A crystal orientation detection method and related apparatus
By using a synchrotron radiation source and rotating the sample, combined with diffraction vectors and crystal plane indices, the problem of detecting the internal crystal orientation of complex blade structures was solved, achieving high-precision crystal orientation analysis.
Patent Information
- Application Number
- CN202511217544.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-28
- Publication Date
- 2025-11-07
- Estimated Expiration
- 2045-08-28
AI Technical Summary
Existing technologies are insufficient to accurately detect the internal matrix crystal orientation and recrystallized grain orientation of complex structures such as hollow blades and double-walled hollow blades.
The sample under test is irradiated with rays generated by a synchrotron radiation source. The positions of the transmitted and diffracted light spots are collected at different angles by rotating the sample. The transformation relationship between the sample coordinate system and the crystal coordinate system is constructed by combining the diffraction vector and the preset crystal plane index, and the crystal orientation is determined.
It achieves accurate and complete detection of crystal orientation in blades with complex structures, reduces blind spots, and improves detection precision.
Smart Images

Figure CN120741531B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of crystal detection, in particular to a crystal orientation detection method and related device. BACKGROUND
[0002] Single crystal superalloy is the core material of turbine blades of high-end devices such as aircraft engines and gas turbines, and the turbine blades are exposed to extreme environments of high temperature, high pressure, high stress and strong oxidation / corrosion for a long time. In order to ensure the performance of the turbine blade, the single crystal superalloy as the core material thereof needs to meet the stringent comprehensive performance requirements. Among them, the crystal orientation is the core quality index of the single crystal superalloy blade.
[0003] At present, the crystal orientation of the single crystal superalloy blade is usually tested by visual inspection or laboratory X-ray diffraction technology, but with the development of technology, the blade has gradually developed into a hollow blade and a double-wall hollow blade, and the internal matrix crystal orientation and recrystallized grain orientation cannot be detected.
[0004] Therefore, there is an urgent need for a crystal orientation detection method to accurately detect the crystal orientation of a complex structure blade. SUMMARY
[0005] In view of the above problems, the present application provides a crystal orientation detection method and related device to achieve the purpose of accurately detecting the crystal orientation of a complex structure blade. The specific scheme is as follows:
[0006] The first aspect of the present application provides a crystal orientation detection method applied to a controller of a crystal orientation detection system, wherein the crystal orientation detection system further comprises a synchrotron radiation source and a detector arranged on both sides of a to-be-detected sample respectively, and the crystal orientation detection method comprises:
[0007] controlling the synchrotron radiation source to generate a ray which is perpendicular to a to-be-detected region of the to-be-detected sample;
[0008] controlling the to-be-detected sample to rotate at a preset interval, determining a rotation angle of the to-be-detected sample after rotation, and acquiring transmission light and diffraction light of the to-be-detected region at each rotation angle corresponding to the ray, and the transmission light spot position and the diffraction light spot position corresponding to the transmission light and the diffraction light collected by the detector respectively, wherein the rotation angle is an offset angle of the to-be-detected sample relative to an initial angle;
[0009] determining a diffraction vector of the diffraction light in a sample coordinate system corresponding to each rotation angle based on the transmission light spot position and the diffraction light spot position, wherein the sample coordinate system is a three-dimensional coordinate system constructed with the center of the to-be-detected region as the origin;
[0010] According to the preset crystal plane index corresponding to at least one of the rotation angles and the diffraction vector, an expression representing a conversion relationship between the sample coordinate system and a crystal coordinate system is determined as the crystal orientation of the sample to be measured.
[0011] In a possible implementation, the determination of the diffraction vector of the diffraction light in the sample coordinate system corresponding to each of the rotation angles respectively based on the transmission light spot position and the diffraction light spot position comprises:
[0012] The vector processing is performed on the transmission light spot position and the diffraction light spot position corresponding to each of the rotation angles to obtain the diffraction vector of the diffraction light in the sample coordinate system corresponding to each of the rotation angles respectively, and the vector processing comprises:
[0013] Based on the transmission light spot position and the diffraction light spot position, a diffraction radius of the diffraction light in a laboratory coordinate system is determined, the laboratory coordinate system being a three-dimensional coordinate system with the same direction as the sample coordinate system and with the transmission light spot position as the origin;
[0014] A diffraction angle of the irradiated crystal plane of the rotation angle is obtained.
[0015] Based on the diffraction angle and the diffraction radius, a first diffraction vector of the diffraction light in the laboratory coordinate system is determined.
[0016] According to the conversion relationship between the laboratory coordinate system and the sample coordinate system, a diffraction vector of the diffraction light in the sample coordinate system corresponding to the rotation angle is determined.
[0017] In a possible implementation, according to the preset crystal plane index corresponding to at least one of the rotation angles and the diffraction vector, an expression representing a conversion relationship between the sample coordinate system and a crystal coordinate system is determined as the crystal orientation of the sample to be measured, comprising:
[0018] According to the preset crystal plane index corresponding to at least one of the rotation angles and the diffraction vector, a linear regression equation is constructed.
[0019] Based on the linear regression equation, a conversion matrix of the sample coordinate system to the crystal coordinate system is determined as the crystal orientation of the sample to be measured.
[0020] In a possible implementation, the process of presetting the crystal plane index comprises:
[0021] Based on the diffraction vector corresponding to at least one of the rotation angles respectively, a diffraction pole figure of the sample to be measured is determined.
