Novel ceramic wave-absorbing microsphere material and preparation method thereof
A technology of microspheres and ceramics, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of loss and disappearance of electromagnetic absorption performance, low ferromagnetic resonance frequency, etc., and achieve good interface effect, good fluidity and solubility. , easy-to-prepare effects
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Embodiment 1
[0024] Iron acetylacetonate powder (1 g) was added to polysilicon acetylene liquid (9 g), and an appropriate amount of tetrahydrofuran was added at the same time to completely dissolve the iron acetylacetonate powder and mix by stirring. The mixture was dropped into simethicone and stirred at 1000 rpm. After stirring for 2 hours, it was cured in an oven at 200°C for 4 hours, and then the precursor microspheres were separated from the simethicone by centrifugation;
[0025] The infrared image of the iron-containing resin microspheres obtained after separation is shown in figure 1 Shown at 2165cm -1 2040cm -1 The peaks at -Si-H bond and -C≡C- stretching vibration peaks respectively, 1260 cm -1 and 1420 cm -1 It is caused by Si-CH3 vibration. In particular, the Si-H bond of PSA reacts with iron acetylacetonate to generate a new Si-O-Fe bond corresponding to 1023 to 1016 cm -1 range, which makes -Si-O- at 1037 cm -1 The peak broadens at 2165 cm -1 The Si-H bond weakens at...
Embodiment 2
[0027] First, the nickel acetylacetonate powder (1 g) was added to the PSA liquid (9 g), and at the same time an appropriate amount of tetrahydrofuran was added to completely dissolve the nickel acetylacetonate powder and mixed by stirring. The mixture was dropped into simethicone and stirred at 1000 rpm. After stirring for 2 hours, the emulsion was cured in an oven according to the following steps: 1 hour at 180°C, 1 hour at 200°C, and 2 hours at 220°C. The precursor microspheres were then separated from the simethicone by centrifugation. After separation, pyrolysis of the polymer was carried out in a high-temperature alumina tube furnace under an ultra-high-purity nitrogen atmosphere. The tube furnace was heated from room temperature to 1000 °C at a heating rate of 3 °C / min for another 2 h. The XRD pattern of the prepared ceramic microwave-absorbing microspheres is as follows figure 2 shown. The peaks of the SiC phase appeared at 35.54°, 59.92° and 71.69°, corresponding...
Embodiment 3
[0029] First, the cobalt acetylacetonate powder (2 g) was added to the PSA liquid (8 g), and at the same time, an appropriate amount of acetone was added to completely dissolve the cobalt acetylacetonate powder and mix by stirring. The mixture was dropped into simethicone and stirred at 1000 rpm. After stirring for 2 hours, the emulsion was cured in an oven according to the following steps: 1 hour at 160°C, 1 hour at 190°C, and 2 hours at 200°C. The precursor microspheres were then separated from the simethicone by centrifugation. After separation, pyrolysis of the polymer was carried out in a high-temperature alumina tube furnace under a high-purity nitrogen atmosphere. The tube furnace was heated from room temperature to 1200 °C at a heating rate of 5 °C / min for another 4 h. The microwave-absorbing properties of the prepared ceramic microwave-absorbing microspheres are as follows: image 3 shown.
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