An upconversion glass-ceramic composite material of selectively rare earth-doped scandium-based fluoride nanocrystals
A technology based on fluorinated nanometer and glass ceramics, which is applied in glass furnace equipment, glass manufacturing equipment, manufacturing tools and other directions, can solve problems such as mismatch and difficult doping, and achieve the effects of low cost and simple preparation process.
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[0024] The preparation method of the above-mentioned glass-ceramics, the method is prepared by adopting the traditional melting quenching method and subsequent crystallization heat treatment, and the specific preparation process is as follows:
[0025] The powder raw material SiO 2 、Al 2 o 3 、K 2 CO 3 , KF, LnF 3 、ScF 3 , LnF 3 (Ln=Y, Yb, Lu) and ErF 3 Weigh the compound according to molar percentage, grind it evenly in an agate mortar, put it in a crucible, heat it in a resistance furnace to 1350-1550°C and keep it warm for 0.5-1 hour, then quickly pour the molten glass into 400-500°C for preheating Shaped in a copper mold; the annealed glass is heated and kept at 600-800°C for 2 hours to make it crystallize, and the KSc-containing 2 f 7 Nanocrystalline transparent glass-ceramic composites.
Embodiment 1
[0026] Embodiment 1: SiO 2 、Al 2 o 3 、K 2 CO 3 , KF, ScF 3 , YbF 3 and ErF 3 According to 44.4SiO 2 :6Al 2 o 3 :9K 2 CO 3:18.8KF:20ScF 3 :1.6YbF 3 :0.2ErF 3 The ratio (molar ratio) is accurately weighed, ground evenly in an agate mortar, placed in a crucible, heated to 1500°C in a resistance furnace for 30 minutes, and then quickly poured the molten glass into a preheated 400°C Forming in a copper mold; the annealed glass continues to be heated at 750°C for 2 hours to crystallize it to obtain Yb 3+ / Er 3+ Doped KSc 2 f 7 Embedded transparent glass-ceramic composite.
[0027] The X-ray diffraction pattern shows that the precursor glass is a typical amorphous structure, and the orthorhombic structure KSc is precipitated in the aluminosilicate glass substrate after heat treatment 2 f 7 crystal phase ( figure 1 ), the transmission electron microscope observation shows that there are a large number of KSc with a size of about 40-50nm uniformly distributed in th...
Embodiment 2
[0028] Embodiment 2: SiO 2 、Al 2 o 3 、K 2 CO 3 , KF, ScF 3 , YbF 3 and ErF 3 According to 38SiO 2 :6Al 2 o 3 :9K 2 CO 3 :18.8KF:16ScF 3 :12YbF 3 :0.2ErF 3 The ratio (molar ratio) is accurately weighed, ground evenly in an agate mortar, placed in a crucible, heated to 1500°C in a resistance furnace for 30 minutes, and then quickly poured the molten glass into a preheated 400°C Forming in a copper mold; the annealed glass continues to be heated at 750 ° C for 2 hours to make it crystallize, and Er 3+ Doped with orthorhombic structure KYb 2 f 7 and the orthogonal structure KSc 2 f 7 A transparent glass-ceramic composite of dual-phase nanocrystals, the sample emits bright red light under excitation at 980nm.
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