A strategy has been adopted for simultaneous morphology manipulation and upconversion luminescence enhancement of β-NaYF4:Yb3+/Er3+ microcrystals by simply tuning the KF dosage. X-ray power diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and photoluminescence spectra (PL) were used to characterize the samples. The influence of molar ratio of KF to Y3+ on the crystal phase and morphology has been systematically investigated and discussed. It is found that the molar ratio of KF to Y3+ can strongly control the morphology of the as-synthesized β-NaYF4 samples because of the different capping effect of F− ions on the different crystal faces. The possible formation mechanism has been proposed on the basis of a series of time-dependent experiments. More importantly, the upconversion luminescence of β-NaYF4:Yb3+/Er3+ was greatly enhanced by increasing the molar ratio of KF to RE3+ (RE = Y, Yb, Er), which is attributed to the distortion of local crystal field symmetry around lanthanide ions through K+ ions doping. This synthetic methodology is expected to provide a new strategy for simultaneous morphology control and remarkable upconversion luminescence enhancement of yttrium fluorides, which may be applicable for other rare earth fluorides.

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XAFS has been used to investigate the local structure evolutions of ultrafine amorphous NiB alloy during the annealed crystallization process. A nanocrystalline Ni phase with the local structure of crystalline Ni-like and a crystalline Ni3B, have been produced for ultrafine amorphous NiB alloy under the annealed temperature of 573 K. The results rule out Rojo et al.'s devitrification mechanism of Ni80B20 amorphous alloy in which they considered that an amorphous pure Ni phase is formed in the first exothermic process. However, our results are almost identical with Riveiro et al.'s conclusion in which the intermediate state is interpreted as two metastable crystalline phases of Ni3B and Ni-rich NiB alloy. With the annealed temperature going onto 773 K, the ultrafine NiB sample is further decomposed and crystallized into crystalline Ni with long-range order.

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