Rod-like niobium pentoxide template grain and preparation method thereof
A technology of niobium pentoxide and crystal grains, which is applied in the field of rod-shaped niobium pentoxide template grains and its preparation, which can solve the problems of unsuitable nanorods and achieve the effect of improving piezoelectric performance and simple preparation process
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[0032] As an example, specifically, the preparation method of the present invention may include the following steps.
[0033] (1) Weigh Nb according to the ratio of raw material and molten salt 1:1~10 (mass ratio) 2 O 5 And soluble sodium salt powder, pour ethanol into it, and use ZrO 2 Balls, steel balls, or agate balls are used as media and mixed in a ball mill for 1 to 3 hours. Wherein, the soluble sodium salt may be at least one of sodium chloride, sodium nitrate, sodium sulfate and sodium carbonate. The ball mill may be, for example, a planetary ball mill. Preferably, before weighing the raw material powder, it can be baked at 100°C to 150°C for more than 3 hours to obtain a dry raw material powder.
[0034] (2) Heat and dry the raw materials after ball milling, and put them into a closed crucible for synthesis: put the crucible with powder into a heating device such as a muffle furnace, and quickly heat up to 1000 at a rate of 5-10°C / min ~1100℃, after incubation for 40~80, ...
Embodiment 1
[0039] ① Ingredients ball mill: Weigh AR grade Nb 2 O s (99.96%) 40.1263g, AR grade NaCl (99.80%) 40.1266g, add a certain amount (depending on the fluidity of the slurry) of absolute ethanol, and use ZrO in a planetary ball mill 2 The balls are mixed with the medium for 2 hours, and the mixed slurry is dried in an oven at 80℃;
[0040] ②Molten salt reaction: The dried powder is put into an alumina crucible with a cover, and put into a muffle furnace for synthesis. The synthesis conditions are 1050℃, the temperature is kept for 60min, the heating rate is 5℃ / min, and the cooling rate is 5℃ / min after the completion of the heat preservation;
[0041] ③Washing and drying: Put the reacted powder into a suitable size beaker, and wash it repeatedly with hot deionized water until no C1 is detected in the filtrate - until. Filter and dry the washed powder to obtain rod-shaped Nb 2 O 5 Powder.
[0042] The XRD diffraction pattern of the niobium pentoxide powder prepared in this example is show...
Embodiment 2
[0044] ① Ingredients ball mill: Weigh AR grade Nb 2 O 5 (99.96%) 40.0015g, AR grade NaCl (99.80%) 40.0013g, add a certain amount (depending on the fluidity of the slurry) of absolute ethanol, use ZrO in a planetary ball mill 2 The balls are mixed with the medium for 2 hours, and the mixed slurry is dried in an oven at 80℃;
[0045] ②Molten salt reaction: The dried powder is put into an alumina crucible with a cover, and put into a muffle furnace for synthesis. The synthesis condition is 1050℃, the temperature is kept for 60 minutes, the heating rate is 10C / min, and the temperature drop rate is 5C / min after the completion of the heat preservation;
[0046] ③Washing and drying: Put the reacted powder into a suitable size beaker, and wash it repeatedly with hot deionized water until no C1 is detected in the filtrate - until. Filter and dry the washed powder to obtain rod-shaped Nb 2 O 5 powder.
[0047] The XRD diffraction pattern of the niobium pentoxide powder prepared in this exampl...
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