[0022] acquire a standard diffraction pole figure corresponding to a crystal type of the sample to be measured;
[0023] determine a crystal plane index of different crystal planes of the sample to be measured according to a difference between the diffraction pole figure and the standard diffraction pole figure.
[0024] The second aspect of the present application provides a crystal orientation detection system, comprising: a controller, and a synchrotron radiation source and a detector arranged on two sides of a sample to be measured respectively, and the sample to be measured, the synchrotron radiation source and the detector are in the same horizontal plane;
[0025] The synchrotron radiation source is configured to generate a ray, which is vertically irradiated on a to-be-measured region of the sample to be measured.
[0026] The detector is configured to collect a transmission light spot position of transmission light and a diffraction light spot position of diffraction light of the to-be-measured region on the ray.
[0027] The controller is configured to implement the crystal orientation detection method of the first aspect or any implementation manner of the first aspect.
[0028] The third aspect of the present application provides a crystal orientation detection device, which is applied to the controller in the crystal orientation detection system of the second aspect, and the crystal orientation detection device comprises:
[0029] The control irradiation unit is configured to control the ray generated by the synchrotron radiation source to be vertically irradiated on a to-be-measured region of the sample to be measured.
[0030] The position acquisition unit is configured to control the sample to be measured to rotate at a preset interval, determine a rotation angle of the sample to be measured after rotation, and acquire the transmission light spot position and the diffraction light spot position corresponding to the transmission light and the diffraction light of the to-be-measured region on the ray respectively collected by the detector at each rotation angle, the rotation angle being an offset angle of the sample to be measured relative to an initial angle.
[0031] The diffraction vector determination unit is configured to determine a diffraction vector of the diffraction light in a sample coordinate system corresponding to each rotation angle respectively based on the transmission light spot position and the diffraction light spot position, the sample coordinate system being a three-dimensional coordinate system constructed with the center of the to-be-measured region as an origin.
[0032] The crystal orientation determination unit is configured to determine an expression representing a conversion relationship between the sample coordinate system and a crystal coordinate system as a crystal orientation of the sample to be measured according to a preset crystal plane index corresponding to at least one rotation angle and the diffraction vector.
[0033] In a possible implementation, the diffraction vector determination unit comprises:
[0034] a diffraction radius determination sub-unit configured to determine a diffraction radius of the diffracted light in a laboratory coordinate system based on the position of the transmitted light spot and the position of the diffracted light spot, the laboratory coordinate system being a three-dimensional coordinate system with the same direction as the sample coordinate system and with the position of the transmitted light spot as an origin;
[0035] a diffraction angle acquisition sub-unit configured to acquire a diffraction angle of the irradiated crystal face at the rotation angle;
[0036] a first vector determination sub-unit configured to determine a first diffraction vector of the diffracted light in the laboratory coordinate system based on the diffraction angle and the diffraction radius;
[0037] a vector conversion sub-unit configured to determine a diffraction vector of the diffracted light in the sample coordinate system corresponding to the rotation angle according to a conversion relationship between the laboratory coordinate system and the sample coordinate system.
[0038] In a possible implementation, the crystal orientation determination unit comprises:
[0039] an equation construction sub-unit configured to construct a linear regression equation according to the preset crystal face index corresponding to each of the rotation angles and the diffraction vector;
[0040] an orientation determination sub-unit configured to determine a conversion matrix from the sample coordinate system to a crystal coordinate system as the crystal orientation of the sample to be measured based on the linear regression equation.
[0041] In a possible implementation, the functional unit for presetting the crystal face index comprises:
[0042] a diffraction pole figure determination unit configured to determine a diffraction pole figure of the sample to be measured based on the diffraction vector corresponding to each of the rotation angles;
[0043] a standard pole figure acquisition unit configured to acquire a standard diffraction pole figure corresponding to the crystal type of the sample to be measured;
[0044] a crystal face index determination unit configured to determine the crystal face index of different crystal faces of the sample to be measured according to the difference between the diffraction pole figure and the standard diffraction pole figure.
[0045] The fourth aspect of the present application provides a computer storage medium, the storage medium carrying one or more computer programs, when the one or more computer programs are executed by an electronic device, the electronic device can implement the crystal orientation detection method of the first aspect or any implementation manner of the first aspect.
[0046] By the technical solution, the crystal orientation detection method provided by the application first uses the rays generated by the synchrotron radiation source to irradiate the to-be-detected region of the to-be-detected sample. Due to the high penetration ability of the rays generated by the synchrotron radiation source, the internal structure of the to-be-detected sample diffracts the rays, thereby providing a basis for the crystal orientation test. Further, the conversion relationship between the crystal coordinate system and the sample coordinate system is derived by using the preset crystal face indices of the crystal sample at different rotation angles and the vector information of the diffraction light of the crystal face in the sample coordinate system that can be measured, so as to determine the crystal orientation of the crystal sample.
[0047] Further, the conversion relationship between the sample coordinate system and the crystal coordinate system is determined by combining the crystal face indices and the diffraction vectors of multiple crystal faces, thereby improving the accuracy of the crystal orientation test. BRIEF DESCRIPTION OF DRAWINGS
[0048] The above and other features, advantages, and aspects of the embodiments of the present disclosure will become more apparent with reference to the following detailed description when taken in conjunction with the accompanying drawings. Throughout the drawings, the same or similar reference numerals refer to the same or similar elements. It should be understood that the drawings are schematic, and the original and elements are not necessarily drawn according to the scale.
