X-ray diffraction testing device
By innovatively combining zero-dimensional and two-dimensional detectors in a combined X-ray detector, the problems of high cost and low direct light utilization in large-area two-dimensional X-ray diffractometers have been solved, achieving low-cost and high-precision diffraction testing.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-04
- Publication Date
- 2026-03-10
AI Technical Summary
Existing large-area two-dimensional X-ray diffractometers are expensive and have low direct light utilization, and require multi-position imaging followed by image processing to eliminate detector gap interference.
A combined X-ray detector is used, including a rotating stage, a zero-dimensional detector, and multiple two-dimensional detectors. The zero-dimensional detector is located in the center and is coaxial with the rotation axis to receive direct light. The two-dimensional detectors are stitched together in the same plane to form a whole pattern. The rotating stage enables multi-position imaging and image processing to eliminate gap interference. The zero-dimensional detector is used to monitor changes in direct light to improve testing accuracy.
It achieves low-cost, large-area diffraction testing, overcoming the high cost and low direct light utilization of traditional two-dimensional X-ray diffractometers. It obtains complete diffraction patterns through multi-position photography and image processing, thereby improving testing accuracy.
Smart Images
Figure CN121633153A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the field of X-ray diffraction technology, in particular to an X-ray diffraction testing device. BACKGROUND
[0002] X-ray diffraction analysis is a technique for analyzing the structure of a substance using the diffraction effect of X-rays in crystalline substances, which is widely used in scientific research, medical treatment and enterprise production, and its commonly used equipment includes an X-ray diffractometer. Currently, a two-dimensional X-ray diffractometer is commonly used for structural analysis of oriented or textured samples. As can be seen from the analysis of a common two-dimensional X-ray diffraction pattern, for a non-oriented sample such as a well-dispersed powder sample, the diffraction pattern will present multiple concentric circles (i.e. Debye rings), such as the diffraction pattern of a corundum powder sample shown in FIG. 1; for an oriented sample, the diffraction pattern will change from rings to points and / or arcs, and the orientation or texture of the sample can be analyzed according to the distribution of the points and / or arcs. In general, the direction of the diffraction points and / or arcs of an oriented sample is the same as or perpendicular to the direction of the stretching, shearing and other actions that cause the orientation, i.e. when the sample is placed facing the X-rays, these diffraction points and / or arcs will appear in the vertical or horizontal direction (i.e. the meridian direction or the equatorial direction) of the two-dimensional diffraction pattern, such as the diffraction pattern of a polyester fiber sample shown in FIG. 2. Figure 1 Figure 2
[0003] The two-dimensional detector inside the two-dimensional X-ray diffractometer has the characteristic that the larger the area, the more expensive the price, because a large-area two-dimensional detector is composed of multiple small sub-detectors densely spliced together, and the process is relatively complex, and the signal output and yield are limited. The two-dimensional detector includes a CCD detector, a gas ionization detector and a semiconductor detector, among which the semiconductor detector becomes the mainstream due to its high sensitivity, high signal-to-noise ratio and mature technology. Taking a two-dimensional semiconductor detector as an example, the cost of a two-dimensional semiconductor detector with a pixel size of about 100 um and 60-80K pixels has been reduced to 30-40 thousand yuan, but a two-dimensional semiconductor detector with 200-500K pixels still costs 30-50 thousand yuan, and a larger two-dimensional semiconductor detector can only be made by splicing more two-dimensional semiconductor detectors with 200-500K pixels, and the price will be more expensive. In addition, there are still several pixel-sized gaps between the small sub-detectors in the large-area two-dimensional detector, and when a diffraction point and / or arc falls into these gaps during testing, multiple position photographs need to be taken to obtain multiple pictures, which need to be spliced, fused and processed to obtain a complete diffraction pattern.
[0004] Therefore, the large-area two-dimensional X-ray diffractometer in the prior art is high in cost, and still needs to eliminate the interference of the gaps in the detector by image processing after multiple position photography. SUMMARY
[0005] In order to overcome the above-mentioned deficiencies of the prior art, the present application provides a novel X-ray diffraction testing device, which can realize large-area diffraction testing function at a cost much lower than that of a large-area two-dimensional X-ray diffractometer, and overcome the inherent defect of low utilization rate of direct light of a conventional two-dimensional X-ray diffractometer.
