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Method for preparing hexagonal piece self-assembled gamma-MnS microcrystalline spheres

A self-assembled, hexagonal sheet technology, applied in the field of preparation of γ-MnS microcrystalline spheres, can solve the problems of difficult process control, low reaction rate, long reaction time, etc., and achieve uniform size, low energy consumption, and short reaction period. Effect

Active Publication Date: 2014-01-29
胡淑婷
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, radio frequency irradiation [Lokhande C D, Ennaoui A, Patil P S, et al. Process and characterization of chemical bath deposited manganese sulphide (MnS) thin films [J]. Thin solid films, 1998, 330: 70-75.] , microwave irradiation method [Wang S B, Li K W, Zhai R, et al.Synthwsis of metastable γ-manganese sulfide crystallite by microwave irradiation[J]. Mater Chem Phys, 2005, 91: 298-300.], molecular beam epitaxy (molecular beam epitaxy, MBE) [OKAJIMA M, TOHDA J. Heteroepitaxial growth of MnS on GaAs substrates [J]. J Cryst Growth, 1992, 117 (1-4): 810-815.], reflux method [Qi Yuanchun, Zhao Yanbao, Xu Hongtao. Preparation and characterization of γ-MnS nanocrystals with controllable morphology [J]. Chemical Research, 2006, 17(6): 60-62.] and other preparation methods have also been applied to the synthesis of MnS nanomaterials, Yet these methods are all more complicated, and technique is difficult to control, and reaction rate is lower, and reaction time is longer, and because a large amount of H is arranged in the process of synthetic manganese sulfide 2 S gas generation, if the reaction is carried out in an open system, it will inevitably cause some pollution to the environment

Method used

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  • Method for preparing hexagonal piece self-assembled gamma-MnS microcrystalline spheres
  • Method for preparing hexagonal piece self-assembled gamma-MnS microcrystalline spheres

Examples

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Embodiment 1

[0017] 1) Analytical pure manganese nitrate (Mn(NO 3 ) 2 4H 2 O) added to deionized water to make Mn 2+ A transparent solution A with a concentration of 0.08mol / L;

[0018] 2) Add analytically pure thioacetamide (C 2 h 5 NS), so that the Mn in the solution 2+ / C 2 h 5 The molar concentration ratio of NS is 1:2, and the obtained solution B is uniformly stirred by magnetic force;

[0019] 3) adding analytically pure hexamethylenetetramine to solution B, so that the concentration of hexamethylenetetramine in the solution is 0.06mol / L, forming precursor solution C;

[0020] 4) Put the precursor solution C at room temperature for 1.5h to obtain solution D;

[0021] 5) Pour solution D into a microwave hydrothermal reactor with a filling degree of 48%, then seal the reactor, put it into a microwave hydrothermal reactor with temperature and pressure dual control, and select the temperature control mode or pressure control mode for reaction , the temperature in the temperatur...

Embodiment 2

[0025] 1) Analytical pure manganese nitrate (Mn(NO 3 ) 2 4H 2 O) added to deionized water to make Mn 2+ A transparent solution A with a concentration of 0.1mol / L;

[0026] 2) Add analytically pure thioacetamide (C 2 h 5 NS), so that the Mn in the solution 2+ / C 2 h 5 The molar concentration ratio of NS is 1:1, and the obtained solution B is uniformly stirred by magnetic force;

[0027] 3) adding analytically pure hexamethylenetetramine to solution B, so that the concentration of hexamethylenetetramine in the solution is 0.08mol / L to form precursor solution C;

[0028] 4) Put the precursor solution C at room temperature for 2 hours to obtain solution D;

[0029] 5) Pour solution D into a microwave hydrothermal reaction kettle with a filling degree of 50%, then seal the reaction kettle, put it into a microwave hydrothermal reaction instrument with dual temperature and pressure control, and select the temperature control mode or pressure control mode for reaction , the...

Embodiment 3

[0032] 1) Analytical pure manganese nitrate (Mn(NO 3 ) 2 4H 2 O) added to deionized water to make Mn 2+ A transparent solution A with a concentration of 0.5mol / L;

[0033] 2) Add analytically pure thioacetamide (C 2 h 5 NS), so that the Mn in the solution 2+ / C 2 h 5 The molar concentration ratio of NS is 1:5, and the obtained solution B is uniformly stirred by magnetic force;

[0034] 3) adding analytically pure hexamethylenetetramine to solution B, so that the concentration of hexamethylenetetramine in the solution is 1.5mol / L to form precursor solution C;

[0035] 4) Put the precursor solution C at room temperature for 1 hour to obtain solution D;

[0036] 5) Pour the solution D into the microwave hydrothermal reaction kettle with a filling degree of 55%, then seal the reaction kettle, put it into the microwave hydrothermal reaction instrument with dual temperature and pressure control, and select the temperature control mode or the pressure control mode for reacti...

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Abstract

The invention relates to a method for preparing hexagonal piece self-assembled gamma-MnS microcrystalline spheres. The method comprises the following steps: 1, adding manganese nitrate to deionized water to prepare a solution A; 2, adding thioacetamide to the solution A to obtain a solution B; 3, adding hexamethylenetetramine to the solution B to form a predecessor solution C; 4, allowing the predecessor solution to stand at room temperature to obtain a solution D; 5, dumping the solution D to a microwave hydrothermal reaction vessel, sealing the reaction vessel, putting the reaction vessel into a temperature and pressure controlled microwave hydrothermal reaction instrument, carrying out a reaction in a temperature control mode or a pressure control mode, and naturally cooling the reaction vessel after ending the reaction; and 6, opening the hydrothermal reaction vessel, centrifuging and collecting the obtained product, washing the product by deionized water and waterless ethanol respectively, and drying the product in a vacuum drying box to obtain the hexagonal piece self-assembled gamma-MnS microcrystalline spheres. The method which adopts a simple microwave hydrothermal process to prepare the microcrystalline spheres has the advantages of short reaction period, low energy consumption, and realization of one-step completing of the reaction in a liquid phase without post treatments. The prepared gamma-MnS microcrystalline spheres are self-assembled by regular hexagonal pieces, and the sizes of the gamma-MnS microcrystalline spheres are uniform.

Description

technical field [0001] The invention belongs to a preparation method of manganese sulfide, a semiconductor material with a wide band gap, and in particular relates to a preparation method of gamma-MnS microcrystal spheres self-assembled from hexagonal sheets. Background technique [0002] Metal sulfides are an important class of semiconductor materials, which are widely used in optical devices, photovoltaic cells, energy storage media, and catalysis. MnS is a weakly magnetic semiconductor of VIIB-VIA with a bandgap width of 3.7eV. It has potential applications in the preparation of solar cell window / buffer materials and short-wave optoelectronic devices [ki s J, Tang K B, Yang Q, et al.Solvothermal synthesis of metastable γ-MnS hollow spheres and control of their phase[J]. Eur J lnorg Chem, 2005: 4124-4128.] MnS generally has three phases, namely octahedral coordination, green and stable rock-salt structure α- MnS(RS); tetrahedrally coordinated, pink metastable zinc blende ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G45/00B82Y40/00
Inventor 黄剑锋辛宇曹丽云吴建鹏费杰李嘉胤
Owner 胡淑婷
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