CN111289546A - Preparation and characterization method of precious metal superfine wire EBSD test sample - Google Patents
Preparation and characterization method of precious metal superfine wire EBSD test sample Download PDFInfo
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/203—Measuring back scattering
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/2005—Preparation of powder samples therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20058—Measuring diffraction of electrons, e.g. low energy electron diffraction [LEED] method or reflection high energy electron diffraction [RHEED] method
Abstract
The invention relates to a preparation and characterization method of an EBSD test sample of a noble metal superfine wire. A precious metal superfine wire sample is stretched and adhered to the top end of an inclined plane of a double-inclined sample table, and is placed in a sample bin to select a sample section preparation and test area; the tilting sample stage is used for carrying out carbon plating treatment, ion beam cutting and ion beam surface polishing treatment on a sample in a view field to obtain a cross section observation sample of the noble metal superfine wire without surface stress, and observing and obtaining a microstructure morphology image of a wire cross section observation area through ion beam channel contrast imaging; and (3) tilting the double-tilting sample stage until the observation section and the incident electron beam form an angle of 70 degrees, and performing electron back scattering diffraction detection on the section of the superfine wire material by using a CCD (charge coupled device) detector to obtain an EBSD (electron back scattering) image and crystallography information of the section of the sample micro-area. The EBSD and ion beam channel contrast image combination provided by the invention provides more systematic and comprehensive data support for micro-area analysis of the noble metal superfine wire, and can expand the comprehensive analysis range of a sample.
Description
Technical Field
The invention relates to a preparation and characterization method of an EBSD test sample of a noble metal superfine wire, belonging to the technical field of noble metal superfine wire test.
Background
Noble metal superfine wires are commonly used in key positions of precise electronic functional devices, but the traditional technology of the finished product of the noble metal superfine wires with a tiny dimension (the diameter is less than phi 0.1 mm) cannot represent the tissue structure of the superfine wires, and the microstructure evolution law of the noble metal superfine wires is indirectly inferred by adopting the sheet structure of the alloy. And the wire and the sheet generate larger tissue difference in the deformation process, and the characterization method cannot accurately and objectively reflect the real tissue structure. The lack of accuracy hinders the research work of noble metal superfine wire recrystallization texture analysis, superfine composite wire phase identification and thickness measurement, twin preferred orientation, grain boundary distribution and the like, thereby restricting the development of the material.
The noble metal superfine wire has fine size and strong plasticity, so that a good cross-section sample is difficult to obtain by a conventional sample preparation method for micro texture analysis.
Disclosure of Invention
The invention provides a preparation and characterization method of an EBSD test sample of a noble metal superfine wire, aiming at the problems in the prior art, the invention uses a channel contrast imaging to observe the grain size before an EBSD surface scanning acquisition chrysanthemum pool line, finds areas such as defects, deformation areas, recrystallization grains and the like, characterizes dislocation structures, twin boundaries and deformation zones, and then adopts an EBSD technology to calibrate the crystal orientation of the area of interest; the combination of the EBSD and the channel contrast image improves the spatial resolution and the comprehensive analysis range of the EBSD; therefore, the method can solve the problems that the traditional technical method can not accurately represent the recrystallization texture of the noble metal superfine wire, the phase identification and thickness measurement of the superfine composite wire, the preferred orientation of twin crystals, the grain boundary distribution and the like.
The Focused Ion Beam (FIB) has the functions of nano-graph processing, ion beam channel contrast imaging, precise positioning section preparation, TEM sample preparation, continuous section processing imaging, microelectronic element circuit editing, chip repairing and the like; for noble metal ultra-fine wire polycrystalline material, the orientation of each grain is different. When the incident beam irradiates the surface of the sample, the included angle between the crystal face of the surface layer of the sample and the incident beam is different, and when the included angle between the incident beam and the crystal face is larger, the more signals overflow the surface of the sample, and the higher the image brightness is; conversely, the smaller the angle between the incident beam and the facets, the more channels are formed between the facets, and the less signal spills over the sample surface, the darker the image. For the polycrystalline material with uniform components and polished planes, the crystal grains with larger relative orientation difference are brighter in imaging, so that the orientation distribution condition of the crystal grains of the noble metal superfine wire can be known qualitatively; the ion beam channel microscopic imaging can observe the orientation contrast of a polycrystalline sample, and shows the grain boundary without metallographic corrosion, particularly twin grain boundary and subboundary, so as to evaluate the property of plastic deformation and the recrystallization process of the noble metal superfine wire subjected to multi-pass drawing and high accumulated deformation degree.
