A method for preparing hot-dip coating transmission samples by reduction-oxidation delamination method

Abstract

A method for preparing hot-dip coating transmission samples by reduction-oxidation delamination method, taking steel plates and putting them into a hot-dip galvanizing simulator after pickling and alkali washing; in the annealing stage, the steel plates are firstly subjected to reduction treatment, and after reduction, the steel plates are subjected to oxidation treatment , and then immersed in the hot-dip bath, after the hot-dip bath, use an air knife to purge to obtain a hot-dip-coated steel plate; Fold, the coating will be separated from the substrate automatically, use tweezers and other tools to remove the coating; transmission sample preparation. Compared with the prior art, the beneficial effects of the present invention are: the present invention provides a method for preparing hot-dip coating transmission samples by reduction-oxidation delamination method, the sample preparation method is simple, and the complete information of the coating can be obtained in the transmission electron microscope . The sample prepared by the method completely reproduces the organization, structure and composition of the coating after the hot-dip process.

Description

technical field [0001] The invention relates to the field of hot-dip coating technology and transmission detection, in particular to a method for preparing a hot-dip coating transmission sample by a reduction-oxidation delamination method. Background technique [0002] The magnification of the transmission electron microscope can reach more than 50,000 times, and the extremely microscopic characteristics and components of the tested sample can be clearly seen, which plays a vital role in the analysis and research of the macroscopic properties of the material, but because the sample needs to be sufficiently thin So that the rays can penetrate the sample, so the preparation of the sample by transmission electron microscope has always been a difficult problem, especially for the observation of the coating sample. Taking the hot-dip coating as an example, the thickness of the coating is often several microns to tens of microns, which needs to be combined with the coating for max...

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Problems solved by technology

[0005] However, this method is greatly affected by the properties of the glue and the sample, especially during the mechanical grinding process. Since the final thickness of the grinding is generally 30 to 100 microns, the sample is in a thin film state at this time, and its resistance to deformation is very poor. Although the glue has been cured, it is very brittle, especially in the film state, it is very easy to break

In order to prevent the sample from detaching from the copper tube, some researchers used the method of resin embedding, but in the case of extremely thin, the cured resin is also relatively brittle, and it is easy to be brittle under the action of mechanical force (pressure and friction). to break the sample out of the copper ring

In the process of ion thinning, there is a large performance difference between the adhesive, resin material and coating material, and the adhesive is easy to fall off in pieces, causing the two combined samples to separate, or the thin area is concentrated at the adhesive, and the There are no thin areas on the sample to be observed, which cannot be observed under the TEM

Therefore, the sample preparation success rate of this method is low, and the sample thin area is less

[0006] Patent CN 102323119 A discloses a method for preparing rust layer samples, which mainly adopts welding and liquid silver sealing means. The performance of liquid silver is different from the rust layer, especially when preparing very thin transmission samples, no matter whether it is grinding Or ion thinning, the difference in performance will cause different forms of damage to the silver and rust layers (that is, two materials with different properties). Once the main substance to be observed is ground off in advance or the ion thinning disappears, it will have a great impact on the test. Big

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