Short rod-shaped TbPO4 powder with excellent luminescence property and preparation method thereof

A short rod-shaped technology with luminescent properties, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of low cost, low temperature development, etc., and achieve good repeatability, short preparation cycle, and high crystallinity.

Active Publication Date: 2014-08-13
SHAANXI UNIV OF SCI & TECH
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the above methods provide some ways to synthesize rare-earth phosphate nanomaterials with good morphology, it is of great significance to develop low-temperature, low-cost, and simple methods to synthesize rare-earth phosphates with nano / micro-level structures.
[0003] So far, there are no literature and patent reports on the synthesis of short rod-shaped TbPO with good luminescent properties under low-temperature hydrothermal conditions using water as a solvent without adding any surfactants, templates, and dispersants. 4

Method used

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  • Short rod-shaped TbPO4 powder with excellent luminescence property and preparation method thereof
  • Short rod-shaped TbPO4 powder with excellent luminescence property and preparation method thereof
  • Short rod-shaped TbPO4 powder with excellent luminescence property and preparation method thereof

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preparation example Construction

[0023] A short rod-shaped TbPO with good luminescent properties 4 The preparation method of powder comprises the following steps:

[0024] Step 1): Add Tb(NO 3 ) 3 ·6H 2 O was dissolved in deionized water, stirred for 5-10min to form a terbium salt solution with a concentration of 0.09mol / L; 4 h 2 PO 4 The solution is evaporated to recrystallization, and the crystals are dissolved in deionized water to form NH with a concentration of 1.8mol / L 4 h 2 PO 4 solution, the NH 4 h 2 PO 4 solution, with terbium salt solution according to PO 4 3- :Tb 3+ = 40:1 molar ratio mixed, and when mixed, terbium salt solution was added dropwise to NH 4 h 2 PO 4 Stir in the solution for 10-20min, then use ammonia water and dilute HNO 3 Adjust the pH of the precursor solution to pH=3 to obtain the precursor solution;

[0025] Step 2): Transfer the precursor solution obtained in step 1) to a reactor lined with polytetrafluoroethylene, and the volume filling degree of the reactor i...

Embodiment 1

[0030] Step 1: Add 0.9mmol(Tb(NO 3 ) 3 ·6H 2 O) was dissolved in deionized water, stirred for 5min, and 36mmolNH 4 h 2 PO 4 Dissolve in deionized water, heat the solution until recrystallization, then add deionized water, terbium salt and NH with a concentration of 1.8mol / L 4 h 2 PO 4 According to PO 4 3- :Tb 3+ = 40:1 molar ratio mixing, terbium salt solution was added dropwise to NH 4 h 2 PO 4 In the solution, stir for 10 minutes to form a precursor solution, using ammonia water and dilute HNO 3 Adjust the pH of the precursor solution to pH=3;

[0031] Step 2: Transfer the precursor solution to a reactor lined with polytetrafluoroethylene, and the volume filling degree of the reactor is 80%;

[0032] Step 3: Using low-temperature hydrothermal method, set the hydrothermal reaction temperature to 100°C and the holding time to 8h, take out the white precipitate formed after the reaction, centrifuge, wash with deionized water three times, and dry in a 70°C constant t...

Embodiment 2

[0034] Step 1: Add 0.9mmol(Tb(NO 3 ) 3 ·6H 2 O) be dissolved in deionized water, stir 8min, 36mmolNH 4 h 2 PO 4 Dissolve in deionized water, heat the solution until recrystallization, then add deionized water, terbium salt and NH 4 h 2 PO 4 According to PO 4 3- :Tb 3+ = 40:1 molar ratio mixing, terbium salt solution was added dropwise to NH 4 h 2 PO 4 solution, stirred for 15 minutes to form a precursor, using ammonia and dilute HNO 3 Adjust the pH of the precursor solution to pH=3;

[0035] Step 2: Transfer the precursor solution to a reactor lined with polytetrafluoroethylene, and the volume filling degree of the reactor is 60%;

[0036] Step 3: Using low-temperature hydrothermal method, set the hydrothermal reaction temperature to 100°C and the holding time to 8h, take out the white precipitate formed after the reaction, centrifuge it, wash it with deionized water three times, and dry it in a constant temperature drying oven at 60°C 12h, get short rod TbPO 4...

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Abstract

The invention discloses short rod-shaped TbPO4 powder with excellent luminescence property and a preparation method thereof. The preparation method is characterized by comprising the following steps: adopting terbium trinitrate and monoammonium phosphate as raw materials, respectively dissolving terbium salt and NH4H2PO4 into deionized water according to a molar ratio of PO4<3-> and Tb<3+> being (40:1), evaporating the NH4H2PO4 solution to be recrystallized, dissolving the crystallized substance into the deionized water, mixing with the terbium salt solution, and stirring; adjusting the pH value to 3 to form a precursor solution; placing the precursor solution into a reaction kettle with a polytetrafluoroethylene lining to have hydrothermal reaction; preserving the heat, centrifuging the generated white precipitate, washing with deionized water, and drying the white precipitate to obtain the short rod-shaped TbPO4 powder. The short rod-shaped hexagonal-phase TbPO4 powder is synthesized by adopting the low-temperature hydrothermal method, simple operation is realized, the preparation period is short, the crystals are regular, the crystal grain is uniform, the crystallization degree is high, the dispersion property is good, and the luminescence property is good.

Description

technical field [0001] The present invention relates to a short rod-shaped TbPO 4 The preparation method of powder, in particular to a short rod-shaped TbPO with good luminescent properties 4 Powder and its preparation method. Background technique [0002] Due to the unique electronic layer structure of rare earth elements, rare earth compounds exhibit many excellent optical, electrical and magnetic functions, especially rare earth ions have the advantages of rich fluorescence emission lines, high fluorescence intensity and long fluorescence lifetime, etc., and are widely used in Various lighting and display devices. It has broad application prospects in various fields such as display and lighting. Usually, reverse micelles, microemulsions, hydrothermal, sol-gel methods are used, and specific additives and templates are added to obtain corresponding nanoscale rare earth phosphates with special morphology. TbPO 4 As a green powder has been widely concerned. For example, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
Inventor 刘运陈玉柏史晓磊李晋阳左浩强
Owner SHAANXI UNIV OF SCI & TECH
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