Method for preparing V2O3 nano-crystal grain ceramic
A nano-grain and ceramic technology, which is applied in the field of preparation of V2O3 and its dopant nano-grain ceramics, can solve the problems of poor electrical stability of ceramics, serious loss of furnace body, high production cost, etc., and achieves low forming pressure and low energy consumption The effect of low consumption and low cost
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Embodiment 1
[0019] with V 2 o 5 , the reaction of oxalic acid and hydrochloric acid to prepare VOCl 2 solution, and then react this solution with ammonium bicarbonate to synthesize the vanadyl (IV) basic ammonium carbonate precursor. The precursor is ultrasonically crushed to a particle size of 1-2 μm, and then reduced and pyrolyzed at 400 ° C for 60 minutes under hydrogen flow to obtain V 2 o 3 Nano-powder. The powder is pressed at 300MPa, placed in a tube furnace or tunnel furnace, and filled with water-saturated H 2 Exclude the air in the furnace, then heat it to 1400°C and keep it for 5 minutes, then cool it down to 800-900°C with a program and then cool it naturally. The average particle diameter is about 60nm, and the crystal grain is spherical nano-V 2 o 3 ceramics. Its Tt 1 At about -120°C, the resistivity jump is greater than 5 orders of magnitude.
Embodiment 2
[0021] Apply the method similar to embodiment 1, use VOCl 2 solution, CrCl 3 The Cr-doped vanadyl (IV) basic ammonium carbonate precursor was synthesized by reacting the solution with ammonium bicarbonate. The Cr-doped precursor was ultrasonically crushed to a particle size of 1-2 μm, and then reduced and pyrolyzed at 800°C for 20 minutes under hydrogen flow to obtain (V 0.993 Cr 0.007 ) 2 o 3 Nano-powder. This powder is compressed at 150MPa, then sintered at 1250°C for 15min in the same manner as in Example 1 to obtain agglomerate sintered bodies of 2 to 3 μm, with an average grain diameter of less than 100nm, and the crystal form is quasi-spherical ( V 0.993 Cr 0.007 ) 2 o 3 ceramics. Its Tt 2 At about 77°C, the resistivity jump is greater than 2 orders of magnitude.
Embodiment 3
[0023] Apply the method similar to embodiment 1, use VOCl 2 solution, AlCl 3Solution and ammonium bicarbonate were reacted to synthesize Al-doped vanadyl (IV) basic ammonium carbonate precursor, and the Al-doped precursor was ultrasonically crushed to a particle size of 1-2 μm, and then reduced and pyrolyzed at 600°C for 40 minutes under hydrogen flow to obtain (V 0.986 Al 0.014 ) 2 o 3 Nano-powder. This powder is compressed at 200MPa, and then passed through H 2 Sintered at 1150°C for 80min, the agglomerate sintered body is about 1.5μm, the average grain diameter is less than 100nm, and the crystal shape is quasi-spherical (V 0.986 Al 0.014 ) 2 o 3 ceramics. Its Tt 2 At about -65°C, the resistivity jumps by about 3 orders of magnitude.
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