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Method of greenly preparing rare-earth potassium orthophosphate nano/micro crystal

A technology of orthophosphate and microcrystals, applied in the field of hydrothermal synthesis, can solve the problems of complex process, high production cost, unfavorable environmental protection and rational application of resources, and achieve the effect of simple process, convenient operation and convenient industrial operation

Inactive Publication Date: 2009-08-26
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Although the above-mentioned methods provide some approaches for synthesizing rare earth phosphate nanomaterials, there are still deficiencies, such as solid-phase reactions usually requiring high temperature, excessive phosphorus and complicated procedures to obtain nanoscale phosphates, although the solution method does not require high The reaction temperature, but the inevitable by-products, the adjustment of the acidity of the solution will result in higher production costs and complex processes, which is not conducive to environmental protection and rational use of resources

Method used

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  • Method of greenly preparing rare-earth potassium orthophosphate nano/micro crystal
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  • Method of greenly preparing rare-earth potassium orthophosphate nano/micro crystal

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Embodiment 1: Preparation of lanthanum phosphate nanowires or nanorods

[0032] (1) Add 2.0×10 -4 mol of La 2 o 3, phosphorus pentoxide or phosphoric acid, La 2 o 3 The molar ratio is 1:1, after adding deionized water to make the filling degree of the reactor reach 60-80%, the reactor is sealed;

[0033] (2) Then transfer the reaction kettle to a temperature-controlled furnace, and control the reaction temperature to be 100°C, 140°C, 160°C, and 250°C at a heating rate of 10°C / min, and heat at this temperature for 24, 24, and 24, respectively. 6, 18, 48, 1 hour.

[0034] (3) After the reaction was completed, the reactor was taken out and cooled to room temperature naturally.

[0035] (4) Take out the precipitate obtained in the reaction, wash it three times with deionized water and absolute ethanol alternately, and centrifuge after each washing to obtain the desired product.

[0036] figure 1 The X-ray powder diffraction patterns of the products obtained under di...

Embodiment 2

[0037] Embodiment 2: Preparation of lanthanum phosphate nanorods or nanoparticles

[0038] (1) Add 2.0×10 -4 mol of La 2 o 3 , phosphorus pentoxide or phosphoric acid, La 2 o 3 The molar ratios are 50:1, 100:1 and 200:1 respectively, add deionized water to make the reactor fill degree reach, after 50-60%, seal the reactor;

[0039] (2) Then, the reaction kettle was transferred to a temperature-controlled furnace, and the reaction temperature was controlled to be 160° C. at a heating rate of 8.5° C. / minute, and heated at this temperature for 24 hours.

[0040] (3) After the reaction was completed, the reactor was taken out and cooled to room temperature naturally.

[0041] (4) Take out the precipitate obtained in the reaction, wash it three times with deionized water and absolute ethanol alternately, and centrifuge after each washing to obtain the desired product.

[0042] from image 3 Visible a), the LaPO obtained when the molar ratio P / La=50 4 The scanning electron m...

Embodiment 3

[0043] Embodiment 3: prepare Nd, Sm, Gd phosphate nanomaterial

[0044] Take 2.0×10 respectively -4 mol of Nd 2 o 3 , Sm 2 o 3 , Gd 2 o 3 , and 50 microliters of phosphoric acid solution (85%) are raw materials, adding deionized water makes the degree of filling of the reactor reach 60-80%, the control reaction temperature is respectively 140 ° C, 250 ° C, and the reaction time is 24 hours. Other operating processes and Example 1 is the same. Figure 4 The SEM photo of the resulting part of the product given in , shows that the product is a nano-scale particle.

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Abstract

The invention belongs to the field of micro / nano material preparation technology and hydrothermal synthesis technology, and specifically relates to a green method for preparing rare earth orthophosphate nano / micro crystals. The specific steps are: use phosphorus pentoxide or phosphoric acid and rare earth metal oxides as precursors, use deionized water or absolute ethanol as solvent, place them in a container, and the molar ratio of phosphorus pentoxide or phosphoric acid and rare earth metal oxides 1 to 200, the amount of solvent added is 50-80% of the volume of the container; put the container containing the mixture in a temperature-controlled furnace, and increase the temperature at a rate of 8.5-11.5°C / min, according to the requirements of different characteristics of the product to be obtained, In the range of 100°C-250°C, keep at a certain temperature and heat at a constant temperature for 1-48 hours, take out the container, and naturally cool to room temperature; wash and centrifuge to obtain the desired product. The invention realizes that in a specific hydrothermal reaction system, the insoluble rare earth oxides and phosphorus pentoxide or phosphoric acid in the normal state are directly used as precursors, and through changes in temperature and time, the proportion of reactants and additives Addition can control the morphology and crystal form of the product.

Description

technical field [0001] The invention belongs to the field of micro / nano material preparation technology and hydrothermal synthesis technology, and specifically relates to a method for preparing rare earth orthophosphate nano / micro crystals. Background technique [0002] Rare earth elements are favored in phosphors because of their unique 4f-layer electronic structure and the excellent performance of excitation light in line spectrum or narrow band spectrum. At the same time, rare earth phosphates have broad application prospects in medicine, nuclear industry, electricity, laser, magnetism, and other fields. With the development of nanotechnology, the demand for nanoscale rare earth orthophosphate will increase. The preparation method of the rare earth orthophosphate of reported nanoscale mainly comprises solid-phase method and solution method: solid-phase method is usually with excessive phosphorus pentoxide or phosphoric acid, ammonium dihydrogen phosphate is phosphorus so...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/26C01B25/45C01F17/00
Inventor 吴庆生董凤强马杰
Owner TONGJI UNIV
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