Détermination de faibles quantités de terres rares dans une matrice inorganique par une méthode de RMN
TL;DRAbstract
Determine the doping level is essential to optimize the properties of materials, e.g. luminescence. We present an original high-accuracy method based on the 31P solid-state NMR relaxation to determine low concentrations (< 1 %) of paramagnetic lanthanide ions. Our method was first applied to a model compound, LaPO4, within the incorporation of the dopant is known. NMR experiments under static and MAS (15 kHz) conditions reveal that the 31P relaxation time T1 is strongly affected by the presence of paramagnetic ions in the vicinity of the phosphorous nuclei. A linear variation of 1 / T1 as a function of neodymium (Nd3+) or gadolinium (Gd3+) concentration is shown in the 0-10 at.% range for a homogeneous distribution of the doping ions in the matrix. In the case of a solid-state synthesis at 1450 °C, relaxation measurements show that the homogeneous distribution of doping ions is ensured when the mixing of oxide precursors is performed mechanically, in contrast with the manual grinding.
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Determine the doping level is essential to optimize the properties of materials, e.g. luminescence. We present an original high-accuracy method based on the 31P solid-state NMR relaxation to determine low concentrations (< 1 %) of paramagnetic lanthanide ions. Our method was first applied to a model compound, LaPO4, within the incorporation of the dopant is known. NMR experiments under static and MAS (15 kHz) conditions reveal that the 31P relaxation time T1 is strongly affected by the presence of paramagnetic ions in the vicinity of the phosphorous nuclei. A linear variation of 1 / T1 as a function of neodymium (Nd3+) or gadolinium (Gd3+) concentration is shown in the 0-10 at.% range for a homogeneous distribution of the doping ions in the matrix. In the case of a solid-state synthesis at 1450 °C, relaxation measurements show that the homogeneous distribution of doping ions is ensured when the mixing of oxide precursors is performed mechanically, in contrast with the manual grinding.
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