Method for rapidly and nondestructively measuring internal crystal orientation of single crystal material

Abstract

The invention provides a method for rapidly, accurately and nondestructively measuring the internal crystal orientation of a single crystal material, and belongs to the field of testing of the internal crystal orientation of the single crystal material. According to the method, an azimuth angle of any crystal face on the surface of a single crystal sample is tested through a conventional X-ray diffractometer, a mapping relation between a sample coordinate system and a crystal coordinate system is established, and an orientation test and calculation method suitable for a high-energy ray transmission diffraction light path is provided; by reducing the scanning range of the sample table goniometer and the Euler ring, the testing efficiency of the internal orientation of the single crystal is improved; the invention provides a method for realizing zero calibration and error correction of an internal orientation test by a high-energy ray diffraction instrument through secondary measurement of the orientation angle of the internal crystal of the single crystal, and the test precision and repeatability of the internal orientation angle are improved. According to the invention, the efficiency, the accuracy and the precision of the nondestructive testing of the internal orientation of the single crystal are improved.

Description

Technical Field

[0001] This invention belongs to the field of orientation testing of single crystal materials, and specifically relates to a rapid and non-destructive method for determining the internal crystal orientation of single crystal materials. Background Technology

[0002] Single-crystal materials, due to their complete periodicity and absence of grain boundaries, possess irreplaceable application value in high-end manufacturing fields such as aerospace, energy, and electronics. The particles within a single crystal are arranged regularly and periodically in three-dimensional space, exhibiting long-range order throughout the crystal. Because the lattice arrangement is directional, single crystals exhibit anisotropy, meaning that different directions within a single crystal possess different physical properties. Therefore, determining the internal orientation of a single crystal is crucial for its understanding and application. However, due to the influence of thermal fields, stress fields, and subsequent processing deformations during crystal growth, the surface orientation of a single crystal often deviates from its true internal orientation. Using surface orientation solely as a basis for process evaluation or performance prediction will directly reduce the reliability of components in service. This is especially true for complex single-crystal components, where the internal orientation often differs from the surface orientation, with more significant deviations and testing difficulties occurring in areas of structural abrupt change such as pores.

[0003] Currently, for orientation determination of single-crystal materials, only large-scale scientific facilities such as neutron or synchrotron radiation can achieve non-destructive testing, which is insufficient to meet the needs of production sites. Only short-wavelength characteristic X-ray diffraction technology has the potential to determine internal orientation in-situ, non-destructively, and accurately. However, these methods require the X-rays to penetrate the entire sample. -κ or - Performing large-angle scans within space to search for diffraction signals that satisfy the Bragg condition results in long test times, slow measurement speeds, low accuracy, and low efficiency, making it difficult to meet the rapid detection needs of industrial production. Furthermore, differences in θ-axis zero-point drift, mechanical backlash, and clamping methods between different devices can easily introduce systematic errors, causing inconsistent orientation results for the same sample on different devices, affecting data comparability and the uniformity of quality standards. Summary of the Invention

[0004] To address the aforementioned issues, this invention provides a rapid, non-destructive method for determining the internal crystal orientation of single-crystal materials. First, a conventional X-ray diffractometer is used to quickly acquire the surface orientation. Then, through coordinate transformation and vector calculation, the precise range of the azimuth angle of the internal orientation is estimated, thereby narrowing the scanning range of transmission diffraction detection to a smaller area, achieving rapid "surface-to-interior" positioning. Simultaneously, symmetrical testing is performed on both sides of the same sample, and differential calculation is used to eliminate zero-point offset of the equipment, significantly improving testing accuracy and consistency between equipment. This method not only improves the efficiency of single-crystal internal orientation detection but also provides reliable data support for material performance prediction, process optimization, and quality control, achieving a strategy for internal orientation determination that balances speed and accuracy.

