A method for measuring the texture of aluminum alloy can body material plate by XRD

Abstract

The invention discloses a method for measuring the texture of aluminum alloy can body material plate by XRD, which belongs to the technical field of plate texture measurement, including fixing the dried sample and the sample fixing block together on the XRD sample stage with plasticine, the X-axis centering notch coincides with the X-axis of the XRD sample stage, the Y-axis centering notch coincides with the Y-axis of the XRD sample stage, and the rolling direction of the sample is parallel to the Y-axis of the XRD sample stage; measuring the physical phase after successful calibration, performing texture measurement after the physical phase measurement is completed, selecting the texture sample stage, setting the starting angle, ending angle, scanning mode, scanning speed and slit conditions of the test voltage and current input measurement; performing data processing after the texture measurement is completed, and obtaining the pole figure PF of the material corresponding to the sample and the three-dimensional orientation diagram ODF of the polycrystalline material. The invention standardizes the method for testing the texture of materials by X-ray method, and ensures the accuracy and repeatability of testing the texture of can body material plate by XRD.

Description

Technical Field

[0001] The invention discloses a method for measuring the texture of a plate material of an aluminum alloy can body by XRD, and belongs to the technical field of plate texture measurement. Background Art

[0002] When metal materials are deformed by rolling, stretching, extrusion, etc., due to the action of external forces, the grains will be arranged along certain directions, showing more or less statistical uneven distribution (different orientation probability distribution). This phenomenon is called preferential orientation, and this organizational structure is called texture. The existence of texture has a very important influence on various electrical, magnetic, thermal, and mechanical properties of materials. Therefore, measuring the texture of metal materials has important guiding significance for understanding the plastic deformation law of metals and controlling the processing technology.

[0003] The production process of aluminum alloy can body material plate includes homogenizing, hot rough rolling and hot finishing rolling of aluminum alloy ingots, and the final rolling thickness is 0.2-0.4mm. The rolled plate undergoes more than 40 processes to be made into the aluminum cans we see. Therefore, the above plate is required to have good deep drawing forming performance, fatigue resistance, corrosion resistance, excellent surface quality, high strength, sufficient plasticity, small earing rate and strict dimensional deviation, which requires the material to have suitable chemical composition, excellent metallurgical quality, reasonable texture and plate shape tolerance, etc. At present, the measurement of macro texture is mainly based on XRD. XRD texture test requires high flatness on both sides of the sample, otherwise the measurement result will be inaccurate.

[0004] When measuring the XRD texture of aluminum alloy can body material plates, the method used is to saw the plate with a thickness of 0.259mm into a rectangular sample of 15mm*15mm, and then use plasticine to stick the sample on the XRD multifunctional sample table. When sticking, pay attention to the rolling direction of the sample parallel to the longitudinal axis of the sample table, and it cannot be skewed. The sample is firmly fixed on the sample table and flattened using a level, and then the sample is calibrated and tested. The disadvantage of this method is that due to the thinness of the sample, it is inevitable to cause deformation of the sample during sawing or shearing. When fixing the sample, it causes the sample to be fixed on the sample table with plasticine. After the level is calibrated with a level, the deformed sample rebounds during the test, resulting in the upper and lower surfaces of the sample being non-parallel, which ultimately affects the accuracy of the texture measurement results and leads to extremely poor repeatability of the results. The texture results of the same sample tested at different times vary greatly.

[0005] The existing patents of sample fixing devices for XRD texture measurement, such as the sample fixing device for superconducting tape XRD texture measurement disclosed in the prior art CN201510206310.3, invented a sample fixing device for vacuum adsorption, which is only suitable for measuring very thin and easily deformed superconducting tape samples. For can plates, due to their thick thickness, the sample fixing and vacuum adsorption effects are not good. Therefore, in view of the limitations of samples in the existing X-ray diffractometer texture analysis, a method for sample preparation and test analysis of can material samples with coil deformation is designed and invented, which is an urgent need for material texture measurement. Summary of the invention

[0006] The object of the present invention is to provide a method for measuring the texture of aluminum alloy can body plate material by XRD, so as to solve the problem of low accuracy of plate texture measurement in the prior art.

