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Praseodymium-doped calcium titanate luminescent powder and preparation method thereof

A technology of calcium titanate and luminescent powder, which is applied in the direction of luminescent materials, chemical instruments and methods, and can solve the problems of long synthesis time, high sintering temperature, and low sintering temperature

Inactive Publication Date: 2009-09-30
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Synthesis of CaTiO by traditional high-temperature solid-state method 3 There are shortcomings such as high sintering temperature, long synthesis time, and irregular morphology of particles (S.Y.Yin, D.H.Chen, W.J.Tang, Mater.Sci.Eng.B.136, 193(2007); B.Jancar, M.Valant , D. Suvorov, Chem. Mater. 16, 1075 (2004))
Sol-Gel Synthesis of CaTiO 3 The operation is simple and the sintering temperature is low, but it is also difficult to control the particle size of the product so that it is difficult to obtain a product with a regular shape (E. Pinel, P Boutinaud, J

Method used

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  • Praseodymium-doped calcium titanate luminescent powder and preparation method thereof
  • Praseodymium-doped calcium titanate luminescent powder and preparation method thereof
  • Praseodymium-doped calcium titanate luminescent powder and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0022] The starting material used was calcium carbonate CaCO 3 (analytical pure), tetrabutyl titanate Ti(OC 4 h 9 ) 4 (analytical pure), praseodymium oxide Pr 6 o 11 (99.99%), concentrated nitric acid HNO 3 (analytical pure), citric acid (analytical pure), polyethylene glycol (analytical pure). CaTiO 3 :Pr 3+ In phosphor, Pr 3+ The doping concentration is controlled at about 0.5% Ca 2+ atomic fraction.

[0023] Weigh 0.1g (1mmol) CaCO 3 , 0.009g (0.005mmol) Pr 6 o 11 Dissolve in dilute nitric acid, heat and stir to drive out the acid until the pH value of the solution is 2-3, then heat until it melts; after cooling to room temperature, add 0.34g (1mmol) n-butyl titanate, water-ethanol solution 20mL (the volume ratio of water and ethanol is 1:9), then add 0.42g (2mmol) citric acid (ratio to metal ions: 2:1) as a complexing agent, and stir for 2 hours to obtain a homogeneous transparent sol precursor. The resulting precursor solution was introduced into a spray dry...

Embodiment 2

[0025] Weigh 0.1g CaCO 3 , 0.009gPr 6 o 11Dissolve in dilute nitric acid, heat and stir to drive out the acid until the pH value of the solution is 2-3, then heat until it melts; after cooling to room temperature, add 0.34g of n-butyl titanate, 20mL of water-ethanol solution (water The volume ratio with ethanol is 1:9), then add 0.42g citric acid (ratio with metal ion is 2:1) as complexing agent, add 0.4g (0.002mol / L) polyethylene glycol, stir for 2 hours That is, a homogeneous transparent sol precursor is obtained. The resulting precursor solution was introduced into a spray dryer (BüCHI Mini SprayDryer B-191) and spray-dried to obtain a precursor powder sample. Put the precursor into a temperature-programmed furnace, raise the temperature to 800 °C at a rate of 1 °C / min, and then keep the temperature at this temperature for 3 hours to obtain CaTiO 3 :Pr 3+ Phosphor. In this implementation, a sample with a PEG concentration of 0.002 mol / L and a calcination temperature o...

Embodiment 3

[0027] Weigh 0.1g CaCO 3 , 0.009g Pr 6 o 11 Dissolve in dilute nitric acid, heat and stir to drive out the acid until the pH value of the solution is 2-3, then heat until it melts; after cooling to room temperature, add 0.34g of n-butyl titanate, 20mL of water-ethanol solution (water The volume ratio with ethanol is 1:9), then add 0.42g citric acid (ratio with metal ion is 2:1) as complexing agent, add 0.8g (0.004mol / L) polyethylene glycol, stir for 2 hours That is, a homogeneous transparent sol precursor is obtained. The resulting precursor solution was introduced into a spray dryer (BüCHI Mini SprayDryer B-191) and spray-dried to obtain a precursor powder sample. Put the precursor into a temperature-programmed furnace, raise the temperature to 800 °C at a rate of 1 °C / min, and then keep the temperature at this temperature for 3 hours to obtain CaTiO 3 :Pr 3+ Phosphor. In this implementation, a sample with a PEG concentration of 0.004 mol / L and a calcination temperature...

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Abstract

The invention provides praseodymium-doped calcium titanate luminescent powder and a preparation method thereof. The preparation method comprises the following steps: at room temperature, weighing a certain amount of CaCO3 and Pr6O11 solid according to a molar ratio of Pr<3+> / Ca<2+> of 0.005 / 1, dissolving the solid in dilute nitric acid, heating and stirring the solution to remove excessive acid, and heating the solution to a melting state after the pH value of the solution reaches 2 to 3; after the solution is cooled to room temperature, adding 20 milliliters of tetrabutyl titanate and 20 milliliters of water-ethanol solution into the solution according to a stoichiometric proportion, then adding a certain amount of citric acid as complexing agent into the solution, adding polyethylene glycol into the solution, and stirring the solution for 2 hours to obtain an even transparent sol precursor; spraying and drying the obtained precursor solution to obtain precursor powder; and putting the precursor powder into a programmed temperature rising furnace, heating the precursor powder to between 600 and 1,000 DEG C, and then keeping the precursor powder for 3 hours at a constant temperature to obtain CaTiO3:Pr<3+> luminescent powder. The praseodymium-doped calcium titanate luminescent powder prepared by the method has good crystallization degree and high purity, and is a CaTiO3 pure phase of a perovskite structure.

Description

(1) Technical field [0001] The invention relates to a luminescent powder, specifically a praseodymium-doped calcium titanate luminescent powder. The invention also relates to a preparation method of the praseodymium-doped calcium titanate luminescent powder. (2) Background technology [0002] CaTiO 3 It has a perovskite structure and has certain electrical conductivity. CaTiO 3 It has excellent performance in low-voltage behavior and is a potential low-voltage cathodoluminescence host material. CaTiO 3 :Pr 3+ Phosphor powder is a low-voltage cathodoluminescent material with excellent red light emission, and has potential application prospects in field emission devices. In addition, the luminescent powder coating screen with monodisperse non-agglomeration, spherical shape, and small size distribution (about 0.5-2 microns in diameter) has the characteristics of high packing density, low light scattering, high brightness, and high definition. aroused widespread concern. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/67
Inventor 杨飘萍盖世丽王文鑫牛娜贺飞
Owner HARBIN ENG UNIV
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