[0005] To achieve the above objectives, the technical solutions adopted in the embodiments of the present invention are as follows: This invention provides a rapid and non-destructive method for determining the internal crystal orientation of a single-crystal material, the method comprising the following steps: Step S1: Establish an XYZ three-dimensional rectangular coordinate system as the sample coordinate system based on the single crystal material sample to be tested; Step S2: Using any axis of the sample coordinate system as the diffraction vector direction, a conventional X-ray diffractometer is used to test the surface crystal orientation of any test crystal plane in the sample, using the first test angle. The second test angle χ) represents, where the first test angle is... To test the angle between the projection of the crystal plane normal onto the coordinate plane perpendicular to the diffraction vector direction and the clockwise coordinate axis, the second test angle χ is the angle between the test crystal plane normal and the diffraction vector direction; Step S3: Establish the mapping relationship between the sample coordinate system and the crystal coordinate system, based on the measured first test angle. The second test angle χ characterizes the crystal surface orientation as a vector representation in the sample coordinate system; Step S4: Based on the vector representation of crystal surface orientation, calculate two rotation angles suitable for determining the internal orientation of a single crystal using high-energy X-ray transmission diffraction equipment. The theoretical value of the first rotation angle Ψ is... XRD The theoretical value of the second rotation angle K XRD Wherein, the first rotation angle Ψ is the angle of rotation of the goniometer; the second rotation angle K is the angle of rotation of the Euler ring; Step S5, based on the calculated theoretical value Ψ of the first rotation angle XRD Theoretical value of the second rotation angle K XRD The range of the first rotation angle Ψ was determined using a high-energy X-ray transmission diffraction device. XRD Second rotation angle range K XRD ±Δ; where, Δ and Ψ are the threshold values ​​for the changes in the first rotation angle Ψ and the second rotation angle K, respectively. Step S6: Using a single crystal sample with known orientation as a standard, the zero point position of the rotation angle of the goniometer in the high-energy X-ray transmission diffraction equipment is calibrated. After calibration, the Euler ring plane is perpendicular to the incident X-ray. Step S7, based on the calibrated device and the determined first rotation angle range Ψ XRD Second rotation angle range K XRD ±Δ is used to perform a single-crystal internal orientation scan test on the single-crystal material sample to be tested, so as to obtain the accurate internal orientation of the crystal.

[0006] As a preferred embodiment of the present invention, step S6, calibrating the zero-point position of the rotation angle of the goniometer in the high-energy ray transmission diffraction equipment, includes: Step S61: The standard sample used for calibration has two symmetrical and flat surfaces; the zero point of the goniometer is... ; Step S62: Inject the high-energy X-ray incident beam perpendicular to the test surface of the standard sample. Rotate the standard sample so that the single crystal orientation coincides with the diffraction vector direction. At this time, the intensity of the high-energy X-ray diffraction line reaches its maximum value. Record the first rotation angle at this moment, and denote it as the first calibration angle. Flip the standard sample and incident the high-energy rays perpendicular to the other surface of the standard sample. The other surface is symmetrical and parallel to the test surface. Rotate the standard sample so that the single crystal orientation coincides with the diffraction vector direction. At this time, the intensity of the high-energy ray diffraction line reaches its maximum value again. Record the first rotation angle at this time as the second calibration angle Ψ2. Step S63, according to the first calibration angle Calculate the theoretical zero point Ψ0 of the goniometer using the second calibration angle Ψ2; Step S64, rotate the goniometer to – Set the zero point to zero to complete the zero-point calibration of the equipment.

[0007] In a preferred embodiment of the present invention, the parallelism of the two symmetrical and flat surfaces in step S61 is less than 0.02°.

[0008] In a preferred embodiment of the present invention, step S63 calculates the theoretical zero point Ψ0 of the goniometer; the formula is as follows: = [2 – ( + )] / 2; (7) In equation (7), 2 The diffraction angle is the known orientation crystal plane in the standard sample.

[0009] In a preferred embodiment of the present invention, when establishing the sample coordinate system in step S1, if the crystal is a cuboid, the sample normal ND is defined as the Z-axis, the sample length direction LD is defined as the Y-axis, and the sample transverse direction TD is defined as the X-axis.

