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Triangular-pyramid-shaped Ni3S2.9 homogeneous superlattice film electrode material and preparation method and application thereof

A thin-film electrode, superlattice technology, applied in active material electrodes, nanotechnology for materials and surface science, negative electrodes, etc., can solve problems such as low crystal electron mobility, and achieve simple process and good electrical conductivity. , the effect of good electrochemical properties

Active Publication Date: 2019-12-06
XUCHANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In these heterostructures, the heterogeneous interface can induce cross-arrangement of band edges, improve the band edge structure at the interface, and improve the mobility of electrons at the interface to a certain extent, but the problem of low electron mobility inside the crystal still remains. Difficult to solve

Method used

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  • Triangular-pyramid-shaped Ni3S2.9 homogeneous superlattice film electrode material and preparation method and application thereof
  • Triangular-pyramid-shaped Ni3S2.9 homogeneous superlattice film electrode material and preparation method and application thereof
  • Triangular-pyramid-shaped Ni3S2.9 homogeneous superlattice film electrode material and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0043] In a 50mL round-bottomed flask, 3.0mmol (96.0mg) of sulfur powder and 25mL of 6mol / L NaOH aqueous solution were refluxed at 90°C for 3 hours to obtain NaOH containing 2 S, Na 2 S 2 and Na 2 S 3 Pale yellow alkaline aqueous solution of polysulfides.

[0044] Analysis results of active sulfur components: The light yellow alkaline aqueous solution was used to detect the species category of active sulfur by ultraviolet-visible absorption (UV-vis) spectroscopy. Such as figure 1 shows that the strong absorption edge in the range of 250–280nm is the S 2- The characteristic absorption of , while the strong absorption peak at 300 nm originates from S 2 2- , the weaker absorption peak at 370 nm originates from S 3 2- , without the absorption peaks of other sulfur species (S 4 2- , S 5 2- and S 6 2- Absorption peaks at 420nm, 438nm and 450nm respectively) appear in the absorption spectrum, indicating that the active sulfur component of the light yellow alkaline aque...

Embodiment 2

[0046] Take nickel foil (0.1072g, 1.8mmol) with an area of ​​1cm×2cm and place it in a polytetrafluoroethylene liner of a 20mL reactor, add 2mL of the polysulfide light yellow alkaline aqueous solution prepared in Example 1, and seal the reaction Place the kettle in a constant temperature drying oven, control the temperature at 180°C, react at a constant temperature for 12 hours, and cool to room temperature naturally; take out the reacted nickel foil, wash it 4 times with distilled water and absolute ethanol successively, and vacuum dry the oven (0.1 Pa) Dry at 60°C for 30min to obtain S 2 Doped nickel-based sulfide superlattice thin-film electrode materials.

[0047] Product analysis results: powder X-ray diffraction (XRD) analysis shows that the product has hexagonal phase Ni 3 S 2 All the characteristic diffraction peaks, without any impurity diffraction peaks, but the diffraction angle of the diffraction peaks is slightly larger than that of the hexagonal phase Ni 3 S ...

Embodiment 3

[0049] Take nickel foil (0.1071g, 1.8mmol) with an area of ​​1cm × 2cm and place it in a polytetrafluoroethylene liner of a 20mL reactor, add 2mL of the polysulfide light yellow alkaline aqueous solution prepared in Example 1, and seal the reaction Place the kettle in a constant temperature drying oven, control the temperature at 160°C, react at a constant temperature for 12 hours, and cool to room temperature naturally; take out the reacted nickel foil, wash it 4 times with distilled water and absolute ethanol successively, and vacuum dry the oven (0.1 Pa) Dry at 60°C for 30min to obtain S 2 Doped nickel-based sulfide thin film materials.

[0050] Product analysis results: The elemental composition of the product is Ni by EDS elemental analysis 3 S 2.7 (Ni:S=52.63:47.37), according to the formula Ni 3 S 2-x (S 2 ) x , whose chemical formula can be expressed as Ni 3 S 1.3 (S 2 ) 0.7 , 35% of the S atoms in the lattice are covered by S 2 replace. Powder X-ray diffra...

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Abstract

The invention discloses a triangular-pyramid-shaped Ni3S2.9 homogeneous superlattice film electrode material and a preparation method and application thereof. The method comprises the steps: preparingpolysulfide light yellow alkaline aqueous solution (containing Na2S, Na2S2 and Na2S3) through the simple chemical reaction between sulfur powder and NaOH aqueous solution, and then carrying out hydrothermal reaction with nickel foil; adjusting the temperature of hydrothermal reaction to achieve the balanced distribution of the S2 doped atoms in Ni3S2 crystal lattices, and finally obtaining the S2doped Ni3S2.9 superlattice thin film electrode material with the chemical composition of Ni3(S)1.1(S2)0.9. The prepared Ni3(S)1.1(S2)0.9 superlattice is of a multi-order triangular-pyramid-shaped structure and uniformly grows on a nickel foil substrate, and the superlattice structure is composed of Ni-S and Ni-S2 atomic layers which are periodically alternated. According to the method, water is used as a reaction medium, no organic solvent, additive or surfactant is used, and the method belongs to an environment-friendly reaction. Because the raw materials are easy to obtain, the price is low, the operation is simple, a superlattice product with high additional value is obtained by a wet chemical method, and considerable economic benefits are achieved.

Description

technical field [0001] The invention belongs to the field of inorganic nanometer materials, in particular to a kind of triangular tower conical Ni 3 S 2.9 Preparation method of homogeneous superlattice material and its application as thin film electrode material. Background technique [0002] Thin-film electrode materials have broad application prospects in energy storage devices such as lithium-ion batteries and supercapacitors. Carbon-based electrode materials are commonly used as negative electrode materials in energy storage devices such as commercial lithium-ion batteries and supercapacitors due to their good conductivity. However, the low energy storage specific capacity of carbon-based electrode materials restricts the further improvement of the performance of energy storage devices. . At present, the scientific community is focusing on exploring and finding high specific capacity electrode materials to replace carbon-based electrode materials to obtain high energy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01G11/30H01G11/24H01G11/26C01B21/086B82Y30/00H01M10/0525
CPCB82Y30/00C01B21/0865C01P2002/72C01P2002/84C01P2004/03H01G11/24H01G11/26H01G11/30H01M4/5815H01M10/0525H01M2004/021H01M2004/027Y02E60/10
Inventor 高远浩韩雪鹏周文嵩岳红伟李伟雷岩
Owner XUCHANG UNIV
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