiation; and g) correcting the alignment and / or positioning of the X-ray source relative to the measurement object. Attached Figure Description

[0037] The invention and its other advantageous embodiments and developments will now be described and illustrated in more detail with reference to the examples shown in the accompanying drawings. According to the invention, features obtained from the specification and drawings can be applied individually or in any combination. In the drawings: Figure 1 It is a schematic diagram of the object being measured; Figure 2 This is a schematic diagram of an X-ray fluorescence apparatus with a measurement object. Figure 3 This is a plan view of the worktable of the X-ray fluorescence apparatus; Figure 4 This is a schematic flowchart illustrating the operation of an X-ray fluorescence device; Figure 5 It is a schematic flowchart for determining the first quantities used to measure the alignment and / or arrangement of objects; Figure 6 It is a schematic diagram used to determine information for determining error vectors from digital images; Figure 7It is a schematic flowchart for determining the alignment of a measurement object using digital images; Figure 8 It is a schematic flowchart for determining information used to determine error vectors from digital images; and Figure 9 This is a schematic diagram of the process steps used to calibrate an X-ray fluorescence device. Detailed Implementation

[0038] Figure 1 This is a view of the measured object 100, according to Figure 2 The measurement object 100 can be used for the calibration of the X-ray fluorescence device 9. The measurement object 100 has a body 110 and at least one mark 112 disposed on the body 110. The body 110 comprises a first material M-1 and / or the body 110 is formed of the first material M-1, and the mark 112 is formed of a second material M-2 different from the first material M-1. The second material M-2 may be a heavy metal, such as lead. The first material M-1 is preferably not a heavy metal.

[0039] The first material M-1 may include at least one of the following materials: a) PTFE, polytetrafluoroethylene; b) PMA, polymethyl acrylate; c) PMMA, polymethyl methacrylate; d) PC, polycarbonate; e) PE, polyethylene.

[0040] Preferably, the first material M-1 has relatively high purity, for example, it is free of additives and / or, for example, free of colorants and / or metal additives.

[0041] Compared to the second material, the first material M-1 emits relatively low X-ray fluorescence emission when exposed to X-ray radiation RS.

[0042] Figure 2 The X-ray fluorescence device 9 is shown schematically. The X-ray radiation RS is provided by the X-ray source 10.

[0043] The electromagnetic radiation ES2 emitted by the object being measured 100 is detected by detector 12 (e.g., photodetector) for X-ray fluorescence emission and detector 12' (particularly an optical detection device, e.g., an image sensor or digital camera).

[0044] The object to be measured 100 can be placed on the worktable 20 or formed integrally with the worktable 20.

[0045] The object to be measured 100 can be placed on the sample stage 20 manually and / or automatically. The sample stage 20 can be designed as an automated sample stage, such that the table surface and the object to be measured 100 arranged or integrally formed on the table surface can be moved, for example, by means of an electric actuator 21.

[0046] A visible light beam device 18, particularly a laser pointer, may also be provided for aligning the object to be measured 100 on the sample stage 20 or measuring stage 20. This beam device 18 is adjacent to the X-ray source 10 and preferably separate from and aligned with the X-ray source 10. Advantageously, the beam device 18 can also be connected via a driver 11, by which the position of the beam device 18 can be changed together with the X-ray source. The beam device 18 for emitting visible light is oriented along the direction of the sample stage 20. This beam device 18 is particularly useful in arrangements of X-ray fluorescence devices 9, where the distance between the X-ray optics or at least one collimator and the surface of the sample stage 20 is small.

[0047] To align the object 100 on the measuring stage 20, the measuring stage 20 can be moved outside the area of ​​the X-ray radiation RS. Then, the object 100 can be aligned on the sample stage 20 using the beam device 18. Specifically, the markings 112 on the object 100 can have a supporting effect. The measuring stage 20 is then returned to its starting position, allowing the X-ray beam RS to be directed onto the object 100 to verify the calibration of the X-ray fluorescence device 9.

