Preparation method of micron-scale nickel-based superalloy powder transmission electron microscope thin film sample

Abstract

The invention belongs to the technical field of preparation and characterization of alloy materials, and discloses a method for preparing a micron-sized nickel-based superalloy powder transmission electron microscope film sample. The method is as follows: adding nickel-based alloy powder into the electroplating solution and stirring to obtain a suspension; then placing the cathode nickel sheet and the anode nickel sheet in the suspension to obtain uniform nickel-based alloy powder on the cathode nickel sheet; The power supply is electroplated, the nickel-plated layer embeds the nickel-based alloy powder, and then it is mechanically thinned and punched into a disc with a diameter of 3mm, and then ground into a wedge-shaped sample in the thickness direction; it is attached to the opening of the open copper ring , the thin end of the wedge is close to the center of the opening of the copper ring, and then the open copper ring with the sample attached is placed in the ion thinning instrument for ion thinning to obtain a thin film sample area that can be observed by the transmission electron microscope. The method of the invention has the advantages of short time consumption, good coating quality and good embedding effect of nickel-based superalloy powder.

Description

Technical field [0001] The present invention belongs to the preparation and characterization of alloy materials, and more particularly to a micrometer nickel-based high-temperature alloy powder transmitted electron microscopy film sample. Background technique [0002] The microscopic analysis of powder materials is an important method of studying powder tissue and performance, and is a necessary way to further improve material properties. Microstructure analysis of powder materials inevitably involve the preparation of transmitted electron microscopy samples. Some powder materials can be made into suspensions by breaking the powder, and prepared by supporting membrane dispersion. However, there is a difficulty in the preparation of the sample, but the powder particles are required to have no damage to the powder particles. Although the former has achieved some effectiveness in the study of the preparation of the transmissive electron microscope film:,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,...

AI Technical Summary

Problems solved by technology

However, for powder materials that require no damage to the powder particles and are coarse and hard, it brings certain difficulties to sample preparation.

Although predecessors have made some achievements in the preparation of TEM films from powder materials: such as the use of electroless nickel plating, copper plating, glue embedding, etc., these methods are not suitable for the preparation of TEM film samples of large-particle nickel-based superalloy powders. still difficult

For example, the superalloy particles embedded by electroplating copper method, because the hardness of the particles is much higher than that of the embedded copper coating, and the compatibility of copper and nickel powder is worse than that of nickel, the particles will fall off during the ion thinning process, and the thinning process In , copper is more easily thinned, resulting in particles without a carrier

However, electroless nickel plating often takes a long time for the preparation of large-particle nickel-based superalloy powder transmission electron microscope films, and the quality of its coating is worse than that of electroplating, and the nickel powder cannot be tightly embedded.

In addition, when glue is used for embedding, since the hardness of the superalloy particles is much higher than that of the glue-embedded bonding matrix, direct slicing will come out of the matrix

Finally, in terms of mechanical thinning, block slicing has been used in the past, which takes a long time and has a low yield

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