Abstract
The [(Pt(NH3)4)x(Pd(NH3)4)1–x]CrO4 single-phase solid solution (x = 0.5-0.6) is prepared by the cocrystallization of [Pt(NH3)4](NO3)2 and [Pd(NH3)4](NO3)2 aqueous solutions with ammoniac (NH4)2CrO4. The structure and parameters of the tetragonal (I41/amd, Z = 4) unit cell (a = 7.3091(1) Å, c = 15.2720(6) Å) of this compound and the molar fraction of Pt (x = 0.568(7)) are determined using the single-crystal X-ray diffraction method. The unit cell parameters of the studied crystal are additionally refined by an original method (a = 7.3207(9) Å, c = 15.2527(19) Å, V = 817.4(3) Å3) and are further utilized to refine also the molar fraction of Pt using Zen′s law (x = 0.57(1)). A single crystal of [(Pt(NH3)4)0.57(Pd(NH3)4)0.43]CrO4 and two samples of the synthesized product selected from the total mass are thermally decomposed in hydrogen. A study of thermolysis products by XRD, scanning and transmission electron microscopy methods demonstrates the formation of a Pt0.49Pd0.38Cr0.13 nanoalloy included in the Cr2O3 matrix in the form of blocks (~1 µm) and smaller (>2 nm) spherical formations.
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Funding
The synthesis of the samples was funded by the Russian Science Foundation (project No. 22-23-00672, https://rscf. ru/project/22-23-00672/). The authors thank the Ministry of Science and Higher Education of the Russian Federation and the Priority 2030 program.
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Russian Text © The Author(s), 2023, published in Zhurnal Strukturnoi Khimii, 2023, Vol. 64, No. 9, 116969.https://doi.org/10.26902/JSC_id116969
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Serebrennikova, P.S., Lagunova, V.I., Zadesenets, A.V. et al. PREPARATION OF NANOALLOYS OF THE Pt–Pd–Cr SYSTEM UNDER THERMAL DECOMPOSITION OF [(Pt(NH3)4)x(Pd(NH3)4)1–x]CrO4 COMPLEX SALTS. J Struct Chem 64, 1686–1701 (2023). https://doi.org/10.1134/S0022476623090123
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DOI: https://doi.org/10.1134/S0022476623090123