CN102426125B - Preparation method for baseband oblique section for EBSD test, and analysis method thereof - Google Patents
Preparation method for baseband oblique section for EBSD test, and analysis method thereof Download PDFInfo
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Abstract
一种EBSD测试用基带斜截面的制备方法及分析方法，属于高温超导涂层导体的基带领域。其步骤包括：(1)将制备好的冷轧基带剪切成合适的大小，进行机械抛光处理成斜截面；(2)将抛光好的基带进行清洗；(3)将清洗好的冷轧基带进行再结晶退火处理；(4)采用EBSD技术分析样品表面的晶粒取向；(5)对测试结果进行统计分析。该方法操作简单，可缩短样品制备过程，节约测试时间，同时获得所需要的全部测试信息。The invention discloses a preparation method and an analysis method of a baseband inclined section for EBSD testing, which belong to the field of basebands of high-temperature superconducting coated conductors. The steps include: (1) cutting the prepared cold-rolled base strip into a suitable size, and performing mechanical polishing to form an oblique section; (2) cleaning the polished base strip; (3) cleaning the cleaned cold-rolled base strip Carry out recrystallization annealing treatment; (4) adopt EBSD technology to analyze the grain orientation of the sample surface; (5) carry out statistical analysis to the test result. The method is simple to operate, can shorten the sample preparation process, save test time, and obtain all required test information at the same time.
Description
技术领域technical field
本发明属于高温超导涂层导体的基带领域，具体涉及一种EBSD测试用Ni-W合金基带斜截面的制备及分析方法。The invention belongs to the field of basebands of high-temperature superconducting coated conductors, in particular to a method for preparing and analyzing oblique sections of Ni-W alloy basebands for EBSD testing.
背景技术Background technique
近年来，各技术发达国家都将第二代涂层导体的实用化研究作为21世纪超导材料研究和发展的热点，并取得了一系列突破性的进展。作为涂层超导体多层结构中的重要组成部分合金金属基带起到了支撑、外延过渡层和超导薄膜层以及承载部分电流的重要作用，因此制备具有双轴织构的金属韧性基带是获得高性能涂层超导线材的关键因素之一。目前，Ni5at.%W是使用范围最广的金属基带之一，世界范围内已有多家公司和科研单位能够大规模（>100M）生产该种织构基带，但其应用于YBCO织构基底材料，依然在机械性能和磁性能上存在不足。各研究小组分别把研究的重点放在高钨含量Ni-W合金基带的制备上。2005年，休斯顿大学的Zhou X.Y.（Appl.Supercond，17(2007)3828-3431）采用纯度为99.99%的镍粉和钨粉，用120目的网筛选后，得到颗粒大小为5-6μm的镍粉和钨粉，随后进行了30min的高能球磨，最后进行烧结和轧制，退火再结晶后在Ni9.0at.%W中得到了超过90%（<15°）的强立方织构。2008年，德国Dresen IFW研究小组的J Eickemeyer（Supercond Sci.Technol，21(2008)105012）报道了他们在Ni7.5at.%W基带方面的研究结果，通过改变工艺，最终得到了92.5%的再结晶立方织构。2011年，德国Dresen IFW研究小组的,JEickemeyer（Supercond.Sci.Technol，23(2010)085012.）通过引入多次的中间回复退火处理，在Ni-9.0at.%W中得到了立方织构含量(<9.5°)高达96%的强立方织构。世界范围内的很多研究小组分别就熔炼工艺或者粉末冶金制备工艺、冷轧变形量、退火工艺（温度，时间，气氛）等关键环节的技术参数进行了广泛的研究与报道，在优化的工艺条件下可以得到成分均匀，取向单一，表面平整的立方织构金属基带，同时也对再结晶织构的形成过程进行了简单表征。In recent years, all technologically developed countries have regarded the practical research of second-generation coated conductors as a hot spot in the research and development of superconducting materials in the 21st century, and have made a series of breakthroughs. As an important part of the coated superconductor multilayer structure, the alloy metal base band plays an important role in the support, epitaxial transition layer and superconducting thin film layer, as well as carrying part of the current. One of the key factors for coating superconducting wires. At present, Ni5at.%W is one of the most widely used metal substrates. Many companies and scientific research institutes around the world have been able to produce this textured substrate on a large scale (>100M), but it is applied to YBCO textured substrates. However, there are still deficiencies in mechanical properties and magnetic properties. Each research group focused their research on the preparation of Ni-W alloy substrate with high tungsten content. In 2005, Zhou X.Y. (Appl.Supercond, 17(2007) 3828-3431) of the University of Houston used nickel powder and tungsten powder with a purity of 99.99%, and screened them with a 120 mesh screen to obtain nickel powder with a particle size of 5-6μm and tungsten powder, followed by high-energy ball milling for 30 minutes, and finally sintering and rolling. After annealing and recrystallization, a strong cubic texture of more than 90% (<15°) was obtained in Ni9.0at.%W. In 2008, J Eickemeyer (Supercond Sci.Technol, 21(2008) 105012) of the Dresen IFW research group in Germany reported their research results on the Ni7.5at.%W baseband. By changing the process, they finally obtained a 92.5% regeneration Crystalline cubic texture. In 2011, JEickemeyer (Supercond.Sci.Technol, 23(2010)085012.) of the Dresen IFW research group in Germany obtained the cubic texture content in Ni-9.0at.%W by introducing multiple intermediate recovery annealing treatments. (<9.5°) Up to 96% strong cubic texture. Many research groups around the world have conducted extensive research and reports on the technical parameters of key links such as smelting process or powder metallurgy preparation process, cold rolling deformation, and annealing process (temperature, time, atmosphere). A cubic textured metal substrate with uniform composition, single orientation, and flat surface can be obtained under the following conditions, and the formation process of the recrystallized texture is also simply characterized.
