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Method for preparing europium-doped calcium titanate CaTiO3: Eu3 plus fluorescent powder by solvent-thermal method

A solvothermal method and fluorescent powder technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of low luminous efficiency and achieve high chemical stability, small size, and good dispersion

Inactive Publication Date: 2010-12-22
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the luminous efficiency of the currently developed red phosphors for white LEDs is low and cannot meet the requirements, we need to find new and efficient red phosphors for white LEDs

Method used

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  • Method for preparing europium-doped calcium titanate CaTiO3: Eu3 plus fluorescent powder by solvent-thermal method
  • Method for preparing europium-doped calcium titanate CaTiO3: Eu3 plus fluorescent powder by solvent-thermal method
  • Method for preparing europium-doped calcium titanate CaTiO3: Eu3 plus fluorescent powder by solvent-thermal method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Measure 1.716ml of n-tetrabutyl titanate, dissolve it in 10ml of absolute ethanol, add 50ml of 0.5mol / L ammonia solution ammonia water dropwise to make it all react as titanium hydroxide precipitate, and wash with water three times to remove excess ammonia ions. Then add 25ml of ethanolamine, 25ml of ethylenediamine, 5ml of deionized water, 2.6163g of calcium acetate, 0.05069g of europium nitrate, 3.3g of sodium hydroxide, and 1ml of polyethylene glycol, and stir for 30min at a rotation speed of 350r / min, so that All solutes are completely dispersed. The above solution and precipitate were poured into a reaction kettle with a volume of 80ml, then put into an oven, kept at 180°C for 14 hours, and then cooled to room temperature. After the reaction, the product was collected by centrifugation, washed with deionized water and hydrochloric acid with pH = 2-3, and then dried at 60°C for 24 hours to obtain CaTiO 3 :Eu 3+ Phosphor.

[0022] figure 1 It is the X-ray diffr...

Embodiment 2

[0026] Measure 1.716ml of n-tetrabutyl titanate, dissolve it in 20ml of absolute ethanol, add 25ml of 1mol / L ammonia water dropwise to make it all react into titanium hydroxide precipitation, and wash with water three times to remove excess ammonia ions. Add 20ml of ethanolamine, 20ml of ethylenediamine, 3.5ml of deionized water, 2.5370g of calcium acetate, 0.2028g of europium nitrate, 3.8g of sodium hydroxide, and 1.4ml of polyethylene glycol, and stir for 25min at a rotation speed of 400r / min. , so that all solutes are completely dispersed. The above solution and precipitate were poured into a reaction kettle with a volume of 80ml, then put into an oven, kept at 200°C for 12 hours, and then cooled to room temperature. After the reaction, the product was collected by centrifugation, and the product was washed with deionized water and hydrochloric acid with a pH of 2 to 3, and then dried at 60°C for 28 hours to obtain CaTiO 3 :Eu 3+ Phosphor.

[0027] The X-ray test results...

Embodiment 3

[0031]Measure 1.716ml of n-tetrabutyl titanate, dissolve it in 30ml of absolute ethanol, add 8ml of 3mol / L ammonia water dropwise to make it all react to precipitate titanium hydroxide, and wash with water three times to remove excess ammonia ions. Then add 15ml of ethanolamine, 15ml of ethylenediamine, 3ml of deionized water, 2.3780g of calcium acetate, 0.5069g of europium nitrate, 4.7g of sodium hydroxide, and 1ml of polyethylene glycol, and stir for 20min at a rotation speed of 500r / min, so that All solutes are completely dispersed. The above solution and precipitate were poured into a reaction kettle with a volume of 80ml, then put into an oven, kept at 220°C for 10 hours, and then cooled to room temperature. After the reaction, the product was collected by centrifugation, and the product was washed with deionized water and hydrochloric acid with pH = 2-3, and then dried at 80°C for 20 hours to obtain CaTiO 3 :Eu 3+ Phosphor.

[0032] The X-ray test results show that th...

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Abstract

The invention relates to a method for preparing europium-doped calcium titanate CaTiO3: Eu3 plus fluorescent powder by the solvent-thermal method, which comprises the following steps: (1) dissolving tetrabutyl titanate in anhydrous ethanol at room temperature, simultaneously carrying out magnetic stirring, dripping ammonia solution into the mixed solution, obtaining white precipitate, centrifugating and washing a product; (2) mixing and stirring ethylenediamine, ethanolamine, deionized water, calcium acetate, europium nitrate, sodium hydroxide and polyethylene glycol, pouring the solution andthe product into a reaction kettle, increasing the temperature to 180-220 DEG C and carrying out reaction for 8-12h; and (3) collecting the reaction product in a centrifugation way after the reactionis finished, respectively washing the product with acid and deionized water, drying, and obtaining the CaTiO3: Eu3 plus fluorescent powder. The preparation method has simple process, low synthesis temperature and is applicable to industrial production, and the prepared fluorescent powder has the advantages of good dispersivity, high chemical stability, high crystal phase purity, small size and hollow pipe-like structure.

Description

technical field [0001] The present invention belongs to CaTiO 3 The field of preparation, in particular to a solvothermal preparation of europium-doped calcium titanate CaTiO 3 :Eu 3+ phosphor method. Background technique [0002] As the core material of white LED, phosphor powder has always been a hot research topic in the field of lighting, and the performance of phosphor powder also directly affects the development of white light LED. There are many ways to prepare phosphors. At present, the main synthetic methods are: high-temperature solid-state reaction method, sol-gel method, homogeneous co-precipitation method, low-temperature combustion synthesis method, hydrothermal synthesis method, microwave radiation synthesis method, polymer network Gel method, surface diffusion method, etc. In 1996, Japan's Nichia Chemical Corporation first developed a high-efficiency white light source by combining yellow light series yttrium aluminum garnet (YAG) phosphors with blue LEDs...

Claims

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Application Information

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IPC IPC(8): C09K11/67
Inventor 王宏志孙壮李耀刚张青红
Owner DONGHUA UNIV
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