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Method for detecting non-metallic inclusions in steel

A technology for non-metallic inclusions and detection methods, which is used in measurement devices, preparation of test samples, and material analysis using measurement secondary emissions. The analysis results are unreliable and other problems, so as to reduce the manual workload and errors caused by manual labor, the detection speed is fast, and the manual workload is reduced.

Pending Publication Date: 2021-07-09
HEBEI IRON AND STEEL
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The main disadvantages of the traditional detection method of non-metallic inclusions combined with electrochemical extraction and field emission scanning electron microscopy are: 1. The electrolyte uses acidic or alkaline solutions. During the electrolysis process, the electrolyte will dissolve part of the oxides. 2. Carbide is difficult to remove for electrolytic samples that have not undergone solid solution treatment; 3. Field emission scanning electron microscopy detects inclusions, the analysis speed is slow, the manual working measuring tool is large, and there are no inclusions in 99% of the field of view that need to be judged manually Inclusions, 100mm 2 The scanning time of the detection area is about 10 hours; 4. The analysis results are unreliable, the field emission electron microscope is a static scanning, the analysis is that the collected pictures are not the actual samples, and the inclusions and pollutants cannot be effectively distinguished

Method used

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  • Method for detecting non-metallic inclusions in steel
  • Method for detecting non-metallic inclusions in steel
  • Method for detecting non-metallic inclusions in steel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1: The detection method of non-metallic inclusions in Benxi Steel is as follows.

[0040] (1) After the GCr15 bearing steel sample to be tested is solid-solution strengthened at 1000°C, it is made into a rod-shaped sample; the stainless steel sleeve is used as the cathode, the rod-shaped sample is used as the anode, and the cellulose acetate semi-permeable membrane is used to isolate it. / cm 2 Electrolytic extraction is performed under a constant current; the proportion of the electrolyte is: tetramethylammonium chloride 0.01g / ml, acetylacetone 0.1ml / ml, and the rest is 99wt% methanol solution.

[0041] (2) Dissolve the electrolyte solution after electrolysis in absolute ethanol, and filter it with a 1um polypropylene microporous membrane; the inclusions on the filter membrane are dissolved again in absolute ethanol solution, and pass through 500Gs, 1000GS, 1500GS , 2000GS, 2500GS, 3000GS and 3500GS magnetic separation, filter with 1um polypropylene microporous...

Embodiment 2

[0045]Example 2: The detection method of non-metallic inclusions in Benxi Steel is as follows.

[0046] (1) After the 60Si2Mn spring steel sample to be tested is solid-solution strengthened at 1000°C, it is made into a rod-shaped sample; the stainless steel sleeve is used as the cathode, the rod-shaped sample is used as the anode, and the cellulose acetate semi-permeable membrane is used to isolate it. / cm 2 Electrolytic extraction is performed under a constant current; the proportion of the electrolyte is: tetramethylammonium chloride 0.01g / ml, acetylacetone 0.1ml / ml, and the rest is 99wt% methanol solution.

[0047] (2) Dissolve the electrolyte solution after electrolysis in absolute ethanol, and filter it with a 1um polypropylene microporous membrane; the inclusions on the filter membrane are dissolved again in absolute ethanol solution, and pass through 500Gs, 1000GS, 1500GS , 2000GS, 2500GS, 3000GS and 3500GS magnetic separation, filter with 1um polypropylene microporous...

Embodiment 3

[0051] Example 3: The detection method of non-metallic inclusions in the steel is as follows.

[0052] (1) After the GCr15 bearing steel sample to be tested is solid-solution strengthened at 1100°C, it is made into a rod-shaped sample; the stainless steel sleeve is used as the cathode, the rod-shaped sample is used as the anode, and the cellulose acetate semi-permeable membrane is used to isolate it. / cm 2 Electrolytic extraction is performed under a constant current; the proportion of the electrolyte is: tetramethylammonium chloride 0.05g / ml, acetylacetone 0.25ml / ml, and the rest is 95wt% methanol solution.

[0053] (2) Dissolve the electrolyte solution after electrolysis in absolute ethanol, and filter it with a 1um polypropylene microporous membrane; the inclusions on the filter membrane are dissolved again in absolute ethanol solution, and pass through 500Gs, 1000GS, 1500GS , 2000GS, 2500GS, 3000GS and 3500GS magnetic separation, filter with 1um polypropylene microporous ...

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Abstract

The invention discloses a method for detecting non-metallic inclusions in steel, which adopts the following process: carrying out solid solution strengthening on a sample to be detected to prepare a rod-shaped sample; taking a stainless steel sleeve as a cathode, taking a rod-shaped sample as an anode, and performing electrolytic extraction by adopting a semipermeable membrane for isolation, wherein the electrolyte comprises the following components in proportion: 0.01 g / ml-0. 1 g / ml of tetramethylammonium chloride, 0.1 ml / ml-0. 25 ml / ml of acetylacetone and the balance of a methanol solution with the mass fraction of 95%-99%; dissolving the electrolyzed electrolyte in absolute ethyl alcohol, and filtering by using a filter membrane; dissolving the inclusions on the filter membrane in the absolute ethyl alcohol solution again, and obtaining clean inclusions after magnetic separation and filtering; inlaying clean inclusions on a metal plane with a conductive adhesive, and spraying platinum to prepare an ASPEX observation sample; and detecting the ASPEX observation sample by using an ASPEX automatic scanning electron microscope to obtain detection information of all extracted inclusions. According to the method, the non-metallic inclusions in the steel can be nondestructively, completely and quickly detected, and the manual workload and errors caused by manual work are greatly reduced.

Description

technical field [0001] The invention belongs to the field of electrochemical and physical detection, in particular to a method for detecting non-metallic inclusions in steel. Background technique [0002] Many studies have shown that the type, size, distribution and quantity of non-metallic inclusions in steel have a great influence on the quality of steel. Non-metallic inclusions destroy the continuity of the steel matrix structure, can reduce the mechanical properties and fatigue properties of the steel, and deteriorate the cold and hot workability and some physical and chemical indicators of the steel. Accurate and complete characterization of non-metallic inclusions in steel is particularly important to improve the cleanliness of steel. [0003] The main disadvantages of the traditional detection method of non-metallic inclusions combined with electrochemical extraction and field emission scanning electron microscopy are: 1. The electrolyte uses acidic or alkaline solut...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/04G01N23/22G01N23/2202G01N1/34G01N1/40
CPCG01N23/04G01N23/22G01N23/2202G01N1/34G01N1/4077G01N2001/4088
Inventor 马超齐建军陈红卫田志强张洪起
Owner HEBEI IRON AND STEEL
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