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Method for synthesizing nickel diselenide nanocrystal in polyalcohol-base solution

A nickel diselenide, nanocrystal technology, applied in the field of nanomaterials, can solve the problems of difficult control of chemical components, unfavorable large-scale production, high toxicity of commonly used solvents, etc., and achieves the effects of good consistency, low cost and simple operation.

Inactive Publication Date: 2013-12-25
TIANJIN UNIV
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Problems solved by technology

[0004] The object of the present invention is to overcome the shortcomings of the prior art, such as time-consuming, energy-consuming, high cost, complicated operation, unfavorable for large-scale production, difficult control of chemical components, and high toxicity of commonly used solvents. For the first time, liquid-phase chemical synthesis is adopted method - hot injection method, which provides a mild reaction condition, which is beneficial to ensure product purity, controllable stoichiometric ratio, green and non-toxic, and low cost to prepare NiSe 2 nanocrystal approach

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  • Method for synthesizing nickel diselenide nanocrystal in polyalcohol-base solution
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  • Method for synthesizing nickel diselenide nanocrystal in polyalcohol-base solution

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[0022] The raw materials used in the present invention are commercially available analytically pure raw materials, and the present invention will be further described below in conjunction with the examples.

[0023] The present invention prepares NiSe in triethylene glycol system 2 The nanoparticle process is as follows:

[0024] (1) Preparation of precursor solution

[0025] Weigh 0.25mmol, that is, 0.0747g nickel nitrate hexahydrate, dissolve it in 10ml triethylene glycol, stir at room temperature for 45min, and obtain a stable nickel precursor cation source solution; add 40ml triethylene glycol to a three-neck round bottom flask, and add Selenium powder, then add 0.1g polyvinylpyrrolidone, PVP for short, and magnetically stir for 5min to obtain anion source solution; wherein the Ni / Se molar ratios are 1:2, 1:1.9, 1:1.8, 1:1.7 respectively.

[0026] (2) Synthesis of NiSe by reflux reaction 2

[0027] Put the three-necked bottle in a heat pack, inject nitrogen gas into th...

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Abstract

The invention discloses a method for synthesizing a nickel diselenide nanocrystal in a polyalcohol-base solution, which comprises the following steps: (1) weighing 0.25mmol of nickel nitrate hexahydrate, and dissolving in 10ml of triethylene glycol to obtain a nickel precursor cation source solution; adding 40ml of triethylene glycol into a three-neck round-bottom flask, adding selenium powder, and adding 0.1g of polyvinylpyrrolidone to obtain an anion source solution, wherein the Ni / Se mol ratio is respectively 1:2, 1:1.9, 1:1.8 and 1:1.7; and (2) slowly heating the anion solution to 210-270 DEG C while quickly injecting the cation source solution, and reacting under reflux to synthesize the NiSe2 nanocrystal solution. The method has the advantages mild whole reaction conditions, high safety, low toxicity, low cost, single and stable product phase and favorable repetitiveness, and is simple to operate, and the stoichiometric proportion and material feeding have favorable consistency.

Description

technical field [0001] The present invention relates to nanomaterials, in particular to a method for synthesizing NiSe in polyol-based solutions 2 nanocrystal approach. Background technique [0002] Ni-Se compounds are transition metal chalcogenide semiconductor materials, due to the Ni valence electronic structure (3d 8 4s 2 ) characteristics and the difference in electronegativity between Ni and Se lead to the existence of a variety of Ni-Se compounds, and the properties of each substance are also different. where NiSe 2 In recent years, materials have been widely concerned and applied in the fields of electricity, magnetism and optics. NiSe 2 It is a narrow bandgap semiconductor material, usually in two forms of pyrite (cubic crystal structure) and marcasite (orthorhombic crystal structure), it is a Pauli paramagnetic substance in the ground state, and the magnetic susceptibility coefficient is about 1×10 -6 emu / g shows a slight increase with increasing temperature ...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/04B82Y30/00
Inventor 靳正国刘彤李佳
Owner TIANJIN UNIV
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