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A Method for Preparing Rare Earth Orthophosphate Monodisperse Spherical Up/Down Conversion Phosphor Powder Using Microwave Uniform Precipitation

A technology for single and uniform precipitation of orthophosphate, applied in the field of material science, to achieve mass production, low cost, great flexibility and universal applicability

Active Publication Date: 2019-08-23
NORTHEASTERN UNIV LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the characteristic that rare earth orthophosphate tends to grow anisotropically at higher temperature or after a long time of precipitation reaction, its monodisperse spherical powder has never been prepared by uniform precipitation method.

Method used

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  • A Method for Preparing Rare Earth Orthophosphate Monodisperse Spherical Up/Down Conversion Phosphor Powder Using Microwave Uniform Precipitation
  • A Method for Preparing Rare Earth Orthophosphate Monodisperse Spherical Up/Down Conversion Phosphor Powder Using Microwave Uniform Precipitation
  • A Method for Preparing Rare Earth Orthophosphate Monodisperse Spherical Up/Down Conversion Phosphor Powder Using Microwave Uniform Precipitation

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Experimental program
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Effect test

Embodiment 1

[0039] A method for preparing rare earth orthophosphate monodisperse spherical up / down conversion phosphors by microwave uniform precipitation, comprising the following steps:

[0040] (1) 50mmol phosphoric acid, 2.5mmol ammonium sulfate and 250mmol urea are fully dissolved in water;

[0041] (2) Add 5mmol Y(NO 3 ) 3 ;

[0042] (3) while stirring, the pH of the resulting mixed solution was adjusted to 1.0 with nitric acid, and it was placed in a microwave reactor for 8 minutes, and the output power of the microwave reactor was 650W;

[0043] (4) centrifugal separation, cleaning and drying, obtain the rare earth yttrium phosphate monodisperse spherical powder;

[0044] (5) Calcining the obtained rare earth yttrium phosphate monodisperse spherical powder at 1000° C. for 2 hours to obtain rare earth yttrium phosphate monodisperse spherical powder with good crystallinity.

[0045]The obtained microwave homogeneous precipitation reaction product is a monodisperse spherical powd...

Embodiment 2

[0047] A method for preparing rare earth orthophosphate monodisperse spherical up / down conversion phosphors by microwave uniform precipitation, comprising the following steps:

[0048] (1) 50mmol phosphoric acid, 2.5mmol ammonium sulfate and 250mmol urea are fully dissolved in water;

[0049] (2) Add 5mmol La(NO 3 ) 3 ;

[0050] (3) while stirring, the pH of the resulting mixed solution was adjusted to 0.9 with nitric acid, and it was placed in a microwave reactor for 8 minutes, and the output power of the microwave reactor was 700W;

[0051] (4) centrifugal separation, cleaning and drying, to obtain monodisperse spherical powder of rare earth lanthanum phosphate;

[0052] (5) Calcining the obtained rare earth lanthanum phosphate monodisperse spherical powder at 1000° C. for 2 hours to obtain rare earth lanthanum phosphate monodisperse spherical powder with good crystallinity.

[0053] The resulting microwave homogeneous precipitation reaction product is a monodisperse hex...

Embodiment 3

[0056] A method for preparing rare earth orthophosphate monodisperse spherical up / down conversion phosphors by microwave uniform precipitation, comprising the following steps:

[0057] (1) fully dissolve 100mmol phosphoric acid, 2.5mmol ammonium sulfate and 250mmol urea in water;

[0058] (2) Add 5mmol Y(NO 3 ) 3 ;

[0059] (3) while stirring, the pH of the resulting mixed solution was adjusted to 1.2 with nitric acid, and it was placed in a microwave reactor for 8 minutes, and the output power of the microwave reactor was 750W;

[0060] (4) centrifugal separation, cleaning and drying, obtain the rare earth yttrium phosphate monodisperse spherical powder;

[0061] (5) Calcining the obtained rare earth yttrium phosphate monodisperse spherical powder at 800° C. for 4 hours to obtain rare earth yttrium phosphate monodisperse spherical powder with good crystallinity.

[0062] The diameter of the obtained microwave uniform precipitation reaction product is about 1.5 μm, and its...

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Abstract

The invention belongs to the field of material science and particularly relates to a method to prepare rare-earth orthophosphate monodisperse spherical upconversion / downconversion phosphor via microwave homogeneous precipitation, comprising the steps of 1) dissolving phosphoric acid, a sulfur source and urea in ionic water, wherein the molar ratio of the phosphoric acid, phosphate and urea is (5-20):(0.2-4):(20-100); 2) adding rare-earth nitrate into the mixed solution above, wherein the molar ratio of the total quantity of rare-earth ions to the added phosphate is controlled to 1:(5-20); 3) adding nitric acid into the mixed solution to allow reaction; 4) centrifugally separating the reacted solution, washing, and drying to obtain rare-earth orthophosphate monodisperse spherical powder; 5)calcining the rare-earth orthophosphate monodisperse spherical powder of step 4 at 600-1100 DEG C for 2-8 h. The method has high reaction speed, is good and efficient, is low in cost and easy to operationally control and is suitable for batch production.

Description

technical field [0001] The invention belongs to the field of material science, and in particular relates to a method for preparing rare earth orthophosphate monodisperse spherical up / down conversion fluorescent powder by means of microwave uniform precipitation. Background technique [0002] Monodisperse spherical powders have been proven to have great application potential in fields such as lighting, drug delivery, and biomarkers. Among the many methods for preparing monodisperse spherical powder, the emulsion polymerization method and the urea-based uniform precipitation method are the most efficient, and the former is generally used to prepare polymer latex balls and silica balls, and the latter is mostly used to prepare rare earth basic carbonic acid salt balls. A large number of studies have shown that spherical powders with a diameter greater than or equal to 100nm are formed through the agglomeration of countless smaller particles, rather than through a simple "nucle...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/81
Inventor 朱琦王志浩李继光李晓东孙旭东
Owner NORTHEASTERN UNIV LIAONING
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