Mn<4+> doped red fluorescent material and preparation method thereof
A technology for red fluorescence and raw materials, applied in the field of Mn4+-doped red fluorescent materials and their preparation, can solve the problems of low light emission color rendering index of white LEDs, harm to human health and environment, poor chemical stability, etc., and achieve enhanced photoluminescence. , low cost, good stability
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[0032] Example 1: Preparation by high temperature solid phase method (Mg 1-y A y ) 2 (Ti 1-z B z ) 1-x O 4 :xMn 4+ (B=Zr; x=0.001, y=0, z=0.01), the raw materials used are analytical pure MgO, TiO 2 , ZrO 2 And MnO 2 ; Then accurately weigh the raw materials according to the molar ratio in the chemical reaction equation and add 5wt% NH 4 F flux, grind and mix evenly with an agate mortar to obtain a precursor; put the precursor into a 25×25mm alumina crucible, then place it in a muffle furnace, and heat up to 800°C in an air atmosphere for pre-sintering. Keep the temperature for 6 hours, take it out and re-grind to make it evenly mixed. After the second sintering, keep it at 1400°C for 10 hours in an air atmosphere. Place the obtained sample in an agate mortar and grind it to obtain Mg. 2 (Ti 0.99 Zr 0.01 ) 0.999 O 4 :0.1%Mn 4+ Phosphor. X-ray powder diffraction (XRD) analysis results show that the XRD pattern of the sample is g2 TiO 4 The standard powder diffraction file 25-1157 ...
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[0033] Example 2: Preparation by high temperature solid phase method (Mg 1-y A y ) 2 (Ti 1-z B z ) 1-x O 4 :xMn 4+ (A=Ca, B=Zr; x=0.0015, y=0.01, z=0.01), the raw materials used are analytical pure MgO, CaCO 3 , TiO 2 , ZrO 2 And MnO 2 ; Then accurately weigh the raw materials according to the ratio of the chemical reaction equation and add 3wt% LiF flux, grind and mix uniformly with an agate mortar to obtain the precursor, put the precursor into a 25×25mm alumina crucible, and then place it in In the muffle furnace, pre-sintering is carried out in an air atmosphere to 600°C for 8 hours. After taking it out, it is ground again to make it evenly mixed. The secondary sintering is kept at 1200°C in an air atmosphere for 10 hours. The sample is ground in an agate mortar, and finally (Mg 0.99 Ca 0.01 ) 2 (Ti 0.99 Zr 0.01 ) 0.9985 O 4 : 0.15% Mn 4+ Phosphor. X-ray powder diffraction analysis results show that the XRD pattern of the sample is g2 TiO 4 The standard PDF#25-1157 card matc...
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[0034] Example 3: Preparation by high temperature solid phase method (Mg 1-y A y ) 2 (Ti 1-z B z ) 1-x O 4 :xMn 4+ (A=Ca, B=Si; x=0.001, y=0.01, z=0.005), the raw materials used are analytical pure MgO, CaCO 3 , TiO 2 , SiO 2 And MnO 2 ; Then accurately weigh the raw materials according to the ratio of the chemical reaction equation and add 5wt% LiF flux, grind and mix uniformly with an agate mortar to obtain the precursor, and put the precursor into a 25×25mm alumina crucible, and then place it in In the muffle furnace, pre-sintering is carried out in an air atmosphere to 600°C for 8 hours. After taking it out, it is ground again to make it evenly mixed. The secondary sintering is held in an air atmosphere at 1150°C for 8 hours to obtain The sample is ground in an agate mortar, and finally (Mg 0.99 Ca 0.01 ) 2 (Ti 0.995 Si 0.005 ) 0.999 O 4 :0.1%Mn 4+ Phosphor. X-ray powder diffraction analysis results show that the obtained phosphor is a pure phase. Under the excitation of 28...
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