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Title: Synthesis and characterization of single crystal Zircon-Hafnon Zr(1–x)Hf(x)SiO4 solid solutions and the comparison with the reaction products of a TEOS-based hydrothermal route
Author(s): Neumann, Andreas
Kahlenberg, Volker
Lerche, IanLook up in the Integrated Authority File of the German National Library
Stöber, StefanLook up in the Integrated Authority File of the German National Library
Pöllmann, HerbertLook up in the Integrated Authority File of the German National Library
Issue Date: 2024
Type: Article
Language: English
Abstract: Two synthesis routes of the zircon–hafnon solid solution series were carried out. The high-temperature route uses the growth of single crystals via a flux mixture that has been cooled down slowly from 1400 °C over 4 weeks. The reaction products were colorless and idiomorphic without byproducts. The hydrothermal tetraethoxysilane (TEOS)-based route represents the low-temperature method at 200 °C for approximately 7 days. The hydrothermal route yielded a white powder and scanning electron microscopy analysis thereof did not reveal any specific idiomorphic properties. However, the synthesis also featured some byproducts besides the zircon–hafnon solid solutions. Thermogravimetric analysis coupled with differential scanning calorimetry, and mass spectroscopy indicated, that hydrothermal reaction products feature the presence of organic residues originating from the starting materials. However, a specific dependency on the hafnium content could not be observed due to the data scatter. Infrared (IR) analysis revealed the presence of Zr/Hf-oxides. The structural characterization demonstrated that properties change constantly with the hafnium amount, however, gradual variations of some properties related to the composition of the solid solution series depend in part on the synthesis route, considering the c/a ratio and IR modes. Furthermore, analyses of the single crystals by Raman spectroscopy and μXRF suggested a nonequilibrated crystal growth based on the starting composition.
Open Access: Open access publication
License: (CC BY 4.0) Creative Commons Attribution 4.0(CC BY 4.0) Creative Commons Attribution 4.0
Journal Title: ACS omega
Publisher: ACS Publications
Publisher Place: Washington, DC
Volume: 9
Issue: 14
Original Publication: 10.1021/acsomega.3c06960
Page Start: 15781
Page End: 15803
Appears in Collections:Open Access Publikationen der MLU