Novel barium metal organic coordination polymer and preparation method and application of thereof
A coordination polymer, metal-organic technology, applied in the direction of 2/12 group organic compounds without C-metal bonds, indium organic compounds, platinum group organic compounds, etc., can solve difficult preparation, affect particle size, long period and other problems, to achieve the effect of excellent luminous performance and good thermal stability
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Embodiment example 1
[0035] Using hydrothermal method to synthesize barium metal organic coordination polymer, its steps are:
[0036] (1) Preparation of Ir 2 (ppy) 4 Cl 2
[0037] Add 0.01 mole of IrCl 3 ·3H 2 O and 0.02 moles of 2-phenylpyridine were dissolved in a mixed solvent consisting of 4.00-4.20 moles of ethylene glycol ether and 2.60-2.80 moles of water, and reacted under reflux for 24 hours to obtain a pale yellow precipitate, which was cooled to room temperature and filtered. Then wash with ethanol and acetone to get Ir 2 (ppy) 4 Cl 2 ;
[0038] The reaction equation is as follows
[0039] 2IrCl 3 ·3H 2 O+4ppy→Ir 2 (ppy) 4 Cl 2 +4H + +4Cl -
[0040] (2) Synthetic Ir(ppy) 2 (Hdcbpy)
[0041] 0.02 mole of H 2 dcbpy and 0.01 mole of Ir obtained in step (1) 2 (ppy) 4 Cl 2 Add to 37.00 moles or more of methanol solution, then add more than 0.052 moles of anhydrous sodium carbonate, reflux for more than 3 hours to obtain an orange solution;
[0042] Then the methanol solvent is evaporated to obtain an ...
Embodiment example 2
[0054] Thermogravimetric analysis and X-ray powder diffraction were used to determine the thermal stability of the material of the present invention. Use Netzsch STA449C thermal analyzer to test the mass change of samples from room temperature to 1100°C at 10°C / min, such as Figure 4 It is the barium metal organic coordination polymer {Ba 3 [Ir 6 (ppy) 12 (dcbpy) 6 (H 2 O) 4 ]}·10H 2 Thermogravigram of O crystal. In addition, heat an appropriate amount of samples at 200°C for 6 hours to perform an X-ray powder test. The obtained spectrum is as follows image 3 As shown, it is similar to the X-ray simulation spectrum of the single crystal ( figure 1 ) Very good overlap, indicating that it can still maintain a stable framework at 200°C and has good thermal stability.
Embodiment example 3
[0056] Use EdinberghAnalyticalinstrumentFLS920 test to obtain optical information.
[0057] {Ba 3 [Ir 6 (ppy) 12 (dcbpy) 6 (H 2 O) 4 ]}·10H 2 Test of O excitation spectrum, fluorescence lifetime and quantum yield test. Such as Figure 5 Shown is the {Ba 3 [Ir 6 (ppy) 12 (dcbpy) 6 (H 2 O) 4 ]}·10H 2 Excitation spectrum of O crystal; Image 6 This is {Ba 3 [Ir 6 (ppy) 12 (dcbpy) 6 (H 2 O) 4 ]}·10H 2 Emission pattern of O crystal.
[0058] As shown in the figure, the maximum excitation wavelength is 468nm, which is in the visible light band; its emission peak is 558nm, which shows yellow light, the fluorescence lifetime is 9.86us, and the quantum yield is 16%, compared to Ir(ppy) 2 (Hdcbpy) (fluorescence lifetime: 7.8us, quantum yield: 6.8%) has been greatly improved.
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