[0049] Figure 1 A flowchart of a crystal orientation detection method provided by an embodiment of the application is shown in the figure;
[0050] Figure 2 A structural diagram of a crystal orientation detection system provided by an embodiment of the application is shown in the figure;
[0051] Figure 3 A schematic diagram of crystal diffraction provided by an embodiment of the application is shown in the figure;
[0052] Figure 4 A structural diagram of a crystal orientation detection device provided by an embodiment of the application is shown in the figure. DETAILED DESCRIPTION
[0053] The embodiments of the application are described below in conjunction with the drawings. The terms used in the embodiment part of the application are only used to explain the specific embodiments of the application, and are not intended to limit the application.
[0054] The embodiments of the application are described below in conjunction with the drawings. Those skilled in the art can know that, as technology develops and new scenarios appear, the technical solutions provided by the embodiments of the application are also applicable to similar technical problems.
[0055] The terms "first", "second", and the like in the description and in the claims of the present application and above-described drawings are used to distinguish similar objects, and do not necessarily indicate a specific order or sequence. It should be understood that the terms so used are interchangeable under appropriate circumstances and are merely employed to distinguish one object from another. Furthermore, the terms "comprise", "have", and any variations thereof are intended to cover a non-exclusive inclusion, such that processes, methods, systems, products, or devices that comprise a list of elements are not necessarily limited to those elements, but can include other elements not expressly listed or inherent to such processes, methods, systems, products, or devices.
[0056] To solve the problem that the internal matrix crystal orientation and recrystallization grain orientation cannot be detected for hollow blades and double-wall hollow blades in the prior art, the embodiments of the present application provide a crystal orientation detection method. The crystal orientation detection method of the embodiments of the present application will be described in detail below with reference to the drawings.
[0057] Referring to Figure 1 , Figure 1 A flowchart of the crystal orientation detection method provided by the embodiments of the present application is shown in FIG. 1. The crystal orientation detection method provided by the embodiments of the present application can include steps S110 to S150, which will be described in detail below. Figure 1
[0058] It should be noted that the crystal orientation detection method provided by the embodiments of the present application is applied to a controller of a crystal orientation detection system. Referring to Figure 2 , a structural diagram of the crystal orientation detection system provided by the embodiments of the present application, the system can further include a synchrotron radiation source and a detector, wherein the synchrotron radiation source and the detector are respectively arranged on two sides of a to-be-detected sample, and together realize the crystal orientation test of the to-be-detected sample. The to-be-detected sample can be a crystal sample, or a turbine blade mentioned in the above background art, or other objects made of crystals as core materials, which are not limited herein.
[0059] On the basis of the above crystal orientation detection system, the controller performs the following steps:
[0060] Step S110, control the rays generated by the synchrotron radiation source to vertically irradiate the to-be-detected region of the to-be-detected sample.
[0061] Step S120, control the to-be-detected sample to rotate at a preset interval, and determine the rotation angle of the to-be-detected sample after rotation. The rotation angle is the deviation angle of the to-be-detected sample relative to the initial angle.
[0062] The rays generated by the synchrotron radiation source have strong penetration, and the penetration depth and effect depend on the energy of the rays. The greater the energy, the stronger the penetration ability. The tester can determine the requirements of the test requirements of the to-be-tested crystal on the penetration of the rays according to the structure of the to-be-tested crystal and the type of the crystal, and adjust the synchrotron radiation source so that the rays generated by the synchrotron radiation source can meet the test requirements. For example, if the to-be-tested sample is a hollow blade and a double-walled hollow blade, and the internal matrix crystal orientation and recrystallized grain orientation need to be detected, the intensity of the rays of the synchrotron radiation source is determined according to the type of the crystal material of the blade and the thickness of the blade, so that the rays can penetrate the blade, so that the detector can collect the transmission light and diffraction light signals of the internal crystal to the rays, and provide a basis for subsequent crystal orientation detection.
[0063] While controlling the rays to vertically irradiate the to-be-tested region of the to-be-tested sample, the to-be-tested sample is controlled to rotate, so that the detector collects information of diffraction effects of the rays at different angles of the to-be-tested region, thereby obtaining more comprehensive diffraction data of the to-be-tested sample. These diffraction data contain structure information of the to-be-tested sample in different directions, which helps to more accurately determine the crystal information of the to-be-tested sample.
[0064] Optionally, referring to Figure 3 The crystal diffraction diagram provided by the embodiment of the present application takes the center (x, y, z) of the to-be-tested region of the to-be-tested sample as the center of the sample coordinate system, and the direction in which the rays generated by the synchrotron radiation source enter is the X axis. The direction perpendicular to the X axis upward is the longitudinal axis Z. In the embodiment of the present application, the to-be-tested sample is controlled to rotate around the Z axis at a preset interval. It can be understood that because the center of the to-be-tested region is located on the straight line where the Z axis is located, even if the to-be-tested sample rotates around the Z axis, the position of the to-be-tested sample will not change, and only the angle at which the to-be-tested sample is irradiated by the synchrotron radiation source changes. Based on this, the detector collects diffraction information of the to-be-tested region at different angles to the rays at the rear of the to-be-tested sample.
