Short-wavelength characteristic X-ray diffraction device and test method

Abstract

The invention discloses a short-wavelength characteristic X-ray diffraction device and a test method, which are applied to the technical field of X-rays, an incident collimator is positioned between an X-ray source and a sample table so as to irradiate short-wavelength characteristic X-rays to the circle center of a diffractometer circle; the receiving focusing collimator is located on the other side, opposite to the incident collimator, of the sample table, and the light incident side of the receiving focusing collimator points to the center of the circle of the diffractometer; the small array detector is located on the light emitting side of the receiving focusing collimator so as to obtain diffraction original data through exposure of the receiving focusing collimator; part of data of the diffraction Debye ring can be obtained through single exposure of the small array detector, and the width of an image corresponding to the obtained diffraction original data is 2 times to 4 times of the diffraction peak of a single diffraction crystal face. After a specific diffraction peak theoretical angle is selected, all information of a diffraction peak of a diffraction crystal face can be obtained through one-time exposure, so that internal diffraction information testing can be rapidly carried out.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of short wavelength characteristic X-ray technology, in particular to a short wavelength characteristic X-ray diffraction device and a testing method. BACKGROUND

[0002] The short wavelength characteristic X-ray diffraction technology can non-destructively detect the internal residual stress, texture and phase of a material workpiece by using an X-ray tube as a radiation source. For example, the short wavelength characteristic X-ray diffraction technology can non-destructively detect and analyze the internal residual stress, texture, phase and orientation of a crystal material such as steel, aluminum alloy, titanium alloy and ceramic.

[0003] The short wavelength characteristic X-ray diffraction technology uses strong penetrating characteristic X-rays (such as WKα, AuKα, AgKα, UKα and WKβ) emitted by a heavy metal target X-ray tube to penetrate materials such as aluminum alloy with a thickness of centimeters. In combination with a slit and a collimator, the short wavelength characteristic X-ray diffraction technology can realize the testing and analysis of internal diffraction information in a fixed position and direction by a small laboratory instrument, and is used for non-destructive determination of stress, phase, texture and single crystal orientation.

[0004] The short wavelength characteristic X-ray diffraction technology has the problem of low efficiency in scanning and testing diffraction spectra by a single point detector. The so-called single point detector scanning is to use a single point detector to step scan for internal diffraction information testing. This method has low testing efficiency. Therefore, how to provide a high-efficiency short wavelength characteristic X-ray diffraction device is a problem to be solved by those skilled in the art. SUMMARY

[0005] The purpose of the present application is to provide a short wavelength characteristic X-ray diffraction device which can quickly test internal diffraction information. Another purpose of the present application is to provide a testing method which can quickly test internal diffraction information.

[0006] To solve the above technical problems, the present application provides a short wavelength characteristic X-ray diffraction device, comprising an X-ray source, an incident collimator, a sample stage, a receiving and focusing collimator and a small array detector. The sample stage is used to fix the measured part of the sample at the center of the diffractometer circle, the X-ray source is used to emit short wavelength characteristic X-rays, and the incident collimator is located between the X-ray source and the sample stage to irradiate the short wavelength characteristic X-rays to the center of the diffractometer circle. The receiving and focusing collimator is located on the other side of the sample stage relative to the incident collimator, and the light entrance side of the receiving and focusing collimator is directed to the center of the diffractometer circle. The small array detector is located on the light exit side of the receiving focusing collimator to obtain diffraction raw data by exposure of the receiving focusing collimator; the single exposure of the small array detector is used to obtain a partial diffraction Debye ring, and the obtained diffraction raw data correspond to an image with a width of 2-4 times the peak width of a diffraction peak of a diffraction crystal face.

[0007] Optionally, the receiving focusing collimator is a single-channel receiving focusing collimator, and the extensions of the two inner sides of the single-channel receiving focusing collimator are focused on the center of the diffractometer circle.

[0008] Optionally, the receiving focusing collimator and the small array detector are fixedly connected with a goniometer, and the goniometer is used to drive the receiving focusing collimator and the small array detector to rotate around the center of the goniometer circle.

[0009] Optionally, the receiving focusing collimator and the small array detector are arranged on an arc-shaped track, and the goniometer is used to drive the receiving focusing collimator and the small array detector to move along the arc-shaped track, and the arc-shaped track is concentric with the center of the goniometer circle.

[0010] Optionally, the small array detector is a linear array detector, and the pixel size of the linear array detector along the rotation direction of the goniometer ranges from 0.01 mm to 0.2 mm, and the pixel size of the linear array detector perpendicular to the rotation direction of the goniometer ranges from 5 mm to 30 mm. Alternatively, the small array detector is a pixel array detector, and the pixel size of the pixel array detector along the rotation direction of the goniometer ranges from 0.01 mm to 0.2 mm, and the pixel size of the pixel array detector perpendicular to the rotation direction of the goniometer ranges from 0.01 mm to 0.2 mm.

[0011] Optionally, the size of the detection area of the small array detector ranges from 4 mm to 50 mm along the scanning direction, and ranges from 10 mm to 50 mm perpendicular to the scanning direction.

[0012] Optionally, the light passing section of the incident collimator is rectangular, the light exit of the incident collimator is provided with an adjusting track extending perpendicular to the scanning direction, the adjusting track is provided with an adjusting block, and the adjusting block moves along the adjusting track.

[0013] The application further discloses a testing method, which applies the short-wavelength characteristic X-ray diffraction device. The sample is fixed on the center of the diffractometer circle through the sample table; The short-wavelength characteristic X-ray is emitted to the sample through the X-ray source, and the small array detector is exposed at a preset angle to obtain diffraction raw data. processing the diffraction raw data to obtain diffraction peaks of single diffraction crystal face, and analyzing based on the diffraction peaks.

