Aqueous solution growth at 200 °C and characterizations of pure, 17O- or D-based herbertsmithite ZnxCu4-x(OH)6Cl2 single crystals

Abstract The aqueous solution growth of mm-sized, pure, 17O- or D-enriched herbertsmithite ZnxCu4-x(OH)6Cl2 single crystals is presented. A relationship between x values, antisite disorder amounts and the growth temperature is established. The crystal chemical composition and stability, structural phase and antisite disorder amounts have been characterized by powder X-ray diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), Electron Probe Micro Analysis/Wavelength Dispersive Spectroscopy (EPMA/WDS), Inductively Coupled Plasma/Atomic Emission Spectroscopy analysis (ICP/AES), coupled Thermo Gravimetric Analysis-Mass Spectrometry (TGA/MS) and magnetic susceptibility measurements. An unambiguous relationship between the c lattice parameter and the x value has been found.