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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- CN102426125B CN102426125B CN 201110421618 CN201110421618A CN102426125B CN 102426125 B CN102426125 B CN 102426125B CN 201110421618 CN201110421618 CN 201110421618 CN 201110421618 A CN201110421618 A CN 201110421618A CN 102426125 B CN102426125 B CN 102426125B
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Abstract
The invention relates to a preparation method for a baseband oblique section for an EBSD test, and an analysis method thereof, and belongs to the field of the baseband of the high temperature superconducting coat conductor. The steps comprise: (1) cutting the prepared cold-rolled baseband into the baseband with the appropriate size, and carrying out mechanical polishing to form the oblique section; (2) cleaning the polished baseband; (3) carrying out treatments of recrystallization and annealing for the cleaned cold-rolled baseband; (4) adopting the EBSD technology to analyze the grain orientation of the sample surface; (5) carrying out statistical analysis for the test results. According to the present invention, the method is simple, the preparation process for the sample can be shortened, the test time can be saved, and all the required test information can be concurrently obtained.
Description
Technical field
The invention belongs to the base band field of conductor of high-temperature superconductor coat, be specifically related to preparation and analytical approach that Ni-W alloy base band oblique section is used in a kind of EBSD test.
Background technology
In recent years, each technology developed country is all with the practical research of the second generation coating conductor focus as 21 century superconductor research and development, and obtained a series of breakthrough progress.Played the vital role of support, extension transition bed and superconducting thin film layer and bearing part electric current as the important component part alloying metal base band in the coating superconductor sandwich construction, therefore to have the metal toughness base band of biaxial texture be one of key factor that obtains the high-performance coating superconducting wire in preparation.At present, Ni5at.%W is to use one of metal base band widest in area, have the (〉 100M on a large scale of many companies and R﹠D institution in the world wide) produce this kind texture base band, but it is applied to YBCO textured substrate material, still exists not enough in mechanical property and magnetic property.Each research group is respectively in the preparation that focuses on Ni-W alloy base band with high W content of research.2005, the Zhou X.Y.(Appl.Supercond of University of Houston, 17 (2007) 3828-3431) employing purity is 99.99% nickel powder and tungsten powder, after the choosing of 120 purpose mesh screens, obtaining grain size is nickel powder and the tungsten powder of 5-6 μ m, carried out the high-energy ball milling of 30min subsequently, carried out sintering and rolling at last, in Ni9.0at.%W, obtained surpassing 90%(＜15 ° behind the annealing recrystallization) strong cubic texture.2008, the J Eickemeyer(Supercond Sci.Technol of Germany Dresen IFW research group, 21 (2008) 105012) report their result of study aspect the Ni7.5at.%W base band, by changing technology, finally obtained 92.5% recrystallization cubic texture.2011, Germany Dresen IFW research group, J Eickemeyer(Supercond.Sci.Technol, 23 (2010) 085012.) handle by the middle recovery annealing of introducing repeatedly, in Ni-9.0at.%W, obtained the strong cubic texture of cubic texture content (＜9.5 °) up to 96%.Worldwide a lot of research group is respectively with regard to smelting technology or powder metallurgy preparation technology, cold rolling reduction, annealing process (temperature, time, atmosphere) etc. the technical parameter of key link has carried out research widely and report, it is even to obtain composition under optimized process conditions, be orientated single, the cubic-textured metal base band of surfacing has also been carried out simple sign to the forming process of recrystallization texture simultaneously.
Traditional method for making sample and analytical approach require to prepare the sample in base band surface and base band cross section respectively and carry out the EBSD information acquisition, add up comparative analysis then and obtain complete sample message.But because the EBSD measuring technology belongs to the microcosmic field tests, it is a kind of microcosmic characterization method, roughness reaction to sample surfaces is very sensitive, its test specification also has certain limitation, just there is very big error for the surface sample of different preparation methods' acquisitions and the detecting information of cross-sectional sample so, and then interpretation of result affected, and operation steps complexity.
Summary of the invention
In order to solve surface sample and the cross-sectional sample otherness in sample preparation, the present invention proposes a kind of brand-new preparation thinking, and for preparing a kind of oblique section exactly, makes it in when test information in collected specimens surface and cross section simultaneously.The present invention mainly discloses preparation method and the analytical approach that the base band oblique section is used in a kind of EBSD test, can be used to step analysis simultaneously or characterize the surperficial recrystallization texture with the cross section of base band change, and the deformation texture of as analysed basis belt surface is to the influence of recrystallization texture differentiation.This method is simple to operate, can shorten the specimen preparation process, saves the test duration, but can obtain test and the needed full detail of interpretation of result.
