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Preparation method of novel Fe<1-x>TM<x>S single crystal material

A technology of fe1-xtmxs and fe1.6-xtmxs2, which is applied in the field of preparation of single crystal materials, can solve the problems of preparation failure, violent reaction, and difficulty in controlling the content of transition metal elements, so as to improve quality and stability, and make the preparation process safe simple effect

Active Publication Date: 2021-08-10
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the traditional preparation method, impurity phases with hexagonal structure are easy to be produced, and the content of transition metal elements is difficult to control. At the same time, elemental potassium and sulfur elements will react violently, which may easily lead to preparation failure or poor crystal quality.

Method used

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  • Preparation method of novel Fe&lt;1-x&gt;TM&lt;x&gt;S single crystal material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] a. Preparation FE 1.6-x CO x S 2 Polycrystalline: Put the iron powder, cobalt powder and sulfur powder according to Fe 1.6-x CO x S 2 The atomic ratio was weighed, and the raw material was grinded in a mortar in a mortar for more than 30 minutes, and then the ground sample was sealed into a vacuum quartz, and then the quartz pipe was placed in a box furnace to sinter at 500 ° C for 24 hours. After cooling to room temperature to get Fe 1.6-x CO x S 2 Polycrystalline;

[0026] b. Preparation k 0.8 FE 1.6-x CO x S 2 Single crystal: 1.6G Fe 1.6-x CO x S 2 Polycrystalline and 0.328 g of the potassium were sealed into vacuum quartzers, followed by sintering the quartz pipe in a box furnace at 1000 ° C for 24 hours and slowly cooled to 700 ° C at a rate of 5 ° C / h, and dissociated K 0.8 FE 1.6-x CO x S 2 Single crystal;

[0027] c. Formulated a mixed solution under an inert atmosphere, adding 0.12 g of sodium hydroxide and 0.23 g of thiourea to 10 ml of water to give a mixed sol...

Embodiment 2

[0032] a. Preparation FE 1.6-x Ni x S 2 Polycrystalline: Push iron powder, nickel powder and sulfur powder according to Fe 1.6-x Ni x S 2 The atomic ratio was weighed, and the raw material was grinded in a mortar for more than 30 minutes, and then the grinding sample was sealed into a vacuum quartz, then put the quartz pipe in the box furnace was sintered at 450 ° C for 24 hours. After cooling to room temperature to get Fe 1.6-x Ni x S 2 Polycrystalline;

[0033] b. Preparation k 0.8 FE 1.6-x Ni x S 2 Single crystal: 0.16g Fe 1.6-x Ni x S 2 Polycrystalline and 0.328 g of a single potassium enclosed in vacuum quartzers, then put the quartz pipe in a box furnace at 1020 ° C for 24 hours and slowly cooled to 700 ° C at a rate of 5 ° C / h, and dissociated K 0.8 FE 1.6-x Ni x S 2 Single crystal;

[0034]c. Formulated a mixed solution under an inert atmosphere, adding 0.12 g of sodium hydroxide and 0.23 g of thiourea to 10 ml of water to give a mixed solution.

[0035] d. Press K again...

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Abstract

The invention discloses a preparation method of a novel Fe<1-x>TM<x>S single crystal material, TM is a transition metal including one of cobalt, nickel and copper elements, x is the stoichiometric number of TM, and x is more than or equal to 0.01 and less than or equal to 0.5. The preparation method comprises the following steps: step a, preparing Fe<1.6-x>TM<x>S2 polycrystals; step b, preparing a K<0.8>Fe<1.6-x>TM<x>S<2> single crystal; step c, preparing an aqueous solution of thiourea and sodium hydroxide; step d, adding iron powder, TM powder and K<0.8>Fe<1.6-x>TM<x>S<2> single crystal into the solution in the step c to obtain a mixed solution; step e, carrying out heat-preservation reaction on the mixed solution; and step f, washing the reacted solution with water and ethanol to obtain the Fe<1-x>TM<x>S single crystal with the tetragonal structure. According to the method, transition metal elements are successfully doped into the FeS single crystal with the tetragonal structure, Fe<1.6-x>TM<x>S2 polycrystal is used as a precursor, the content of the transition metal elements is accurately controlled, the reaction between elemental potassium and elemental sulfur in the growth process of the K<0.8>Fe<1.6-x>TM<x>S<2> single crystal is weakened, the cost is low, the process is simple, the raw materials are non-toxic, and the prepared single crystal is high in quality, large in size and suitable for industrial production. The method has important significance on the physical property research of the Fe<1-x>TMxS material system and the application of magnetic devices.

Description

Technical field [0001] The present invention relates to a new type of Fe 1-x TM x The method of preparing the S single crystal material is the field of preparation method of single crystal materials. Background technique [0002] In 2016, the ferromic superconductor FES single crystal was successfully prepared by hydrothermalization, and the superconducting transition temperature was 4.5k. Four-square structures FES superconductor as the simplest iron-based superconductor, with large anisotropy and lower upper velocons, and studies of angular distinguishing optical electronics indicate that their interior has large electronically associations. The FESE superconductors of the same structure do not have a structural phase change and an electron-liquid crystal phase at low temperatures, which makes it an important material associated between high temperature superconducting mechanism and electron liquid crystal phase and superconducting transition. [0003] Although FES superconduct...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/46C30B7/14
CPCC30B29/46C30B7/14
Inventor 陈飞袁鹏马仁海吕文来张金仓
Owner SHANGHAI UNIV
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