A preparation and characterization method of an EBSD test sample of a noble metal superfine wire is characterized by comprising the following steps:
(1) stretching and bonding a noble metal superfine wire sample to the top end of the inclined plane of the double-inclined sample table, then placing the sample in a sample bin, sealing the sample bin and vacuumizing, observing the position of the noble metal superfine wire sample by using a secondary electron microscope of a double-beam scanning electron microscope, adjusting the position of the noble metal superfine wire sample in a visual field, and selecting a section preparation and test area of the noble metal superfine wire sample;
(2) the method comprises the steps that a tilting double-tilting sample stage is arranged until a noble metal superfine wire sample in a view field is perpendicular to a focused ion beam of a double-beam scanning electron microscope, the noble metal superfine wire sample in the view field is subjected to carbon plating treatment to form a carbon-plated protective film, the focused ion beam of the double-beam scanning electron microscope is used for carrying out ion beam rough cutting on the noble metal superfine wire sample, then ion beam current density is reduced step by step to carry out ion beam fine cutting treatment, ion beam surface polishing treatment is carried out to obtain a cross section observation sample of the noble metal superfine wire without surface stress, and a microstructure morphology image of the cross section observation area of the noble metal superfine wire is observed and obtained through ion beam channel contrast imaging;
(3) tilting the double-tilt sample table until the angle between the observation section of the noble metal superfine wire and the incident electron beam is 70 degrees, and performing electron back scattering diffraction detection on the section of the superfine wire by using a CCD (charge coupled device) detector to obtain an EBSD (electron back scattering) image and crystallographic information of the micro-area section of the noble metal superfine wire sample;
the inclination of the double-inclined sample table in the step (1) is 36 degrees, and two ends of the noble metal superfine wire sample are tightened and are parallel to the intersection line of two inclined planes of the double-inclined sample table;
the carbon-plated protective film is located at 1/2 mm in diameter of the precious metal superfine wire sample in the visual field, and the thickness of the carbon-plated protective film is 2-3 mu m;
the voltage for rough cutting of the ion beam in the step (2) is 30 KV;
further, the ion beam current density of the ion beam rough cutting in the step (2) is 15 nA, the ion beam current densities which are gradually reduced in the ion beam fine cutting treatment are 5nA, 2nA and 1nA in sequence, and the ion beam current density of the ion beam surface polishing treatment is 0.3 nA;
the tilting double-tilting sample stage in the step (3) rotates 180 degrees along the x-y direction, and then tilts 34 degrees clockwise to enable the observation section of the noble metal superfine wire to form an included angle of 70 degrees with the incident electron beam;
the step length of the electron back scattering diffraction detection in the step (3) is 0.02-0.1 mu m;
furthermore, the diameter of the noble metal superfine wire sample is 5-50 μm, and the length of the observation section of the noble metal superfine wire along the stretching direction of the noble metal superfine wire is not more than 100 μm.
The invention has the beneficial effects that:
(1) according to the preparation and characterization method of the precious metal superfine wire EBSD test sample, the FIB function of a double-beam electron microscope is utilized to perform surface stress-free cutting processing on the precious metal superfine wire sample, and meanwhile, the EBSD function of the double-beam electron microscope is utilized to realize microstructure observation and orientation characterization of a section sample; according to the method, the FIB-EBSD technology is used for in-situ preparation, the whole preparation and characterization process does not need to take the precious metal superfine wire sample out of a sample cavity of an instrument for processing, so that the influence of environment or artificial external force is avoided, the EBSD information of the sample section can be accurately and immediately obtained, the accuracy of sample characterization and analysis is effectively improved, and the defects that the prior art lacks key characterization technologies in the aspects of precious metal superfine wire sample recrystallization texture analysis, superfine composite wire phase identification and thickness measurement, twin crystal preferred orientation, grain boundary distribution and the like can be effectively overcome;
(2) according to the invention, ion beam channel contrast imaging and the EBSD technology are combined, microstructure information with a larger view field can be obtained, the channel contrast imaging is firstly used for observing the grain size, defects, deformation areas, recrystallized grains and other areas are found, a dislocation structure, twin boundaries and deformation zones are represented, and then the EBSD technology is adopted for carrying out crystal orientation calibration on an interested area; the combination of the EBSD and the channel contrast image improves the spatial resolution and the comprehensive analysis range of the EBSD; the method can provide more systematic and comprehensive data support for the micro-area analysis of the noble metal superfine wire, and can expand the comprehensive analysis range of the sample.