[0014] Optionally, the method further comprises: stepping the small array detector and the receiving focusing collimator, and performing, after each step, the step of exposing at a preset angle by the small array detector to obtain diffraction raw data, to obtain diffraction raw data corresponding to multiple diffraction crystal faces; processing the diffraction raw data to obtain diffraction peaks of single diffraction crystal face, and analyzing based on the diffraction peaks. accumulating the diffraction raw data obtained in each exposure as exposure data of a diffraction angle corresponding to the center of the small array detector in the exposure; processing the diffraction raw data to obtain diffraction peaks of single diffraction crystal face, and analyzing based on the diffraction peaks.

[0015] Optionally, the method further comprises: stepping the small array detector and the receiving focusing collimator, and performing, after each step, the step of exposing at a preset angle by the small array detector to obtain diffraction raw data, to obtain diffraction raw data corresponding to multiple diffraction crystal faces; processing the diffraction raw data to obtain diffraction peaks of single diffraction crystal face, and analyzing based on the diffraction peaks. processing the diffraction raw data to obtain diffraction peaks of single diffraction crystal face, and analyzing based on the diffraction peaks.

[0016] The short-wavelength characteristic X-ray diffraction device provided by the application comprises an X-ray source, an incident collimator, a sample table, a receiving focusing collimator and a small array detector. The sample table is used to fix a measured part of a sample at the center of a diffractometer circle. The X-ray source is used to emit short-wavelength characteristic X-rays. The incident collimator is located between the X-ray source and the sample table, and is used to irradiate the short-wavelength characteristic X-rays to the center of the diffractometer circle. The receiving focusing collimator is located on the other side of the sample table relative to the incident collimator, and the light-in side of the receiving focusing collimator is directed to the center of the diffractometer circle. The small array detector is located on the light-out side of the receiving focusing collimator, and is used to obtain diffraction raw data by exposure through the receiving focusing collimator. Single exposure of the small array detector is used to obtain a part of a diffraction Debye ring. The width of the corresponding image of the obtained diffraction raw data is 2-4 times the peak width of the diffraction peak of a single diffraction crystal face.

[0017] The width of the diffraction original data obtained by setting the small array detector single exposure corresponds to 2-4 times the peak width of the diffraction peak of a diffraction crystal face, so that after a specific angle is selected, the whole information of the diffraction peak in a diffraction crystal face can be obtained by one-time exposure, and thus the internal diffraction information test can be quickly performed.

[0018] The application also provides a test method, which also has the beneficial effects described above, and will not be described here. BRIEF DESCRIPTION OF DRAWINGS

[0019] In order to more clearly illustrate the technical solutions of the embodiments of the present application or the prior art, the following will briefly introduce the drawings needed to be used in the embodiments or the prior art description. Obviously, the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can also be obtained without creative labor on the basis of these drawings.

[0020] Figure 1 A structural schematic diagram of a short-wavelength characteristic X-ray diffraction device provided by the embodiment of the present application; Figure 2 A structural schematic diagram of a focusing collimator in the embodiment of the present application; Figure 1 Figure 3 A structural schematic diagram of an incident collimator in the embodiment of the present application; Figure 1 Figure 4 A flowchart of a test method provided by the embodiment of the present application; Figure 5 A generated diffraction peak schematic diagram in the embodiment of the present application; Figure 4 Figure 6 A flowchart of a specific test method provided by the embodiment of the present application; Figure 7 A generated diffraction peak schematic diagram in the embodiment of the present application; Figure 6 Figure 8 A flowchart of another specific test method provided by the embodiment of the present application; Figure 9 A diffraction spectrum schematic diagram in the embodiment of the present application; Figure 10 A diffraction original data acquisition schematic diagram in the embodiment of the present application.

[0021] In the figure: 1. X-ray source, 2. Incident collimator, 21. Adjustment track, 22. Adjustment block, 3. Sample table, 4. Receiving focusing collimator, 5. Small array detector, 51. Pixel, 6. Goniometer, 7. Arc track, 8. Host computer, 9. Remote terminal. DETAILED DESCRIPTION​​​​

[0022] The core of this invention is to provide a short-wavelength characteristic X-ray diffraction device. In existing technologies, short-wavelength characteristic X-ray diffraction techniques suffer from low efficiency in single-point detector scanning and testing of diffraction spectra.

[0023] The present invention provides a short-wavelength characteristic X-ray diffraction device, comprising an X-ray source, an incident collimator, a sample stage, a receiving focusing collimator, and a miniature array detector. The sample stage is used to fix the sample to be measured at the center of the diffractometer. The X-ray source is used to emit short-wavelength characteristic X-rays. The incident collimator is located between the X-ray source and the sample stage to irradiate the center of the diffractometer with the short-wavelength characteristic X-rays. The receiving focusing collimator is located on the other side of the sample stage relative to the incident collimator, with the incident side of the receiving focusing collimator pointing towards the center of the diffractometer. The miniature array detector is located on the emitting side of the receiving focusing collimator to acquire raw diffraction data through exposure via the receiving focusing collimator. A single exposure of the miniature array detector is used to acquire a portion of the diffraction Debye rings. The width of the image corresponding to the acquired raw diffraction data is 2 to 4 times the peak width of the diffraction peak of one diffraction crystal plane.

[0024] By setting the width of the image corresponding to the raw diffraction data obtained by a single exposure of a small array detector to be 2 to 4 times the peak width of the diffraction peak of a diffraction crystal plane, it is ensured that after selecting a specific angle, all the information of the diffraction peak in a diffraction crystal plane can be obtained in one exposure, thus enabling rapid testing of internal diffraction information.

