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Pyrite structural iron-based ternary chalcogenide single crystal material and preparation method thereof

A single crystal material and structural iron technology, applied in the field of material science, can solve the problems of easy impurity, complexity, and complex requirements, and achieve the effect of good crystallization performance, simple equipment, and good repeatability

Active Publication Date: 2018-02-09
HENAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since most cubic iron chalcogen single crystals need to be synthesized under high pressure (Inorg Chem, 15, 3031, 1976; Inorg Chem 7, 2208, 1968), and the preparation equipment is expensive and complex, so compared with other two phases, Its research is very scarce
In recent years, cubic iron chalcogenides have made progress in photovoltaic research (Adv.Energy Mater.1,748, 2011), but the samples are nanocrystals synthesized by hydrothermal, and the physical properties of nanomaterials and bulk materials are quite different; Cubic iron chalcogenide polycrystalline thin film, but the equipment is expensive and complex and prone to impurities (J Mater Sci, 48, 4914, 2013; Thin Solid Films, 516, 7116, 2008), which is not conducive to more research
Additionally, most existing cubic iron chalcogenides are limited to binary materials
Obviously, these factors greatly limit the research on the basic physical properties and applications of such materials

Method used

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  • Pyrite structural iron-based ternary chalcogenide single crystal material and preparation method thereof
  • Pyrite structural iron-based ternary chalcogenide single crystal material and preparation method thereof
  • Pyrite structural iron-based ternary chalcogenide single crystal material and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] This embodiment is a pyrite structure iron chalcogen single crystal FePd 2 Se 6 The preparation process and its structural, electrical, and magnetic tests.

[0030] 1. Single crystal preparation

[0031] 1), weighing raw materials and sealing

[0032] Weigh 0.1071g of Fe block, 0.4083g of Pd block and 1.5152g of Se powder, grind and mix them and put them into an alumina crucible, then put the crucible into a quartz tube. Vacuum the quartz tube and then fill it with argon, repeat 5 times, and finally evacuate again, the pressure is 10 -3 Pa;

[0033] 2), heating and annealing process

[0034] Put the quartz tube sealed with the crucible in the high-temperature annealing furnace, and start to set the temperature program. It took 12 hours to raise the room temperature to 300°C; keep warm at 300°C for 12 hours; rise from 300°C to 900°C and take 12 hours; keep warm at 900°C for 4 hours; cool down from 900°C to 300°C and take more than 200 hours. During every 12 hours,...

Embodiment 2

[0046] This embodiment is a pyrite structure iron chalcogen single crystal FePd 2 Se 6 preparation process and its structure.

[0047] 1. Single crystal preparation

[0048] 1), weighing raw materials and sealing

[0049] Weigh a certain mass of Fe powder, Pd powder and Se powder with the ratio of Fe:Pd:Se 3:1:15, grind and mix them, put them into an alumina crucible, and then put the crucible into a quartz tube. Vacuum the quartz tube and then fill it with argon, repeat 5 times, and finally evacuate again, the pressure is 10 -2 Pa;

[0050] 2), heating and annealing process

[0051] Put the quartz tube sealed with the crucible in the high-temperature annealing furnace, and start to set the temperature program. It took 12 hours to raise the room temperature to 300°C; 12 hours to keep at 300°C; 24 hours to rise from 300°C to 950°C; 4 hours to keep at 900°C; 200 hours to cool down from 950°C to 300°C. Every 24 hours, make the furnace slightly vibrate or shake for 1 minute...

Embodiment 3

[0055] This embodiment is a pyrite structure iron chalcogen single crystal FePd 2 Se 6 preparation process and its structure.

[0056] 1. Single crystal preparation

[0057] 1), weighing raw materials and sealing

[0058] Weigh a certain mass of Fe powder, Pd powder and Se powder with the ratio of Fe:Pd:Se 1:3:20, grind and mix them, put them into an alumina crucible, and then put the crucible into a quartz tube. Vacuum the quartz tube and then fill it with argon, repeat 5 times, and finally evacuate again, the pressure is 10 -2 Pa;

[0059] 2), heating and annealing process

[0060] Put the quartz tube sealed with the crucible in the high-temperature annealing furnace, and start to set the temperature program. It takes 10 hours to raise the room temperature to 300°C; 10 hours to keep at 300°C; 24 hours to rise from 300°C to 1000°C; 4 hours to keep at 1000°C; 220 hours to cool down from 1000°C to 300°C. Every 48 hours, make the furnace slightly vibrate or shake for 2 mi...

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PUM

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Abstract

The present invention relates to a pyrite structural iron-based ternary chalcogenide single crystal material and a preparation method thereof. The molecular formula of the single crystal material is FePd2Se6, and the lattice constants a, b, and c satisfy the following relationship: a=b=c=6.045(3) angstroms, the electrical transport shows metallicity, the magnetism shows that a significant hysteresis loop exists at 1.8K, and the preparation method comprises the following sequential steps: 1) a Fe source, a Pd source and a Se source are weighed, the weighed materials are mixed and loaded into analuminium oxide crucible, and then the aluminium oxide crucible is sealed; and 2) the sealed aluminium oxide crucible is placed into a high-temperature annealing furnace, and a program begins to setfor heating; and then a fluxing agent Se is removed by adopting centrifugation to obtain the FePd2Se6 single crystal. According to the invention, the pyrite structural iron-based ternary chalcogenidesingle crystal FePd2Se6 is prepared by using a self fluxing agent method, and has the advantages of low costs, easy control, good repeatability, simple equipment and the like.

Description

technical field [0001] The invention relates to a pyrite-structure iron-based ternary chalcogen single crystal material and a preparation method thereof, belonging to the field of material science. Background technique [0002] Iron chalcogenides have attracted much attention due to their fascinating properties, such as superconductivity, thermoelectricity and photovoltaic effects (Sci.Technol.Adv.Mat.13,054305,2012; Adv.Energy Mater.1,748,2011; , 9424, 2014). Currently, most studies on iron chalcogenides focus on the hexagonal and tetragonal phases. Since most cubic iron chalcogen single crystals need to be synthesized under high pressure (Inorg Chem, 15, 3031, 1976; Inorg Chem 7, 2208, 1968), and the preparation equipment is expensive and complex, so compared with other two phases, Its research is very scarce. In recent years, cubic iron chalcogenides have made progress in photovoltaic research (Adv.Energy Mater.1,748, 2011), but the samples are nanocrystals synthesized...

Claims

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Application Information

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IPC IPC(8): C30B29/46C30B9/00
CPCC30B9/00C30B29/46
Inventor 田建军高惠平田军锋范素娟秦勉贾彩虹施度美亚·彼得罗维奇张伟风
Owner HENAN UNIVERSITY
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