A short-wavelength characteristic X-ray diffraction device and method based on array detection

Abstract

The present invention discloses a short-wavelength characteristic X-ray diffraction measuring device based on array detection, and a measurement and analysis method based on the device. The array detector of the diffraction measuring device only detects and receives diffraction lines originating from the material diffraction of the measured part of the sample and passing through the light hole of the receiving collimator, and other stray lines passing through the light hole of the receiving collimator, and rays passing through the positioning hole; the extension line of the inner cone edge 1 of the light hole and the extension line of the inner cone edge 2 thereof intersect on the center line of the incident X-ray beam, and the intersection point is the center of the diffractometer circle of the device, and the measured part of the sample is located at the center of the diffractometer circle of the device; the method adopts the diffraction measuring device. The present invention can be used to quickly and non-destructively detect the diffraction pattern of a part inside a centimeter-level thick sample, that is, one or more diffraction Debye rings or diffraction spots, to achieve rapid and non-destructive detection and analysis of the crystal structure and structural changes of a part inside the sample, such as the physical phase, texture, stress, etc.

Description

Technical Field

[0001] The present invention belongs to the technical field of X-ray nondestructive testing, and in particular relates to a short-wavelength characteristic X-ray diffraction measuring device based on array detection, and a measuring and analyzing method based on the device. Background Art

[0002] The article "Research on the Uniformity of Residual Stress and Grain Orientation in Pre-stretched Thick Aluminum Plates" published by Zheng Lin et al. in the journal "Precision Forming Engineering" introduces the use of SWXRD-1000 short-wavelength X-ray diffractometer to non-destructively detect the distribution of WKα1 diffraction intensity along the diffraction angle 2θ of a material at a certain position inside a 20mm-25mm thick pre-stretched aluminum plate, that is, the diffraction spectrum. However, when using this short-wavelength X-ray diffractometer for detection, only the WKα1 diffraction intensity in one direction can be measured each time. It is necessary to step and scan to measure the WKα1 diffraction intensity at dozens of 2θ points to measure only the Al(111) crystal plane diffraction spectrum of the measured part and calculate the Al(111) crystal plane spacing, which takes tens of minutes; if the full diffraction spectrum of the material at that position is to be measured, it will take several hours to perform step scanning, and what is measured is only a small part of the diffraction information of the diffraction pattern. In summary, the aforementioned diffraction spectrum testing and analysis technology has the problem of too long measurement time and very little diffraction information. In addition, it will take longer to use it for fixed-point non-destructive testing and analysis of the internal phase, texture, residual stress, etc. of materials / workpieces, which greatly restricts the application of this technology. Therefore, how to obtain more diffraction information faster and more methods and devices have become the focus of attention in this technical field.

[0003] In addition, document CN111380880A provides a diffraction device, including an X-ray irradiation system, which irradiates X-rays to the measurement part of the sample under test; an X-ray detection system, which simultaneously detects multiple diffracted X-rays formed by the diffraction of X-rays from multiple parts of the sample under test, to simultaneously measure the X-ray diffraction intensity distribution of multiple parts of the sample under test; wherein the detected X-rays are short-wavelength characteristic X-rays; and the X-ray detection system is a parallel light array detection system. Although the device can quickly detect the uniformity of crystal orientation inside the workpiece, it is for simultaneous imaging of one direction of the diffraction of multiple parts of the sample, and cannot achieve multi-directional simultaneous imaging of the diffraction of one part of the sample, and cannot achieve simultaneous imaging of the Debye ring or diffraction pattern of the diffraction of one part of the sample, and it is even more impossible to perform rapid non-destructive detection and analysis of the phase, texture, stress, etc. of the material of one part of the sample based on the simultaneously imaged Debye ring or diffraction pattern. Summary of the invention

[0004] The purpose of the present invention is to provide a short-wavelength characteristic X-ray diffraction measurement device based on array detection, and a measurement and analysis method based on the device, which can at least be used for fixed-point rapid non-destructive detection and analysis of the physical phase, texture, and stress inside the sample, thereby solving the problem that existing diffraction devices and methods cannot achieve fixed-point rapid non-destructive detection and analysis.

[0005] The object of the present invention is achieved by adopting the technical solution described below.

[0006] A short-wavelength characteristic X-ray diffraction measurement device based on array detection, comprising an X-ray irradiation system, a sample stage and an X-ray detection system;

[0007] The X-ray irradiation system includes a radiation source and an incident collimator. The radiation source includes a heavy metal target X-ray tube with an atomic number greater than 55, and a high-voltage power supply with a supply voltage of more than 160 kV and its controller. The incident collimator is used to limit the divergence, cross-sectional shape and size of the X-ray beam incident on the sample. The X-rays emitted by the X-ray irradiation system pass through the incident collimator to form an incident X-ray beam and irradiate the measured part of the sample (the samples in the present invention refer to the measured samples) fixed on the sample stage. The X-ray detection system is used to measure the intensity and distribution of short-wavelength characteristic X-rays diffracted from the measured part inside the sample at a fixed point; the X-ray detection system includes a receiving collimator and an array detector matched to the receiving collimator;

[0008] Features:

[0009] The array detector detects and receives only the diffraction lines originating from the diffraction of the material at the measured part of the sample and passing through the light hole A of the receiving collimator, as well as other stray lines passing through the light hole A of the receiving collimator;

[0010] The extension line of the inner cone edge 1 of the light hole A and the extension line of the inner cone edge 2 thereof intersect on the center line of the incident X-ray beam, and the intersection point is the center of the diffractometer circle of the device, and the measured part of the sample is located at the center of the diffractometer circle of the device.

[0011] As a preferred solution, each detection pixel of the array detector is single-photon measurement, and a multi-energy array detector with two or more energy thresholds is used. Through the set energy threshold, each pixel can measure a short-wavelength characteristic X-ray; or, the array detector uses an energy dispersion array detector, and each pixel can measure one or more short-wavelength characteristic X-rays. As a more preferred solution, the array detector is installed in a shielding box that shields stray X-rays.

[0012] As a preferred solution, the light-through hole B of the incident collimator is a circular hole or a rectangular hole, the length of the incident collimator is 20 mm to 200 mm, and the divergence is 0.02° to 0.5°.

[0013] As a preferred embodiment, the length of the receiving collimator is 100 mm to 1200 mm, the angle between the inner cone edge 1 of the light hole A of the receiving collimator and the incident X-ray beam is γ, and the value range of γ is 2° to 10°; the angle between the inner cone edge 1 and the inner cone edge 2 of the light hole A is δ, and the value range of δ is 0.5° to 6°, and γ+δ is not greater than 12°.

[0014] In order to facilitate operation and further improve the accuracy of the detection results, a positioning hole of a diffraction pattern is provided in the middle of the receiving collimator, the axis of the positioning hole coincides with the center line of the incident X-ray beam (i.e., the center axis of the incident collimator), and an X-ray absorber is also provided in the positioning hole; the X-ray absorber can prevent the array detector from being damaged by the high-flux incident X-ray beam, and can determine the position of the maximum intensity of the transmitted X-ray by detecting the intensity distribution of the incident X-ray passing through the X-ray absorber, that is, determine the center position of the Debye ring or the diffraction pattern when diffraction occurs;

[0015] The incident collimator, the receiving collimator and the shielding box of the array detector are all made of heavy metal materials that meet the shielding requirements, and are used to shield stray X-rays from other parts and other directions, and only allow X-rays to pass through the light hole B of the incident collimator, the light hole A of the receiving collimator, the positioning hole and its X-ray absorber, and then enter the detection area of ​​the array detector through the receiving window of the shielding box of the array detector.

[0016] As two preferred solutions of the present invention, the X-ray irradiation system, the sample stage and the X-ray detection system are fixed on the same platform, the sample is fixed on the translation stage of the sample stage, the translation stage is fixed on the Φ angle turntable, the Φ angle turntable is fixed on the Ψ angle turntable, the Ψ angle turntable is fixed on the same platform, and the rotation axes of the Φ angle turntable and the Ψ angle turntable are perpendicular to each other and intersect at the center of the diffractometer circle, so that: regardless of the Φ angle rotation or the Ψ angle rotation, the measured part of the sample is always located at the center of the diffractometer circle;

[0017] or,

[0018] The X-ray irradiation system and the X-ray detection system are fixed on the Ψ angle turntable, and the Ψ angle turntable is fixed on a platform together with the sample stage composed of a translation stage and a Φ angle turntable, the sample is fixed on the translation stage of the sample stage, the translation stage is fixed on the Φ angle turntable, the Φ angle turntable is fixed on the one platform, and the rotation axes of the Φ angle turntable and the Ψ angle turntable are perpendicular to each other and intersect at the center of the diffractometer circle, so that: no matter whether the Φ angle or the Ψ angle is rotated, the measured part of the sample is always located at the center of the diffractometer circle.

[0019] Furthermore, the center line of the positioning hole and the center line of the incident collimator are in a straight line and are parallel to the Z axis of the translation stage when Ψ=0°. Regardless of whether the sample is rotated or translated, the coordinates of the center position of the diffracted Debye ring do not change, that is, the coordinate position of the incident X-ray beam reaching the array detector does not change, and the coordinates of the center position of the Debye ring are set to (0,0,0), as Figure 6 The distance t from the center of the diffractometer circle of the device to the array detector is 150 mm to 1500 mm, that is, the distance from the measured part of the sample to the array detector is t.

[0020] The device described in the present invention can intuitively measure the Debye ring diffracted by the measured part, and obtain a diffraction pattern similar to that obtained by an X-ray diffraction flat camera. When the diffraction pattern is measured by exposure, the diffraction peak in a certain direction of the (hkl) crystal plane is determined to obtain the coordinates of the center of the Debye ring (x, y, -t), such as Figure 6 As shown, the diffraction angle 2θ of the diffraction peak satisfies Therefore, after determining the peak and obtaining its coordinates (x, y, -t), the diffraction angle 2θ can be calculated.

[0021] As a preferred solution, the specification range of each pixel of the array detector is 0.02mm-0.2mm; the array detector adopts a cadmium telluride array detector, a cadmium zinc telluride array detector or a gallium arsenide array detector.

[0022] The measurement and analysis method based on the aforementioned short-wavelength characteristic X-ray diffraction measuring device adopts the transmission diffraction method of short-wavelength characteristic X-rays, and its steps are as follows.

