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Preparation method of phosphorus-selenium co-doped niobium disulfide nano material

A technology of niobium disulfide and nanomaterials, applied in chemical instruments and methods, inorganic chemistry, niobium compounds, etc., to achieve the effects of overcoming uneven product morphology, high purity and simple production process

Active Publication Date: 2021-07-23
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the method of preparing phosphorus-selenium co-doped niobium disulfide by thermal injection has not been reported yet.

Method used

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  • Preparation method of phosphorus-selenium co-doped niobium disulfide nano material
  • Preparation method of phosphorus-selenium co-doped niobium disulfide nano material
  • Preparation method of phosphorus-selenium co-doped niobium disulfide nano material

Examples

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Effect test

Embodiment 1

[0035] Example 1 Preparation of phosphorus-selenium co-doped niobium disulfide nanoflowers

[0036] Put 4mL of oleylamine into a three-necked flask for magnetic stirring, raise the temperature to 130°C under the protection of nitrogen, keep it for 20 minutes, then cool down naturally, put 1.6mmol of niobium pentachloride and degassed oleylamine in the three-necked flask Mix in medium and magnetically stir, raise the temperature to 300°C under the protection of nitrogen, inject 8mmol CS 2 Sulfur source, kept at this temperature for 2 hours, then naturally lowered to 200°C, injected the prepared TOP-Se (1mmol-0.3mmol) solution, the system temperature rose rapidly to 320°C, kept for 1 hour, and the reaction ended , the solution was naturally cooled to room temperature, washed with n-hexane and methanol, and then freeze-dried. like figure 1 As shown, the X-ray diffraction spectrum picture (XRD) of phosphorus-selenide co-doped niobium disulfide nanoflowers is very well compared w...

Embodiment 2 2

[0037] The preparation of embodiment 2 niobium disulfide nanosheets

[0038] Put 4 mL of oleylamine and 1.6 mmol of niobium pentachloride into a three-neck flask for magnetic stirring, and raise the temperature to 300 °C at a rate of 5 °C / min under the protection of nitrogen, and inject 8 mmol of CS 2 The sulfur source was kept at this temperature for 3 hours, then the temperature was naturally lowered, the solution was naturally cooled to room temperature, the sample was washed with n-hexane and methanol, and then freeze-dried. Figure 6~7 Scanning electron micrographs with scale bars of 3 μm and 2 μm, respectively, which are obviously different from nanoflowers and evenly distributed. Figure 8-9 Transmission electron micrographs with scale bars of 500 nm and 200 nm, respectively. It is clearly seen that NbS 2 Nanosheets and NbS 2 Nanoflowers have a smaller diameter in comparison, about 200nm.

[0039] The phosphorus-selenium co-doped niobium disulfide nanoflowers and ni...

Embodiment 3

[0040] Embodiment 3 electrocatalytic hydrogen evolution performance test

[0041] Electrochemical catalytic properties of phosphorus-selenide co-doped niobium disulfide nanoflowers and niobium disulfide nanosheets were measured by electrochemical workstation. like Figure 20As shown, it is phosphorus selenium co-doped niobium disulfide nanoflowers, niobium disulfide nanosheets in acidic solution 0.5MH 2 SO 4 Linear sweep voltammetry curves and Tafel slope curves in . It can be seen that after the regulation of morphology and the influence of phosphorus-selenium co-doping, at 10mA cm -2 The overpotential increased from -0.534V of NBS nanosheets to -0.368V of P-Se co-doped NbS nanoflowers under the current density of -0.585V. The current density of nanoflowers can reach 130mA cm -2 , while at the same overpotential, the current density of niobium disulfide nanosheets is only 13.8mAcm -2 . like Figure 21 As shown, the change of Tafel slope is also obvious, from 406.4mV / d...

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Abstract

The invention discloses a preparation method of a phosphorus-selenium co-doped niobium disulfide nano material, and belongs to the technical field of clean energy storage and conversion material preparation. The preparation method comprises the following steps: mixing niobium pentachloride and degassed oleylamine, performing magnetic stirring, performing heating to 300 DEG C under the protection of nitrogen, injecting a CS2 sulfur source, keeping for 2 hours at the temperature, performing natural cooling to 200 DEG C, injecting a TOP-Se solution prepared in advance, quickly heating the system to 320 DEG C, keeping for 1 hour, ending the reaction, and performing natural cooling, washing and freeze-drying to obtain the niobium-doped carbon quantum dot. The phosphorus and selenium co-doped niobium disulfide nanoflower is obtained. According to the invention, the synthesis of the phosphorus-selenium co-doped niobium disulfide nano material with controllable morphology is realized for the first time, the vacancy of the transition metal sulfide synthesis technology is filled, and conditions are provided for the research of the nano material in the field of catalytic materials.

Description

technical field [0001] The invention belongs to the technical field of preparation of clean energy storage and conversion materials, in particular to a method for preparing phosphorus-selenium co-doped niobium disulfide nanomaterials. Background technique [0002] h 2 Because of its wide range of sources, high combustion calorific value, and non-polluting products, it is considered to be a renewable and clean energy that replaces traditional fossil fuels. Electrolyzed water is the cleanest and most sustainable method of hydrogen production, and has become an important direction for the development of hydrogen production in the future. Pt-based noble metals have excellent performance in the hydrogen evolution reaction (HER) of water electrolysis, but their high price and scarce reserves limit their application in practical production. Therefore, the design and development of economical and efficient hydrogen evolution reaction catalysts is crucial for large-scale hydrogen p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G33/00
CPCC01G33/00C01P2004/03C01P2004/04C01P2004/61C01P2004/62
Inventor 肖冠军沈威刘锦阳隋永明邹勃
Owner JILIN UNIV
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