Nano-film transmission electron microscope in-situ heating chip sample preparation method

Abstract

The invention discloses a nano-film transmission electron microscope in-situ heating chip sample preparation method. The method comprises the following steps: (1) selecting a liquid injection device;(2) cleaning and fixing the liquid injection device; (3) bending one end of a copper wire into a copper ring; (4) moving the copper ring to a position near the thin film sample, and fishing up the thin film sample to the copper ring; (5) extruding a liquid drop from the liquid in the microsyringe; (6) moving the copper ring to a position near the liquid drop at the tip of the microsyringe, so thatthe film sample is adsorbed on the liquid drop; (7) accurately adsorbing the liquid drops in a sample observation area, and then moving away the microsyringe; (8) naturally drying the chip; and (9) heating and baking the naturally dried chip. Accurate titration of the nano-film in the Si3N4 film observation area in the transmission electron microscope in-situ heating chip can be realized, hydrophilic treatment on the Si substrate is not needed, the cost is reduced, the influence of surface tension on the film is avoided, the sample preparation success rate is improved, and the risk of damageto a chip electrode is reduced.

Description

technical field [0001] The invention relates to the technical field of in-situ test sample preparation for a transmission electron microscope, in particular to a sample preparation method for in-situ heating chips for a nanometer film. Background technique [0002] The in-situ heating experiment of transmission electron microscope based on MEMS chip can observe the dynamic physical and chemical process of nanomaterials (including nanoparticles, powder and thin film samples) at the atomic scale, and is a good way to study the morphology, structure and performance of nanomaterials in the process of preparation and service. Effective means of changing and reaction mechanism. Commercial TEM in situ heating chips generally consist of Si substrates, metal heating ring electrodes and Si with holes. 3 N 4 Thin film, Si covered metal heating ring electrode 3 N 4 The thin film functions to support nanomaterials, conduct heat, and be transparent to electron beams. On the conventio...

AI Technical Summary

Problems solved by technology

[0003] The traditional film scooping method has the following disadvantages: (1) If the film sample is small, it is easier to attach to the surface of the Si substrate during scooping, so it is necessary to prepare a film sample with a larger cross-sectional area than the chip groove to ensure Some samples can fall into the groove as much as possible and adhere to the observation area; (2) Since the Si substrate itself is hydrophobic, it is necessary to use special equipment (such as a plasma cleaner for oxygen source) to clean the chip before fishing. Hydrophilic treatment, the steps are cumbersome and the cost is high; (3) For a small film sample, even if it falls into the observation area in the groove, the solvent will gradually move to the surface under the action of surface tension during the solvent evaporation process. The bottom of the inner wall of the groove causes the film to move and attach outside the observation area; (4) There is a risk of damaging the chip electrode during the process of chip clamping and film removal