Preparation method, performance and application of novel green light-emitting material terbium lead multi-borate
A luminescent material, terbium lead borate technology, applied in the direction of luminescent material, polycrystalline material growth, boron compound, etc., to achieve the effect of simple process, low cost, high chemical stability and thermal stability
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Embodiment 1
[0014] Embodiment 1: grow compound PbTbB by cosolvent method 7 o 13 Single crystals with a size of about 0.1 mm are suitable for single crystal diffraction experiments to determine the molecular formula and fine crystal structure of compounds. The heating device for crystal growth is an ordinary muffle furnace, and the heat sensing device is a platinum-rhodium thermocouple. Choose PbO and B 2 o 3 The mixture acts as a flux to spontaneously nucleate and grow crystalline PbTbB 7 o 13 . The raw material used for the crystal is B 2 o 3 , Pb 3 o 4 , Tb 4 o 7 . The specific operation steps are as follows: after weighing the above-mentioned raw materials according to a certain dose, mix and grind them with an agate mortar and mix them evenly, put them into a platinum crucible and compact them, and heat up to 930°C in a muffle furnace until the mixture is completely melted to form Uniform and transparent light yellow liquid. After constant temperature for 24 hours, cool d...
Embodiment 2
[0015] Embodiment 2: adopt high temperature solid-phase synthesis method synthetic compound PbTbB 7 o 13 The pure phase powder, the raw materials used are PbO, Tb 2 o 3 , B 2 o 3 . Its chemical reaction equation is: 2PbO + Tb 2 o3 +7B 2 o 3 → 2PbTbB 7 o 13 . The specific operation steps are as follows: After weighing the above-mentioned raw materials according to a certain proportion, carefully grind them in a mortar, mix them evenly, put them into a platinum crucible, put them into a muffle furnace, raise the temperature to 400°C, and pre-fire at a constant temperature for 10 hours. Then the crucible was taken out after cooling, poured out the sample, re-grinded evenly, put it into the platinum crucible again, calcined in the muffle furnace at 820°C for 40 hours, and turned off the power of the muffle furnace. After cooling, take out the crucible to obtain a white powder sample, which is the compound PbTbB 7 o 13 The pure powder was tested by powder X-ray diffr...
Embodiment 3
[0016] Example 3: PbTbB 7 o 13 The single crystal diffraction data of Bruker Apex2 CCD diffractometer, Mo-Kαradiation, λ = 0.71073 Å at room temperature with ω The scanning method is collected, the data is restored by SAINT, and the multi-scan method is used for absorption correction before being used for structural analysis. The single crystal structure analysis was completed on a PC computer through the SHELX-2014 program package. The coordinates of the heavy atoms Pb and Tb were determined by the direct method, and the coordinates of the other lighter atoms B and O were given by the difference Fourier synthesis method. For all Atomic coordinates and thermal anisotropy parameters are performed based on F 2 The full-matrix least squares plane refinement to convergence. Finally, the structure was checked by the PLATON program, and no type A crystallographic errors were detected.
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