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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AI-Extracted 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 remo...

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.

Application Domain

Cell electrodesSecondary cells +2

Technology Topic

ElectrospinningElectro conductivity +13

Image

Examples

Experimental program(3)

Example Embodiment

[0032]Example 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 stir thoroughly to form a uniform spinning solution.

[0034](2) Put the spinning solution in step (1) into a syringe and connect it with a 0.7 mm needle. Electrospinning is carried out using electrostatic spinning equipment to obtain phosphomolybdic acid/PVP composite fiber membrane. Among them, the aluminum foil-covered cylinder is 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) Put the phosphomolybdic acid/PVP composite fiber membrane obtained in step (2) in a temperature-programmed muffle furnace, set the heating rate to 2°C/min, and react in an air atmosphere at 280°C for 2h. Then it was transferred to a tube furnace, heated to 700°C at a rate of 5°C/min under a nitrogen atmosphere and kept for 2h, and then cooled naturally to obtain a molybdenum phosphide/carbon fiber composite material.

[0036]The SEM image of the molybdenum phosphide/carbon fiber composite material prepared in Example 1 is as followsfigure 1 Shown.

[0037]The prepared molybdenum phosphide/carbon fiber composite material is used for the negative electrode of sodium ion battery for specific capacity, rate performance and cycle performance test. The test results are shown infigure 2 It can be seen from the figure that the molybdenum phosphide/carbon fiber composite material prepared in the examples of this application has a low capacity decay under high current, a high capacity retention rate, and a specific capacity of more than 100mAh/g at a current density of 5A/g .

Example Embodiment

[0038]Example 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 stir thoroughly to form a uniform spinning solution.

[0040](2) Put the spinning solution in step (1) into a syringe and connect it with a 0.7 mm needle. Electrospinning is performed using electrostatic spinning equipment to obtain composite fiber membranes. Among them, the aluminum foil-covered cylinder is 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) Place the composite fiber membrane obtained in step (2) in a temperature-programmed muffle furnace, set the heating rate to 2° C./min, and react in an air atmosphere at 280° C. for 1 hour. After that, it was transferred to a tube furnace, heated to 800°C at a rate of 2°C/min under a nitrogen atmosphere and kept for 2h, and cooled naturally to obtain a molybdenum phosphide/carbon fiber composite material.

[0042]The prepared molybdenum phosphide/carbon fiber composite material is used for the negative electrode of sodium ion battery for specific capacity, rate performance and cycle performance test. The test results are shown inimage 3 It can be seen from the figure that the molybdenum phosphide/carbon fiber material prepared in the examples of the application has excellent rate performance, and the specific capacity is more than 150 mAh/g at a current density of 2 A/g.

Example Embodiment

[0043]Example 3

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

[0045](2) Put the spinning solution in step (1) into a syringe and connect it with a 0.7 mm needle. Electrospinning is carried out using electrostatic spinning equipment to obtain phosphomolybdic acid/PVP composite fiber membrane. Among them, the aluminum foil-covered cylinder is the receiver, the negative high voltage is -2kV, and 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 a heating rate of 2°C/min, and react in an air atmosphere at 230°C for 2h. Then transferred to tube furnace, in Ar/H2Atmosphere (volume ratio Ar:H2=0.95:0.05), the temperature is increased to 800°C at a rate of 2°C/min and the temperature is kept for 2h, and the molybdenum phosphide/carbon fiber composite material is obtained after natural cooling.

[0047]The prepared molybdenum phosphide/carbon fiber composite material is used for the negative electrode of sodium ion battery for specific capacity, rate performance and cycle performance test. The test results are shown inFigure 4, It can be seen from the figure that the specific capacity above 100mAh/g can still be maintained after 1000 cycles under 1A/g current.

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

AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Examples

Example Embodiment

Example Embodiment

Example Embodiment

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Description & Claims & Application Information

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