[0006] To achieve the above-mentioned purposes, the technical scheme adopted by the present application to solve its technical problems is that the X-ray diffraction testing device comprises:
[0007] The combined X-ray detector is used for receiving X-rays and outputting digital images, and comprises a rotating table, a zero-dimensional detector and a plurality of two-dimensional detectors arranged on the rotating table, the plurality of two-dimensional detectors are used for receiving diffraction light and spliced into an integral pattern in the same plane, and the zero-dimensional detector is used for receiving direct light and arranged coaxially with the rotating shaft of the rotating table in the center of the integral pattern.
[0008] In some embodiments, the zero-dimensional detector is a CCD detector, a gas ionization detector or a semiconductor detector.
[0009] In some embodiments, the two-dimensional detector is a CCD detector, a gas ionization detector or a semiconductor detector.
[0010] In some embodiments, the integral pattern is a rectangle.
[0011] In some embodiments, the plurality of two-dimensional detectors are of the same size and shape.
[0012] In some embodiments, the rotating table comprises a carrier, and the carrier comprises a limiting groove for limiting installation of the two-dimensional detectors.
[0013] In some embodiments, the zero-dimensional detector is installed in a gap formed by arrangement of the plurality of two-dimensional detectors.
[0014] In some embodiments, the X-ray diffraction testing device further comprises:
[0015] The X-ray source is used for providing X-rays required for testing;
[0016] The sample table comprises a sample carrier for fixing a sample;
[0017] The host computer is connected to the combined X-ray detector, and is used for receiving, processing and displaying digital images output by the combined X-ray detector.
[0018] In some embodiments, the X-ray source, the sample carrier and the zero-dimensional detector are located on the same straight line.
[0019] In some embodiments, the host computer is connected to and controls the X-ray source.
[0020] By means of the technical scheme, the present application has the following advantages over the prior art:
[0021] The present application is contrary to the conventional technical concept of increasing the number of pixels of a single two-dimensional detector, and instead, according to the regularity of a common two-dimensional X-ray diffraction pattern, covers the main features of the diffraction pattern of a sample oriented in the meridian direction and the equatorial direction by combining multiple two-dimensional detectors for receiving diffraction light arranged regularly and separated from each other, so that the function of large-area diffraction testing can be realized at a cost much lower than that of a large-area two-dimensional X-ray diffractometer, although the gaps formed between the multiple two-dimensional detectors are much larger than the gaps between small sub-detectors in a single large-area two-dimensional detector, when a diffraction point and / or an arc falls into these larger gaps, the interference of the gaps can still be eliminated by multi-position photography and image processing, so that a complete diffraction pattern is obtained, and a rotating table is arranged to carry and rotate the two-dimensional detector;
[0022] In addition, since the intensity of the diffraction light generated after the X-ray irradiates the sample is generally only one ten-thousandth of the incident light or even less, and the maximum detectable light intensity of the two-dimensional detector is generally less than the light intensity of the X-ray source, the two-dimensional detector in the prior art is usually provided with a direct light blocking element to block direct light to protect the detector itself, and the combined X-ray detector in the present application further includes a zero-dimensional detector located at the center of the multiple two-dimensional detectors and the rotating shaft of the rotating table for receiving direct light, which not only replaces the direct light blocking element to play a protective role, but also effectively utilizes the direct light, senses the change of the intensity of the direct light, and conveniently judges whether the sample is cut into the light path to guide the sample to be quickly adjusted in place, and can also monitor the fluctuation of the light source during the testing process and correct the error to improve the testing accuracy, overcoming the inherent defect of the traditional two-dimensional X-ray diffractometer that the utilization rate of direct light is not high. BRIEF DESCRIPTION OF DRAWINGS
[0023] Figure 1 A two-dimensional X-ray diffraction pattern of a corundum powder sample.
[0024] Figure 2 A two-dimensional X-ray diffraction pattern of a polyester fiber sample.
[0025] Figure 3 A structural schematic diagram of an embodiment one of the X-ray diffraction testing device proposed by the present application.
[0026] Figure 4 A perspective view of the combined X-ray detector in the embodiment one of the X-ray diffraction testing device proposed by the present application.
[0027] Figure 5 A front view of the zero-dimensional detector and the four two-dimensional detectors in the combined X-ray detector in the embodiment one of the X-ray diffraction testing device proposed by the present application.
