Method for synthesizing beta-phase indium selenide flaky nanocrystalline by using hydrazine hydrate-assisted polyhydric alcohol solution

A nanocrystal, hydrazine hydrate technology, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve problems such as high cost and pollution, and achieve low cost, good repeatability, and mild reaction conditions. Effect

Inactive Publication Date: 2015-01-21
TIANJIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the disadvantages of high cost and pollution in the prior art, the present invention adopts a low-carbon chain polyol solvent with less pollution, low toxicity, high boiling point and low cost as the reaction medium, adopts a polyol-based solution chemical synthesis method, and uses hydrazine hydrate As a reaction auxiliary agent, it provides a preparation In which is safe in process, green and non-toxic, simple in operation, low in cost, stable and single in the synthetic product phase, and beneficial to product purity and stoichiometric control. 2 Se 3 Flaky Nanocrystal Method

Method used

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  • Method for synthesizing beta-phase indium selenide flaky nanocrystalline by using hydrazine hydrate-assisted polyhydric alcohol solution
  • Method for synthesizing beta-phase indium selenide flaky nanocrystalline by using hydrazine hydrate-assisted polyhydric alcohol solution
  • Method for synthesizing beta-phase indium selenide flaky nanocrystalline by using hydrazine hydrate-assisted polyhydric alcohol solution

Examples

Experimental program
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Effect test

Embodiment 1

[0039] The process parameters of Examples 1-6 are injection temperature / reflux temperature. From the results in Table 2, it can be concluded that in Example 1, that is, when the injection temperature / reflow temperature is 170 / 170°C, the phase of the synthesized product is Se without In 2 Se 3 phase generated. As the injection temperature / reflow temperature increases to 210 / 210°C, Se is reduced to generate α-In 2 Se3 , the synthetic product phase of Example 3 is a single α-In 2 Se 3 . The injection temperature / reflux temperature increased from 250 / 250°C to 270 / 270°C, and the synthetic products of Examples 5 and 6 were single sheet-like β-In 2 Se 3 . The stoichiometric ratios of Examples 2-6 are all close to the stoichiometric ratio of the reaction solution In:Se=1:1.5, and Example 6 is the best. The morphology of the synthesized product increases with temperature, and the α-In 2 Se 3 to β-In 2 Se 3 Phase transition, the morphology changes from granular to flake. Fr...

Embodiment 11

[0041] The process parameter of embodiment 11,12 is that the addition amount of hydrazine hydrate is different. Wherein the synthetic product of embodiment 11 is γ-In 2 Se 3 Mixed phase with Se, Example 12 is β-In 2 Se 3 , γ-In 2 Se 3 Mixed phase with Se. From the results of the stoichiometric ratio of the synthetic products in Examples 11, 12, and 6, with the increase of hydrazine hydrate, the stoichiometric ratio of the synthetic product is closer to the ideal stoichiometric ratio of In:Se=1:1.5. At the same time, in Example 6, Se is fully reduced to form a single phase β-In 2 Se 3 . From the above analysis, it can be seen that, for the parameters of the amount of hydrazine hydrate added, Example 6 is the optimum amount of hydrazine hydrate added, which is 0.1 ml.

[0042] figure 1 It is the XRD spectrum of the synthetic product of Example 6, as can be seen from the figure that the product is a single sheet-like β-In 2 Se 3 .

[0043] figure 2 It is the SEM pi...

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Abstract

The invention discloses a method for synthesizing beta-phase indium selenide flaky nanocrystalline by using a hydrazine hydrate-assisted polyhydric alcohol solution. The method comprises the following steps: firstly, weighing 0.1mol of tetrahydrate indium chloride and dissolving into 10ml of triethylene glycol to obtain a cationic precursor solution; additionally, adding 40ml of triethylene glycol to a three-necked round-bottomed flask; adding 0.15mmol of selenium powder, adding 0.1ml of hydrazine hydrate and introducing nitrogen to obtain an anionic source reaction base fluid; putting the three-neck bottle into a thermal reaction reflux device, introducing nitrogen, slowly heating the anionic source reaction base fluid, quickly injecting the cationic precursor solution until the injection temperature / reflux temperature ranges from 250 / 250 DEG C to 270 / 270 DEG C, so as to obtain a reaction solution containing indium selenide nanocrystalline; and centrifugally separating and purifying the reaction solution to prepare In2Se3 nanocrystalline. The entire reaction of the method is mild in condition, safe, low in toxicity, simple and convenient to operate and low in cost; the product is single and stable in phase and relatively good in repeatability, and the stoichiometric ratio accords with the standard ratio.

Description

technical field [0001] The invention relates to nanometer materials, in particular to a method for synthesizing β-phase indium selenide flake nanocrystals from a polyol-based solution. Background technique [0002] Indium Selenide (In 2 Se 3 ) as a metal chalcogenide of Group III–VI has excellent visible light absorption performance and phase change storage performance, and is widely used in the fields of photodetectors, optical filter devices, sensors, solar cells, photo-water splitting components, and phase change memories. have potential application value. InSe is an n-type semiconductor with a direct bandgap. In 2 Se 3 It has a double-layer structure, and the strong chemical bond force within the layer and the weak van der Waals force between the layers make indium selenide have an anisotropic structure, which in turn has excellent electrical, optical, and magnetic properties. [0003] In 2 Se 3 It has a variety of crystal structures, namely α, β, γ, δ, and κ, am...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/04B82Y30/00B82Y40/00
CPCC01B19/04C01P2002/72C01P2002/85C01P2004/03C01P2004/64
Inventor 靳正国李彤霏王健赖俊云
Owner TIANJIN UNIV
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