[0010] In a preferred embodiment of the present invention, step S3 characterizes the crystal plane orientation as a vector representation in the sample coordinate system, as follows: , i =X or Y or Z (4) in: ,

[0011] In equation (4), ( , , The vector representation of the corresponding crystal plane orientation in the sample coordinate system. express i The unit vector along the axis.

[0012] In a preferred embodiment of the present invention, in step S4, the theoretical value Ψ of the first rotation angle is... XRD The theoretical value of the second rotation angle K XRD The calculation formula is: (5) (6) In equations (5)-(6), 2θ is the diffraction angle of the sample test crystal plane.

[0013] In a preferred embodiment of the present invention, the diffraction angle 2θ in the transmission diffraction mode ranges from 0 to 90°.

[0014] As a preferred embodiment of the present invention, the high-energy ray transmission diffraction equipment in step S4 includes a short-wavelength characteristic X-ray diffractometer, a neutron diffractometer, or a high-energy synchrotron radiation hard X-ray diffractometer.

[0015] In a preferred embodiment of the present invention, when determining the internal orientation of the single crystal using the calibrated equipment in step S7, the high-energy incident rays are incident along the positive X-axis direction of the sample coordinate system, and the Z-axis of the sample coordinate system is vertically upward; the rotating goniometer tilts the sample, and the range of the rotating goniometer is the first rotation angle range Ψ. XRD Then, by rotating the Euler ring, the sample is made to rotate around the surface normal at a second rotation angle K. XRD Rotating within the ±Δ range, when the crystal plane normal coincides with the diffraction vector, the high-energy X-ray diffraction line reaches its maximum value, and the value of the maximum peak is recorded. The combination of K) represents the polar coordinates of the measured crystal plane in the sample coordinate system.

[0016] The solutions of the embodiments of the present invention have the following beneficial effects: The rapid and non-destructive method for determining the internal crystal orientation of single-crystal materials provided in this invention establishes a mathematical conversion model between the surface orientation and internal orientation of a single crystal, proposes a precise calibration method for the zero point of the goniometer in a transmission diffraction testing device, eliminates the systematic error in the calibration of the internal orientation of a single crystal, and thus completes the non-destructive determination of the internal crystal orientation of a single-crystal material, with an orientation angle testing accuracy better than 0. Meanwhile, compared to the inefficient and time-consuming process of obtaining diffraction images by simply using equipment such as neutron diffraction and synchrotron radiation to determine the internal orientation of a single crystal, which requires extensive exploration of rotation angle regions, this invention, based on XRD, first determines the interval between the first and second rotation angles of high-energy X-ray transmission diffraction equipment such as SWXRD to reduce the scanning range and improve the efficiency of the equipment in finding the orientation angle during testing. Overall, this invention improves the accuracy, precision, speed, and efficiency of crystal orientation determination, reduces systematic errors, and enhances universality, providing a new approach for industrial applications.

[0017] Of course, implementing any product or method of the present invention does not necessarily require achieving all of the advantages described above at the same time. Attached Figure Description

[0018] To more clearly illustrate the technical solutions in the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0019] Figure 1 This is a schematic diagram illustrating the determination of the coordinate system of the material sample in an embodiment of the present invention; Figure 2 This is a schematic diagram of the conventional X-ray diffraction and reflection optical path test principle in an embodiment of the present invention; Figure 3 This is a schematic diagram of the transmission optical path for single-crystal orientation determination using a high-energy X-ray transmission diffraction device in an embodiment of the present invention. Figure 4 This is the first calibration optical path diagram of the high-energy ray transmission diffraction equipment in this embodiment of the invention; Figure 5 This is the second calibration optical path diagram of the high-energy ray transmission diffraction equipment in this embodiment of the invention.

