Method for preparing micron-order nickel-based high-temperature alloy powder transmission electron microscope film sample

Abstract

The invention belongs to the technical field of alloy material preparation and representation, and discloses a method for preparing a micron-order nickel-based high-temperature alloy powder transmission electron microscope film sample. The method comprises the following steps: adding nickel-based alloy powder into an electroplating liquid, and stirring so as to obtain a suspension; putting a cathode nickel piece and an anode nickel piece into the suspension so as to obtain uniform nickel-based alloy powder on the cathode nickel piece; connecting a power supply to implement electroplating, wrapping the nickel-based alloy powder with a nickel plated layer, performing mechanical thinning so as to obtain a circular piece of which the diameter is 3 mm, and further grinding so as to obtain a sample which takes the shape of a wedge in a thickness direction; and pasting the sample at the opening of an opened copper ring, enabling the thin end of the wedge to be close to the opening center of the copper ring, and putting the opened copper ring with the sample into an ion thinning instrument for ion thinning, thereby obtaining a film sample area for transmission electronic microscopy observation. The method provided by the invention has the advantages of being short in time, high in plated layer quality and good in wrapping effect of the nickel-based high-temperature alloy powder.

Description

technical field [0001] The invention belongs to the technical field of preparation and characterization of alloy materials, and in particular relates to a method for preparing a micron-sized nickel-based superalloy powder transmission electron microscope film sample. Background technique [0002] The microscopic analysis of powder materials is an important method to study the structure and properties of powders, and it is a necessary way to further improve the properties of materials. The microstructural analysis of powder materials necessarily involves the preparation of TEM samples. Some powder materials can be prepared by crushing the powder, grinding to make a suspension, and using a supported film dispersion method. 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 materi...

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

Images