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Preparation method and application of molybdenum phosphide/carbon fiber composite material

A composite material and carbon fiber technology, applied in the direction of phosphide, fiber chemical characteristics, rayon manufacturing, etc., can solve the problems of difficult removal of long-chain organic solvents, corrosiveness, phosphine toxicity, etc., to improve cycle stability, The effect of strong solubility and high redox activity

Pending Publication Date: 2021-01-22
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the most reported synthetic routes generally use organic phosphorus sources with high boiling points in the oil phase under an inert atmosphere. The disadvantages are that the reaction is flammable and corrosive at a relatively high decomposition temperature (300°C), and the long-chain organic solvents Difficult to remove
Another common synthetic route uses sodium hypophosphite to decompose at the intake end to generate phosphine, which is entrained by inert gas and reacts with metal precursors (metal oxides, hydroxides, metal organic framework compounds, etc.) to synthesize phosphides. The downside is that phosphine is extremely toxic and deadly

Method used

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  • Preparation method and application of molybdenum phosphide/carbon fiber composite material
  • Preparation method and application of molybdenum phosphide/carbon fiber composite material
  • Preparation method and application of molybdenum phosphide/carbon fiber composite material

Examples

Experimental program
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Effect test

Embodiment 1

[0033] (1) Mix 0.5 mL of 70% phytic acid solution with 9.5 mL of DMF, add 0.5 g of phosphomolybdic acid and 1.5 g of polyvinylpyrrolidone, and fully stir to form a uniform spinning solution.

[0034] (2) Fill the spinning solution in step (1) into a syringe and connect it with a 0.7mm needle. Electrospinning is carried out by using an electrospinning device to obtain a phosphomolybdic acid / PVP composite fiber membrane. Among them, the aluminum foil-wrapped cylinder is used as the receiver, the negative high voltage is -2kV, the positive high voltage is 14kV, the receiving distance is 15cm, the relative humidity is 50%, and the ambient temperature is 50°C.

[0035] (3) Place the phosphomolybdic acid / PVP composite fiber membrane obtained in step (2) in a temperature-programmed muffle furnace, set the heating rate at 2°C / min, and react in an air atmosphere of 280°C for 2h. Then it was transferred to a tube furnace, and the temperature was raised to 700°C at a rate of 5°C / min und...

Embodiment 2

[0039] (1) Mix 1 mL of 70% phytic acid solution with 9 mL of DMF, add 0.5 g of phosphomolybdic acid and 0.6 g of polyacrylonitrile, and fully stir to form a uniform spinning solution.

[0040] (2) Fill the spinning solution in step (1) into a syringe and connect it with a 0.7mm needle. Electrospinning is carried out by using an electrospinning device to obtain a composite fiber membrane. Among them, the aluminum foil-wrapped cylinder is used as the receiver, the negative high voltage is -2kV, the positive high voltage is 14kV, the receiving distance is 15cm, the relative humidity is 50%, and the ambient temperature is 50°C.

[0041] (3) The composite fiber membrane obtained in step (2) was placed in a temperature-programmed muffle furnace with a heating rate of 2° C. / min, and reacted in an air atmosphere of 280° C. for 1 h. Then it was transferred to a tube furnace, and the temperature was raised to 800°C at a rate of 2°C / min under a nitrogen atmosphere and kept for 2h. After...

Embodiment 3

[0044] (1) Mix 0.5mL of 70% phytic acid solution with 9.5mL of DMF, add 0.25g of phosphomolybdic acid and 1.5g of polyvinylpyrrolidone, and fully stir to form a uniform spinning solution.

[0045](2) Fill the spinning solution in step (1) into a syringe and connect it with a 0.7mm needle. Electrospinning is carried out by using an electrospinning device to obtain a phosphomolybdic acid / PVP composite fiber membrane. Among them, the aluminum foil-wrapped cylinder is used as the receiver, the negative high voltage is -2kV, the positive high voltage is 14kV; the receiving distance is 15cm; the relative humidity is 40%, and the ambient temperature is 55°C.

[0046] (3) Place the phosphomolybdic acid / PVP composite fiber membrane obtained in step (2) in a temperature-programmed muffle furnace, set the heating rate at 2°C / min, and react in an air atmosphere of 230°C for 2h. transferred to a tube furnace under Ar / H 2 Atmosphere (volume ratio Ar:H 2 =0.95:0.05), the temperature was r...

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Abstract

The invention belongs to the technical field of transition metal phosphide composite materials. The invention provides a preparation method and application of a molybdenum phosphide / carbon fiber composite material. The preparation method comprises the steps of preparation of a spinning solution from a phosphorus source, a molybdenum source and a carbon source, electrostatic spinning, pre-oxidationand high-temperature carbonization, and the preparation method provided by the invention is simple to operate and can realize continuous production. Phosphomolybdic acid is dissolved in a phytic acidsolution to prepare the spinning solution, and the prepared spinning solution is stable and high in dispersity; the interaction force between transition metal and phosphide can be enhanced, and the phosphorus content of a product can be increased; the conductivity of the spinning solution is effectively improved, and the cycling stability and the rate capability of the molybdenum phosphide / carbonfiber composite material are improved. The molybdenum phosphide / carbon fiber composite material prepared by the invention is high in specific capacity, stable in circulation and excellent in rate capability when being applied to a negative electrode of a sodium-ion battery. The molybdenum phosphide / carbon fiber composite material still keeps the specific capacity of 100 mAh / g or above after 1000times of circulation under the current density of 1A / g, and thus is high in capacity retention rate.

Description

technical field [0001] The application belongs to the technical field of transition metal phosphide composite materials, and in particular relates to a preparation method and application of a molybdenum phosphide / carbon fiber composite material. Background technique [0002] The low cost and abundance of sodium sources and the similarity in chemical properties and electrochemical behavior between sodium and lithium make sodium-ion batteries considered to be an ideal replacement for lithium-ion batteries, but sodium-ion batteries suffer from poor cycle stability and low The capacity limits its large-scale energy storage applications. Anode is an important part of Na-ion batteries, and transition metal phosphides are promising anode materials for Na-ion batteries due to their low intercalation voltage, low polarization, and high capacity. Currently, transition metal phosphides have been synthesized by hydrothermal / solvothermal methods, high-energy ball milling, electrodeposit...

Claims

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Application Information

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IPC IPC(8): D01F9/21D01F9/22D01F1/10C01B25/08H01M4/58H01M4/62H01M10/054
CPCD01F9/21D01F9/22D01F1/10C01B25/08H01M4/5805H01M4/625H01M10/054Y02E60/10
Inventor 刘振江张海燕
Owner GUANGDONG UNIV OF TECH
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