[0048] Main body 110 ( Figure 1 At least in some areas there is layer 114, layer 114 is exposed to X-ray radiation RS ( Figure 2 When the electromagnetic radiation ES1 is emitted at an intensity IS within a predetermined wavelength range WLB, the electromagnetic radiation ES1 can be detected, for example, by a detector 12'.

[0049] Layer 114 is preferably a fluorescent coating. The fluorescent coating 114 may include one of the following materials: a) rock salt (sodium chloride); b) lithium fluoride; c) potassium chloride; d) Na2O2 (sodium peroxide).

[0050] The predetermined wavelength range WLB of layer 114 is in the range between 300 nm and 1100 nm, particularly in the range between 400 nm and 800 nm, for example in the human visible wavelength range. This allows the user to, for example, simply perceive optically and / or detect via an image detector 12' (e.g., a digital camera 12') that operates in the same or at least similar wavelength range.

[0051] Optionally, the predetermined wavelength range WLB of layer 114 may be at least partially outside the human visible wavelength range, which may be detected, for example, by a suitable digital camera 12' (e.g., including at least one image sensor with corresponding spectral sensitivity) or a photodetector 12 (e.g., may include a PIN diode). For example, the image sensor may be of the CCD (charge-coupled device) type or the CMOS (complementary metal-oxide-semiconductor) type, or it may be of other types.

[0052] Designation 112 includes one of the aforementioned materials M-1, wherein electromagnetic radiation ES1 is emitted at an intensity IRf when exposed to X-ray radiation RS. During this process, due to the selection of material M-1, X-ray fluorescence radiation including a predetermined intensity IRf is emitted.

[0053] according to Figure 1 The mark 112 may include at least two intersecting lines 112a, 112b, such as straight lines, which are aligned orthogonally to each other.

[0054] The mark 112 preferably includes at least one circle 112c, wherein the circle 112c is concentrically arranged with the intersection point 112ab of at least two intersecting lines or straight lines 112a, 112b.

[0055] Layer 114 can be arranged within circle 112c. In particular, layer 114 extends entirely within circle 112c. This makes it possible to assess the alignment of X-ray source 10 or X-ray radiation RS relative to the object being measured with particular precision, in order to determine whether the X-ray radiation RS is concentrically oriented with circle 112.

[0056] The measuring object 100 has a sheet-like shape, and the thickness D1 of the measuring object 100 is ( Figure 2 The thickness D1 of the measured object 100 is less than at least one external dimension of the measured object 100 in the direction perpendicular to the thickness D1. For example, the thickness D1 of the measured object 100 is less than the width B1 of the measured object. Figure 1 The width B1 and height H1 of the surface 100a with mark 112 of the object being measured are less than the object 100.

[0057] Figure 4 A method for operating an X-ray fluorescence apparatus 9 having an X-ray source 10 emitting X-ray radiation RS is schematically illustrated. The method includes: exposing the object to be measured 100 at least temporarily to X-ray radiation RS. Figure 2 ); Detection 204 ( Figure 4 Electromagnetic radiation ES1, ES2 emitted by at least one component 112, 114 of the object being measured 100, for example, said electromagnetic radiation is emitted due to the object being measured 100 being exposed to X-ray radiation RS; and through at least one photodetector 12 ( Figure 2 The X-ray source 10 and at least one digital camera 12' determine at least one first quantity G1, G2 based on the detected electromagnetic radiation ES1, ES2, the first quantity characterizing the alignment of the X-ray source 10 with the object being measured 100.

[0058] exist Figure 4 The determination of the first quantity G2 by at least one photodetector 12 is symbolically shown in step 206a, and... Figure 4 The determination of the first quantity G1 by at least one digital camera 12' is symbolically shown in step 206b.

[0059] After the first exposure 202 of the object to be measured to the X-ray radiation RS, alignment 200 is performed. For example, the X-ray source 10 is manually aligned with the object to be measured and / or the object to be measured and the X-ray source 10 are manually aligned 200a and / or automatically aligned 200b by a driver 21 and / or manually.

[0060] Automatic alignment 200b can be performed based on digital image or video data streams captured by digital camera 12' or camcorder.

