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Novel sheet stacked spherical structure rare earth oxysulfide and preparation method and application thereof

A rare earth sulfur oxide, a new type of technology, applied in the preparation/processing of rare earth metal compounds, rare earth metal sulfides, chemical instruments and methods, etc., can solve the problems of uneven product size, irregular morphology, and environmental pollution, etc. To achieve the effect of simple preparation method, high yield and low energy consumption

Pending Publication Date: 2022-04-22
XIAMEN INST OF RARE EARTH MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has the disadvantages of high reaction temperature, high energy consumption, uneven product size and irregular shape, and the steam generated by the solid sulfur element used at high temperature will pollute the environment.

Method used

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  • Novel sheet stacked spherical structure rare earth oxysulfide and preparation method and application thereof
  • Novel sheet stacked spherical structure rare earth oxysulfide and preparation method and application thereof
  • Novel sheet stacked spherical structure rare earth oxysulfide and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Weigh 1mmol of rare earth gadolinium nitrate (0.451g), 1.2mmol of ammonium persulfate (0.274g) in a 25mL glass bottle, add 8mL of ethanol and 8mL of water, stir well in the hydrothermal reaction kettle, and then raise the temperature of the reaction kettle to 110°C , keep 3h. Take out the reaction kettle and cool it to room temperature, wash with ethanol / water mixed solvent with a volume ratio of 1:1, suction, filter and dry to obtain a composite phase rare earth gadolinium oxysulfide. Then at 5% H 2 / 95%N 2 Calcined at 850°C for 2 hours under a mixed atmosphere to obtain a single-phase rare earth gadolinium oxysulfide (Gd 2 o 2 S).

[0050] figure 1 Middle (a) is the xrd characterization figure of composite phase type and single phase type rare earth gadolinium oxysulfide prepared in this embodiment, as can be seen from the results in the figure, rare earth sulfur oxide can be realized from composite phase type to The transformation of the crystalline phase of a ...

Embodiment 2

[0053] Take by weighing the mixture of 1mmol rare earth gadolinium nitrate (0.406g) and europium nitrate (0.045g) (control Eu 3+ The molar weight of ions accounts for 10% of the total molar weight of rare earth ions), 1.5mmol (0.342g) of ammonium persulfate is placed in a 25mL glass bottle, 8mL of ethanol and 8mL of water are added, in a hydrothermal reactor, stir well, and then the reaction The kettle was heated to 110°C and kept for 3h. Take out the reactor and cool it to room temperature, wash with ethanol / water mixed solvent with a volume ratio of 1:1, filter and dry to obtain Eu 3+ Ion-doped complex-phase rare earth gadolinium oxysulfide. Then at 5% H 2 / 95%N 2 Calcined at 850°C for 2h under a mixed atmosphere to obtain single-phase Eu 3+ Ion-doped rare earth gadolinium oxysulfide (Gd 2 o 2 S:Eu 3+ ).

[0054] figure 1 (b) is Eu 3+ The xrd characterization diagrams of the ion-doped complex-phase and single-phase rare earth gadolinium oxysulfide, as can be seen f...

Embodiment 3

[0059] Weigh the mixture of 1mmol rare earth yttrium nitrate (0.364g) and europium nitrate (0.023g) (control Eu 3+ The molar weight of ions accounts for 5% of the total molar weight of rare earth ions), 1.5mmol (0.342g) of ammonium persulfate is placed in a 25mL glass bottle, 8mL of ethanol and 8mL of water are added, in a hydrothermal reactor, stir well, and then the reaction The kettle was heated to 110°C and kept for 3h. Take out the reactor and cool it to room temperature, wash with ethanol / water mixed solvent with a volume ratio of 1:1, filter and dry to obtain Eu 3+ Ion-doped complex-phase rare earth yttrium oxysulfide. Then at 5% H 2 / 95%N 2 Calcined at 850°C for 2h under a mixed atmosphere to obtain single-phase Eu 3+ Ion-doped rare earth yttrium oxysulfide (Y 2 o 2 S:Eu 3+ ).

[0060] Figure 4 (a) is Eu 3+ The xrd characterization diagrams of ion-doped composite-phase and single-phase rare earth yttrium oxysulfide, as can be seen from the results in the fig...

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Abstract

The invention discloses a novel sheet-stacked spherical structure rare earth oxysulfide and a preparation method and application thereof.The preparation method comprises the steps that persulfate is used as a sulfur source and a morphology regulating agent and is evenly mixed with a rare earth salt precursor solution, and then the composite rare earth oxysulfide which is monodisperse, uniform in size and of a sheet-stacked spherical structure is prepared through a hydrothermal method; and after high-temperature calcination reduction, the single-phase rare earth oxysulfide with excellent performance is prepared. The method disclosed by the invention avoids environmental pollution caused by steam generated by sulfur volatilization in solid heat reaction, and has the advantages of environmental friendliness, low energy consumption, high economic benefit, simple process flow, good product dispersity, uniform particle size distribution, spherical structure formed by stacking sheets, good product chemical stability and the like; and controllable adjustment of the two rare earth sulfur oxides with different phase structures is realized, so that the prepared rare earth doped sulfur oxide luminescent material has relatively good luminescent property.

Description

technical field [0001] The invention relates to the field of rare earth luminescent materials, in particular to a novel monodisperse, sheet-stacked spherical structure rare earth sulfur oxide, its preparation method and its application in luminescent materials. Background technique [0002] Rare earth oxysulfide is an excellent luminescent substrate, which has the characteristics of narrow spectral band, high color purity, high light absorption and conversion efficiency, and good physical and chemical stability. It is important in the fields of information, lighting, and imaging. Applications. An ideal luminescent material must have a narrow particle size distribution, no agglomeration, and a spherical structure as much as possible, which is conducive to obtaining high-quality device coatings, thereby improving luminous efficiency and service life. At present, the main method for preparing rare earth sulfur oxide luminescent materials is high-temperature solid-phase method ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/10C01F17/294C09K11/84
CPCC01F17/10C01F17/294C09K11/7701C09K11/7789C01P2002/72C01P2002/52C01P2004/03C01P2006/60C01P2004/32C01P2004/64
Inventor 申仲荣詹晨阳
Owner XIAMEN INST OF RARE EARTH MATERIALS
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