Foil manufacturing process parameter screening method and system
Using X-ray diffraction technology to measure the characteristic pattern of metal foil, determine the range of grain size and diffraction peak area ratio, solve the problem of difficulty in measuring grain size during the rolling process of ultra-thin foil, and achieve rapid and accurate determination process parameters, improving efficiency and product quality.
Patent Information
- Application Number
- CN202411217333.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-02
- Publication Date
- 2025-01-24
- Estimated Expiration
- 2044-09-02
AI Technical Summary
In the prior art, during the rolling and production process of ultra-thin metal foils below 100 μm, metallographic observation of rolled metal foils is difficult, resulting in inaccurate measurement of grain size or inability to measure, which in turn affects the determination of process parameters and leads to Unstable product quality and waste of raw materials.
The X -ray diffraction technology measures the raw material and the characteristic map of the sample of the metal foil, and the judgment information and comparison information are generated to determine the scope of the grain size and the ratio of the diffraction peak area, and then record and store the corresponding process parameters.
It achieves the rapid and accurate determination of appropriate process parameters in the metal foil production process, reduces raw material waste, improves work efficiency, and reduces the complex operations of performance testing by providing reference standards for qualified products.
Smart Images

Figure CN118762784B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of metal foil manufacturing, and in particular to a process parameter screening method and system, electronic equipment, and computer-readable medium in a metal foil manufacturing process. Background Art
[0002] Organic light-emitting diodes generally use vacuum evaporation technology to prepare organic electroluminescent films. The key step is to deposit sub-pixel light-emitting points, heat the organic light-emitting material in a vacuum environment, sublimate it, and form pixels of corresponding shapes on the substrate through a fine metal mask (Fine Metal Mask, FMM) with special sub-pixel pattern through holes. The FMM is a consumable made of metal foil with a thickness of less than 100μm. Commonly used metals include nickel alloys and stainless steel. With the emergence of technologies such as AR (Augmented Reality) and VR (Virtual Reality), the requirements for screen resolution are gradually increasing. Higher resolution means smaller pixels, and the corresponding through-hole size on the FMM is smaller. As for the etching method that is currently the most widely used to prepare FMM, the thickness of the raw material metal foil is required to be thinner (<25μm). The quality of FMM determines the quality of the sub-pixels of the micron-level screen, which ultimately affects the screen imaging effect of the organic light-emitting diode. Therefore, very stringent requirements are put forward for the foil rolling technology for FMM.
[0003] In the prior art, it is difficult to observe the metallographic structure of the rolled metal foil during the rolling process of ultra-thin foils below 100 μm, resulting in inaccurate or impossible grain size measurement. Therefore, in order to achieve better product quality during production, a large number of tests are generally required, and the most appropriate process parameters are determined by comparing the performance of the rolled foil. This will cause a large amount of raw material waste, and the performance detection is relatively cumbersome, which will greatly affect the efficiency. Summary of the invention
[0004] The present invention aims to solve one of the technical problems in the related art to a certain extent. To this end, the present invention provides a foil manufacturing process parameter screening method and system, electronic equipment, and computer-readable medium, which can quickly and accurately determine the appropriate process parameters in the metal foil production process, save raw materials, and improve work efficiency.
[0005] A first aspect of the present invention discloses a method for screening process parameters of foil manufacturing, comprising: obtaining a first characteristic spectrum of a metal foil raw material, and generating determination information according to the first characteristic spectrum, wherein the first characteristic spectrum is measured by an X-ray diffraction measurement module, and the determination information includes a first range obtained by multiplying the diffraction peak area ratio of each crystal plane of the first characteristic spectrum by a first amplitude coefficient, and a second range obtained by multiplying the average grain size of multiple crystal planes by a second amplitude coefficient;
[0006] Obtaining a second characteristic spectrum of the forged test sample, and generating comparative information according to the second characteristic spectrum, wherein the forged test sample is forged using the forging process parameters in the database, the second characteristic spectrum is measured by an X-ray diffraction measurement module, and the comparative information includes actual diffraction peak area ratios of each crystal plane of the second characteristic spectrum, and actual average grain sizes of multiple crystal planes;
[0007] Compare the actual diffraction peak area ratio with the first range and the actual average grain size range with the second range;
[0008] When the actual diffraction peak area ratio falls within the first range and the actual average grain size falls within the second range, the corresponding forging process parameters are recorded and stored as qualified forging process parameters.
[0009] In the present technical solution, X-ray diffraction is used to measure the foil raw material and the test sample of the same material, and the first range and the second range can be obtained according to the measured first characteristic spectrum, and the actual diffraction peak area and the average grain size corresponding to the measured second characteristic spectrum and the first range and the second range are compared. As long as the actual diffraction peak area and the average grain size satisfy both the first range and the second range, it can be determined that the process parameters corresponding to the test sample are qualified process parameters. It can be seen that the grain size of smaller foils can be accurately measured by using X-ray diffraction technology. By obtaining the first range and the second range, it is equivalent to providing a reference standard for qualified products. In actual operation, it is only necessary to measure the test samples that meet the first range and the second range by X-ray diffraction technology to quickly determine the qualified process parameters, which reduces the complex operation of performance testing of the test samples and improves efficiency.