[0061] In particular, pattern recognition methods (e.g., “pattern recognition”) can be used to determine the markings 112 of the object 100 being measured on a digital image or in a video data stream, and if necessary, determine and / or influence the relative alignment of the X-ray source 10 and the object 100 being measured relative to each other, which can improve the accuracy of the alignment 200.

[0062] To determine the first quantities G1 and G2 of the intensity IS and IRf of electromagnetic radiation ES1 and ES2, we can use the following... Figure 5 Provide the following operations: 210 Change the arrangement AN (e.g., position) and / or alignment AUSR (e.g., angular alignment) of the measurement object 100 relative to the X-ray source 10; 212 Repeat at least temporary exposure 202 of the measurement object 100 ( Figure 4 ) Detection of X-ray radiation and electromagnetic radiation ES1', ES2' 204 ( Figure 5 The method determines the intensity IS and IRf generated in front of the marker 112 and layer 114 of the measurement object 100 due to the exposure of the measurement object to X-ray radiation; and determines the changes G1' and G2' in the first quantities G1 and G2 based on the detected electromagnetic radiation ES1' and ES2', and changes 216 in the arrangement and / or alignment of the measurement object relative to the X-ray source based on the changes in the first quantities G1 and G2. Optionally, in other exemplary embodiments, one or more of the methods or operations 210, 212, 214, and 216 may be repeated, for example, until the desired alignment or arrangement is achieved, for example, the X-ray radiation RS relative to the intersection 112ab ( Figure 1 (or concentric alignment of circle 114)

[0063] according to Figure 6Preferably, the following operations are provided: determining 220+ values ​​ES-W-1, ES-W-2, ES-W-3, wherein the multiple values ​​characterize the electromagnetic radiation emitted by the marker 112 and layer 114 of the measurement object 100 due to the exposure of the measurement object 100 to X-ray radiation, wherein each of at least two of the multiple values ​​ES-W-1, ES-W-2, ES-W-3 is associated with a different arrangement and / or alignment of the measurement object 100 relative to the X-ray source 10; and determining 222 information I-AUSR based on at least two of the multiple values ​​ES-W-1, ES-W-2, ES-W-3 by at least one vector (e.g., error vector), wherein the information characterizes the alignment (e.g., misalignment) and / or arrangement of the X-ray source 10 relative to the measurement object 100.

[0064] First quantity G1 ( Figure 4 ) can be at least one digital image of the object 100, for example, using a digital camera 12' ( Figure 2 ).

[0065] The first quantity G2 can be the spectrum determined by detector 12 used to detect X-ray fluorescence emission from marker 112.

[0066] according to Figure 7 The method may include: 230 changing the arrangement and / or alignment of the object to be measured 100 relative to the X-ray source; 232 repeating the detection of at least temporary exposure of the object to X-ray radiation RS and electromagnetic radiation ES2'' emitted by at least one component 112, 114 of the object to be measured due to exposure of the object to X-ray radiation RS, said detection being the recording of at least one additional digital image DB-2; 234 determining a change G1' of a first quantity G1 based on the recorded digital images DB-1, DB-2; and 236 changing the arrangement and / or alignment of the object to be measured relative to the X-ray source again based on the change G1' of the first quantity G1. Before changing 230, a first digital image DB-1 may be recorded first, then the change 230 may be performed, and then a second digital image or another digital image DB-2 may be recorded. Based on the difference between the first digital image and the second digital image, it can be determined whether misalignment still exists between the X-ray source 10 and the object to be measured 100, or whether the change has resulted in the desired alignment, rather than the aforementioned deviation.

[0067] according to Figure 8The method may further include: determining a plurality of digital images DB-1, DB-2, DB-3, the plurality of digital images representing electromagnetic radiation emitted by at least one component 112, 114 of the measurement object 100 due to the measurement object being exposed to X-ray radiation RS, wherein each of at least two of the plurality of digital images DB-1, DB-2, DB-3 is associated with a different arrangement and / or alignment of the measurement object 100 relative to the X-ray source 10; and determining 242 information I-AUSR' based on at least two of the plurality of digital images DB-1, DB-2, DB-3 by at least one vector (e.g., an error vector), the information representing the alignment (e.g., misalignment) and / or arrangement of the X-ray source 10 relative to the measurement object 100.

