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CN-121978135-A - Electron microscopic analysis method for hydrogen distribution in nanoscale resolution metal material

CN121978135ACN 121978135 ACN121978135 ACN 121978135ACN-121978135-A

Abstract

The application relates to an electron microscopic analysis method for hydrogen distribution in a nanoscale resolution metal material, and belongs to the technical field of transmission electron microscope microscopic analysis. The electron microscopic analysis method of the hydrogen distribution in the nano-scale resolution metal material comprises the steps of carrying out pixel point scanning acquisition on a region to be detected of a sample to be detected to obtain an electron energy loss spectrum data set P ij , carrying out zero loss peak centering treatment to obtain an electron energy loss spectrum data set A ij , carrying out peak intensity standardization treatment to obtain an electron energy loss spectrum data set N ij , selecting a plasma peak signal spectral line in N ij to obtain a plasma peak signal spectral line data set E ij , carrying out Gaussian smoothing treatment to obtain a plasma peak signal spectral line data set S ij , reading a peak position value of the plasma peak signal spectral line in S ij , carrying out two-dimensional imaging by adopting gray level imaging, and reflecting the hydrogen absorption degree by using an image gray level to obtain the hydrogen distribution microscopic information in a metal material transmission electron microscope image. The application can obtain the hydrogen distribution image with nanoscale high spatial resolution in the metal material.

Inventors

  • Zou Chengqin
  • Shen Huahai
  • LI MUHONG
  • QI LIN
  • ZHOU XIAOSONG

Assignees

  • 中国工程物理研究院核物理与化学研究所

Dates

Publication Date
20260505
Application Date
20260317

Claims (10)

  1. 1. An electron microscopic analysis method of hydrogen distribution in a nano-scale resolution metal material, comprising: Loading a sample to be tested in a transmission electron microscope, wherein the sample to be tested is made of a metal material; Selecting an electron energy loss spectrum surface acquisition mode, and carrying out pixel point scanning acquisition on a region to be detected of the sample to be detected to obtain an original electron energy loss spectrum data set P ij , wherein the region to be detected is a region where a crystal boundary is located, a region where a phase boundary is located or a region where a hole interface is located; Zeroing an electron energy loss spectrum zero loss peak corresponding to each pixel point in the electron energy loss spectrum data set P ij to obtain a centered electron energy loss spectrum data set A ij ; Taking a plasma peak with the peak position range of the plasma peak of the electron energy loss spectrum of 15 eV-23 eV as a reference peak, and carrying out intensity normalization treatment on the plasma peak of each spectral line in the electron energy loss spectrum data set A ij to obtain an electron energy loss spectrum data set N ij after peak intensity normalization treatment; Selecting a plasma peak signal spectrum line with the range of the peak position value of the plasma peak of the electron energy loss spectrum from 15eV to 23eV from the electron energy loss spectrum data set N ij , and extracting to obtain a plasma peak signal spectrum line data set E ij ; Carrying out Gaussian smoothing on the plasma peak signal spectral line dataset E ij to obtain a plasma peak signal spectral line dataset S ij after Gaussian smoothing; And reading the peak position value of the plasma peak signal spectral line in the plasma peak signal spectral line data set S ij , performing two-dimensional imaging by adopting gray level imaging, and reflecting the hydrogen absorption degree by using the gray level value of the image to obtain the hydrogen distribution microscopic information in the metal material transmission electron microscope image.
  2. 2. The method of electron microscopic analysis of hydrogen distribution in a nano-scale resolution metallic material according to claim 1, wherein the transmission electron microscope optical path is set to a scanning transmission dark field image mode.
  3. 3. The electron microscopic analysis method of hydrogen distribution in a nano-scale resolution metal material according to claim 1, wherein the acquisition step length of the electron energy loss spectrum acquisition mode is 1 nm-50 nm, and the acquisition time of the electron energy loss spectrum acquisition mode to the pixel point is 0.5 s-2 s.
  4. 4. The method according to claim 1, wherein before the scanning acquisition, a camera length, a condenser aperture, and an electron energy loss spectrum receiving aperture are set, and an electron beam is moved into a rear barrel imaging filter, and a receiving aperture angle is set.
  5. 5. The method for electron microscopic analysis of hydrogen distribution in a nano-scale resolution metal material according to claim 4, wherein the camera length is 29.5mm to 58mm.
  6. 6. The electron microscopic analysis method of hydrogen distribution in nano-scale resolution metal material according to claim 4, wherein the aperture size of the condenser diaphragm is 20 μm to 70 μm.
  7. 7. The method of electron microscopic analysis of hydrogen distribution in a nano-scale resolution metallic material according to claim 4, wherein the electron energy loss spectrum receiving diaphragm aperture is 2.5mm.
  8. 8. The electron microscopic analysis method of hydrogen distribution in a nano-scale resolution metal material according to claim 4, wherein the receiving aperture angle is 12.78 mrad-25.12 mrad.
  9. 9. The electron microscopic analysis method of hydrogen distribution in a nano-scale resolution metal material according to any one of claims 1 to 8, wherein the thickness of the sample to be measured is 50nm to 100nm.
  10. 10. The electron microscopic analysis method for hydrogen distribution in the nanoscale resolution metal material according to claim 9, wherein the preparation method of the sample to be detected comprises the steps of preparing a transmission electron microscope sample with the thickness of 150-200 nm by adopting a focusing ion beam microscope, and then thinning the thickness of the transmission electron microscope sample to 50-100 nm by adopting a microbeam fixed-point ion thinning system.