[0010] Furthermore, the first amplitude coefficient includes a first lower limit coefficient and a first upper limit coefficient, and the second amplitude coefficient includes a second lower limit coefficient and a second upper limit coefficient.
[0011] Furthermore, the method also includes screening parameters of the heat treatment process, including the following steps:
[0012] Obtaining theoretical mechanical properties of the first raw material after heat treatment, and obtaining a first heat treatment performance value according to the theoretical mechanical properties, wherein the theoretical mechanical properties are obtained from a database;
[0013] Acquire actual mechanical properties of the heat-treated test sample, and obtain a second heat-treatment performance value according to the actual mechanical properties, wherein the heat-treated test sample is heat-treated using heat-treatment process parameters in a database;
[0014] comparing the first heat treatment performance value and the second heat treatment performance value;
[0015] In the case where the deviation between the first heat treatment performance value and the second heat treatment performance value is less than the heat treatment deviation coefficient, the corresponding heat treatment process parameters are recorded and stored as qualified heat treatment process parameters.
[0016] Furthermore, the heat treatment process includes secondary heat treatment after cold rolling and tertiary heat treatment after precision rolling. The theoretical mechanical properties are obtained and written into the database according to the formula: x=x0-k*ΔD, wherein x represents the performance parameters of the plate after heat treatment; x0 represents the performance parameters of the plate before heat treatment after cold rolling; k represents the empirical coefficient at different temperatures, wherein the k value ranges from 0 to 10; ΔD represents the difference in the average grain size of the raw material before and after heat treatment, and the ΔD is obtained by measuring the average grain size of the raw material before and after heat treatment through an X-ray diffraction measurement module and calculating the difference, and the mechanical properties include yield strength, tensile strength and hardness.
[0017] Furthermore, it also includes parameter screening of stress relief heat treatment process, including:
[0018] Obtaining a third characteristic spectrum of the second raw material and a mechanical property value before stress relief heat treatment, and obtaining a grain size before stress relief heat treatment according to the third characteristic spectrum; wherein the third characteristic spectrum is measured by an X-ray diffraction measurement module, and the blank;
[0019] Obtaining the grain size after stress relief heat treatment and the mechanical property value after stress relief heat treatment of the stress relief heat treatment test sample, wherein the grain size before stress relief heat treatment is measured by an X-ray diffraction measurement module, and the stress relief heat treatment test sample is obtained by stress relief using stress relief heat treatment process parameters in the database;
[0020] Obtain the stress relief heat treatment deviation coefficient;
[0021] Comparing the grain size before and after the stress relief heat treatment and the mechanical property value before and after the stress relief heat treatment;
[0022] When the deviation of the grain size after stress relief heat treatment and the grain size before stress relief heat treatment, and the deviation of the mechanical property value before stress relief heat treatment and the mechanical property value after stress relief heat treatment both meet the stress relief heat treatment deviation coefficient, the corresponding stress relief heat treatment process parameters are recorded and stored as qualified stress relief heat treatment process parameters.
[0023] Furthermore, the stress relief heat treatment deviation coefficient includes a first deviation for judging the grain size deviation, the first deviation is ±6nm, and the deviation between the grain size after the stress relief heat treatment and the grain size before the stress relief heat treatment satisfies the stress relief heat treatment deviation coefficient, which means that the deviation falls within the range of the first deviation.
[0024] Furthermore, the stress relief heat treatment deviation coefficient includes a second deviation for judging the deviation of the mechanical property value, and the second deviation is set to 5%. The deviation between the mechanical property value before the stress relief heat treatment and the mechanical property value after the stress relief heat treatment satisfies the stress relief heat treatment deviation coefficient, which means that the deviation between the mechanical property value before the stress relief heat treatment and the mechanical property value after the stress relief heat treatment is less than the second deviation.
[0025] The second aspect of the present invention discloses an electronic device, comprising: one or more processors; a memory on which one or more computer programs are stored, and when the one or more computer programs are executed by the one or more processors, the one or more processors implement the process parameter screening method described in the first aspect.
[0026] A third aspect of the present invention discloses a computer-readable medium having a computer program stored thereon, wherein the computer program, when executed by a processor, implements the process parameter screening method described in the first aspect.
[0027] The fourth aspect of the present invention discloses a process parameter screening system, comprising an X-ray diffraction measurement module and a mechanical property detection module, and also comprising the electronic device of the second aspect, wherein the electronic device is communicatively connected with the X-ray diffraction measurement module and the mechanical property detection module, the mechanical property detection module is used to detect the mechanical properties of the test sample, and the X-ray diffraction measurement module is used to measure the characteristic spectrum of the material.