The present invention mainly discloses preparation and the analytical approach that the base band oblique section is used in a kind of EBSD test, the recrystallization texture that can be used to while as analysed basis belt surface and cross section changes, and the deformation texture of as analysed basis belt surface may further comprise the steps the influence that recrystallization texture develops:
1) is that the cold rolling alloy base band of 60～100um need be sheared according to test with average thickness, carries out mechanical buffing then and be processed into the oblique section that its key is that cold rolling base band needs be fixed on the grinding tool with gradient with glue, in order to polish.In carrying out polishing process, alloy base band is evenly exerted pressure, thereby obtain to have the alloy base band of oblique section, wherein the polishing of part zone is serious, the top layer of base band top layer 30um～50um is removed, reach the sandwich layer position of base band, this regional recrystallization texture is formed be not subjected to outer effects of Deformation Weaving of Friction Welding, the polishing of another part zone is more shallow, has namely kept the base band top layer of part;
2) polished base band is cleaned: polished base band is put into carried out the decontamination cleaning in the acetone soln, put into then and carry out secondary cleaning in the ethanol solution, carry out ultrasonic deionization at last and clean in distilled water, oven dry is preserved;
3) at Ar/H
2Under mixed gas protected, cleaned cold rolling base band carried out conventional recrystallization annealing handle, obtain twin shaft cubic-textured metal base band; Adopt the grain orientation of EBSD technical Analysis oblique section sample surfaces;
4) above-mentioned test result is analyzed, can be analyzed the influence that surperficial deformation texture develops recrystallization texture.
Formation, the growth process of step 3) in order to analyze the different phase cubic texture, can carry out the recrystallization processing (annealing in process) of different temperatures to base band, for example in order to study surface deformation texture to the influence of sandwich layer cubic texture forming core, can take initial recrystallization to handle to it.
This method is simple to operate, can shorten the specimen preparation process, saves the test duration, obtains needed whole detecting information simultaneously.This invention simultaneously recrystallization texture in as analysed basis belt surface and cross section changes, and the deformation texture of as analysed basis belt surface is to the influence of recrystallization texture differentiation.
Description of drawings
The synoptic diagram of the oblique section sample that Fig. 1 has prepared;
The EBSD orientation maps of the Ni7W oblique section sample surfaces after Fig. 2 embodiment 1 annealing;
The ODF sectional view of the non-cubic texture of Ni7W oblique section sample surfaces after Fig. 3 embodiment 1 annealing (
);
The ODF sectional view of the non-cubic texture of Fig. 4 initial recrystallization Ni7W sample in cross section sandwich layer (
).
Embodiment
The present invention will be further described below in conjunction with specific embodiment, but the present invention need not be limited to following examples.Analyze formation, the growth process of different phase cubic texture, can carry out the recrystallization processing (annealing in process) of different temperatures to base band, for example in order to study surface deformation texture to the influence of sandwich layer cubic texture forming core, can take initial recrystallization to handle to it.
Embodiment 1
With total deformation quantity＞99%, average thickness is the sample that the cold rolling Ni7at.%W alloy base band of 72um cuts into the 5mm*10mm size, be fixed on surfacing, the bright and clean magnesium alloy grinding tool with certain slope with glue, evenly exert pressure to bonding firmly, in order to polish.In carrying out polishing process, alloy base band is evenly exerted pressure, thereby obtain the alloy base band of oblique section, wherein the polishing of part zone is serious, remove on the top layer that is about to about the about 30um in base band top layer, reached the sandwich layer position of base band, this regional recrystallization texture has been formed be not subjected to outer effects of Deformation Weaving of Friction Welding, this zone shows as the recrystallization texture of alloy base band sandwich layer behind the high annealing; Another part zone polishing is more shallow, has namely kept the base band top layer of part, and recrystallization texture that should the zone after the recrystallization annealing is with similar without the top layer texture of polishing.The oblique section sample that has prepared as shown in Figure 1.Polished base band put into carry out decontamination in the acetone soln and clean, scavenging period is 5min, puts into then and carries out secondary cleaning in the ethanol solution, scavenging period is 5min, carry out ultrasonic deionization at last and clean in distilled water, scavenging period is 3min, and oven dry is preserved stand-by; Cleaned cold rolling Ni7at.%W alloy base band is carried out recrystallization annealing handle, treatment temperature is 1450 ℃, insulation 1h, and whole recrystallization processing procedure is at Ar/H
2Carry out under mixed gas protected preventing that sample is oxidized.
Test with the Ni7at.%W alloy base band sample that the scanning electron microscope system (SEM:JEOL JSM-6500F) that is equipped with the EBSD annex handled recrystallization, the surface sweeping scope is 500um*700um, and the surface sweeping step-length is 1um, uses
Software is to the grain orientation distribution statistics.Annealing retread cross-sectional sample the surface microstructure distribution of orientations as shown in Figure 2, the left side is the more shallow zone of polishing for the serious zone of polishing, right side, wherein different colours is represented to depart from bigger crystal grain with cube orientation.The EBSD analysis result shows, polish serious zone and formed certain rotation cube orientation twin and annealing twin (crystal grain of colour among Fig. 2) after thermal treatment, and it is then fewer to polish more shallow zone.Fig. 3 is the retread ODF figure (φ of non-cubic texture of cross-sectional sample of high annealing of the present invention
2=0 °), Fig. 4 is the ODF figure (φ of the non-cubic texture of initial recrystallization alloy base band sandwich layer
2=0 °), more as can be known, both non-cubic textures are formed closely similar, all contain rotation cubic texture and annealing twin texture.Above result can illustrate that the deformation texture of Ni7at.%W alloy base band initial surface is to the vital role that is formed with of the whole cubic texture of base band, in the perfect recrystallization process, the cubic texture that the surface forms can be annexed the non-cubic texture on the whole base band thickness, makes whole base band all present strong cubic texture.