Description

Electron microscopic analysis method for hydrogen distribution in nanoscale resolution metal material Technical Field The application relates to the technical field of transmission electron microscope microscopic analysis, in particular to an electron microscopic analysis method for hydrogen distribution in a nanoscale resolution metal material. Background The metal material has important application value in the hydrogen storage field and the nuclear energy field, and can form metal hydride by hydrogen absorption so as to realize hydrogen storage, while the metal material in the nuclear energy field can cause hydrogen embrittlement failure due to hydrogen permeation in a hydrogen environment. The analysis of the hydrogen distribution in the metal material can provide important information for the hydrogen diffusion reaction mechanism and the hydrogen distribution characteristics in the hydrogen storage metal or nuclear energy metal material, and has important application prospects in the fields of metal material hydrogen absorption mechanism research, hydrogen embrittlement resistant material design and the like. Currently, analysis techniques for hydrogen distribution in metallic materials mainly include Secondary Ion Mass Spectrometry (SIMS), three-dimensional Atomic Probe Tomography (APT), reflected Electron Energy Loss Spectroscopy (REELS), and the like. SIMS is analyzed by ion etching samples point by point from surface to bulk phase, with spatial resolution typically on the order of hundred nanometers. On one hand, APT requires to make a sample into a needle point, so that the difficulty of sample preparation is increased, and on the other hand, the needle point processing accelerates the hydrogen loss in the original hydrogen-containing metal sample, so that analysis errors are caused. REELS is mainly used for the surface chemistry and adsorption research of solid samples, and the spatial resolution is only up to the micron level. Therefore, the technology for analyzing the hydrogen distribution in the metal material still has the problems of insufficient spatial resolution and large analysis error introduced by needle tip sample preparation, and the nanoscale microscopic analysis of the hydrogen distribution in the metal material is difficult to realize due to the extremely small atomic number of hydrogen elements, so that the research on the aspects of hydrogen diffusion paths, hydrogen interface distribution characteristics, hydrogen absorption uniformity, hydrogen absorption mechanisms and the like in the metal material is limited. Therefore, it is necessary to develop an electron microscopic analysis method of hydrogen distribution in a nano-scale resolution metal material to realize nano-scale microscopic analysis of hydrogen distribution in the metal material. Disclosure of Invention The application aims to provide an electron microscopic analysis method for hydrogen distribution in a nanoscale resolution metal material, which aims to solve the technical problem that the analysis of a hydrogen diffusion path, hydrogen interface distribution characteristics, hydrogen absorption uniformity or a hydrogen absorption reaction mechanism in the metal material is inaccurate because the hydrogen distribution in the metal material cannot be accurately distinguished. The application provides an electron microscopic analysis method of hydrogen distribution in a nanoscale resolution metal material, which comprises the steps of loading a sample to be detected in a transmission electron microscope; the sample to be measured is a metal material; selecting an electron energy loss spectrum surface acquisition mode, and carrying out pixel point scanning acquisition on a region to be detected of a sample to be detected to obtain an original electron energy loss spectrum data set P ij; the method comprises the steps of determining a region to be measured as a region where a grain boundary is located, a region where a phase boundary is located or a region where a hole interface is located, i represents the number of rows where pixel points are located, j represents the number of columns where pixel points are located, i and j are positive integers greater than or equal to 1, zeroing an electron energy loss spectrum zero loss peak corresponding to each pixel point in an electron energy loss spectrum data set P ij to obtain a centrally processed electron energy loss spectrum data set A ij, performing intensity normalization processing on each spectral line plasma peak in the electron energy loss spectrum data set A ij by taking a plasma peak with the peak value range of 15 eV-23 eV as a reference peak, obtaining an electron energy loss spectrum data set N ij after peak intensity normalization processing, selecting a plasma peak with the peak value range of 15 eV-23eV in the electron energy loss spectrum data set N ij, extracting a plasma peak signal data set E ij, performing imaging on the plasma peak with the peak