[0068] According to Figure 6 and Figure 8 In a preferred embodiment, the method includes sending information I-AUS, I-AUSR' characterizing the alignment and / or arrangement of the X-ray source 10 relative to the measurement object 100 to the drive unit 21 via 224a, so as to change the arrangement and / or alignment of the measurement object 100 relative to the X-ray source 10. This enables closed-loop control of the arrangement and / or alignment of the measurement object relative to the X-ray source.

[0069] The method may further include notifying the user (224b) of information IAUSR, IAUSR', which characterize the alignment and / or arrangement of the X-ray source relative to the object being measured. This allows, for example, manual adjustment of the alignment and / or arrangement or notification of the current alignment and / or arrangement to the user.

[0070] It can also be stipulated that the target be aligned with 200 ( Figure 4 It is performed based on at least one digital image DB-1.

[0071] The method specifically involves using a measurement object 100 to check the matching between the light field and the X-ray field. This allows for a simple inspection of the geometrical matching between the X-ray beam and the optical inspection device (especially a digital camera). The measurement object 100 is manually placed, for example, on a sample stage 20 (…). Figure 3 The measurement object 100 is moved to a predetermined test position on the sample stage 20. Optionally or additionally, an automated stage can be used to move the measurement object 100 to the test position. Optionally or additionally, the measurement object 100 may have been integrally formed with the sample stage 20 at a predetermined position. In more exemplary embodiments, the position of the measurement object 100 may be accessible, for example, for the aforementioned inspection of the matching between the light field and the X-ray field.

[0072] To accurately align the object being measured 100, a crosshair mark 112 can be applied using a structure that absorbs X-ray radiation RS (e.g., a second material M-2, such as lead). For example, a concentric ring or circle 112c, also made of lead or the second material M-2, can be applied around the crosshairs 112a, 112b, which, for example, define a center 112ab.

[0073] Circle 112c ( Figure 1 The annular diameter D of the collimator can correspond to the collimator diameter of the collimator K, which is used, for example, to project an X-ray source 10 at a nominal distance from the measuring stage 20, such as... Figure 2 As shown. For example, as Figure 2 As schematically shown, the collimator K is arranged in the beam path of the X-ray radiation RS between the X-ray source 10 and the object being measured 100.

[0074] For example, the standard component or laser pointer of the X-ray source 10, or the X-ray measurement system containing it, is first aligned relative to the measuring stage 20 or the object to be measured 100 located on or arranged in the measuring stage, such that, for example, the crosshairs 112a, 112b of the object to be measured coincide with the crosshairs of the standard component or laser pointer.

[0075] Optionally, a pattern recognition algorithm is executed, wherein a digital image of the object 100 being measured is recorded, for example, by a CCD camera 12', and analyzed automatically. This allows the CCD camera to perform a predetermined alignment of the object 100 being measured, which can be automated. This eliminates the need for the user to precisely align the measuring stage / standard, thereby eliminating further errors.

[0076] Preferably, collimator K is selected. Figure 2 ), such that the projection of the collimator onto the worktable plane 100a (standard part) corresponds to the diameter D of the ring 112c on the measuring object 100. Figure 1 Other diameters of the collimator K are also possible, as described below.

[0077] After the object 100 has been aligned, it is irradiated with X-ray radiation RS, and an optical image of the object 100 is captured, for example, by a CCD camera 12'. If the setup of the devices 10, 20, 100 is ideally matched with respect to the light field and the X-ray field, the area of ​​the object 100 irradiated by the X-ray radiation RS precisely covers the interior of circle 112c. This can be identified from the digital image of the CCD camera 12' by the determined intensity values ​​of pixels IS1 of the image region corresponding to the interior of circle 112c. These determined intensity values ​​IS1 are compared with predetermined intensity values ​​IS of layer 114, which are preferably stored in a controller. If they match, at least the object 100 is correctly aligned with the digital camera. Illumination deviations of circle 112c, such as areas that are too large (greater than circle 112c) or too small (less than circle 112c), indicate a change in the distance between the focal point of the X-ray source 10 and the measuring stage 20. This error can be eliminated by adjusting the collimator K or the X-ray optics.