传统的制样方法与分析方法要求分别制备基带表面与基带截面的样品并进行EBSD信息采集，然后进行统计对比分析得到完整的样品信息。但是由于EBSD测试技术属于微观测试领域，是一种微观表征手段，对样品表面的粗糙度反应非常灵敏，其测试范围也有一定的局限性，那么对于不同制备方法获得的表面样品与截面样品的测试信息就存在很大的误差，进而对结果分析造成一定的影响，并且操作步骤复杂。Traditional sample preparation and analysis methods require the preparation of baseband surface and baseband cross-section samples respectively and the collection of EBSD information, and then statistical comparative analysis to obtain complete sample information. However, since EBSD testing technology belongs to the field of microscopic testing, it is a microscopic characterization method, which is very sensitive to the roughness of the sample surface, and its testing range is also limited. There is a large error in the information, which will have a certain impact on the result analysis, and the operation steps are complicated.
发明内容Contents of the invention
为了解决表面样品与截面样品在制样上的差异性，本发明提出一种全新的制备思路，那就是制备一种斜截面，使其在测试时可以同时采集样品表面与截面的信息。本发明主要公开了一种EBSD测试用基带斜截面的制备方法及分析方法，可用来同时一步分析或表征基带表面与截面的再结晶织构转变，并分析基带表面的形变织构对再结晶织构演变的影响。该方法操作简单，可缩短样品制备过程，节约测试时间，但是可以获得测试及结果分析所需要的全部信息。In order to solve the difference in sample preparation between surface samples and cross-section samples, the present invention proposes a brand-new preparation idea, that is, to prepare an oblique cross-section so that the information of the surface and cross-section of the sample can be collected simultaneously during testing. The invention mainly discloses a preparation method and an analysis method of a baseband oblique section for EBSD testing, which can be used to simultaneously analyze or characterize the recrystallization texture transformation of the baseband surface and the section, and analyze the effect of the deformation texture of the baseband surface on the recrystallization texture. impact on structural evolution. The method is simple to operate, can shorten the sample preparation process and save test time, but can obtain all the information required for the test and result analysis.
