A method of forming composition-modified barium titanate ceramic particulate includes mixing a plurality of precursor materials and a precipitant solution to form an aqueous suspension. The plurality of precursors include barium nitrate, titanium chelate, and a metal or oxometal chelate. The precipi
A method of forming composition-modified barium titanate ceramic particulate includes mixing a plurality of precursor materials and a precipitant solution to form an aqueous suspension. The plurality of precursors include barium nitrate, titanium chelate, and a metal or oxometal chelate. The precipitant solution includes tetraalkylammonium hydroxide and tetraalkylammonium oxalate. The method further includes treating the aqueous suspension at a temperature of at least 150° C. and a pressure of at least 200 psi, and separating particulate from the aqueous suspension after treating.
대표청구항▼
1. A method for preparing a ceramic powder, the method comprising: injecting a first solution stream into a reactor the first solution stream comprising a first precursor material including a barium source, a second precursor including a titanium source, and a third precursor comprising a metal ion
1. A method for preparing a ceramic powder, the method comprising: injecting a first solution stream into a reactor the first solution stream comprising a first precursor material including a barium source, a second precursor including a titanium source, and a third precursor comprising a metal ion or oxometal ion and a chelating agent, the chelating agent being an alpha-hydroxycarboxylic acid;concurrently with injecting the first solution stream into the reactor, injecting a second solution stream into the reactor, the second solution stream comprising a precipitant solution including an oxalate compound and tetraalkylammonium hydroxide, to cause co-precipitation of hydrated hydroxide-oxalate precipitates in a combined solution, wherein the hydrated hydroxide-oxalate precipitates are partially crystalline, wherein injecting the first solution stream and the second solution stream into the reactor is performed at a turbulence factor of at least 1.5×107 cm/s3, wherein a residence time within the reactor is at least 50 milliseconds;hydrothermally treating the hydrated hydroxide-oxalate precipitates of the combined solution in an aqueous suspension by heating the aqueous suspension at a temperature of at least 150° C. at a treatment pressure of at least 200 psi; andafter hydrothermally treating, decomposing and calcining to form the ceramic powder including composition-modified barium titanate particles. 2. The method of claim 1, wherein after decomposing and calcining, excluding particles having a size of less than 0.1 micrometers and excluding particles having a size greater than 10 micrometers, the composition-modified barium titanate particles have an average particle size in a range of 0.6 micrometers to 1.5 micrometers. 3. The method of claim 1, wherein heating the aqueous suspension solution is performed for a time period of 4 hours to 8 hours. 4. The method of claim 1, wherein hydrothermally treating the hydrated hydroxide-oxalate precipitates of the combined solution includes adding the aqueous suspension at a temperature of not greater than 100° C. to a hydrothermal treatment vessel while heating the hydrothermal treatment vessel and while releasing steam from the hydrothermal treatment vessel. 5. The method of claim 1, wherein after decomposing and calcining, the ceramic powder is free of ball-milling debris. 6. The method of claim 1, wherein the composition-modified barium titanate particles include (Ba1-α-μ-νAμDνCaα)[Ti1-x-δ-μ′-ν′MnδA′μD′ν′Zrx]zO3, where A=Ag, A′=Dy, Er, Ho, Y, Yb, or Ga; D=Nd, Pr, Sm, or Gd; D′=Nb or Mo, 0.10≤x≤0.25; 0≤μ≤0.01, 0≤μ′≤0.01, 0≤ν≤0.01, 0≤ν′≤0.01, 00, α>0, δ>0, and μ>0.
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