[0078] Alternatively or additionally, if the deviation does not disappear, the alignment and / or arrangement of the X-ray source 10 relative to the object being measured 100 can also be changed. For example, the distance between components 10, 20 and / or 100 can be changed by at least one drive device 21 until the area of ​​the object being measured 100 irradiated by the X-ray radiation RS completely covers the interior of the circle 112c.

[0079] The height and / or position of the X-ray source 10 can also be adjusted relative to the worktable 20 using an adjustment device.

[0080] The lateral displacement between components 10, 20, and 100 can also be analyzed based on the digital image from the CCD camera 12', and can be changed, reduced, or eliminated by the adjustment device of component 21 and / or X-ray source 10.

[0081] An error vector can be determined based on one or more digital images recorded by the CCD camera 12' or image data of the images, the error vector representing the alignment (e.g., angular alignment in one or more spatial directions, particularly misalignment) and / or arrangement (e.g., distance in one or more spatial directions) of the X-ray source 10 relative to the object being measured 100.

[0082] The alignment and / or arrangement of the X-ray source 10 relative to the object being measured 100 can be changed manually and / or automatically based on the error vector.

[0083] In other words, based on the digital image or an error vector that can be determined from the digital image, the display (or arrangement and / or alignment) of the optical crosshairs of the measuring device with the X-ray source 10 (e.g., for X-ray fluorescence) can now be corrected accordingly so that the user can take measurements at exactly the same points that are also displayed, for example, by means of the optical crosshairs.

[0084] Alternatively, a collimator diameter smaller or larger than the collimator diameter described above can also be used. The projection of the X-ray radiation RS onto the measurement object 100 associated with the collimator K can be determined using the intercept theorem. Deviations in projection size and / or position (e.g., arrangement and / or alignment) can also be evaluated using this deviation collimator diameter value, similar to the embodiments described above, for example, to determine the error vector of the crosshair (e.g., the optical crosshair of the measuring device containing the X-ray source 10) correction offset.

[0085] Preferably, the largest available collimator diameter is used, which can improve the accuracy of the measurement.

[0086] Other embodiments involve structures in which there is no image sensor or digital camera 12' but only a (photoelectric) detector 12. In these embodiments, the object to be measured 100 is positioned on the measuring stage 20 such that the crosshairs 112a, 112b of the object to be measured ( Figure 1 The center (intersection 112ab) of the object is irradiated by a target device (e.g., a laser pointer) that indicates the alignment of the X-ray source RS. The measurement begins from an assumed position, i.e., the position indicated by the laser pointer, whereby the object being measured 100 is thus exposed to X-ray radiation RS.

[0087] Preferably, the arrangement and / or alignment of the automated stages 20, 21 relative to the X-ray source 10 and the measurement object 100 are varied in the axial direction. This changes the area of ​​the measurement object 100 irradiated by the X-ray radiation RS, and therefore also changes the signal ES1 detected by the detector 12 due to the exposure of the measurement object 100 to the X-ray radiation RS, which is generated, for example, by a marker 112 in the form of a lead structure 112. When the illumination of the measurement object 100 is low, the signal strength of the signal ES1 decreases accordingly with the decrease of the X-ray radiation RS.

[0088] For example, the signal strength characterizing signal ES1 is determined for three different relative positions and / or arrangements of components 10 and 100 relative to each other, such as the count rate of detector 12. These three different relative positions and / or arrangements include an assumed center point (e.g., represented by the incident laser pointer signal at intersection 112ab), variations along a first spatial direction (e.g., X-variation), and variations along a second spatial direction (e.g., Y-variation). The X-axis corresponds to the width range B1 of the surface 100a of the object being measured, and the Y-axis corresponds to the height range H1 of the surface 100a of the object being measured.

