Preparation method of flaky iron sulfide single crystal nano-material

A technology of ferric tetrasulfide and nano-single crystal, which is applied in chemical instruments and methods, single crystal growth, single crystal growth, etc. It can solve the problems of poor phase purity, difficulty in controlling the morphology of ferric tetrasulfide, and lack of monodisperse tetrasulfide Tri-iron nano-single crystal and other problems, to achieve the effect of regular shape, controllable particle size and shape, and cheap raw materials

Inactive Publication Date: 2015-04-08
LANZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there are also studies on the synthesis of ferric sulfide in the current literature reports, the general phase purity is poor, and most of them contain other sulfur iron compounds.
At the same time, the morphology of iron tetrasulfide is also difficult to control in the reported synthesis process, and it is difficult to obtain nanocrystals of iron tetrasulfide with uniform size, regular morphology and controllability.
At present, there is no report on the preparation method of monodisperse, single phase, uniform size and controllable morphology of iron tetrasulfide nano single crystals.

Method used

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  • Preparation method of flaky iron sulfide single crystal nano-material
  • Preparation method of flaky iron sulfide single crystal nano-material
  • Preparation method of flaky iron sulfide single crystal nano-material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1 A preparation method of sheet-shaped iron tetrasulfide nanometer single crystal, comprising the following steps:

[0038] ⑴Mix the iron source—ferrous chloride with a concentration of 0.05mol / L and trioctylphosphine oxide (TOPO) at a molar ratio of 1:1.5, and dissolve in oleylamine, stir and pass the purity to 98.5% After removing oxygen from the above nitrogen or argon gas, an iron source precursor is obtained.

[0039] Among them: the mass volume ratio (g / ml) of iron source and oleylamine is 1:50.

[0040] (2) Heating the iron source precursor to 120° C. in an oil bath and stirring for 1.5 hours to obtain an iron source solution.

[0041] (3) Dissolve the sulfur source—sulfur powder in oleylamine, and after stirring and passing argon or nitrogen with a purity of more than 98.5% to remove oxygen, obtain a sulfur source solution.

[0042] Among them: the mass volume ratio (g / ml) of sulfur source and oleylamine is 1:50.

[0043] (4) Heating the sulfur ...

Embodiment 2

[0047] Example 2 A preparation method of sheet-shaped iron tetrasulfide nanometer single crystal, comprising the following steps:

[0048] ⑴Mix the iron source—ferrous chloride with a concentration of 0.5 mol / L and trioctylphosphine oxide (TOPO) at a molar ratio of 1:3, and dissolve in oleylamine, stir and pass the purity to 98.5% After removing oxygen from the above nitrogen or argon gas, an iron source precursor is obtained.

[0049] Among them: the mass volume ratio (g / ml) of iron source and oleylamine is 1:150.

[0050] (2) Heating the iron source precursor to 170° C. in an oil bath and stirring for 0.5 hours to obtain an iron source solution.

[0051] (3) Dissolve the sulfur source—thiourea in oleylamine, and after stirring and passing argon or nitrogen with a purity of more than 98.5% to remove oxygen, obtain a sulfur source solution.

[0052] Among them: the mass volume ratio (g / ml) of sulfur source to oleylamine is 1:100.

[0053] (4) Heating the sulfur source...

Embodiment 3

[0057] Example 3 A preparation method of sheet-shaped iron tetrasulfide nanometer single crystal, comprising the following steps:

[0058] ⑴Mix the iron source—ferrous chloride with a concentration of 0.25 mol / L and trioctylphosphine oxide (TOPO) at a molar ratio of 1:2.5, and dissolve in oleylamine, stir and pass the purity to 98.5% After removing oxygen from the above nitrogen or argon gas, an iron source precursor is obtained.

[0059] Among them: the mass volume ratio (g / ml) of iron source and oleylamine is 1:100.

[0060] (2) Heating the iron source precursor to 150° C. in an oil bath and stirring for 1 hour to obtain an iron source solution.

[0061] (3) Dissolve the sulfur source—sulfur powder in oleylamine, and after stirring and passing argon or nitrogen with a purity of more than 98.5% to remove oxygen, obtain a sulfur source solution.

[0062] Among them: the mass volume ratio (g / ml) of sulfur source to oleylamine is 1:75.

[0063] (4) Heating the sulfur so...

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PUM

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Abstract

The invention relates to a preparation method of a flaky iron sulfide single crystal nano-material. The method comprises the following steps of: (1) mixing an iron source and trioctylphosphine oxide, dissolving in oleylamine, stirring, feeding nitrogen or argon to remove oxygen, and then obtaining an iron source precursor; (2) heating and stirring the iron source precursor in oil bath to obtain iron source solution; (3) dissolving a sulfur source in the oleylamine, stirring, feeding argon or nitrogen to remove oxygen, and then obtaining sulfur source solution; (4) heating the sulfur source solution, extracting through a needle tube, quickly injecting into the iron source solution, carrying out warming reaction on the oil bath for heating the iron source, and obtaining a colloid of the flaky iron sulfide single crystal nano-material; and (5) cooling the colloid of the flaky iron sulfide single crystal nano-material to room temperature, adding trichloromethane-ethanol mixed solution, and carrying out washing and centrifugalizing processing for many times until centrifugate on an upper layer is colorless so as to obtain the flaky single-phase iron sulfide single crystal nano-material. The obtained product has uniform grain size and shape, good process repeatability, and stable quality.

Description

technical field [0001] The invention relates to a preparation method of ferric tetrasulfide, in particular to a preparation method of sheet-shaped ferric ferric sulfide nano single crystal. Background technique [0002] As a magnetic material, iron tetrasulfide is a ferromagnetic material. Ferromagnetic materials are widely used in the industrial field, and can be used as microwave absorbing materials, magnetic recording materials, magnetic liquids, and also have a wide range of applications in the field of biomedicine. Iron tetrasulfide can be used in cancer hyperthermia therapy, and its magnetic properties make this material promising as a medium for targeted drug delivery, which can be used in the medical field in the near future (M. Posfai, P. R. Buseck, D. A. Bazylinski and R. B. Frankel , Iron sulfates from magnetotactic bacteria; structure, composition, and phase transitions [J]. Journal of the Mineralogical Society of America. 1998, 83 (11-12), 1469-1481.; Y. S. Cha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/46C30B29/60C30B7/14
Inventor 拜永孝包琰魏成蓉邓爱英胡新军
Owner LANZHOU UNIVERSITY
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