[0020] Explanation of reference numerals in the attached figures: 01 - Diffraction vector direction; 10 - Sample; 11 - Soft X-ray incident line; 12 - 13-Extension of incident light of soft X-rays, 14-χ-axis, 15-Soft X-ray diffraction line, 21-Incident light of high-energy X-rays, 22-Euler ring, 23-Extension of incident light of high-energy X-rays, 24-Goniometer, 25-High-energy X-ray diffraction line, 26-Single crystal orientation, 27-Theoretical zero point Ψ0 of goniometer, 28-Cognitive zero point of goniometer . Detailed Implementation

[0021] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of them. The components of the embodiments of the present invention described and shown in the accompanying drawings can generally be arranged and designed in various different configurations. It should be noted that, without conflict, the embodiments and features in the embodiments of the present invention can also be combined with each other.

[0022] It should be noted that similar reference numerals and letters in the following figures indicate similar items; therefore, once an item is defined in one figure, it does not need to be further defined and explained in subsequent figures. In the description of this invention, the terms "first," "second," "third," "fourth," etc., are used only to distinguish descriptions and should not be construed as indicating or implying relative importance.

[0023] This invention provides a rapid and non-destructive method for determining the internal crystal orientation of single-crystal materials. Based on a three-dimensional rectangular coordinate system established by the sample itself, the surface orientation is obtained using a conventional X-ray diffractometer and converted into a vector representation. Combining the principle of high-energy X-ray diffraction testing, an orientation calculation method suitable for transmission optical paths is proposed, narrowing the scanning range for detecting the crystal orientation using transmission diffraction. This allows for the rapid determination of the internal orientation of a certain crystal orientation in a single-crystal material. Furthermore, through secondary determination of the internal crystal orientation of the single crystal, a method for zero-point calibration and error correction of the internal orientation test using high-energy X-ray diffraction instruments is achieved. This significantly improves the speed, accuracy, and repeatability of single-crystal internal orientation determination, while also reducing the relative deviation caused by differences in the zero points of different internal diffraction detection devices.

[0024] The method for rapid and non-destructive determination of the internal crystal orientation of single-crystal materials includes the following steps: Step S1: Establish an XYZ three-dimensional rectangular coordinate system as the sample coordinate system based on the single crystal material sample to be tested.

[0025] In this step, such as Figure 1As shown, in one executable embodiment, taking the case where the crystal is a cuboid as an example, the sample normal direction (ND) is defined as the Z-axis, the sample length direction (LD) as the Y-axis, and the sample transverse direction (TD) as the X-axis. When the sample shape is other, the same definition method is used, and the executable origin is selected. Once the three-dimensional rectangular coordinate system is determined, it is bound to the single crystal material sample and does not undergo translation or rotation relative to the material itself.

[0026] Step S2: Using any axis of the sample coordinate system as the diffraction vector direction, use an X-ray diffractometer to test the first test angle of any test crystal plane in the sample. The second test angle χ and the diffraction angle 2θ are determined by the test crystal plane, where the first test angle... To test the angle between the projection of the crystal plane normal onto the coordinate plane perpendicular to the diffraction vector direction and the clockwise coordinate axis, the second test angle χ is the angle between the crystal plane normal and the diffraction vector direction.

[0027] In this step, when the diffraction vector is perpendicular to the XOY plane, i.e., the Z-axis is the direction of the diffraction vector, the first test angle is measured. z Second test angle χ z When the diffraction vector is perpendicular to the YOZ plane, i.e., the X-axis is the direction of the diffraction vector, the first test angle is measured. x Second test angle χ x When the diffraction vector is perpendicular to the XOZ plane, i.e., the Y-axis is the direction of the diffraction vector, the first test angle is measured. y Second test angle χ y The diffraction vector lies in the plane of the incident and diffracted rays and is the angle bisector of their angle. Due to the limitations of ordinary X-ray diffractometers, it is impossible to detect all orientations of the same crystal system on a single surface of a sample. Therefore, one or more surfaces may be selected for testing as needed. However, it is also possible to detect the same orientation on multiple surfaces. The first test angle for the same orientation obtained from testing different surfaces is... The first test angle χ differs from the second test angle, but the final calculated coordinate or vector representation of the crystal plane in the three-dimensional coordinate system is the same; different orientations of the first test angle obtained by testing different surfaces. Because the second test angle χ is different, the final calculated coordinate representation of the crystal plane in the three-dimensional coordinate system is also different.