[0023] Step 1: According to the material and thickness of the sample, select short-wavelength characteristic X-rays of appropriate wavelength (such as Wkα1 radiated by a tungsten target X-ray tube, or Ukα1 radiated by a uranium target X-ray tube, etc.), and set two energy thresholds of the array detector so that each pixel of the array detector detects the selected short-wavelength characteristic X-rays (such as Wkα1 or Wkα, or Ukα1 or Ukα, etc.).

[0024] Step 2: Fix the sample on the sample stage and place the measured part of the sample at the center of the diffractometer circle.

[0025] Step 3: According to the selected short-wavelength characteristic X-ray, apply a tube voltage that is 1.5 times higher than the target excitation voltage and start the X-ray irradiation system.

[0026] Step 4, expose and measure the Debye ring or diffraction pattern of the crystalline material at the measured part, determine the peak, compare it with the powder diffraction card, and determine the phase of the crystalline material at the measured part.

[0027] Step 5, if the texture or orientation of the main phase of the measured part is to be tested, the step-scan measurement is performed by rotating the Ψ angle turntable to expose and measure the Debye rings diffracted by the crystal material of the measured part at different Ψ angles; the peak is determined, and the diffraction intensity of the Debye rings of each diffraction crystal plane in each direction is measured; and absorption correction is performed according to the diffraction path length to obtain the diffraction intensity of the Debye rings of each diffraction crystal plane after correction in each direction, and based on this, the transmission pole figures of multiple strong diffraction crystal planes and relatively strong diffraction crystal planes of the main phase are calculated; according to the crystal system type, the transmission pole figures of multiple strong diffraction crystal planes of the main phase are selected, and the full pole figures or orientation distribution function (ODF) of the corresponding diffraction crystal plane are calculated.

[0028] Note: Due to different crystal systems, the symmetry is different. The higher the symmetry of the crystal system, the fewer transmission pole figures are needed to calculate the full pole figure or orientation distribution function (ODF) of the corresponding diffraction crystal plane. That is, the fewer the number of main phase diffraction crystal planes (Debye rings) that need to be calculated in the Debye rings of the crystal material diffraction of the measured part at the above different θ. For example, for the fcc crystal system, it is only necessary to test the transmission pole figures of three strong diffraction crystal planes to calculate the corresponding full pole figure or orientation distribution function (ODF). For example, it is only necessary to use the transmission pole figures of three strong lines such as (111), (200) and (220) crystal planes to calculate the full pole figure or orientation distribution function (ODF) of the corresponding diffraction crystal plane.

[0029] Step 6: If the residual stress of the measured part is to be tested, measure the strains in multiple directions of one (hkl) crystal plane or multiple (hkl) crystal planes of the main phase, and calculate the stress tensor σ of the measured part of the sample based on the stress-strain relationship of elastic mechanics.

[0030] (1) Residual stress test of samples in plane stress state.

[0031] (a) For samples of non-strongly textured materials, the sample and the stress-free standard are rotated by rotating the Ψ angle turntable respectively, so that the surface normal direction of the measured part of the sample and the corresponding part of the stress-free standard coincides with the incident light beam, and then the Debye rings or strong diffraction spots diffracted by each crystal plane of the measured part of the sample and the corresponding part of the stress-free standard are exposed and measured respectively, and the diffraction angle 2θ of each crystal plane in each direction of the measured part of the sample is obtained by peak determination. s-hkl , and the diffraction angle 2θ of each crystal plane in each direction of the corresponding part of the stress-free standard sample 0-hkl Then, for a certain (hkl) crystal plane (such as Al(111) crystal plane), according to the strain

[0032]

[0033] The calculated angle with the surface normal direction of the sample tested part is 90°-θ hkl, the strains ε(90°-θ hkl , Φ) and its distribution;

[0034] Where, d s-hkl is the (hkl) interplanar spacing of the sample in the direction of the measured part, d 0-hkl is the corresponding interplanar spacing in the corresponding direction of the stress-free standard sample, Δd hkl It is the change in the (hkl) crystal plane spacing in the measured direction of the measured part of the sample.

[0035] Since the wavelength of short-wavelength characteristic X-rays is as short as about 0.02nm, the diffraction angle 2θ of the strong diffraction crystal planes and relatively strong diffraction crystal planes of most substances is mostly less than 11°, that is, θ hkl ﹤5.5°(If the selected short wavelength characteristic X-ray is Wk α1 , the diffraction angle 2θ for the crystal plane Al(111) 111 ≈5.12°,θ 111 ≈2.56°), so the strain ε(90°-θ hkl , Φ) and the strain ε(90°, Φ) in each direction of the (hkl) crystal plane perpendicular to the surface normal direction of the sample being measured are very different, that is, less than 5.5°, and can be regarded as equal (0°≤Φ≤180°), that is, ε(90°, Φ)=ε(90°-θ hkl , Φ);

[0036] According to the stress-strain relationship of plane stress problems in elastic mechanics, in the xy plane, the x-axis and y-axis are known to be the principal stress directions, and the strain ε in the x-direction is measured respectively. xx , that is, ε(90°-θ hkl , 90°), and the strain ε in the y direction yy , that is, ε(90°-θ hkl , 0°), and then the two principal stresses σ are calculated according to the following formula xx , σ yy ;

[0037]

[0038]

[0039] In the formula, E hkl is the elastic modulus of the (hkl) crystal plane, ν hkl is the Poisson's ratio of the (hkl) crystal plane;

[0040] The measured strains ε(90°-θ) in the two principal stress directions of the (hkl) crystal plane (such as Al(111) crystal plane) are hkl, 90°) and ε(90°-θ hkl , 0°), the two principal stresses σ perpendicular to the surface normal direction of the sample measured part are calculated by formulas (2) and (3) respectively: xx , σ yy , that is, the plane stress tensor σ of the measured part of the sample;

[0041] If the directions of the two principal stresses are unknown, according to the theory of elasticity, we only need to measure the strains in three directions to calculate the magnitude and direction of the two principal stresses and one shear stress, that is, the plane stress tensor σ of the measured part of the sample;

[0042] Note: (Ψ, Φ) is the coordinate on the (hkl) crystal plane pole figure to represent the crystal plane direction, the X-axis and the Y-axis are perpendicular. Taking the rolled plate as an example, (90°, 0°) represents the rolling direction RD (often defined as coinciding with the Y-axis), (90°, 90°) represents the transverse direction TD (often defined as coinciding with the X-axis), Ψ is the angle from the normal ND (often defined as coinciding with the Z-axis), and it is obvious that 0°≤Ψ≤90°; Φ is the angle of counterclockwise rotation from the RD direction (Y-axis) with the ND direction as the axis (Z-axis), and it is obvious that 0°≤Φ<360°;

[0043] Furthermore, if the Debye rings or strong diffraction spots of multiple strong diffraction crystal planes and relatively strong diffraction crystal planes (hkl) are measured simultaneously, the ε(90°-θ hkl , Φ) and its distribution; the ε(90°-θ hkl , Φ) and their distribution, respectively, we can get the corresponding multiple stress tensors σ, and then use the arithmetic mean method or the least squares method to calculate a more accurate stress tensor That is, the stress tensor can be calculated by exposing and measuring the measured part of the sample and the corresponding part of the stress-free standard sample once.

[0044] b) For samples with strong texture, the direction of strain measurement depends on the texture. It is necessary to select the direction of the diffraction intensity maximum (large pole density or strong diffraction spot) of the strong diffraction crystal plane (hkl) to be measured on the outermost circle of the (hkl) crystal plane pole figure, and between the two principal stresses ε xx , ε yy direction or near direction;

[0045] The sample is rotated by rotating the Ψ angle turntable so that the surface normal direction of the sample's measured part coincides with the incident light beam, and the Debye rings or strong diffraction spots diffracted by each crystal plane of the measured part of the sample and the corresponding part of the stress-free standard are exposed and measured respectively. The strong diffraction spots on the Debye rings are peaked to determine the α and β angles; the α angle is the angle of deflection of a pole density maximum from the x-axis, and the β angle is the angle of deflection of another pole density maximum from the y-axis, such as the transverse direction (TD) and the direction of about 20° away from the rolling direction (RD) on the outermost circle of the Al (111) pole figure of the rolled aluminum plate (such as α = 0°, β = 20°);

[0046] Measure ε(90°-θ hkl , 90°+α), ε(90°-θ hkl ,β), similarly, given that θ hkl ﹤5.5°, that is, ε(90°-θ hkl , Φ) = ε(90°, Φ), the measured strain ε(90°-θ hkl , 90°+α) is recorded as ε α , the measured strain ε(90°-θ hkl , β) is denoted as ε β , and substitute into the following two formulas

[0047]

[0048]

[0049] The two principal stresses σ can be calculated xx , σ yy The principal strain ε xx and ε yy , and then ε xx and ε yy Substituting into formula (2) and (3), we can finally calculate the two principal stresses σ xx , σ yy , that is, the stress tensor σ at the measured part of the sample.

[0050] In summary, for a sample in a plane stress state, the sample is rotated by rotating θ so that the surface normal direction of the sample's measured part coincides with the incident light beam, that is, the incident light is perpendicular to the sample. The Debye rings or strong diffraction spots diffracted by each crystal plane of the measured part of the sample and the corresponding part of the stress-free standard are exposed and measured once respectively. Then, the plane stress tensor σ of the measured part of the sample perpendicular to the surface normal direction of the measured part of the sample can be calculated according to formulas (2) and (3).

[0051] (2) For samples in a general stress state, a stronger diffraction crystal plane (hkl) is selected as the diffraction crystal plane for testing. At least six strains in the (Ψ, Φ) directions need to be measured, and the six Ψ angles cannot be all the same. The difference between the maximum Ψ and the minimum Ψ should be as large as possible, and the difference between the six Φ angles should also be as large as possible. The stress tensor σ of the measured part of the sample can be measured by exposing the Debye rings or strong diffraction spots diffracted by each crystal plane at the measured part of the sample and the corresponding part of the stress-free standard sample at only two different Ψ angles.

