Cage oligomeric silsesquioxane and rare earth ion luminescent material thereof

A technology of polysilsesquioxane and rare earth ions, which is applied in the direction of luminescent materials, silicon organic compounds, chemical instruments and methods, etc., can solve the problems of rare research reports, achieve strong photostability, rich colors, and fluorescence long life effect

Inactive Publication Date: 2013-04-17
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Given that POSS is a nanoparticle with a new structure and a matrix for the preparation of new inorganic-organic hybrid materials, combining POSS with rare earth ions is undoubtedly a topic worthy of research, and there are no research reports in this area yet. more common

Method used

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  • Cage oligomeric silsesquioxane and rare earth ion luminescent material thereof
  • Cage oligomeric silsesquioxane and rare earth ion luminescent material thereof
  • Cage oligomeric silsesquioxane and rare earth ion luminescent material thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] ① Dissolve 580.0mg (10.30mmol) of potassium hydroxide (commercially available) in 9mL of dimethyl sulfoxide, heat in an oil bath at 80°C for 5min until the solution turns yellow, then dissolve 335.5μL (2.15mmol) of 1,6-hexane Add dithiol (commercially available), 575.0mg (2.15mmol) 4'-chloro-2,2':6',2''-terpyridine (commercially available) into the above yellow solution, heat and stir in an oil bath at 70°C for 4h Then stop heating, add 100mL double-distilled water, 30mL dichloromethane to make it precipitate, and centrifuge to obtain a white powdery substance, which is a terpyridine derivative, which is recorded as TpySH.

[0033] ②, Dissolve 137.7mg (0.2175mmol) of octavinyl cage oligomeric silsesquioxane (VPOSS), 663.8mg (1.74mmol) of the above terpyridine derivative (TpySH) in 10mL of chloroform (99.5%) , drop two drops of n-propylamine (2% of the mass of raw material VPOSS) to catalyze, stir and heat in an oil bath at 50°C for 24h to obtain a colorless solution.

...

Embodiment 2

[0045] In the embodiment 1, the steps are wrong! Reference source not found. The obtained terpyridine derivative (TpySH) is replaced with acrylic acid (AA) (commercially available), and the oligomeric silsesquioxane compound is denoted as VPOSS-8AA, and all the other conditions are the same as in Example 1, and finally a rare earth / cage type Oligomeric silsesquioxane synthetic rare earth luminescent material.

[0046] The VPOSS-8AA was determined by nuclear magnetic analysis and mass spectrometry, and the luminescent properties of the material (such as absorption spectrum, emission spectrum, excitation spectrum, fluorescence decay curve, etc.) Thermal stability was determined by scanning calorimetry.

[0047] The NMR of the tested ionic liquid is as follows:

[0048] 1 H NMR (DMSO): δ7.953 (s, 8H), δ6.090 (d, 16H), δ2.891 (s, 27H), δ2.731 (s, 25H).

[0049] The physical and chemical parameters of the material tested are as follows:

[0050] Excitation spectrum (detection...

Embodiment 3

[0054] Change the rare earth europium chloride in step ④ in Example 1 to rare earth neodymium chloride to prepare a luminescent material. All the other conditions are with embodiment 1.

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Abstract

The invention relates to cage oligomeric silsesquioxane and a rare earth ion luminescent material thereof. According to the invention, octavinyl polyhedral oligomeric silsesquioxane (VPOSS) is adopted as a matrix and a terpyridine derivative (TpySH) is grafted on the double bond connected with the Si atom at the apex of a VPOSS polyhedron so as to prepare the novel cage oligomeric silsesquioxane (VPOSS-8TpySH) which is capable of coordinating with rare earth ion to form a metal complex on the one hand and capable of absorbing energy and transferring the absorbed energy to the rare earth ion on the other hand. The obtained rare earth compound/oligomeric silsesquioxane material has the advantages of rich luminescent color, high colour purity, long fluorescent lifetime (0.58ms), high quantum efficiency (19.8), good heat stability (400 DEG C) and high light stability, is an optical material of great value and can be applied to the fields of displaying and imaging, new light sources, X-ray intensifying screens and the like.

Description

Technical field: [0001] The invention belongs to the field of rare earth functional materials, in particular to a preparation method of a cage-type oligosilsesquioxane and a rare earth ion luminescent material. Background technique [0002] Rare earth ions have excellent luminescent properties (such as high color purity, long fluorescence lifetime, rich emission lines, etc.) due to their unique 4f-layer electron configuration. , Luminescent materials and other fields have potential application value. [0003] The general molecular formula of polysilsesquioxane is (RSiO3 / 2)n (the atomic ratio of O and Si in the molecule is 3:2), and R in the formula can be H, alkyl, alkylene, aryl, Aryl groups or substituents of these groups. Polysilsesquioxanes have random, cage, trapezoidal, and bridge structures, among which polysilsesquioxanes with cage structures are called polyhedral oligomeric silsesquioxanes (POSS for short). The molecular structure of POSS is a hybrid structure, w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/21C09K11/06
Inventor 李焕荣张盼宁陈晓凡
Owner HEBEI UNIV OF TECH
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