[0028] Figure 6 This is a schematic diagram showing the connection relationship of some components in Embodiment 1 of the X-ray diffraction testing device proposed in this invention.
[0029] Figure 7 This is a flowchart illustrating the operation of an embodiment of the X-ray diffraction testing device proposed in this invention.
[0030] Figure 8 This is a schematic diagram illustrating the principle of obtaining an incomplete diffraction pattern in the first test of the X-ray diffraction testing device proposed in this invention, used for X-ray diffraction testing of polyester fiber samples.
[0031] Figure 9 This is a schematic diagram illustrating the principle of obtaining a complete diffraction pattern through two tests when using the X-ray diffraction testing device proposed in this invention for X-ray diffraction testing of polyester fiber samples.
[0032] In the figure: 1. Combined X-ray detector; 11. Rotary stage; 111. Carrier; 1111. Baffle; 1112. Limiting groove; 112. Rotation drive device; 12. Zero-dimensional detector; 13. Two-dimensional detector; 131. Receiving panel; 132. Outer frame; 2. X-ray source; 3. Sample stage; 31. Sample carrier; 4. Main unit; 41. Display screen. Detailed Implementation
[0033] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.
[0034] Combination Figures 3 to 6 The first embodiment of the X-ray diffraction testing device proposed in this invention includes:
[0035] A combined X-ray detector 1 is used to receive X-rays and output digital images. It includes a rotating stage 11, a zero-dimensional detector 12, and four two-dimensional detectors 13 mounted on the rotating stage 11. The zero-dimensional detector 12 is a semiconductor detector that receives light at a single point. The four two-dimensional detectors 13 are all semiconductor detectors of the same size and shape, with their receiving panels 131 and end faces being square. The four two-dimensional detectors 13 are used to receive diffracted light and are assembled into a large square in the same plane. The zero-dimensional detector 12 receives direct light and is located in the center of the large square, coaxially with the rotation axis of the rotating stage 11. A carrier 111 is provided on the upper part of the rotating stage 11. The unit is equipped with a rotary drive device 112, and the carrier 111 is rotatably connected to the rotary drive device 112. The carrier 111 is surrounded by baffles 1111 forming a square limiting groove 1112. Four two-dimensional detectors 13 are respectively attached to the four end corners of the limiting groove 1112. The zero-dimensional detector 12 is located in the gap formed by the arrangement of the four two-dimensional detectors 13. The zero-dimensional detector 12 and the four two-dimensional detectors 13 are all connected and fixed to the carrier 111 by bolts. The rotary drive device 112 is used to drive the carrier 111 to rotate and can accurately control and record the rotation angle. It includes a motor, a reducer, a motor encoder and a motor controller. Since it belongs to the prior art, its connection relationship and working principle will not be described in detail.
[0036] X-ray source 2, which provides the X-rays required for the test, is specifically a multi-capillary microfocus X-ray source;
[0037] The sample stage 3 includes a sample carrier 31, which is used to fix the sample. During the test in Example 1, the X-ray source 2, the sample carrier 31, and the zero-dimensional detector 12 are always located on the same straight line.
[0038] The host computer 4 specifically includes a computer with a display screen 41. The host computer 4 is connected to the combined X-ray detector 1 and is used to receive, process, and display the digital images output by the combined X-ray detector 1. Specifically, the host computer 4 is simultaneously connected to the zero-dimensional detector 12, four two-dimensional detectors 13, and the rotation drive device 112. The host computer 4 simultaneously receives and processes the direct light digital images output by the zero-dimensional detector 12 and the diffraction light digital images output by the two-dimensional detectors 13, and acquires and controls the motion state and rotation angle of the rotating stage 11. The host computer 4 is also connected to and controls the X-ray source 2. The host computer 4 is equipped with a computer operating system, which is installed with the diffraction pattern processing and analysis software specifically designed for Embodiment 1. This software has intelligent and automated features. It achieves integrated control of the X-ray source 2, the combined X-ray detector 1, and the host computer 4 itself. Through a human-computer interaction interface, users can perform test and analysis operations through traditional keyboard and mouse, screen touch, or other control methods. It has functions such as sample arrival judgment, light source fluctuation monitoring and error correction, image processing, and online analysis. Finally, it outputs diffraction patterns and analysis results to complete the material structure analysis or characterization of a specific property of the sample.