[0025] To enable those skilled in the art to better understand the present invention, the invention will be further described in detail below with reference to the accompanying drawings and specific embodiments. Obviously, the described embodiments are merely some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Example 1

[0026] Please refer to Figures 1 to 3 , Figure 1 This is a schematic diagram of the structure of a short-wavelength characteristic X-ray diffraction device provided in an embodiment of the present invention; Figure 2 for Figure 1 A schematic diagram of the structure of the focusing collimator in the middle receiver; Figure 3 for Figure 1 A schematic diagram of the incident collimator.

[0027] See Figure 1In the embodiment, the short-wavelength characteristic X-ray diffraction device comprises an X-ray source 1, an incident collimator 2, a sample stage 3, a receiving focusing collimator 4 and a small array detector 5; the sample stage 3 is used to fix the measured part of the sample at the center of the diffractometer circle, the X-ray source 1 is used to emit short-wavelength characteristic X-rays, the incident collimator 2 is located between the X-ray source 1 and the sample stage 3 to irradiate the short-wavelength characteristic X-rays to the center of the diffractometer circle; the receiving focusing collimator 4 is located on the other side of the sample stage 3 relative to the incident collimator 2, the light entrance side of the receiving focusing collimator 4 points to the center of the diffractometer circle; the small array detector 5 is located on the light exit side of the receiving focusing collimator 4 to acquire diffraction raw data by exposure of the receiving focusing collimator 4; the single exposure of the small array detector 5 is used to acquire part of the diffraction Debye ring, and the width of the acquired diffraction raw data corresponds to 2-4 times the peak width of the diffraction peak of a diffraction crystal face.

[0028] The sample stage 3 is used to fix the measured part of the sample at the center of the diffractometer circle, and the specific structure of the sample stage 3 can refer to the prior art, which will not be repeated here. The X-ray source 1 is used to emit short-wavelength characteristic X-rays, and the emission direction of the X-ray source 1 needs to point to the center of the diffractometer circle, so that the short-wavelength characteristic X-rays can irradiate the measured part of the sample fixed on the sample stage 3 during use, i.e. the part of the sample to be measured. The specific structure of the X-ray source 1 can refer to the prior art, which will not be repeated here. In the embodiment, an incident collimator 2 is usually arranged between the X-ray source 1 and the sample stage 3, and the function of the incident collimator 2 is to limit the propagation path of the short-wavelength characteristic X-rays, so as to ensure that the short-wavelength characteristic X-rays emitted by the X-ray source 1 can accurately irradiate the center of the diffractometer circle. That is, in the embodiment, the X-ray source 1 emits short-wavelength characteristic X-rays, the short-wavelength characteristic X-rays are collimated by the incident collimator 2 and irradiate the center of the diffractometer circle, and the measured part of the sample is fixed at the center of the diffractometer circle by the sample stage 3. The wavelength range of the short-wavelength characteristic X-rays is usually 0.01-0.1 nm, which is not limited in the embodiment. In the embodiment, it is usually required that the short-wavelength characteristic X-rays can penetrate a certain thickness of the sample, so as to analyze the material structure at a certain depth of the sample.

[0029] For the sample table 3, the short wavelength characteristic X-rays are incident from one side thereof, and the diffraction X-rays carrying sample information are emitted from the other side of the sample table 3. Therefore, in the present embodiment, the receiving focusing collimator 4 is located on the other side of the sample table 3 relative to the incident collimator 2, and the light entrance side of the receiving focusing collimator 4 is directed to the center of the diffraction goniometer circle. The receiving focusing collimator 4 is used to focus and propagate the diffraction X-rays carrying sample information to the small array detector 5 for detection, and therefore the light entrance side of the receiving focusing collimator 4 needs to be directed to the center of the diffraction goniometer circle to ensure that the diffraction X-rays can be incident to the receiving focusing collimator 4. The small array detector 5 needs to be located on the light exit side of the receiving focusing collimator 4, so that the receiving focusing collimator 4 can transmit the diffraction X-rays to the receiving focusing collimator 4, i.e. the small array detector 5 can acquire diffraction raw data by exposure through the receiving focusing collimator 4. Generally, the short wavelength characteristic X-rays irradiated to the sample are also referred to as incident rays, and the diffraction X-rays emitted from the sample are referred to as diffraction rays.

[0030] It should be noted that the detector used in the present embodiment is the small array detector 5. The array detector means that the detector can detect diffraction X-rays within a certain range along the scanning direction, i.e. the direction of circumferential movement around the center of the diffraction goniometer circle, i.e. the direction of rotation of the goniometer 6, rather than only detecting the diffraction X-rays of a single point. For example, if the length of the small array detector 5 along the scanning direction is 4 mm, the small array detector 5 can detect diffraction X-rays within a range of 4 mm along the scanning direction. Compared with the single-point detector, the small array detector 5 can detect more data in one exposure process.

[0031] The small array detector 5 can only acquire part of the diffraction Debye ring in one exposure process, unlike the large array detector which can acquire the entire diffraction Debye ring, and therefore the array detector used in the present embodiment is the small array detector 5.

[0032] Specifically, in the embodiment, the width of the image corresponding to the diffraction raw data obtained by single exposure of the small array detector 5 is 2-4 times the peak width of the diffraction peak of a diffraction crystal face. The image corresponding to the diffraction raw data is an image including the diffraction peak obtained by processing the diffraction raw data. In the embodiment, after the small array detector 5 is adjusted to a preset angle, the diffraction raw data is obtained by single exposure, and the diffraction raw data obtained by single exposure is processed to obtain a complete image of the diffraction peak of a diffraction crystal face, because the width of the image generated by single exposure of the small array detector 5 is 2-4 times the peak width of the diffraction peak of a diffraction crystal face. However, because the width of the image generated by single exposure of the small array detector 5 is only 2-4 times the peak width of the diffraction peak of a diffraction crystal face, the small array detector 5 cannot obtain the diffraction peaks of all diffraction crystal faces, that is, the small array detector 5 can only obtain part of the diffraction Debye ring, that is, part of the data of the diffraction Debye ring, but cannot obtain the complete diffraction Debye ring.