[0089] Three count rates associated with three locations are related to the area of ​​the measurement object 100 theoretically irradiated by X-ray radiation RS, and a corresponding error vector is determined, according to which the alignment and / or arrangement can be changed until a predetermined alignment is actually achieved, which enables accurate measurement by X-ray radiation RS.

[0090] Accuracy can be significantly increased by including additional measurement points (in addition to the three measurement points mentioned above as examples).

[0091] Figure 9 Another exemplary method for calibrating an X-ray fluorescence device is described. The method includes: a) providing 401 a measurement object 100, for example, for X-ray fluorescence analysis; b) enabling 402 an X-ray source 10 to be effectively and / or precisely aligned and / or positioned relative to the measurement object 100, and / or vice versa; c) ensuring 403 that a light field that can be optically detected by a camera (e.g., a digital camera) corresponds to an area (“X-ray field”) that can be exposed to X-ray radiation from the X-ray source, such as components like collimators (K), filters, and apertures present independently of the beam path of the X-ray radiation; d) checking 404 the alignment and / or positioning of the X-ray source relative to the measurement object 100; e) assisting 405 the user in aligning and / or positioning the X-ray source 10 relative to the measurement object, and / or vice versa; f) selecting 406a a collimator and / or another field-shaping element for positioning in the beam path of the X-ray radiation; and g) correcting 407 the alignment and / or positioning of the X-ray source 10 relative to the measurement object 100.

Claims

1. A measurement object (100) for calibrating an X-ray fluorescence device (9), the X-ray fluorescence device (9) emitting X-ray radiation (RS) through an X-ray source (10), and the X-ray fluorescence device (9) including a detector for evaluating X-ray fluorescence, the measurement object having a body (110) and at least one mark (112) disposed on the body (110), wherein, The body (110) is formed of a first material (M-1), the mark (112) on and / or within the body (110) is formed of a second material (M-2) different from the first material (M-1), and the first material (M-1) emits a relatively low X-ray fluorescence emission when exposed to the X-ray radiation (RS) compared to the second material (M-2), and the body (110) has a layer (114) in at least some regions, the layer (114) being aligned with the mark (112), wherein: The layer (114) emits electromagnetic radiation (ES1) at a predetermined intensity (IS) within a predetermined wavelength range (WLB) when exposed to the X-ray radiation (RS), the predetermined wavelength range (WLB) being between 300 nm and 1100 nm; and The marker (112) emits X-ray fluorescence radiation (ES2) at a predetermined intensity (IRf) when exposed to the X-ray radiation (RS).

2. The measuring object (100) according to claim 1, wherein, The layer (114) and the marker (112) can be exposed to the X-ray radiation (RS) at least partially at the same time.

3. The measuring object (100) according to claim 1, wherein, The second material (M-2) is a heavy metal, and / or the first material (M-1) is not a heavy metal.

4. The measuring object (100) according to claim 1, wherein, The centroid (FS) of the layer (114) and the centroid (FM) of the marker (112) are the same.

5. The measuring object (100) according to claim 1, wherein, The layer (114) has a fluorescent coating, or the layer (114) is a fluorescent coating.

6. The measuring object (100) according to claim 1, wherein, The mark (112) has at least two intersecting lines (112a, 112b) that are orthogonally aligned with each other.

7. The measuring object (100) according to claim 6, wherein, The mark (112) has at least one circle (112c), and the circle (112c) is arranged concentrically with the intersection point (112ab) of the at least two intersecting lines (112a, 112b), and the layer (114) extends over the entire area within the circle (112c).

8. The measuring object (100) according to claim 1, wherein, The body (110) has a sheet-like shape, and / or the thickness (D1) of the body (110) is less than at least one external dimension of the body (110) in the direction perpendicular to the thickness (D1).

