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Low-temperature liquid phase synthesizing method of monodisperse square crystalline phase ferrous selenide square nanometer sheet

A synthesis method and tetragonal crystal phase technology, applied in the field of iron selenide, can solve the problems of unfavorable in-depth research, highly toxic iron pentacarbonyl, expensive reagents, etc., and achieve the effect of controllable particle size and good dispersibility

Inactive Publication Date: 2010-06-30
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reagents used here are expensive and iron pentacarbonyl is highly toxic, and the morphology of the obtained products is not uniform, which is not conducive to further in-depth research.

Method used

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  • Low-temperature liquid phase synthesizing method of monodisperse square crystalline phase ferrous selenide square nanometer sheet
  • Low-temperature liquid phase synthesizing method of monodisperse square crystalline phase ferrous selenide square nanometer sheet
  • Low-temperature liquid phase synthesizing method of monodisperse square crystalline phase ferrous selenide square nanometer sheet

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 0.04M anhydrous ferrous chloride (FeCl 2 ) of oleylamine solution 7.5ml into the three-necked flask, high-purity argon (99.99%) protected heating to 110 ° C until the solid is completely dissolved to obtain a mixed solution; after 0.5ml oleic acid is injected into the flask, Add the prepared selenium-trioctylphosphorus (Se-TOP) at a ratio of 1:1. Se-TOP refers to dissolving Se powder in trioctylphosphorus. In experiments, it is usually prepared as a 1M solution, because selenium is solid, it is usually dissolved in trioctylphosphine. Set the reaction temperature to 320° C., and react for 20 minutes; monodisperse tetragonal iron selenide nanosheets are prepared. The XRD diffraction peaks of the product are as figure 1 As shown in curve 1; the shape is as figure 2 shown. Such as figure 1 As shown in the middle curve 1, all the diffraction peaks can correspond to the standard peak of tetragonal β-FeSe at the bottom (JCPDS No.85-0735), which shows that the obtained pr...

Embodiment 2

[0022] 0.04M anhydrous FeCl 2 Add 7.5ml of oleylamine solution of tetradecyl glycol and 0.4M into a three-necked flask, and heat it to 140°C under the protection of high-purity argon (99.99%) until the solid is completely dissolved to obtain a mixed solution; 0.5ml of oleic acid is injected After arriving in the three-necked flask, add selenium-trioctylphosphorus (Se-TOP) prepared according to the molar ratio of iron ion and selenium 1:1, set the reaction temperature at 330°C, and react for 15 minutes; monodisperse tetragonal crystals are obtained phase iron selenide nanosheets. The XRD diffraction peaks of the product are as figure 1 As shown in #2, all the diffraction peaks can correspond to the standard peak of tetragonal β-FeSe at the bottom (JCPDS No.85-0735), so it can be known that the obtained product is a pure tetragonal β-FeSe structure.

Embodiment 3

[0024] 0.025M anhydrous FeCl 2 Ferrous chloride and 7.5 ml of oleylamine solution of tetradecyl glycol of 0.2M were mixed and added into a three-necked flask, protected and heated to 130° C. until the solid was completely dissolved under high-purity argon (99.99%) to obtain a mixed solution; After 0.3ml of oleic acid was injected into the flask, the prepared selenium-trioctylphosphorus (Se-TOP) was added according to the molar ratio of iron ion and selenium 1:1, the reaction temperature was set to 300°C, and the reaction was carried out for 5 minutes; Dispersed tetragonal iron selenide nanosheets. The XRD diffraction peaks of the product are as figure 1 As shown in #3, all the diffraction peaks correspond to the standard peaks of the tetragonal β-FeSe at the bottom (JCPDS No.85-0735), which shows that the obtained product is a pure tetragonal β-FeSe structure.

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Abstract

The invention discloses a low-temperature liquid phase synthesizing method of monodisperse square crystalline phase ferrous selenide square nanometer sheet. The method comprises the following steps of: heating oil amine solution of anhydrous FeC12 to 100-140 DEG C under the protection of high-purity argon until the solid is completely dissolved; adding oleic acid and the prepared trioctylphosphine phosphor of selenium to react for 5-45min at 280-330 DEG C to prepare the monodisperse square crystalline phase ferrous selenide nanometer sheet, wherein the volume ratio of oil amine solution of anhydrous FeC12 to oleic acid is 30:1-3, and the molar ratio of iron ion to selenium is 1:1. The method is a liquid phase synthesizing method of ferrous selenide and can obtain the product directly in the solution at low temperature without calcinations in comparison with the solid phase method. Compared with other liquid phase methods, the method ensures that the obtained product has better regular two-dimensional nanometer structure, the granule has controllable and even size as well as good dispersity and the material is non-toxic FeC12.

Description

technical field [0001] The invention relates to iron selenide of inorganic nanometer materials, in particular to a low-temperature liquid-phase synthesis method of tetragonal crystal phase iron selenide nanosheets with a monodisperse superconducting structure. Background technique [0002] Tetragonal iron selenide (β-FeSe) has broad application prospects in electronic components due to its unique magnetic properties, electrochemical properties and superconducting properties. [0003] At present, the main methods of preparing iron selenide at home and abroad can be divided into high-temperature solid-phase reaction method and liquid-phase synthesis method. The solid-phase reaction method is a traditional method, which can prepare components with adjustable components. Important synthetic method for iron properties. Solid phase reaction methods include: solid phase reaction traditional process, self-propagating combustion synthesis method, low temperature combustion synthesis...

Claims

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Application Information

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IPC IPC(8): C01B19/04
Inventor 陈立桥吴明娒展红全杨贤锋
Owner SUN YAT SEN UNIV
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