[0007] A method for measuring the texture of an aluminum alloy can body material plate by XRD, using a sample fixing device for measuring the texture of an aluminum alloy can body material plate by XRD, the sample fixing device comprising a sample fixing block, an X-axis sample centering auxiliary line, a Y-axis sample centering auxiliary line, an X-axis centering notch and a Y-axis centering notch, the sample fixing device being fixed on an XRD sample stage by plasticine, the method comprising:

[0008] Step 1, use a precision cutting saw to saw the sample into rectangular blocks;

[0009] Step 2, fix the sawn sample on the sample fixing device with strong glue, referring to the X-axis sample centering auxiliary line and the Y-axis sample centering auxiliary line, and the rolling direction of the sawn sample is parallel to the Y-axis sample centering auxiliary line;

[0010] Step 3, sanding and metallographic polishing the fixed sample to obtain a pretreated sample;

[0011] Step 4, rinsing the pretreated sample with alcohol and drying it;

[0012] Step 5, fix the dried sample together with the sample fixing block on the XRD sample stage with plasticine, the X-axis centering notch coincides with the X-axis of the XRD sample stage, the Y-axis centering notch coincides with the Y-axis of the XRD sample stage, the rolling direction of the sample is parallel to the Y-axis of the XRD sample stage, and a level is placed on the sample for leveling again to obtain the installed sample;

[0013] Step 6, turning on the X-ray diffractometer and the water cooler, and aging the X-ray diffractometer;

[0014] Step 7, after the X-ray diffractometer aging is completed, the tube voltage and tube current are manually controlled to the test setting range;

[0015] Step 8, calibrate the installed sample and the sample fixing block, start the automatic calibration program of the calibration instrument, and perform calibration;

[0016] Step 9, after successful calibration, measure the physical phase, select the corresponding sample stage, set the test voltage, current, input measurement start angle, end angle, scanning mode, scanning speed and slit conditions;

[0017] Step 10, after the physical phase measurement is completed, the texture measurement is performed, the texture sample stage is selected, and the test voltage, current, input measurement start angle, end angle, scanning mode, scanning speed and slit conditions are set;

[0018] Step 11: After the texture measurement is completed, data processing is performed to obtain the pole figure PF of the material corresponding to the sample and the three-dimensional orientation diagram ODF of the polycrystalline material.

[0019] The size of the rectangular block is 15mm×15mm, the thickness is 0.259mm, and the thickness of the sample fixing block is 5mm.

[0020] During calibration, insert three copper absorbers into the calibration instrument;

[0021] When measuring the physical phase and texture, remove the copper absorber and replace it with Kβ Absorbing film to obtain monochromatic X-rays.

[0022] The XRD sample stage is provided with vertically intersecting X-axis and Y-axis;

[0023] The X-axis specimen centering auxiliary line and the Y-axis specimen centering auxiliary line intersect vertically and are located at the top of the sample fixture;

[0024] The X-axis centering notch and the Y-axis centering notch are both line-shaped, and the two cross each other vertically and are arranged at the bottom of the sample fixing device.

[0025] Use sandpaper ranging from 1500# to 2000# for grinding.

[0026] Use a hair dryer to blow the pretreated specimen.

[0027] The voltage for aging of the X-ray diffractometer was 20KV and the current was 20mA;

[0028] The test setting range of the control tube voltage and tube current is tube voltage range 20KV-50KV, and tube current range 2mA-60mA.

[0029] When measuring the physical phase, set the test voltage to 40KV, the current to 20mA, the input measurement starting angle to 5°-20°, the ending angle to 70-90°, the scanning speed to 2° / min -10° / min, and the incident slit to 2mm-10mm.

[0030] When measuring the physical phase, find the diffraction peak position of each test surface. The test surfaces are 111 crystal plane, 200 crystal plane and 220 crystal plane, and the corresponding angle ranges are 30-40°, 40-50°, and 60-70°, respectively. After determining the diffraction peak position of each test surface, directly input the corresponding diffraction peak angle in the subsequent texture parameter determination.

[0031] The corresponding angles of the 111, 200 and 220 crystal planes are 37.77°, 44.02° and 64.43° respectively.

[0032] Compared with the prior art, the present invention has the following beneficial effects: it avoids the problem that the sample cannot be polished on both sides to keep the upper and lower surfaces of the sample parallel due to its thinness; the method of using strong glue to stick to the sample fixture avoids the problem of inaccurate test results caused by deformation of the sample during the test due to the elasticity of the sample when using plasticine to fix it; at the same time, X-axis and Y-axis auxiliary lines are engraved on the upper surface of the sample fixture, which is convenient for ensuring that the rolling direction of the sample is parallel to the Y-axis auxiliary line during the sample pasting process; the X-axis and Y-axis notches below the sample fixture can ensure that the sample fixture and the sample are installed on the X-ray diffractometer to ensure that the X-axis and Y-axis auxiliary lines on the sample table coincide, and ensure that the rolling direction of the sample is parallel to the Y-axis direction of the X-ray diffractometer when it is installed. At the same time, the method of testing the texture of the material by X-ray method is standardized, and the accuracy and repeatability of the texture of the can body material plate tested by XRD are guaranteed from several aspects such as sample preparation, X-ray opening, and parameter setting during the test. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 A sample fixing device of the present invention;

