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A kind of method for preparing iron-selenium superconductor

A technology of superconductor and iron selenium, applied in the direction of binary selenium/tellurium compound, metal selenide/telluride, nanotechnology, etc., to achieve the effect of simple process and low cost

Active Publication Date: 2020-12-18
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Using soluble selenium and iron precursors as raw materials, a β-FeSe superconductor with superconductivity was synthesized at low temperature by solvothermal method. This method of preparing β-FeSe superconductor through chemical solution has not been reported.

Method used

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  • A kind of method for preparing iron-selenium superconductor
  • A kind of method for preparing iron-selenium superconductor
  • A kind of method for preparing iron-selenium superconductor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Mix selenium powder (1mmol), polyvinylpyrrolidone (60mg), sodium hydroxide (11mmol) and ethylene glycol (10ml), seal the reaction kettle and heat it to 433K, and keep it warm for 3 hours to obtain a selenium-ethylene glycol solution . Ferrous sulfate (0.75mmol) and ethylene glycol (10ml) were mixed and ultrasonically dissolved to obtain an iron-ethylene glycol solution. Mix the selenium-containing ethylene glycol solution and the iron-containing ethylene glycol solution, seal them in a 50ml solvothermal reaction kettle under a nitrogen atmosphere, heat the reaction kettle to 493K, and keep it warm for 24 hours to obtain β-FeSe nanosheets. The β-FeSe nanosheets were centrifuged and washed 3 times with absolute ethanol, dried in vacuo, and stored in vacuo.

[0025] The crystal structure of the product was determined by x-ray diffraction, and the phase was determined to be β-FeSe with a tetragonal crystal structure, such as figure 1 shown. Its scanning electron microsco...

Embodiment 2

[0027] Selenium powder (0.5mmol), polyvinylpyrrolidone (50mg), cetyltrimethylammonium bromide (5mg), sodium hydroxide (5.5mmol) and ethylene glycol (10ml) were mixed, and the reaction kettle was sealed and heated to 433K, and keep it warm for 3 hours to obtain a selenium-ethylene glycol solution. Ferrous sulfate (0.375mmol) and ethylene glycol (10ml) were mixed and ultrasonically dissolved to obtain an iron-ethylene glycol solution. Mix the selenium-containing ethylene glycol solution and the iron-containing ethylene glycol solution, seal them in a 50ml solvothermal reaction kettle under a nitrogen atmosphere, heat the reaction kettle to 433K, and keep it warm for 12 hours, then heat it to 493K, and keep it warm After 72 hours, β-FeSe nanosheets were obtained. The β-FeSe nanosheets were centrifuged and washed 3 times with absolute ethanol, dried in vacuo, and stored in vacuo.

[0028] Transmission electron microscope (TEM) photos, high-resolution transmission electron micros...

Embodiment 3

[0030]Selenium powder (0.5mmol), cetyltrimethylammonium bromide (35mg), sodium hydroxide (5.5mmol) and ethylene glycol (10ml) were mixed, and the reaction kettle was sealed and heated to 433K, and kept for 3 hours , to obtain a selenium-ethylene glycol solution. Ferrous sulfate (0.375mmol) and ethylene glycol (10ml) were mixed and ultrasonically dissolved to obtain an iron-ethylene glycol solution. Mix the selenium-containing ethylene glycol solution and the iron-containing ethylene glycol solution, seal them in a 50ml solvothermal reaction kettle under a nitrogen atmosphere, heat the reaction kettle to 513K, and keep it warm for 24 hours to obtain β-FeSe nanosheets. The β-FeSe nanosheets were centrifuged and washed 3 times with absolute ethanol, dried in vacuo, and stored in vacuo.

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Abstract

The present invention provides a method for preparing an iron selenium (beta-FeSe) superconductor having a tetragonal crystal structure, soluble iron and selenium precursors as raw materials are mixedwith an appropriate amount of a reducing organic solvent, sodium hydroxide and a surfactant in a reactor. After being sealed in an oxygen-free environment, the mixture is heated to reaction temperature and held for a certain period of time to obtain a superconductive beta-FeSe superconducting nanosheet. The method has the advantages of simple process, low preparation temperature, short reaction time, and non-toxic and harmless raw materials, and is capable of synthesizing a tetragonal crystal structure beta-FeSe sheet superconducting material with a thickness of 10-200 nm and a side length of500 nm to about 10 mu m. The tetragonal crystal structure beta-FeSe sheet superconducting material can be used to prepare nanoscale superconducting devices.

Description

technical field [0001] The invention belongs to the field of inorganic functional nanometer materials, and in particular relates to a method for preparing iron-selenide superconductors. Background technique [0002] Among FeSe binary compounds, the NiAs-type FeSe high-temperature phase with a hexagonal crystal structure is a magnetic semiconductor material, while the PbO-type β-FeSe low-temperature phase with a tetragonal crystal structure is an Fe-based superconducting material. Since β-FeSe superconductor has the simplest crystal structure among iron-based superconductors, it is very important to understand the relationship between the structure of iron-based superconductors and superconducting properties, and is widely used in the research of physics and materials. [0003] Through traditional solid-state reaction methods [such as American Academy of Sciences (P.Natl.Acad.Sci.USA) 2008,105,14262-14264], molten salt method [crystal growth and design (Cryst.Growth Des.) 200...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B19/04B82Y40/00
CPCC01B19/007C01P2002/01C01P2002/20C01P2002/72C01P2002/80C01P2004/03C01P2004/62C01P2004/64C01P2006/40
Inventor 李达李少杰潘德胜李勇韩拯耿殿禹刘伟张志东
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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