[0028] These features and advantages of the present invention will be disclosed in detail in the following specific embodiments and drawings. The best embodiments or means of the present invention will be described in detail in conjunction with the drawings, but they are not intended to limit the technical solutions of the present invention. In addition, there are multiple features, elements, and components that appear in each of the following texts and drawings, and different symbols or numbers are marked for convenience, but they all represent components with the same or similar structures or functions. BRIEF DESCRIPTION OF THE DRAWINGS
[0029] The present invention will be further described below in conjunction with the accompanying drawings:
[0030] Figure 1 This is a flow chart of forging process parameter screening of one embodiment of the present invention;
[0031] Figure 2 This is a flow chart of heat treatment process parameter screening of one embodiment of the present invention;
[0032] Figure 3 A stress relief heat treatment process screening flow chart of one embodiment of the present invention;
[0033] Figure 4 A metal foil processing flow chart of one embodiment of the present invention;
[0034] Figure 5 An example of an Invar XRD diffraction pattern of one embodiment of the present invention and an Invar standard pdf comparison card diagram;
[0035] Figure 6 This is a metallographic structure diagram of a foil cross section of one embodiment of the present invention;
[0036] Figure 7 This is an example diagram of the metallographic structure of regular grains according to one embodiment of the present invention;
[0037] Figure 8 A flowchart of an implementation of the electronic device provided by the present invention;
[0038] Fig. 9 The present invention provides a flowchart of an implementation of a computer-readable medium.
[0039] In the figure, 101 is a processor; 102 is a memory; 103 is an I / O interface; and 104 is a bus. DETAILED DESCRIPTION
[0040] Embodiments of the present invention are described in detail below, examples of which are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements with the same or similar functions. The embodiments in the implementation manner are intended to be used to explain the present invention and should not be construed as limiting the present invention.
[0041] References in this specification to "one embodiment" or "an example" or "an example" mean that a particular feature, structure, or characteristic described in conjunction with the embodiment itself may be included in at least one embodiment of the present patent disclosure. The appearance of the phrase "in one embodiment" in various places in the specification does not necessarily refer to the same embodiment.
[0042] The production process of metal foil generally includes smelting, forging, rolling, heat treatment and other main steps, and finally obtains the finished product with target quality and thickness. The specific process flow chart is shown in Figure 4 .
[0043] In addition to squeezing the grains into flat strips, the rolling deformation of metal foil can also refine the substructure inside the grains. A grain is composed of many cells with different orientations. In addition, plastic deformation causes the grains to fragment and the dislocations to multiply, eventually leading to the accumulation of dislocations between grain boundaries and subgrain boundaries. The dislocation density increases rapidly, the metal's ability to resist deformation and damage by external forces increases, and the mechanical properties of the foil also improve. Therefore, a smaller grain size is beneficial to metal foil. However, in addition to converting most of the work done by external forces into heat energy during the rolling process, the remaining small part remains inside the metal, forming residual internal stress, which will cause the foil to deform macroscopically, uneven in shape, and even prone to micro cracks that lead to foil breakage. Therefore, we must heat treat the metal foil to restore the metal structure. This process hardly changes the metal's microstructure. On the premise of ensuring the excellent mechanical properties obtained after work hardening, the internal stress is eliminated to improve the quality of the metal foil. However, the large deformation of metal foil leads to high storage energy, which makes it more likely to undergo recrystallization during heat treatment. The deformed grains will change shape and recrystallize and grow. Overly large grains will eventually lead to a sharp decrease in the mechanical properties of the foil.
[0044] It can be seen that the organizational state of the material has a key influence on the performance of the material. The most commonly used characteristic of the organizational state is the grain size, which directly determines the main performance indicators of the material such as strength and hardness. Therefore, we can control the grain size of each process in the foil production process to adjust the process parameters to obtain materials with qualified performance.
[0045] The usual grain size can be obtained by metallographic observation using image processing software, because the grain morphology of most metal materials is relatively regular and clear grain boundaries are very beneficial to the definition of grain size, such as Figure 7 However, the thickness of the metal foil used in FMM is thin, and the rolling deformation is extremely large. The corresponding grains are stretched and deformed in the rolling direction and the perpendicular rolling direction, and are flattened in the thickness direction. The final shape is as follows Figure 6 The metallographic structure of the foil cross section is shown. The grain boundaries between the grains with such a large deformation can no longer be distinguished by metallographic microscope observation, so the usual method of measuring grain size cannot be used.
