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Preparation method of one-dimensional SiO<2>: Eu<3+> fiber luminescent material with dimension controllable

A technology of luminescent materials and fibers, applied in the directions of luminescent materials, chemical characteristics of fibers, chemical instruments and methods, etc., can solve the problems of long preparation period, difficult morphology control, poor reproducibility, etc.

Active Publication Date: 2015-11-25
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] However, the above method has a long preparation period, requires high temperature and high pressure and other conditions, and has low yield, difficult shape control, poor reproducibility, and difficult mass production.

Method used

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  • Preparation method of one-dimensional SiO&lt;2&gt;: Eu&lt;3+&gt; fiber luminescent material with dimension controllable
  • Preparation method of one-dimensional SiO&lt;2&gt;: Eu&lt;3+&gt; fiber luminescent material with dimension controllable
  • Preparation method of one-dimensional SiO&lt;2&gt;: Eu&lt;3+&gt; fiber luminescent material with dimension controllable

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Mix 1.5gTEOS, 2mL ethanol, 3mL acetic acid, and 2mL water evenly, and stir for 30min.

[0025] (2) Add 2.0g of PVP and stir for more than 1 hour to completely dissolve the PVP.

[0026] (3) Let the above solution stand still so that there are no air bubbles in the solution. This is the electrospinning solution. Measure 2 mL with a syringe for later use.

[0027] (4) Turn on the electrospinning machine and adjust various parameters. The flow rate is 0.2mm / min, the receiving distance is 20cm, and the voltage is 20KV (cathode voltage-4KV, anode voltage 16KV).

[0028] (5) Turn on the voltage, connect one end to the receiver aluminum foil (cathode) and the other end to the needle (anode) of the syringe used for electrospinning to perform electrospinning.

[0029] (6) After spinning, the sample is placed in a muffle furnace and calcined at 600°C for 2 hours to obtain undoped rare earth SiO 2 fiber.

Embodiment 2

[0031] Except for the situation described below, the rest are the same as in Example 1, and 2mLH 2 O was replaced by adding 1.15mLH 2 O and 0.85mLEu(NO 3 ) 3 (1M) solution.

[0032] figure 1 The SiO prepared when the amount of europium nitrate is 0mL and 0.85mL is given in 2 XRD comparison chart of fibers. From the figure, we found that the addition of europium ions did not change the crystal form of the fiber, but still showed the characteristic peaks of amorphous silica, and the intensity decreased after doping, indicating that Eu 3+ Successful doping into the silica matrix reduces the symmetry of the three-dimensional network structure of silica.

[0033] figure 2 SiO obtained when the volume V (water + europium nitrate) given in (a) is 2.0 mL 2 : Eu 3+ SEM of the fiber, it can be found from the figure that the prepared SiO 2 :Eu 3+ The shape of the fiber is uniform, and the diameter is about 510nm.

Embodiment 3

[0035] Except for the situation described below, the rest are the same as in Example 1, and 2mLH 2 O was replaced by adding 0.65mLH 2 O and 0.85mLEu(NO 3 ) 3 (1mol / L) solution.

[0036] figure 2 The SiO obtained when the volume V (water + europium nitrate) is 1.5 mL is given in (b). 2 : Eu 3+ SEM of the fiber, it can be found from the figure that the prepared SiO 2 : Eu 3+ The morphology of the fibers is uniform, and the diameter is about 917nm.

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Abstract

The invention provides a preparation method of a one-dimensional SiO<2> luminescent material with europium ions doped and the dimension controllable and belongs to the field of inorganic luminescent materials. According to the method, an electrostatic spinning method is adopted, and the high-temperature calcination after-treatment is combined, one-dimensional SiO<2> fibers with europium doped are prepared out, and the method is characterized in that the fibers are synthesized by one step, the yield is high, the shape and appearance are uniform, Eu<3+> ions exist in the fibers stably, the washing process is not required, and impurity components can be completely removed through the high-temperature calcination in air, thereby pure and homogeneous SiO<2> : Eu<3+> fibers are obtained. Under the ultraviolet excitation, the fibers present obvious transition from <5>D<0> to <7>F<2> of the Eu<3+> ions, and the fibers are in bright red under the illumination of an ultraviolet lamp. The preparation method is great in operability and good in reproducibility, an obtained product is stable in performance and excellent in light-emitting, and the possibility of applying one-dimensional fluorescent materials with rare-earth ions doped to preparation of opto devices and optical sensors in future is provided.

Description

technical field [0001] The invention belongs to the technical field of inorganic luminescent materials, in particular to one-dimensional SiO with controllable size doped with europium ions 2 Preparation method of luminescent material. Background technique [0002] In recent years, one-dimensional nanomaterials (such as tubes, rods, and fibers) have attracted great attention due to their unique physical and chemical properties as well as a wide range of applications. In particular, the three-dimensional network structure of one-dimensional silica materials determines its good thermal stability, chemical stability and superior mechanical properties, and has been widely used in biology, electricity and optics and other fields. At the same time, the photoluminescent properties of silicon dioxide itself also determine that it is an excellent rare earth ion doped host material. [0003] Due to the unique 4f electron layer structure of lanthanide doped materials, the photolumines...

Claims

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Application Information

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IPC IPC(8): D01F9/08D01F1/10C09K11/59
Inventor 邹海峰陈杰盛野郑克岩宋艳华
Owner JILIN UNIV
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