[0034] Figure 2 This is a diagram showing the springback texture results of a sample not using the present invention;

[0035] Figure 3 This is a diagram showing the springback texture results of the sample of the present invention;

[0036] The reference numerals include: 1 - sample fixing block, 2 - X-axis sample centering auxiliary line, 3 - Y-axis sample centering auxiliary line, 4 - X-axis centering notch, 5 - Y-axis centering notch. DETAILED DESCRIPTION

[0037] In order to make the purpose, technical solution and advantages of the present invention clearer, the technical solution of the present invention is described clearly and completely below. Obviously, the described embodiments are part of the embodiments of the present invention, but not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0038] A method for measuring the texture of aluminum alloy can body material plate by XRD, using a sample fixing device for measuring the texture of aluminum alloy can body material plate by XRD, the sample fixing device comprises a sample fixing block 1, an X-axis sample centering auxiliary line 2, a Y-axis sample centering auxiliary line 3, an X-axis centering notch 4 and a Y-axis centering notch 5, and the sample fixing device is fixed on an XRD sample stage by plasticine, and the method comprises:

[0039] Step 1, use a precision cutting saw to saw the sample into rectangular blocks;

[0040] Step 2, referring to the X-axis sample centering auxiliary line 2 and the Y-axis sample centering auxiliary line 3, fix the sawn sample on the sample fixing device with strong glue, and the rolling direction of the sawn sample is parallel to the Y-axis sample centering auxiliary line 3;

[0041] Step 3, sanding and metallographic polishing the fixed sample to obtain a pretreated sample;

[0042] Step 4, rinsing the pretreated sample with alcohol and drying it;

[0043] Step 5, fix the blow-dried sample together with the sample fixing block 1 on the XRD sample stage with plasticine, the X-axis centering notch 4 coincides with the X-axis of the XRD sample stage, the Y-axis centering notch 5 coincides with the Y-axis of the XRD sample stage, the rolling direction of the sample is parallel to the Y-axis of the XRD sample stage, and a level is placed on the sample for leveling again to obtain the installed sample;

[0044] Step 6, turning on the X-ray diffractometer and the water cooler, and aging the X-ray diffractometer;

[0045] Step 7, after the X-ray diffractometer aging is completed, the tube voltage and tube current are manually controlled to the test setting range;

[0046] Step 8, calibrate the installed sample with the sample fixing block 1, start the automatic calibration program of the calibration instrument, and perform calibration;

[0047] Step 9, after successful calibration, measure the physical phase, select the corresponding sample stage, set the test voltage, current, input measurement start angle, end angle, scanning mode, scanning speed and slit conditions;

[0048] Step 10, after the physical phase measurement is completed, the texture measurement is performed, the texture sample stage is selected, and the test voltage and current input measurement start angle, end angle, scanning mode, scanning speed and slit conditions are set;

[0049] Step 11: After the texture measurement is completed, data processing is performed to obtain the pole figure PF of the material corresponding to the sample and the three-dimensional orientation diagram ODF of the polycrystalline material.

[0050] The size of the rectangular block is 15 mm × 15 mm, the thickness is 0.259 mm, and the thickness of the sample fixing block 1 is 5 mm.

[0051] During calibration, insert three copper absorbers into the calibration instrument;

[0052] When measuring the physical phase and texture, remove the copper absorber and replace it with Kβ Absorbing film to obtain monochromatic X-rays.

[0053] The XRD sample stage is provided with vertically intersecting X-axis and Y-axis;

[0054] The X-axis sample centering auxiliary line 2 and the Y-axis sample centering auxiliary line 3 are vertically intersected and are arranged on the top of the sample fixing device;

[0055] The X-axis centering notch 4 and the Y-axis centering notch 5 are both in the shape of lines, and the two intersect vertically and are arranged at the bottom of the sample fixing device.

[0056] Use sandpaper ranging from 1500# to 2000# for grinding.

[0057] Use a hair dryer to blow the pretreated specimen.

[0058] The voltage for aging of the X-ray diffractometer was 20KV and the current was 20mA;

[0059] The test setting range of the control tube voltage and tube current is tube voltage range 20KV-50KV, and tube current range 2mA-60mA.

[0060] When measuring the physical phase, set the test voltage to 40KV, the current to 20mA, the input measurement starting angle to 5°-20°, the ending angle to 70-90°, the scanning speed to 2° / min -10° / min, and the incident slit to 2mm-10mm.