[0065] In step S130, the transmission light and diffraction light of the to-be-tested region to the rays at each rotation angle collected by the detector correspond to the transmission light spot position and the diffraction light spot position, respectively.
[0066] In step S140, based on the transmission light spot position and the diffraction light spot position, the diffraction vector of the diffraction light corresponding to each rotation angle in the sample coordinate system is determined.
[0067] After the radiation irradiates the to-be-tested region, two beams of light are usually generated, one of which is a transmission light obtained by directly transmitting part of the light in the radiation through the to-be-tested sample, and the other of which is a diffraction light formed by a diffraction phenomenon occurring when the radiation interacts with the to-be-tested sample. The transmission light and the diffraction light form a transmission light spot and a diffraction light spot respectively. The detector captures the transmission light spot and the diffraction light spot and records the position coordinates thereof. Based on this, in the embodiments of the present application, the detector can use a pixel array detector, wherein each pixel corresponds to a specific position, and when a photon hits a certain pixel, the pixel generates an electrical signal, so that the photon position is recorded. Based on this, the detector can collect the positions of the transmission light spot and the diffraction light spot.
[0068] The detector reads the transmission light spot position and the diffraction light spot position of the to-be-tested region for the radiation collected by the detector once per rotation of the to-be-tested sample. It can be understood that the direction of the transmission light is usually the same as the direction of the radiation irradiation, and therefore the transmission light spot position corresponds to the position of the irradiated region in the to-be-tested region, and the position and intensity distribution of the diffraction light spot reflect important information of the structure of the to-be-tested sample, such as lattice parameters, atomic arrangement, etc.
[0069] Further, the transmission light spot position and the diffraction light spot position corresponding to each rotation angle are processed respectively to obtain a diffraction vector of the to-be-tested region for the radiation at each rotation angle, which is a vector representation of the diffraction light relative to the sample coordinate system. It can be understood that the crystal orientation refers to the spatial arrangement direction of a certain crystal face or crystal direction in a crystal relative to an external reference coordinate system (such as a sample coordinate system or a laboratory coordinate system). Therefore, in the embodiments of the present application, the transmission light spot position and the diffraction light spot position in the laboratory coordinate system, i.e. the coordinate system under the pixel array of the detector, are collected by the detector first, and then the vector information of the diffraction light in the sample coordinate system is determined by using the transmission light spot position and the diffraction light spot position and the positional relationship between the laboratory coordinate system and the sample coordinate system. Further, the relative relationship between the crystal coordinate system and the sample coordinate system is derived according to the relationship among the sample coordinate system, the crystal coordinate system and the diffraction vector, so that the crystal orientation of the to-be-tested sample is detected.
[0070] In a possible implementation, for each rotation angle corresponding to a transmission light spot position and a diffraction light spot position, vector processing is performed to obtain a diffraction vector of the diffraction light corresponding to each rotation angle in a sample coordinate system, and the vector processing includes: determining a diffraction radius of the diffraction light in a laboratory coordinate system based on the transmission light spot position and the diffraction light spot position, the laboratory coordinate system being a three-dimensional coordinate system with the same direction as the sample coordinate system and taking the transmission light spot position as an origin; obtaining a diffraction angle of the irradiated crystal surface at the rotation angle; determining a first diffraction vector of the diffraction light in the laboratory coordinate system based on the diffraction angle and the diffraction radius; and determining the diffraction vector of the diffraction light corresponding to the rotation angle in the sample coordinate system according to a conversion relationship between the laboratory coordinate system and the sample coordinate system.
[0071] With reference to Figure 3 The determination process of the diffraction vector of the diffraction light corresponding to one rotation angle in the sample coordinate system is taken as an example for description, and the determination of the diffraction vectors of other rotation angles can be correspondingly referred to, which will not be described herein again.
[0072] Specifically, based on the transmission light spot position and the diffraction light spot position (y det ,z det ), and a pixel size p of each pixel in the pixel array detector, the diffraction radius t in the laboratory coordinate system is determined with reference to the following formula (1). It can be understood that the laboratory coordinate system is a pixel coordinate system of the pixel array detector, the origin of the pixel coordinate system is the position of the transmission light spot, and the directions of the coordinate axes of the pixel coordinate system are the same as the directions of the coordinate axes in the sample coordinate system.
[0073] (1)
[0074] Further, the crystal surface and the diffraction angle 2θ at the rotation angle are determined by comparing reference data in a material standard card (such as a JCPDS / ICDD card). Based on this, the object distance D of the detector in the current test environment is determined with reference to formula (2), and then the complete coordinates of the diffraction light spot position in the laboratory coordinate system can be determined as (D, y det ,z det ).
[0075] (2)
[0076] The direction of the diffraction light is determined by using the object distance D and the diffraction light spot position , where a and b are the components of the diffraction light in the Y axis and the Z axis of the laboratory coordinate system, respectively, and the direction e D is unitized to obtain the vector .
[0077] The direction of the diffraction light is unitized to obtain the vector with the incident light direction , determine the first diffraction vector in the laboratory coordinate system . Further, in combination with the current rotation angle of the sample to be measured , obtain the diffraction vector e of the diffraction light in the sample coordinate system, refer to the following formula (3).
