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Preparation and lossless recovery method of inlaid sample

A recovery method and thermosetting technology, which are applied in the preparation of test samples, cleaning methods using liquids, chemical instruments and methods, etc., can solve the problems of acetone being toxic, flammable, and scarce of samples, and achieve a simple recovery process, Guaranteed integrity and strong design effects

Active Publication Date: 2020-08-07
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are some problems in the above two methods: the mechanical treatment method is easy to destroy the integrity of the sample in the process of removing the mounting material, and there is inevitably the problem of residual mounting material, especially for samples with irregular and porous surfaces. The problem of mosaic material residue is more prominent
Regarding the high-temperature treatment method, firstly, acetone is toxic and flammable, and epoxy vapor is irritating to human skin and mucous membranes during heat treatment; secondly, in the process of removing the mosaic material with a scraper, it is easy to damage the surface of the sample, and For samples with irregular and porous surfaces, it is also difficult to avoid serious residues of mounting materials
For quasi-in-situ experiments, even if multiple samples of the same batch are used, errors will inevitably be introduced; at the same time, if samples are rare or expensive, multi-sample experiments are obviously difficult to achieve

Method used

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  • Preparation and lossless recovery method of inlaid sample
  • Preparation and lossless recovery method of inlaid sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Mix bisphenol A diglycidyl ether and glutaric anhydride uniformly at a molar ratio of 1:1, and then add (2,4,6)-tris(dimethylaminomethyl)phenol at 0.3% of the mass sum of the two , and mix the three evenly to obtain the prepared mosaic material.

[0032] Spray release agent on the inner wall of the mosaic mold, then slowly inject part of the prepared mosaic material into the mosaic mold, then place the cleaned and dried sample to be mosaic in the mosaic mold, and then slowly inject the remaining mosaic material Until the sample is completely submerged; place the mosaic mold in an oven at 130°C under normal pressure for 6 hours to ensure that the mosaic material is completely cured.

[0033] After the observation of the microscopic morphology of the sample is completed, according to the mass ratio of the mounting material and the alcohol small molecule solvent of 1:4, the mounting sample is completely immersed in ethylene glycol, and then the reaction vessel is sealed and ...

Embodiment 2

[0035] Mix bisphenol A diglycidyl ether and glutaric anhydride evenly at a molar ratio of 1:2, and then add (2,4,6)-tris(dimethylaminomethyl)phenol at 2% of the mass sum of the two , and mix the three evenly to obtain the prepared mosaic material.

[0036] Spray release agent on the inner wall of the mosaic mold, then slowly inject part of the prepared mosaic material into the mosaic mold, then place the cleaned and dried sample to be mosaic in the mosaic mold, and then slowly inject the remaining mosaic material Until the sample is completely submerged; place the mosaic mold in an oven at 150°C under normal pressure for 2 hours to ensure that the mosaic material is completely cured.

[0037] After the observation of the microscopic morphology of the sample is completed, according to the mass ratio of the mounting material and the alcohol small molecule solvent of 1:4, the mounting sample is completely immersed in ethylene glycol, and then the reaction vessel is sealed and pla...

Embodiment 3

[0039] Mix bisphenol A diglycidyl ether and glutaric anhydride uniformly at a molar ratio of 1:1, and then add (2,4,6)-tris(dimethylaminomethyl)phenol at 2% of the mass sum of the two , and mix the three evenly to obtain the prepared mosaic material.

[0040] Spray release agent on the inner wall of the mosaic mold, then slowly inject part of the prepared mosaic material into the mosaic mold, then place the cleaned and dried sample to be mosaic in the mosaic mold, and then slowly inject the remaining mosaic material Until the sample is completely submerged; place the mosaic mold in an oven at 130°C under normal pressure for 6 hours to ensure that the mosaic material is completely cured.

[0041] After the observation of the microscopic morphology of the sample is completed, according to the mass ratio of the mounting material and the alcohol small molecule solvent of 1:4, the mounting sample is completely immersed in ethylene glycol, and then the reaction vessel is sealed and ...

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Abstract

The invention discloses a preparation and lossless recovery method of an inlaid sample. The preparation and lossless recovery method comprises the following steps of: inlaying a to-be-inlaid sample bytaking glutaric anhydride cured thermosetting epoxy resin as an inlaying material to finish the preparation of the inlaid sample; performing cutting, grinding, polishing and the like on the inlaid sample according to microstructure observation requirements; and using alcohol micromolecular solvents such as ethylene glycol or propylene glycol to degrade the inlaying material after observing the microstructure of the sample, taking out the sample after fully degrading the inlaying material, cleaning and drying the sample, and realizing the lossless recycling of the sample for standby application. According to the method, mechanical treatment on the sample in a sample recovery process is avoided, and the integrity of the sample is guaranteed; the complete degradation of the inlaying materialcan be realized; and residues of the inlaying material on the surface and inside the sample are effectively avoided.

Description

technical field [0001] The invention belongs to the technical field of mosaic materials, and in particular relates to a preparation and non-destructive recovery method of mosaic samples, which are suitable for sample preparation and sample recovery before and after temperature-resistant (>160°C) material microscopic morphology observation. Background technique [0002] The micro-morphological characteristics of materials greatly affect the performance of materials. At the same time, with the continuous improvement of material processing precision, researchers' demand for observation of material micro-morphology is also increasing. Among them, the use of scanning electron microscopes to observe the microscopic morphology of materials has been widely used in various fields, which is of great significance for improving the material preparation process, exploring the evolution of the microscopic morphology of materials during service, and predicting the service life of materia...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/2202G01N23/2251G01N1/28G01N1/32G01N1/36B08B3/08
CPCB08B3/08G01N1/286G01N1/32G01N1/36G01N23/2202G01N23/2251G01N2001/2873G01N2001/366
Inventor 杨晶晶杨熙娴范学领赵文哲
Owner XI AN JIAOTONG UNIV
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