[0039] like Figure 7 As shown, the workflow of Example 1 is as follows:
[0040] S1: Fix the sample onto the sample carrier 31, adjust the sample position, and turn on the X-ray source 2 and the main unit 4;
[0041] S2: The host 4, i.e., the diffraction pattern processing and analysis software, determines whether the sample is in place based on the light intensity of the X-ray source 2 and the light intensity of the direct light received by the zero-dimensional detector 12. If the difference between the two light intensities is less than the preset threshold, the host 4 determines that the sample is not in place and issues an alarm, prompting the user to readjust the sample position. The test can only begin when the host 4 determines that the sample is in place. If the difference between the two light intensities is greater than the preset threshold, the host 4 determines that the sample is in place and prompts the user to start the test.
[0042] S3: X-rays emitted from X-ray source 2 diffract after passing through the sample, and the diffracted light is received by four two-dimensional detectors 13 and output as digital images to host 4. Host 4 processes the digital images and displays the diffraction pattern on display screen 41. The user observes the diffraction pattern and judges whether the pattern features are complete and meet the test requirements based on the known sample information and diffraction imaging rules. If so, the user operates host 4 to output the complete diffraction pattern and its analysis results obtained by the completion processing based on the diffraction pattern. If not, the user can control the carrier 111 to rotate by a specified angle once or multiple times through host 4 to obtain one or more new diffraction patterns. Finally, host 4 splices and fuses all the diffraction patterns to obtain the complete diffraction pattern. The user then performs relevant operations according to the test requirements and outputs the analysis results.
[0043] When Example 1 was used for X-ray diffraction testing of polyester fiber samples, the first time, as... Figure 8 When the four two-dimensional detectors 13 are arranged to form a large square, with the two diagonals aligned vertically and horizontally, the pair of two-dimensional detectors 13 located at the top and right cover the diffraction points and / or arcs in the vertical and horizontal directions. Although the resulting diffraction pattern is incomplete, the complete pattern features are sufficient to meet the testing and analysis requirements. The second time, as... Figure 9 The four two-dimensional detectors 13 are rotated 45° clockwise or counterclockwise to form a large square with two adjacent sides in the vertical and horizontal directions, respectively, resulting in a new incomplete diffraction pattern. The two diffraction patterns are then simply stacked to synthesize a complete diffraction pattern. The imaging part corresponding to the receiving panel 131 of the two-dimensional detector 13 and the unimaging part corresponding to the gap between the two-dimensional detectors 13 complement each other in the two incomplete diffraction patterns.
[0044] In other embodiments of the present invention:
[0045] The types of detectors used for both the zero-dimensional detector 12 and the two-dimensional detector 13 are not limited. Preferably, the zero-dimensional detector 12 is a CCD detector, a gas ionization detector, or a semiconductor detector, and the two-dimensional detector 13 is a CCD detector, a gas ionization detector, or a semiconductor detector.
[0046] The number of two-dimensional detectors 13 is no less than two, thus enabling the integration of small and large components;
[0047] The size and shape of a single two-dimensional detector 13, as well as the overall pattern formed by multiple two-dimensional detectors 13, are not limited, as long as a complete diffraction pattern can be obtained by rotating multiple two-dimensional detectors 13 and processing the image after multi-position photography. However, preferably, the multiple two-dimensional detectors 13 are the same size and shape, and both the single two-dimensional detector 13 and the overall pattern formed by multiple two-dimensional detectors 13 are rectangular. For example, in Embodiment 1, the single two-dimensional detector 13 and the overall pattern formed by multiple two-dimensional detectors 13 are both squares, and a square is also a type of rectangle. This is because the receiving panel 131 and the outer contour of the end face of the conventional commercially available two-dimensional detector 13 are all rectangular, and the rectangular shape of the single detector and the overall pattern can reduce the number of rotation photographys, make the rotation angle value fixed and easy to adjust, and facilitate uniform image processing and regular output. Of course, the two-dimensional detector 13 can also be customized to obtain a non-rectangular or even irregularly shaped receiving panel 131 and outer contour of the end face, such as a rhombus. Four rhombus-shaped two-dimensional detectors 13 of the same size can be spliced into a large rhombus.
