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Solvothermal preparation method of NbS2 nanosheet self-assembled hollow microspheres

A hollow microsphere and nanosheet technology, which is applied in chemical instruments and methods, inorganic chemistry, niobium compounds, etc., can solve the problem that the thermal preparation method of nanosheets is not reported in literature, etc. Simple, unique looking effects

Active Publication Date: 2021-11-26
QIQIHAR UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Nb 2 Nanosheet self-assembled hollow microspheres and their solvothermal preparation methods have not been reported in the literature

Method used

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  • Solvothermal preparation method of NbS2 nanosheet self-assembled hollow microspheres
  • Solvothermal preparation method of NbS2 nanosheet self-assembled hollow microspheres

Examples

Experimental program
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Embodiment 1

[0024] (1) Measure 100ml of chloroform, remove the moisture in the chloroform by distillation with the assistance of calcium chloride or phosphorus pentoxide, and set aside.

[0025] (2) Measure 70ml chloroform, weigh 2g NbCl 5 Place in a polytetrafluoroethylene reactor liner with a capacity of 110ml, and stir for 30min.

[0026] (3) Measure 8ml of di-tert-butyl sulfide, add it to the lining of the polytetrafluoroethylene reactor and stir evenly. Close the reaction kettle, set the temperature at 220°C, and keep warm for 24 hours under magnetic stirring conditions.

[0027] (4) Centrifuge the reacted bottom sediment in a centrifuge with a rotating speed of 4000r / min, wash and centrifuge three times with deionized water and absolute ethanol respectively, and centrifuge for 5min each time to collect the washed product.

[0028] (5) The washed product was vacuum-dried at 50° C. for 4 h. For simplicity, this product is denoted as sample S1.

Embodiment 2

[0030] (1) Measure 100ml of dimethylformamide, remove the moisture in the dimethylformamide by distillation with the assistance of calcium chloride or phosphorus pentoxide, and set aside.

[0031] (2) Measure 60ml dimethylformamide, weigh 2g NbCl 5 Place in a polytetrafluoroethylene reactor liner with a capacity of 110ml, and stir for 30min.

[0032] (3) Measure 7ml of carbon disulfide, add it to the lining of the polytetrafluoroethylene reactor and stir evenly. Close the reaction kettle, set the temperature at 200°C, and keep warm for 72h under the condition of magnetic stirring.

[0033] (4) Centrifuge the reacted bottom sediment in a centrifuge with a rotating speed of 4000r / min, wash and centrifuge three times with deionized water and absolute ethanol respectively, and centrifuge for 5min each time to collect the washed product.

[0034] (5) The washed product was vacuum-dried at 50° C. for 4 h. For simplicity, this product is denoted as sample S2.

Embodiment 3

[0036] (1) Measure 100ml of acetonitrile, remove the moisture in the acetonitrile by distillation with the assistance of calcium chloride or phosphorus pentoxide, and set aside.

[0037] (2) Measure 50ml acetonitrile, weigh 2g NbCl 5 Place in a polytetrafluoroethylene reactor liner with a capacity of 110ml, and stir for 30min.

[0038] (3) Measure 10 g of thioacetamide, add it to the lining of the polytetrafluoroethylene reactor and stir evenly. Close the reaction kettle, set the temperature at 170°C, and keep warm for 24 hours under magnetic stirring conditions.

[0039] (4) Centrifuge the reacted bottom sediment in a centrifuge with a rotating speed of 4000r / min, wash and centrifuge three times with deionized water and absolute ethanol respectively, and centrifuge for 5min each time to collect the washed product.

[0040] (5) The washed product was vacuum-dried at 50° C. for 4 h. For simplicity, this product is denoted as sample S3.

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Abstract

The invention discloses a solvothermal preparation method of NbS2 nanosheet self-assembled hollow microspheres. According to the preparation method, niobium pentachloride is used as a niobium source in an organic solvent environment, diethyl sulfide or other sulfur-containing compounds are used as a sulfur source, and the NbS2 nanosheet self-assembled hollow microspheres are prepared through a high-temperature reaction for a certain time. According to the preparation method, the NbS2 nano material is prepared by a simple one-step solvothermal method, the complex preparation process of the existing NbS2 nano material is greatly optimized, and meanwhile, the obtained NbS2 hollow nano microsphere is of a hollow open pore structure and is controllable in size and morphology. According to the invention, the problem of preparing the NbS2 nano material through a solvothermal method at a relatively low temperature is solved. The adopted raw materials are cheap, the preparation process is simpler, and the product NbS2 nanosheet self-assembled hollow microspheres are unique in morphology. The NbS2 nanosheet self-assembled hollow microspheres can be applied to the fields of electromagnetic wave absorption, catalysis, energy storage, biosensing and the like.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic nanometer materials, and relates to a kind of NbS 2 A solvothermal preparation method of nanosheet self-assembled hollow microspheres. Background technique [0002] Transition metal dichalcogenides are fundamental building blocks for heterostructure design due to the many interesting properties they exhibit, such as mostly heterointerfaces, abundant active sites and appropriate defects, charge density wave states, tunable bandgap, etc. , in electronic devices, catalysis, energy storage, biosensing and some other functional fields have great potential for development, and have received extensive attention from scientists in recent years. [0003] Niobium disulfide (NbS 2 ), as a kind of transition metal dichalcogenides, has close to zero Gibbs free energy, special charge density wave, and higher than tungsten disulfide (WS 2 ), molybdenum disulfide (MoS 2 ) richer edges and active sites ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G33/00
CPCC01G33/00C01P2004/34C01P2004/45C01P2002/72C01P2004/03
Inventor 张德庆张慧斌杨秀英曹茂盛
Owner QIQIHAR UNIVERSITY
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