[0033] Correspondingly, the above-mentioned incident collimator 2 needs to allow all the diffraction raw data required by single exposure of the small array detector 5 to pass through, that is, the internal channel of the above-mentioned incident collimator 2 needs to have a certain width, and the width of the internal channel needs to correspond to the size of the small array detector 5. The incident collimator 2 needs to at least allow all the diffraction raw data corresponding to the diffraction peak of a diffraction crystal face to pass through at least once exposure of the small array detector 5, and be transmitted to the small array detector 5 for exposure.

[0034] Referring to Figure 2 Specifically, in the embodiment, the receiving focusing collimator 4 can be a single-channel receiving focusing collimator 4, and the extensions of the two inner sides of the single-channel receiving focusing collimator 4 are focused on the center of the diffractometer circle. The single-channel receiving focusing collimator 4 is a receiving focusing collimator 4 having only one internal channel. The internal channel of the single-channel receiving focusing collimator 4 has a cross section in the transverse direction, that is, a cross section in the scanning direction, which is usually trapezoidal; and a cross section in the vertical direction, that is, a cross section perpendicular to the scanning direction, which is usually rectangular. The internal channel of the single-channel receiving focusing collimator 4 has two side walls, that is, inner side walls. The cross section of the inner side wall in the scanning direction is an inner side. In order to ensure that the single-channel receiving focusing collimator 4 can transmit the diffraction X-rays to the small array detector 5, it is necessary to ensure that the extensions of the two inner sides of the single-channel receiving focusing collimator 4 are focused on the center of the diffractometer circle, so that the diffraction X-rays passing through the single-channel receiving focusing collimator 4 can irradiate the small array detector 5.

[0035] Specifically, in the embodiment, the small array detector 5 is a linear array detector, the pixel size of the linear array detector along the rotation direction of the goniometer 6 ranges from 0.01 mm to 0.2 mm, and the pixel size of the linear array detector along the direction perpendicular to the rotation direction of the goniometer 6 ranges from 5 mm to 30 mm; or, the small array detector 5 is a pixel array detector, the pixel size of the pixel array detector along the rotation direction of the goniometer 6 ranges from 0.01 mm to 0.2 mm, and the pixel size of the pixel array detector along the direction perpendicular to the rotation direction of the goniometer 6 ranges from 0.01 mm to 0.2 mm. The rotation direction of the goniometer 6 is the scanning direction, and the small array detector 5 in the embodiment can be a linear array detector or a pixel array detector. When the small array detector 5 is a linear array detector, the pixel 51 size of the linear array detector along the scanning direction ranges from 0.01 mm to 0.2 mm. Limiting the pixel 51 size of the linear array detector along the scanning direction to the range from 0.01 mm to 0.2 mm can ensure the accuracy of the generated diffraction peak and avoid the need for multiple exposures to obtain the data of one diffraction peak. In the direction perpendicular to the scanning direction, the pixel 51 size of the linear array detector can be equal to the length of the linear array detector in the direction perpendicular to the scanning direction. In this case, the pixel 51 size of the linear array detector in the direction perpendicular to the scanning direction can be specifically 5 mm to 30 mm. In this case, the single pixel 51 is usually in a linear structure.

[0036] When the small array detector 5 is a pixel array detector, the pixel 51 size of the pixel array detector along the scanning direction also ranges from 0.01 mm to 0.2 mm. Limiting the pixel 51 size of the pixel array detector along the scanning direction to the range from 0.01 mm to 0.2 mm can ensure the accuracy of the generated diffraction peak and avoid the need for multiple exposures to obtain the data of one diffraction peak. In the direction perpendicular to the scanning direction, the pixel 51 size of the pixel array detector can be equal to the size of the pixel array detector in the scanning direction, i.e., the pixel size along the direction perpendicular to the rotation direction of the goniometer 6 ranges from 0.01 mm to 0.2 mm. In this case, the pixel 51 of the pixel array detector can be in a dot array structure.

[0037] In the embodiment, the detection area size of the small array detector 5 has a length in the scanning direction ranging from 4 mm to 50 mm and a length in the direction perpendicular to the scanning direction ranging from 10 mm to 50 mm, so as to ensure that the small array detector 5 can generate a complete image of one diffraction peak in one exposure process. The detection area size is the size corresponding to the area used by the small array detector 5 for exposure detection.

[0038] In the embodiment, the receiving focusing collimator 4 and the small array detector 5 can be fixedly connected with the goniometer 6, and the goniometer 6 is used to drive the receiving focusing collimator 4 and the small array detector 5 to rotate around the center of the goniometer 6. Generally, the center of the goniometer 6 is coincident with the center of the diffraction instrument circle, and the goniometer 6 can adjust the angle between the receiving focusing collimator 4, the small array detector 5 and the short-wavelength characteristic X-ray incident from the sample, so that the small array detector 5 can detect the diffraction raw data of different diffraction angles 2θ. The diffraction instrument can move the receiving focusing collimator 4 and the small array detector 5 along the arc-shaped path in a step-by-step manner, and the center of the arc-shaped path is the center of the goniometer 6. That is, in the embodiment, the receiving focusing collimator 4 and the small array detector 5 can be driven to any angle by rotating the goniometer 6, and the specific structure of the goniometer 6 can refer to the prior art, which will not be described here.

