Transparent rare earth ion-doped hexagonal sodium yttrium fluoride oxyfluoride glass-ceramics and preparation method thereof

A technology of rare earth ions and sodium yttrium fluoride, which is applied in the field of rare earth ion doped β-NaYF4 oxyfluoride glass-ceramics and its preparation, can solve problems such as unsatisfactory, glass devitrification, and excessively large nanocrystal crystallization size. Achieve the effect of improving the luminous efficiency of up-conversion

Inactive Publication Date: 2017-07-14
WUHAN UNIV OF TECH
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  • Abstract
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Problems solved by technology

However, for rare earth-doped oxyfluoride glasses of general composition, low-temperature heat treatment can only obtain α-NaYF 4 , while β-NaYF 4 It is often obtained through a higher heat treatment temperature. At this time, the size of the nanocrystalline crystallization is too large, and the silicate phase is precipitated, resulting in devitrification of the glass, and the obtained α-NaYF 4 with β-NaYF 4 mixed phase, so it does not really play a role in β-NaYF 4 The advantages in up-conversion luminescence cannot meet the requirements of practical applications

Method used

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  • Transparent rare earth ion-doped hexagonal sodium yttrium fluoride oxyfluoride glass-ceramics and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0025] The glass composition (S1) of the present embodiment is: SiO 2 :60mol%, Al 2 o 3 : 9mol%, Na 2 O: 16mol%, NaF: 7mol%, YF 3 :8mol%, ErF 3 : 0.5mol%, raw material selection of analytically pure SiO 2 、Al 2 o 3 、Na 2 CO 3 , NaF and spectrally pure YF 3 with ErF 3 . Weigh the raw material SiO according to the above mole percentage 2:13.5529g,Al 2 o 3 :3.4498g,Na 2 CO 3 :6.3753g,NaF:1.1050g,YF 3 :4.3880g,ErF 3 : 0.4215g, fully mixed evenly with a ball mill mixer, placed in a dense corundum crucible, melted at 1500°C for 1.5 hours; then poured the resulting glass melt on a metal copper mold for rapid compression molding, and annealed at 350°C 3h to obtain a transparent precursor glass; then heat-treat the precursor glass at 650°C for 2 hours to obtain a transparent rare earth ion doped β-NaYF 4 Oxyfluorine glass-ceramics. figure 1 It is the X-ray diffraction pattern of the glass-ceramic after heat treatment of sample S1, compared with the PDF card, the cr...

Embodiment 2

[0027] The glass composition (S2) of the present embodiment is: SiO 2 :60mol%, Al 2 o 3 :7mol%, Na 2 O: 18mol%, NaF: 7mol%, YF 3 :8mol%, ErF 3 : 0.5mol%, raw material selection of analytically pure SiO 2 、Al 2 o 3 、Na 2 CO 3 , NaF and spectrally pure YF 3 with ErF 3 . Weigh the raw material SiO according to the above mole percentage 2 :13.5529g,Al 2 o 3 :2.6832g,Na 2 CO 3 : 7.1722g, NaF: 1.1050g, YF 3 :4.3880g,ErF 3 : 0.4215g, fully mixed evenly with a ball mill mixer, placed in a dense corundum crucible, melted at 1500°C for 1.5 hours; then poured the resulting glass melt on a metal copper mold for rapid compression molding, and annealed at 350°C 3h to obtain a transparent precursor glass; then heat-treat the precursor glass at 650°C for 2 hours to obtain a transparent rare earth ion doped β-NaYF 4 Oxyfluorine glass-ceramics. Figure 4 It is the X-ray diffraction pattern of the glass-ceramic sample after heat treatment of sample S2, compared with the PDF c...

Embodiment 3

[0029] The glass composition (S3) of the present embodiment is: SiO 2 :60mol%, Al 2 o 3 :5mol%, Na 2 O: 18mol%, NaF: 7mol%, YF 3 :10mol%, ErF 3 : 0.5mol%, raw material selection of analytically pure SiO 2 、Al 2 o 3 、Na 2 CO 3 , NaF and spectrally pure YF 3 with ErF 3 . Weigh the raw material SiO according to the above mole percentage 2 :13.5529g,Al 2 o 3 : 1.9166g,Na 2 CO 3 : 7.1722g, NaF: 1.1050g, YF 3 :5.4850g,ErF 3 : 0.4215g, fully mixed evenly with a ball mill mixer, placed in a dense corundum crucible, melted at 1500°C for 1.5 hours; then poured the resulting glass melt on a metal copper mold for rapid compression molding, and annealed at 350°C 3h to obtain a transparent precursor glass; then heat-treat the precursor glass at 650°C for 3 hours to obtain a transparent rare earth ion doped β-NaYF 4 Oxyfluorine glass-ceramics. Figure 7 It is the X-ray diffraction pattern of the glass-ceramic sample after heat treatment of sample S3, compared with the PDF...

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Abstract

The invention provides a transparent rare earth ion-doped hexagonal sodium yttrium fluoride oxyfluoride glass-ceramics and a preparation method thereof. The glass is prepared from the following compositions: 50-70mol% of SiO2, 3-12mol% of Al2O3, 15-20mol% of Na2O, 5-12mol% of NaF and 5-12mol% of YF3, and a sum of the compositions is 100 percent; and the glass also is prepared from ErF3 which accounts for 0.1-1mol% of the sum of the compositions, wherein the molar content ratio of SiO2 to Al2O3 is larger than 6.5. Compared with silicate glass, the hexagonal sodium yttrium fluoride oxyfluoride glass-ceramics has lower phonon energy (as low as 230cm<-1>), lowers the multi-phonon nonradiative relaxation rate of rare earth ions, and thus enabling the up-conversion luminescence efficiency of the rare earth ions in the glass-ceramics to be obviously improved.

Description

technical field [0001] The invention relates to the field of luminescent materials, in particular to a transparent rare earth ion doped β-NaYF 4 Oxyfluoride glass-ceramic and its preparation method. Background technique [0002] Rare earth-doped upconversion luminescent materials have attracted extensive attention in various fields because of their unique luminescent properties. However, up-conversion phosphors prepared by synthesis methods such as water / solvothermal method, liquid phase co-precipitation method, and thermal decomposition method have limitations in the application of solid-state lasers due to their high scattering and opacity. Therefore, we expect to obtain bulk upconversion materials with high transparency, good chemical and mechanical stability. [0003] Oxide glass has obvious advantages in chemical stability, mechanical strength and other indicators, but the phonon energy of oxide glass is too high, which leads to the unsatisfactory up-conversion lumine...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C10/16C03C4/12
CPCC03C10/16C03C4/12
Inventor 韩建军刘亚丽刘超赵志永
Owner WUHAN UNIV OF TECH
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