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Single-phase titanium diselenium nano-sheet prepared by solution method and method and application of nano-sheet

A titanium diselenide and nanosheet technology, applied in the field of nanomaterials, can solve the problems of environmental pollution, skin burns, differences in sample components, etc., and achieve the effects of high operational accessibility, short reaction time, and simple method.

Inactive Publication Date: 2018-08-24
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Even so, differences in sample composition caused by temperature gradients inside the high-temperature furnace are often unavoidable
Second, although there is also liquid-phase synthesis, the solvents used are toxic and unfavorable to the health of experimenters (Yang Jun, Zhang Yufei, Zhang Yizhou et al., S-Doped TiSe 2 Nanoplates / Fe 3 o 4 Nanoparticles Heterostructure [J], Small, 2017, 13, 42), the TOP (trioctylphosphine, Trioctylphosphine) used in it, the hazard category is 1B, if it is accidentally splashed during use and contacts the skin, it will cause severe skin damage. Burns and even eye damage, and also pollute the environment

Method used

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  • Single-phase titanium diselenium nano-sheet prepared by solution method and method and application of nano-sheet
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  • Single-phase titanium diselenium nano-sheet prepared by solution method and method and application of nano-sheet

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] First, in a 50 mL two-necked bottle, inject 5 mL of oleylamine and 7 mL of octadecene, and disperse the selenium powder in the mixed solvent to obtain the precursor A of the selenium source. Then, high-purity nitrogen gas was introduced, the mixed solution A was stirred, and a mechanical pump was used to pump air, and at the same time, the temperature was raised to 115° C., and the temperature was kept for 35 minutes. After cooling down to room temperature, repeated gas scrubbing several times to obtain an oxygen-free and water-vapour-free environment. Subsequently, 10 mmol TiCl was added 4 , so that TiCl 4 : The molar ratio of Se is 1:0.4. Under continuous stirring and a protective atmosphere, the temperature was raised to 260° C. and kept for 30 minutes to complete the growth of nanocrystals, then the heating was stopped, and the reaction system was cooled to room temperature. Then, after centrifugation at 9500r / min, wash with ethanol and cyclohexane three times, p...

Embodiment 2

[0055] First, in a 50 mL two-necked bottle, inject 5 mL of oleylamine and 7 mL of octadecene, and disperse the selenium powder in the mixed solvent to obtain the precursor A of the selenium source. Then, high-purity nitrogen gas was introduced to stir the mixed solution A, and a mechanical pump was used to pump air. At the same time, the temperature was raised to 120 ° C, kept for 20 minutes, and repeated several times to obtain an oxygen-free and water-vapour-free environment. After cooling down to room temperature, add 10mmol TiCl 4 , so that TiCl 4 : The molar ratio of Se is 1:0.7. Under continuous stirring and a protective atmosphere, the temperature was raised to 300° C. and kept for 35 minutes to complete the growth of nanocrystals, then the heating was stopped, and the reaction system was cooled to room temperature. Then, after centrifugation at 8000r / min, wash with ethanol and cyclohexane three times, pour off the solution, and dry at 70°C for 15min to obtain a dark ...

Embodiment 3

[0059] First, in a 50 mL two-necked bottle, inject 5 mL of oleylamine and 7 mL of octadecene, and disperse the selenium powder in the mixed solvent to obtain the precursor A of the selenium source. Then, high-purity nitrogen gas was introduced to stir the mixed solution A, and a mechanical pump was used to pump air. At the same time, the temperature was raised to 130 ° C, kept for 30 minutes, and repeated several times to obtain an oxygen-free and water-vapour-free environment. After cooling down to room temperature, add 5mmol TiCl 4 , so that TiCl 4 : The molar ratio of Se is 1:2. Under continuous stirring and a protective atmosphere, the temperature was raised to 240° C. and kept for 60 minutes to complete the growth of nanocrystals, then the heating was stopped, and the reaction system was cooled to room temperature. Then, after centrifugation at 9000r / min, wash with ethanol and cyclohexane three times, pour off the solution, and dry at 75°C for 15min to obtain a dark bro...

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Abstract

The invention relates to a single-phase titanium diselenium nano-sheet prepared by a solution method and a method and an application of the nano-sheet. The method includes the steps: dispersing selenium powder in a high-boiling-point solvent to obtain precursor solution A; adding a titanium source into the precursor solution A to obtain mixed solution B; heating the mixed solution B to reach the temperature of 240-300 DEG C under continuous stirring and protective atmosphere, and keeping the temperature for 30min to 90min; cooling mixture to reach indoor temperature after temperature keepingis completed, and separating, washing and drying the mixture to obtain the single-phase titanium diselenium nano-sheet. The molar ratio of the titanium source to the selenium powder is 1:(0.4-3). By aliquid phase method, a high-temperature and time consumption solid phase stage is avoided, complex devices are omitted, the pure hexagonal-phase TiSe2 nano-sheet can be synthesized by keeping the temperature of 240-300 DEG C for 30min-90min according to the conditions such as the molar ratio of the titanium source to the selenium powder of 1: (0.4-3), and the nano-sheet can be used for the fieldof photocatalysis.

Description

technical field [0001] The invention belongs to the field of nanomaterials, and in particular relates to a single-phase titanium diselenide nanosheet prepared by a solution method, a method and an application thereof. Background technique [0002] After graphene became a star material in the field of materials research, two-dimensional layered materials have received extensive attention. When the thickness of two-dimensional layered materials is reduced to the nanometer scale, or even atomic layer thickness, the two-dimensional layered materials show their strange physical, chemical, optical, electrical and other properties. First-class universities and research institutes at home and abroad have shown great interest in two-dimensional layered materials, and have carried out research in full swing from the preparation methods of materials to their various functional applications. So far, the number of members of the two-dimensional layered material family has increased to f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/00B82Y30/00B82Y40/00B01J27/057
CPCB82Y30/00B82Y40/00C01B19/007B01J27/0573C01P2002/72C01P2004/20C01P2004/03C01P2002/84B01J35/39
Inventor 葛万银焦思怡殷立雄常哲徐美美叶晓慧张荔
Owner SHAANXI UNIV OF SCI & TECH
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