[0046] Based on this, see Appendix Figure 1 ,We propose a method for screening foil manufacturing process parameters, including:
[0047] In step S110, a first characteristic spectrum of the metal foil raw material is obtained, and judgment information is generated according to the first characteristic spectrum, wherein the first characteristic spectrum is measured by an X-ray Powder diffractometer (XRD) measurement module, and the judgment information includes a first range obtained by multiplying a diffraction peak area ratio of each crystal plane of the first characteristic spectrum by a first amplitude coefficient, and a second range obtained by multiplying an average grain size of multiple crystal planes by a second amplitude coefficient;
[0048] In step S120, a second characteristic spectrum of the forged test sample is obtained, and comparison information is generated according to the second characteristic spectrum, wherein the forged test sample is forged using the forging process parameters in the database, the second characteristic spectrum is measured by an X-ray diffraction measurement module, and the comparison information includes actual diffraction peak area ratios of each crystal plane of the second characteristic spectrum, and actual average grain sizes of multiple crystal planes;
[0049] In step S130, the actual diffraction peak area ratio is compared with the first range and the actual average grain size range is compared with the second range;
[0050] When the actual diffraction peak area ratio falls within the first range and the actual average grain size falls within the second range, the corresponding forging process parameters are recorded and stored as qualified forging process parameters.
[0051] In the present technical solution, X-ray diffraction is used to measure the foil raw material and the test sample of the same material, and the first range and the second range can be obtained according to the measured first characteristic spectrum, and the actual diffraction peak area and the average grain size corresponding to the measured second characteristic spectrum and the first range and the second range are compared. As long as the actual diffraction peak area and the average grain size satisfy both the first range and the second range, it can be determined that the process parameters corresponding to the test sample are qualified process parameters. It can be seen that the grain size of smaller foils can be accurately measured by using X-ray diffraction technology. By obtaining the first range and the second range, it is equivalent to providing a reference standard for qualified products. In actual operation, it is only necessary to measure the test samples that meet the first range and the second range by X-ray diffraction technology to quickly determine the qualified process parameters, which reduces the complex operation of performance testing of the test samples and improves efficiency.
[0052] Since in actual use, the actual diffraction peak area ratio and the actual average grain size of the test sample are difficult to be a fixed value, and the actual diffraction peak area ratio and the actual average grain size that make the performance of the material stable are a range value, it is only necessary to keep the actual diffraction peak area ratio and the actual average grain size within a certain range to ensure the stability of the performance of the material, and the range is an empirical value. In actual use, the present invention can determine the first amplitude coefficient and the second amplitude coefficient based on experience, and the first amplitude coefficient includes a first lower limit coefficient and a first upper limit coefficient, and the second amplitude coefficient includes a second lower limit coefficient and a second upper limit coefficient. In actual application, the first amplitude coefficient and the second amplitude coefficient can be written into the processor respectively, and the processor obtains the first range and the second range according to the peak area ratio and the average grain size of each crystal plane of the first characteristic spectrum obtained, and the product of the first amplitude coefficient and the second amplitude coefficient. It should be noted that the first amplitude coefficient can be set to be different for each different crystal plane. For example, the characteristic spectrum of Invar alloy has five diffraction peaks, and the diffraction peak of each crystal plane is multiplied by the first amplitude coefficient to obtain the corresponding range. For example: multiply the diffraction peak area percentage of crystal plane (111) by 1±A% to obtain the diffraction peak area percentage range of crystal plane (111); multiply the diffraction peak area percentage of crystal plane (200) by 1±B% to obtain the diffraction peak area percentage range of crystal plane (200), etc. Of course, it should be noted that the first lower limit coefficient and the first upper limit coefficient of each crystal plane may also be different. For example, the diffraction peak area percentage of crystal plane (220) can be obtained by multiplying the product of (1-C% and 1+D%, where C≠D) to obtain the diffraction peak area percentage range of crystal plane (220).
[0053] Of course, it should be noted that if the actual diffraction peak area ratio does not meet the first range and / or the actual average grain size does not meet the second range, then another set of forging process parameters is selected from the database again and steps S110, S120, and S130 are repeated until qualified forging process parameters are obtained. It should be noted that the forging process parameters in the database can be parameters obtained based on historical experience or process parameters with similar material properties written into the database, that is, multiple sets of different forging process parameters are stored in the database.
[0054] In addition, it should be noted that the forging process parameters include but are not limited to the forging temperature, and the forging temperature is divided into the initial forging temperature and the final forging temperature. The selection of the forging process parameters of the present invention is further described below through specific examples:
[0055] The following uses Invar alloy as an example to explain the screening method and process of forging process parameters;
[0056] See attached Figure 5First, the characteristic spectrum of Invar alloy is measured by X-ray diffraction, combined with the standard PDF reference card of Invar alloy and the XRD judgment conditions of Invar alloy are obtained according to the first amplitude coefficient and the second amplitude coefficient, as shown in the following table:
[0057]
[0058] It can be seen that each crystal plane index corresponds to a diffraction peak area ratio range and an average grain size range. The area ratio of each diffraction peak of the forging blank XRD after forging falls within the above range, and the average grain size meets the judgment information, which means that the forging blank obtained by the forging process is qualified.
