A kind of preparation method of acid niobium oxygen monoatomic layer sheet

A technology of niobium oxyphosphate and niobium oxyphosphate precursors, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., to achieve the effects of high efficiency, high concentration, and high proportion of monolayers

Active Publication Date: 2022-06-21
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It should be pointed out that most of the niobium oxyphosphate materials reported in the existing literature are three-dimensional mesoporous systems, and there are no publications focusing on the synthesis and control of layered phase acid niobium oxyphosphate and the exfoliation of single-atom thin layer structures.

Method used

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  • A kind of preparation method of acid niobium oxygen monoatomic layer sheet
  • A kind of preparation method of acid niobium oxygen monoatomic layer sheet
  • A kind of preparation method of acid niobium oxygen monoatomic layer sheet

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Experimental program
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Effect test

Embodiment 1

[0028] Weigh 0.5 g of commercial grade niobium oxalate powder, transfer it to a 250 mL three-necked flask that has been pre-cleaned and dried, and add 80 mL of deionized water and 5 mL of commercial grade phosphoric acid in turn; The three-necked flask was transferred and fixed on the oil bath reaction system equipped with a condensation reflux device, and the reaction solution was continuously stirred until a transparent and clear solution was formed, and then the reaction temperature was adjusted to 120 ° C for 15 hours of reaction. After the reaction, the system was cooled to room temperature, and the white precipitated product at the bottom of the bottle was taken and transferred to a Buchner funnel completely sealed on the suction filter bottle with two layers of filter paper inside, and the white product was repeatedly pumped five times with deionized water. Filter and wash, and transfer the fully washed product to a blast drying oven and dry it at 60 °C for 8 hours to ob...

Embodiment 2

[0030] Weigh 0.5 g of commercial grade niobium oxalate powder, transfer it to a 250 mL three-necked flask that has been pre-cleaned and dried, and add 80 mL of deionized water and 5 mL of commercial grade phosphoric acid in turn; The three-necked flask was transferred and fixed on the oil bath reaction system equipped with a condensation reflux device, and the reaction solution was continuously stirred until a transparent and clear solution was formed, and then the reaction temperature was adjusted to 120 ° C for 15 hours of reaction. After the reaction, the system was cooled to room temperature, and the white precipitated product at the bottom of the bottle was taken and transferred to a Buchner funnel completely sealed on the suction filter bottle with two layers of filter paper inside, and the white product was repeatedly pumped five times with deionized water. Filter and wash, and transfer the fully washed product to a blast drying oven and dry it at 60 °C for 8 hours to ob...

Embodiment 3

[0032]Weigh 0.5 g of commercial grade niobium oxalate powder, transfer it to a 250 mL three-necked flask that has been pre-cleaned and dried, and add 80 mL of deionized water and 5 mL of commercial grade phosphoric acid in turn; The three-necked flask was transferred and fixed on the oil bath reaction system equipped with a condensation reflux device, and the reaction solution was continuously stirred until a transparent and clear solution was formed, and then the reaction temperature was adjusted to 120 ° C for 15 hours of reaction. After the reaction, the system was cooled to room temperature, and the white precipitated product at the bottom of the bottle was taken and transferred to a Buchner funnel completely sealed on the suction filter bottle with two layers of filter paper inside, and the white product was repeatedly pumped five times with deionized water. Filter and wash, and transfer the fully washed product to a blast drying oven and dry it at 60 °C for 8 hours to obt...

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Abstract

The invention belongs to the technical field of chemical material synthesis, in particular to a method for preparing acid niobium oxygen monoatomic layer flakes. The method of the invention comprises: adopting a chemical liquid phase synthesis method to prepare a precursor block of acid niobium phosphate, washing and drying the block to obtain a powder; adopting an ultrasonic solvent-assisted stripping method to prepare acid niobium phosphate The monoatomic layer sheet is a uniform and stable ultra-thin nanosheet colloid. The prepared monoatomic layer flakes of acid niobium oxygen phosphate have a lateral size of tens of nanometers to hundreds of nanometers and a thickness of about 1 nm, and can realize stable dispersion at a high concentration of 10 mg / mL in aqueous phase or ethanol solvent. The synthesis and exfoliation yields achieved using this method can be stably maintained above 98%. The method of the invention is simple, convenient, safe and efficient, and has potential value for the application research of layered acid phosphorus niobium oxide in the fields of electrochemical energy storage, photoelectric conversion devices, chemical catalysis, electrocatalysis and the like.

Description

technical field [0001] The invention belongs to the technical field of chemical material synthesis, and in particular relates to a preparation method of acid niobium phosphate monoatomic layer flakes. Background technique [0002] Since British scientists exfoliated graphene with a thickness of a single carbon atom from pyrolytic graphite in 2004, this ultra-thin two-dimensional material is characterized by its structural characteristics of single or multiple carbon atomic layers, extremely high electron mobility High efficiency, good mechanical flexibility, chemical stability and optical transparency, as well as excellent electrical and thermal conductivity, have begun to show broad application prospects in lithium-ion batteries, supercapacitors, solar cells, thermally conductive films, etc. Taking graphene as an opportunity and breakthrough, a series of two-dimensional layered materials such as hexagonal boron nitride (h-BN), transition metal dichalcogenides (TMDs), layere...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/37
CPCC01B25/372C01P2002/72C01P2004/04
Inventor 胡林峰武泽懿江乐田文超
Owner FUDAN UNIV
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