[0061] When measuring the physical phase, find the diffraction peak position of each test surface. The test surfaces are 111 crystal plane, 200 crystal plane and 220 crystal plane, and the corresponding angle ranges are 30-40°, 40-50°, and 60-70°, respectively. After determining the diffraction peak position of each test surface, directly input the corresponding diffraction peak angle in the subsequent texture parameter determination.

[0062] The corresponding angles of the 111, 200 and 220 crystal planes are 37.77°, 44.02° and 64.43° respectively.

[0063] In the present invention, the sample is cut by a precision cutting saw instead of scissors to avoid deformation of the sample caused by the shear effect. When the sample is glued to the sample fixing block 1 by strong glue, the surface of the sample to be tested can be polished to ensure the horizontality of the test surface, avoiding the phenomenon that the sample falls out during the grinding and polishing process when the sample is inlaid; when the sample is glued to the sample fixing block 1 by strong glue, it can be ensured that it always remains horizontal during the sample test process, and the sample will not be uneven due to the test rebound, affecting the accuracy and repeatability of the test results; the thickness of the sample fixing block 1 can facilitate manual polishing and does not affect the maximum thickness requirement of the XRD texture determination. The data of the present invention uses the ODF diagram to express the orientation distribution of the entire space, which can avoid the limitation that the PF diagram uses two-dimensional graphics to describe the orientation distribution of three-dimensional space.

[0064] The present invention fixes the sample on the sample fixing block through the design of the sample fixing device. The sample thickness is 0.259mm and the fixing block thickness is 5mm. After sticking together, manual grinding and polishing can be conveniently performed, which solves the problem that the sample is too thin and needs to be embedded and polished. The sample is stuck on the fixing block for grinding and polishing, which solves the problem that the embedded sample is easy to fall off during the grinding and polishing process. The sample fixing block of the invention, the X-axis and Y-axis centering auxiliary lines on the sample installation surface can ensure that the sample rolling direction is parallel to the Y-axis auxiliary line every time, which is convenient for the fixation of the sample. The sample fixing block of the invention, the X-axis centering notch 4 and the Y-axis centering notch 5 below the fixing block can ensure that the Y-axis of the sample fixing block coincides with the Y-axis of the X-ray diffractometer when the sample fixing block is installed, and ensure that the sample rolling direction is parallel to the Y-axis direction of the X-ray diffractometer. Aging before the start of the X-ray diffractometer test can increase the service life of the X-ray light tube. Manual pressurization and increase of tube current before the start of the X-ray diffractometer test can avoid sudden pressurization to damage the X-ray light tube. Calibration of the sample before each experiment can ensure that the level of the sample's detection surface is parallel to the upper and lower surfaces, thereby improving the accuracy of the test. Before testing the sample, the texture of the aluminum alloy sample is first tested physically to find the diffraction peak position of each test surface. The test surfaces are 111, 200, and 220, and the corresponding 2-fold angle range is 30-40°, 40-50°, and 60-70°, respectively. Accurately determine the diffraction peak position of each test surface and directly input the corresponding diffraction peak angle when determining the texture parameters later. After the determination is completed, data processing is performed to obtain the corresponding material PF map and ODF map, completing the material texture test. The data uses the ODF map to express the orientation distribution of the entire space, which can avoid the limitation of the PF map using two-dimensional graphics to describe the orientation distribution of three-dimensional space.

[0065] The sample fixing device of the present invention is as follows Figure 1As shown, the sample fixing block 1, the X-axis sample centering auxiliary line 2, the Y-axis sample centering auxiliary line 3, the X-axis centering notch 4 and the Y-axis centering notch 5, the sample rebound texture result diagram of the sample not using the present invention is as shown in Figure 2 As shown in the figure, different colors represent the rebound texture level, the maximum value is 6.765, the minimum value is 0.001, and the rebound texture results of the sample of the present invention are as follows: Figure 3 As shown, different color legends in the figure represent the rebound texture level, with the maximum value being 16.022 and the minimum value being 0.001.

