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Preparation and characterization of nanocrystalline titania powders by sonochemical synthesis

机译:声化学合成法制备纳米晶二氧化钛粉及其表征

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摘要

Nanocrystalline mesoporous titania powders were synthesized by hydrolyzing titanium isopropoxide in ethanol-water mixtures which were ultrasonically treated without using any templates or chemicals. Titanium isopropoxide-ethanol mixture was added dropwise to a water-ethanol mixture placed in an ultrasonic bath. The properties of the sonochemically synthesized powder were compared with those of the powders prepared without ultrasonic treatment along with Degussa P-25 titania powder. The phase structure, crystallite size, surface area, particle size, powder density were determined and sintering behavior was analyzed in this work. The nanotitania powder prepared during ultrasonic induced hydrolysis (TiO 2-U) was determined to be formed from a mixture of anatase and brookite phases at 25°C. The brookite phase in nanotitania powder prepared without ultrasonic treatment (TiO 2-NoU) was detected at 70°C. The anatase-rutile phase transformation was completed in the 500-700°C range for both powders. The average crystallite sizes of the powders at 25°C were determined as 10 and 5nm for TiO 2-NoU and TiO 2-U, respectively. The surface area decreased from 238 to106m 2/g for TiO 2-NoU and from 287 to 82m 2/g for TiO 2-U when the calcination temperature was increased from 200 to 500°C. The evolution of the N 2 adsorption-desorption behavior with calcination temperature and the corresponding pore size distributions/volumes was attributed to the formation of closely packed submicron aggregates during powder synthesis and calcination. The sintering behavior was concluded to be controlled by 7-10nm crystallites and the submicron aggregates. The determination of the densification behavior of titania powders prepared by different methods with various levels of dopants may prove to be very useful for a better understanding of the phase/pore structure evolution which is crucial for a significant number of applications.
机译:纳米晶介孔二氧化钛粉末是通过在乙醇-水混合物中水解异丙氧基钛而合成的,该混合物无需使用任何模板或化学药品即可进行超声处理。将异丙醇钛-乙醇混合物滴加到置于超声浴中的水-乙醇混合物中。将超声化学合成粉末的性能与未经超声处理的Degussa P-25二氧化钛粉末的性能进行了比较。确定了相结构,微晶尺寸,表面积,粒度,粉末密度,并分析了烧结行为。经测定,在25°C下由锐钛矿相和板钛矿相的混合物形成了超声诱导水解过程中制备的纳米二氧化钛粉末(TiO 2-U)。在70°C下检测到未经超声处理(TiO 2-NoU)制备的纳米二氧化钛粉末中的板钛矿相。两种粉末都在500-700°C范围内完成了锐钛矿-金红石相转变。对于TiO 2-NoU和TiO 2-U,在25℃下粉末的平均微晶尺寸确定为10nm和5nm。当煅烧温度从200℃提高到500℃时,表面积从TiO 2 -NoU的238降至106m 2 / g,从TiO 2 -U的表面积从287降低至82m 2 / g。 N 2吸附-解吸行为随煅烧温度的变化以及相应的孔径分布/体积的变化归因于粉末合成和煅烧过程中紧密堆积的亚微米聚集体的形成。结论是7-10nm的微晶和亚微米聚集体控制了烧结行为。用不同水平的掺杂剂通过不同方法制备的二氧化钛粉末的致密化行为的测定可能被证明对于更好地理解对于大量应用至关重要的相/孔结构演变非常有用。

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