[0028] like Figure 2As shown, when using conventional X-rays for testing, a standard X-ray diffractometer (laboratory θ-2θ type) is used for measurement. The soft X-ray incident beam 11 enters the sample 10 after incident, and is rotated... Axis 12 allows the sample to rotate around the surface normal (0-360°), and axis 14 tilts the sample (0-90°). When the crystal plane normal coincides with the diffraction vector, soft X-ray diffraction line 15 reaches its maximum value. Record the points where the maximum peak appears. By combining , χ), we can obtain the polar coordinates of the {hkl} crystal plane normal in the XYZ coordinate system.

[0029] Step S3: Establish the mapping relationship between the sample coordinate system and the crystal coordinate system, based on the measured first test angle. The second test angle χ represents the crystal surface orientation as a vector representation in the sample coordinate system.

[0030] In this step, two test angles measured with any axis in the sample coordinate system as the diffraction vector direction are used to characterize the crystal plane normal of the sample, and further to characterize the crystal plane orientation. The selected crystal plane orientation, i.e., the crystal plane normal, is represented as a vector in the coordinate system as follows: When the X-axis is selected as the diffraction vector direction, the corresponding test surface is the YOZ plane. The vector representation of the current crystal plane orientation in the sample coordinate system is as follows: ( , , ) X =(cosχ z , sinχ z sin z , sinχ z cos z (1) When the Y-axis is selected as the diffraction vector direction, the corresponding test surface is the XOZ plane. The vector representation of the current crystal plane orientation in the sample coordinate system is as follows: ( , , ) Y =(sinχ y sin y , cosχ y , sinχ y cos y (2) When the Z-axis is selected as the diffraction vector direction, the corresponding test surface is the XOY plane. The vector representation of the current crystal plane orientation in the sample coordinate system is as follows: ( , , ) Z =(sinχ z cos z , sinχ z sin z , cosχ z (3) Unifying the crystal orientation vectors in the above three axial cases into a general matrix form, it can be expressed as: , i =X or Y or Z (4) in: ,

[0031] In equation (4), ( , , The vector representation of the corresponding crystal plane orientation in the sample coordinate system. express i The unit vector along the axis.

[0032] In this step, during routine X-ray diffraction testing, it should be noted that when detecting the orientation of the YOZ plane, the Z-axis should be perpendicular to the plane containing the incident and diffracted rays, and the Y-axis should be parallel to that plane; similarly, when detecting the orientation of the XOZ plane, the Z-axis should be perpendicular to the plane containing the incident and diffracted rays, and the X-axis should be parallel to that plane; when detecting the orientation of the XOY plane, the Y-axis should be perpendicular to the plane containing the incident and diffracted rays, and the X-axis should be parallel to that plane.

[0033] Step S4: Based on the vector representation of the crystal surface orientation, calculate the theoretical value Ψ of the first rotation angle Ψ suitable for testing with high-energy X-ray transmission diffraction equipment. XRD The theoretical value of the second rotation angle K XRD Wherein, the first rotation angle Ψ is the angle of rotation of the goniometer; the second rotation angle K is the angle of rotation of the Euler ring.

[0034] In this step, the theoretical value Ψ of the first rotation angle... XRD The theoretical value of the second rotation angle K XRD The calculation formula is: (5) (6) In equations (5)-(6), 2θ is the diffraction angle of the sample test crystal plane. The diffraction angle is a fixed value, which can be determined by high-energy X-ray transmission diffraction equipment through diffraction angle scanning test. The diffraction angle range of the transmission diffraction mode is 0-90°.

[0035] It should be noted that the high-energy X-ray transmission diffraction equipment mentioned in this step includes short-wavelength characteristic X-ray diffractometers (SWXRD), neutron diffractometers, or high-energy synchrotron radiation hard X-ray diffractometers, etc. Figure 3 As shown, the high-energy ray transmission diffraction device includes, in addition to the basic ray generating device, at least a goniometer and an Euler ring.