[0078] (3)
[0079] Step S150, according to the preset crystal plane index corresponding to at least one rotation angle and the diffraction vector, determine the expression representing the conversion relationship between the sample coordinate system and the crystal coordinate system as the crystal orientation of the sample to be measured.
[0080] Based on the above method, the diffraction vector corresponding to each rotation angle is determined, and the diffraction vector of each rotation angle and the preset crystal plane index corresponding to each rotation angle are used to establish linear regression equations in the sample coordinate system and the crystal coordinate system respectively, so as to determine the matrix of the sample coordinate system to the crystal coordinate system, and the matrix is used as the crystal orientation of the sample to be measured.
[0081] In a possible implementation, the preset crystal plane index can be determined by the crystal type, and the crystal plane index is determined by the standard diffraction crystal plane corresponding to the crystal type. Specifically, the process of determining the preset crystal plane index includes: determining the diffraction pole figure of the sample to be measured based on the diffraction vector corresponding to at least one rotation angle; obtaining the standard diffraction pole figure corresponding to the crystal type of the sample to be measured; and determining the crystal plane index of different crystal planes of the sample to be measured according to the difference between the diffraction pole figure and the standard diffraction pole figure.
[0082] Using the polar projection method, the diffraction signals of the diffraction crystal planes of the sample to be measured at all rotation angles are drawn into the X-ray diffraction pole figure, and at the same time, the standard diffraction pole figure of the single crystal material corresponding to the sample to be measured is compared, so as to determine the crystal plane index of different poles, which is used as the preset crystal plane index of the sample to be measured.
[0083] Further, according to the preset crystal plane index and the diffraction vector corresponding to at least one rotation angle, a linear regression equation is constructed; and based on the linear regression equation, a conversion matrix of the sample coordinate system to the crystal coordinate system is determined as the crystal orientation of the sample to be measured.
[0084] The diffraction vector e in the sample coordinate system obtained in the above step S140 is denoted as (X, Y, Z), and the preset crystal plane index is (h1, k1, l1), wherein the crystal plane index in the X-axis direction of the sample coordinate system is (u, v, w), the crystal direction index in the Y-axis direction is (r, s, t), and the crystal direction index in the Z-axis direction is (h, k, l). Based on this, the regression equation of the following formula (4) is established:
[0085] (4)
[0086] Wherein, (X1, Y1, Z1), (X2, Y2, Z2), (X3, Y3, Z3) represent diffraction vectors under different rotation angles respectively, (h1, k1, l1), (h2, k2, l2), (h3, k3, l3) are the indices of the crystal surface corresponding to (X1, Y1, Z1), (X2, Y2, Z2), (X3, Y3, Z3) under the rotation angle. The crystal coordinate system is fixed in the internal grain of the sample to be measured, and the three crystal axes
[100] ,
[010] ,
[001] of the grain are X axis, Y axis and Z axis.
[0087] The above formula (4) uses the diffraction vectors and the indices of the crystal surface corresponding to the three rotation angles, which are only exemplary, and in the embodiments of the present application, the conversion relationship between the sample coordinate system and the crystal coordinate system can also be determined by establishing a regression equation through the diffraction vectors and the indices of the crystal surface of more than three groups of different crystal surfaces, and the following formula (5) is obtained as the crystal orientation of the sample to be measured.
[0088] (5)
[0089] Wherein, S represents the sample coordinate system, C represents the crystal coordinate system, G represents the matrix of the conversion relationship between the sample coordinate system and the crystal coordinate system, and g is the inverse matrix of G.
[0090] In summary, the crystal orientation detection method provided by the present application first uses the rays generated by the synchrotron radiation source to irradiate the to-be-measured region of the sample to be measured. Due to the high penetration ability of the rays generated by the synchrotron radiation source, the internal structure of the sample to be measured diffracts the rays, providing a basis for crystal orientation testing. Further, the conversion relationship between the crystal coordinate system and the sample coordinate system is derived by using the indices of the crystal surface of the preset crystal sample under different rotation angles and the vector information of the diffraction light of the crystal surface in the sample coordinate system, so as to determine the crystal orientation of the crystal sample.
[0091] Further, by rotating the sample to be measured, as many diffraction signals of different crystal surfaces of the sample to be measured as possible are collected to reduce the blind area of the crystal surface detection of the sample to be measured. Further, the conversion relationship between the sample coordinate system and the crystal coordinate system is determined by combining the indices of the crystal surface and the diffraction vectors of multiple crystal surfaces, and the accuracy of the crystal orientation test is improved.
[0092] Next, the actual application of the crystal orientation detection method provided by the present application is exemplarily illustrated in combination with the following embodiments.
[0093] The monochromatic surface spot is generated by the synchrotron radiation source, the measured area is irradiated vertically to the surface of the measured sample, the detector is placed vertically to the synchrotron radiation source behind the measured sample, and the transmitted light and the diffracted light after transmission and diffraction of the measured area are collected. At the same time, the measured sample is controlled to rotate along the longitudinal axis Z of the sample coordinate system at a preset rotation angle range, such as-45°~45°, at a rotation interval angle of 0.1°, and the rotation angle of the measured sample after each rotation is recorded , and the transmitted light spot position and the diffracted light spot position collected by the detector corresponding to each rotation angle.