Drawings
FIG. 1 is a schematic diagram of the principle of preparing noble metal ultra-fine wire by a dual-beam scanning electron microscope;
FIG. 2 is a diagram of a real object after cutting of the coating position and section of a noble metal ultrafine wire protective film by FIB cutting;
FIG. 3 is an image of ion beam channel contrast after FIB cutting of an ultrafine Ag wire of 10 μm diameter according to example 1;
FIG. 4 is an image of ion beam channel contrast after FIB cutting of an ultrafine Ag wire of example 1 having a diameter of 20 μm;
FIG. 5 is an image of ion beam channel contrast of a cross section of a noble metal Ag ultra-fine wire of example 2 having a diameter of 20 μm;
FIG. 6 is an image of the ion beam channel contrast of the cross section of the noble metal AgAuPd ultrafine wire of example 2 having a diameter of 20 μm;
FIG. 7 is an image of ion beam channel contrast of a cross section of a 20 μm diameter noble metal Au ultra-fine wire of example 2;
FIG. 8 is an image of ion beam channel contrast of a cross section of a noble metal Au/Ag ultra-fine wire of example 2 having a diameter of 20 μm;
FIG. 9 is an EBSD-IPF drawing of a cross section of a noble metal Ag ultra-fine wire having a diameter of 20 μm in example 2;
FIG. 10 is an EBSD-IPF orientation view of a cross section of the noble metal AgAuPd ultrafine wire of example 2 having a diameter of 20 μm;
FIG. 11 is an EBSD-IPF drawing of a cross section of the ultrafine noble metal Au wire of 20 μm diameter of example 2;
FIG. 12 is an EBSD-IPF drawing of a cross section of the noble metal Au/Ag ultrafine wire of example 2 having a diameter of 20 μm.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
The field emission double-number electron microscope in the embodiment of the invention is produced by FEI company under the flag of Thermal Fisher, the model number of the field emission double-number electron microscope is VERSA 3D, the accessory EBSD probe is produced by EDAX company, the model number of the accessory EBSD probe is HIKARI-SERIES, the data acquisition software is EDAX-OIM V7, and the data Analysis software is TSL OIM Analysis 7.