[0036] Step S5, based on the calculated theoretical value Ψ of the first rotation angle XRD Theoretical value of the second rotation angle K XRD The range of the first rotation angle Ψ was determined using a high-energy X-ray transmission diffraction device. XRD Second rotation angle range K XRD ±Δ; where, Δ and Δ are the threshold values ​​for the changes in the first rotation angle Ψ and the second rotation angle K, respectively.

[0037] In this step, when determining the angle range, the variation threshold is selected based on the conventional X-ray diffraction test scan curve. And the value of Δ.

[0038] Step S6: Using a single crystal sample with known orientation as a standard, the zero point position of the rotation angle of the goniometer in the high-energy X-ray transmission diffraction equipment is calibrated. After calibration, the Euler ring plane is perpendicular to the incident X-ray.

[0039] like Figure 4 and Figure 5 As shown, specifically, the calibration process includes: Step S61: The standard sample used for calibration has two symmetrical and flat surfaces with a parallelism of less than 0.02°; the zero point of the goniometer is... 28.

[0040] In this step, the position considered the true zero point for the goniometer always deviates from the absolute zero point position by a certain degree. This deviation angle is the initial zero point angle, or the perceived zero point. 28. The calibration process also involves finding the optimal deviation angle, i.e., the theoretical zero point Ψ027, based on the existing standard sample.

[0041] In step S62, the high-energy incident beam 21 is incident perpendicularly to the test surface of the standard sample 10. The standard sample 10 is rotated so that the single crystal orientation 26 coincides with the diffraction vector direction 01. At this time, the intensity of the high-energy diffracted beam 25 reaches its maximum value. The first rotation angle at this time is recorded, which is the angle through which the goniometer rotates during this process, and is recorded as the first calibration angle. Flip the standard sample 10 and direct the high-energy ray incident line 21 perpendicular to the direction of the other surface of the standard sample 10. The other surface is symmetrical and parallel to the test surface. Rotate the standard sample 10 so that the single crystal orientation 26 coincides with the diffraction vector direction 01. At this time, the intensity of the high-energy ray diffraction line 25 reaches its maximum value again. Record the first rotation angle at this time as the second calibration angle Ψ2.

[0042] Step S63, calculate the theoretical zero point Ψ027 of the goniometer, using the following formula: = [2 – ( + )] / 2; (7) In equation (7), 2 The diffraction angle is the known orientation crystal plane in the standard sample.

[0043] Step S64, rotate the goniometer to – Set the zero point to zero to complete the zero-point calibration of the equipment.

[0044] In high-energy X-ray transmission diffraction (XRD) equipment such as SWXRD, the Euler ring is mounted on a goniometer, with the axis of the Euler ring intersecting the axis of the goniometer at a single point. When the goniometer rotates, it carries the Euler ring along with it, while the Euler ring rotates about its central axis. Using a single-crystal sample with a known orientation and two symmetrical and parallel surfaces, the second rotation angle and diffraction angle are measured when light rays incident perpendicularly from the two surfaces diffract along the known orientation within the sample. The goniometer is then adjusted to the theoretical zero point position, at which point the plane of the Euler ring is perpendicular to the incident light rays.

[0045] Step S7, based on the calibrated high-energy ray transmission diffraction equipment and the determined first rotation angle range Ψ XRD Second rotation angle range K XRD ±Δ is used to perform orientation tests on the single-crystal material sample to obtain the precise internal orientation of the crystal.

