Synthesis and Property of the Mn Doped Oxide Red Phosphors in the Calcium Aluminates Koji INOUE, Shinya IWATA and Shinobu HASHIMOTO Recently, the deve
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1 Synthesis and Property of the Mn Doped Oxide Red Phosphors in the Calcium Aluminates Koji INOUE, Shinya IWATA and Shinobu HASHIMOTO Recently, the development of new sulfide-free phosphors with high efficiency is urgently needed for VFDs and FEDs. The fabrication of Calcium Aluminate and the effect of partially substituted Mn on the photoluminescence (PL) were investigated in this research. In the samples annealed at 1923 K for 3 h in air, red photoluminescence was observed.the PL material is expected as a low-cost and red light-emitting diodes. Key words : Red Phosphor, Calcium Aluminates, Photoluminescence(PL), VFD, FED, LED 1-7) CA Eu 2+ CaAl2O4 :Eu 2+ 1) Nd 3+ CaAl 2 O 4 :Eu 2+, Nd 3+ 2) CA2 Ce 3+ CaAl4O7 :Ce 3+ 3) CA6 Mn 4+ CaAl12O19 :Mn 4+ 4) Cr 3+ CaAl 12 O 19 :Cr 3+ 5) C3A Eu 3+ Ca 3 Al 2 O 6 :Eu 3+ 6) C12A7 Eu 2+ Ca12Al14O33 :Ce 3+ 7) 1 C12A7 8) CA Eu 2+ Eu 3+ 3) 14) Nd 3+, Dy 3+, Ti 3+, Er 3+, Ho 3+ Li +, Na +, K + 4), 10)-13) 15) Er 3+ 16) Mn 2+ Ce 3+ 17) Ce 3+ CA2 Ce 3+ Tb 3+ 5) Pr 3+ 18) Mn 4+ 6) Mg 2+ 19) CA6 Cr 3+ 7) Eu 2+ 20) Ce 3+ 21) C3A Eu 3+ 8) Eu 2+ Nd 3+ 22) Cl - 23 C12A7 Ce 3+ 9) Er 3+ 24) Au - 25) LED CaAl12O19 :Mn 4+ CaAl 12 O 19 magneto-plumbite structure CaAl 12 O 19
2 ) 1 CaAl12O19 5 Al 3+ Al (1 ) (1 ) 12 Ca 2+ 5 CaAl12O19 :Mn A. Bergstein W.B. White 4)CaAl 12 O 19 CaAl 12 O 19 PL Mn 2+, Mn 3+, Mn 4+ Mn nm Mn nm LED CaAl 12 O 19 : Mn 4+ LED LED GaN Y3Al5O12: Ce 3+ GaN 400 nm LED CaAl 12 O 19 : Mn 4+ Mn nm 500nm LED LED CaAl 12 O 19 : Mn 4+ 9) CaF2 MgF2 Mn 4+ CaAl12O19: Mn 4+ 2 CaAl 12 O 19 : Mn ) Mg 12-13) Mn CaAl 12 O 19 :Mn 4+ Mn Mn Al 0.5 mol% 20 mol% (CaAl12-xO19: Mnxx = ) Mn Mn Mn CaAl 12-x O 19 : Mn x
3 1)(CaCO399.99%, 10m) 2)(-Al 2 O %, 5m) 3)()(MnO99.0%, 2-3m) 2 (Electron Spin Resonance ESR) ESR 3 Mn CaAl 12-x O 19 : Mn x (x = 0.000, 0.005, 0.010, 0.020, 0.025, 0.050, 0.100)XRD CaAl12-xO19: Mnx MnO Al2O3 x= K3 200K/h 200K/h X X-ray DiffractionXRD (PhotoluminescencePL) Intensity(a.u.) JCPDS card Diffraction angle 2θ (deg.) 3 CaAl 12 O 19 MnO Al 2 O 3 CaCO K CaO CO2 CaO 1923K CaO Al 2 O 3 Al 2 O 3 4 CaAl 12-x O 19 : Mn x 2= 67
4 XRD Normalized intensity (a.u.) Diffraction angle 2θ (deg.) 4 Mn Ca 2+ = 100 pm, Al 3+ = 53 pm, Mn 4+ = 53 pm, Mn 2+ = 67 pm Mn 2+, Mn 4+ Ca 2+ Mn 2+, Mn 4+ Ca 2+ Al 3+ Mn 2+, Mn 4+, Al 3+ Mn 4+ Al 3+ Mn 2+ Mn 2+ Al 3+ Mn 4+ Al 3+ Mn 4+ Mn 2+ Mn 4+ -Mn 2+ Mn Mn 2+, Mn 4+ Mn 4+ Mn 2+ 5 CaAl12-xO19: Mnx (x = 0.000, 0.005, 0.010, 0.020) PL 6 CaAl 12-x O 19 : Mn x (x =0.020, 0.025, 0.050, 0.100) PL Mn em =655 nm, ex =325 nm 400nm A2 4 T 1, 2 T 2, 4 T 2 325, 385, 462 nm 2 T 1, 2 E 4 A 2 643, 655 nm
5 665 nm 2 E 4 A2 4, 12,13) PL 5 66, 19) Mn E/B 4 T 1 2 T 2 4 T 2 2 T 1 2 E 8 Mn 2 mol%(x = 0.020) Mn 14) Mn x = nm Δ/B 8 Mn 655 nm 4 A 2 9 Mn CaAl 12-x O 19 : Mn x x = 0.000, 0.005, 0.010, 0.020, 0.025, 0.050, 0.100)ESR Intensity (a.u.) x (in CaAl 12-x O 19 : Mn ) x G Fe 3+ 15, 16, x = 0 Fe 3+ x = G Mn ))Mn I = 5/2