[0039] Further, when the weight of the receiving focusing collimator 4 and the small array detector 5 is heavy, the embodiment can specifically set the receiving focusing collimator 4 and the small array detector 5 on the arc-shaped track 7, and the goniometer 6 is used to drive the receiving focusing collimator 4 and the small array detector 5 to move along the arc-shaped track 7, and the arc-shaped track 7 is concentric with the center of the goniometer 6. That is, the embodiment can additionally set an arc-shaped track 7 to bear the weight of the receiving focusing collimator 4 and the small array detector 5, and support the receiving focusing collimator 4 and the small array detector 5. Generally, the detector support that can move on the arc-shaped track 7 is set first, and the receiving focusing collimator 4 and the small array detector 5 are installed on the detector support, and the goniometer 6 drives the detector support to move. The goniometer 6 drives the receiving focusing collimator 4 and the small array detector 5 to move along the arc-shaped track 7 in a step-by-step manner. Obviously, the arc-shaped track 7 needs to be concentric with the center of the goniometer 6, so as to ensure that the receiving focusing collimator 4 can always point to the center of the goniometer 6, and the small array detector 5 can always obtain the diffraction raw data. Specifically, the focal length of the receiving focusing collimator 4 in the embodiment is generally 5mm to 100mm, and the length of the receiving focusing collimator 4 itself is generally 100mm to 1000mm, which focuses on the center of the diffraction instrument circle, and the focal point does not change when the goniometer 6 rotates. The detection plane of the small array detector 5 is generally perpendicular to the straight-through light of the diffraction X-ray passing through the receiving focusing collimator 4, and the beam of the straight-through light of the diffraction X-ray is generally located on the center line of the effective detection area of the detector.

[0040] Generally, the small array detector 5 and the goniometer 6 need to be connected with the host computer 8, which will directly control the movement of the goniometer 6 and receive the data received by the small array detector 5. The host computer 8 also needs to be connected with the remote terminal 9 to accept the control of the remote terminal 9.

[0041] Referring to Figure 3 In the embodiment, the light passing section of the incident collimator 2 is generally rectangular, and the light outlet of the incident collimator 2 is provided with an adjusting track 21 extending in the direction perpendicular to the scanning direction; the adjusting track 21 is provided with an adjusting block 22 moving along the adjusting track 21. The adjusting block 22 can move in the direction perpendicular to the scanning direction along the adjusting track 21, and the adjusting block 22 has a blocking effect on the short-wavelength characteristic X-ray, so as to block the short-wavelength characteristic X-ray and adjust the size of the light passing section of the incident collimator 2. The specific material of the adjusting block 22 can be set according to actual conditions, and is not limited here.

[0042] The short-wavelength characteristic X-ray diffraction device provided in the embodiment has the width of the diffraction raw data corresponding to the image obtained by single exposure of the small array detector 5 being 2 times to 4 times the peak width of the diffraction peak of a diffraction crystal face, so that after a specific angle is selected, the whole information of the diffraction peak in a diffraction crystal face can be obtained by one-time exposure, and the internal diffraction information test can be quickly performed. Embodiment two

[0043] Referring to Figure 4 and Figure 5 , Figure 4 The flow chart of the test method provided in the embodiment of the application; Figure 5 The diffraction peak diagram generated by Figure 4 The diffraction peak diagram generated by

[0044] The test method provided in the embodiment is specifically the steps executed by the short-wavelength characteristic X-ray diffraction device provided in the above embodiment for sample testing, and the short-wavelength characteristic X-ray diffraction device provided in the above embodiment needs to be used to realize the test method. The specific structure of the short-wavelength characteristic X-ray diffraction device has been described in detail in the above embodiment, and will not be repeated here.

[0045] Referring to Figure 4 In the embodiment, the test method includes: S101: fixing the to-be-tested part of the sample at the center of the diffraction instrument by the sample table.

[0046] After the X-ray source 1, the incident collimator 2, the sample table 3, the receiving focusing collimator 4 and the small array detector 5 are installed and the optical path between the structures is debugged, the sample is fixed on the sample table 3, and the position of the sample to be measured is located at the center of the diffractometer circle.

[0047] Then, the receiving focusing collimator 4 and the small array detector 5 are usually moved to the theoretical diffraction angle corresponding to the diffraction plane to be detected. Of course, if the angle of the receiving focusing collimator 4 and the small array detector 5 is adjusted when the short-wavelength characteristic X-ray diffractometer is installed, this step can be omitted.

[0048] S102: Emitting short-wavelength characteristic X-rays from the X-ray source to the sample, and exposing the small array detector at a preset angle to obtain diffraction raw data.

[0049] The preset angle can be the theoretical diffraction angle corresponding to the diffraction plane to be detected. In this step, the X-ray source 1 emits short-wavelength characteristic X-rays to the sample, and the small array detector 5 obtains diffraction raw data at the preset angle. Due to the structure of the small array detector 5 in this embodiment, it is possible to obtain the complete diffraction peak image of the detected diffraction plane.

[0050] S103: Processing the diffraction raw data to obtain a diffraction peak of a diffraction plane, and analyzing based on the diffraction peak.

[0051] Referring to Figure 5 In this step, the diffraction raw data is processed. The specific processing process can refer to the prior art, which will not be described here. In this embodiment, the small array detector 5 can obtain the data of the entire diffraction peak corresponding to the detected diffraction plane in one exposure. This step is specifically to process the diffraction raw data, so as to obtain the image of the diffraction peak of a diffraction plane, and then analyze based on the diffraction peak. Specifically, the internal residual stress, texture, phase, and orientation information can be analyzed based on the information of the diffraction peak. The specific analysis content is not limited here.

