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Cocoon-shaped TbPO4 powder with good luminescence property and preparation method thereof

A technology of luminescence performance, NH4H2PO4, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as pollution, and achieve the effects of good dispersion, good repeatability, and uniform grain size

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

AI Technical Summary

Problems solved by technology

Although Yu Ranbo et al. used phosphoric acid as the phosphorus source, hexagonal TbPO was obtained under the condition of excess phosphorus 4 , (Chinese Invention Patent: Publication No.: CN101481103B, Application No.: CN200910078276) makes synthesis technology improved, but raw material H 3 PO 4 Has low toxicity and is easy to pollute the environment
[0003] So far, there is no literature or patent report on the formation of cocoon-like TbPO with good luminescent properties under low-temperature hydrothermal conditions using water as solvent without using any surfactants, templates and dispersants. 4

Method used

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  • Cocoon-shaped TbPO4 powder with good luminescence property and preparation method thereof
  • Cocoon-shaped TbPO4 powder with good luminescence property and preparation method thereof
  • Cocoon-shaped TbPO4 powder with good luminescence property and preparation method thereof

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preparation example Construction

[0022] A cocoon-like TbPO with good luminescent properties 4 The preparation method of powder comprises the following steps:

[0023] Step 1): Add Tb(NO 3 ) 3 ·6H 2 O was dissolved in deionized water and stirred for 5-10min to form a terbium salt solution; the NH 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 2.7mol / 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+ = 60:1 molar ratio mixed, and when mixed, the terbium salt solution was added dropwise to the NH 4 h 2 PO 4 Stir in the solution for 10min, then use ammonia water and dilute HNO 3 Adjust the pH of the precursor solution to pH=2, and then obtain the precursor solution;

[0024] Step 2): Transfer the precursor solution obtained in step 1) to a reactor lined with polytetrafluoroethylene, and the volume filling degree of the reactor is 60%-80%;

[00...

Embodiment 1

[0029] Step 1: Add 0.9mmol of Tb(NO 3 ) 3 ·6H 2 O was dissolved in deionized water, stirred for 5min, and 54mmol of NH 4 h 2 PO 4 Dissolve in deionized water, heat the solution until recrystallization, then add deionized water to obtain NH with a concentration of 2.7mol / L 4 h 2 PO 4 In deionized water, the terbium salt and NH 4 h 2 PO 4 Deionized water solution according to PO 4 3- :Tb 3+ =60:1 molar ratio mixed, 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=2;

[0030]Step 2: Transfer the precursor solution to a reactor lined with polytetrafluoroethylene, and the volume filling degree of the reactor is 80%;

[0031] Step 3: Using low-temperature hydrothermal method, set the hydrothermal reaction temperature to 100°C and the holding time to 24h, take out the white precipitate formed after the reaction, cent...

Embodiment 2

[0033] Step 1: Add 0.9mmol of Tb(NO 3 ) 3 ·6H 2 O was dissolved in deionized water, stirred for 10 min, and 54 mmol of NH 4 h 2 PO 4 Dissolve in deionized water, heat the solution until recrystallization, then add deionized water to obtain NH with a concentration of 2.7mol / L 4 h 2 PO 4 In deionized water, the terbium salt and NH 4 h 2 PO 4 Deionized water solution according to PO 4 3- :Tb 3+ =60:1 molar ratio mixed, 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=2;

[0034] Step 2: Transfer the precursor solution to a reactor lined with polytetrafluoroethylene, and the volume filling degree of the reactor is 60%;

[0035] Step 3: Using low-temperature hydrothermal method, set the hydrothermal reaction temperature to 100°C and the holding time to 24h, take out the white precipitate formed after the reaction, ...

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Abstract

The invention discloses cocoon-shaped TbPO4 powder with a good luminescence property and a preparation method thereof. The preparation method comprises the following steps: respectively dissolving the raw materials terbium trinitrate and NH4H2PO4 into deionized water according to the condition that the molar ratio of PO4<3-> to Tb<3+> is 60:1, evaporating the NH4H2PO4 solution to recrystallize, dissolving the crystal substance into deionized water, mixing with the terbium trinitrate solution, and stirring; regulating the pH to be 2 so as to form a precursor solution, transferring the precursor solution into a reaction kettle with a lining of teflon, carrying out hydrothermal reaction, carrying out heat preservation, then centrifuging the generated white precipitate, washing with deionized water, and then drying so as to obtain the cocoon-shaped TbPO4 powder. The cocoon-shaped hexagonal phase TbPO4 powder is synthesized by virtue of a low temperature hydrothermal method, is simple to prepare, has short preparation cycle, is regular and uniform, has high degree of crystallinity and good dispersibility, and has good luminescence property.

Description

technical field [0001] The invention relates to a cocoon-like TbPO 4 Preparation method of powder, in particular to a cocoon-like TbPO with good luminescent properties 4 Powder and its preparation method. Background technique [0002] Due to their unique electronic layer structure, rare earth compounds exhibit excellent properties in light, electricity, and magnetism. In particular, rare earth elements have spectroscopic properties, chemical stability, and thermal stability that cannot be compared with ordinary elements. The rare earth compounds are widely used in various lighting, display instruments, medicine and military fields, especially in the application of phosphors. At present, nanoscale rare earth compounds with good morphology have potential application prospects, and nanoscale rare earth phosphate compounds with good morphology mainly use phosphoric acid as the phosphorus source, through reverse micelles, microemulsions, hydrothermal, sol-gel By adding specifi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
Inventor 刘运陈玉柏史晓磊张进
Owner SHAANXI UNIV OF SCI & TECH
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