From above analysis as can be known, adopt a kind of EBSD test preparation and analytical approach of base band oblique section of the present invention, can adopt a secondary figure analysis simultaneously or characterize the surperficial recrystallization texture with the cross section of base band to change, and the deformation texture of as analysed basis belt surface is to the influence of recrystallization texture differentiation.
Claims (1)
1. an EBSD tests preparation and the analytical approach of using the base band oblique section, it is characterized in that, may further comprise the steps:
1) with average thickness be 60～100um cold rolling alloy base band according to the test need shear, carry out mechanical buffing then and be processed into the oblique section, its key is that cold rolling base band needs to be fixed on the grinding tool with gradient with glue, in order to polish, in carrying out polishing process, alloy base band is evenly exerted pressure, thereby obtain to have the alloy base band of oblique section, wherein the polishing of part zone is serious, the top layer of base band top layer 30um～50um is removed, reach the sandwich layer position of base band, this regional recrystallization texture is formed be not subjected to outer effects of Deformation Weaving of Friction Welding, the polishing of another part zone is more shallow, has namely kept the base band top layer of part;
2) polished base band is cleaned: polished base band is put into carried out the decontamination cleaning in the acetone soln, put into then and carry out secondary cleaning in the ethanol solution, carry out ultrasonic deionization at last and clean in distilled water, oven dry is preserved;
3) at Ar/H
2Under mixed gas protected, cleaned cold rolling base band carried out conventional recrystallization annealing handle, obtain twin shaft cubic-textured metal base band; Adopt the grain orientation of EBSD technical Analysis oblique section sample surfaces;
4) above-mentioned test result is analyzed, can be analyzed the influence that surperficial deformation texture develops recrystallization texture.
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| CN103389316B (en) * | 2013-07-19 | 2016-02-03 | 武汉钢铁(集团)公司 | silicon steel texture measurement method |
| CN111999323A (en) * | 2020-08-13 | 2020-11-27 | 中国科学院金属研究所 | In-situ EBSD observation method for microscopic orientation evolution of magnesium alloy recrystallized grains |
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| JP2004152904A (en) * | 2002-10-29 | 2004-05-27 | Kyocera Corp | Electrolytic copper foil, film and multilayer wiring substrate therewith, and method of manufacturing the same |
| CN201163266Y (en) * | 2008-02-28 | 2008-12-10 | 宁波宝新不锈钢有限公司 | Metallographic specimen clamper |
| CN101319974A (en) * | 2008-07-18 | 2008-12-10 | 昆明理工大学 | Method for preparing aluminum/lead system laminar composite material metallic phase example and display organization |
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| JP2004093517A (en) * | 2002-09-04 | 2004-03-25 | Jeol Ltd | X-ray analysis apparatus |
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| JP2004152904A (en) * | 2002-10-29 | 2004-05-27 | Kyocera Corp | Electrolytic copper foil, film and multilayer wiring substrate therewith, and method of manufacturing the same |
| CN201163266Y (en) * | 2008-02-28 | 2008-12-10 | 宁波宝新不锈钢有限公司 | Metallographic specimen clamper |
| CN101319974A (en) * | 2008-07-18 | 2008-12-10 | 昆明理工大学 | Method for preparing aluminum/lead system laminar composite material metallic phase example and display organization |
| CN102051666A (en) * | 2010-12-20 | 2011-05-11 | 北京工业大学 | Electrolytic polishing method for EBSD analysis of cold-rolled NiW alloy baseband |
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| 刘丹敏等.银基带再结晶织构的EBSD分析.《低温物理学报》.2005,第27卷(第5期), |
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| 银基带再结晶织构的EBSD分析;刘丹敏等;《低温物理学报》;20051130;第27卷(第5期);859-863 * |
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Effective date of registration: 20170717 Address after: 530000 Guangxi Nanning city Shuangyong Road No. 32 South Lake Garden 4-2004 Patentee after: Guo Fuliang Address before: 100124 Chaoyang District, Beijing Ping Park, No. 100 Patentee before: Beijing University of Technology |
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Effective date of registration: 20221020 Address after: A1501, Innovation Plaza, No. 2007, Pingshan Avenue, Liulian Community, Pingshan Street, Pingshan District, Shenzhen, Guangdong 518118 Patentee after: Shenchuang Superconductor (Shenzhen) Technology Co.,Ltd. Address before: 4-2004, Nanhu Jingyuan, No. 32, Shuangyong Road, Nanning, Guangxi 530000 Patentee before: Guo Fuliang |
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