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A kind of organic hybrid rare earth lead silver iodine quaternary compound and its preparation method

A quaternary compound and organic hybrid technology, applied in the direction of organic chemistry, etc., to achieve the effects of optimizing photoelectric performance, convenient separation and purification of products, and high yield

Inactive Publication Date: 2016-01-20
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The purpose of the first aspect of the present invention is to overcome the defect that the existing room temperature diffusion method can only synthesize lead-iodide ternary compounds containing rare earth complex ions and silver-iodine ternary compounds containing rare earth complex ions, and provide a kind of compound with clear structure and semiconductor properties. Excellent new organic hybrid rare earth lead silver iodine quaternary compound

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment one: [Eu(DMSO) 7 (DMF)]Pb 3 Ag 4 I 13

[0029] Eu(NO 3 ) 3 (0.169 g, 0.5 mmol), PbI 2 (0.692 g, 1.5 mmol), AgNO 3 (0.340 g, 2 mmol) and KI (0.664 g, 4 mmol) were added to 3.0 ml of DMSO and 0.5 ml of DMF, and reacted at a constant temperature of 70 ° C for 3 hours under constant stirring. After being cooled to room temperature, it was allowed to stand at 0° C. for 3 days, and yellow crystals were precipitated, which were filtered and washed with 5 ml of cold ethanol. The yield was 85%. Elemental analysis: C, 7.86; H, 1.54; N, 2.79; S, 0.85%, C 23 h 55 N 7 o 8 SEuPb 3 Ag 4 I 13 Theoretical: C, 8.02; H, 1.61; N, 2.85; S, 0.93%. Infrared absorption spectrum data (KBr, cm -1 ): 1666s (C=O), 1479s, 1433s, 1380s, 1246s, 1106s, 1049m (C-N), 1012s (S-O), 953m, 677s, 537w, 429m (Eu-O). Loss of DMSO and DMF ligands in the temperature range 115–278°C when heated, determined by solid-state absorption spectroscopy: semiconductor energy gap E g =2.51eV. ...

Embodiment 2

[0030] Embodiment two: [Yb(DMSO) 7 (DMF)]Pb 3 Ag 4 I 13

[0031] Yb(NO 3 ) 3 (0.180 g, 0.5 mmol), PbI 2 (0.692 g, 1.5 mmol), AgNO 3 (0.340 g, 2 mmol) and KI (0.830 g, 5 mmol) were added to 2.6 ml of DMSO and 0.4 ml of DMF, and reacted at 80°C for 2.5 hours under constant stirring. After being cooled to room temperature, it was allowed to stand at 0°C for 3 days, and yellow crystals were precipitated, filtered, washed with 5 ml of cold ethanol, and the yield was 81%. Elemental analysis: C, 7.88; H, 1.55; N, 2.73; S, 0.86%, C 23 h 55 N 7 o 8 BYZGR 3 Ag 4 I 13 Theoretical: C, 7.97; H, 1.60; N, 2.83; S, 0.93%. Infrared absorption spectrum data (KBr, cm -1 ): 1661s (C=O), 1493s, 1433s, 1378s, 1248s, 1108s, 1053m (C-N), 1012s (S-O), 961m, 857w, 674s, 677s, 540w, 431m (Yb-O). Loss of DMSO and DMF ligands in the temperature range 110–270°C, determined by solid-state absorption spectroscopy: semiconductor energy gap E g =2.42eV.

Embodiment 3

[0032] Embodiment three: [Y(DMSO) 7 (DMF)]Pb 3 Ag4 I 13

[0033] Set Y(NO 3 ) 3 (0.137 g, 0.5 mmol), PbI 2 (0.692 g, 1.5 mmol), AgNO 3 (0.340 g, 2 mmol) and KI (0.830 g, 5 mmol) were added to 2.6 ml of DMSO and 0.4 ml of DMF, and reacted at a constant temperature of 70 ° C for 4 hours under constant stirring. After being cooled to room temperature, it was allowed to stand at 0° C. for 3 days, and yellow crystals were precipitated, which were filtered and washed with 5 ml of cold ethanol. The yield was 93%. Elemental analysis: C, 7.91; H, 1.57; N, 2.80; S, 0.88%, C 23 h 55 N 7 o 8 SYPb 3 Ag 4 I 13 Theoretical: C, 8.17; H, 1.64; N, 2.90; S, 0.95%. Infrared absorption spectrum data (KBr, cm -1 ): 1660s (C=O), 1492s, 1438s, 1380s, 1248s, 1108s, 1054m (C-N), 1006s (S-O), 955m, 860m, ​​674s, 671s, 540w, 407m (Y-O). Loss of DMSO and DMF ligands in the 110–262°C temperature range, determined by solid-state absorption spectroscopy: semiconductor energy gap E g =2.67eV....

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Abstract

The invention discloses an organic hybrid rare-earth Pb-Ag-I quaternary compound which has a general formula [Ln(DMSO)7(DMF)]Pb3Ag4I13, wherein Ln is rare-earth metal, DMF is N,N-dimethylformamide, and DMSO is dimethylsulfoxide. The organic hybrid rare-earth Pb-Ag-I quaternary compound is explicit in structure; a [PbxAgyIz]n-ternary ion structure is effectively adjusted and controlled by mixing [Ln(DMSO)7(DMF)]3 and rare-earth coordination ions, and further, the photoelectric performance of the rare-earth Pb-Ag-I quaternary compound is optimized. The invention also provides a preparation method of the rare-earth Pb-Ag-I quaternary compound. The preparation method comprises the following steps of: with available rare earth nitrate and silver nitrate as raw materials instead of rare-earth iodide and silver iodide, introducing rare-earth nitrate to a Pb / Ag / I ternary system, and carrying out a one-step reaction in a DMF and DMSO mixed organic solvent under a heating condition to prepare the rare-earth Pb-Ag-I quaternary compound. According to the rare-earth Pb-Ag-I quaternary compound and the preparation method thereof, the synthesis steps are simple, the rare-earth Pb-Ag-I quaternary compound is convenient to separate and purify and the yield is high.

Description

technical field [0001] The invention relates to an organic hybrid rare-earth lead-silver-iodide quaternary compound and a preparation method thereof. Background technique [0002] Organic hybrid lead iodide and silver iodide are excellent semiconductor and optoelectronic materials, and have broad application prospects in inorganic-organic hybrid materials and composite materials. I – The ion has four pairs of lone pairs of electrons, which can be monodentate and Pb 2+ and Ag + Ion coordination, and can be μ-I, μ 3 -I and μ 4 -I bridging coordination mode and Pb 2+ and Ag + The ions are coordinated to form structurally diverse [Pb x I y ] n– , [Ag x I y ] m– Binary ions. Under the action of organic cationic templates, lead iodine and silver iodine not only exhibit structural diversity, which endow iodides with unique optoelectronic and semiconducting properties, but also their optoelectronic and semiconducting properties are influenced and regulated by organic ca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F19/00
Inventor 贾定先王芳汤春英
Owner SUZHOU UNIV
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