Solvent-thermal synthesis of lanthanum phosphate nanorod

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...

Examples

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.

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...

Examples

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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