[0052] (a) For samples of non-strong textured materials, first rotate to Ψ=Ψ1, and expose the Debye rings diffracted by each crystal plane at the measured part of the sample and the corresponding part of the stress-free standard sample. Then, the sample is rotated to Ψ=Ψ2, and the difference between Ψ2 and Ψ1 is as large as possible. The Debye rings diffracted by each crystal plane are exposed again at the measured part of the sample and the corresponding part of the stress-free standard sample. Peak determination, select the peak determination results 2θ in the six directions of the (hkl) crystal plane s-hkl and 2θ 0-hkl , calculated by formula (1) to obtain 6 (Ψ i , Φ i ) direction (hkl) crystal plane strain ε(Ψ i , Φ i ), and strain

[0053] ε(Ψ i ,Φ i )=a i 2 ε xx +b i 2 ε yy +c i 2 ε yy +2a i b i ε xy +2b i c i ε yz +2c i a i ε zx ……………………(6)

[0054] In the formula, a i 、b i 、c i are the strain ε(Ψ i ,Φ i ) direction cosines in X, Y, and Z, a i = sinΨ i cosΦ i , b i = sinΨ i sinΦi , c i =cosΦ i .

[0055] The strains ε(Ψ i , Φ i ) and its direction cosines are substituted into equation (6) and the linear equations are solved simultaneously to obtain the strain ε ij (i=x,y,z; j=x,y,z); by ε ij The three principal strains ε can be obtained by linear transformation D XX , ε D YY , ε D ZZ Finally, the stress tensor σ (or the three principal stresses σ) of the measured part of the sample is calculated by formula (7) D XX , σ D YY , σ D ZZ size and direction),

[0056]

[0057] In formula (7), E is the elastic modulus of the (hkl) crystal plane, and ν is the Poisson's ratio of the (hkl) crystal plane.

[0058] Obviously, if the three principal stresses σ are known D XX , σ D YY , σ D ZZ direction, only three (Ψ i , Φ i ) direction, and the stress tensor σ of the measured part of the sample is obtained. The stress tensor σ can be calculated by exposing and measuring the measured part of the sample and the corresponding part of the stress-free standard sample twice.

[0059] Furthermore, since the Debye rings of multiple strong diffraction crystal planes and relatively strong diffraction crystal planes (hkl) are measured simultaneously, multiple ε(Ψ i , Φ i ), we can get the corresponding multiple stress tensors σ, and then use the arithmetic mean method or the least squares method to calculate a more accurate stress tensor That is, the stress tensor can be accurately calculated by exposing and measuring the measured part of the sample and the corresponding part of the stress-free standard sample twice.

[0060] (b) For residual stress testing of samples with strong texture materials, the direction of the strain measurement is determined according to the texture conditions. It is necessary to select the direction of the diffraction intensity maximum (large extreme density or strong diffraction spot) of the strong diffraction crystal plane (hkl) to be measured to measure the strain.

[0061] By rotating Ψ to expose and measure the Debye rings diffracted by the measured part of the sample and the corresponding part of the stress-free standard sample at different Ψ angles, six strong diffraction spots of the strong diffraction crystal plane and the relatively strong diffraction crystal plane (hkl) are selected, that is, the directions of the six diffraction intensity maxima or strong diffraction spots are determined, and the strain ε (Ψ) in the six directions is calculated by formula (1) i , Φ i ), according to formula (6), the three principal strains ε can be obtained by simultaneous linear equations and linear transformation. D XX , ε D YY , ε D ZZ , and then according to the elastic mechanics formula (7), the stress tensor σ (or the three principal stresses σ) of the measured part of the sample is finally obtained. D XX , σ D YY , σ D ZZ size and direction).

[0062] It should be noted that the strains in the six directions may not be in the same {h1k1l1} crystal plane family, that is, the strains in some directions are measured using the (h1k1l1) crystal plane, while the strains in the remaining directions are measured using the (h2k2l2) crystal plane. However, in the formula for calculating stress from strain, the elastic modulus E corresponding to the measured strain is used. hkl , Poisson's ratio ν hkl .

[0063] Note: For the preparation of stress-free standards, please refer to the relevant standards or literature. It can be prepared by annealing or wire cutting.

[0064] Step 7: If you want to test the internal phase, texture, and stress of another part of the sample, repeat steps 4, 5, and 6 until all the parts to be tested are tested. The computer processes the data to obtain the internal phase, texture, stress, etc. and their distribution of each part of the sample.

[0065] Beneficial effects: The present invention can be used to quickly and nondestructively detect the diffraction pattern of a part inside a sample with a thickness of centimeters, that is, one or more diffraction Debye rings or diffraction spots, to achieve rapid and nondestructive detection and analysis of the crystal structure and structural changes of a part inside the sample, such as the physical phase, texture, stress, etc. The detection efficiency is improved by more than 10 times compared with the technology and instruments described in the technical background, and the diffraction information measured each time is more and more accurate, which greatly improves the detection efficiency and accuracy; the present invention can realize multi-directional simultaneous imaging of the diffraction of a part of the sample, realize the simultaneous imaging of the Debye rings or diffraction patterns of a part of the sample, and can be based on the simultaneous imaging of the Debye rings Or diffraction pattern to conduct rapid nondestructive detection and analysis of the phase, texture, stress, etc. of a part of the sample; the operation process of rapid nondestructive detection and analysis of the internal phase, texture, stress, etc. and their distribution of materials / workpieces using the scheme of the present invention is simple and reliable. More importantly, the device and method provided by the present invention have a simple device structure and low cost, which overcomes the limitations of high-energy synchrotron radiation hard X-ray diffraction devices and technologies that are difficult to commercialize and promote and apply, as well as the low testing efficiency of the technical scheme disclosed in the background technology, and provides enterprises, universities and research institutions with an instrument device and method with similar functions and comparable detection efficiency to high-energy synchrotron radiation hard X-ray diffraction devices. BRIEF DESCRIPTION OF THE DRAWINGS

[0066] Figure 1 is a schematic diagram of a diffraction device of the present invention;

[0067] Figure 2 is a schematic cross-sectional view of a circular light-through hole of an incident collimator of a diffraction device of the present invention;

[0068] Figure 3 is a schematic cross-sectional view of a rectangular light aperture of an incident collimator of a diffraction device of the present invention;

[0069] Figure 4 is a top view of the receiving collimator of the present invention (viewed from the thin diameter end of the receiving collimator);

[0070] Figure 5 is a radial cross-sectional schematic diagram of a receiving collimator of the present invention;

[0071] Figure 6 It is a schematic diagram of measuring the diffraction angle 2θ by the array detector of the diffraction device of the present invention;

[0072] Figure 7 Schematic diagram of the orientation coordinate system of the crystal plane (hkl) measured inside the sample;

[0073] Figure 8 The orientation of the measured crystal plane (hkl) inside the sample is represented in this pole figure;

[0074] Fig. 9is a measurement and calculation block diagram used in an embodiment of the present invention;

[0075] Fig.10 It is a typical texture {111} pole figure of rolled aluminum plate.

[0076] In the figure: 1-X-ray tube, 2-incident collimator, 21-light hole of incident collimator, 3-sample, 31-translation stage, 32-Φ angle turntable, 33-Ψ angle turntable, 4-receiving collimator, 5-array detector, 51-shielding box of array detector, 6-light hole of receiving collimator, 61-inner cone of light hole, 62-outer cone of light hole, 7-incident X-ray passing through incident collimator, 8-diffracted ray passing through receiving collimator, 9-center of diffractometer circle, 10-positioning hole on receiving collimator, 11-X-ray absorber, 12-transmitted ray passing through X-ray absorber. DETAILED DESCRIPTION

[0077] The present invention is further described below in conjunction with the accompanying drawings and specific embodiments. It is pointed out that the following embodiments cannot be understood as limiting the scope of protection of the present invention. Some non-essential improvements and adjustments made by ordinary technicians in this field based on the contents of the present invention are all within the scope of protection of the present invention.

[0078] Example 1

[0079] This embodiment first describes a short-wavelength characteristic X-ray diffraction measurement device based on array detection. Figures 1 to 5 As shown, it includes an X-ray irradiation system, a sample stage and an X-ray detection system, etc. The X-rays emitted by the X-ray irradiation system pass through the incident collimator 2 to form an incident X-ray 7, which irradiates the measured part of the sample 3 fixed on the sample stage; the X-ray detection system is used to measure the intensity and distribution of the short-wavelength characteristic X-rays diffracted from the measured part inside the sample at a fixed point; wherein the X-ray irradiation system includes a radiation source and an incident collimator 2, the incident collimator 2 limits the divergence, cross-sectional shape and size of the X-ray beam incident to the sample 3, the radiation source includes a heavy metal target X-ray tube 1 with an atomic number greater than 55, and a high-voltage power supply with a supply voltage of more than 160kV and its controller; the X-ray detection system includes a receiving collimator 4 and an array detector 5 matched to the receiving collimator 4, and the X-ray beam 7 vertically enters the X-ray detection system. The X-ray irradiation system, the sample stage and the X-ray detection system are fixed on the same platform or a bracket.

[0080] Among them, the array detector 5 detects and receives the diffraction line 8 originated from the diffraction of the material at the measured part of the sample and passing through the light hole 6 of the receiving collimator 4, as well as other stray lines passing through the light hole 6 of the receiving collimator 4; the X-ray detection system is characterized in that: the center line of the incident X-ray beam 7 is the central axis of the light hole 6, the inner cone edge 61 of the light hole 6 and the extension line of the inner cone edge 62 of the light hole 6 intersect at a point on the center line of the incident X-ray beam 7, which point is the center point 9 of the diffractometer circle of the device, and the measured part of the sample is located at the center point 9 of the diffractometer circle of the device.

[0081] Among them, the X-ray irradiation system is an X-ray machine, the anode target of its X-ray tube is made of heavy metal materials such as tungsten, gold, uranium, etc. with an atomic number greater than 46, and emits short-wavelength X-rays at a voltage of 120kV-600kV.

[0082] Among them, each detection pixel of the array detector 5 is a single-photon measurement, and it is a multi-energy array detector with 2 or more energy thresholds. Through the set energy threshold, each pixel can measure a short-wavelength characteristic X-ray; in addition, the array detector 5 can also use an energy dispersion array detector, that is, each pixel can measure a multi-channel energy spectrum. The size specification range of each pixel of the array detector 5 is 0.02mm-0.2mm. The array detector 5 is a cadmium telluride array detector, or a cadmium zinc telluride array detector, or a gallium arsenide array detector.