Example 1: a preparation and characterization method of an EBSD test sample of a noble metal superfine wire comprises the following steps:
(1) stretching and bonding a noble metal Ag superfine wire sample with the diameter of 10 mu m to the top end of the inclined surface of a double-inclined sample table, wherein the inclination of the double-inclined sample table is 36 degrees, and two ends of the noble metal Ag superfine wire sample are tightened and are parallel to the intersection line of the two inclined surfaces of the double-inclined sample table; placing the noble metal Ag superfine wire sample in a sample bin, sealing the sample bin, vacuumizing, observing the position of the noble metal Ag superfine wire sample by using a secondary electron microscope of a double-beam scanning electron microscope, adjusting the position of the noble metal Ag superfine wire sample in a visual field, and selecting a section preparation and test area of the noble metal Ag superfine wire sample;
(2) the method comprises the steps that a tilting double-tilting sample table is rotated to a position where a noble metal Ag superfine wire sample in a view field is perpendicular to a focused ion beam of a double-beam scanning electron microscope, and a carbon-plated protective film is formed in a region to be observed of the noble metal Ag superfine wire sample in the view field through carbon plating so as to protect the tissue structure of the wire surface from being damaged by the ion beam, wherein the carbon-plated protective film is located at 1/2 of the diameter of the noble metal Ag superfine wire sample in the view field, and the average thickness of the carbon-plated protective film is 2.2 mu m; carrying out ion beam rough cutting on the to-be-observed area of the noble metal Ag superfine wire sample at the position of the diameter 1/2 of the noble metal Ag superfine wire sample by using a focused ion beam of a double-beam scanning electron microscope, wherein the voltage of the ion beam rough cutting is 30KV, and the current density of the ion beam for the ion beam rough cutting is 15 nA; then keeping the voltage for cutting the ion beam at 30KV, and reducing the current density of the ion beam step by step to carry out ion beam fine cutting treatment, wherein the current density of the ion beam reduced step by step in the ion beam fine cutting treatment is 5nA, 2nA and 1nA in sequence; keeping the voltage for cutting the ion beam at 30KV, and performing ion beam surface polishing treatment to obtain a section observation sample of the noble metal Ag superfine wire without surface stress, wherein the current density of the ion beam subjected to the ion beam surface polishing treatment is 0.3 nA; the schematic diagram of the principle of preparing noble metal Ag superfine wire by a double-beam scanning electron microscope is shown in figure 1, the position of the coating film of the noble metal Ag superfine wire by FIB cutting and the real object diagram after the section cutting are finished are shown in figure 2, and the dark-colored strip-shaped covering layer in figure 2 is a carbon protective film; observing and obtaining a microstructure and morphology image of a section observation area of the noble metal Ag superfine wire through ion beam channel contrast imaging, wherein the microstructure and morphology image is shown in figure 3, as can be seen from figure 3, the Ag superfine wire has obvious structural difference along the drawing direction, the grain size is gradually reduced from left to right, a large grain area mostly has equiaxial crystals, a preferred orientation texture disappears, and a small grain area mainly has the texture and fine grains; the length of the observation section processed by the ion beam along the stretching direction of the noble metal superfine wire is about 70 mu m;
(3) the angle between the observation section of the noble metal Ag superfine wire and the incident electron beam is 70 degrees by tilting the double-tilting sample platform, wherein the tilting double-tilting sample platform rotates 180 degrees along the x-y direction, and then tilts 34 degrees clockwise to form an included angle of 70 degrees between the observation section of the noble metal Ag superfine wire and the incident electron beam; the electron back scattering diffraction detection is carried out on the section of the superfine wire material through a CCD detector, and the grain size of the wire material is small, so that the EBSD can accurately collect the crystallography data of the Ag superfine wire material, the detection step length is set to be 0.05 mu m, and the EBSD image and the crystallography information of the micro-area section of the noble metal Ag superfine wire material sample are obtained.
Example 2: a preparation and characterization method of an EBSD test sample of a noble metal superfine wire comprises the following steps:
(1) respectively stretching and bonding precious metal (four alloys with different components, namely Ag, AgAuPd, Au and Au/Ag) superfine wire samples with the diameter of 20 mu m to the top end of the inclined plane of the double-inclined sample table, wherein the inclination of the double-inclined sample table is 36 degrees, and the two ends of the precious metal superfine wire samples are tightened and are parallel to the intersection line of the two inclined planes of the double-inclined sample table; placing the noble metal superfine wire material sample in a sample bin, sealing the sample bin, vacuumizing, observing the position of the noble metal superfine wire material sample by using a secondary electron microscope of a double-beam scanning electron microscope, adjusting the position of the noble metal superfine wire material sample in a visual field, and selecting a section preparation and test area of the noble metal superfine wire material sample;
