Cocoon-shaped TbPO4 powder with good luminescence property and preparation method thereof
A technology of luminescence performance, NH4H2PO4, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as pollution, and achieve the effects of good dispersion, good repeatability, and uniform grain size
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[0022] A cocoon-like TbPO with good luminescent properties 4 The preparation method of powder comprises the following steps:
[0023] Step 1): Add Tb(NO 3 ) 3 ·6H 2 O was dissolved in deionized water and stirred for 5-10min to form a terbium salt solution; the NH 4 h 2 PO 4 The solution is evaporated to recrystallization, and the crystals are dissolved in deionized water to form NH with a concentration of 2.7mol / L 4 h 2 PO 4 solution, the NH 4 h 2 PO 4 solution, with terbium salt solution according to PO 4 3- :Tb 3+ = 60:1 molar ratio mixed, and when mixed, the terbium salt solution was added dropwise to the NH 4 h 2 PO 4 Stir in the solution for 10min, then use ammonia water and dilute HNO 3 Adjust the pH of the precursor solution to pH=2, and then obtain the precursor solution;
[0024] Step 2): Transfer the precursor solution obtained in step 1) to a reactor lined with polytetrafluoroethylene, and the volume filling degree of the reactor is 60%-80%;
[00...
Embodiment 1
[0029] Step 1: Add 0.9mmol of Tb(NO 3 ) 3 ·6H 2 O was dissolved in deionized water, stirred for 5min, and 54mmol of NH 4 h 2 PO 4 Dissolve in deionized water, heat the solution until recrystallization, then add deionized water to obtain NH with a concentration of 2.7mol / L 4 h 2 PO 4 In deionized water, the terbium salt and NH 4 h 2 PO 4 Deionized water solution according to PO 4 3- :Tb 3+ =60:1 molar ratio mixed, terbium salt solution was added dropwise to NH 4 h 2 PO 4 In the solution, stir for 10 minutes to form a precursor solution, using ammonia water and dilute HNO 3 Adjust the pH of the precursor solution=2;
[0030]Step 2: Transfer the precursor solution to a reactor lined with polytetrafluoroethylene, and the volume filling degree of the reactor is 80%;
[0031] Step 3: Using low-temperature hydrothermal method, set the hydrothermal reaction temperature to 100°C and the holding time to 24h, take out the white precipitate formed after the reaction, cent...
Embodiment 2
[0033] Step 1: Add 0.9mmol of Tb(NO 3 ) 3 ·6H 2 O was dissolved in deionized water, stirred for 10 min, and 54 mmol of NH 4 h 2 PO 4 Dissolve in deionized water, heat the solution until recrystallization, then add deionized water to obtain NH with a concentration of 2.7mol / L 4 h 2 PO 4 In deionized water, the terbium salt and NH 4 h 2 PO 4 Deionized water solution according to PO 4 3- :Tb 3+ =60:1 molar ratio mixed, terbium salt solution was added dropwise to NH 4 h 2 PO 4 In the solution, stir for 10 minutes to form a precursor solution, using ammonia water and dilute HNO 3 Adjust the pH of the precursor solution=2;
[0034] Step 2: Transfer the precursor solution to a reactor lined with polytetrafluoroethylene, and the volume filling degree of the reactor is 60%;
[0035] Step 3: Using low-temperature hydrothermal method, set the hydrothermal reaction temperature to 100°C and the holding time to 24h, take out the white precipitate formed after the reaction, ...
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