[0083] The distance t from the center 9 of the diffractometer circle of the device to the array detector 5 is 150 mm to 1500 mm.

[0084] A positioning hole 10 is provided in the middle of the receiving collimator 4, the axis of the positioning hole 10 coincides with the center line of the incident collimator 2, and an X-ray absorber 11 is also provided in the positioning hole 10. The X-ray absorber 11 can prevent the array detector 5 from being damaged by the high-flux incident X-ray beam 7, and at the same time, can determine the position of the maximum intensity of the transmitted X-ray 12 by detecting the intensity distribution of the incident X-ray 12 passing through the X-ray absorber 9, that is, determine the center position of the Debye ring when diffraction occurs.

[0085] The incident collimator 2, the receiving collimator 4 and the shielding box 51 of the array detector 5 are all made of sufficiently thick heavy metal materials with a large atomic number such as tungsten, lead, gold, etc., and only allow X-rays to pass through the light hole 21 of the incident collimator 2, the light hole 6 and the positioning hole 10 of the receiving collimator 4, and pass through the receiving window of the shielding box 51 of the array detector 5 to enter the detection area of ​​the array detector 5, thereby shielding X-rays from other directions.

[0086] The sample 3 is fixed on the translation stage 31 of the sample stage, the translation stage 31 is fixed on the Φ angle rotation stage 32, the Φ angle rotation stage 32 is fixed on the Ψ angle rotation stage 33, and the rotation axes of the Φ angle rotation stage 32 and the Ψ angle rotation stage 33 are perpendicular to each other and intersect at the center of the diffractometer circle 9, so that: regardless of the Φ angle rotation or the Ψ angle rotation, the measured part of the sample 3 is always located at the center of the diffractometer circle 9. The center line of the positioning hole 10 and the center line of the incident collimator 2 are on a straight line, and are parallel to the Z axis of the translation stage 31 when Ψ=0°.

[0087] In a specific application, the light hole 21 of the incident collimator 2 is a single circular hole or a rectangular hole, the length of the incident collimator 2 is 20 mm to 200 mm, and the divergence of the incident collimator 2 is 0.02° to 0.5°; the length of the receiving collimator 4 is 100 mm to 1200 mm, and the angle between the inner cone edge 61 of the light hole 6 and the incident X-ray beam 7 is γ, and the value range of γ is 2° to 10°; the angle between the inner cone edge 61 and the inner cone edge 62 of the light hole 6 is δ, and the value range of δ is 0.5° to 6°, and γ+δ is not greater than 12°.

[0088] The short-wavelength characteristic X-ray diffraction measuring device is controlled by a computer for movement and measurement. The movements of the translation stage 31, the Φ angle rotating stage 32, and the Ψ angle rotating stage 33 are all controlled and implemented by the computer, and measurement and analysis are performed according to the program. The block diagram of the measurement, control, and calculation process involved is shown in Fig. 9 shown.

[0089] By using the short-wavelength characteristic X-ray diffraction measurement device, the Debye ring diffracted by the measured part can be measured intuitively, and a diffraction pattern similar to that of an X-ray diffraction flat-panel camera can be obtained.

[0090] Example 2

[0091] The samples of this embodiment are made of crystalline materials with a thickness less than the maximum measurable thickness. For example, for iron products, when UKα1 is used for testing, the maximum measurable thickness is about 10 mm.

[0092] Based on the diffraction device in the embodiment, the light hole 21 of the incident collimator 2 is selected to be a single circular hole, the length of the incident collimator 2 is 20mm~200mm, and the divergence of the incident collimator 2 is 0.02°~0.5°; the length of the receiving collimator 4 is 100mm~1200mm, and the angle between the inner cone edge 61 of the light hole 6 and the incident X-ray beam 7 is γ, and the value range of γ is 2°~10°; the angle between the inner cone edge 61 and the inner cone edge 62 of the light hole 6 is δ, and the value range of δ is 0.5°~6°.

[0093] The test and analysis method provided in this embodiment adopts the transmission method of short-wavelength characteristic X-rays, and the steps include:

[0094] Step 1, according to the material and thickness of the sample, select a short-wavelength characteristic X-ray of appropriate wavelength (such as Wkα1 radiated by a tungsten target X-ray tube, or Ukα1 radiated by a uranium target X-ray tube, etc.), and set two energy thresholds of the array detector 5 so that each pixel of the array detector detects the selected short-wavelength characteristic X-ray such as Wkα1, or Ukα1, etc.;

[0095] Step 2, fix the sample 3 on the sample stage, and place the measured part of the sample at the center of the diffractometer circle through the X, Y, and Z translation systems controlled by a computer;

[0096] Step 3, according to the selected short-wavelength characteristic X-ray, apply a tube voltage that is 1.5 times higher than the target excitation voltage, and start the X-ray irradiation system;

[0097] Step 4, using a computer to control exposure and measure the Debye ring diffracted by the crystalline material at the measured part, determine the peak, and compare it with the powder diffraction card to determine the phase of the crystalline material at the measured part;

[0098] Step 5, if the texture of the main phase of the measured part is to be tested, the measurement and analysis is carried out under computer control, and the step-scan measurement is carried out by rotating Ψ, and the Debye rings of the crystal material of the measured part in different Ψ directions are exposed and measured; the peak is determined, and the diffraction intensity of each diffraction crystal plane Debye ring in each direction is measured; and absorption correction is performed according to the diffraction path length to obtain the diffraction intensity of each diffraction crystal plane Debye ring in each direction after correction, and based on this, the transmission pole figures of multiple strong diffraction crystal planes and relatively strong diffraction crystal planes of the main phase are calculated; according to the crystal system type, the transmission pole figures of multiple strong diffraction crystal planes of the main phase are selected, and the full pole figure or orientation distribution function ODF of the corresponding diffraction crystal plane is calculated;

[0099] Note: Due to different crystal systems, the symmetry is different. The higher the symmetry of the crystal system, the fewer transmission pole figures are needed to calculate the full pole figure or orientation distribution function ODF of the corresponding diffraction crystal plane, that is, the fewer Debye rings of the main phase diffraction crystal plane that need to be calculated in the Debye rings of the crystal material diffraction of the measured part at the above different θ. For example, for the fcc crystal system, only the transmission pole figures of three strong diffraction crystal planes need to be tested to calculate the corresponding full pole figure or orientation distribution function ODF. For example, only the transmission pole figures of the three strong lines of the 111, 200, and 220 crystal planes need to be measured to calculate the full pole figure or orientation distribution function ODF of the corresponding diffraction crystal plane.

[0100] Step 6: If the residual stress of the measured part is to be tested, the measurement and analysis are performed under computer control;

[0101] (1) Residual stress test for non-strong textured material samples;

[0102] a) For a sample in a plane stress state, the sample is rotated by rotating the angle Ψ so that the surface normal direction of the measured part of the sample and the corresponding part of the stress-free standard coincides with the incident light beam 7, and the Debye rings diffracted by each crystal plane of the measured part of the sample and the corresponding part of the stress-free standard are exposed and measured respectively, and the diffraction angle 2θ of each crystal plane in each direction of the measured part of the sample is obtained by peak determination. s-hkl , and the diffraction angle 2θ of each crystal plane in each direction of the corresponding part of the stress-free standard sample 0-hkl Then, for a certain (hkl) crystal plane, such as Al(111) crystal plane, according to the strain

[0103] ε=(sinθ 0-hkl / sinθ s-hkl )-1……………………(1)

[0104] The calculated angle with the surface normal direction of the sample tested part is 90°-θ hkl , the strain ε(90°-θ hkl , Φ) and its distribution;

[0105] Since the wavelength of short-wavelength characteristic X-rays is as short as about 0.02nm, the diffraction angle 2θ of the strong diffraction crystal plane and the relatively strong diffraction crystal plane of most substances is less than 11°, that is, θ hkl ﹤5.5° If the short wavelength characteristic X-ray selected is Wk α1 , the diffraction angle 2θ for the crystal plane Al(111) 111 ≈5.12°,θ 111 ≈2.56°, so the strain ε(90°-θ hkl , Φ) is very different from the strain ε(90°, Φ) in each direction of the hkl crystal plane perpendicular to the surface normal direction of the sample being measured, that is, less than 5.5°, and can be regarded as equal 0°≤Φ≤180°. Let ε(90°, Φ)ε=(90°-θ hkl , Φ).

[0106] According to the stress-strain relationship of plane stress problems in elastic mechanics, in the xy plane, the x-axis and y-axis are known to be the principal stress directions, and the strain ε in the x-direction is measured respectively. xx , that is, ε(90°-θ hkl , 90°), and the strain ε in the y direction yy , that is, ε(90°-θ hkl , 0°), and then according to the following formula

[0107]

[0108]

[0109] The two principal stresses σ are calculated xx , σ yy , where E hkl is the elastic modulus of the hkl crystal plane, ν hkl is the Poisson's ratio of the hkl crystal plane.

[0110] The measured strains ε(90°-θ hkl , 90°) and ε(90°-θ hkl , 0°), the two principal stresses σ perpendicular to the surface normal direction of the sample measured part are calculated by formulas (2) and (3) respectively: xx , σ yy , that is, the plane stress tensor σ of the measured part of the sample.

[0111] If the directions of the two principal stresses are unknown, according to the theory of elasticity, it is only necessary to measure the strains in three directions to calculate the magnitude and direction of the two principal stresses and one shear stress, that is, the plane stress tensor σ of the measured part of the sample.

[0112] Note: If Figure 7 , Figure 8 As shown, (Ψ, Φ) is the coordinate on the hkl crystal plane polar diagram to represent the crystal plane direction, the X axis and the Y axis are perpendicular. Taking the rolled plate as an example, (90°, 0°) represents the rolling direction RD, which is often defined as coinciding with the Y axis, and (90°, 90°) represents the transverse direction TD, which is often defined as coinciding with the X axis; Ψ is the angle from the normal ND, which is often defined as coinciding with the Z axis. Obviously, 0°≤Ψ≤90°; Φ is the angle of the ND direction, which is rotated counterclockwise from the Z axis, and starts from the RD direction Y axis.

