Method for producing ultrafine metal wire vertical section transmission electron microscope sample film

Abstract

A method for producing an ultrafine metal wire vertical section transmission electron microscope sample film comprises the following steps: cutting a metal wire sample, and straightening and fixing the cut metal wire sample; attaching a pair of circular molybdenum rings to the upper part and the lower part of the metal wire in order to make the metal wire exposed from the hollow parts of the circular molybdenum rings, and shearing the metal wire outside the molybdenum rings to complete packaging; and placing the packaged molybdenum rings on the sample table of an ion thinner, performing thinning under an ion energy of 1-5 Kev at an ion beam incidence angle of 1-10 DEG, observing the sample thinning situation, and taking out the sample after the middle of the metal wire is perforated or broken in order to obtain the ultrafine metal wire vertical section transmission electron microscope sample film. The method has the advantages of simplicity in operation, high success rate, low sample production cost, avoiding of deformation, pollution, non-crystallization and other problems in the sample production process, and great reduction of the sample taking and storing difficulty, and can bewidely used to produce vertical section samples of metal wires having ultrafine diameters.

Description

technical field [0001] The invention belongs to the field of transmission electron microscope sample preparation, and provides a method for preparing ultrafine metal wire (minimum diameter 0.05mm) longitudinal section transmission electron microscope film samples. Background technique [0002] Transmission electron microscopy is an important means to observe the microstructure of metal materials. To observe the material structure by transmission electron microscope, the premise is to prepare qualified thin film samples. The methods for preparing transmission film samples are mainly electrolytic double spray method, focused ion beam cutting method, ion beam thinning method and so on. [0003] It is very difficult to prepare thin film samples of ultra-fine metal wires (diameter ≤0.3mm). 1) Electrolytic double-spray thinning method, the diameter of the sample preparation fixture is Φ3.0mm, and the sample that is too small cannot cover the holes in the fixture. During the el...

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Problems solved by technology

1) Electrolytic double-spray thinning method, the diameter of the sample preparation fixture is Φ3.0mm, and the sample that is too small cannot cover the holes in the fixture. During the electrolytic double-spray process, the sample cannot remain stable in the two electrolyte columns , causing the sample to be easily deformed and damaged; at the same time, because the photoelectric sensing system cannot be used to automatically determine whether it is perforated, the sample preparation process will be uncontrolled

It is difficult to guarantee the quality of samples by electroplating, splicing, bonding and other methods to prepare samples

In addition, the preservation and observation of samples after preparation are difficult

2) Focused ion beam thinning method (FIB), requires expensive special equipment (scanning electron microscope equipped with ion gun, micromanipulator), long sample preparation time and high cost; for samples with extremely small size (diameter ≤ 0.3mm) It is difficult in the process of clamping and sampling. In addition, the focused ion beam will cause amorphous structure in the sample during the sample preparation process, resulting in misjudgment of tissue observation and material analysis.

3) The ion beam thinning method, the fixture is prepared for samples of standard size, direct ion beam bombardment of thin metal wire samples will cause the wire to break from the middle, making subsequent sampling and transfer very difficult, and the sample is vulnerable Contamination, difficult to fix on the TEM sample stage, etc.

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