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Light-emitting organic metal silver compound with binary emission as well as preparation and application thereof

A technology of silver complexes and organometallics, which is applied in the preparation and optical properties of organometallic silver halide cluster complexes, can solve the problems of temperature and luminescence sensing staying in the ideal stage, and achieve high actual production repeatability, strong photoinduced Excellent effect of luminescence and thermal stability

Active Publication Date: 2018-11-23
SHANTOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These problems have led to the fact that the luminescence sensing of this type of material is still in the ideal stage.

Method used

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  • Light-emitting organic metal silver compound with binary emission as well as preparation and application thereof
  • Light-emitting organic metal silver compound with binary emission as well as preparation and application thereof
  • Light-emitting organic metal silver compound with binary emission as well as preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] 1. Organic ligand 1-methyl-4-(3-(5-phenyl-pyrazol) base) pyridinium nitrate (HL-NO 3 ) synthetic route such as figure 1 As shown, it mainly includes the following steps:

[0060] The first step: Potassium tert-butoxide (11.2g, 0.1mol) was dissolved in 200ml tetrahydrofuran, after stirring evenly, add acetophenone (14.0ml, 0.11mol) and methyl 4-picolinate (12.0ml, 0.10mol ), after stirring for 12 hours, 60 mL of an aqueous solution containing 20 mL of acetic acid was added to the substance, and after sufficient stirring, the mixture was extracted with 3 × 20 mL of ether, and the desired product was obtained after the ether was spin-dried in vacuo.

[0061] The second step: the product from the previous step was dissolved in 200 ml of ethanol and hydrazine hydrate (10 ml, 0.20 mol), refluxed for 12 hours, and vacuum rotary evaporated, and the product was recrystallized with methanol and water to obtain the product.

[0062] The third step: the product of the previous st...

Embodiment 2

[0080] metal complex [Ag 2 Br 2 L] n preparation of

[0081] AgBr (0.05mmol, 0.009g), HL-NO 3 (0.05mmol, 0.015g), acetonitrile (1.0ml), ammonia water (0.5ml), and DMAC (1.0ml) were added to the reaction kettle, ultrasonicated for 15min, sealed and heated at 80-100°C for 3-5 days, and then Cool to 30°C at a rate of 3°C per hour. Open the kettle, filter, wash away impurities with a small amount of methanol, and obtain yellow columnar crystals after drying at room temperature. The same operation steps, different solvent combinations: acetonitrile (2ml), ammonia (0.5ml), ethanol (0.5ml); acetonitrile (2.0ml), ammonia (0.5ml), dimethylformamide (0.5ml); acetonitrile (2ml), ammonia (0.5ml), methanol (0.5ml); acetonitrile (2ml), ammonia (0.5ml) dimethyl sulfoxide (0.5ml); acetonitrile (2ml), ammonia (0.5ml) can be combined [Ag 2 Br 2 L] n . Variable temperature powder diffraction pattern as Figure 19 shown, from Figure 19 It can be seen that the complex [Ag 2 Br 2L] ...

Embodiment 3

[0084] metal complex [Ag 2 LCl 2 ] n preparation of

[0085] In the polytetrafluoroethylene liner of a reaction kettle with a volume of 12mL, metal salt AgCl (0.1mmol, 15mg) was added, and the ligand HL-NO 3 (0.1 mmol, 29.8 mg), acetonitrile (4.0 mL) and methanol (2.0 mL), ammonia (1.0 mL), water (1.0 mL). After half an hour of sonication with an ultrasonic instrument, cover the lid of the inner liner and seal the inner liner into the stainless steel shell of the reaction kettle, heat to 120°C and keep the temperature constant for 72 hours, then cool to 30°C at a rate of 3°C / h, filter and After washing with water, yellow columnar crystals were obtained.

[0086] The prepared metal complex [Ag 2 LCl 2 ] n The crystallographic data are shown in Table 2, [Ag 2 LCl 2 ] n Belongs to the monoclinic system P2 1 The / n space group is a simple one-dimensional chain complex, such as Figure 25 shown. Its asymmetric unit contains a proton-removing ligand, two Ag atoms and tw...

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Abstract

The invention relates to a series of silver halogen series compounds with a one-dimensional chain-shaped structure. A chemical formula is [Ag2LX2]n or [Ag2X2L]n, wherein n is a non-zero natural number; X is selected from halogen atoms including Cl, Br, I and the like; L is 1-methyl-4-(3-(5-phenyl-pyrazole)yl)pyridine. Along the changes of temperature, a certain linear function relation is formed between a ratio of a low-energy emission peak and high-energy emission strength of the light-emitting organic metal silver compound with the binary emission, and the temperature. Preparation comprisesthe following steps: (1) uniformly stirring an organic ligand and AgX in a solvent according to a certain mass ratio and carrying out solvothermal reaction; (2) keeping constant temperature for 3 to 5days under the temperature of 80 to 120 DEG C and cooling to 30 DEG C at the cooling speed of 3 to 5 DEG C / h, so as to obtain a lot of light yellow columnar crystals. The compound provided by the invention has good thermal stability, and the temperature detection accuracy can be effectively improved through self-correction light-emitting sensing of the temperature; the compound can be used as a self-correction molecular-based light-emitting thermometer, and a temperature testing range is relatively wide. The preparation cost is relatively low, the process is simple and the energy consumptionis low.

Description

technical field [0001] The invention relates to the preparation and optical properties of an organometallic silver halide cluster complex, and relates to a luminescent organometallic silver complex with binary emission and its preparation and self-correcting luminescent temperature sensing application. Background technique [0002] Temperature is an important basic physical parameter, and its accurate detection is crucial to scientific research and the development of modern technology. The traditional temperature sensor is a contact thermometer. During the temperature measurement process, the thermometer needs to be in contact with the measured object for a certain period of time to achieve the heat transfer effect. The contact detection conditions of this type of thermometer limit its scope of application, making it unable to meet the temperature detection of specific external conditions, such as the temperature measurement of fast-moving objects and sub-micron materials. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F1/10C09K11/06G01K11/20
CPCC07F1/005C09K11/06C09K2211/188G01K11/20
Inventor 黄晓春金伟光
Owner SHANTOU UNIV
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