[0113] Furthermore, if the Debye rings of multiple strong diffraction crystal planes and relatively strong diffraction crystal planes hkl are measured at the same time, the ε(90°-θ hkl , Φ) and its distribution; the ε(90°-θ hkl , Φ) and their distribution, and calculate them separately, we can get the corresponding multiple stress tensors σ, and take the average value to get a more accurate stress tensor That is, the stress tensor can be calculated by exposing and measuring the measured part of the sample and the corresponding part of the stress-free standard sample once.

[0114] b) For samples with strong texture, the direction of strain measurement depends on the texture. It is necessary to select the direction of the diffraction intensity maximum (large pole density or strong diffraction spot) of the strong diffraction crystal plane (hkl) to be measured on the outermost circle of the (hkl) crystal plane pole figure, and between the two principal stresses εxx , ε yy direction or nearby direction.

[0115] The sample is rotated by rotating the angle Ψ so that the surface normal direction of the measured part of the sample and the corresponding part of the stress-free standard coincides with the incident light beam 7, and the Debye rings diffracted by each crystal plane of the measured part of the sample and the corresponding part of the stress-free standard are exposed and measured respectively. The strong diffraction spots on the Debye rings are determined to determine the peaks, and the angles α and β are determined; the angle α is the angle of deflection of a pole density maximum from the x-axis, and the angle β is the angle of deflection of another pole density maximum from the y-axis, such as the transverse TD on the outermost circle of the Al{111} pole figure of the rolled aluminum plate and the direction deviating from the rolling direction RD by about 20°, such as α=0°, β=20°, such as Fig.10 As shown;

[0116] According to method a) to measure ε(90°-θ hkl , 90°+α), ε(90°-θ hkl ,β), similarly, given that θ hkl <5.5°, that is, ε(90°, Φ)=ε(90°-θ hkl , Φ), the measured strain ε(90°-θ hkl , 90°+α) is recorded as ε α , the measured strain ε(90°-θ hkl , β) is denoted as ε β , and substitute into the following two formulas

[0117]

[0118]

[0119] The two principal stresses σ can be calculated xx , σ yy Strain in the direction ε xx and ε yy , and then ε xx and ε yy Substitute into formula 2 and 3, and finally, the two principal stresses σ are calculated. xx , σ yy , that is, the stress tensor σ at the measured part of the sample.

[0120] In summary, for a sample in a plane stress state, the sample 3 is rotated by rotating Ψ so that the surface normal direction of the measured part of the sample and the corresponding part of the stress-free standard coincides with the incident light beam 7, that is, the incident light beam 7 is perpendicular to the sample 3, and the Debye rings diffracted by each crystal plane of the measured part of the sample and the corresponding part of the stress-free standard are exposed and measured once respectively. Then, the plane stress tensor σ of the measured part of the sample perpendicular to the surface normal direction of the measured part of the sample can be calculated according to formulas (2) and (3).

[0121] (2) For samples in a general stress state, a strong or relatively strong diffraction crystal plane (hkl) is selected as the diffraction crystal plane for testing. At least six strains in the (Ψ, Φ) directions need to be measured. The six Ψ angles cannot be all the same, and the differences between the six Φ angles should be as large as possible.

[0122] a) For samples of non-strong textured materials, first rotate to Ψ=Ψ1, and expose the Debye rings diffracted by each crystal plane at the measured part of the sample and the corresponding part of the stress-free standard sample. Then, the sample is rotated to Ψ=Ψ2, and the difference between Ψ2 and Ψ1 is as large as possible. The measured part of the sample and the corresponding part of the stress-free standard sample are exposed to measure the Debye rings diffracted by each crystal plane. Peak determination, select the peak determination results 2θ in the six directions of the hkl crystal plane s-hkl and 2θ 0-hkl ,, calculated by formula (1) we get 6 (Ψ i , Φ i ) direction hkl crystal plane strain ε(Ψ i , Φ i ).

[0123] ε(Ψ i ,Φ i )=a i 2 ε xx +b i 2 ε yy +c i 2 ε yy +2a i b i ε xy +2b i c i ε yz +2c i a i ε zx ………………(6)

[0124] Among them, a i 、b i 、c i are the strain ε(Ψ i ,Φ i ) direction cosines in X, Y, and Z, a i = sinΨ i cosΦ i , b i = sinΨ i sinΦ i , c i =cosΨ i .

[0125] The strains ε(Ψi , Φ i ) and its direction cosines are substituted into Equation 6 and the linear equations are solved simultaneously to obtain the strain ε ij (i=x,y,z; j=x,y,z); by ε ij The three principal strains ε can be obtained by linear transformation D XX , ε D YY , ε D ZZ Finally, the stress tensor σ or three principal stresses σ of the measured part of the sample are obtained. D XX , σ D YY , σ D ZZ size and direction;

[0126]

[0127] In formula (7), E is the elastic modulus of the (hkl) crystal plane, and ν is the Poisson's ratio of the (hkl) crystal plane.

[0128] Obviously, if the three principal stresses σ are known D XX , σ D YY , σ D ZZ direction, only three Ψ i , Φ i The strain in the direction can be used to calculate the stress tensor σ of the measured part of the sample. That is, the measured part of the sample and the corresponding part of the stress-free standard sample are exposed and measured twice respectively, and the stress tensor σ of the measured part of the sample can be calculated.

[0129] Furthermore, since the Debye rings of multiple strong diffraction crystal planes and relatively strong diffraction crystal planes (hkl) are measured simultaneously, multiple ε(Ψ i , Φ i ), we can get the corresponding multiple stress tensors σ, and take the average value to get a more accurate stress tensor That is, the stress tensor can be accurately calculated by exposing and measuring the measured part of the sample and the corresponding part of the stress-free standard sample twice.

[0130] b) For residual stress testing of samples of strongly textured materials, the direction of strain measurement depends on the texture conditions. It is necessary to select the direction of the diffraction intensity maximum (large extreme density or strong diffraction spot) of the strongly diffraction crystal plane (hkl) to be measured to measure the strain.

[0131] By rotating the Ψ exposure to measure the Debye rings diffracted by the measured part of the sample at different Ψ angles and the corresponding part of the stress-free standard sample, six strong diffraction spots of the strong diffraction crystal plane and the relatively strong diffraction crystal plane (hkl), that is, six strong diffraction spots with the maximum diffraction intensity, are selected, the peaks are determined, and the strain ε (Ψ i , Φ i ), and then through linear transformation, we can get three principal strains ε D XX , ε D YY , ε D ZZ , and then according to the elastic mechanics formula 7, the stress tensor σ or the three principal stresses σ of the measured part of the sample are finally obtained D XX , σ D YY , σ D ZZ size and direction.

[0132] It should be noted that the strains in the six directions may not be in the same {h1k1l1} crystal plane family, that is, the strains in some directions are measured using the (h1k1l1) crystal plane, while the strains in the remaining directions are measured using the (h2k2l2) crystal plane. However, in the formula for calculating stress from strain, the elastic modulus E corresponding to the measured strain is used. hkl , Poisson's ratio ν hkl .

[0133] Step 7: If you want to test the internal phase, texture, and stress of another part of the sample, repeat steps 4, 5, and 6 until all the parts to be tested are tested. The computer processes the data to obtain the internal phase, texture, stress, etc. and their distribution of each part of the sample.

[0134] Example 3

[0135] The sample of this embodiment is a crystalline material product with a thickness less than the maximum measurable thickness. For example, for an aluminum product, when the WKα1 test is used, the maximum measurable thickness is about 40 mm. The device used in this embodiment is basically the same as that in embodiment 1, except that:

[0136] The X-ray irradiation system and the X-ray detection system are fixed on the Ψ angle turntable 33, and the Ψ angle turntable 33 is fixed on a platform together with the sample stage composed of a translation stage 31 and a Φ angle turntable 32. The sample 3 is fixed on the translation stage 31 of the sample stage, and the translation stage 31 is fixed on the Φ angle turntable 32. The Φ angle turntable 32 is fixed on the platform, and the rotation axes of the Φ angle turntable 32 and the Ψ angle turntable 33 are perpendicular to each other and intersect at the center of the diffractometer circle 9, so that: regardless of the Φ angle rotation or the Ψ angle rotation, the measured part of the sample 3 is always located at the center of the diffractometer circle 9.

[0137] The test and analysis method steps are similar to those in Example 2.

[0138] Example 4

[0139] The sample in this embodiment is a 20mm thick 200mm RD × 200mm RD rolled aluminum plate, which is in a plane stress state, and the directions of its principal stress and principal strain are in the rolling direction RD and transverse direction TD respectively. The diffraction crystal plane is the Al(111) crystal plane, Fig.10 This is its typical texture {111} pole figure. In the outermost circle of the pole figure, refer to Figure 7 and Figure 8 The strain and stress directions in Fig.10 As shown, in the (90°, 90°) and (90°, 270°) directions, α=0° or 180°, that is, the lateral direction is the direction of the maximum diffraction intensity of the Al(111) crystal plane; in the (90°, -18.5°), (90°, 18.5°) and (90°, 161.5°), (90°, 198.5°) directions, that is, the 18.5° direction deviating from the rolling direction is the direction of the maximum diffraction intensity of the Al(111) crystal plane.

[0140] The device and method used in this embodiment refer to those in Embodiment 1, and the main difference lies in the selection of various parameters, which are as follows.

[0141] The diffraction device used includes an X-ray irradiation system consisting of a 225KV reflective tungsten target X-ray machine 1 + an incident collimator 2, a sample stage consisting of a translation stage 31 + a Φ angle turntable 32 + a Ψ angle turntable 33, and an X-ray detection system consisting of a receiving collimator 4 + an array detector 5 + a shielding box 51 of the array detector. The device is controlled by a computer program to perform measurement and analysis. The X-ray irradiation system, the sample stage and the X-ray detection system are fixed on the same platform or a bracket.

[0142] The incident X-ray 7 is perpendicular to the X-ray detection system, and the array detector 5 detects and receives the diffraction line 8 originated from the diffraction of the material at the measured part of the sample and passing through the annular light hole 6 of the receiving collimator 4, and the scattered rays from other directions are shielded by the receiving collimator 4 and the shielding box 51 of the array detector 5; the center line of the incident X-ray 7 is the central axis of the annular light hole 6, and the extension lines of the inner cone edge 61 of the light hole 6 and the outer cone edge 62 of the light hole 6 intersect at a point on the center line of the incident X-ray 7, which is the center point of the diffractometer circle 9 of the device, and the measured part of the sample 3 is located at the center point 9 of the diffractometer circle of the device.