[0094] On the basis of the hardware structure of the above crystal orientation system, the laboratory coordinate system, the sample coordinate system and the crystal coordinate system are established. Referring to Figure 3 , the positive direction of the X axis of the laboratory coordinate system is the incident direction of the ray, and the Z axis is the direction perpendicular to the X axis and vertically upward; the sample coordinate system is consistent with the laboratory coordinate system when the rotation angle is 0; the crystal coordinate system is fixed in the grain inside the sample, and the three crystal axes
[100] ,
[010] and
[001] of the grain are the X axis, the Y axis and the Z axis.
[0095] The diffracted radius t in the laboratory coordinate system is determined by using the transmitted light spot position and the diffracted light spot position (y det ,z det ) corresponding to each rotation angle and the pixel size of the pixel array in the detector. Specifically, in the experiment of the present example, multiple rotations can be performed to determine the diffracted radius t corresponding to multiple rotation angles, as shown in Table 1 below.
[0096] Table 1 Diffracted radius corresponding to sample rotation angle
[0097]
[0098] Further, by comparing the material standard card, the diffraction angle 2θ of the crystal face corresponding to each rotation angle is determined, so as to determine the geophysical prospecting distance corresponding to the rotation angle in the experiment by combining the geometric relationship between the diffracted radius and the diffraction angle. The direction vector of the diffracted light is determined by using the geophysical prospecting distance. The direction vector of the diffracted light is normalized, and the direction vector of the incident light is determined, so as to jointly determine the direction vector of the diffraction vector in the laboratory coordinate system , i.e. the first diffraction vector. Further, the first diffraction vector in the laboratory coordinate system is determined by using the rotation angle corresponding to the first diffraction vector, and the diffraction vector e after conversion to the sample coordinate system. Based on this, the diffracted light spot coordinates and the diffraction vector corresponding to each rotation angle in Table 1 are determined, as shown in Table 2.
[0099] Table 2 Calculation results of diffraction vectors
[0100]
[0101] X-ray diffraction pole figures were plotted for all diffraction crystal planes using the stereographic projection method. These figures were then compared with standard diffraction pole figures for single-crystal materials to determine the crystal plane indices at different poles. Linear regression equations were established in both the sample and crystal coordinate systems to determine the transformation matrix from the sample to the crystal coordinate system, thus completing the determination of crystal orientation. The transformation matrix between the sample and crystal coordinate systems for the crystal characterization curve in this example is: .
[0102] The above describes a crystal orientation detection method provided by the embodiments of this application. The following describes the apparatus for performing the crystal orientation detection method described above.
[0103] Please see Figure 4 , Figure 4 This is a schematic diagram of a crystal orientation detection device provided in an embodiment of this application. Figure 4 As shown, the crystal orientation detection device is used in the controller of a crystal orientation detection system, and includes:
[0104] The irradiation control unit 100 is used to control the rays generated by the synchrotron radiation source to vertically irradiate the test area of the sample to be tested.
[0105] The position acquisition unit 200 is used to control the sample to be tested to rotate at a preset interval, determine the rotation angle of the sample to be tested after rotation, and acquire the transmitted light spot position and the diffracted light spot position of the transmitted light and the diffracted light of the test area at each rotation angle collected by the detector. The rotation angle is the deviation angle of the sample to be tested relative to the initial angle.
[0106] The diffraction vector determination unit 300 is used to determine the diffraction vector of the diffracted light in the sample coordinate system corresponding to each rotation angle based on the position of the transmitted light spot and the position of the diffracted light spot. The sample coordinate system is a three-dimensional coordinate system constructed with the center of the region to be measured as the origin.
[0107] The crystal orientation determination unit 400 is used to determine an expression characterizing the transformation relationship between the sample coordinate system and the crystal coordinate system based on at least one preset crystal plane index corresponding to the rotation angle and the diffraction vector, as the crystal orientation of the sample to be tested.
[0108] In one possible implementation, the diffraction vector determination unit includes:
[0109] a diffraction radius determination sub-unit configured to determine a diffraction radius of the diffracted light in a laboratory coordinate system based on the transmitted light spot position and the diffracted light spot position, the laboratory coordinate system being a three-dimensional coordinate system with the same direction as the sample coordinate system and with the transmitted light spot position as an origin;
[0110] a diffraction angle acquisition sub-unit configured to acquire a diffraction angle of the irradiated crystal face at the rotation angle;
[0111] a first vector determination sub-unit configured to determine a first diffraction vector of the diffracted light in the laboratory coordinate system based on the diffraction angle and the diffraction radius;
[0112] a vector conversion sub-unit configured to determine a diffraction vector of the diffracted light in the sample coordinate system corresponding to the rotation angle according to a conversion relationship between the laboratory coordinate system and the sample coordinate system.
[0113] In a possible implementation, the crystal orientation determination unit comprises:
[0114] an equation construction sub-unit configured to construct a linear regression equation according to the preset crystal face index corresponding to each of the rotation angles and the diffraction vector;
[0115] an orientation determination sub-unit configured to determine a conversion matrix of the sample coordinate system to a crystal coordinate system as the crystal orientation of the sample to be measured based on the linear regression equation.
[0116] In a possible implementation, the process of presetting the crystal face index by the crystal orientation determination unit comprises: determining a diffraction pole figure of the sample to be measured based on the diffraction vector corresponding to each of the rotation angles; acquiring a standard diffraction pole figure corresponding to the crystal type of the sample to be measured; and determining the crystal face index of different crystal faces of the sample to be measured according to the difference between the diffraction pole figure and the standard diffraction pole figure.
