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Preparation method of Ca1-XSi2O2N2:EuX fluorescent fiber membrane with hollow structure

A technology for fluorescent fibers and fiber membranes, which is used in fiber processing, heating/cooling fabrics, textiles, and papermaking, etc., and can solve the problems of inability to continuously prepare a large number of hollow fibers, limited preparation methods, and complex spinning parameters.

Inactive Publication Date: 2015-01-14
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the characteristics of hollow fibers, the preparation methods are very limited, such as traditional hydrothermal method, chemical vapor deposition method, template method, etc. (SONG Peng et al.Sensors and Actuators B:Chemical,2010,147(1):248-254) It is impossible to continuously prepare a large number of hollow fibers
In recent years, coaxial electrospinning technology is often used to synthesize core-shell structure materials and hollow nanomaterials, but the selection of inner and outer layer solvents is more difficult, and the setting of spinning parameters is also more complicated, which greatly limits the synthesis range. (ZHAN Si-Hui et al. Journal of Colloid and Interface Science, 2007, 308(1): 265-270)

Method used

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  • Preparation method of Ca1-XSi2O2N2:EuX fluorescent fiber membrane with hollow structure
  • Preparation method of Ca1-XSi2O2N2:EuX fluorescent fiber membrane with hollow structure
  • Preparation method of Ca1-XSi2O2N2:EuX fluorescent fiber membrane with hollow structure

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 1mL of ultrapure water, 18mL of absolute ethanol and 1mL of DMF and mix; dissolve 0.0196g of europium nitrate and 0.3978g of calcium nitrate in the mixed solvent, and then add 0.69mL of TEOS. After continuous stirring for 30 min, slowly add 0.9 g PVP (molecular weight 50,000) and 2.4 g PVP (molecular weight 1,300,000) under high-speed stirring, and continue stirring for 6 h, the solution is clear and transparent.

[0030] The obtained precursor solution was subjected to electrospinning: at room temperature, the humidity was controlled at 30%, the spinning voltage was set to 6kv, the propulsion speed of the propulsion pump was 0.2mL / h, and the receiving distance was 10cm.

[0031] The as-spun fibers obtained above were calcined in an air atmosphere with a heating rate of 0.8°C / min and a calcining temperature of 500°C. After 4 hours of heat preservation, the temperature was naturally lowered to obtain a Ca-Si-O-Eu fiber membrane with a hollow structure.

[0032] The ...

Embodiment 2

[0034]Mix 1.5mL ultrapure water, 17mL absolute ethanol and 1.5mL DMF; dissolve 0.0429g europium nitrate and 0.6852g calcium nitrate in the mixed solvent, and then add 1.08mL TEOS. After stirring continuously for 30 min, slowly add 1.1 g PVP (molecular weight 50,000) and 2 g PVP (molecular weight 1,300,000) under high-speed stirring, and continue stirring for 6 h, the solution is clear and transparent.

[0035] The obtained precursor solution was subjected to electrospinning: at room temperature, the humidity was controlled at 20%, the spinning voltage was set to 8kv, the propulsion speed of the propulsion pump was 0.8mL / h, and the receiving distance was 14cm.

[0036] The as-spun fibers obtained above were calcined in an air atmosphere with a heating rate of 1°C / min and a calcination temperature of 550°C. After holding for 3 hours, the temperature was naturally lowered to obtain a Ca-Si-O-Eu fiber membrane with a hollow structure.

[0037] Transfer the calcined fiber membrane ...

Embodiment 3

[0039] Mix 2mL of ultrapure water, 16mL of absolute ethanol and 2mL of DMF; dissolve 0.1018g of europium nitrate and 0.9847g of calcium nitrate in the mixed solvent, and then add 1.45mL of TEOS. After continuous stirring for 30 min, 1.3 g of PVP (molecular weight 50,000) and 1.7 g of PVP (molecular weight 1,300,000) were slowly added under high-speed stirring, and stirring was continued for 6 h, and the solution was clear and transparent.

[0040] The obtained precursor solution was subjected to electrospinning: at room temperature, the humidity was controlled at 10%, the spinning voltage was set to 12kv, the propulsion speed of the propulsion pump was 1.5mL / h, and the receiving distance was 18cm.

[0041] The as-spun fibers obtained above were calcined in an air atmosphere with a heating rate of 1.5°C / min and a calcination temperature of 600°C. After holding for 2 hours, the temperature was naturally lowered to obtain a Ca-Si-O-Eu fiber membrane with a hollow structure.

[00...

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Abstract

The invention relates to a preparation method of a Ca1-XSi2O2N2:EuX fluorescent fiber membrane with a hollow structure. In the method, europium nitrate, calcium nitrate and tetraethyl orthosilicate (TEOS) are taken as raw materials. The method comprises the steps of feeding the raw materials into a solvent; evenly mixing to obtain a evenly mixed solution, feeding a certain amount of polyvinylpyrrolidone into the evenly mixed solution, and stirring to obtain a transparent spinning solution; carrying out electrostatic spinning to obtain an original fiber membrane; calcining the obtained fiber membrane in an air atmosphere to obtain a Ca-Si-O-Eu fiber membrane with the hollow structure; nitriding the Ca-Si-O-Eu fiber membrane in an ammonia atmosphere to obtain the Ca1-XSi2O2N2:EuX fluorescent fiber membrane with the hollow structure. The Ca1-XSi2O2N2:EuX fluorescent fiber membrane is a pure inorganic fluorescent fiber membrane, and is suitable for remote encapsulation of a high-power white light LED. Due to the design of the hollow structure, a relatively large quantity of gas-solid reaction interfaces are provided for the nitridation of the fluorescent membrane, so that the energy consumption in reaction is reduced.

Description

technical field [0001] The invention belongs to the field of preparation of fluorescent materials, in particular to a Ca 1-x Si 2 o 2 N 2 :Eu x Preparation method of fluorescent fiber membrane. Background technique [0002] YAG:Ce phosphor is the earliest application and is currently the most important LED phosphor. After decades of hard exploration, the luminous efficiency of white LEDs encapsulated with YAG:Ce phosphors has been greatly improved through component fine-tuning, structural optimization, and gradual improvement of the preparation process. However, YAG:Ce phosphor has been unable to solve some problems, including poor thermal stability, low color rendering index, and high color temperature. For this reason, people have been actively searching for a new luminescent material for LEDs. Rare earth-doped nitride crystal materials have attracted widespread attention in recent years due to their low excitation energy, wide emission spectrum, and high color rende...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D06M11/60D04H1/4382D04H1/728D06C7/00
Inventor 王宏志崔博李耀刚张青红
Owner DONGHUA UNIV