9. A method for verifying the calibration of an X-ray fluorescence apparatus (9), the X-ray fluorescence apparatus (9) comprising an X-ray source (10) emitting X-ray radiation (RS), at least one collimator (K) or X-ray optics for focusing the X-ray radiation (RS), and a first detector (12) and a second detector (12') for evaluating the X-ray fluorescence radiation emitted by a measurement object (100) exposed to the X-ray radiation (RS), the method comprising: The measurement object (100) according to claim 1 is exposed (202) to the X-ray radiation (RS) at least temporarily; For the predetermined wavelength range (WLB) of the layer (114), the second detector (12') is used to detect (204) a first quantity (G1) of the intensity (IS1) of the electromagnetic radiation (ES1) of the layer (114) of the measurement object (100); and / or The first amount (G2) of the intensity (IRf1) of the X-ray fluorescence radiation (ES2) from the mark (112) of the measured object (100) is detected (204) using the first detector (12). Determine the match or first difference (DS) between the detected intensity (IS1) of the first quantity (G1) of the layer (114) and the predetermined intensity (IS) of the layer (114); and / or Determine a match or a second difference (DM) between the detected intensity (IRf1) of a first quantity (G2) of the mark (112) and the predetermined intensity (IRf) of the mark (112). and When at least one of the first difference (DS) and the second difference (DM) is determined, misalignment of the measurement object (100) is detected, or readjustment of the first detector (12) and the second detector (12'), the at least one collimator (K), or the X-ray source (10) of the X-ray optics and / or the X-ray fluorescence device (9).

10. The method according to claim 9, wherein: When the detected intensity (IS1) of the layer (114) matches the predetermined intensity (IS) of the layer (114) within permissible limits, and when the second difference (DM) exists, it is determined that the X-ray source (10), the at least one collimator (K) or the X-ray optics and / or the first detector (12) for detecting the X-ray fluorescence radiation is misaligned, and the second detector (12') for detecting the electromagnetic radiation in the predetermined wavelength range (WLB) is calibrated; or When the intensity (IRf1) of the detected mark (112) matches the predetermined intensity (IRf) of the mark (112) within permissible limits, and when the first difference (DS) exists, it is determined that the X-ray source (10), the at least one collimator (K), or the X-ray optics and / or the first detector (12) for detecting the X-ray fluorescence radiation is calibrated, and the second detector (12') for detecting the electromagnetic radiation (ES1) within the predetermined wavelength range (WLB) is misaligned.

11. The method according to claim 9, wherein: When the first difference (DS) and the second difference (DM) are determined in the first step, the measurement object (100) is moved on the measurement stage (20) and adjusted relative to the second detector (12'), and when the predetermined intensity (IS) of the layer (114) is detected to match the detected intensity (IS1) of the layer (114), a matching or second difference (DM) detection is performed on the intensity of the mark (112); or When the first difference (DS) and the second difference (DM) are determined, in a first step, the measurement object (100) is adjusted on the measurement stage (20) of the X-ray fluorescence apparatus (9) relative to the second detector (12') for detecting the electromagnetic radiation (ES1) within the predetermined wavelength range (WLB), and when the first difference (DS) is further determined, the readjustment of the detection of the electromagnetic radiation (ES1) by the second detector (12') for the predetermined wavelength range (WLB) is determined.

12. The method according to claim 9, wherein: The measuring stage (20) of the X-ray fluorescence device (9) is moved outside the area of ​​the X-ray radiation (RS); The object to be measured (100) is aligned on the measuring stage (20) by a visible beam device (18), and the visible beam device (18) is arranged adjacent to the X-ray source (10); The measuring stage (20) is moved back into the area of ​​the X-ray radiation (RS); The matching or determination of the first difference (DS) of the layer (114) and / or the matching or determination of the second difference (DM) of the tag (112) are performed; as well as When the first difference (DS) is determined, the readjustment of the second detector (12') used to detect the electromagnetic radiation (ES1) within the predetermined wavelength range (WLB) is detected, or when the second difference (DM) is determined, the readjustment of the visible beam device (18) is detected.

