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Novel method for organically synthesizing FeSe superconductor precursor powder

An organic synthesis and superconductor technology, applied in the direction of binary selenium/tellurium compounds, etc., can solve the problems of difficult control of reaction products, achieve the effects of improving synthesis efficiency, reducing synthesis cost, and improving powder purity

Active Publication Date: 2013-12-11
GRIMAT ENG INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because the available selenium source—sodium selenosulfate can only provide selenium ions under alkaline conditions, the precipitation of ferric hydroxide will occur in the process, making the control of the reaction product difficult to achieve in the synthesis.

Method used

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  • Novel method for organically synthesizing FeSe superconductor precursor powder
  • Novel method for organically synthesizing FeSe superconductor precursor powder
  • Novel method for organically synthesizing FeSe superconductor precursor powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 0.1 mol FeCl 2 powder mixed with 0.1 mol selenium powder, FeCl 2 The powder is analytically pure powder without crystal water, placed in a high-pressure reactor lined with stainless steel and polytetrafluoroethylene plastic at room temperature, and 30ml of ethylenediamine and an equivalent amount of ethylene glycol were added to the high-pressure In the kettle, after stirring, the autoclave was covered. Among them, ethylene glycol is used as an organic complexing agent, and ethylene glycol is used as a reducing agent.

[0029] The kettle was then heated to 180°C for 2 hours. Amino groups in ethylenediamine can reduce selenium to selenium ions, which can be combined with iron ions to form FeSe 2 powder.

[0030] The FeSe deposited in the autoclave 2 The powder was washed, centrifuged, filtered 5 times and dried, then the obtained powder was placed in a quartz boat.

[0031] The annealing environment is a vacuum chamber with a mechanical pump that can heat the sampl...

Embodiment 2

[0033] 0.1 mol FeCl 2 Mix the powder with 0.1 mole of selenium powder, place it in a polytetrafluoroethylene-lined autoclave at room temperature, add 30ml of ethylenediamine and an equivalent amount of ethylene glycol into the autoclave in turn, and cover the autoclave after stirring . Among them, ethylene glycol is used as an organic complexing agent, and ethylenediamine is used as a reducing agent.

[0034] The kettle was then heated to 160°C for 4 hours. The amino groups in ethylenediamine can reduce selenium to selenium ions, which can be combined with free iron ions to form FeSe 2 powder.

[0035] The FeSe deposited in the autoclave 2 The powder was washed, centrifuged, filtered 5 times and dried, then the obtained powder was placed in a quartz boat.

[0036] The annealing environment is a vacuum chamber that can heat the sample, and a vacuum pump is used to maintain the vacuum degree of the chamber at 5×10 -2 After Pa is below, the temperature is raised to 700°C at...

Embodiment 3

[0038] Put 0.1 mol FeCl 2 The powder is mixed with 0.1 mole of selenium powder, placed in an autoclave lined with polytetrafluoroethylene at room temperature, 25ml of ethylenediamine and twice the volume of ethylene glycol are added to the autoclave in turn, and the autoclave lid is closed after stirring. combine. Among them, ethylene glycol is used as an organic complexing agent, and ethylenediamine is used as a reducing agent.

[0039] The kettle was then heated to 120°C for 8 hours. The amino groups in ethylenediamine can reduce selenium to selenium ions, which can be combined with free iron ions to form FeSe 2 powder.

[0040] The FeSe deposited in the autoclave 2 The powder was washed, centrifuged, filtered 8 times and dried, then the resulting powder was placed in a quartz boat.

[0041] The annealing environment is a vacuum chamber that can heat the sample, and a vacuum pump is used to maintain the vacuum degree of the chamber at 1×10 -3 Pa, after the vacuum is st...

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Abstract

The invention relates to a novel method for organically synthesizing FeSe superconductor precursor powder, which comprises the following steps: (1) mixing FeCl2 powder and selenium powder in an Fe / Se mol ratio of 1:1, and putting into a high-pressure autoclave (high-pressure reaction kettle) at room temperature; (2) sequentially adding ethylene diamine and ethylene glycol in a volume ratio of 1:1-1:3 into the high-pressure autoclave, stirring and covering the high-pressure autoclave; (3) heating the high-pressure autoclave to 120-200 DEG C, and holding for 1-8 hours; (4) cleaning and filtering the deposit FeSe2 powder in the high-pressure autoclave 5-8 times, and drying; and (5) putting the powder in an open vacuum system, and carrying out vacuum heat treatment to obtain the FeSe high-purity powder. The Fe-Se high-purity powder is in a square phase structure. The invention has the advantages of high efficiency and low cost, reduces the impurity phases, and is suitable for mass synthesis of FeSe superconducting precursor powder.

Description

technical field [0001] The invention relates to a method for preparing a novel superconductor precursor powder, in particular to a method for preparing high-purity FeSe powder by using an oxygen-free organic compound-vacuum annealing method. Background technique [0002] Iron-based superconductors have become a new research boom in the field of superconductivity and condensed matter physics in recent years. Among them, FeSe has become a potential substitute for low-temperature superconducting applications due to its simple structure and low toxicity, such as metal-clad wires and strips. In order to have an accurate and in-depth understanding of the physical properties of FeSe-type superconductors, high-quality precursor powders are indispensable. [0003] At present, the main way to prepare samples is solid-phase synthesis, that is, weighing, grinding and sintering iron powder and selenium powder according to the stoichiometric ratio. Due to the low melting point of seleniu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B19/04
Inventor 柴青林华志强王磊屈飞
Owner GRIMAT ENG INST CO LTD
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