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Preparation method of porous calcite fluorescent material used for preparing fluorescent sensor

A fluorescent sensor and fluorescent material technology, applied in the direction of luminescent materials, fluorescence/phosphorescence, chemical instruments and methods, etc., can solve the problems of complex instruments, the influence of europium ion light absorption and emission performance, and the sensor is not suitable for actual testing, etc., to achieve increased area, weaken concentration quenching effect, reduce the effect of concentration quenching

Inactive Publication Date: 2019-08-23
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the luminescence of europium ions is limited by problems such as temperature quenching and concentration quenching, which have a great impact on the light absorption and emission properties of europium ions.
[0006] Currently existing lead ion sensing methods are: atomic absorption spectrometry, plasma mass spectrometry (ICP-MS) and voltammetry usually require expensive and complex instruments, as well as strict test conditions, these sensors are not suitable for practical testing

Method used

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  • Preparation method of porous calcite fluorescent material used for preparing fluorescent sensor
  • Preparation method of porous calcite fluorescent material used for preparing fluorescent sensor
  • Preparation method of porous calcite fluorescent material used for preparing fluorescent sensor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-1

[0038] Example 1-1, a method for preparing a macroporous mayenite bulk fluorescent material, the following steps are performed in sequence:

[0039] 1) At room temperature, dissolve 0.04 g of the phase separation inducer polyethylene oxide (PEO, with a molecular weight of 100,000) in a mixed solvent composed of 2.0 ml of water and 2.0 ml of ethanol, stir magnetically, and then add the 1.000g (0.0026mol) aluminum nitrate nonahydrate [Al(NO 3 ) 3 9H 2 O], 0.800g (0.0034mol) calcium nitrate tetrahydrate [Ca(NO 3 ) 2 4H 2 O], 0.2g (0.00055mol) of europium chloride hexahydrate (EuCl 3 ·6H 2 0), and after adding 0.4ml of drying control agent (formamide) and 0.4ml of complexing agent (ethylene glycol) and stirring evenly for 60min, add 2.0ml of gel accelerator (PO) and in an ultrasonic instrument (parameter is frequency 53KHz, Output power 100%, water temperature 20 ℃) ​​in ultrasonic for 60 seconds;

[0040] 2), put the uniform and transparent sol liquid obtained in step 1) ...

Embodiment 1-2

[0048] The phase separation inducer polyethylene oxide in step 1) of Example 1-1 was changed from 0.04 g to 0.12 g; the rest were the same as in Example 1-1.

[0049] Observation by scanning electron microscope at low and high magnifications shows that the obtained mayenite still has a coherent macropore structure, but with the increase of the amount of PEO, the diameter of the macropores decreases as ( figure 2 , about 0.7 μm), the porosity is 74%. This is due to the further progress of PEO phase separation. After the fluorescence test, its luminous intensity decreased slightly (such as Figure 4 ).

Embodiment 1-3

[0051] The phase separation inducer polyethylene oxide in step 1) of Example 1-1 was changed from 0.04 g to 0.24 g; the rest were the same as in Example 1-1.

[0052] The low-power and high-power observations of the scanning electron microscope show that the microscopic morphology of the mayenite block has changed to the accumulation of mayenite particles, that is, it does not present a coherent macropore structure such as ( image 3 ). This is because as the amount of PEO increases, the phase separation effect of PEO is further enhanced, and excessive phase separation occurs. After fluorescence test, its luminous intensity further decreased (such as Figure 4 ).

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Abstract

The invention discloses a preparation method of a porous calcite fluorescent material used for preparing a fluorescent sensor. The preparation method comprises the following steps: dissolving phase separation inducer in mixed solvent, magnetic stirring, adding aluminum nitrate nonhydrate, calcium nitrate tetrahydrate as precursor, europium chloride hexahydrate as dopant, adding drying control agent and complexing agent, uniformly stirring, and adding gel promoter for ultrasonic treatment; aging that obtained sol in a sealed container, placing the aged gel in a non-sealed container, and dryingand heat treating the sol to obtain the Eu (europium)-doped porous calcite fluorescent material. Europium Eu3+ is used as rare earth doped ion, the macroporous Eu-doped calcite phosphors prepared by sol-gel associated phase separation can enhance the fluorescence intensity of the phosphors in the visible light band.

Description

technical field [0001] The invention belongs to the field of preparation of metal ion fluorescence sensors, in particular to a preparation method of porous mayenite lead ion fluorescence sensors. Background technique [0002] Due to the need for public safety and environmental protection, scholars are interested in the analytical detection of environmentally harmful ions. With the rapid development of industry worldwide and the excessive use of fresh water resources, the problem of water resources polluted by metal ions has become a very serious global problem today. Emissions of toxic heavy metal ions pose a challenge to plans to maintain a sustainable environment due to the toxicity of metals present in the environment and the threat to human life and ecosystems. Therefore, as a fast and effective detection method, the fluorescence sensor is widely used in the field of ion detection. [0003] Fluorescence sensor is a kind of optical sensor, which uses fluorescence to exp...

Claims

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Application Information

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IPC IPC(8): C09K11/64G01N21/64
CPCC09K11/7734G01N21/643
Inventor 郭兴忠王睿杨辉
Owner ZHEJIANG UNIV
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