[0059] Embodiment 1:
[0060] The metal raw materials were melted and refined according to the weight percentage of 34~38% Ni, the total content of <5% trace elements Si, Mn, Cr, Mo, and the balance of Fe to obtain Invar ingots. The ingots were forged to obtain forgings with a thickness of 2cm, and two forging conditions were selected: Condition 1, the initial forging temperature was 1050~1100℃, and the final forging temperature was 900~950℃; Condition 2, the initial forging temperature was 1175~1200℃, and the final forging temperature was 870~925℃. XRD tests were performed on the head and tail of the ingots, as well as the forgings obtained under two different conditions, and the data obtained are shown in Table 1:
[0061]
[0062] It can be seen from Table 1 that the XRD composition of the head and tail of the ingot in Example 1 is significantly different and deviates greatly from the standard, indicating that its organizational uniformity is extremely poor. After forging, the XRD composition of the billet is close to the standard. However, the main difference between Condition 2 and Condition 1 is that the initial forging temperature of Condition 2 is higher and the final forging temperature is lower, the forging process is more complete, and the billet organization is judged OK. Therefore, the forging process parameters of Condition 2 are more appropriate here, and the initial forging temperature of 1175~1200℃ and the final forging temperature of 870~925℃ are selected as qualified forging process parameters.
[0063] During the forging process, the head and tail of the forging blank generally have very poor structural uniformity compared to the middle part. If the head and tail of the forging blank meet the reference standard, then the forging blank can be considered to meet the marking. Therefore, the test sample selection in step S12 should at least include the head sample and tail sample of the raw material after forging, and of course, the middle sample can also be included. In order to ensure accuracy, multiple samples can be selected in each part for testing. When all samples meet the reference standard, it can be considered that the forging process parameters of the test sample are qualified forging process parameters. At this time, the qualified forging process parameters will be recorded and stored.
[0064] One embodiment of the present invention further includes screening parameters of the heat treatment process, see the attached Figure 2 ,include:
[0065] S210, obtaining theoretical mechanical properties of a first raw material (in this embodiment, the raw material before heat treatment in this process needs to be processed, and the raw material has been processed in the process of metal foil before heat treatment) after heat treatment, and obtaining a first heat treatment performance value according to the theoretical mechanical properties, wherein the theoretical mechanical properties are obtained from a database;
[0066] S220, obtaining actual mechanical properties of the heat-treated test sample, and obtaining a second heat-treatment performance value according to the actual mechanical properties, wherein the heat-treated test sample is heat-treated using heat-treatment process parameters in a database;
[0067] S230, comparing the first heat treatment performance value and the second heat treatment performance value;
[0068] S240, when the deviation between the first heat treatment performance value and the second heat treatment performance value is less than the heat treatment deviation coefficient, record and store the corresponding heat treatment process parameters as qualified heat treatment process parameters.
[0069] It should be noted that the heat treatment process parameters in the database may be parameters obtained based on historical experience, or process parameters of similar material properties may be written into the database, that is, multiple sets of different heat treatment process parameters are stored in the database.
[0070] In addition, the above-mentioned heat treatment process includes secondary heat treatment after cold rolling and tertiary heat treatment after precision rolling. The theoretical mechanical properties are obtained and written into the database according to the formula: x=x0-k*ΔD, wherein x represents the performance parameters of the plate after heat treatment; x0 represents the performance parameters of the plate before heat treatment after cold rolling; k represents the empirical coefficient at different temperatures, wherein the k value ranges from 0 to 10; ΔD represents the difference in the average grain size of the raw material before and after heat treatment, and the ΔD is obtained by measuring the average grain size of the raw material before and after heat treatment through an X-ray diffraction measurement module and calculating the difference, and the mechanical properties include yield strength, tensile strength and hardness.
[0071] The following is a detailed description of the screening of heat treatment process parameters through specific examples:
[0072] Example 2: Cold rolling to obtain 300μm thick Invar sheet, subject it to secondary heat treatment, requiring the yield strength drop of this pass to be ≤20%, the tensile strength drop to be ≤25%, and the hardness drop to be ≤25%. Heat treatment condition 1: 780℃, treatment for 3.5min, yield strength temperature empirical coefficient k is 1.5MPa / nm, tensile strength temperature empirical coefficient k is 3.1MPa / nm, and hardness temperature empirical coefficient k is 1.4 / nm; condition 2: 690℃, treatment for 2.2min, yield strength temperature empirical coefficient k is 1.2MPa / nm, tensile strength temperature empirical coefficient k is 2.7MPa / nm, and hardness temperature empirical coefficient k is 1.1 / nm. The yield strength, tensile strength and hardness of the 300μm cold-rolled sheet before heat treatment were measured, and the results were calculated according to the empirical formula as shown in Table 2 below:
[0073]
[0074] Comparing the actual measured values with the calculated values, it can be seen from the results that after heat treatment, the grain size of the plate increases significantly, and the mechanical properties also weaken. The heat treatment temperature of condition 1 is higher, the grain size is larger, and the mechanical properties decrease more significantly. After heat treatment under condition 2, the mechanical properties of the tile plate are qualified. Comparing the calculated values with the actual measured values, it can be seen that the consistency between the two is good, and the setting of the empirical coefficient makes the calculated value slightly lower than the actual measured value, which can better ensure the safety of material use. Condition 2 is selected as the qualified secondary heat treatment process parameters.
