XAFS investigation of [Pd(NH3)4][AuCl4]2 and its thermolysis products

• Published in: Journal of thermal analysis and calorimetry 2010-11, Vol.102 (2), p.703-708
• Main Authors: Nedoseykina, Tatiana, Plyusnin, Pavel, Shubin, Yuri, Korenev, Sergey
• Format: Article
• Language: English
• Subjects: Analytical Chemistry; Chemistry; Chemistry and Materials Science; Chlorides; Chlorine; Decomposition; Gold; Inorganic Chemistry; Measurement Science and Instrumentation; Nanoparticles; Palladium; Physical Chemistry; Polymer Sciences; Residues; Thermogravimetry
• ISSN: 1388-6150; 1588-2926; 1572-8943
• DOI: 10.1007/s10973-010-0723-y

Thermolysis of double complex salt [Pd(NH 3 ) 4 ][AuCl 4 ] 2 has been studied in helium atmosphere from ambient to 350 °C. The XAFS of Pd K and Au L 3 edges and thermogravimetry measurements have been carried out to characterize the intermediates and the final product. In the temperature range 115–160 °C the complex is decomposed to form Pd(NH 3 ) 2 Cl 2 and AuCl 4− x N x species with x ranging from 2 to 3. Subsequent heating of the intermediate up to 300 °C leads to the total loss of NH 3 . The Au–Cl and Au–Au bonds form the local environment of Au at the stage of decomposition while only four chlorine atoms are around Pd. At the temperature of 330 °C the Au and Pd nanoparticles as well as residues of palladium chloride are detected. The final product consists of separated Au and Pd nanoparticles.