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

A composite material, molybdenum phosphide technology, applied in the direction of phosphide, fiber chemical characteristics, electrochemical generator, etc., can solve the problems of corrosive waste acid, consumption of active components, consumption of template agent, etc., to improve conductivity , good magnification performance, simple operation

Inactive Publication Date: 2021-01-15
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional pore-making method usually adopts the route of using a hard template in the synthesis and then removing it by reagents. For example, in the patent (CN110479332A), phosphorus source / molybdenum source / carbon source are used as raw materials, and sodium chloride is used as a pore-forming agent. After freeze-drying, calcining , washed with water to obtain porous molybdenum phosphide nanosheets, the process is cumbersome and consumes a large amount of template agent
Or use a large number of surfactant self-assembly methods to construct the pore structure. For example, in the patent (CN110350181A), hydrofluoric acid is used to etch nano-silicon particles to form holes to prepare nano-porous silicon negative electrode materials, which requires strict pre-treatment of raw materials. processing, and the use of hydrofluoric acid consumes active components and produces corrosive spent acid

Method used

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

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) Mix 1 mL of 70% phytic acid solution with 9 mL of DMF, add 0.5 g of phosphomolybdic acid and 0.5 mL of pyrrole and continue to stir, then add 1.2 g of polyvinylpyrrolidone, and stir fully to form a uniform spinning solution.

[0039] (2) Fill the spinning solution in step (1) into a syringe. The composite fiber membrane is prepared by electrospinning with an electrospinning device. Among them, the aluminum foil-wrapped cylinder is used as the receiver, the negative high voltage is -2kV, the positive high voltage is 12kV, the receiving distance is 15cm, the relative humidity is 50%, and the ambient temperature is 50°C.

[0040] (3) Place the composite fiber membrane obtained in step (2) in a tube furnace, heat up to 800° C. at a rate of 2° C. / min under an argon atmosphere and keep it warm for 2 hours. After natural cooling, porous molybdenum phosphide / Carbon fiber composite material.

[0041] The SEM figure of the porous molybdenum phosphide / carbon fiber composite...

Embodiment 2

[0044] (1) Mix 1.5mL of 70% phytic acid solution with 8.5mL of DMF, add 0.5g of phosphomolybdic acid and 0.5mL of pyrrole and continue to stir, then add 1.2g of polyvinylpyrrolidone, and fully stir to form a uniform spinning solution.

[0045] (2) Fill the spinning solution in the step (1) into a syringe, and perform electrostatic spinning with an electrostatic spinning 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 12kV, the receiving distance is 15cm, the relative humidity is 50%, and the ambient temperature is 50°C.

[0046](3) Place the composite fiber membrane obtained in step (2) in a tube furnace, raise the temperature to 700°C at a rate of 2°C / min under nitrogen atmosphere and keep it warm for 1h, and obtain porous molybdenum phosphide / carbon fiber after natural cooling composite material.

[0047] The prepared porous molybdenum phosphi...

Embodiment 3

[0049] (1) Mix 1 mL of 70% phytic acid solution with 9 mL of DMF, add 0.5 g of phosphomolybdic acid and 1.5 mL of pyrrole and continue to stir, then add 1.2 g of polyvinylpyrrolidone, and stir fully to form a uniform spinning solution.

[0050] (2) Fill the spinning solution in the step (1) into a syringe, and perform electrostatic spinning with an electrostatic spinning 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 10kV; the receiving distance is 15cm; the relative humidity is 45%, and the ambient temperature is 55°C.

[0051] (3) The composite fiber membrane obtained in step (2) is placed in a tube furnace, under Ar / H 2 Atmosphere (volume ratio Ar:H 2 =0.95:0.05), the temperature was raised to 800°C at a rate of 2°C / min and held for 2 hours, and the porous molybdenum phosphide / carbon fiber composite material was obtained after natural coolin...

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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 porous molybdenum phosphide / carbon fiber composite material. The preparation method comprises the steps of dissolving a phosphorus source and a molybdenum source into a solution, adding a pore forming agent and a carbon source to prepare aspinning solution, carrying out electrostatic spinning, and carrying out high-temperature carbonization. A dispersed and uniform pore channel structure is generated on the surface of the fiber through shrinkage during pyrolysis of the pore forming agent, and the volume effect caused by ion intercalation and deintercalation in the cyclic process can be effectively relieved, so that the cyclic stability of the material is improved. According to the preparation method, an etching agent and a template agent do not need to be used, a large number of centrifuging and washing processes are avoided,the operation is easy, the morphology is stable and controllable, and continuous preparation is facilitated. The porous molybdenum phosphide / carbon fiber composite material prepared by the invention is used as a negative electrode of a sodium-ion battery, still keeps the specific capacity of 100mAh / g or above after being circulated for 1200 times under the current density of 1A / g, and has good rate capability.

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 porous molybdenum phosphide / carbon fiber composite material. Background technique [0002] Compared with lithium-ion batteries, the performance of sodium-ion batteries is slightly worse when discharged at a high rate, but because of its low manufacturing cost, relatively stable material structure and performance, and safe use, sodium-ion batteries have unique advantages in large-scale energy storage for power grids and other energy storage fields. own advantages. [0003] Transition metal phosphides based on conversion reaction energy storage mechanism, higher theoretical capacity and lower sodium storage voltage are known as ideal candidates for anode materials for sodium ion batteries, but phosphides have poor rate performance and large volume in cycles Bloat hinders its commercializ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/08D01F9/21D01F9/22H01M4/58H01M4/62H01M10/054
CPCC01B25/08C01P2004/03C01P2006/40D01F9/21D01F9/22H01M4/5805H01M4/625H01M10/054Y02E60/10
Inventor 张海燕刘振江
Owner GUANGDONG UNIV OF TECH
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