(2) the method comprises the steps that a tilting double-tilting sample table is arranged until a precious metal superfine wire sample in a view field is perpendicular to a focused ion beam of a double-beam scanning electron microscope, and a carbon-plated protective film is formed in a region to be observed of the precious metal superfine wire sample in the view field through carbon plating so as to protect the tissue structure of the surface of the wire from being damaged by the ion beam, wherein the carbon-plated protective film is located at 1/2 of the diameter of the precious metal superfine wire sample in the view field, and the average thickness of the carbon-plated protective film is 2.5 mu m; carrying out ion beam rough cutting on the to-be-observed area of the precious metal superfine wire sample at the position of the diameter 1/2 of the precious metal superfine wire sample by using a focused ion beam of a double-beam scanning electron microscope, wherein the voltage of the ion beam rough cutting is 30KV, and the current density of the ion beam for the ion beam rough cutting is 15 nA; then keeping the voltage for cutting the ion beam at 30KV, and reducing the current density of the ion beam step by step to carry out ion beam fine cutting treatment, wherein the current density of the ion beam reduced step by step in the ion beam fine cutting treatment is 5nA, 2nA and 1nA in sequence; keeping the voltage for cutting the ion beam at 30KV, and performing ion beam surface polishing treatment to obtain a section observation sample of the noble metal superfine wire material without surface stress, wherein the current density of the ion beam subjected to the ion beam surface polishing treatment is 0.3 nA; the schematic diagram of the principle of preparing the noble metal superfine wire by the double-beam scanning electron microscope is shown in figure 1; observing and obtaining a microstructure morphology image of a noble metal Ag filament section observation area with the diameter of 20 mu m through ion beam channel contrast imaging, wherein the microstructure morphology image is shown in a figure 4; as can be seen from FIG. 4, the Ag ultra-fine wire material has obvious structural difference along the drawing direction, the grain size gradually decreases from left to right, the major grain region is mostly equiaxial, the preferred orientation texture disappears, and the minor grain region is mainly texture and fine grains; the length of the observation section processed by the ion beam along the stretching direction of the noble metal superfine wire can reach 100 mu m; the imaging graphs of the ion beam channel contrast of the sections of the noble metal superfine wires with the diameter of 20 mu m are shown in figures 5-8, wherein the figure 5 shows an Ag wire, the figure 6 shows an AgAuPd wire, the figure 7 shows an Au wire, and the figure 8 shows an Au/Ag composite wire, and as can be seen from the figures 5-8, the channel contrast of the four superfine wires shows a typical deformed wire texture grain structure, but the distribution ranges along the diameter direction are different, the length-diameter ratio difference of preferred orientation grains is larger, in addition, twin crystals exist in the wire texture, but the quantity and the size of the twin crystals are different, and quantitative analysis shows that the Ag and the AgAuPd wires have thick annealing twin crystal textures;
(3) the angle between the observation section of the noble metal superfine wire and the incident electron beam is 70 degrees by tilting the double-tilting sample stage, wherein the tilting double-tilting sample stage rotates 180 degrees along the x-y direction, and then tilts 34 degrees clockwise to form an included angle of 70 degrees between the observation section of the noble metal superfine wire and the incident electron beam; the electron back scattering diffraction detection is carried out on the section of the superfine wire material by a CCD detector, because the grain size of the wire material is fine, in order to ensure that EBSD can accurately collect the crystallographic data of the noble metal superfine wire material, the detection step size is set to be 0.07 mu m, EBSD images and crystallographic information of the micro-area section of a noble metal superfine wire material sample are obtained, EBSD-IPF orientation diagrams of the sections of different material noble metal superfine wire materials with the diameter of 20 mu m are shown in figures 9-12, wherein figure 9 is an EBSD-IPF orientation diagram of the section of Ag superfine wire material, figure 10 is an EBSD-IPF orientation diagram of the section of AuAgPd superfine wire material, figure 11 is an EBSD-IPF orientation diagram of the section of Au superfine wire material, figure 12 is an EBSD-IPF orientation diagram of the section of Au/Ag superfine wire material, the IPF orientation analysis of the section structure of the wire material shows that the Ag wire material has a wire structure with the [001] orientation, and the orientation in other three component alloy wire materials has different, twin crystal sizes in the microstructures of the four wires are different, but the orientation of the twin crystal sizes is more inclined to the [111] direction; with reference to fig. 5-12, before EBSD surface scanning, channel contrast imaging is used to observe crystal grains, so that the wire can be analyzed to have different characteristic recrystallization regions, and then EBSD technology is used to select the recrystallization regions to perform crystal orientation calibration, such as annealing twin crystals and deformation texture, so that various wire crystal grains, orientations, textures and crystal boundaries are found to have different characteristics, analysis of the Ag ultrafine wire finds that a large number of twin crystal structures exist in the structure, the core of the wire generates a typical annealing twin crystal structure, the twin crystal structure is fine at the edge, the Au/Ag composite wire does not have a typical twin crystal structure, the equiaxed crystal grains at the edge are slightly large, and the core is a slender filament texture.