[0143] The sample 3 is fixed on the translation stage 31 of the sample stage, the translation stage 31 is fixed on the Φ angle turntable 32, the Φ angle turntable 32 is fixed on the Ψ angle turntable 33, the Ψ angle turntable 33 is fixed on the same platform, and the rotation axes of the Φ angle turntable 32 and the Ψ angle turntable 33 are perpendicular to each other and intersect at the center of the diffractometer circle 9, so that: regardless of the Φ angle rotation or the Ψ angle rotation, the measured part of the sample 3 is always located at the center of the diffractometer circle 9.

[0144] The array detector 5 is a 2 mm thick cadmium telluride array detector, each detection pixel size is 0.1 mm × 0.1 mm, each detection pixel is single photon measured, and it is a dual-energy array detector with 2 energy thresholds, each pixel of which can measure the diffracted Wkα1 characteristic X-ray.

[0145] The length of the incident collimator 2 is 100 mm, the cross section of the light-through hole 21 thereof is a single square hole with a side length of 0.2 mm, and the divergence of the incident collimator 2 is 0.45°.

[0146] The length of the receiving collimator 4 is 200 mm, and the cross section of the light hole 6 is a single annular hole. The half-apex angle γ of the inner cone edge 61, that is, the angle γ between the inner cone edge 61 and the incident X-ray beam 7, is 4.5°; the angle δ between the inner cone edge 61 and the inner cone edge 62 of the light hole 6 is 1.5°; the radius of the annular hole at the small end of the receiving collimator 4 close to the sample 3 is 3.93 mm and 5.25 mm respectively; the radius of the annular hole at the large end of the receiving collimator 4 installed on the array detector 5 is 19.67 mm and 26.28 mm respectively; the measured part of the sample 3, that is, the center of the diffractometer circle 9, is 50 mm away from the small end of the receiving collimator 4;

[0147] The distance from the center of the diffractometer 9 to the array detector 5 is 250 mm;

[0148] A circular positioning hole 10 with a diameter of 1 mm is provided in the middle of the receiving collimator 4, the axis of the positioning hole 10 coincides with the center line of the light hole 21 of the incident collimator 2, and an X-ray absorber 11 is also provided in the positioning hole 10. The X-ray absorber 11 can prevent the array detector 5 from being directly irradiated and damaged by the high-flux incident X-ray beam 7, and at the same time, can determine the position of the maximum intensity of the incident X-ray beam passing through the X-ray absorber 9 by detecting the intensity distribution of the incident X-ray 12 passing through the X-ray absorber 11, that is, determine the center position of the Debye ring when diffraction occurs.

[0149] The incident collimator 2, the receiving collimator 4 and the shielding box 51 of the array detector 5 are all made of sufficiently thick heavy metal materials such as tungsten, lead, gold, etc., and only allow the diffraction rays 8 passing through the light holes 21 of the incident collimator 2 and the light holes 6 of the receiving collimator 4, as well as the incident X-rays 12 passing through the positioning holes 10 and their X-ray absorbers 11, to enter the detection area of ​​the array detector 5 through the receiving window of the shielding box of the array detector 5, thereby shielding stray X-rays from other parts and other directions.

[0150] The test analysis method of this embodiment comprises the following steps:

[0151] Step 1: The sample is a 200mm×200mm 20mm thick rolled aluminum plate. By setting the upper and lower thresholds of the detected photon energy to 55keV and 61keV respectively, the short-wavelength characteristic X-ray Wkα is selected, and each pixel of the array detector detects Wkα. In view of the coarse grains of the rolled aluminum plate, the swaying method is used to increase the number of grains involved in the diffraction spectrum in the following exposure measurement to suppress the influence of the coarse grains on the measurement;

[0152] Step 2, fix a 20 mm thick rolled aluminum plate with a size of 200 mm in RD direction × 200 mm in TD direction on the sample stage so that the incident ray is perpendicular to the aluminum plate, the TD direction is parallel to the X axis, and the RD direction is parallel to the Y axis, and the measured part is placed at the center of the diffractometer circle through the X, Y, and Z translation systems;

[0153] Step 3, set the tube voltage to 200Kv, the tube current to 4mA, and start the X-ray irradiation system;

[0154] Step 4, the measurement and analysis is performed under computer control, the sample is exposed and measured for 100 seconds, the Debye ring diffracted by the crystalline material at the measured part is determined, and the peak is compared with the powder diffraction card to determine that the Debye ring of the crystalline material at the measured part belongs to Al111 whose main phase is fcc crystal system;

[0155] Step 5, the measurement and analysis is performed under computer control, and the step-scan measurement is performed by rotating Ψ, and the Debye rings diffracted by the crystal material at different locations of the measured parts are measured for 200 seconds respectively; the peak is determined, and the diffraction intensity of the Debye rings of each diffraction crystal plane in each direction is measured; and the texture is measured to be a rolling texture;

[0156] Step 6, the computer controls the measurement and analysis to test the internal residual stress of the strongly textured rolled aluminum plate in the plane stress state. The principal stress directions are the rolling direction RD and the transverse direction TD. The two principal stresses can be calculated by measuring the strain in the two directions. 111 ≈2.56°, strain ε(90°-θ 111, Φ) is very different from the strain ε(90°, Φ) in each direction of the 111 crystal plane perpendicular to the surface normal direction of the sample being tested, and can be considered equal, that is, ε(90°, Φ)=ε(90°-θ 111 ,Φ), so through two (90°-θ 111 The two principal stresses can be calculated by measuring the strain in the φ direction, as follows:

[0157] a. By moving the translation stage 31, the measured part of the sample is translated to the center of the diffractometer circle 9; by rotating Ψ, the sample is rotated to Ψ = 0°, so that the incident light beam 7 is vertically incident on the sample and passes through the measured part of the sample; the exposure measurement is performed for 200s, and the Debye ring diffracted by the Al (111) crystal plane is measured; on the measured Debye ring diffracted by the Al (111) crystal plane, there are 6 diffraction intensity maximum directions, which are (90°-θ 111 , 90°) and (90°-θ 111 , 270°) direction, and the (90°-θ 111 , -β), (90°-θ 111 ,β),(90°-θ 111 , 180°-β), (90°-θ 111 , 180°+β) direction; determine the peak, and obtain the 2θ deviation from the α angle direction near the two transverse TD of the sample tested part. s-111TDα , 4 rolling directions near RD with a deviation of 2θ from the β angle direction s-111RDβ ;

[0158] b. By moving the translation stage, the corresponding part of the stress-free standard sample is translated to the center of the diffractometer circle; by rotating the sample to Ψ = 0°, the incident light beam 7 is vertically incident on the stress-free standard sample and passes through the corresponding part of the stress-free standard sample; similarly, the exposure measurement is performed for 200s, and the 2θ deviation from the α angle direction near the two transverse TDs of the corresponding thickness part of the stress-free standard sample can be measured and calculated. 0-111TDα , 4 rolling directions near RD with a deviation of 2θ from the β angle direction 0-111RDβ ;

[0159] c. Select one peak result 2θ that deviates from the α angle direction near the transverse TD from the peak results of the measured part of the sample and the corresponding thickness part of the stress-free standard sample. s-111TDα and 2θ 0-111TDα , and a peak result 2θ in the β angle direction that deviates from the rolling direction near RD s-111RDβ and 2θ 0-111RDβ ,, or the arithmetic mean of the two transverse TD peak determination results and the arithmetic mean of the four α angle peak determination results that deviate from the rolling direction RD, according to formula (1)ε=(sinθ 0-111 / sinθs-111 )-1, and the strain ε of the sample measured part near the transverse TD deviating from the α angle direction is calculated respectively α =ε(90°-θ 111 , 90°), and the strain ε that deviates from the β angle direction near the rolling direction RD β =ε(90°-θ 111 , 18.5°), at this time α=0°, β=18.5°;

[0160] d. The measured strain ε α , ε β Substituting α=0° and β=18.5° into formula (4) and (5), the two principal strains ε of the measured part of the sample can be calculated. xx and ε yy ; Then ε xx and ε yy Substituting into formula (2) and (3), the two principal strains σ of the measured part of the sample can be calculated: xx and σ yy That is, σ TD and σ RD , and obtain the stress tensor σ of the measured part of the sample;

[0161] Step 7: If you want to test the stress of other parts inside the aluminum plate sample, repeat a, b, c, d until all the parts to be tested are tested, and the internal stress and its distribution of the aluminum plate sample are obtained.

[0162] Example 5

[0163] The sample of this embodiment is a 100mm×15mm nickel-based high-temperature alloy with a thickness of 6mm and directionally crystallized. The device used in this embodiment is the same as that in embodiment 3, and the main difference is that:

[0164] (1) Using a 225KV reflection gold target X-ray machine 1 as the radiation source, measure the diffraction pattern of Aukα;

[0165] (2) The length of the incident collimator 2 is 50 mm, the cross section of the light-through hole 21 is a single circular hole with a diameter of 0.05 mm, and the divergence of the incident collimator 2 is 0.11°;

[0166] (3) The array detector 5 is a 3 mm thick gallium arsenide array detector, each detection pixel size is 0.055 mm × 0.055 mm, each detection pixel is single photon measurement, and it is a dual-energy array detector with 2 energy thresholds, each pixel of which can measure the diffracted Aukα characteristic X-ray.

[0167] (4) The length of the receiving collimator 4 is 300 mm, and the cross section of its light hole 6 is a single annular hole. The semi-apex angle γ of its inner cone edge 61, that is, the angle γ between the inner cone edge 61 and the incident X-ray beam 7 is 3.5°; the angle δ between the inner cone edge 61 and the inner cone edge 62 of the light hole 6 is 4.0°; the radius of the annular hole at the small end close to the sample 3 is 6.1 mm and 13.2 mm respectively; the radius of the annular hole installed at the large end of the array detector 5 is 24.5 mm and 52.7 mm respectively; the distance from the measured part of the sample 3, that is, the center of the diffractometer circle 9, to the small end of the receiving collimator 4 is 100 mm; the distance from the center of the diffractometer circle 9 to the array detector 5 is 400 mm;

[0168] (5) A circular positioning hole 10 with a diameter of 2 mm is provided in the middle of the receiving collimator 4, the axis of the positioning hole 10 coincides with the center line of the light hole 21 of the incident collimator 2, and an X-ray absorber 11 is also provided in the positioning hole 10. The X-ray absorber 11 can prevent the array detector 5 from being directly irradiated and damaged by the high-flux incident X-ray beam 7, and at the same time, can determine the position of the maximum intensity of the incident X-ray beam 12 passing through the X-ray absorber 11 by detecting the intensity distribution of the incident X-ray 12 passing through the X-ray absorber 11, that is, determine the center position of the Debye ring when diffraction occurs.

