Investigation into the Palladium-Europium Acetate Reductive Decomposition with Synchrotron Radiation-Based X-ray Diffraction and X-ray Absorption Spectroscopy
Научная публикация
Общее |
Язык:
Английский,
Жанр:
Статья (Full article),
Статус опубликования:
Опубликована,
Оригинальность:
Оригинальная
|
Журнал |
Zeitschrift fur Anorganische und Allgemeine Chemie
ISSN: 0044-2313
, E-ISSN: 1521-3749
|
Вых. Данные |
Год: 2014,
Том: 640,
Номер: 12-13,
Страницы: 2577-2582
Страниц
: 6
DOI:
10.1002/zaac.201400258
|
Ключевые слова |
Heterometallic complexes; Palladium; Nanoparticles; X-ray diffraction; EXAFS spectroscopy |
Авторы |
Khramov Evgeny
1
,
Belyakova Olga
2
,
Murzin Vadim
1,3
,
Veligzhanin Alexey
1
,
Chernyshov Alfred
1
,
Vargaftik Mikhail
4
,
Kozitsyna Natalya
4
,
Zubavichus Yan
1,2
|
Организации |
1 |
Kurchatov Centre of Converging of Nano-, Bio-, Information and Cognitive Sciences and Technologies National Research Center “Kurchatov Institute”
|
2 |
Laboratory for Polymer Structure Research A.N.Nesmeyanov Institute of Organoelement Compounds of theRussian Academy of Sciences
|
3 |
Group for Structural Investigations A.V. Topchiev Institute of Petrochemical Synthesis of the Russian Academy of Sciences
|
4 |
Laboratory of Metal Complex Catalysis Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences
|
|
The reductive decomposition of the complex Pd2Eu2(μ,η2‐OOCMe)2(μ‐OOCMe)8(H2O)2·(HOOCMe)2 upon heating from room temperature to 500 °C in a hydrogen atmosphere was investigated by in situ synchrotron radiation‐based X‐ray absorption fine structure spectroscopy (XAFS) including observations of X‐ray near‐edge structure (XANES) and extended absorption fine structure (EXAFS) at Pd K‐ and Eu L3‐edges and synchrotron X‐ray diffraction (XRD). The Pd‐Eu2O3 nanocomposite was found to be the final thermolysis product. The decomposition proceeds via series of intermediate crystalline phases, including europium(II) and (III) anhydrous acetates and EuO(CH3COO) oxidoacetate. Surprisingly, the major fraction of europium occurs in the reduced form Eu2+ within a limited temperature range of 200–300 °C. Presumably, the reversible Eu3+↔Eu2+ redox‐process is associated with the stability of nanocrystalline palladium hydride, which acts as a stronger reducing agent as compared to molecular hydrogen.