The method not only can finish the preparation and processing of the unstressed section of the superfine noble metal wire sample, but also can immediately carry out microstructure observation and orientation analysis on the section of the superfine noble metal wire sample, and the combination of the EBSD and the ion beam channel contrast image can provide more systematic and comprehensive data support for the micro-area analysis of the superfine noble metal wire, and can expand the comprehensive analysis range of the sample.
While the present invention has been described in detail with reference to the specific embodiments thereof, it will be apparent to those skilled in the art that the present invention is not limited to the embodiments described above, and that various changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (6)
1. A preparation and characterization method of an EBSD test sample of a noble metal superfine wire is characterized by comprising the following steps:
(1) stretching and bonding a noble metal superfine wire sample to the top end of the inclined plane of the double-inclined sample table, then placing the sample in a sample bin, sealing the sample bin and vacuumizing, observing the position of the noble metal superfine wire sample by using a secondary electron microscope of a double-beam scanning electron microscope, adjusting the position of the noble metal superfine wire sample in a visual field, and selecting a section preparation and test area of the noble metal superfine wire sample;
(2) the method comprises the steps that a tilting double-tilting sample stage is arranged until a noble metal superfine wire sample in a view field is perpendicular to a focused ion beam of a double-beam scanning electron microscope, the noble metal superfine wire sample in the view field is subjected to carbon plating treatment to form a carbon-plated protective film, the focused ion beam of the double-beam scanning electron microscope is used for carrying out ion beam rough cutting on the noble metal superfine wire sample, then ion beam current density is reduced step by step to carry out ion beam fine cutting treatment, ion beam surface polishing treatment is carried out to obtain a cross section observation sample of the noble metal superfine wire without surface stress, and a microstructure morphology image of the cross section observation area of the noble metal superfine wire is observed and obtained through ion beam channel contrast imaging;
(3) and (3) tilting the double-tilting sample stage until the angle between the observation section of the noble metal superfine wire and the incident electron beam is 70 degrees, and performing electron back scattering diffraction detection on the section of the superfine wire by using a CCD (charge coupled device) detector to obtain an EBSD (electron back scattering) image and crystallographic information of the micro-area section of the noble metal superfine wire sample.
2. The method for preparing and characterizing EBSD test samples of noble metal ultra-fine wires according to claim 1, wherein: in the step (1), the inclination of the double-inclined sample table is 36 degrees, and two ends of the noble metal superfine wire sample are tightened and are parallel to the intersection line of two inclined planes of the double-inclined sample table.
3. The method for preparing and characterizing EBSD test samples of noble metal ultra-fine wires according to claim 1, wherein: the carbon-plated protective film is located at 1/2 mm in diameter of the precious metal superfine wire sample in the visual field, and the thickness of the carbon-plated protective film is 2-3 μm.
4. The method for preparing and characterizing EBSD test samples of noble metal ultra-fine wires according to claim 1, wherein: the ion beam current density of the ion beam rough cutting in the step (2) is 15 nA, the ion beam current densities which are gradually reduced in the ion beam fine cutting treatment are 5nA, 2nA and 1nA in sequence, and the ion beam current density of the ion beam surface polishing treatment is 0.3 nA.
5. The method for preparing and characterizing EBSD test samples of noble metal ultra-fine wires according to claim 1, wherein: and (3) the step length of the electron back scattering diffraction detection in the step (3) is 0.02-0.1 mu m.
6. The method for preparing and characterizing EBSD test samples of noble metal ultra-fine wires according to claim 1, wherein: the diameter of a noble metal superfine wire sample is 5-50 mu m, and the length of the observation section of the noble metal superfine wire along the stretching direction of the noble metal superfine wire is not more than 100 mu m.
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