Method for preparing phosphoric acid rare earth monocrystalline nano-thread

A single crystal nanometer, rare earth phosphate technology, applied in the direction of single crystal growth, single crystal growth, chemical instruments and methods, etc., to achieve the effect of strong applicability, high crystallinity, and pure phase state

Inactive Publication Date: 2003-11-19
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the research on rare earth phosphate at home and abroad mainly focuses on the preparation and properties of its bulk and nanocrystalline materials (K.Riwotzki et al., Angew.Chem.Int.E

Method used

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  • Method for preparing phosphoric acid rare earth monocrystalline nano-thread
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  • Method for preparing phosphoric acid rare earth monocrystalline nano-thread

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Experimental program
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Effect test

Embodiment 1

[0024] Embodiment 1 Lanthanum phosphate nanowire

[0025] Add 0.0022 moles of phosphoric acid to 40 milliliters of 0.05 moles of lanthanum nitrate solution. After mixing evenly, the pH is 0.8. The cup-shaped container made of polytetrafluoroethylene containing the above solution is placed in a closed pressure-resistant stainless steel reaction kettle. And react under corresponding autogenous pressure for 17 hours. Then, cool to room temperature, filter, wash and dry at 60°C to obtain a white powder. The product was identified by powder X-ray diffraction as monoclinic lanthanum phosphate ( figure 1 ); Observing this product with a transmission electron microscope is a nanowire, with a length of 1-3 microns and a width of 20-50 nanometers ( figure 2 ). Electron diffraction proved that the lanthanum phosphate nanowires were single crystals.

Embodiment 2

[0026] Embodiment 2 Ceric phosphate rice noodles

[0027] Add 0.0022 moles of phosphoric acid to 40 milliliters of 0.05 moles of cerous nitrate solution, and after mixing uniformly, the pH is 0.8, and the cup-shaped container made of polytetrafluoroethylene material that fills the above solution is placed in a closed pressure-resistant stainless steel reaction kettle, at 220 ℃ under corresponding autogenous pressure to react for 17 hours. Then, cool to room temperature, filter, wash and dry at 60°C to obtain a white powder. The product was identified by powder X-ray diffraction as monoclinic cerium phosphate ( image 3 ); Observing with transmission electron microscope that this product is a nanowire, the length is 2-5 microns, and the width is 20-100 nanometers ( Figure 4 ). Electron diffraction proves that the cerium phosphate nanowires are single crystals.

Embodiment 3

[0028] Embodiment 3 europium phosphate nanowire

[0029] Add 0.0022 moles of ammonium dihydrogen phosphate to 40 milliliters of 0.05 moles of cerous nitrate solution, and after mixing evenly, the pH is 1. Place the cup-shaped container made of polytetrafluoroethylene containing the above solution in a closed pressure-resistant stainless steel reaction kettle , reacted at 240°C and corresponding autogenous pressure for 24 hours. Then, cool to room temperature, filter, wash and dry at 60°C to obtain a white powder. The product was identified by powder X-ray diffraction as monoclinic europium phosphate ( Figure 5 ); Observing with a transmission electron microscope that the product is a nanowire, the length is 3-10 microns, and the width is 50-200 nanometers ( Image 6 ). Electron diffraction proves that the europium phosphate nanowires are single crystals.

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Abstract

A process for preparing monocrystal nanowires of RE phosphate includes such steps as diluting inorganic RE salt with deionized water, adding phosphoric acid, dihydrogen phosphate, hydrogen phosphate, phosphate, or their mixture, regulating pH to 0.5-3, reacting at 200-260 deg.c for 6-36 hr in sealed pressure reactor, cooling, filtering, washing and drying. Its advantages are high crystalline level and low cost.

Description

Technical field: [0001] The invention relates to a method for preparing inorganic nanometer materials, in particular to a method for preparing rare earth phosphate single crystal nanowires. Background technique: [0002] In recent years, one-dimensional nanomaterials (including nanowires, nanobelts, nanotubes, and nanorods) have attracted great research interest, mainly due to the unique properties of one-dimensional nanomaterials compared with bulk materials and their Electronic and optoelectronic nano-devices and biochemical probes have great application prospects. In one-dimensional nanomaterials, nanowires are important connectors and active components for assembling nanodevices. [0003] Due to the unique 4f electron configuration, rare earth elements have excellent photoelectromagnetic properties, and have been widely used in permanent magnets, phosphors, catalysts and other fields. As an important rare earth inorganic salt, rare earth phosphate is mainly used in the...

Claims

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Application Information

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IPC IPC(8): C30B29/14C30B29/62
Inventor 张亚文严纯华廖春生严铮光司锐
Owner PEKING UNIV
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