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An element grain boundary segregation semi-quantitative method based on a scanning electron microscope

A technology of grain boundary segregation and scanning electron microscopy, which is applied in the direction of measuring devices, analyzing materials, and using wave/particle radiation for material analysis, etc., can solve the problems of inability to define grains, quantitative analysis, and low resolution, and achieve easy operation, The effect of simple characterization process and convenient sample preparation

Inactive Publication Date: 2018-09-25
SHANGHAI UNIV
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  • Application Information

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Problems solved by technology

However, due to the expansion of the electron beam inside the sample in SEM, the resolution is low. If the EDS point analysis is performed on the grain boundary, the obtained point data contains the composition information of the adjacent grains, which cannot be simply analyzed. Qualitative and quantitative analysis of grain boundaries, which has become an urgent technical problem to be solved

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  • An element grain boundary segregation semi-quantitative method based on a scanning electron microscope
  • An element grain boundary segregation semi-quantitative method based on a scanning electron microscope
  • An element grain boundary segregation semi-quantitative method based on a scanning electron microscope

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Embodiment 1

[0023] The filled-type skutterudite thermoelectric materials prepared by traditional fusion annealing combined with plasma sintering method SPS, according to the different annealing time, the samples with annealing time of 1 day, 3 days and 7 days were respectively named as sample 1, sample 2 and Sample 3, as a material sample.

[0024] In this embodiment, a semi-quantitative method for grain boundary segregation of elements based on scanning electron microscopy comprises the following steps:

[0025] a. Sample preparation: first cut the material sample into small pieces, then grind and polish the surface of the sample on diamond sandpaper with a particle size of 6 μm, 3 μm, 1 μm and 0.5 μm in turn, and finally polish it into a mirror surface, before putting it into the SEM sample chamber Perform plasma cleaning on the sample to remove the surface contamination of the material sample and obtain a clean sample;

[0026] b. Semi-quantitative analysis of the energy spectrum at t...

Embodiment 2

[0055] This embodiment is basically the same as Embodiment 1, especially in that:

[0056] A single crystal of quasi-skutterudite structure was prepared by flux growth method as a material sample. A scanning electron microscope-based semiquantitative method for elemental grain boundary segregation was employed. The method includes sample preparation and energy spectrum analysis at the grain boundary, according to the public The amount of segregation at the grain boundary is obtained, where the solid solution values ​​of the segregation elements at the grain boundary and within the grain are defined respectively N r b is the bit density of the reference element, and the electron beam spot diameter d can be obtained by simulating the Monte Carlo electron trajectory with the software Casino 1 , and then according to the announcement The chemical breadth of segregated elements at grain boundaries can be obtained. The invention realizes semi-quantitative grain boundary seg...

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Abstract

An element grain boundary segregation semi-quantitative method based on a scanning electron microscope is disclosed. The method includes sample preparation, energy spectrum analysis at a grain boundary, and acquisition of a segregation amount at the grain boundary according to an equation shown in the description. Segregation element solid solution values at the grain boundary and in crystal grains are defined respectively in the description. N<r> is the number density of a reference element. The diameter d1 of an electron beam spot can be obtained by Monte Carlo electron trajectory simulation with software Casino, and the chemical width of the segregation element at the grain boundary can be obtained according to an equation shown in the description. The method achieves semi-quantitative analysis of grain boundary segregation under the platform of the scanning electron microscope and has advantages of simple sample preparation, relatively easy operation, and the like. In the method, an energy spectrum is collected at the grain boundary through the scanning electron microscope, and contribution of crystal grains is deducted from the grain boundary energy spectrum to obtain chemical component information at the grain boundary. The method can be widely applied in the technical field of material characterization.

Description

technical field [0001] The invention relates to a method for measuring and analyzing chemical composition information at grain boundaries, in particular to a method for measuring and analyzing chemical composition information at grain boundaries under the platform of a scanning electron microscope, which is applied to the technical field of material characterization. Background technique [0002] The structure and composition of grain boundaries have an important impact on the properties of materials. For metal materials, the intergranular fracture, corrosion, diffusion and segregation in the material will be affected by the grain boundary structure and grain boundary characteristics; for thermoelectric materials, atoms on the grain boundary can effectively increase phonon scattering and reduce thermal conductivity. , to improve performance. To gain an in-depth understanding of the dependence between material properties and grain boundaries, it is necessary to measure the c...

Claims

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Application Information

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IPC IPC(8): G01N23/2202G01N23/2251
CPCG01N23/2202G01N23/2251
Inventor 邢娟娟梅静顾辉胡冬力姜颖胡添翼
Owner SHANGHAI UNIV
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