[0066] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit the same. Although the present invention has been described in detail with reference to the aforementioned embodiments, a person skilled in the art should understand that the technical solutions described in the aforementioned embodiments may still be modified, or some or all of the technical features may be replaced by equivalents, and these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for measuring the texture of aluminum alloy can body material plate by XRD, using a sample fixing device for measuring the texture of aluminum alloy can body material plate by XRD, the sample fixing device comprising a sample fixing block, an X-axis sample centering auxiliary line, a Y-axis sample centering auxiliary line, an X-axis centering notch and a Y-axis centering notch, the sample fixing device is fixed on the XRD sample stage by plasticine, characterized in that: The method comprises: Step 1, use a precision cutting saw to saw the sample into rectangular blocks; Step 2, fix the sawn sample on the sample fixing device with strong glue, referring to the X-axis sample centering auxiliary line and the Y-axis sample centering auxiliary line, and the rolling direction of the sawn sample is parallel to the Y-axis sample centering auxiliary line; Step 3, sanding and metallographic polishing the fixed sample to obtain a pretreated sample; Step 4, rinsing the pretreated sample with alcohol and drying it; Step 5, fix the dried sample together with the sample fixing block on the XRD sample stage with plasticine, the X-axis centering notch coincides with the X-axis of the XRD sample stage, the Y-axis centering notch coincides with the Y-axis of the XRD sample stage, the rolling direction of the sample is parallel to the Y-axis of the XRD sample stage, and a level is placed on the sample for leveling again to obtain the installed sample; Step 6, turning on the X-ray diffractometer and the water cooler, and aging the X-ray diffractometer; Step 7, after the X-ray diffractometer aging is completed, the tube voltage and tube current are manually controlled to the test setting range; Step 8, calibrate the installed sample and the sample fixing block, open the automatic calibration program of the calibration instrument, and perform calibration; Step 9, after successful calibration, measure the physical phase, select the corresponding sample stage, set the test voltage, current, input measurement start angle, end angle, scanning mode, scanning speed and slit conditions; Step 10, after the physical phase measurement is completed, the texture measurement is performed, the texture sample stage is selected, and the test voltage, current, input measurement start angle, end angle, scanning mode, scanning speed and slit conditions are set; Step 11: After the texture measurement is completed, data processing is performed to obtain the pole figure PF of the material corresponding to the sample and the three-dimensional orientation diagram ODF of the polycrystalline material.

2. The method for measuring the texture of aluminum alloy can body sheet material by XRD according to claim 1, characterized in that: The size of the rectangular block is 15mm×15mm, the thickness is 0.259mm, and the thickness of the sample fixing block is 5mm.

3. The method for measuring the texture of aluminum alloy can body sheet material by XRD according to claim 1, characterized in that: During calibration, insert three copper absorbers into the calibration instrument; When measuring the physical phase and texture, remove the copper absorber and replace it with Kβ Absorbing film to obtain monochromatic X-rays.

4. The method for measuring the texture of aluminum alloy can body sheet material by XRD according to claim 1, characterized in that: The XRD sample stage is provided with vertically intersecting X-axis and Y-axis; The X-axis specimen centering auxiliary line and the Y-axis specimen centering auxiliary line intersect vertically and are located at the top of the sample fixture; The X-axis centering notch and the Y-axis centering notch are both line-shaped, and the two cross each other vertically and are arranged at the bottom of the sample fixing device.

5. The method for measuring the texture of aluminum alloy can body sheet material by XRD according to claim 1, characterized in that: Use sandpaper ranging from 1500# to 2000# for grinding.

6. The method for measuring the texture of aluminum alloy can body sheet material by XRD according to claim 1, characterized in that: Use a hair dryer to blow the pretreated specimen.

7. The method for measuring the texture of aluminum alloy can body sheet material by XRD according to claim 1, characterized in that: The voltage for aging of the X-ray diffractometer was 20KV and the current was 20mA; The test setting range of the control tube voltage and tube current is tube voltage range 20KV-50KV, and tube current range 2mA-60mA.

8. The method for measuring the texture of aluminum alloy can body sheet material by XRD according to claim 1, characterized in that: When measuring the physical phase, set the test voltage to 40KV, the current to 20mA, the input measurement starting angle to 5°-20°, the ending angle to 70-90°, the scanning speed to 2° / min -10° / min, and the incident slit to 2mm-10mm.

9. The method for measuring the texture of aluminum alloy can body sheet material by XRD according to claim 1, characterized in that: When measuring the physical phase, find the diffraction peak position of each test surface. The test surfaces are 111 crystal plane, 200 crystal plane and 220 crystal plane, and the corresponding angle ranges are 30-40°, 40-50°, and 60-70°, respectively. After determining the diffraction peak position of each test surface, directly input the corresponding diffraction peak angle in the subsequent texture parameter determination.

10. The method for measuring the texture of aluminum alloy can body sheet material by XRD according to claim 9, characterized in that: The corresponding angles of the 111, 200 and 220 crystal planes are 37.77°, 44.02° and 64.43° respectively.

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