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Near infrared fluorescence temperature sensing method and material

A sensing method, fluorescent temperature technology, applied in the field of temperature sensing, can solve the problems of limited detection depth and application, and achieve the effect of excellent detection accuracy and excellent detection depth

Active Publication Date: 2016-09-28
PEKING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

On the other hand, most luminescent temperature materials utilize photoexcitation or photoemission properties in the ultraviolet or visible wavelength range, which greatly limits their detection depth and application in biological analysis.

Method used

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  • Near infrared fluorescence temperature sensing method and material
  • Near infrared fluorescence temperature sensing method and material
  • Near infrared fluorescence temperature sensing method and material

Examples

Experimental program
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Effect test

Embodiment 1

[0065] Embodiment 1, synthetic photosensitive ligand DFQZ (in the formula I, R 1 , R 2 is ethyl; R 3 , R 4 is butyl; R 5 =R 6 =R 7 =R 8 = methyl)

[0066] In the present embodiment, the DFQZ synthetic route, experimental conditions and each step yield are as follows:

[0067]

[0068] The specific operation steps are as follows:

[0069] 1) Synthesis of 2-(N,N-diethyl)-7-bromofluorene (compound 2)

[0070] In a 100ml round bottom flask, 2-amino-7-bromofluorene (compound 1) (1.0g, 3.8mmol) was dissolved in 60ml of glacial acetic acid. Place the reaction solution in an ice-water bath, slowly add 1.6g NaBH 4 (42.7mmol), heating makes the reaction solution rise to room temperature, then slowly adds 1.6gNaBH 4 , heating the reaction solution to 85° C. and maintaining it for 40 minutes. After the reaction was complete, it was cooled to room temperature, and NaOH aqueous solution was added to make the system neutral. The product was extracted three times with dichloro...

Embodiment 2

[0078] Embodiment 2, synthetic photosensitive complex Yb (tta) 3 · DFQZ (in formula III, R 1 , R 2 is ethyl; R 3 , R 4 is butyl; R 5 = R 6 = R 7 = R 8 = methyl)

[0079] Under stirring conditions, Yb(NO 3 ) 3 ·xH 2 O (470.0mg, 1.0mmol) ethanol solution (15mL) was added dropwise to HTTA (666.6mg, 3.0mmol) ethanol solution (15mL), and stirring was continued at room temperature, while ammonia water was added dropwise to adjust the pH value of the solution to neutral. After heating the reaction at 80-85° C. for 3 h, it was cooled to room temperature. Spin to dry ethanol to obtain a light yellow solid, wash the solid repeatedly with water, add benzene to dissolve the solid, and use anhydrous CaCl 2 dry. After filtering off the desiccant, distill off the solvent under reduced pressure to obtain a light yellow oil, add petroleum ether, heat, filter out the insoluble matter, distill off the petroleum ether under reduced pressure, and dry under vacuum to obtain the produc...

Embodiment 3

[0084] Embodiment 3, preparation is based on PMMA-Yb (tta) 3 · DFQZ temperature sensor

[0085] 1 mg Yb(tta) was mixed with stirring 3 DFQZ was dissolved in 10 mL of acetone solution containing 9 mg of polymethyl methacrylate (PMMA), and then the resulting mixed solution was dropped onto a 1.2 cm × 1.7 cm × 0.1 cm quartz plate, and dried in vacuum at 40 ° C for 12 hours to remove the solvent and form PMMA-Yb(tta) with a thickness of about 2.1 μm 3 ·DFQZ fluorescent temperature sensing film.

[0086] Image 6 PMMA-Yb(tta) under nitrogen atmosphere 3 ·The emission spectrum of DFQZ film at 78-328K. Unlike previously reported organic rare earth complexes, PMMA-Yb(tta) 3 ·The fluorescence intensity of DFQZ film increased significantly. At the same time, the temperature is increased from 78K to 328K, and the quantum yield of luminescence is increased by 5 times, from 0.2% to 1.0%.

[0087] Figure 7 a) and b) are PMMA-Yb(tta) under nitrogen and oxygen atmosphere respectivel...

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Abstract

The invention discloses a near infrared light emitting temperature sensing method and a key material thereof. The ratio of fluorescence intensity in the wavelength range of 900 to 970nm and fluorescence intensity in the wavelength range of 900 to 985nm in the emission spectrum of Yb3+ or the logarithmic value thereof, or the ratio or the logarithmic value of the fluorescence intensities of two light emitting bands respectively located near 945nm and 976nm in the emission spectrum of Yb3+ or the logarithmic value thereof is used as the parameter of measurement temperature. According to the sensing method and the material, the problem that temperature detection is disturbed by oxygen concentration in a traditional fluorescence temperature sensing technology is overcome; a rare earth light emitting material provided by the invention exhibits a unique light emitting characteristic; due to the features, the temperature sensing method and the material have the excellent near infrared light emitting temperature measurement accuracy and confidence.

Description

technical field [0001] The invention relates to temperature sensing technology, in particular to a near-infrared fluorescent temperature sensing method and materials for realizing the sensing method. Background technique [0002] Temperature is one of the basic parameters of various science and technology. Compared with the traditional contact temperature sensor, the luminescence temperature sensor has the advantages of fast response time, non-contact measurement method, and high spatial resolution (R.J.Meier, et al., Chem.Soc.Rev.2013, 42, 7834) , so it has broad application prospects in aspects such as live cell analysis, aerodynamic research, high voltage or strong electromagnetic environment monitoring, coating research and development, and food storage (M.Schaeferling, et al., Adv.Funct.Mater.2008, 18, 1399). [0003] Luminescence temperature sensors are usually based on the luminescence properties of photoluminescent materials, such as the luminescence wavelength pos...

Claims

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Application Information

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IPC IPC(8): G01J5/00C07F5/00C09K11/06C07D403/14
CPCC07D403/14C07F5/003C09K11/06C09K2211/1059C09K2211/182G01J5/00
Inventor 王远黄彦捷汤敏贤
Owner PEKING UNIV
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