[0075] Embodiment three:
[0076] The 100μm thick Invar sheet was obtained by precision rolling and subjected to three heat treatments, requiring that the yield strength, tensile strength and hardness reduction of each pass were ≤50%. Heat treatment condition 1: 700℃, speed 20m / min, a certain proportion of hydrogen and nitrogen mixed atmosphere protection, yield strength temperature empirical coefficient k is 2.7 MPa / nm, tensile strength temperature empirical coefficient k is 3.1MPa / nm, hardness temperature empirical coefficient k is 1.2 / nm; condition 2: 700℃, speed 60m / min, a certain proportion of hydrogen and nitrogen mixed atmosphere protection, each temperature empirical coefficient k is the same as condition 1. The yield strength, tensile strength and hardness of the 100μm cold-rolled sheet before heat treatment were measured, and the results were calculated according to the empirical formula as shown in Table 3:
[0077]
[0078] Comparing the actual measured values with the calculated values, it can be seen from the results that after heat treatment, the grain size of the plate increases significantly, and the mechanical properties also weaken. The difference between condition 1 and condition 2 lies in the different heat treatment speeds. The grain sizes of the two are almost the same, and their mechanical properties are almost the same, indicating that at this temperature, the heat treatment speed can be increased to increase production capacity, or the heat treatment temperature can be reduced to reduce energy consumption. Comparing the calculated values with the actual measured values, it can be seen that the consistency between the two is good, and the setting of the empirical coefficient makes the calculated value slightly lower than the actual measured value, which can better ensure the safety of the material. Screening conditions 1 and 2 are qualified heat treatment process parameters for three heat treatments after qualified precision rolling.
[0079] See attached Figure 3 One embodiment of the present invention further includes screening parameters of the stress relief heat treatment process, including:
[0080] S310, obtaining a third characteristic spectrum of the second raw material (in this embodiment, the raw material before the stress relief heat treatment is required in this process, and the raw material has been processed in the process of the metal foil before the stress relief heat treatment) and a mechanical property value before the stress relief heat treatment, and obtaining a grain size before the stress relief heat treatment according to the third characteristic spectrum; wherein the third characteristic spectrum is obtained by measuring by an X-ray diffraction measurement module;
[0081] S320, obtaining the grain size of the stress relief heat treatment test sample after the stress relief heat treatment and the mechanical property value after the stress relief heat treatment, wherein the grain size before the stress relief heat treatment is measured by an X-ray diffraction measurement module, and the stress relief heat treatment test sample is obtained by stress relief using the stress relief heat treatment process parameters in the database;
[0082] S330, obtaining a stress relief heat treatment deviation coefficient;
[0083] S340, comparing the grain size before and after the stress relief heat treatment, and the mechanical property value before and after the stress relief heat treatment;
[0084] S350, when the deviation of the grain size after the stress relief heat treatment and the grain size before the stress relief heat treatment, and the deviation of the mechanical property value before the stress relief heat treatment and the mechanical property value after the stress relief heat treatment both satisfy the stress relief heat treatment deviation coefficient, record and store the corresponding stress relief heat treatment process parameters as qualified stress relief heat treatment process parameters.
[0085] It should be noted that the stress relief heat treatment process parameters in the database may be parameters obtained based on historical experience, or process parameters of similar material properties may be written into the database, that is, multiple sets of different stress relief heat treatment process parameters are stored in the database.
[0086] The stress relief heat treatment deviation coefficient of one embodiment of the present invention includes a first deviation for judging the grain size deviation, the first deviation is ±6nm, and the deviation between the grain size after the stress relief heat treatment and the grain size before the stress relief heat treatment satisfies the stress relief heat treatment deviation coefficient, which means that the deviation falls within the range of the first deviation.
[0087] The stress relief heat treatment deviation coefficient also includes a second deviation for judging the deviation of the mechanical property value, and the second deviation is set to 5%. The deviation between the mechanical property value before the stress relief heat treatment and the mechanical property value after the stress relief heat treatment satisfies the stress relief heat treatment deviation coefficient, which means that the deviation between the mechanical property value before the stress relief heat treatment and the mechanical property value after the stress relief heat treatment is less than the second deviation.
[0088] In the process of screening the process parameters of stress relief heat treatment, the present invention also uses X-ray diffraction to measure the grain size, and sets two judgment conditions: grain size deviation and mechanical property value deviation. In this way, by measuring the grain size and mechanical properties before and after the stress relief heat treatment, it is possible to determine whether the blank is qualified, which provides a reference standard, reduces the number of tests, and improves efficiency.