[0046] In this step, when determining the orientation of a single crystal using a calibrated high-energy X-ray transmission diffraction device, such as... Figure 3As shown, the high-energy incident ray 21 is incident along the positive X-axis of the sample coordinate system, and the Z-axis of the sample coordinate system is vertically upward. After the high-energy incident ray 21 enters the sample 10, it is perpendicular to the plane containing the Euler rings, that is, perpendicular to the sample surface, and must coincide with the coordinate axes of the sample coordinate system. The rotating goniometer 24 tilts the sample, and the range of the rotating goniometer is the first rotation angle range Ψ. XRD Then, by rotating the Euler ring 22, the sample is made to rotate around the surface normal at a second rotation angle K. XRD Rotating within the ±Δ range, when the crystal plane normal coincides with the diffraction vector 01, the high-energy X-ray diffraction line 25 reaches its maximum value. The point at which the maximum peak appears is recorded. The K) combination represents the polar coordinates of the measured crystal plane in the sample coordinate system, thereby accurately determining the internal orientation of the single crystal sample to be tested.

[0047] The rapid and non-destructive method for determining the internal crystal orientation of single-crystal materials described in this embodiment of the invention was applied to a nickel-based single-crystal sample for surface orientation testing. The testing equipment used was SWXRD, and the testing planes were the YOZ plane and the XOZ plane, respectively.

[0048] For the YOZ plane, the test crystal plane is {002}, and the orientation (χ, The internal orientation is (20, 16). According to the calculation, the corresponding internal orientation is (87.62, 19.19). After calibration, the internal orientation (Ψ, K) is measured to be (87.34, 19.54), and the test error is less than 0.1°.

[0049] For the XOZ plane, the test crystal plane is {002}, and the orientation (χ, The internal orientation is (5, 12). According to the calculation, the corresponding internal orientation is (4.41, 4.89). After calibration, the internal orientation (Ψ, K) is measured to be (4.62, 5.23).

[0050] Therefore, the rapid and non-destructive method for determining the internal crystal orientation of single-crystal materials provided in this embodiment of the invention has an orientation angle testing accuracy better than 0. This improves the accuracy, precision, and speed of crystal orientation determination, reduces systematic errors, and enhances universality, providing new ideas for industrial applications.

[0051] The above description is merely a preferred embodiment of the present invention and an explanation of the technical principles employed, and is not intended to limit the scope of the claimed invention, but merely to illustrate preferred embodiments of the invention. Those skilled in the art should understand that the scope of the invention is not limited to the specific combinations of the above-described technical features, but should also cover other technical solutions formed by arbitrary combinations of the above-described technical features or their equivalents without departing from the inventive concept. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention.

Claims

1. A rapid and non-destructive method for determining the internal crystal orientation of a single-crystal material, characterized in that, The method includes the following steps: Step S1: Establish an XYZ three-dimensional rectangular coordinate system as the sample coordinate system based on the single crystal material sample to be tested; Step S2: Using any axis of the sample coordinate system as the diffraction vector direction, a conventional X-ray diffractometer is used to test the surface crystal orientation of any test crystal plane in the sample, using the first test angle. The second test angle χ) represents, where the first test angle is... To test the angle between the projection of the crystal plane normal onto the coordinate plane perpendicular to the diffraction vector direction and the clockwise coordinate axis, the second test angle χ is the angle between the test crystal plane normal and the diffraction vector direction; Step S3: Establish the mapping relationship between the sample coordinate system and the crystal coordinate system, based on the measured first test angle. The second test angle χ characterizes the crystal surface orientation as a vector representation in the sample coordinate system; Step S4: Based on the vector representation of crystal surface orientation, calculate two rotation angles suitable for determining the internal orientation of a single crystal using high-energy X-ray transmission diffraction equipment. The theoretical value of the first rotation angle Ψ is... XRD The theoretical value of the second rotation angle K XRD Wherein, the first rotation angle Ψ is the angle of rotation of the goniometer; the second rotation angle K is the angle of rotation of the Euler ring; Step S5, based on the calculated theoretical value Ψ of the first rotation angle XRD Theoretical value of the second rotation angle K XRD The range of the first rotation angle Ψ was determined using a high-energy X-ray transmission diffraction device. XRD Second rotation angle range K XRD ±Δ; where, Δ and Ψ are the threshold values ​​for the changes in the first rotation angle Ψ and the second rotation angle K, respectively. Step S6: Using a single crystal sample with known orientation as a standard, the zero point position of the rotation angle of the goniometer in the high-energy X-ray transmission diffraction equipment is calibrated. After calibration, the Euler ring plane is perpendicular to the incident X-ray. Step S7, based on the calibrated device and the determined first rotation angle range Ψ XRD Second rotation angle range K XRD ±Δ is used to perform a single-crystal internal orientation scan test on the single-crystal material sample to be tested, so as to obtain the accurate internal orientation of the crystal.