13. The method according to claim 9, wherein, Before the at least temporary exposure (202) to the X-ray radiation (RS), the alignment (200) of the X-ray source (10) with the object being measured (100) is performed, and / or vice versa, wherein manual alignment (200a) is output via a representation in the display of the X-ray fluorescence device (9), or automatic alignment (200b) is initiated by the controller of the X-ray fluorescence device (9).

14. The method according to claim 9, wherein, Starting from the first amount (G1) of the intensity (IS1) of the electromagnetic radiation (ES1) and the first amount (G2) of the intensity (IRf1) of the X-ray fluorescence radiation (ES2), the method further includes: Change (210) the arrangement and / or alignment of the measurement object (100) relative to the X-ray source (10); Repeat (212) the detection (204) of the at least temporary exposure (202) of the measurement object (100) to the X-ray radiation (RS) and the electromagnetic radiation (ES1', ES2') emitted by at least one component of the measurement object (100) due to the exposure (202) of the measurement object (100) to the X-ray radiation (RS); and (214) The change (G1', G2') of the first quantity (G1, G2) is determined based on the detected electromagnetic radiation (ES1', ES2').

15. The method according to claim 14, wherein, Based on the changes (G1', G2') of the first quantities (G1, G2), the arrangement and / or alignment of the measurement object (100) relative to the X-ray source (10) are changed again (216).

16. The method of claim 14, further comprising: Determine (220) a plurality of values ​​(ES-W-1, ES-W-2, ES-W-3), the plurality of values ​​characterizing electromagnetic radiation (ES1', ES2') emitted by at least one component of the measured object (100) due to the measured object (100) being exposed (202) to the X-ray radiation (RS), wherein each of at least two of the plurality of values ​​(ES-W-1, ES-W-2, ES-W-3) is associated with a different arrangement and / or alignment of the measured object (100) relative to the X-ray source (10); and Based on at least two of the plurality of values ​​(ES-W-1, ES-W-2, ES-W-3), determine (222) the alignment and / or arrangement of the X-ray source (10) relative to information (I-AUSR), which characterizes the measurement object (100) by at least one vector.

17. The method according to claim 9, wherein: The first quantity (G1) of the electromagnetic radiation (ES1) of the layer (114) is detected by the layer (114) through multiple digital images (DB-1, DB-2, DB-3) of the measurement object (100); as well as The method further includes: Determine (240) a plurality of digital images (DB-1, DB-2, DB-3), each of which has a different arrangement and / or alignment of the measured object (100) relative to the X-ray source (10); and Information (I-AUSR') characterizing the misalignment and / or arrangement of the X-ray source (10) relative to the measurement object (100) is determined (242) by at least two of the plurality of digital images (DB-1, DB-2, DB-3) using at least one vector.

18. The method of claim 16, further comprising: Information (I-AUSR; I-AUSR') characterizing the alignment and / or arrangement of the X-ray source (10) relative to the measurement object (100) is sent (224a; 244a) to at least one drive unit (11; 21) to change the arrangement and / or alignment of the measurement object (100) relative to the X-ray source (10); and / or Information (I-AUSR; I-AUSR') characterizing the alignment and / or arrangement of the X-ray source (10) relative to the measurement object (100) is communicated to the user (224b; 244b).

19. The method of claim 9, further comprising: a) Provide (401) the measurement object (100) for X-ray fluorescence analysis; b) To enable the X-ray source (10) to be aligned and / or arranged (402) relative to the object being measured (100), and / or vice versa; c) Ensure that (403) the field of view that can be detected by camera optics corresponds to the area exposed to the X-ray radiation (RS) from the X-ray source (10), the X-ray radiation (RS) being independent of the components present in the beam path of the X-ray radiation (RS); d) Inspect (404) the alignment and / or arrangement of the X-ray source (10) relative to the object being measured (100); e) Assist (405) the user in aligning and / or positioning the X-ray source (10) relative to the object being measured (100), and / or vice versa; f) Select (406) collimator (K) and / or another field shaping element for arrangement in the beam path of the X-ray radiation (RS); and g) Correct (407) the alignment and / or arrangement of the X-ray source (10) relative to the object being measured (100).

Images