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Preparation method of praseodymium-doped calcium titanate luminescent powder

A technology of calcium titanate and luminescent powder, which is applied in the direction of luminescent materials, chemical instruments and methods, etc., can solve the problems that it is difficult to obtain regular morphology, the particle size of the product is difficult to control, and the particles are easy to agglomerate and have irregular morphology. The effect of long synthesis time, simple operation and high sintering temperature

Inactive Publication Date: 2012-08-08
HARBIN ENG UNIV
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  • 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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  • Preparation method of praseodymium-doped calcium titanate luminescent powder
  • Preparation method of praseodymium-doped calcium titanate luminescent powder
  • Preparation method of praseodymium-doped calcium titanate luminescent powder

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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 0.1gCaCO 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 Spray Dryer 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 0.1gCaCO 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 Spray Dryer 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 a preparation method of praseodymium-doped calcium titanate luminescent powder. The method comprises: under room temperature, and according to Pr<3+> / Ca<2+> in a mole ratio of 0.005 / 1, weighing certain amounts of CaCO3 and Pr6O11 solids which are dissolved in dilute nitric acid, conducting heating to expel excess acid, and when the pH value of the solution reaches 2-3, reheating the solution to a melt state; leaving the solution to cool to room temperature, then respectively adding stoichiometric titanium tetrabutoxide and 20mL of a water-ethanol solution, then adding a certain amount of citric acid as a complexing agent, adding polyethylene glycol, and carrying out stirring for 2h, thus obtaining a transparent sol precursor; subjecting the obtained precursor solution to spray drying so as to obtain precursor powder; putting the precursor into a programmed heating furnace, and heating the precursor to a temperature of 600DEG C-1000DEG C, then maintaining the temperature constant for 3h, thus obtaining CaTiO3:Pr<3+> fluorescent powder. The praseodymium-doped calcium titanate fluorescent powder prepared by the method of the invention has good crystallization degree and high purity, and is a CaTiO3 pure phase in a perovskite structure.

Description

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. Background technique [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. As the p...

Claims

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Application Information

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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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