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Preparation of doped calcium titanate (CaTiO3: Eu3+) fluorescent powder

A technology of fluorescent powder and calcium titanate, applied in chemical instruments and methods, titanium compounds, luminescent materials, etc., can solve the problems of low luminous efficiency and achieve high chemical stability, simple process, and high purity

Inactive Publication Date: 2009-03-04
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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  • Preparation of doped calcium titanate (CaTiO3: Eu3+) fluorescent powder
  • Preparation of doped calcium titanate (CaTiO3: Eu3+) fluorescent powder
  • Preparation of doped calcium titanate (CaTiO3: Eu3+) fluorescent powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Weigh 9.912g of calcium nitrate tetrahydrate and 3.568g of europium nitrate hexahydrate, add them into a beaker, and then add 100ml of absolute ethanol; weigh 17.000g of n-tetrabutyl titanate, add them into a beaker, and then add 100ml of absolute ethanol. Stir the above two mixtures for 30 minutes to form a solution; add the mixed ethanol solution of the above-mentioned europium salt and calcium salt to the n-tetrabutyl titanate ethanol solution, and stir for 8 minutes at the same time to form a sol; place the sol at a temperature of 5°C for 10 minutes, To obtain a wet gel, put the wet gel into an oven at 50°C and dry it for 15 hours to obtain a dry gel; finally, calcinate the obtained precursor at 1400°C for 2 hours to obtain europium-doped calcium titanate CaTiO 3 :Eu 3+ Phosphor.

[0018] figure 1 It is the X-ray diffraction pattern of the fluorescent powder synthesized in this embodiment, it can be seen that the diffraction peaks are consistent with the diffracti...

Embodiment 2

[0022] Weigh 9.676g of calcium nitrate tetrahydrate and 4.014g of europium nitrate hexahydrate, add them into a beaker, and then add 50ml of absolute ethanol; weigh 17.000g of n-tetrabutyl titanate, add them into a beaker, and then add 50ml of absolute ethanol. Stir the above two mixtures for 20 minutes to form a solution; add the mixed ethanol solution of the above-mentioned europium salt and calcium salt to the n-tetrabutyl titanate ethanol solution, and stir for 10 minutes at the same time to form a sol; place the sol at 10°C for 20 minutes, To obtain a wet gel, put the wet gel into an oven at 120°C and dry it for 18 hours to obtain a dry gel; finally, calcinate the obtained precursor at 1300°C for 4 hours to obtain europium-doped calcium titanate CaTiO 3 :Eu 3+ Phosphor.

[0023] The X-ray test results show that the diffraction peaks are consistent with the diffraction peaks of calcium titanate in the cubic phase, and no diffraction peaks belonging to other oxides of calc...

Embodiment 3

[0027] Weigh 9.440g of calcium nitrate tetrahydrate and 4.460g of europium nitrate hexahydrate, add them into a beaker, and then add 60ml of absolute ethanol; weigh 17.000g of n-tetrabutyl titanate, add them into a beaker, and then add 60ml of absolute ethanol. Stir the above two mixtures for 25 minutes to form a solution; add the mixed ethanol solution of the above-mentioned europium salt and calcium salt to the n-tetrabutyl titanate ethanol solution, and stir for 12 minutes at the same time to form a sol; place the sol at 20°C for 30 minutes, To obtain a wet gel, put the wet gel into an oven at 80°C and dry it for 20 hours to obtain a dry gel; finally, calcinate the obtained precursor at 1400°C for 6 hours to obtain europium-doped calcium titanate CaTiO 3 :Eu 3+ Phosphor.

[0028] The X-ray test results show that the diffraction peaks are consistent with the diffraction peaks of calcium titanate in the cubic phase, and no diffraction peaks belonging to other oxides of calci...

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Abstract

The invention relates to a preparation method of Eu-doping calcium titanate CaTiO3:Eu<3+> fluorescent powders, which comprises the steps as follows: a soluble europium salt, a calcium salt and Ti(OC4H9)4 are weighed according to the mole ratio that is 1:49:50 to 1:4:5 among Eu<3plus>, Ca<2plus> and Ti<4plus>, and are respectively dissolved in absolute ethyl alcohol, and the confected solution is stirred for ample dissolution; (2) a mixed ethanol solution of the europium salt and the calcium salt is added in an ethanol solution of Ti(OC4H9)4, and a sol is obtained through stirring; (3) the sol is placed at the temperature ranging from 0 to 50 DEG C to obtain a wet gel which is put in a baking box for drying; (4) the dried gel is milled into powders, the obtained powders are calcined for 2 to 8 hours to obtain the CaTiO3:Eu<3plus> fluorescent powders. In the preparation method, the prepared CaTiO3:Eu<3plus> fluorescent powders have high chemical durability, small grain size, pure crystalling phase and low calcination temperature; the preparation method has simple technology, and is easy for industrialized production.

Description

technical field [0001] The invention belongs to the field of phosphor preparation, in particular to a europium-doped calcium titanate (CaTiO 3 :Eu 3+ ) The preparation method of fluorescent powder. 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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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/00C09K11/78
Inventor 王宏志付嘉鹏李耀刚张青红
Owner DONGHUA UNIV
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