Transmission electron microscope sample preparation device and method capable of positioning position of thin region
A technology for transmission electron microscope samples and preparation devices, which is applied in the preparation of test samples and material analysis using radiation. It can solve problems such as difficult positioning and achieve the effects of no ion damage, precise control, and low cost.
Active Publication Date: 2021-07-09
NANJING UNIV OF SCI & TECH
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Problems solved by technology
[0004]
Aiming at the problem of difficult positioning in the existing TEM electrolytic double-spray sample preparation process, the purpose of the present invention is to provide a new TEM sample preparation device based on the principle of local electrochemical polishing, so as to realize precise positioning of the region of interest of the metal electron microscope sample Polishing, to obtain a local electron beam transparent area for transmission electron microscope microstructure research, which greatly facilitates the analysis of material structure and performance relationship, and improves work efficiency
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Embodiment 1
[0067] Below, the preparation of transmission electron microscope samples by electrolytic polishing at the boundary point of deformation twins in pure copper is taken as an example to illustrate the use process of the present invention:
[0068] (1) Processing of the original sample: firstly, the deformed copper sheet sample was cut to a 0.8 mm thick sheet by a wire electric discharge machine, and the sample was thinned to 40 microns by sandpaper of different grain sizes. Surface scratches were removed by conventional electrolytic polishing. The surface of the sample was etched out of twins by chemical etching solution. A sample with a diameter of 3 mm was punched out by an electron microscope sample punch. The sample is thinned to the through-hole by the double-jet thinning process, and the macro-thinning around the hole is realized, such as Figure 4 shown. Put the double-sprayed sample 26 into the metal clamp block I23 of the anode sample holder, and then tighten the nut...
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Abstract
The invention belongs to the field of material testing, and particularly relates to a transmission electron microscope sample preparation device and method capable of positioning the position of a thin region. The device comprises an electrochemical reaction unit, an in-situ observation unit, a sample mounting unit, a polishing positioning unit, an image acquisition unit and a control system, the electrochemical reaction unit adopts a cathode polishing needle to perform electrolytic polishing on a sample connected with an anode; the in-situ observation unit is used for observing the side face and the front face of the sample and determining and positioning the distance between the cathode polishing needle and the surface of the sample; the sample mounting unit is used for mounting a sample and adjusting the position of the sample; the polishing positioning unit is used for adjusting the position and distance of the cathode polishing needle relative to the sample surface; and the image acquisition unit is used for acquiring a real-time image of the sample and displaying the real-time image on the control system. The device has the characteristic that ion implantation cannot be introduced in the local electrolytic polishing process, has the advantages that the area needing to be polished can be accurately positioned, and the like, and a new sample preparation method is provided for structural characterization of a micro-scale sample.
Description
technical field [0001] The invention belongs to the technical field of material testing, in particular to a transmission electron microscope sample preparation device and method capable of locating the position of a thin area. Background technique [0002] Transmission electron microscopy is widely used in the analysis of microscopic morphology, crystal orientation and microregion composition of various metal materials, which is of great significance for establishing the relationship between material structure and performance and revealing the mechanism of microscopic deformation. Electron beams can only penetrate materials with a certain thickness (<100nm) for imaging. Therefore, it is necessary to prepare extremely thin electron beam transparent samples by different technical means before conducting transmission electron microscope observation. There are two main types of traditional methods for preparing metallic material TEM samples. The first type is electrochemical...
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IPC IPC(8): G01N23/04G01N1/32
CPCG01N23/04G01N1/32
Inventor 王振宇鲍伟康尤泽升
Owner NANJING UNIV OF SCI & TECH