[0117] To sum up, first, the rays generated by the synchrotron radiation source are used to irradiate the to-be-measured region of the sample to be measured. Due to the high penetration ability of the rays generated by the synchrotron radiation source, the internal structure of the sample to be measured diffracts the rays, providing a basis for crystal orientation testing. Further, the crystal face index of the crystal face of the preset crystal sample at different rotation angles and the vector information of the diffraction light of the crystal face in the sample coordinate system are used to derive the conversion relationship between the crystal coordinate system and the sample coordinate system, thereby determining the crystal orientation of the crystal sample.
[0118] And, by rotating the sample to be measured, as many diffraction signals of different crystal faces of the sample to be measured as possible are collected, and the blind area of the crystal face detection of the sample to be measured is reduced. Further, the conversion relationship between the sample coordinate system and the crystal coordinate system is determined by combining the indices of the crystal faces and the diffraction vectors of the multiple crystal faces, and the accuracy of the crystal orientation test is improved.
[0119] The embodiment of the present application further provides a computer storage medium, which carries one or more computer programs, and when the one or more computer programs are executed by an electronic device, the electronic device can implement any crystal orientation detection method provided by the embodiment of the present application.
[0120] In addition, it should be noted that the above-described device embodiments are only schematic, and the units described as separate components may or may not be physically separate, and the components shown as units may or may not be physical units, i.e., they may be located in one place, or distributed on multiple network units. Some or all of the modules can be selected according to actual needs to achieve the purpose of the embodiment. In addition, in the device embodiment provided by the present application, the connection relationship between the modules indicates that there is a communication connection between them, which can be implemented as one or more communication buses or signal lines.
[0121] Through the description of the above embodiments, those skilled in the art can clearly understand that the present application can be implemented by means of software and necessary general hardware, and of course, it can also be implemented by special hardware including special integrated circuits, special CPUs, special memories, special components, etc. Generally, functions completed by computer programs can be easily implemented by corresponding hardware, and the specific hardware structure for implementing the same function can also be various, such as analog circuits, digital circuits or special circuits. However, for the present application, software program implementation is a better embodiment. Based on this understanding, the technical solutions of the present application can be embodied in the form of a software product, which is stored in a readable storage medium, such as a computer's floppy disk, U disk, mobile hard disk, ROM, RAM, magnetic disk or optical disk, etc., including a plurality of instructions to make a computer device (which can be a personal computer, training device, or network device, etc.) execute the methods described in various embodiments of the present application.
[0122] In the above embodiments, all or part can be realized by software, hardware, firmware or any combination thereof. When realized by software, it can be realized in the form of a computer program product in whole or in part.
[0123] The computer program product includes one or more computer instructions. When the computer program instructions are loaded and executed on a computer, the processes or functions described in the embodiments of the present application are generated in whole or in part. The computer can be a general-purpose computer, a special-purpose computer, a computer network, or other programmable devices. The computer instructions can be stored in a computer-readable storage medium or transmitted from one computer-readable storage medium to another computer-readable storage medium, for example, the computer instructions can be transmitted from one website, computer, training device or data center to another website, computer, training device or data center through wired (such as coaxial cable, optical fiber, digital subscriber line (DSL)) or wireless (such as infrared, wireless, microwave, etc.). The computer-readable storage medium can be any available medium that can be stored by the computer or a data storage device such as a training device, a data center, etc. integrated with one or more available media sets. The available media can be a magnetic medium (for example, a floppy disk, a hard disk, a magnetic tape), an optical medium (for example, a DVD), or a semiconductor medium (for example, a solid state disk (SSD)), etc.
Claims
1. A method of detecting crystal orientation, characterized by, The application discloses a controller applied to a crystal orientation detection system, and the crystal orientation detection system further comprises a synchrotron radiation light source and a detector arranged on two sides of a sample to be detected. The controller controls the synchrotron radiation light source to generate a ray which is vertically irradiated on a region to be detected of the sample to be detected. The controller controls the sample to be detected to rotate at a preset interval, determines a rotation angle of the sample to be detected after rotation, and acquires transmission light and diffraction light of the region to be detected at each rotation angle, and corresponding transmission light spot positions and diffraction light spot positions of the detector, wherein the rotation angle is an angle of deviation of the sample to be detected relative to an initial angle. Based on the transmission light spot positions and the diffraction light spot positions, a diffraction vector of the diffraction light corresponding to each rotation angle in a sample coordinate system is determined, wherein the sample coordinate system is a three-dimensional coordinate system constructed with a center of the region to be detected as an origin. According to a preset crystal plane index corresponding to at least one rotation angle and the diffraction vector, an expression representing a conversion relationship between the sample coordinate system and a crystal coordinate system is determined as a crystal orientation of the sample to be detected. The preset crystal plane index includes the following steps: Based on the diffraction vector corresponding to at least one rotation angle, a diffraction pole figure of the sample to be detected is determined. A standard diffraction pole figure corresponding to a crystal type of the sample to be detected is acquired. According to a difference between the diffraction pole figure and the standard diffraction pole figure, a crystal plane index of different crystal planes of the sample to be detected is determined.
