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A method for preparing hollow indium sulfide microspheres at atmospheric pressure and low temperature without template

A template-free, indium sulfide technology, applied in chemical instruments and methods, inorganic chemistry, gallium/indium/thallium compounds, etc., can solve the problems of volatile carbon disulfide, cytotoxicity, and less one-time preparation, and achieve easy Separation and cleaning, controllable size and wall thickness, uniform shape results

Inactive Publication Date: 2018-10-23
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] There are many problems in the above methods: firstly, the hydrothermal method or the solvothermal method adopts high-pressure equipment such as small-scale hydrothermal reactors, the process is complex, the amount of one-time preparation is small, and it is difficult to produce in batches; secondly, the reaction system must be heated to 150-180 ℃, there is a certain risk, time-consuming (10-24 hours), and large energy consumption; third, some sulfur sources are highly toxic, carbon disulfide is volatile and has cytotoxicity, and thiosemicarbazide is a highly toxic substance, requiring production equipment Airtight, operators should wear protective equipment to hinder related production
Fourth, organic solvents are often used in the synthesis process, such as ethanol, benzene, etc., which are flammable and some are toxic
But so far, there has been no template-free synthesis of hollow In in aqueous phase at atmospheric pressure and low temperature. 2 S 3 microsphere report

Method used

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  • A method for preparing hollow indium sulfide microspheres at atmospheric pressure and low temperature without template
  • A method for preparing hollow indium sulfide microspheres at atmospheric pressure and low temperature without template
  • A method for preparing hollow indium sulfide microspheres at atmospheric pressure and low temperature without template

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Mix 50mL 0.004mol / L indium nitrate aqueous solution with 50mL 0.004mol / L 2-methyl-thiopropionamide aqueous solution, then add 1mol / L hydrochloric acid aqueous solution to adjust the pH value to 2.2, microwave heating reaction at 90°C for 15min, statically Place, remove the supernatant, centrifuge, wash, and freeze-dry to obtain the product. The product had a wall thickness of 80 nm and a diameter of ~900 nm. The SEM picture, TEM picture and XRD picture of the product are shown in the appendix figure 1 , 2 and 3.

Embodiment 2

[0031] Mix 50mL 0.004mol / L indium nitrate aqueous solution with 50mL 0.004mol / L 2-p-phenylmethylthioacetamide aqueous solution, then add 0.5mol / L hydrochloric acid aqueous solution to adjust the pH value to 2.5, and then heat it with microwave at 80℃ for 25min. , stand still, remove the supernatant, centrifuge, wash, and freeze-dry to obtain the product. The product has a wall thickness of 70 nm and a diameter of ~800 nm.

Embodiment 3

[0033] Mix 50mL of 0.008mol / L indium chloride aqueous solution with 50mL of 0.024mol / L 2-methyl-thiopropionamide aqueous solution, then add 1mol / L hydrochloric acid aqueous solution to adjust the pH value to 2.2, and react with microwave at 90°C for 15min, Stand still, remove the supernatant, centrifuge, wash, and freeze-dry to obtain the product. The product had a wall thickness of 70 nm and a diameter of ~900 nm.

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Abstract

The invention relates to a method for preparing hollow indium sulfide micro-spheres at normal pressure and low-temperature and without a template. The method comprises the following steps: mixing indium saline aqueous solution and thioacid amide aqueous solution with magnetic stirring; regulating pH; then heating and reacting in a microwave opening system; cooling; filtering; washing with water; and freezing and drying to obtain the hollow indium sulfide micro-spheres. According to the method, the template is not used, and the product can be directly obtained by once reaction; other additives are not added during the reaction; the prepared hollow indium sulfide micro-spheres are high in dispersing performance, and uniform in particle size; the size and wall thickness can be controlled; the shape is consistent; and the stability is high; the heating reaction is carried out in a normal-pressure opening system through a microwave assisting method, so that high temperature and high pressure which are necessary for a water heating method or a solvent heating method can be avoided, and as a result, the safety is high, and the energy can be saved; the method and the technological processes are simple, and environment-friendly; the reaction is carried out in a water phase; the product is easily separated and washed; the yield is high; and the mass production can be carried out.

Description

technical field [0001] The invention belongs to the field of preparation of indium sulfide microspheres, in particular to a method for preparing hollow indium sulfide microspheres at normal pressure and low temperature without a template. Background technique [0002] Indium sulfide In 2 S 3 It is a direct narrow bandgap semiconductor material with a forbidden band width of 2-2.2eV at room temperature. It has good chemical stability and excellent photoelectric and thermoelectric properties. In 2 S 3 It has been applied in optical and electrical devices, such as photovoltaic solar cells, photoconductors, superionic conductors, lithium-ion batteries. [0003] Currently on In 2 S 3 The research on materials is relatively popular, and the prepared In 2 S 3 The product also has a variety of different forms, including nanoparticles, rods, ribbons, tubes and hollow microspheres. The synthesis of hollow microspheres mostly adopts the template method. For example, Gao et al....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G15/00
CPCC01G15/00C01P2002/72C01P2004/03C01P2004/04C01P2004/34C01P2004/62
Inventor 邢彦军朱燕杰
Owner DONGHUA UNIV
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