[0048] Preferably, a rotatable and fixed carrier 111 is provided on the rotating stage 11 to load the zero-dimensional detector 12 and the two-dimensional detector 13. More preferably, a limiting groove 1112 matching the shape of the two-dimensional detector 13 is provided on the carrier 111 to limit the installation of the two-dimensional detector 13. This not only makes installation convenient but also ensures the shape accuracy of the overall graphic obtained by splicing. In the first embodiment, a baffle 1111 is used to form a large square limiting groove 1112. Multiple small square two-dimensional detectors 13 are limited by the four corners of a single large square limiting groove 1112. In addition, the limiting groove 1112 and the two-dimensional detector 13 can be matched one-to-one to achieve the limiting installation.
[0049] Since the outer contour of the end face of the conventional commercially available two-dimensional detector 13 and the receiving panel 131 are both rectangular, and the receiving panel 131 is surrounded by a rectangular outer frame 132, even if two two-dimensional detectors 13 are tightly attached to one side, a large gap is still formed at the attachment point of the pair of receiving panels 131. Therefore, it is preferable that multiple two-dimensional detectors 13 are arranged at intervals, and the zero-dimensional detector 12 is installed in the gap formed by the arrangement of multiple two-dimensional detectors 13. The zero-dimensional detector 12 and multiple two-dimensional detectors 13 are all fixedly installed on the rotating table 11. If multiple two-dimensional detectors 13 are coplanarly and tightly spliced, the zero-dimensional detector 12 can only be installed and fixed on the surface of multiple two-dimensional detectors 13, which increases the difficulty of production and assembly.
[0050] The X-ray source 2, sample carrier 31, and zero-dimensional detector 12 are always located on the same straight line during the test. Specifically, the X-ray source 2, sample, and zero-dimensional detector 12 are always located on the same straight line, and the direction of the line is not limited. When the line is horizontal, the sample carrier 31 can be a glass slide holder. In addition, the sample stage 3 generally includes a detachable fixing mechanism for replacing the sample carrier 31 and a displacement mechanism for adjusting the position of the sample carrier 31.
[0051] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these modifications and improvements all fall within the scope of protection of the present invention. Therefore, the scope of protection of this patent should be determined by the appended claims.
Claims
1. An X-ray diffraction testing device, characterized by Comprise: A combined X-ray detector (1) for receiving X-rays and outputting digital images, comprising a rotating table (11) and a zero-dimensional detector (12) and a plurality of two-dimensional detectors (13) arranged on the rotating table (11), the plurality of two-dimensional detectors (13) being used for receiving diffraction light and being spliced into an integral pattern in the same plane, and the zero-dimensional detector (12) being used for receiving direct light and being arranged coaxially with the rotating shaft of the rotating table (11) in the center of the integral pattern.
2. The X-ray diffraction testing device of claim 1, wherein, The zero-dimensional detector (12) is a CCD detector, a gas ionization detector or a semiconductor detector.
3. The X-ray diffraction testing device of claim 1, wherein, The two-dimensional detector (13) is a CCD detector, a gas ionization detector or a semiconductor detector.
4. The X-ray diffraction testing device of claim 1, wherein, The integral pattern is a rectangle.
5. The X-ray diffraction testing device of claim 1, wherein, The plurality of two-dimensional detectors (13) are the same in size and shape.
6. The X-ray diffraction testing device of claim 1, wherein, The rotating table (11) comprises a carrier (111) comprising a limiting groove (1112) for limiting the installation of the two-dimensional detector (13).
7. The X-ray diffraction testing device of claim 1, wherein, The zero-dimensional detector (12) is installed in the gap formed by the arrangement of the plurality of two-dimensional detectors (13).
8. The X-ray diffraction testing device of claim 1, wherein, Also comprise: An X-ray source (2) for providing X-rays required for testing; A sample table (3) comprising a sample carrier (31) for fixing a sample; A host computer (4) connected to the combined X-ray detector (1) for receiving, processing and displaying the digital images output by the combined X-ray detector (1).
9. The X-ray diffraction testing device of claim 8, wherein, The X-ray source (2), the sample carrier (31) and the zero-dimensional detector (12) are located on the same straight line.
10. The X-ray diffraction testing device of claim 8, wherein, The host computer (4) is connected to and controls the X-ray source (2).