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Optical oxygen sensing composite material and preparation method thereof

A composite material and oxygen sensing technology, applied in the field of Eu complex-based optical oxygen sensing composite material and its preparation

Inactive Publication Date: 2010-06-02
CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the only optical oxygen sensing material using Eu(III) complexes as light-emitting molecules is Eu(PHEN)(TTA) 3 However, the sensitivity of this material is only 1.91, while the practical application index sensitivity of oxygen sensing materials should be greater than or equal to 3.0

Method used

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  • Optical oxygen sensing composite material and preparation method thereof
  • Optical oxygen sensing composite material and preparation method thereof
  • Optical oxygen sensing composite material and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0050] The preparation of the second ligand 10H-dipyridyl[f,h]indole[3,2-b]quinoline (DPIQ) of the present invention comprises the following steps:

[0051] a. Synthesis of ligand 1,10-o-phenanthroline-5,6-dioxime

[0052] Weigh 0.42 g of 1,10-phenanthroline-5,6-dione, 0.486 g of hydroxylammonium hydrochloride, and 3.00 g of barium carbonate, dissolve them in 30 ml of ethanol, and reflux for 12 hours. After removing ethanol under reduced pressure, add 40ml of 0.2M hydrochloric acid solution to the residue, stir for 30 minutes, filter with suction, wash the filter cake with water, ethanol and ether respectively, and dry under vacuum at 80°C to obtain a yellow solid 1,10-phenanthroline -5,6-dioxime 0.464g (95% yield).

[0053] b. Synthesis of ligand 1,10-o-phenanthroline-5,6-diamine

[0054] Weigh 0.4g of 1,10-phenanthroline-5,6-dioxime and 0.4g of Pd / C (10%), dissolve in 100ml of absolute ethanol, and heat under the protection of nitrogen. At the same time, a mixed solution ...

Embodiment 2

[0058] Eu(DPIQ)(TTA) according to the present invention 3 Preparation of complexes.

[0059] Weigh 0.147 g of the first ligand 4,4,4-trifluoro-1,12-thiophene (TTA) and 0.071 g of the second ligand DPIQ, dissolve in 10 ml of ethanol, and neutralize with NaOH to pH=7. EuCl 3 ·6H 2 O 0.081g was dissolved in 10ml of pure water, poured into the reaction solution, heated and stirred at 60°C for 1 hour, a precipitate formed, filtered and dried to obtain a white solid Eu(DPIQ)(TTA) 3 0.08 g (70% yield).

[0060] Eu(DPIQ)(TTA) obtained above was tested under oxygen, nitrogen and air conditions 3 emission spectrum, such as figure 1 shown. Eu(DPIQ)(TTA) 3 The emission spectra in different gas atmospheres show that Eu 3+ Narrowband characteristic emission from Eu 3+ of 5 D. 0 - 7 f 2 The transition emission intensity decreases with the increase of oxygen concentration.

Embodiment 3

[0062]Eu(DPIQ)(TTA) described in the present invention 3 / MCM-41 Optical Oxygen Sensing Composite Fabrication.

[0063] Weigh Eu(DPIQ)(TTA) respectively 3 0.01g, 0.02g, 0.03g, dissolved in 10ml of dichloromethane, added 1g of inorganic mesoporous molecular sieve MCM-41 respectively, stirred at room temperature for 6-12 hours, filtered, washed with dichloromethane until the solution was free from UV light color. Dry at 60°C for 1-2 days, grind and place in a desiccator to obtain yellow powder Eu(DPIQ)(TTA) with doping concentrations of 10mg / g, 20mg / g and 30mg / g respectively 3 / MCM-41.

[0064] The emission spectra of the composite material under different oxygen concentrations under the above-mentioned different doping concentrations were measured, as shown in figure 2 shown. Depend on figure 2 It can be seen that the luminescence intensity of the composite material is greatly quenched with the increase of oxygen concentration. The result was linearly fitted to obtain ...

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Abstract

The invention relates to an oxysensitive optical oxygen sensing function material suitable for preparing an optical oxygen sensor, in particular to an optical oxygen sensing composite material and a preparation method thereof. An Eu (DPIQ)(TTA)3 complex serving as a light-emitting molecule is physically doped into a mesoporous molecular sieve serving as a carrier material. The Eu (DPIQ)(TTA)3 complex has a structural formula. The composite material has characteristics of long fluorescent life span, large Stoke displacement, narrow-band emission and high stability, can eliminate the interference of the background light source in most visible areas, thereby having relatively great application potential in the aspect of the integrated sensor taking OLED as the excitation light source.

Description

technical field [0001] The invention relates to an oxygen-sensitive optical oxygen sensing functional material suitable for preparing an optical oxygen sensing device, in particular to a novel optical oxygen sensing composite material based on Eu(III) complex and a preparation method thereof. Background technique [0002] As we all know, living organisms can only maintain various physiological functions when there is a continuous supply of oxygen. Oxygen is widely involved in various fields of social life, so the detection of oxygen is of great significance in biology, medicine, industry, environment and other aspects. The commonly used oxygen detection methods are the Winkler iodometric method and the Clark dissolved oxygen electrode method. The former method needs to fix the dissolved oxygen in water and cannot be detected online; the latter method uses the oxidation-reduction reaction of the electrode itself to detect the concentration of oxygen and determine Oxygen is c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06G01N21/64
Inventor 李斌左青卉王樱蕙刘艳红
Owner CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI
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