[0169] This test and analysis method refers to Example 4, the main difference from which is:

[0170] (1) Step 1: The sample is a 100 mm × 15 mm nickel-based high-temperature alloy with a thickness of 6 mm. The upper and lower energy thresholds of the detected photons are set to 65 keV and 73 keV respectively, and the short-wavelength characteristic X-ray Aukα is selected. Each pixel of the array detector detects Aukα;

[0171] (2) Step 2, the length direction is parallel to the X-axis, and the width direction is parallel to the Y-axis;

[0172] (3) Step 3, set the tube voltage to 200Kv, the tube current to 12mA, and turn on the X-ray irradiation system;

[0173] (4) Step 4: The sample is exposed and measured for 200 seconds. Based on the comparison of the three strong lines, it is determined that the main phases of the crystalline material in the measured part are simple cubic AlNi3 and fcc Ni;

[0174] (5) Step 5, measuring the diffraction intensity of the Debye spots or rings of each diffraction crystal plane at different Ψ angles in each direction, and determining that it is a strongly oriented texture;

[0175] (6) Step 6: From the test results of step 5 above, select 6 strong diffraction spots of AlNi3, which can be 6 strong diffraction spots of different diffraction crystal planes and diffraction directions, and expose and measure the measured part of the sample and the corresponding part of the stress-free standard sample for 400 seconds, for a total of 12 times. The strains in 6 directions are measured and calculated, and then substituted into formula (6) to solve the linear equations together to obtain the strain ε ij (i=x,y,z; j=x,y,z); by ε ij The three principal strains ε can be obtained by linear transformation D XX , ε D YY , ε D ZZ and its direction; then the calculated ε D XX , ε D YY , ε D ZZ Substituting into formula (7), the stress tensor σ or the three principal stresses σ at the measured part of the sample can be calculated. D XX , σ D YY , σ D ZZ Size and direction

[0176] It should be noted that the elastic modulus E used in the calculation hkl and Poisson's ratio ν hkl are the values ​​of hkl of the corresponding crystal planes respectively.

[0177] Example 6

[0178] The sample of this embodiment is a low-carbon rolled steel plate with a thickness of 8 mm and a size of 400 mm in RD direction and 300 mm in TD direction, which is in a plane stress state, and its principal stress directions are RD and TD respectively. The device used in this embodiment is the same as that in embodiment 4, and the main difference therefrom is that:

[0179] (1) Using a 320KV reflection uranium target X-ray machine 1 as the radiation source, measure the diffraction pattern of Ukα1;

[0180] (2) The length of the incident collimator 2 is 75 mm, the cross section of the light-through hole 21 is a single circular hole with a diameter of 0.05 mm, and the divergence of the incident collimator 2 is 0.08°;

[0181] (3) The array detector 5 is a 2 mm thick cadmium telluride array detector, each detection pixel of which has a size of 0.075 mm × 0.075 mm, each detection pixel of which is single-photon measurement, and a dual-energy array detector with two energy thresholds, each pixel of which can measure the diffracted Ukα1 characteristic X-ray;

[0182] (4) The length of the receiving collimator 4 is 675 mm, and the cross section of its light hole 6 is a single annular hole. The semi-apex angle γ of its inner cone edge 61, that is, the angle γ between the inner cone edge 61 and the incident X-ray beam 7 is 3.0°; the angle δ between the inner cone edge 61 and the inner cone edge 62 of the light hole 6 is 4.0°; the radius of the annular hole at the small end close to the sample 3 is 3.9 mm and 9.2 mm respectively; the radius of the annular hole at the large end installed on the array detector 5 is 39.3 mm and 92.1 mm respectively; the measured part of the sample 3, that is, the center of the diffractometer circle 9, is 75 mm away from the small end of the receiving collimator 4; the distance from the center of the diffractometer circle 9 to the array detector 5 is 750 mm;

[0183] (5) A circular positioning hole 10 with a diameter of 2 mm is provided in the middle of the receiving collimator 4, which is used to determine the position of the maximum intensity of the incident X-ray beam 12 passing through the X-ray absorber 11, that is, to determine the center position of the Debye ring when diffraction occurs.

[0184] The test and analysis method used in this embodiment refers to that in Embodiment 4, the main difference therefrom is that:

[0185] (1) Step 1: The sample is a low-carbon rolled steel plate with a thickness of 8 mm and a length of 400 mm in RD direction and 300 mm in TD direction, which is in a plane stress state, and its principal stress directions are RD and TD respectively; by setting the upper and lower energy thresholds of the detection photons to 93 keV and 103 keV respectively, the short-wavelength characteristic X-ray Aukα is selected, and each pixel of the array detector detects Aukα;

[0186] (2) Step 3, set the tube voltage to 280Kv, the tube current to 5mA, and start the X-ray irradiation system;

[0187] (3) Step 4: The sample is exposed and measured for 900 seconds. Based on the comparison of the three strong lines, it is determined that the main phase of the crystalline material in the measured part is α-Fe of the bcc crystal system;

[0188] (4) Step 5, rotating the sample 3 by rotating Ψ, so that the incident light beam 7 vertically enters the sample and passes through the measured part of the sample, and vertically enters the stress-free standard sample and passes through its corresponding part; respectively, the exposure measurement is performed for 1200 s, and the Debye rings diffracted by the strong diffraction crystal planes such as α-Fe(110), α-Fe(200), and α-Fe(211) at the measured part of the sample and the corresponding part of the stress-free standard sample are measured;

[0189] (5) On the Debye ring of the α-Fe(110) crystal plane diffraction of the measured sample, there are four directions of maximum diffraction intensity, namely, the (90°-θ 110 , 90°) and (90°-θ 110 , 270°) direction, and (90°-θ near the two rolling directions RD 110 , 0°), (90°-θ 110 , 180°) direction, θ 110 The peak is about 1.78°, and the 2θ values ​​near the two transverse TDs of the sample are obtained. s-110TD , 2θ near the rolling direction RD s-110RD Similarly, on the Debye ring of the α-Fe(110) crystal plane diffraction at the corresponding part of the stress-free standard sample, the 2θ near the two transverse TDs at the corresponding part of the stress-free standard sample were obtained respectively. 0-110TD , 2θ near the rolling direction RD 0-110RD

[0190] (6) Select one transverse TD peak result and one rolling direction RD peak result from the peak results of the measured part of the sample and the corresponding thickness part of the stress-free standard sample, or the arithmetic mean of two transverse TD peak results and the arithmetic mean of two rolling direction RD peak results, and calculate it by ε=(sinθ 0-110 / sinθ s-110 )-1, and the transverse TD strain ε(90°-θ 110 , 90°) and the strain ε(90°-θ 110 , 0°);

[0191] (7) Given that θ 110 ≈1.78°<5.5°, let ε TD =ε(0°,90°)9=ε(90°-θ 110 , 90°), ε RD =ε(90°,0°)=ε(90°-θ 110 , 0°), and the measured strain ε TD and ε RD Substituting into formula (2) and (3), we can calculate the principal stresses σ in two directions: TD and σ RD , that is, the tensor σ of the measured part of the sample.

[0192] (8) Similarly, on the Debye ring of the α-Fe (200) or α-Fe (211) crystal plane diffraction of the measured part of the sample, several directions of the maximum diffraction intensity are measured to measure the strain, and the two principal strains ε are calculated by formulas (4) and (5) TD and εRD , and then the principal stresses σ in two directions are calculated by formulas (2) and (3): TD and σ RD , that is, the tensor σ of the sample being measured. To improve accuracy, take their arithmetic mean to obtain the principal stress σ in two directions of the sample being measured TD and σ RD , that is, the stress tensor σ.

[0193] Using the measuring device and method in Example 4, taking the measurement of the Al (111) crystal plane diffraction spectrum of a portion (the measured portion) inside a 20 mm thick aluminum plate as an example, it only takes a few minutes, and the test efficiency is about 10 times higher than the technical solution in the background technology disclosed in the literature; moreover, a precision goniometer with a double turntable is not required, and the structure and operation method are greatly simplified.

Claims

1. A short-wavelength characteristic X-ray diffraction measurement device based on array detection, comprising an X-ray irradiation system, a sample stage and an X-ray detection system; in, The X-ray irradiation system comprises a radiation source and an incident collimator (2), wherein the radiation source comprises a heavy metal target X-ray tube (1) having an atomic number greater than 55, and a high voltage power supply having a supply voltage of more than 160 kV and a controller thereof; the X-rays emitted by the X-ray irradiation system pass through the incident collimator (2) to form an incident X-ray beam (7) and irradiate a measured portion of a sample fixed on a sample stage; the X-ray detection system is used for point-measuring the intensity and distribution of short-wavelength characteristic X-rays diffracted from the measured portion inside the sample; the X-ray detection system comprises a receiving collimator (4) and an array detector (5) matched to the receiving collimator (4); Features: The array detector (5) detects and receives only the diffraction lines (8) originating from the diffraction of the material in the sample test site and passing through the light aperture A (6) of the receiving collimator (4), as well as other stray lines passing through the light aperture A (6) of the receiving collimator (4); The extension line of the inner cone edge 1 (61) of the light hole A (6) and the extension line of the inner cone edge 2 (62) thereof intersect on the center line of the incident X-ray beam (7), and the intersection point is the center of the diffractometer circle of the device, and the measured part of the sample is located at the center of the diffractometer circle of the device; Each detection pixel of the array detector (5) is single-photon measurement, and a multi-energy array detector with two or more energy thresholds is used. Through the set energy threshold, each pixel can measure a short-wavelength characteristic X-ray; or, the array detector (5) uses an energy dispersion array detector; The length of the receiving collimator (4) is 100 mm to 1200 mm, the angle between the inner cone edge 1 (61) of the light hole A (6) of the receiving collimator (4) and the incident X-ray beam (7) is γ, and the value range of γ is 2° to 10°; the angle between the inner cone edge 1 (61) and the inner cone edge 2 (62) of the light hole A (6) is δ, and the value range of δ is 0.5° to 6°, and γ+δ is not greater than 12°.