本发明主要公开了一种EBSD测试用基带斜截面的制备及分析方法，可用来同时分析基带表面与截面的再结晶织构转变，并分析基带表面的形变织构对再结晶织构演变的影响，包括以下步骤：The invention mainly discloses a method for preparing and analyzing the oblique section of the baseband for EBSD testing, which can be used to simultaneously analyze the transition of the recrystallization texture of the baseband surface and the section, and analyze the influence of the deformation texture of the baseband surface on the evolution of the recrystallization texture , including the following steps:
1)将平均厚度为60～100um的冷轧合金基带按照测试需要进行剪切，然后进行机械抛光处理成斜截面，其关键在于冷轧基带需用胶水固定在具有坡度的磨具上，以便进行抛光。在进行抛光过程中，对合金基带均匀施压，从而获得具有斜截面的合金基带，其中一部分区域抛光严重，将基带表层30um～50um的表层除去，达到基带的芯层位置，使该区域的再结晶织构形成不受外层形变织构的影响，另一部分区域抛光较浅，即保留了部分的基带表层；1) Cut the cold-rolled alloy base strip with an average thickness of 60-100um according to the test requirements, and then perform mechanical polishing to form an oblique section. polishing. During the polishing process, uniform pressure is applied to the alloy base strip to obtain an alloy base strip with an oblique cross-section. Part of the area is severely polished, and the surface layer of 30um to 50um on the surface of the baseband is removed to reach the core layer of the baseband. The formation of crystalline texture is not affected by the deformation texture of the outer layer, and the other part of the area is polished shallower, that is, part of the surface layer of the baseband is retained;
2)把抛光好的基带进行清洗：把抛光好的基带放入到丙酮溶液中进行去污清洗，然后放入到无水乙醇溶液中进行二次清洗，最后在蒸馏水中进行超声去离子清洗，烘干保存；2) Clean the polished baseband: put the polished baseband into acetone solution for decontamination cleaning, then put it into anhydrous ethanol solution for secondary cleaning, and finally perform ultrasonic deionization cleaning in distilled water, dry storage;
3)在Ar/H2混合气体保护下，将清洗好的冷轧基带进行常规的再结晶退火处理，得到双轴立方织构金属基带；采用EBSD技术分析斜截面样品表面的晶粒取向；3) Under the protection of Ar/H 2 mixed gas, the cleaned cold-rolled base strip is subjected to conventional recrystallization annealing treatment to obtain a biaxial cubic textured metal base strip; the grain orientation on the surface of the oblique section sample is analyzed by EBSD technology;
4)对上述测试结果进行分析，可分析表面形变织构对再结晶织构演变的影响。4) By analyzing the above test results, the influence of surface deformation texture on the evolution of recrystallization texture can be analyzed.
步骤3）为了分析不同阶段立方织构的形成、长大过程，可对基带进行不同温度的再结晶处理（退火处理），例如为了研究表面形变织构对芯层立方织构形核的影响，可对其采取初始再结晶处理。Step 3) In order to analyze the formation and growth process of cubic texture in different stages, the baseband can be recrystallized (annealed) at different temperatures, for example, to study the influence of surface deformation texture on the nucleation of cubic texture in the core layer, It can be treated with initial recrystallization.
该方法操作简单，可缩短样品制备过程，节约测试时间，同时获得所需要的全部测试信息。该发明可同时分析基带表面与截面的再结晶织构转变，并分析基带表面的形变织构对再结晶织构演变的影响。The method is simple to operate, can shorten the sample preparation process, save test time, and obtain all required test information at the same time. The invention can simultaneously analyze the transition of the recrystallization texture on the surface of the base tape and the section, and analyze the influence of the deformation texture on the surface of the base tape on the evolution of the recrystallization texture.
附图说明Description of drawings
图1已制备好的斜截面样品的示意图；The schematic diagram of the prepared oblique section sample of Fig. 1;
图2实施例1退火后的Ni7W斜截面样品表面的EBSD取向图；The EBSD orientation diagram of the Ni7W oblique section sample surface after the annealing of Fig. 2 embodiment 1;
图3实施例1退火后的Ni7W斜截面样品表面非立方织构的ODF截面图（
图4初始再结晶Ni7W样品截面芯层非立方织构的ODF截面图（
具体实施方式Detailed ways
下面结合具体的实施例对本发明做进一步说明，但本发明不用限于以下实施例。分析不同阶段立方织构的形成、长大过程，可对基带进行不同温度的再结晶处理（退火处理），例如为了研究表面形变织构对芯层立方织构形核的影响，可对其采取初始再结晶处理。The present invention will be further described below in conjunction with specific examples, but the present invention is not limited to the following examples. To analyze the formation and growth process of cubic texture at different stages, recrystallization treatment (annealing treatment) at different temperatures can be carried out on the baseband. Initial recrystallization treatment.