[0052] For example, if the center of the miniature array detector 5 is set at a position corresponding to a diffraction angle of 0.2°, based on the width of the detection area of ​​the miniature array detector 5, it can detect raw diffraction data within the diffraction angle range of 0.1° to 0.3°. In this embodiment, the center of the miniature array detector 5 can be fixed at the position corresponding to a diffraction angle of 0.2°. Raw diffraction data within the diffraction angle range of 0.1° to 0.3° can be obtained through exposure of the miniature array detector 5, facilitating subsequent analysis based on this raw diffraction data. Since there is no need to move the miniature array detector 5 stepwise, efficient detection can be achieved. Of course, in this step, the exposure time of a single exposure of the miniature array detector 5 is usually relatively long to fully acquire the raw diffraction data corresponding to each diffraction angle within the aforementioned diffraction angle range, achieving the acquisition of complete data for a diffraction peak with only one exposure. The testing method provided in this embodiment sets the width of the image corresponding to the raw diffraction data obtained by a single exposure of a small array detector 5 to be 2 to 4 times the peak width of the diffraction peak of a diffraction crystal plane. This ensures that after selecting a specific angle, all the information of the diffraction peak in a diffraction crystal plane can be obtained in one exposure, thereby enabling rapid testing of internal diffraction information.

[0053] The specific details of the testing method provided in this application will be described in detail in the following embodiments of the invention. Example 3

[0054] Please refer to Figure 6 as well as Figure 7 , Figure 6 A flowchart illustrating a specific testing method provided in an embodiment of the present invention; Figure 7 for Figure 6 A schematic diagram of the generated diffraction peaks.

[0055] See Figure 6 In this embodiment, the testing method includes: S201: Fix the part of the sample to be tested at the center of the diffractometer using the sample stage.

[0056] S202: Short-wavelength characteristic X-rays are emitted to the sample through an X-ray source, and the sample is exposed at a preset angle by a small array detector to obtain raw diffraction data.

[0057] The above S201 to S202 are basically the same as S101 to S102 in the above embodiments. For details, please refer to the above embodiments, and will not be repeated here.

[0058] S203: Stepping-moving miniature array detector and receiving focusing collimator.

[0059] See Figure 7In the embodiment, the range of the integral step movement is a first angle range, and in this step, the exposure of the small array detector 5 at a preset angle to obtain diffraction raw data is performed after each step movement, that is, S202 is performed after each step movement to obtain corresponding diffraction raw data. It should be noted that the first angle range in the embodiment is usually small, and the main purpose is to ensure that all diffraction data of the detected diffraction crystal face are obtained to ensure that the corresponding diffraction peak is generated. The movement of the small array detector 5 and the receiving focusing collimator 4 is to ensure that the diffraction peak of the detected target diffraction crystal face is obtained, and the angle of the scanning is slightly expanded. The ultimate purpose is still to analyze based on the detected diffraction peak.

[0060] It should be noted that the distance of each step movement in this step is usually smaller than the size of the small array detector 5 in the scanning direction, that is, the angle of each step movement is usually smaller than the included angle between the inner walls of the single-channel receiving focusing collimator 4. Therefore, in the embodiment, the diffraction raw data corresponding to a single diffraction crystal face can be obtained multiple times, and the diffraction raw data obtained by the same exposure can be accumulated in the subsequent step to obtain the complete data of the diffraction angle corresponding to the center of the small array detector 5 at the exposure time. Therefore, the exposure time after each step movement in the embodiment can be correspondingly reduced, that is, the exposure time after each step movement in the embodiment can be smaller than the exposure time of obtaining the complete data of a diffraction peak by only one exposure.

[0061] S204: Accumulating the diffraction raw data obtained by the same exposure as the exposure data of the diffraction angle corresponding to the center of the small array detector at the exposure time.

[0062] In this step, the diffraction raw data obtained by the same exposure is accumulated as the exposure data of the diffraction angle corresponding to the center of the small array detector at the exposure time. For example, if the center of the small array detector 5 is arranged at a position corresponding to a diffraction angle of 0.2°, based on the width of the detection area of the small array detector 5, it can detect the diffraction raw data in the diffraction angle range of 0.1° to 0.3°. Therefore, in the embodiment, the center of the small array detector 5 can be fixed at a position corresponding to a diffraction angle of 0.2°, and the diffraction raw data in the diffraction angle range of 0.1° to 0.3° can be obtained by the exposure of the small array detector 5. In this step, the diffraction raw data in the above diffraction angle range is accumulated as the exposure data of the diffraction angle of 0.2°, and the subsequent analysis is based on the exposure data.

[0063] It should be noted that in order to obtain all exposure data in the diffraction angle range of 0.1° to 0.3°, the small array detector 5 needs to be moved step by step in the angle range of 0° to 0.4° and exposed after each step, and then the diffraction raw data obtained by each exposure is accumulated to obtain the complete data of a diffraction peak by multiple exposures.

[0064] It should be noted that since the complete data of a diffraction peak is obtained by multiple exposures in this step, the exposure time of a single exposure is usually shorter than the exposure time used when the complete data of a diffraction peak is obtained by only one exposure. It should also be noted that the overall step range of the small array detector 5 in this embodiment is usually small, and the angle of a single step movement is usually small, so that the complete data of a diffraction peak is obtained by multiple exposures.

[0065] S205: Process the exposure data to obtain a diffraction peak including a single diffraction crystal face, and analyze based on the diffraction peak.

[0066] In this step, the exposure data obtained after accumulation needs to be processed, and the processing process is basically the same as S103 in the above embodiment. For details, please refer to the above embodiment, which will not be repeated here.

[0067] The test method provided in this embodiment can ensure that all diffraction data of the required diffraction crystal face is obtained by moving the small array detector 5 and receiving the focusing collimator 4 to ensure that the corresponding diffraction peak is generated to realize the analysis function.

[0068] The specific content of the test method provided in this application will be described in detail in the following inventive embodiment. Embodiment Four

[0069] Please refer to Figures 8 to 9 , Figure 8 The flowchart of another specific test method provided in this embodiment of the application; Figure 9 The schematic diagram of the diffraction pattern in this embodiment.

[0070] See Figure 8 In this embodiment, the test method comprises: S301: Fix the to-be-tested part of the sample at the center of the diffractometer by the sample table.

