Synthesis of Nanocrystalline Powders in the CеO2〈ZrO2〉–Al2O3 System by the Citrate Sol–Gel Method
Л. В. Морозова
Abstract
Л. В. Морозова
Abstract
Abstract— Weakly aggregated, highly dispersed precursor powders with a specific surface area of 350–360 m2/g have been prepared by the citrate sol–gel method in the CеO2〈ZrO2〉–Al2O3 system. Heat treatment of the precursors in the temperature range 700–1000°C led to the formation of powders based on a fluorite-like Ce0.7Zr0.3O2 solid solution with a crystallite size under 30 nm. The presence of alumina has been shown to inhibit the Ce0.7Zr0.3O2 crystallite growth process. Using low-temperature nitrogen adsorption measurements, we have studied texture characteristics of the powders obtained at 1000°C: they have a specific surface area of 90 and 105 m2/g and a specific pore volume of up to 0.380 cm3/g, with a unimodal pore size distribution in the range 2.5–10 nm. We examine the effect of thermal “aging” at a temperature of 1000°C for 50 h on the structure and particle size of the powders. Based on the experimental data obtained, we propose a process for the synthesis of nanocrystalline mesoporous powders in the CеO2〈ZrO2〉–Al2O3 system for the preparation of supports of an active phase (Pt, Pd, or Rh) in three-way catalysts.
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Abstract— Weakly aggregated, highly dispersed precursor powders with a specific surface area of 350–360 m2/g have been prepared by the citrate sol–gel method in the CеO2〈ZrO2〉–Al2O3 system. Heat treatment of the precursors in the temperature range 700–1000°C led to the formation of powders based on a fluorite-like Ce0.7Zr0.3O2 solid solution with a crystallite size under 30 nm. The presence of alumina has been shown to inhibit the Ce0.7Zr0.3O2 crystallite growth process. Using low-temperature nitrogen adsorption measurements, we have studied texture characteristics of the powders obtained at 1000°C: they have a specific surface area of 90 and 105 m2/g and a specific pore volume of up to 0.380 cm3/g, with a unimodal pore size distribution in the range 2.5–10 nm. We examine the effect of thermal “aging” at a temperature of 1000°C for 50 h on the structure and particle size of the powders. Based on the experimental data obtained, we propose a process for the synthesis of nanocrystalline mesoporous powders in the CеO2〈ZrO2〉–Al2O3 system for the preparation of supports of an active phase (Pt, Pd, or Rh) in three-way catalysts.
Key concepts: Nanocrystalline material, Crystallite, Materials science, Chemical engineering, Specific surface area, Mesoporous material, Atmospheric temperature range, Sintering