GdOS:Er crystals were prepared through high-temperature solid-state reaction method in vacuum, with the vacuum synthesis mechanism determined by thermal analysis. The crystal structure and upconversion luminescence properties were investigated respectively by XRD, TEM and spectrophotometer. Well crystallized GdOS:Er phosphors were prepared under 1000°C in vacuum with a certain excessive amount of sulfur content than stoichiometric. It is confirmed that with the increasing sulfur content the green emission was enhanced and red emission was weakened. The cooperative upconversion luminescence of Er in non-stoichiometric GdOS crystals was interpreted as a result of two photon absorption and the photon avalanche process.
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