Preparation method of pencil-shaped gamma-MnS microcrystal

A pencil and microcrystalline technology, which is applied in the field of preparation of manganese sulfide, a wide bandgap semiconductor material, can solve problems such as difficult process control, low reaction rate, and complexity, and achieve the effects of short reaction cycle, reduced activation energy, and uniform size

Inactive Publication Date: 2012-07-18
SHAANXI UNIV OF SCI & TECH
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

In addition, the hydrothermal method [ZHANG Y C, WANG H, WANG B, et al. Low-temperature hydro-thermal synthesis of pure metastable γ-manganese sulfide (MnS) crys-tallites [J]. J Cryst Growth, 2002, 243 (1 ): 214-217.], solvothermal method [ZHANG X H, CHEN Y Q, JIA C, et al.Two-step solvothermal synthesis-sis of α-MnS spheres: Growth mechanism and characterization[J]. Mater Lett, 2008, 62:125-127.], 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 many more This preparation method has also been applied to the synthesis of MnS nanomaterials, but these methods are more complicated, the process is difficult to control, the reaction rate is low, the reaction time is long, and because there is a large amount of H in the process of synthesizing 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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  • Preparation method of pencil-shaped gamma-MnS microcrystal
  • Preparation method of pencil-shaped gamma-MnS microcrystal

Examples

Experimental program
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Effect test

Embodiment 1

[0016] 1) Analytical pure manganese chloride (MnCl 2 4H 2 O) added to deionized water to make Mn 2+ A transparent solution A with a concentration of 0.1mol / L;

[0017] 2) Add analytically pure thioacetamide (C 2 h 5 NS), so that the Mn in the solution 2+ / C 2 h 5 The molar ratio of NS is 1:0.8, and the solution is ultrasonically dispersed to obtain solution B;

[0018] 3) Pour solution B into a flask and seal it, then put the sealed flask into a microwave-ultraviolet-ultrasonic three-in-one synthetic extraction reaction apparatus, select the "temperature-time" working mode, set the temperature at 85°C, and the magnetic stirring speed 400r / min, add ultraviolet energy, the output power of the ultraviolet lamp is 300W, after reacting for 30min, solution C is obtained;

[0019] 4) Pour solution C into a microwave hydrothermal reactor with a filling degree of 55%, then seal the reactor, put it into a microwave hydrothermal reactor with temperature and pressure dual control,...

Embodiment 2

[0023] 1) Analytical pure manganese chloride (MnCl 2 4H 2 O) added to deionized water to make Mn 2+ A transparent solution A with a concentration of 0.3mol / L;

[0024] 2) Add analytically pure thioacetamide (C 2 h 5 NS), so that the Mn in the solution 2+ / C 2 h 5 The molar ratio of NS is 1:0.5, and the solution is ultrasonically dispersed to obtain solution B;

[0025] 3) Pour solution B into a flask and seal it, then put the sealed flask into a three-in-one microwave, ultraviolet, and ultrasonic three-in-one synthetic extraction reaction apparatus, select the "temperature-time" working mode, set the temperature at 80°C, and the magnetic stirring speed The temperature is 380r / min, add ultraviolet energy, the output power of the ultraviolet lamp is 300W, and the solution C is obtained after 40min of reaction;

[0026] 4) Pour solution C into a microwave hydrothermal reaction kettle with a filling degree of 50%, then seal the reaction kettle, put it into a microwave hydr...

Embodiment 3

[0029] 1) Analytical pure manganese chloride (MnCl 2 4H 2 O) added to deionized water to make Mn 2+ A transparent solution A with a concentration of 0.5mol / L;

[0030] 2) Add analytically pure thioacetamide (C 2 h 5 NS), so that the Mn in the solution 2+ / C 2 h 5 The molar ratio of NS is 1:2, and the solution is ultrasonically dispersed to obtain solution B;

[0031] 3) Pour solution B into a flask and seal it, then put the sealed flask into a three-in-one microwave, ultraviolet, and ultrasonic three-in-one synthetic extraction reaction apparatus, select the "temperature-time" working mode, set the temperature at 75°C, and the magnetic stirring speed 350r / min, add ultraviolet energy, the output power of the ultraviolet lamp is 300W, after reacting for 50min, solution C is obtained;

[0032] 4) Pour solution C into a microwave hydrothermal reactor with a filling degree of 45%, then seal the reactor, put it into a microwave hydrothermal reactor with temperature and pressur...

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Abstract

The invention discloses a preparation method of pencil-shaped gamma-MnS microcrystal. The preparation method comprises the following steps of: adding manganese chloride into de-ionized water to obtain solution A; adding thioacetamide into the transparent solution A and ultrasonically dispersing to obtain solution B; pouring the solution B into a flask and sealing; placing the sealed flask in a microwave, ultraviolet and ultrasonic three-in-one synthesis and extraction reactor; heating; performing ultraviolet irradiation to obtain solution C; pouring the solution C into a microwave hydrothermal reaction kettle; sealing the reaction kettle; placing the reaction kettle in a warm pressing double-control microwave hydrothermal reaction instrument; naturally cooling to room temperature after the reaction is finished; opening the hydrothermal reaction kettle; centrifugally collecting a product; washing with de-ionized water and absolute ethyl alcohol respectively; and drying to obtain the final product, i.e., the pencil-shaped gamma-MnS microcrystal. According to the preparation method, a simple ultraviolet-assisted microwave hydrothermal method preparation process is adopted; the reaction period is short; the energy consumption is low; the reaction is finished in a liquid phase in two steps; and no post-treatment is required. The prepared gamma -MnS microcrystal has a regular pencilshape and more uniform size.

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 a pencil-shaped γ-MnS microcrystal. Background technique [0002] In the field of material synthesis, 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 very important wide bandgap semiconductor with a bandgap energy of 3.7eV. It has potential applications in the preparation of window / buffer materials for solar cells and short-wave optoelectronic devices [ki s J, Tang K B, Yang Q, et al.Solvothermal synthesis of metastableγ-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); tetrahedral coordination, pink metastable sphale...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/00B82Y40/00
Inventor 黄剑锋辛宇曹丽云费杰李嘉胤孟岩
Owner SHAANXI UNIV OF SCI & TECH
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