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A kind of preparation method of phosphorus and selenium co-doped niobium disulfide nanomaterials

A niobium disulfide, nanomaterial technology, applied in chemical instruments and methods, nanotechnology, niobium compounds, etc., to achieve the effect of continuous doping process, huge application value, and high purity

Active Publication Date: 2022-07-01
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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  • A kind of preparation method of phosphorus and selenium co-doped niobium disulfide nanomaterials
  • A kind of preparation method of phosphorus and selenium co-doped niobium disulfide nanomaterials
  • A kind of preparation method of phosphorus and selenium co-doped niobium disulfide nanomaterials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0036] 4mL of oleylamine was put into a three-necked flask for magnetic stirring, heated to 130°C under the protection of nitrogen, kept for 20 minutes, then naturally cooled, 1.6mmol of niobium pentachloride and degassed oleylamine were placed in the three-necked flask. Mixed in medium and magnetically stirred, heated to 300 °C under the protection of nitrogen, injected with 8 mmol CS 2 The sulfur source was kept at this temperature for 2 hours, and then naturally lowered to 200 °C. The TOP-Se (1mmol-0.3mmol) solution prepared in advance was injected, and the temperature of the system was rapidly increased to 320 °C. After 1 hour, 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 pattern (XRD) of the phosphorus-selenium co-doped niobium disulfide nan...

Embodiment 2 2

[0037] Example 2 Preparation of niobium disulfide nanosheets

[0038] 4 mL of oleylamine and 1.6 mmol of niobium pentachloride were placed in a three-necked flask for magnetic stirring. 2 The sulfur source was kept at this temperature for 3 hours, then the temperature was naturally cooled, the solution was naturally cooled to room temperature, the samples were washed with n-hexane and methanol, and then freeze-dried. Figures 6 to 7 Scanning electron micrographs with a scale bar of 3 μm and 2 μm, respectively, are distinct from the nanoflowers and are uniformly distributed. Figures 8 to 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, around 200 nm.

[0039] Surface scanning was carried out on the phosphorus-selenium co-doped niobium disulfide nanoflowers and niobium disulfide nanosheets prepared in Example 1 and Example 2, through Figures 10 to...

Embodiment 3

[0040] Example 3 Electrocatalytic hydrogen evolution performance test

[0041] The electrochemical catalytic properties of phosphorus and selenium co-doped niobium disulfide nanoflowers and niobium disulfide nanosheets were measured using an electrochemical workstation. like Figure 20As shown, for the co-doped niobium disulfide nanoflowers with phosphorus and selenium, the niobium disulfide nanosheets in the acidic solution of 0.5MH 2 SO 4 Linear sweep voltammetry and Tafel slope curves in . It can be seen that after the control of the morphology and the influence of phosphorus and selenium co-doping, at 10 mA cm -2 The overpotential increases from -0.534 V for niobium disulfide nanosheets to -0.368 V for phosphorus-selenium co-doped niobium disulfide nanoflowers at a current density of The current density of nanoflowers can reach 130 mA cm -2 , while at the same overpotential, the current density of the niobium disulfide nanosheets is only 13.8 mAcm -2 . like Figure...

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Abstract

The preparation method of a phosphorus-selenium co-doped niobium disulfide nanomaterial of the invention belongs to the technical field of preparation of clean energy storage and conversion materials. The niobium pentachloride and the degassed oleylamine were mixed and stirred magnetically, heated to 300 °C under the protection of nitrogen, and injected into CS 2 The sulfur source was kept at this temperature for 2 hours, and then naturally lowered to 200°C. The TOP-Se solution prepared in advance was injected. The temperature of the system was rapidly increased to 320°C and kept for 1 hour. , to obtain phosphorus-selenium co-doped niobium disulfide nanoflowers. The invention realizes for the first time the synthesis of niobium disulfide nanomaterials with controllable phosphorus and selenium co-doping morphology, fills the vacancy of such transition metal sulfide synthesis technology, and provides conditions for its research 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 as a renewable and clean energy to replace traditional fossil fuels. Electrolyzed water, the cleanest and most sustainable way to produce hydrogen, 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 application in practical production is limited due to their high price and scarce reserves. Therefore, designing and developing cost-effective hydrogen evolution reaction catalysts is crucial for large-scale electrolysis of water for hydro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/04B82Y40/00C01G33/00
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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