期刊
DALTON TRANSACTIONS
卷 42, 期 14, 页码 5167-5173出版社
ROYAL SOC CHEMISTRY
DOI: 10.1039/c3dt32582b
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资金
- National Nature Science Foundation of China [20821091, 20423005]
- Lujan Center at Los Alamos National Laboratory at LANSCE
- Office of Basic Energy Sciences (DOE)
Single-phased orthorhombic nitridosilicate CaSiN2 powders were prepared at 1550 degrees C in a N-2/H-2 (6%) atmosphere by solid-state reaction using Ca3N2 and Si3N4 as the starting materials. The crystal structure refinements were carried out by the Rietveld method based on the X-ray and neutron powder diffraction data collected at 297 K, respectively. The CaSiN2 phase crystallizes in an orthorhombic unit cell with the space group Pbca (No. 61) and cell parameters a = 5.1334(3) angstrom, b = 10.3090(5) angstrom, c = 14.5756(5) angstrom, Z = 16 (XRD data). Instead of the ideal formula CaSiN2, small amounts of oxygen could be detected in the samples. The O/N composition of orthorhombic CaSiN2-2 delta/3O delta was analyzed by EDX and Rietveld refinement on the neutron powder diffraction data. SAED and HREM characterizations of the crystallites were conducted before the EDX analysis in order to select proper crystallites and exclude other minor second phases of (oxo)nitridosilicates such as cubic CaSiN2 and monoclinic CaSi2O2N2. The luminescence measurements indicate that Ce3+/Li+ co-doped CaSiN2-2 delta/3O delta emits a typical shouldered yellow band peaking at 530 nm (FWHM similar to 120 nm), which originates from the 5d -> 4f transition of Ce3+. The emission band shifts to longer wavelengths with an increment of Ce3+ concentration. The strong excitation band appears in the range of 350-470 nm, which is very favorable for the applications in near-UV and blue phosphor-converted light-emitting diodes (pc-LEDs).
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