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Solvent-thermal synthesis of lanthanum phosphate nanorod

A technology of lanthanum phosphate and nanorods, which is applied in the direction of phosphate, phosphorus oxyacid, etc., can solve the problems of affecting performance, powder agglomeration, poor dispersibility, etc., and achieve improved stability, enhanced application, and good dispersibility Effect

Inactive Publication Date: 2008-12-17
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The high-temperature solid-phase method usually heats for a long time, and finally grinds to obtain a single-phase powder. The crystal shape is good, but the powder agglomeration phenomenon is serious, and the particle size is large; and the ball milling destroys the surface structure, which affects its performance and consumes a lot of energy.
In the precipitation method, a small amount of surfactant can be added to improve the filtration performance of the precipitate and change the crystal shape of the precipitated particles. The sedimentation rate is controlled, the sintering temperature is reduced, and a fine and uniform powder can be obtained, but the precipitate and mother liquor must be aged. Phase purity is not high, crystallinity is not good
The hydrothermal method is carried out at a relatively low temperature, and can produce nanoparticles with high-purity phase, perfect crystallization, good dispersion, and uniform particle size distribution. The operation is simple, the environmental pollution is small, and the prepared product does not need ball milling. However, the current hydrothermal synthesis of lanthanum phosphate nanorods is generally only carried out in aqueous solution, and the obtained lanthanum phosphate nanorods are not uniform in size and poor in dispersion.

Method used

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  • Solvent-thermal synthesis of lanthanum phosphate nanorod
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 10ml of 1.0mol / L lanthanum chloride aqueous solution and 10ml of 1.0mol / L sodium phosphate aqueous solution into 30ml of n-butanol, the molar concentration of lanthanum chloride in the mixed solution is 0.2mol / L, stir until evenly mixed, Phosphoric acid was used to adjust the pH of the solution to 4, transferred to a polytetrafluoroethylene-lined autoclave, and solvothermally reacted for 4 hours at 220° C. in a constant temperature box to prepare lanthanum phosphate nanorods. Such as figure 1 As shown in the middle curve 1, all diffraction peaks can correspond to the standard peaks of the monoclinic lanthanum phosphate at the bottom, thus it can be known that the obtained lanthanum phosphate nanorods are a pure-phase monazite structure, which belongs to the monoclinic system, monazite structure. According to the Scherrer formula D=κ·λ / βcosθ, κ is the Scherrer constant, generally valued at 0.89; λ is the X-ray wavelength, and the value is 0.154056nm in this embodime...

Embodiment 2

[0021] Add 1.0 mol / L lanthanum chloride aqueous solution and 1.0 mol / L sodium phosphate aqueous solution into 30 ml of n-propanol, and other experimental operations and reagent consumption are the same as those in Embodiment 1 to prepare lanthanum phosphate nanorods. Such as figure 1 As shown in middle curve 2, all diffraction peaks can correspond to the standard peaks of the monoclinic lanthanum phosphate at the bottom, thus it can be known that the obtained lanthanum phosphate nanorods are a pure-phase monazite structure. The Scherrer formula can estimate the grain size to be about 7nm.

Embodiment 3

[0023] Add 10ml of 1.5mol / L lanthanum chloride aqueous solution and 15ml of 1.0mol / L sodium phosphate aqueous solution into 25ml of n-butanol, the molar concentration of lanthanum chloride in the mixed solution is 0.3mol / L, stir until it is evenly mixed, Phosphoric acid was used to adjust the pH of the solution to 5, transferred to an autoclave lined with polytetrafluoroethylene, and subjected to solvothermal reaction at 180° C. for 24 hours in an incubator to prepare lanthanum phosphate nanorods. Such as figure 1 As shown in the middle curve 3, all diffraction peaks can correspond to the standard peaks of the monoclinic lanthanum phosphate at the bottom, thus it can be known that the obtained lanthanum phosphate nanorods are a pure-phase monazite structure. The Scherrer formula can estimate the grain size to be about 9nm.

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Abstract

The invention discloses a method for using a solvent to carry out thermosynthesis so as to obtain nanorods of lanthanum phosphate; the method comprises the following steps of: mixing a lanthanum chloride solution with the concentration of 1.0-2.0mol / L and a sodium phosphate solution with the concentration of 1.0-2.0mol / L, wherein, the sodium phosphate and the lanthanum chloride have equal molar ratio; adding an n-butanol solvent and leading the volume ratio of water and the n-butanol to be 0.5 to 2 : 1 with the molar concentration of the lanthanum chloride in the mixed solution being 0.2 to 0.5mol / L; stirring the mixture till the mixture is even; adjusting the PH value of the solution to be 3 to 6 by phosphoric acid and hot reaction is carried out for 6.0 to 48 hours under the condition that the temperature is 140 to 220 DEG C. The synthetic method of the invention is simple, environment-friendly, green and economical, low-temperature, without needing calcination, and can obtain products directly in the solution; the obtained lanthanum phosphate has high purity, belongs to the monoclinic crystal system and is the nano rod with monazite structure; the nano rod has the diameter of less than 10nm, even fineness, single appearance and good dispersity.

Description

technical field [0001] The invention belongs to the technical field of inorganic nanometer materials, and in particular relates to a method for solvothermally synthesizing lanthanum phosphate nanorods. Background technique [0002] Rare earth phosphates have excellent fluorescent properties and high quantum efficiency, and are a class of excellent luminescent materials, suitable for high-density excitation and high-energy quantum excitation environments, and can be used in special glass, laser technology, compact fluorescent lamps, plasma Flat display. Due to the chemical and physical characteristics of the rare earth phosphate itself, lanthanum phosphate (LaPO 4 ) is often used as a good host material for doping other rare earth ions, and plays an important role in optical materials. At the same time, the rare earth phosphate LaPO 4 It has a high melting point and is an oxide fiber coating material suitable for high temperature use. It is compatible with Al 2 o 3 Compo...

Claims

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Application Information

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IPC IPC(8): C01B25/26
Inventor 田俐吴明娒李发琴李秀艳
Owner SUN YAT SEN UNIV
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