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Macroporous mayenite fluorescent material and preparation method thereof

A macroporous mayenite and fluorescent material technology, applied in luminescent materials, chemical instruments and methods, etc., can solve the problem of inability to obtain co-continuous hole structure and morphology, and achieve low cost, enhanced fluorescence intensity, and good luminous intensity. Effect

Active Publication Date: 2018-07-27
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the prior art, the co-precipitation method is used to prepare mayenite doped with rare earth ions; this technology still has the technical defect that the co-continuous pore structure and morphology cannot be obtained

Method used

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  • Macroporous mayenite fluorescent material and preparation method thereof
  • Macroporous mayenite fluorescent material and preparation method thereof
  • Macroporous mayenite fluorescent material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1-1

[0030] Embodiment 1-1, a method for preparing a macroporous mayenite block, the following steps are performed in sequence:

[0031] 1), at room temperature, dissolve 0.04 g of the phase separation inducer polyethylene oxide (PEO, with a molecular weight of 300,000) in a mixed solvent composed of 2.0 ml of water and 4.0 ml of ethanol (alcohol), stir magnetically, and then add as 2.000g aluminum chloride hexahydrate (AlCl 3 ·6H 2 O), 1.044g calcium chloride dihydrate (CaCl 2 2H 2 O), 1 g of terbium chloride nonahydrate (TbCl 3 9H 2 0), and adding 0.4ml of drying control agent (formamide), 0.3ml of chelating agent (ethylene glycol) and stirring for 60min, after stirring evenly, add 1.5ml of gel accelerator (concentration is 25% ammonia water) and ultrasonic for 60 seconds;

[0032] 2), put the uniform and transparent sol liquid obtained in step 1) in an airtight container, gel and age in an oven at 70°C for 24 hours;

[0033] 3) Place the aged white homogeneous gel obtained i...

Embodiment 1-2

[0037] Change the phase separation inducer in step 1) of Example 1-1---polyethylene oxide from 0.04g to 0.08g; the rest are the same as in Example 1-1.

[0038] 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 0.6 μm), the porosity is 72%. 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

[0040] Change the phase separation inducer in step 1) of Example 1-1---polyethylene oxide from 0.04g to 0.12g; the rest are the same as in Example 1-1.

[0041] 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 ), the porosity is 67%. 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 macroporous mayenite fluorescent material. The method comprises the following steps of (1) at room temperature, dissolving a phase separation inducerinto a mixed solvent; after the magnetic stirring, adding aluminum chloride hexahydrate and calcium chloride dihydrate used as precursors; adding terbium chloride nonahydrate, drying control agents and chelating agents; after the uniform stirring, adding gel accelerators; performing ultrasonic treatment for 50 to 70 seconds; (2) putting sol liquid obtained in the step (1) into a sealed container;performing gelling at 50 to 70 DEG C; performing aging for 24+ / - 2h; (3) putting the aged gel obtained in the step (2) into a container; performing drying for 3 to 4d at 50 to 70 DEG C; then, performing heat treatment for 2 to 3h at 900 to 1300 DEG C to obtain the macroporous mayenite fluorescent material. By using the method, the rare earth element doping mayenite fluorescent material with controllable pore dimension, higher porosity and continuous macroporous structures can be obtained.

Description

technical field [0001] The invention belongs to the field of preparation of macroporous mayenite fluorescent material, in particular to a preparation method of mayenite fluorescent material with co-continuous macropore structure. Background technique [0002] In recent years, the research on rare earth elements and rare earth-doped luminescent materials has been developed rapidly. However, rare earths are expensive, so how to effectively reduce the cost of materials and improve their luminous efficiency has become the focus of researchers. Tb 3+ It can emit green fluorescence, has high luminous intensity, high quantum efficiency, and high sensitivity to local environments, and is often used to study the basic physical properties of materials. Therefore Tb 3+ As a typical rare earth dopant ion, it has been widely valued and studied in various fields. Tb 3+ excited state of 5 D. 4 energy level to 7 f 5 The transition emission line of the energy level is in the green s...

Claims

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Application Information

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IPC IPC(8): C09K11/64
CPCC09K11/7749
Inventor 郭兴忠王睿杨辉
Owner ZHEJIANG UNIV
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