2. The short-wavelength characteristic X-ray diffraction measuring device according to claim 1, characterized in that: The light-through hole B (21) of the incident collimator (2) is a circular hole or a rectangular hole. The length of the incident collimator (2) is 20 mm to 200 mm, and the divergence is 0.02° to 0.5°.

3. The short-wavelength characteristic X-ray diffraction measuring device according to claim 2, characterized in that: A positioning hole (10) is provided in the middle of the receiving collimator (4), the axis of the positioning hole (10) coincides with the center line of the incident collimator (2), and an X-ray absorber (11) is also provided in the positioning hole (10); The incident collimator (2), the receiving collimator (4) and the shielding box of the array detector (5) are all made of heavy metal materials that meet shielding requirements and are used to shield stray X-rays from other parts and other directions, and only allow X-rays to pass through the light hole B (21) of the incident collimator (2), the light hole A (6) of the receiving collimator (4), the positioning hole (10) and its X-ray absorber, and then pass through the receiving window of the shielding box of the array detector (5) to enter the detection area of ​​the array detector (5).

4. The short-wavelength characteristic X-ray diffraction measuring device according to claim 3, characterized in that: The X-ray irradiation system, the sample stage and the X-ray detection system are fixed on the same platform, the sample (3) is fixed on the translation stage (31) of the sample stage, the translation stage (31) is fixed on the Φ angle turntable (32), the Φ angle turntable (32) is fixed on the Ψ angle turntable (33), the Ψ angle turntable (33) is fixed on the same platform, and the rotation axes of the Φ angle turntable (32) and the Ψ angle turntable (33) are perpendicular to each other and intersect at the center of the diffractometer circle (9), so that: regardless of the Φ angle rotation or the Ψ angle rotation, the measured part of the sample (3) is always located at the center of the diffractometer circle (9), and its coordinates are set to (0,0,0); or, The X-ray irradiation system and the X-ray detection system are fixed on the Ψ angle turntable (33), and the Ψ angle turntable (33) is fixed on a platform together with a sample stage composed of a translation stage (31) and a Φ angle turntable (32). The sample (3) is fixed on the translation stage (31) of the sample stage, and the translation stage (31) is fixed on the Φ angle turntable (32). The Φ angle turntable (32) is fixed on the one platform, and the rotation axes of the Φ angle turntable (32) and the Ψ angle turntable (33) are perpendicular to each other and intersect at the center of the diffractometer circle (9), so that: regardless of the Φ angle rotation or the Ψ angle rotation, the measured part of the sample (3) is always located at the center of the diffractometer circle (9), and its coordinates are set to (0,0,0).

5. The short-wavelength characteristic X-ray diffraction measuring device according to claim 3 or 4, characterized in that: The center line of the positioning hole (10) and the center line of the incident collimator (2) are on a straight line and are parallel to the Z axis of the translation stage (31) when Ψ=0°. Regardless of whether the sample is rotated or translated, the coordinates of the center position of the diffracted Debye ring do not change. The distance from the center of the diffractometer circle (9) to the array detector (5) is t, and the value of t is between 150 mm and 1500 mm. The coordinates of the center position of the Debye ring are set to (0, 0, -t).

6. The short-wavelength characteristic X-ray diffraction measuring device according to claim 5, characterized in that: The specification range of each pixel of the array detector (5) is 0.02 mm-0.2 mm; the array detector (5) adopts a cadmium telluride array detector, a cadmium zinc telluride array detector or a gallium arsenide array detector.

7. The measurement and analysis method of the short-wavelength characteristic X-ray diffraction measurement device according to any one of claims 1 to 6, characterized in that the steps include: Step 1, selecting a short-wavelength characteristic X-ray with a suitable wavelength according to the material and thickness of the sample, and setting two energy thresholds of the array detector (5); Step 2, fix the sample (3) on the sample stage, and place the measured part of the sample at the center of the diffractometer circle (9); Step 3, according to the selected short-wavelength characteristic X-ray, apply a tube voltage that is 1.5 times higher than the target excitation voltage, and start the X-ray irradiation system; Step 4, exposing and measuring the Debye ring or diffraction pattern of the crystalline material at the measured part, determining the peak, and comparing it with the powder diffraction card to determine the phase of the crystalline material at the measured part; Step 5, if the texture or orientation of the main phase of the measured part is to be tested, the step-scan measurement is performed by rotating the Ψ angle turntable (33), exposing and measuring the Debye rings diffracted by the crystal material of the measured part at different Ψ angles; the peak is determined, and the diffraction intensity of the Debye rings of each diffraction crystal plane in each direction is measured; and absorption correction is performed according to the diffraction path length to obtain the diffraction intensity of the Debye rings of each diffraction crystal plane after correction in each direction, and based on this, the transmission pole figures of multiple strong diffraction crystal planes and relatively strong diffraction crystal planes of the main phase are calculated; according to the crystal system type, the transmission pole figures of multiple strong diffraction crystal planes of the main phase are selected, and the full pole figures or orientation distribution function (ODF) of the corresponding diffraction crystal plane are calculated; Step 6: if the residual stress of the measured part is to be tested, the strains in multiple directions of one (hkl) crystal plane or multiple (hkl) crystal planes of the main phase are measured, and the stress tensor σ of the measured part of the sample is calculated according to the stress-strain relationship of elastic mechanics; Step 7: If you want to test the internal phase, texture, and stress of another part of the sample, repeat steps 4, 5, and 6 until all the parts to be tested are tested, and after data processing, the internal phase, texture, stress, etc. of each part of the sample and their distribution are obtained.

8. The measurement and analysis method according to claim 7, characterized in that: In step 6, for the residual stress test of the sample in the plane stress state, the stress tensor σ of the measured part of the sample can be measured by only exposing and measuring the Debye rings or strong diffraction spots diffracted by each crystal plane of the measured part of the sample and the corresponding part of the stress-free standard sample once respectively; by rotating the Ψ angle turntable (33), the surface normal direction of the measured part of the sample and the corresponding part of the stress-free standard sample is made to coincide with the incident X-ray beam (7), and then the Debye rings diffracted by each crystal plane of the measured part of the sample and the corresponding part of the stress-free standard sample are exposed and measured respectively, and the diffraction angle 2θ of each direction of each crystal plane of the measured part of the sample is obtained by peak determination. s-hkl , and the diffraction angle 2θ of each crystal plane in each direction of the corresponding part of the stress-free standard sample 0-hkl , the strain ε(90°-θ hkl , Φ), the stress tensor σ of the measured part of the sample is calculated by formula (2) and (3); If the Debye rings or strong diffraction spots of multiple strong diffraction crystal planes and relatively strong diffraction crystal planes (hkl) are measured at the same time, the ε(90°-θhkl, Φ) and their distribution of multiple strong diffraction crystal planes and relatively strong diffraction crystal planes (hkl) can be calculated. hkl , Φ) and their distribution, the corresponding multiple stress tensors σ can be calculated respectively, and then the arithmetic mean method or the least squares method can be used to calculate a more accurate stress tensor.

9. The measurement and analysis method according to claim 8, characterized in that: For residual stress test of samples with strong texture, the direction of strain measurement depends on the texture. It is necessary to select the strong diffraction crystal plane (hkl) to be measured, and the direction of the maximum diffraction intensity is on the outermost circle of the (hkl) crystal plane pole figure, and between the two principal stresses ε xx , ε yy Direction or near direction, exposure measurement obtains ε(90°-θ hkl , 90°+α), ε(90°-θ hkl , β), and the two principal stresses σ are calculated by formulas (4) and (5): xx , σ yy The principal strain ε xx and ε yy , and then ε xx and ε yy Substituting into formula (2) and (3), we can finally calculate the two principal stresses σ xx , σ yy , that is, the stress tensor σ at the measured part of the sample.

10. The measurement and analysis method according to claim 7, characterized in that: In step 6, for a sample in a general stress state, the stress tensor σ of the measured part of the sample can be measured by exposing and measuring the Debye rings or strong diffraction spots of each crystal plane diffracted by the measured part of the sample and the corresponding part of the stress-free standard sample at two different angles Ψ respectively. First, the Ψ angle turntable (33) is rotated to make Ψ=Ψ1, and the Debye rings of each crystal plane diffracted by the measured part of the sample and the corresponding part of the stress-free standard sample are exposed and measured respectively. Then, the sample is rotated to Ψ=Ψ2, and the Debye rings or strong diffraction spots of each crystal plane diffracted by the measured part of the sample and the corresponding part of the stress-free standard sample are exposed and measured respectively. Peak determination, select the peak determination results 2θ of the six directions of the (hkl) crystal plane s-hkl and 2θ 0-hkl , calculated by formula (1) to obtain 6 (Ψ i , Φ i ) direction (hkl) crystal plane strain ε(Ψ i , Φ i ); Then, by solving the linear equations from formula (6), the strain ε can be obtained ij (i=x,y,z; j=x,y,z); by ε ij The three principal strains ε can be obtained by linear transformation D XX , ε D YY , ε D ZZ Finally, the stress tensor σ of the measured part of the sample is calculated by formula (7).

11. The measurement and analysis method according to claim 10, characterized in that: For residual stress testing of samples with strong texture, the direction of strain measurement depends on the texture. It is necessary to select the direction of the maximum diffraction intensity of the strong diffraction crystal plane (hkl) to be measured to measure the strain. Specifically, by rotating the Ψ angle turntable (33) to expose and measure the Debye rings diffracted by the measured part of the sample and the corresponding part of the stress-free standard sample at different Ψ angles, select the six strong diffraction spots of the strong diffraction crystal plane and the relatively strong diffraction crystal plane (hkl), determine the peak, and calculate the strain ε (Ψ) in the six directions according to formula (1): i , Φ i ), according to formula (6), the three principal strains ε can be obtained by simultaneous linear equations and linear transformation. D XX , ε D YY , ε D ZZ , and then according to the elastic mechanics formula (7), the stress tensor σ or the three principal stresses σ at the measured part of the sample are finally obtained D XX , σ D YY , σ D ZZ size and direction.

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