实施例1Example 1
将总形变量＞99%，平均厚度为72um的冷轧Ni7at.%W合金基带剪切成5mm*10mm大小的样品，用胶水固定在表面平整、光洁的具有一定坡度的镁合金磨具上，均匀施压至粘结牢固，以便进行抛光。在进行抛光过程中，对合金基带均匀施压，从而获得斜截面的合金基带，其中一部分区域抛光严重，即将基带表层约30um左右的表层除去，达到了基带的芯层位置，使该区域的再结晶织构形成不受外层形变织构的影响，高温退火后该区域表现为合金基带芯层的再结晶织构；另一部分区域抛光较浅，即保留了部分的基带表层，再结晶退火后该区域的再结晶织构与未经抛光的表层织构相类似。已制备好的斜截面样品如图1所示。把抛光好的基带放入到丙酮溶液中进行去污清洗，清洗时间为5min，然后放入到无水乙醇溶液中进行二次清洗，清洗时间为5min，最后在蒸馏水中进行超声去离子清洗，清洗时间为3min，烘干保存待用；对清洗好的冷轧Ni7at.%W合金基带进行再结晶退火处理，处理温度为1450℃，保温1h，整个再结晶处理过程在Ar/H2混合气体保护下进行以防止样品被氧化。Cut the cold-rolled Ni7at.%W alloy base strip with a total deformation of >99% and an average thickness of 72um into a sample with a size of 5mm*10mm, and fix it with glue on a magnesium alloy abrasive tool with a smooth surface and a certain slope. Apply even pressure until the bond is firm for polishing. During the polishing process, uniform pressure is applied to the alloy base strip to obtain an alloy base strip with an oblique cross-section. Part of the area is severely polished, that is, the surface layer of about 30um on the surface of the base strip is removed to reach the core layer of the base strip. The formation of crystal texture is not affected by the deformation texture of the outer layer. After high temperature annealing, this area shows the recrystallization texture of the core layer of the alloy baseband; the other part of the area is polished lightly, that is, part of the baseband surface is retained. After recrystallization annealing The recrystallized texture in this region is similar to that of the unpolished surface. The prepared oblique section samples are shown in Fig. 1. Put the polished baseband into the acetone solution for decontamination and cleaning, the cleaning time is 5 minutes, then put it into the absolute ethanol solution for the second cleaning, the cleaning time is 5 minutes, and finally perform ultrasonic deionization cleaning in distilled water, The cleaning time is 3 minutes, dried and stored for later use; the cleaned cold-rolled Ni7at.%W alloy base strip is subjected to recrystallization annealing treatment at a temperature of 1450°C and kept for 1 hour. Protected to prevent the sample from being oxidized.
用配备EBSD附件的扫描电镜系统（SEM：JEOL JSM-6500F）对再结晶处理过的Ni7at.%W合金基带样品进行测试，扫面范围为500um*700um，扫面步长为1um，用软件对晶粒取向分布统计。退火后斜截面样品的表面晶粒取向分布如图2所示，左侧为抛光严重区域，右侧为抛光较浅区域，其中不同颜色表示与立方取向偏离较大的晶粒。EBSD分析结果显示，抛光严重的区域在热处理后形成了一定的旋转立方取向孪晶和退火孪晶（图2中彩色的晶粒），抛光较浅的区域则比较少。图3为本发明高温退火后斜截面样品的非立方织构的ODF图（φ2=0°），图4为初始再结晶合金基带芯层的非立方织构的ODF图（φ2=0°），比较可知，两者的非立方织构组成非常相似，均含有旋转立方织构和退火孪晶织构。以上结果可以说明Ni7at.%W合金基带原始表面的形变织构对基带整体立方织构的形成有重要作用，在完全再结晶过程中，表面形成的立方织构可以吞并整个基带厚度上的非立方织构，使整个基带都呈现强的立方织构。The recrystallized Ni7at.%W alloy substrate sample was tested with a scanning electron microscope system (SEM: JEOL JSM-6500F) equipped with EBSD accessories. The scanning range was 500um*700um, and the scanning step was 1um. The software counts the grain orientation distribution. The surface grain orientation distribution of the oblique section sample after annealing is shown in Figure 2. The left side is the severely polished area, and the right side is the lightly polished area. Different colors indicate grains that deviate greatly from the cubic orientation. The results of EBSD analysis show that, after heat treatment, the heavily polished area forms certain spin-cubic orientation twins and annealing twins (colored grains in Figure 2), while the less polished area is less. Figure 3 is the ODF diagram of the non-cubic texture of the oblique section sample after high temperature annealing in the present invention (φ 2 =0°), and Figure 4 is the ODF diagram of the non-cubic texture of the core layer of the initially recrystallized alloy base band (φ 2 =0°) °), the comparison shows that the non-cubic texture composition of the two is very similar, both contain rotated cubic texture and annealed twin texture. The above results can show that the deformation texture of the original surface of the Ni7at.%W alloy baseband plays an important role in the formation of the overall cubic texture of the baseband. During the complete recrystallization process, the cubic texture formed on the surface can annex the non-cubic Texture, so that the entire baseband presents a strong cubic texture.
从以上分析可知，采用本发明的一种EBSD测试用基带斜截面的制备及分析方法，可采用一副图同时分析或表征基带表面与截面的再结晶织构转变，并分析基带表面的形变织构对再结晶织构演变的影响。As can be seen from the above analysis, adopting the preparation and analysis method of a baseband oblique section for EBSD testing of the present invention, a pair of pictures can be used to simultaneously analyze or characterize the recrystallization texture transformation of the baseband surface and the cross section, and analyze the deformation texture of the baseband surface. The effect of texture on the evolution of recrystallization texture.
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