2. The crystal orientation detection method according to claim 1, characterized by, The determination of the diffraction vector of the diffraction light corresponding to each rotation angle in the sample coordinate system based on the transmission light spot positions and the diffraction light spot positions includes the following steps: For the transmission light spot positions and the diffraction light spot positions corresponding to each rotation angle, vector processing is performed to obtain the diffraction vector of the diffraction light corresponding to each rotation angle in the sample coordinate system, wherein the vector processing includes the following steps: Based on the transmission light spot positions and the diffraction light spot positions, a diffraction radius of the diffraction light in a laboratory coordinate system is determined, wherein the laboratory coordinate system is a three-dimensional coordinate system constructed with the transmission light spot positions as an origin and having the same direction as the sample coordinate system. A diffraction angle of a crystal plane irradiated by the rotation angle is acquired. Based on the diffraction angle and the diffraction radius, a first diffraction vector of the diffraction light in the laboratory coordinate system is determined. According to a conversion relationship between the laboratory coordinate system and the sample coordinate system, a diffraction vector of the diffraction light corresponding to the rotation angle in the sample coordinate system is determined.
3. The crystal orientation detecting method according to claim 1, characterized by, The determination of the expression representing the conversion relationship between the sample coordinate system and the crystal coordinate system as the crystal orientation of the sample to be detected according to the preset crystal plane index corresponding to at least one rotation angle and the diffraction vector includes the following steps: According to the preset crystal plane index corresponding to at least one rotation angle and the diffraction vector, a linear regression equation is constructed. Based on the linear regression equation, a transformation matrix of the sample coordinate system to a crystal coordinate system is determined as the crystal orientation of the sample to be measured.
4. A crystal orientation detection system characterized by comprising: Comprise: A controller, and a synchrotron radiation source and a detector arranged on both sides of the sample to be measured respectively, and the sample to be measured, the synchrotron radiation source and the detector are in the same horizontal plane; The synchrotron radiation source is used to generate a ray which vertically irradiates a to-be-measured region of the sample to be measured; The detector is used to collect the transmission light spot position of the transmission light and the diffraction light spot position of the diffraction light of the to-be-measured region on the ray; The controller is used to realize the crystal orientation detection method as claimed in any one of claims 1 to 3.
5. A crystal orientation detecting apparatus characterized by comprising: The controller is applied to the crystal orientation detection system as claimed in claim 4, and the crystal orientation detection device comprises: A control irradiation unit is used to control the ray generated by the synchrotron radiation source to vertically irradiate the to-be-measured region of the sample to be measured; A position acquisition unit is used to control the sample to be measured to rotate at a preset interval, determine the rotation angle of the sample to be measured after rotation, and acquire the transmission light spot position and the diffraction light spot position corresponding to the transmission light and the diffraction light of the to-be-measured region on the ray collected by the detector at each rotation angle, wherein the rotation angle is the deviation angle of the sample to be measured relative to the initial angle; A diffraction vector determination unit is used to determine the diffraction vector of the diffraction light in the sample coordinate system corresponding to each rotation angle based on the transmission light spot position and the diffraction light spot position, wherein the sample coordinate system is a three-dimensional coordinate system constructed with the center of the to-be-measured region as the origin; A crystal orientation determination unit is used to determine an expression representing the conversion relationship between the sample coordinate system and the crystal coordinate system as the crystal orientation of the sample to be measured according to the preset crystal plane index corresponding to at least one rotation angle and the diffraction vector; Wherein, the process of presetting the crystal plane index by the crystal orientation determination unit comprises: determining the diffraction pole figure of the sample to be measured based on the diffraction vector corresponding to at least one rotation angle; acquiring the standard diffraction pole figure corresponding to the crystal type of the sample to be measured; and determining the crystal plane index of different crystal planes of the sample to be measured according to the difference between the diffraction pole figure and the standard diffraction pole figure.
6. The crystal orientation detecting apparatus according to claim 5, characterized by The diffraction vector determination unit comprises: A diffraction radius determination subunit is used to determine the diffraction radius of the diffraction light in the laboratory coordinate system based on the transmission light spot position and the diffraction light spot position, wherein the laboratory coordinate system is a three-dimensional coordinate system with the same direction as the sample coordinate system and with the transmission light spot position as the origin; A diffraction angle acquisition subunit is used to acquire the diffraction angle of the irradiated crystal plane at the rotation angle; A first vector determination subunit is used to determine the first diffraction vector of the diffraction light in the laboratory coordinate system based on the diffraction angle and the diffraction radius; A vector conversion subunit is configured to determine a diffraction vector of the diffracted light corresponding to the rotation angle in the sample coordinate system according to a conversion relationship between the laboratory coordinate system and the sample coordinate system.
7. The crystal orientation detecting apparatus according to claim 5, characterized by The crystal orientation determination unit comprises: An equation construction subunit is configured to construct a linear regression equation according to a preset crystal plane index corresponding to at least one of the rotation angles and the diffraction vector. An orientation determination subunit is configured to determine a conversion matrix of the sample coordinate system to a crystal coordinate system as the crystal orientation of the sample to be measured based on the linear regression equation.
8. A computer storage medium, characterized in that The storage medium carries one or more computer programs, and when the one or more computer programs are executed by the electronic device, the electronic device can implement the crystal orientation detection method according to any one of claims 1 to 3.
Citation Information
Patent Citations
Single crystal stress measurement method based on monochromatic X ray diffraction
CN110609047A
Method and system for synchronously detecting texture and stress through neutron diffraction
CN116380955A