Preparation method of N-standard sample suitable for electron probe analysis

An electronic probe, standard sample technology, applied in the direction of using wave/particle radiation for material analysis, analysis of materials, measurement devices, etc. problem, to achieve the effect of improving accuracy and good development prospects

Pending Publication Date: 2021-07-20
WUHAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently such standards are lacking due to the high volatility of N and the complexity of the Fe-N phase diagram
It is very difficult to prepare stable Fe-N bulk samples by traditional metallurgical methods while ensuring a single internal phase

Method used

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  • Preparation method of N-standard sample suitable for electron probe analysis
  • Preparation method of N-standard sample suitable for electron probe analysis
  • Preparation method of N-standard sample suitable for electron probe analysis

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preparation example Construction

[0038] The invention provides a method for preparing an N-standard sample suitable for electron probe analysis, which includes preparing Fe-N alloy samples with different N contents and detecting the prepared standard sample. Specifically include:

[0039] S1. With Fe micropowder and Fe-N compound (the main constituent phase is Fe 4 N or Fe 3 N 1.3 , containing a small amount of Fe) micropowder as raw material, weighing, ball milling and drying according to different N content ratios, to obtain a mixed powder with a mass fraction of N of 0.5-2.0wt.%; 4 N and Fe 3 N 1.3 The compound is used as the starting material, and it is bottled for later use after being dried. Wherein, the N content in the Fe-N compound is determined in advance by using an oxygen, nitrogen and hydrogen combined detector (equipment model: Leco, ONH836).

[0040] The specific method of mixing powder with N content of 0.5-2.0wt.% is as follows: according to the mass fraction of the required standard sa...

Embodiment 1

[0059] The present embodiment provides the N-standard sample whose N content is 0.5-2.0wt%, and its preparation method comprises the following steps:

[0060] Choose Fe powder and Fe 4 N powder is mixed, wherein the N content is set to 0.5, 1.0, 1.5 and 2.0wt% in turn; about Fe 4 For N powder, use an oxygen, nitrogen and hydrogen combined detector (equipment model: Leco, ONH836) to determine the N content in it in advance, and use this as a basis to carry out the above powder mixing scheme.

[0061] Mixed powders with different N contents were ball milled and mixed with absolute alcohol as a dispersant for at least 10 hours, and then placed in a vacuum drying oven with a beaker holder for drying. The drying temperature was set at 100°C for 3 hours. The powders of different components are each 50g after drying.

[0062] Put the dried powders of each component into the mold respectively, use a powder press machine to shape it, seal the sample with a metal molybdenum container,...

Embodiment 2

[0067] This example provides Fe 4 The N-standard sample of N as main phase, its preparation method comprises the following steps:

[0068] Among the embodiment 1, use the oxygen, nitrogen and hydrogen combined detector to detect (equipment model: Leco, ONH836) to determine the content of N in the form of Fe 4 The N-based powder was fully dried in a vacuum oven for 3 hours at a drying temperature of 100°C. Then put it in a mold, use a powder tablet press to shape it, and seal it with a metal molybdenum container, then put it in a dry box for high-pressure sintering. Wherein, the original sample is a cylindrical sample with a diameter of 11-14 mm and a thickness of 1 mm-3.5 mm.

[0069] Put the sealed tablet into a six-sided top large chamber press for high-temperature sintering. Among them, the temperature and pressure of the six-sided top chamber are set to 1100°C and 5GPa. The holding time is 1 hour.

[0070] The samples were polished sequentially on 400, 800, 1500, and ...

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Abstract

The invention relates to a preparation method of an N-standard sample suitable for electron probe analysis, which is suitable for an iron-based alloy system. According to the method, mixed micro powder of iron nitride and metal iron is used as an initial raw material, ultrahigh pressure is used as an auxiliary sintering condition, and a Fe-N blocky sample is obtained through a solid-phase reaction method. According to the method, the X-ray diffraction technology is used for firstly confirming that a sample is composed of a single phase, meanwhile, lattice parameters of phase crystals are obtained, and the N content is determined according to the corresponding relation between the lattice parameters and the N content. Electronic probe quantitative analysis is carried out on element distribution of the sample, and it is proved that distribution of the N element is completely uniform. The invention further proves and establishes a linear relationship between N percentage content and probe signal strength. The linear relationship shows that the Fe-N sample prepared by the method can be used as a standard sample for analyzing the content of the electronic probe N element, and is applied to quantitative analysis of the N element of an iron-based alloy system, especially the field of steel.

Description

technical field [0001] The invention relates to the technical field of electronic probe micro-area analysis, in particular to a method for preparing an N-standard sample for electronic probe micro-area analysis, and the N-standard sample prepared by the method can be applied to the N element in an iron-based alloy system Electron probe quantitative analysis, especially in the field of steel. Background technique [0002] With the development of the iron and steel industry in recent years, N element has received more and more attention as a new alloy element, because N is a strong austenite stable element, which can form room temperature austenite when dissolved in the Fe lattice. Tensitic structure not only enhances the hardness of steel, but also improves its fracture toughness and corrosion resistance. As an alloying element, N can form different phases with Fe, including Fe-N compounds and solid solutions. The phase composition and its distribution characteristics large...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/2202G01N23/223
CPCG01N23/2202G01N23/223
Inventor 胡晓军郎雪婵张新新熊婧宜杨帆
Owner WUHAN UNIV OF TECH
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