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

A quaternary compound and organic hybrid technology, applied in organic chemistry, chemical instruments and methods, luminescent materials, etc., to achieve the effects of simple synthesis steps, optimized photoelectric performance, and high yield

Inactive Publication Date: 2016-03-16
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] Example one: [La(DMF) 8 ] 2 Pb 3 Ag 10 I 22

[0029] La(NO 3 ) 3 (0.162 g, 0.5 mmol), PbI 2 (0.346 g, 0.75 mmol), AgNO 3 (0.425 g, 2.5 mmol) and KI (0.830 g, 5 mmol) were added to 3.0 ml DMF, and reacted at 70°C for 3 hours under constant stirring. After cooling to room temperature and standing at 0°C for 3 days, light yellow crystals were precipitated, which were filtered and washed with 5 ml of cold ethanol. The yield was 78%. Elemental analysis: C,9.71; H,1.90; N,3.77%, C 48 H 112 N 16 O 16 La 2 Pb 3 Ag 10 I 22 Theoretical value: C, 9.58; H, 1.82; N, 3.68%. Infrared absorption spectrum data (KBr, cm -1 ): 1669s (C=O), 1490s, 1433s, 1378s, 1246s, 1108s, 1051m (C-N), 857w, 674s, 533m, 402m (La-O). When heated, the DMF ligand is lost in the temperature range of 110-266°C, solid-state absorption spectrometry: semiconductor energy gap E g =2.54eV.

Embodiment 2

[0030] Embodiment 2: [Eu(DMF) 8 ] 2 Pb 3 Ag 10 I 22

[0031] Put Eu(NO 3 ) 3 (0.169 g, 0.5 mmol), PbI 2 (0.346 g, 0.75 mmol), AgNO 3 (0.425 g, 2.5 mmol) and KI (0.830 g, 5 mmol) were added to 3.0 ml DMF, and reacted at a constant temperature of 80°C for 2 hours under constant stirring. After cooling to room temperature, it was allowed to stand at 2°C for 4 days, and yellow crystals were precipitated, which was filtered and washed with 5 ml of cold ethanol. The yield was 85%. Elemental analysis: C, 9.60; H, 1.81; N, 3.64%, C 48 H 112 N 16 O 16 Eu 2 Pb 3 Ag 10 I 22 Theoretical value: C, 9.66; H, 1.89; N, 3.76. Infrared absorption spectrum data (KBr, cm -1 ): 1671s (C=O), 1488s, 1433s, 1379s, 1246s, 1106s, 1056m (C-N), 860w, 674s, 537w, 425w (Eu-O). When heated, the DMF ligand is lost in the temperature range of 108-270°C, and the solid-state absorption spectrum measurement: semiconductor energy gap E g =2.33eV. Fluorescence spectrum measurement: the maximum emission wavelength is...

Embodiment 3

[0032] Example three: [Y(DMF) 8 ] 2 Pb 3 Ag 10 I 22

[0033] Y(NO 3 ) 3 (0.137 g, 0.5 mmol), PbI 2 (0.346 g, 0.75 mmol), AgNO 3 (0.425 g, 2.5 mmol) and KI (0.664 g, 4 mmol) were added to 3.0 ml DMF, and reacted at 60°C for 3 hours under constant stirring. After cooling to room temperature and standing at 0°C for 3 days, yellow crystals were precipitated, filtered and washed with 5 ml of cold ethanol. The yield was 87%. Elemental analysis: C, 9.69; H, 1.85; N, 3.77%, C 48 H 112 N 16 O 16 Y 2 Pb 3 Ag 10 I 22 Theoretical value: C, 9.87; H, 1.93; N, 3.84. Infrared absorption spectrum data (KBr, cm -1 ): 1668s (C=O), 1488s, 1435s, 1374s, 1246s, 1107s, 1055m (C-N), 856w, 675s, 537w, 401m (Y-O). When heated, the DMF ligand is lost in the temperature range of 110-258°C, solid-state absorption spectrometry: semiconductor energy gap E g =2.64eV. Fluorescence spectrum measurement: the maximum emission wavelength is 682nm respectively.

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Abstract

The invention discloses an organic hybrid rare earth, lead, silver and iodine quaternary compound which has a general formula of [Ln (DMF)8]2Pb3Ag10I22, wherein Ln represents a rare earth metal; and DMF represents N,N-dimethylformamide. The compound has a definite structure, and [Ln(DMF)8]<3+> rare earth coordination ions are used to effectively regulate the structure of [PbxAgyIz]n-ternary ions, thereby optimizing photoelectric properties of the rare earth, lead, silver and iodine quaternary compound. At the same time, a preparation method for the above rare earth, lead, silver and iodine quaternary compound is provided. The [Ln (DMF)8]2Pb3Ag10I22 is prepared by a one-step reaction in a DMF solvent under a heating condition, by introducing a rare earth nitrate to a Pb / Ag / I ternary system and by using easily available rare earth nitrate and silver nitrate to replace rare earth iodide and silver iodide. The preparation method is simple in synthetic steps, convenient for separation and purification of the product and high in yield.

Description

Technical field [0001] The invention relates to an organic hybrid rare earth lead silver iodine quaternary compound and a preparation method thereof. Background technique [0002] Organic hybrid lead iodide and silver iodide are semiconductor and optoelectronic materials with excellent performance, and have broad application prospects in inorganic-organic hybrid materials and composite materials. I - The ion has four lone pairs of electrons, which can be single-tooth and Pb 2+ And Ag + Ion coordination, and can use μ-I, μ 3 -I and μ 4 -I and other bridging coordination methods with Pb 2+ And Ag + Ions coordinate to form various structures [Pb x I y ] n– , [Ag x I y ] m– Binary ions. Under the action of organic cation templates, lead iodine and silver iodine not only show the diversity of structures, and thus endow iodides with unique optoelectronic and semiconductor properties, and their optoelectronic and semiconductor properties are influenced and regulated by organic cations...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F19/00C09K11/06
Inventor 贾定先王芳汤春英
Owner SUZHOU UNIV
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