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Method for preparing FeSe-based superconducting material

A technology of superconducting materials and ball-to-material ratio, which is applied in the field of superconducting material preparation, can solve the problems that the superconducting phase is difficult to achieve Unicom, does not have superconducting performance, and the material has low current-carrying performance, so as to shorten the time required for ball milling , reduce the original particle size, and repeatable results

Active Publication Date: 2014-10-08
NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The main problem in the preparation process of FeSe-based superconducting materials is: because FeSe has two crystal structures, one is the hexagonal phase, in which the ratio of Fe:Se is slightly lower than 1:1, and the hexagonal phase is limited by the structure. FeSe does not have superconducting properties; the other is tetragonal phase, in which -FeSe- is distributed in lamellar form, that is, it becomes a superconducting layer structure similar to -FeAs- and -CuO-, therefore, at around 8K superconducting transition
But this method not only consumes a large amount of energy, but also the best tetragonal phase content can only reach below 80%
In this case, it is difficult for the superconducting phase to achieve Unicom, and the current-carrying performance of the material is low

Method used

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  • Method for preparing FeSe-based superconducting material
  • Method for preparing FeSe-based superconducting material
  • Method for preparing FeSe-based superconducting material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Step 1. In a glove box full of inert gas, place the mixed powder in a vacuum ball mill jar, then seal the vacuum ball mill jar and take it out; the mixed powder is made of iron powder and selenium powder with a molar ratio of 1.15:1 composition, the iron powder is reduced iron powder, the mass purity of the iron powder is not less than 99%, and the mass purity of the selenium powder is not less than 99%;

[0035] Step 2. Place the vacuum ball milling tank containing the mixed powder in step 1 in a high-energy ball mill for high-energy ball milling. The specific process is:

[0036] Step 201: Under the condition that the rotational speed of the high-energy ball mill is 1740r / min, the mixed powder is subjected to high-energy ball milling for 20 minutes, and then the vacuum ball mill tank is taken out and soaked in liquid nitrogen until the mixed powder is cooled below 0°C; the high-energy ball mill The ball-to-material ratio of processing is 1:4;

[0037] Step 202, repea...

Embodiment 2

[0044] Step 1. In a glove box full of inert gas, place the mixed powder in a vacuum ball mill jar, then seal the vacuum ball mill jar and take it out; the mixed powder is composed of iron powder and selenium powder with a molar ratio of 1.25:1 composition, the iron powder is reduced iron powder, the mass purity of the iron powder is not less than 99%, and the mass purity of the selenium powder is not less than 99%;

[0045] Step 2. Place the vacuum ball milling tank containing the mixed powder in step 1 in a high-energy ball mill for high-energy ball milling. The specific process is:

[0046] Step 201: Under the condition that the rotational speed of the high-energy ball mill is 1800r / min, the mixed powder is subjected to high-energy ball milling for 15 minutes, and then the vacuum ball mill tank is taken out and soaked in liquid nitrogen until the mixed powder is cooled below 0°C; the high-energy ball mill The ratio of ball to material to be processed is 1:6;

[0047] Step 2...

Embodiment 3

[0052] Step 1. In a glove box full of inert gas, place the mixed powder in a vacuum ball mill jar, then seal the vacuum ball mill jar and take it out; the mixed powder is made of iron powder and selenium powder with a molar ratio of 0.9:1 composition, the iron powder is reduced iron powder, the mass purity of the iron powder is not less than 99%, and the mass purity of the selenium powder is not less than 99%;

[0053] Step 2. Place the vacuum ball milling tank containing the mixed powder in step 1 in a high-energy ball mill for high-energy ball milling. The specific process is:

[0054] Step 201. Under the condition that the rotational speed of the high-energy ball mill is 1500r / min, the mixed powder is subjected to high-energy ball milling for 30 minutes, and then the vacuum ball mill tank is taken out and soaked in liquid nitrogen until the mixed powder is cooled below 0°C; the high-energy ball mill The ratio of ball to material to be processed is 1:10;

[0055] Step 202, ...

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Abstract

The invention discloses a method for preparing a FeSe-based superconducting material. The method comprises the following steps: 1, putting mixed powder of iron powder and selenium powder into a vacuum ball-milling tank; 2, performing high energy ball-milling treatment on the mixed powder; 3, pressing the mixed powder to obtain a FeSe-base blank; and 4, sintering the FeSe-base blank, thereby obtaining the FeSe-based superconducting material. According to the method disclosed by the invention, a high energy ball-milling machine is adopted to perform high energy ball-milling treatment on the mixed powder within a relatively short time firstly, after the sizes of original grains of the mixed powder are reduced, a Fe-Se solid solution is obtained, Fe and Se in the mixed powder reach atom-grade mixing, the limit on reaction rate in the dispersion process in the sintering treatment is eliminated, the mixed powder is laminated and is subsequently sintered, thereby obtaining the FeSe-based superconducting material with high superconducting phase content and advantages of small energy consumption, short process, high repeatability and the like.

Description

technical field [0001] The invention belongs to the technical field of preparation of superconducting materials, and in particular relates to a preparation method of FeSe-based superconducting materials. Background technique [0002] In 2008, LaO with a critical temperature of 26K was first reported by the Japanese Hosono research group. 1-x f x FeAs, followed by Fe-based high-temperature superconducting materials (FHS) developed rapidly. At present, four main systems have been developed, namely "1111" system (such as LaFeAsOF), "122" system (such as BaFe 2 As 2 ), "111" system (such as LiFeAs) and "11" system (such as FeSe). Similar to the high-temperature copper oxide superconductor (HTS), the crystal structure of FHS is a layered structure, with -FeAs-layer (or -FeSe-layer) as the superconducting layer. [0003] There are three main reasons for the rapid development of FHS. First, it is generally believed that the magnetism of Fe has a destructive effect on electron ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/547C04B35/626H10N60/01
Inventor 李成山张胜楠马小波王亚林
Owner NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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