[0089] The following is a detailed description of the screening of stress relief heat treatment process parameters in conjunction with specific embodiments:
[0090] Embodiment 4:
[0091] The Invar sheet with a thickness of 40 μm was obtained by precision rolling and subjected to stress relief heat treatment. Condition 1: temperature 630°C, tension 20 kgf / mm2, speed 8 m / min, nitrogen atmosphere protection; Condition 2: temperature 400°C, tension 40 kgf / mm2, speed 2 m / min, nitrogen atmosphere protection. The grain size and mechanical properties of the Invar sheet with a thickness of 40 μm before stress relief heat treatment and after different stress relief heat treatment processes were measured as shown in Table 4:
[0092]
[0093] It can be seen from the above-mentioned Example 4 that the ultra-thin Invar sheet material has a large deformation amount and a very high storage energy. The change of heat treatment temperature can cause the grain size to increase rapidly, and the corresponding mechanical properties to deteriorate sharply. Therefore, in practice, whether the stress relief heat treatment process is suitable can be judged based on whether the change range of the grain size before and after the stress relief heat treatment is within the required range. In this embodiment, screening condition 2 is used as a suitable stress relief heat treatment process parameter.
[0094] A second aspect of the present invention discloses an electronic device, such as Figure 8As shown, it includes: one or more processors; a memory, on which one or more computer programs are stored. When the one or more computer programs are executed by the one or more processors, the one or more processors implement the process parameter screening method described in the first aspect.
[0095] The electronic device may further include one or more I / O interfaces 103 connected between the processor 101 and the memory 102 and configured to implement information interaction between the processor 101 and the memory 102 .
[0096] Among them, the processor 101 is a device with data processing capabilities, including but not limited to a central processing unit (CPU), etc.; the memory 102 is a device with data storage capabilities, including but not limited to random access memory (RAM, more specifically SDRAM, DDR, etc.), read-only memory (ROM), electrically erasable programmable read-only memory (EEPROM), flash memory (FLASH); the I / O interface (read-write interface) is connected between the processor and the memory, and can realize information exchange between the processor and the memory, including but not limited to a data bus (Bus), etc.
[0097] In some embodiments, the processor 101 , the memory 102 , and the I / O interface 103 are connected to each other via a bus 104 , and further connected to other components of the electronic device.
[0098] As a third aspect of the present invention, Fig. 9 As shown, a computer readable medium is provided, on which a computer program is stored, wherein when the computer program is executed by a processor, the above-mentioned process parameter screening method provided by the present invention is implemented.
[0099] The fourth aspect of the present invention discloses a process parameter screening system, comprising an X-ray diffraction measurement module and a mechanical property detection module, and also comprising the electronic device of the second aspect, wherein the electronic device is communicatively connected with the X-ray diffraction measurement module and the mechanical property detection module, the mechanical property detection module is used to detect the mechanical properties of the test sample, and the X-ray diffraction measurement module is used to measure the characteristic spectrum of the material.
[0100] When screening process parameters, the characteristic spectrum is measured by X-ray diffraction to obtain the grain size, and automatic comparison is performed, and then the process parameters that meet the conditions are stored and recorded to achieve the preservation of qualified process parameters.
[0101] Of course, when performing heat treatment process parameters, the electronic equipment can obtain the mechanical properties before and after the heat treatment, compare, store and record the process parameters that meet the conditions, and realize the screening of qualified heat treatment process parameters;
[0102] When screening stress relief heat treatment process parameters, the electronic device can obtain the grain size of the plate before and after stress relief heat treatment through the X-ray diffraction module. It can also obtain the mechanical properties before and after stress relief heat treatment and perform automatic comparison, and then store and record the stress relief heat treatment process parameters that meet the conditions.
[0103] The above are only specific embodiments of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that the present invention includes but is not limited to the contents described in the drawings and the above specific embodiments. Any modification that does not deviate from the functional and structural principles of the present invention will be included in the scope of the claims.
