Self-supporting phosphorus/carbon three-dimensional conductive network composite electrode material and preparation method and application thereof
A conductive network and composite electrode technology, applied in the field of nanomaterials and electrochemistry, can solve the problems of poor cycle stability, poor rate performance, poor conductivity of phosphorus-based materials, etc., and achieve high reversible charge-discharge specific capacity, excellent conductivity, high Effect of specific capacity and cycle stability
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[0039] The embodiment of the present invention provides a preparation method of a self-supporting phosphorus / carbon three-dimensional conductive network composite electrode material, including steps:
[0040] S1. Soak bacterial cellulose membrane in ammonium dihydrogen phosphate aqueous solution, freeze and dry the soaked bacterial cellulose membrane; ammonium dihydrogen phosphate inorganic salt can produce more pores and reduce bacteria in the subsequent high-temperature sintering process Volume change of the cellulose membrane;
[0041] S2, sintering the freeze-dried bacterial cellulose film under an inert atmosphere;
[0042] S3, mixing the sintered bacterial cellulose membrane with red phosphorus, and vacuum sintering to obtain a phosphorus-carbon composite material;
[0043] S4. Washing the phosphorus-carbon composite material with carbon disulfide, washing away the by-product white phosphorus produced during the evaporation and condensation of red phosphorus, and drying...
Embodiment 1
[0059] The present embodiment provides the preparation method of self-supporting phosphorus / carbon three-dimensional conductive network composite electrode material, and concrete steps are as follows:
[0060] 1) Soak an appropriate amount of commercial bacterial cellulose membrane in 50mmol / L ammonium dihydrogen phosphate aqueous solution, and stir slowly for 3 days in a water bath at 25°C; cut the soaked bacterial cellulose membrane into a size of about 5cm×5cm Size, frozen in a liquid nitrogen (-196°C) environment; then transfer the sample to a bulk tray dryer for freeze-drying at a sublimation temperature of -50°C and a pressure of 0.035mbar;
[0061] 2) Using a tube furnace, the freeze-dried bacterial cellulose membrane was heated in a nitrogen atmosphere at 2°C min -1 The heating rate is increased to 400°C, kept for 1 hour, and then at 5°C min -1 The heating rate is increased to 800 ° C, and the temperature is kept for 2 hours;
[0062] 3) Mix the sintered bacterial ce...
Embodiment 2
[0073] This embodiment provides the preparation method of self-supporting phosphorus / carbon three-dimensional conductive network composite electrode material, and the difference with embodiment 1 is:
[0074] In step 3), the sintered bacterial cellulose film is mixed with the ground red phosphorus in a weight ratio of 1:2;
[0075] Other steps and parameters are all the same as in Example 1.
[0076] The self-supporting phosphorus / carbon three-dimensional conductive network composite electrode material prepared in this embodiment 2, at 100mA g -1 Under the current density, the first discharge specific capacity can reach 759mAh / g, the charge specific capacity is 504mAh / g, the discharge specific capacity after 250 cycles is 126mAh / g, and the capacity retention rate is 25%. After analysis, it can be speculated that the increase in the relative content of red phosphorus leads to more red phosphorus loaded on the outside of the three-dimensional carbon fiber, rather than confined ...
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