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A method of preparing "nose tip" specimen for fib three-dimensional reconstruction

A technology of three-dimensional reconstruction and nose tip, which is applied in the direction of material analysis, instruments, and measuring devices using wave/particle radiation, which can solve the problems of high cost, reduce sample preparation costs, promote popularization and application, and shorten the use time.

Active Publication Date: 2021-04-02
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide an innovative method for preparing samples for FIB three-dimensional characterization analysis, which solves the problem that the cost of traditional sample preparation methods is too expensive

Method used

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  • A method of preparing "nose tip" specimen for fib three-dimensional reconstruction
  • A method of preparing "nose tip" specimen for fib three-dimensional reconstruction
  • A method of preparing "nose tip" specimen for fib three-dimensional reconstruction

Examples

Experimental program
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Effect test

example 1

[0023] (1) Al-Si alloy ingots are prepared by induction melting;

[0024] (2) The sample is mechanically polished, and the sample area to be tested is marked under an optical microscope;

[0025] (3) if figure 2 As shown in (b), with the area to be tested as the center, leave 0.5mm for the left, right, and front parts respectively, so that the sample is in an "L" shape, and the area to be tested is located at the front end of the "L" shape, and the "L" shaped block is generally Length 4mm, width 3mm, depth 3mm, paste copper tape on the surface of the area to be tested (purpose: to protect the sample to be tested from being polluted by wire cutting oil, and the conduction of copper tape will not affect wire cutting, just remove the copper tape after wire cutting) , use the wire cutting method to cut the sample, and initially form the "nose tip", the width of the "nose tip" is 1mm;

[0026] (4) if figure 2 (d) Polish both sides of the "nose tip" with high-grit sandpaper, fr...

example 2

[0030] (1) Prepare titanium alloy ingot ((Ti-5.5Mo-7.2Al-4.5Zr-2.6Sn-2.1Cr)) by vacuum consumable arc melting; heat treatment at 740°C for 5 hours after forging and solution treatment , water quenching to maintain high temperature microstructure;

[0031] (2) After the sample is mechanically polished, electropolishing is performed to remove the surface layer. Polishing parameters: 25°C, 25V, about 30s, polishing liquid: 6% HClO 4 , 34% CH 3 (CH 2 ) 3 OH and 60% CH 3 OH;

[0032] (3) A sample of 5 mm x 1 mm x 0.5 mm is cut out from the polished sample. Make the area to be measured close to the edge of the sample, and electrochemically polish the sample to a thickness of about 26 μm, such as Figure 5 As shown in (a): Clean the aluminum block with alcohol, and polish the surface of the aluminum block to be glued with sandpaper, stick the sample to the aluminum block with silver glue, and then stick the metal block to the workbench with silver glue, and put it into the vac...

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Abstract

The invention discloses a method for preparing a ''nasal tip-shaped'' sample used for a FIB three-dimensional reconstruction. The method comprehensively applies means of cutting technique, electrochemical polishing and sanding. The method has the process characteristics that: performing a normal gold phase sample preparation; marking a to-be-detected sample under an optical microscope or a scanning electron microscope; performing rough machining by adopting a cutting technique to cut the sample into a L-shaped or strip-shaped sample, the to-be-detected area is located at the front end of the sample and forming a ''nose tip'' preliminarily, wherein the width of the ''nose tip'' is 1 mm or less; polishing the two sides of the ''nose tip'' by a high-mesh sandpaper or corroding the front end of the sample by means of electrochemical polishing to further reduce the width of the ''nose tip'' to 100 [mu]m or less; and refining the ''nose tip'' into a specified size by adopting an FIB system.The method has the advantages that the sample preparation cost is greatly reduced under a condition that the qualities of an obtained sample is consistent with a prepared sample adopting an FIB traditional hole digging technology, and the popularization and application of the FIB in a three-dimensional characterization analysis are forcefully promoted.

Description

technical field [0001] The invention relates to a sample preparation method for three-dimensional characterization analysis of a focused ion beam (Focused Ion beam, FIB). Background technique [0002] FIB processing is a new technology developed in recent decades. It uses electric lens to focus the ion beam into a very small ion beam bombarding the surface of the material, so as to realize the stripping, deposition, implantation, cutting and modification of the material [Document 1 Han Wei, Xiao Siqun. Focused Ion Beam (FIB) and Its Applications[J]. Progress in Materials in China, 2013,32(12):716-727+751.]. In recent years, with the combination of various advanced signal detection modes and the development of FIB-SEM dual-beam system in terms of resolution and stability [Document 2 Jia Zhihong, Wang Xueli, Xing Yuan, Liu Yingying, Liu Qing. FIB-based 3D characterization analysis technology and application progress[J]. China Materials Progress, 2013,32(12):735-741+751.], FIB...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N23/2202
CPCG01N23/2202
Inventor 袁紫樱关舒月冯荣程永建陈晓华
Owner UNIV OF SCI & TECH BEIJING
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