[0071] S302: Emit short-wavelength characteristic X-rays from the X-ray source to the sample, and expose at a preset angle by the small array detector to obtain diffraction raw data.

[0072] S301 to S302 are basically the same as S101 to S102 in the above embodiment, and the details are described in the above embodiment, which will not be repeated here.

[0073] S303: Stepwise moving the small array detector and receiving the focusing collimator.

[0074] In this embodiment, the range of the overall stepwise movement is a second angle range, and in this embodiment, the exposure at the preset angle by the small array detector will be performed after each stepwise movement, that is, S302 described above will be performed after each stepwise movement to expose the small array detector 5 at the preset angle to obtain the diffraction raw data, so as to obtain the diffraction raw data corresponding to a plurality of diffraction planes. It should be emphasized that the second angle range in this embodiment is usually larger, which is usually larger than the first angle range, because this embodiment is to detect a complete diffraction pattern including a plurality of diffraction peaks. The purpose of moving the small array detector 5 and receiving the focusing collimator 4 is to obtain a complete diffraction Debye ring, that is, to obtain the diffraction peaks of a plurality of diffraction planes, and the ultimate purpose is to analyze based on the detected diffraction pattern.

[0075] Correspondingly, the angle of stepwise movement of the small array detector 5 in this step can be large, which can be not less than the width of the detection area of the small array detector 5. For example, if the center of the small array detector 5 is arranged at a position corresponding to a diffraction angle of 0.2° during stepwise movement, based on the width of the detection area of the small array detector 5, it can detect the diffraction raw data in the diffraction angle range of 0.1° to 0.3°. Therefore, the small array detector 5 can be directly moved to a position corresponding to a diffraction angle of 0.4° during stepwise movement, and the diffraction raw data in the diffraction angle range of 0.3° to 0.5° can be detected. By analogy, the diffraction raw data corresponding to a plurality of diffraction planes can be obtained.

[0076] S304: Processing a plurality of diffraction raw data to obtain a diffraction pattern including a plurality of diffraction peaks of a plurality of diffraction planes, and analyzing based on the diffraction pattern.

[0077] Referring to Figure 9 In this step, the diffraction raw data needs to be processed to generate a diffraction pattern including a plurality of diffraction peaks of a plurality of diffraction planes, Figure 9 The angles 1 to n in the above embodiment are angles adjusted in the second angle range, and the analysis based on the diffraction pattern. The specific content of the analysis can be set according to the actual situation, which will not be limited here.

[0078] The test method provided in the embodiment can obtain complete diffraction patterns through moving the small array detector 5 and receiving the focusing collimator 4, so as to realize the analysis function based on the diffraction patterns. Embodiment five

[0079] Referring to Figure 10 , Figure 10 It is a schematic diagram for collecting diffraction raw data in the embodiment.

[0080] Based on the strong penetration of the short-wavelength characteristic X-rays, the embodiment specifically provides a process for testing internal stress of an aluminum alloy plate based on the short-wavelength characteristic X-ray diffraction device, and the specific steps are as follows: S1: Positioning the to-be-tested part of the aluminum alloy plate at the center of the diffraction circle, and then selecting a diffraction crystal plane to be tested, and the Al (311) crystal plane is selected in the embodiment.

[0081] S2: Rotating the detector support to drive the receiving focusing collimator 4 and the small array detector 5 above to rotate, and the angle is the theoretical diffraction angle 2θ of the Al (311) crystal plane, which is 9.819°, and the aluminum alloy sample is rotated to half of the diffraction angle 2θ, which is θ=4.909°.

[0082] S3: Fixing the small array detector 5 to expose, so that the diffraction data of the aluminum alloy plate can be obtained, and the diffraction data is processed to obtain the diffraction spectrum, and the data obtained by the exposure of the small array detector 5 is as shown in Figure 10 .

[0083] S4: Positioning the to-be-tested part of the aluminum alloy plate standard sample at the center of the diffraction circle, and exposing to test the diffraction spectrum.

[0084] S5: Carrying out diffraction spectrum peak fitting analysis of the aluminum alloy plate and the standard sample, and calculating the diffraction angle.

[0085] S6: Moving the sample.

[0086] S7: Repeating steps S3 to S6, so that the diffraction peaks of different parts of the aluminum alloy plate can be obtained.

[0087] S8: According to the Bragg formula and the stress calculation formula, the stress of different parts can be calculated.

[0088] The test method provided in the embodiment sets the width of the diffraction raw data corresponding to the image obtained by single exposure of the small array detector 5 to be 2 times to 4 times the peak width of the diffraction peak of a diffraction crystal plane, so that after a specific angle is selected, all information of the diffraction peak in a diffraction crystal plane can be obtained by one-time exposure, and thus the internal diffraction information test can be quickly carried out.

[0089] The various embodiments described in this specification are presented for the purpose of illustration and description. Each of the embodiments described in this specification are important aspects of the present disclosure, and each of the embodiments can be used independently or in combination with one or more other embodiments.

[0090] Those skilled in the art will further appreciate that the units and algorithms described in the examples presented herein can be implemented in electronic hardware, computer software, or any combination thereof. To clearly illustrate this interchangeability of hardware and software, various components will be described herein generally in terms of their functionality, without reference to the particular manner in which they are implemented. Skilled persons will appreciate that the described functionality can be implemented by one or more computer software programs or general purpose computers programmed with one or more such programs. Such programs can be stored on any computer readable medium, such as random access memory (RAM), read only memory (ROM), magnetic disk, optical disk, nonvolatile memory including flash memory and / or other non-volatile storage, or any other form of tangible computer readable media.

