Российские нанотехнологии. 2019; 14: 43-51
Синтез наночастиц палладия на поверхности оксида церия(IV) под воздействием ультрафиолетового излучения и их диагностика
https://doi.org/10.21517/1992-7223-2019-9-10-43-51Аннотация
Проведен синтез наночастиц палладия с использованием комплексного оксалата палладия в качестве прекурсора в водной среде методом УФ-облучения. Образцы исследованы различными лабораторными методиками, такими как просвечивающая электронная микроскопия, рентгенофлуоресцентный анализ, рентгеновская порошковая дифракция, XAFS-спектроскопия и ИКспектроскопия диффузного отражения с использованием зондирующих молекул CO. Микроизображения, полученные с помощью просвечивающей электронной микроскопии, не позволили отличить наночастицы Pd от материала подложки, но показали отсутствие влияния УФ-излучения на размеры наночастиц CeO2 . Данные рентгенофлуоресцентного анализа показали наличие в материале атомов церия и палладия. Дифрактограммы свидетельствуют о присутствии фаз диоксида церия и металлического палладия, также анализ спектров XAFS за K-краем палладия показал наличие в системе фазы PdO. Приблизительный размер наночастиц палладия оценен по ИК-спектрам после адсорбции CO, он составил не более 2 нм, что существенно меньше среднего размера наночастиц Pd, полученных аналогичным способом без подложки CeO2 (1.5–9.5 нм).
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Title in english. 2019; 14: 43-51
Synthesis of palladium nanoparticles on the cerium(IV) oxide surface under uv radiation and their characterization
https://doi.org/10.21517/1992-7223-2019-9-10-43-51Abstract
Palladium nanoparticles were synthesized in an aqueous solution by UV irradiation using complex palladium oxalate as a precursor. Samples were studied by various laboratory methods, such as TEM, XRF, XRPD, XAFS spectroscopy, and diffuse reflection IR spectroscopy of CO probing molecules. TEM images did not allow to distinguish Pd nanoparticles from the substrate material but showed the absence of the UV radiation influence on the sizes of CeO2 nanoparticles. XRF data showed the presence of cerium and palladium atoms in the material. X-ray diffraction patterns indicate the presence of both a cerium dioxide phase and a phase of metallic palladium, while the analysis of XAFS spectra beyond the K edge of palladium also showed the presence of a PdO phase in the system. The approximate size of palladium nanoparticles was estimated from the infrared spectra after CO adsorption and it was less than 2 nm, which is significantly smaller than the average size of Pd nanoparticles obtained by a similar method without a CeO2 substrate (1.5–9.5 nm).
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