Preparation method of rare-earth-doped strontium fluorophosphate nanoparticles

A nanoparticle, strontium fluorophosphate technology, applied in the field of optical materials, can solve the problems of rare earth ion fluorescence quenching, reduction of fluorescence efficiency, limitation, etc., and achieve the effect of good fluorescence intensity and fluorescence lifetime

Inactive Publication Date: 2011-07-20
XI'AN INST OF OPTICS & FINE MECHANICS - CHINESE ACAD OF SCI
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Problems solved by technology

[0005] The present invention proposes a preparation method of rare earth-doped strontium fluorophosphate nanoparticles, which mainly solves the problem that the presence of a large number of hydroxyl groups in strontium fluorophosphate prepared by the traditional co-precipitation method will cause the fluorescence quenching of doped rare earth ions and greatly reduce the fluorescence. Efficiency, which limits the application of this type of material in the field of optics

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preparation example Construction

[0024] The preparation method of the rare earth-doped strontium fluorophosphate nanoparticles comprises the following steps:

[0025] 1] Mix the rare earth compound or oxide with the aqueous solution of strontium salt, and mix evenly with a magnetic stirrer; then, add the aqueous solution of monohydrogen phosphate and fluoride, and stir for 30 minutes.

[0026] The molar ratio of strontium salt to monohydrogen phosphate is 5:3, the molar ratio of strontium ion to fluoride ion is 5:1-3; the concentration of rare earth ion used is 0.1-1mol / L, the molar ratio of rare earth ion to strontium ion The ratio is 0.005~0.05:1;

[0027] Commonly used rare earth ions are praseodymium, neodymium, samarium, europium, holmium, erbium, thulium, ytterbium, etc., which can be provided by soluble salts of these rare earth ions, such as nitrate, or prepared as a solution with their oxides and nitric acid. The fluoride can be sodium fluoride, ammonium fluoride, etc.; strontium salt is a soluble s...

Embodiment 1

[0033] Weigh 1.047g Sr(NO 3 ) 2 Dissolve in 15ml deionized water, add 0.1ml, 0.25mol / L Pr(NO 3 ) 3 solution (the doping molar ratio is 0.5%) and mix uniformly; weigh 0.396g (NH 4 ) 2 HPO 4 Dissolve 0.042g NaF in 10ml deionized water; mix the above two solutions, and stir for 30 minutes; adjust the pH value of the solution to 3 with 0.01mol / L dilute nitric acid solution, and stir for 1 hour; then, use 0.01mol / L hydrogen The sodium oxide solution adjusted the pH value of the solution to 7, and stirred for 1 hour; the reciprocating cycle was repeated 3 times. The resulting precipitate was centrifuged, washed three times with deionized water and absolute ethanol, and dried in vacuum at 200°C for 5 hours to obtain a white powder.

Embodiment 2

[0035] Weigh 1.047g Sr(NO 3 ) 2 Dissolve in 15ml deionized water, add 0.5ml, 0.1mol / L Nd(NO 3 ) 3 solution (1% molar ratio doping) and mix uniformly; weigh 0.396g (NH 4 ) 2 HPO 4 Dissolve 0.084g NaF in 10ml deionized water, mix the above two solutions, stir for 30 minutes, adjust the pH value of the solution to 3 with 0.1mol / L dilute nitric acid solution, stir for 1 hour, and then add 0.1mol / L The pH value of the solution was adjusted to 7 with sodium hydroxide solution, stirred for 1 hour, and reciprocated 5 times. The obtained precipitate was separated by centrifugation, washed three times with deionized water and absolute ethanol respectively, and dried under vacuum at 70° C. for 24 hours to obtain a white powder. figure 1 Sr prepared for this example5 (PO 4 ) 3 F:Nd 3+ (1% mol) transmission electron microscope image (TEM) of nanoparticle, shows that the morphology of nanoparticle is basically rod-shaped, with a length of about 50nm and a width of about 7nm, and ha...

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Abstract

The invention belongs to the technical field of optical materials, and particularly discloses a preparation method of rare-earth-doped strontium fluorophosphate nanoparticles. The preparation method comprises the following steps of: firstly, mixing a rare earth compound with a strontium salt aqueous solution and uniformly stirring; secondly, adding an aqueous solution of monohydric phosphate and fluoride, adjusting the pH value of the solution to 3 and reacting for 1 hour, thirdly, adjusting the pH value of the solution to 7, reacting for 1 hour and circulating 5-10 times; reacting for multiple hours in a polytetrafluoroethylene-lined stainless steel reaction kettle by undergoing a normal temperature reaction or adopting a hydrothermal synthesis method at the controlled temperature of between 100 DEG C and 200 DEG C; and lastly, separating, washing, and drying in vacuum to obtain the rare-earth-doped strontium fluorophosphate nanoparticles. The method has the characteristics of simple preparation processes, practicability, low cost, wide applicability and application prospect and the like, and meanwhile, is beneficial to overcoming of the defect of high content of hydroxyl on the surface of a nanometer material in a preparing process and prolonging of the fluorescent lifetime of a rare-earth-doped nanometer material.

Description

technical field [0001] The invention belongs to the technical field of optical materials, and in particular relates to a preparation method of rare earth-doped strontium fluorophosphate nanoparticles. Background technique [0002] As an important laser gain medium, rare earth-doped strontium fluorophosphate is used in high-energy and intense laser systems due to its high thermal conductivity and large gain coefficient. [0003] Rare-earth-doped strontium fluorophosphate currently used in lasers is mainly crystal bulk, which is prepared by high-temperature pulling method, and it is difficult to obtain large-sized crystals, which limits the wide application of such materials. At the same time, because the crystal block laser working material itself is prone to damage, it cannot solve the bottleneck problems such as increasing the repetition rate and damage threshold. The nanoscale rare earth doped strontium fluorophosphate material has more excellent optical properties due to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/73H01S3/20B82Y40/00
Inventor 彭波韦玮潘柳华佘江波崔晓霞乔泽邦
Owner XI'AN INST OF OPTICS & FINE MECHANICS - CHINESE ACAD OF SCI
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