[0091] The steps of a method or algorithm described in connection with the embodiments disclosed herein can be embodied directly in hardware, in a software module executed by a processor, or in a combination of the two. A software module can reside in random access memory (RAM), non-volatile memory (ROM), or any other form of tangible memory, whether volatile or non-volatile. The software module can include one or more executable programs, or a portion of an executable program.

[0092] Finally, it should be noted that the terms "first", "second", and the like, herein do not denote any order, quantity, combination, or importance, but rather are used to distinguish one element from another, and the terms "include" and "comprise" and variations thereof do not have to be construed to exclude other elements or steps. In other words, the terms "include" and "comprise" and variations thereof do not have to be construed to be exclusive or to exclude other elements or steps.

[0093] The short-wavelength characteristic X-ray diffraction device and the testing method provided by the present application are described in detail above. The principles and implementation manners of the present application are described by using specific examples in this specification. The above description of the embodiments is only used to help understand the method of the present application and its core idea. It should be pointed out that, for those skilled in the art, without departing from the principles of the present application, some improvements and modifications can be made to the present application, and these improvements and modifications also fall within the protection scope of the claims of the present application.

Claims

1. A short wavelength characteristic X-ray diffraction apparatus characterized by comprising: The X-ray source, the incident collimator, the sample stage, the receiving focusing collimator and the small array detector; The sample stage is used to fix the measured part of the sample at the center of the diffractometer circle, the X-ray source is used to emit short-wavelength characteristic X-rays, and the incident collimator is located between the X-ray source and the sample stage to irradiate the short-wavelength characteristic X-rays to the center of the diffractometer circle; The receiving focusing collimator is located on the other side of the sample stage relative to the incident collimator, and the light entrance side of the receiving focusing collimator is directed to the center of the diffractometer circle; The small array detector is located on the light exit side of the receiving focusing collimator to obtain diffraction raw data through exposure of the receiving focusing collimator; the single exposure of the small array detector is used to obtain part of the diffraction Debye ring, and the obtained diffraction raw data corresponds to an image with a width of 2-4 times the peak width of the diffraction peak of a single diffraction crystal face.

2. The short wavelength characteristic X-ray diffraction apparatus according to claim 1, characterized by, The receiving focusing collimator is a single-channel receiving focusing collimator, and the extensions of the two inner sides of the single-channel receiving focusing collimator are focused on the center of the diffractometer circle.

3. The short wavelength characteristic X-ray diffraction apparatus according to claim 1, characterized by, The receiving focusing collimator and the small array detector are fixedly connected with a goniometer, and the goniometer is used to drive the receiving focusing collimator and the small array detector to rotate around the center of the goniometer.

4. The short wavelength characteristic X-ray diffraction apparatus according to claim 3, characterized by, The receiving focusing collimator and the small array detector are installed on an arc-shaped track, and the goniometer is used to drive the receiving focusing collimator and the small array detector to move along the arc-shaped track, and the arc-shaped track is concentric with the center of the goniometer.

5. The short wavelength characteristic X-ray diffraction apparatus according to claim 1, characterized by, The small array detector is a linear array detector, and the pixel size of the linear array detector along the rotation direction of the goniometer ranges from 0.01 mm to 0.2 mm, and the pixel size of the linear array detector perpendicular to the rotation direction of the goniometer ranges from 5 mm to 30 mm. Or, the small array detector is a pixel array detector, and the pixel size of the pixel array detector along the rotation direction of the goniometer ranges from 0.01 mm to 0.2 mm, and the pixel size of the pixel array detector perpendicular to the rotation direction of the goniometer ranges from 0.01 mm to 0.2 mm.

6. The short wavelength characteristic X-ray diffraction apparatus according to claim 5, characterized by, The length of the size of the detection area of the small array detector along the scanning direction ranges from 4 mm to 50 mm, and the length of the size of the detection area of the small array detector perpendicular to the scanning direction ranges from 10 mm to 50 mm.

7. The short wavelength characteristic X-ray diffraction apparatus according to claim 1, characterized by, The light passing section of the incident collimator is rectangular, the light exit of the incident collimator is provided with an adjusting track extending perpendicular to the scanning direction, the adjusting track is provided with an adjusting block moving along the adjusting track.

8. A test method characterized by, The internal diffraction information test is performed by using the short-wavelength characteristic X-ray diffraction device according to any one of claims 1 to 7, comprising: fixing the measured part of the sample at the center of the diffractometer circle through the sample stage; emitting short-wavelength characteristic X-rays to the sample through the X-ray source, and exposing the small array detector at a preset angle to obtain diffraction raw data; processing the diffraction raw data to obtain a diffraction peak including a single diffraction crystal face, and analyzing based on the diffraction peak.

9. The method of claim 8, wherein, Further comprising: stepping the small array detector and receiving a focusing collimator, and performing, after each step, a step of exposure at a preset angle by the small array detector to obtain diffraction raw data; acquiring diffraction raw data corresponding to a plurality of diffraction planes by a plurality of exposures; processing the diffraction raw data to obtain diffraction peaks of the single diffraction plane, and performing analysis based on the diffraction peaks, including: accumulating the diffraction raw data obtained in the same exposure as exposure data of a diffraction angle corresponding to the center of the small array detector at the time of exposure; processing the exposure data to obtain diffraction peaks of the single diffraction plane, and performing analysis based on the diffraction peaks.

10. The method of claim 8, wherein, Further comprising: stepping the small array detector and receiving a focusing collimator, and performing, after each step, a step of exposure at a preset angle by the small array detector to obtain diffraction raw data, so as to obtain diffraction raw data corresponding to a plurality of diffraction planes; processing the diffraction raw data to obtain diffraction peaks of the single diffraction plane, and performing analysis based on the diffraction peaks, including: processing a plurality of the diffraction raw data to obtain a diffraction spectrum including diffraction peaks of a plurality of diffraction planes, and performing analysis based on the diffraction spectrum.

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