Production of si/c composite particles
A technology of composite particles and pre-compound particles, which is applied in the direction of electrochemical generators, structural parts, electrical components, etc., can solve the problems of expensive, large particle volume increase, inconvenience, etc.
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Embodiment 1
[0106] Embodiment 1 (comparative):
[0107] Spray drying of PAN: Formation of aggregated PAN fibers:
[0108] 12.5 g of polyacrylonitrile (PAN) was dissolved in 500 ml of dimethylformamide (DMF) at room temperature. The resulting dispersion was dried using a Model B-290 laboratory spray dryer with a B-295 inert circuit ( GmbH) and B-296 dehumidifier ( GmbH) (nozzle tip 0.7mm; nozzle cap 1.4mm; nozzle temperature 130°C; N 2 Air flow ~40; aspirator 100%; pump 20%) for spraying and drying.
[0109] figure 1 A SEM image (2500X magnification) of the obtained powder is shown. The product is colorless and consists of fiber coils of nanoscale PAN fibers, and individual shaped PAN spheres.
Embodiment 2
[0110] Embodiment 2 (comparative):
[0111] Production of spray-dried and aggregated C particles of PAN:
[0112] 1.5 g of polyacrylonitrile (PAN) was dissolved in 100 ml of dimethylformamide (DMF) at room temperature. The resulting dispersion was dried using a Model B-290 laboratory spray dryer with a B-295 inert circuit ( GmbH) and B-296 dehumidifier ( GmbH) (nozzle tip 0.7mm; nozzle cap 1.4mm; nozzle temperature 130°C; N 2 Air flow ~30; aspirator 100%; pump 20%) for spraying and drying. A colorless powder was obtained.
[0113] 647 mg of this powder was placed in a fused silica calciner (QCS GmbH) and cascaded conditioning was used, including the use of argon / H 2 As an inert gas N-type probe element, carbonization was carried out in a three-zone tube furnace (TFZ 12 / 65 / 550 / E301; Carbolite GmbH): first, the heating rate was 10 °C / min, the temperature was 300 °C, and the holding time was 90 min. Ar / h 2 The flow rate is 200ml / min; then the heating rate is 10°C / min,...
Embodiment 3
[0115] Embodiment 3 (comparative):
[0116] Production of Aggregated Si / C Composite Particles:
[0117] 12.0 g of polyacrylonitrile (PAN) was dissolved in 800 ml of dimethylformamide (DMF) at room temperature. 8.6 g of silicon nanopowder suspension (20.3% in ethanol, corresponding to 1.75 g of silicon) were dispersed in this PAN solution by ultrasound (Hielscher UIS250V; amplitude 80%, period: 0.9; duration: 30 min). The resulting dispersion was dried using a Model B-290 laboratory spray dryer with a B-295 inert circuit ( GmbH) and B-296 dehumidifier ( GmbH) (nozzle tip 0.7mm; nozzle cap 1.4mm; nozzle temperature 130°C; N 2 Air flow ~30; aspirator 100%; pump 20%) for spraying and drying. 11.1 g of brown powder were obtained (yield 80%).
[0118] 10.6 g of the resulting Si / PAN pre-composite was placed in a sintered quartz sintered boat (QCS GmbH) and cascade conditioning was used, including the use of argon / H 2 N-type thermocouples used as an inert gas were carbonized...
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