Preparation method of electron beam sensitive brittle material transmission electron microscope sample

Abstract

The invention discloses a preparation method of an electron beam sensitive brittle material transmission electron microscope sample. The preparation method comprises the following steps: A, preparinga sheet sample; B, carrying out water milling pre-thinning on the sheet sample; C, performing low-temperature ion sputtering thinning on the pre-thinned sheet sample; and D, carrying out carbon spraying treatment on the surface of the sheet sample subjected to low-temperature ion sputtering thinning, so as to deposite a layer of amorphous carbon film on the surface of the sheet sample. According to the method, measures such as liquid nitrogen cooling, carbon spraying treatment and the like are adopted, so that the influence of adverse factors such as charge accumulation and the like on the microstructure of the sample in the TEM sample preparation process is reduced.

Description

technical field [0001] The invention relates to the technical field of transmission electron microscope sample preparation, in particular to a method for preparing a transmission electron microscope sample of an electron beam-sensitive brittle material. Background technique [0002] In the structure research of electron beam-sensitive brittle materials, micro-nano-scale structural characterization relying on transmission electron microscopy (TEM) has always been a major problem, and the root of this problem lies in the preparation of TEM samples for brittle materials. [0003] Currently widely used TEM sample preparation methods are focused ion beam (FIB) micro-nano processing, ion sputtering thinning and ultrathin sectioning. Focused ion beam FIB prepares TEM samples for transmission electron microscopy. Usually, at an accelerating voltage of 30kV, Ga ions are used to etch the material at a high speed to achieve thinning, which has the advantages of high precision and high ...

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Problems solved by technology

[0004] Compared with the focused ion beam FIB, the Ar ions used for ion sputtering thinning have a smaller atomic mass, but due to the long sputtering time and energy concentration, it is easy to cause the temperature of the material surface to rise and cause burns

Although the ultra-thin section method can avoid the above-mentioned problems, due to the brittleness of the material, the section process will inevitably introduce mechanical damage, resulting in the initiation and propagation of cracks, making it difficult to obtain a complete thin-section sample

On the other hand, even if the above three methods themselves do not cause damage to the microstructure of the material, the charge accumulation during the TEM shooting process of the transmission electron microscope will also cause damage to the microstructure.

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