Claims
1. A method for screening process parameters of foil manufacturing, characterized in that: include: Obtaining a first characteristic spectrum of the metal foil raw material, and generating determination information according to the first characteristic spectrum, wherein the first characteristic spectrum is measured by an X-ray diffraction measurement module, and the determination information includes a first range obtained by multiplying a diffraction peak area ratio of each crystal plane of the first characteristic spectrum by a first amplitude coefficient, and a second range obtained by multiplying an average grain size of multiple crystal planes by a second amplitude coefficient; Obtaining a second characteristic spectrum of the forged test sample, and generating comparative information according to the second characteristic spectrum, wherein the forged test sample is forged using the forging process parameters in the database, the second characteristic spectrum is measured by an X-ray diffraction measurement module, and the comparative information includes actual diffraction peak area ratios of each crystal plane of the second characteristic spectrum, and actual average grain sizes of multiple crystal planes; Compare the actual diffraction peak area ratio with the first range and the actual average grain size range with the second range; When the actual diffraction peak area ratio falls within the first range and the actual average grain size falls within the second range, the corresponding forging process parameters are recorded and stored as qualified forging process parameters; Obtaining theoretical mechanical properties of a first raw material after heat treatment, and obtaining a first heat treatment performance value according to the theoretical mechanical properties, wherein the theoretical mechanical properties are obtained from a database, and the first raw material is a blank before heat treatment; Acquire actual mechanical properties of the heat-treated test sample, and obtain a second heat-treatment performance value according to the actual mechanical properties, wherein the heat-treated test sample is heat-treated using heat-treatment process parameters in a database; comparing the first heat treatment performance value and the second heat treatment performance value; When the deviation between the first heat treatment performance value and the second heat treatment performance value is less than the heat treatment deviation coefficient, recording and storing the corresponding heat treatment process parameters as qualified heat treatment process parameters; Obtaining a third characteristic spectrum of the second raw material and a mechanical property value before stress relief heat treatment, and obtaining a grain size before stress relief heat treatment according to the third characteristic spectrum; wherein the third characteristic spectrum is obtained by measuring with an X-ray diffraction measurement module, and the second raw material is a blank before stress relief heat treatment; Obtaining the grain size after stress relief heat treatment and the mechanical property value after stress relief heat treatment of the stress relief heat treatment test sample, wherein the grain size before stress relief heat treatment is measured by an X-ray diffraction measurement module, and the stress relief heat treatment test sample is obtained by stress relief using stress relief heat treatment process parameters in the database; Obtain the stress relief heat treatment deviation coefficient; Comparing the grain size before and after the stress relief heat treatment and the mechanical property value before and after the stress relief heat treatment; When the deviation of the grain size after stress relief heat treatment and the grain size before stress relief heat treatment, and the deviation of the mechanical property value before stress relief heat treatment and the mechanical property value after stress relief heat treatment both meet the stress relief heat treatment deviation coefficient, the corresponding stress relief heat treatment process parameters are recorded and stored as qualified stress relief heat treatment process parameters.
2. The process parameter screening method according to claim 1, characterized in that: The heat treatment process includes secondary heat treatment after cold rolling and tertiary heat treatment after precision rolling. The theoretical mechanical properties are obtained according to the formula: x=x0-k*ΔD and written into the database, wherein x represents the performance parameters of the plate after heat treatment; x0 represents the performance parameters of the plate before heat treatment after cold rolling; k represents the empirical coefficient at different temperatures, wherein the k value ranges from 0 to 10; ΔD represents the difference in the average grain size of the raw material before and after heat treatment, and the ΔD is obtained by measuring the average grain size of the raw material before and after heat treatment through an X-ray diffraction measurement module and calculating the difference, and the mechanical properties include yield strength, tensile strength and hardness.
3. The process parameter screening method according to claim 1, characterized in that: The stress relief heat treatment deviation coefficient includes a first deviation for determining the grain size deviation, the first deviation is ±6nm, and the deviation between the grain size after the stress relief heat treatment and the grain size before the stress relief heat treatment satisfies the stress relief heat treatment deviation coefficient, which means that the deviation falls within the range of the first deviation.
4. The process parameter screening method according to claim 1, characterized in that: The stress relief heat treatment deviation coefficient includes a second deviation for judging the deviation of the mechanical property value, and the second deviation is set to 5%. The deviation between the mechanical property value before the stress relief heat treatment and the mechanical property value after the stress relief heat treatment satisfies the stress relief heat treatment deviation coefficient, which means that the deviation between the mechanical property value before the stress relief heat treatment and the mechanical property value after the stress relief heat treatment is less than the second deviation.
5. The process parameter screening method according to claim 1, characterized in that: The first amplitude coefficient includes a first lower limit coefficient and a first upper limit coefficient, and the second amplitude coefficient includes a second lower limit coefficient and a second upper limit coefficient.
6. An electronic device, characterized in that: include: one or more processors; A memory having one or more computer programs stored thereon, which, when executed by the one or more computer programs, enable the one or more processors to implement the process parameter screening method according to any one of claims 1 to 5.
7. A computer readable medium having a computer program stored thereon, characterized in that: When the computer program is executed by a processor, the process parameter screening method according to any one of claims 1 to 5 is implemented.
8. A process parameter screening system, characterized in that: It includes an X-ray diffraction measurement module and a mechanical property detection module, and also includes the electronic device as claimed in claim 6, the electronic device is communicatively connected with the X-ray diffraction measurement module and the mechanical property detection module, the mechanical property detection module is used to detect the mechanical properties of the test sample, and the X-ray diffraction measurement module is used to measure the characteristic spectrum of the material.
Citation Information
Patent Citations
Method for non-destructively monitoring grain boundary relaxation strengthened nano-metal and method for determining process parameters
CN115326853A
Frictionless forged aluminum alloy sputtering target with improved properties
US20180223420A1