6 2I+1 = 6 Mn x = G 6 Mn 4+ 16, 18, 20) 3300 G x = x = 0.005, 0.010, G ESR PL x = G (1)10 Mn Mn x = G 4000 G (1)Mn 4+ 16, 18 x = Mn x = G G Mn 11 x = 0.025, 0.050, ESR Exchange Broadening 39), 45), 46) Mn x = Mn CaAl 12 O 19 Al 3+ CaAl12O19 Mn Mn 2+ [x = ] Mn 4+ (, (1)) [x = ] Mn 4+ (, ) [x = ] 1700 G 3300 G Mn 4+ Mn 4+ 1 Al 3+ Ca 2+ Mn 4+ Ca 2+ Mn x = x = Mn Mn CaAl 12 O 19 Mn Mn 2+ [x = ] Mn 4+ (, (1)) [x = ] Mn 4+ (, ) [x = ]
7 JST 1) F. C. Palilla et al, Eu 2+ and Ce 3+ emission in sulphate based phosphors J.Electrochem. Soc., 115, p642 (1968) 2) T. Matsuzawa et al, Preparation and characterization of an Hf 4+ -doped zinc silicate long-lasting phosphorescent material J. Electrochem. Soc., 143, p2670 (1996) 3) Dongdong Jia et al, Luminescence and energy transfer in CaAl4O7 : Tb 3+, Ce 3+ Wu, J. Lumin., 93, p107 (2001) 4) A. Bergstein et al, Manganese-Activated Luminescence in SrAl12O19 and CaAl12O19 J. Electrochem. Soc., 118, p1166 (1971) 5) Vijay Singh et al, Photoluminescence and EPR studies of Cr-doped hibonite (CaAl 12 O 19 ) phosphors Solid State Sci., 10, p1525 (2008) 6) Xiaorui Gao et al, Preparation and photoluminescence property of a loose powder, Ca 3 Al 2 O 6 :Eu 3+ by calcination of a layered double hydroxide precursor J. Solid State Chem.,181, p1776 (2008) 7) E.Tõldsepet al, Synthesis and luminescence properties of Ce 3+ doped nanoporous12cao 7Al 2 O 3 powders and ceramics Opt. Mat., 32, p784 (2010) 8) Katsuro Hayashi et al, Hopping and optical absorption of electrons in nano-porouscrystal12cao 7Al 2 O 3 Nature, 419, p462 (2002) 9) T. Murata et al, Fluorescencepropertiesof 20) D. Ramirez-Rosales et al, Electron spin Mn 4+ in CaAl12O19 compounds as red-emitingphosphorforwhiteled J. Lumin., 114, p207 (2005) 10) Vijay Singh et al, Luminescence and EPR investigations of Mn activated calcium aluminate prepared via combustion method Opt. Mater., 30, 468 (2007) 11) Vijay Singh et al, Photoluminescence and EPR studies of Cr-doped hibonite (CaAl12O19) phosphors Solid State Sci., 10, p1525 (2008) 12) Y. X. Pan et al, MeltingenthalpyΔHmfor describing glass forming ability of bulk metallic glasses Opt. Lett., 33, p1816 (2003) 13),, (), p (1987) 14) M.G. Brik et al, Spectroscopic and crystal field analysis of absorption and photoluminescence properties of red phosphor CaAl12O19:Mn 4+ modified by MgO J. Alloys Compd., 509, p1452 (2011) 15) D. Cordischi et al, ESR and reflectance spectra of manganese in polycrystalline TiO2 (rutile) J. Solid State Chem., 15, p82 (1975) 16) A. Amorelli et al, Photoluminescence of cubic and monoclinic Gd 2 O 3 :Eu phosphors prepared by flame spray pyrolysis J. Chem. Soc., Faraday Trans., 85, 4031 (1989) 17) Vijay Singh et al, Mn 2+ activated MgSrAl 10 O 17 green-emitting phosphor A luminescence and EPR study J. Lumin., 128, p1474 (2008) 18) R. Arroyo et al, Influence of manganese ions on the anatase rutile phase transition of TiO 2 prepared by the sol gel process Mater. Lett., 54, p397 (2002) 19) Vijay Singh et al, Measurement of the average L-shell fluorescence yields in elements 40<Z<53 Physica B., 403, p120 (2008) resonance study of the conversion of Mn 4+ to Mn 2+ in the Pb1 xeuxti1 ymnyo3 ceramic system Solid State Commun., 118, p371 (2001)
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