2. The method according to claim 1, characterized in that, Step S6, which involves calibrating the zero-point position of the goniometer rotation angle in the high-energy ray transmission diffraction equipment, includes: Step S61: The standard sample used for calibration has two symmetrical and flat surfaces; the zero point of the goniometer is... ; Step S62: Inject the high-energy X-ray incident beam perpendicular to the test surface of the standard sample. Rotate the standard sample so that the single crystal orientation coincides with the diffraction vector direction. At this time, the intensity of the high-energy X-ray diffraction line reaches its maximum value. Record the first rotation angle at this moment, and denote it as the first calibration angle. Flip the standard sample and incident the high-energy rays perpendicular to the other surface of the standard sample. The other surface is symmetrical and parallel to the test surface. Rotate the standard sample so that the single crystal orientation coincides with the diffraction vector direction. At this time, the intensity of the high-energy ray diffraction line reaches its maximum value again. Record the first rotation angle at this time as the second calibration angle Ψ2. Step S63, according to the first calibration angle Calculate the theoretical zero point Ψ0 of the goniometer using the second calibration angle Ψ2; Step S64, rotate the goniometer to – Set the zero point to zero to complete the zero-point calibration of the equipment.

3. The method according to claim 2, characterized in that, In step S61, the parallelism of the two symmetrical and flat surfaces is less than 0.02°.

4. The method according to claim 2, characterized in that, Step S63: Calculate the theoretical zero point Ψ0 of the goniometer; the formula is as follows: = [2 – ( + )] / 2；(7) In equation (7), 2 The diffraction angle is the known orientation crystal plane in the standard sample.

5. The method according to claim 1, characterized in that, When establishing the sample coordinate system in step S1, if the crystal is a cuboid, the sample normal ND is defined as the Z-axis, the sample length direction LD as the Y-axis, and the sample transverse direction TD as the X-axis.

6. The method according to claim 1, characterized in that, Step S3 characterizes the crystal plane orientation as a vector representation in the sample coordinate system, with the following general formula: , i =X or Y or Z(4) in: , In equation (4), ( , , The vector representation of the corresponding crystal plane orientation in the sample coordinate system. express i The unit vector along the axis.

7. The method according to claim 6, characterized in that, In step S4, the theoretical value Ψ of the first rotation angle XRD The theoretical value of the second rotation angle K XRD The calculation formula is: (5) ](6) In equations (5)-(6), 2θ is the diffraction angle of the sample test crystal plane.

8. The method according to claim 7, characterized in that, The diffraction angle 2θ in transmission diffraction mode ranges from 0 to 90°.

9. The method according to claim 1, characterized in that, In step S4, the high-energy X-ray transmission diffraction equipment includes a short-wavelength characteristic X-ray diffractometer, a neutron diffractometer, or a high-energy synchrotron radiation hard X-ray diffractometer.

10. The method according to claim 1, characterized in that, In step S7, when determining the internal orientation of a single crystal using calibrated equipment, the high-energy incident rays are incident along the positive X-axis of the sample coordinate system, and the Z-axis of the sample coordinate system is vertically upward; the goniometer is rotated to tilt the sample, and the range of the goniometer is the first rotation angle range Ψ. XRD Then, by rotating the Euler ring, the sample is made to rotate around the surface normal at a second rotation angle K. XRD Rotating within the ±Δ range, when the crystal plane normal coincides with the diffraction vector, the high-energy X-ray diffraction line reaches its maximum value, and the value of the maximum peak is recorded. The combination of K) represents the polar coordinates of the measured crystal plane in the sample coordinate system.

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