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Preparation method of fluorescent hybrid nanoparticles

A hybrid particle and fluorescent nanotechnology, which is applied in the field of fluorescent materials, can solve the problem that the embedded structure does not give an intuitive and effective image, etc., and achieves the effect of improving the fluorescence performance, improving the fluorescence lifetime and easing the trend of fluorescence decay.

Active Publication Date: 2017-01-25
QINGDAO UNIV
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

In 1997, K. Machida and G. Adachi used the sol-gel method to prepare organo-rare earth complexes of europium and terbium embedded in silica, and obtained that the thermal properties and fluorescence properties of the embedding were improved. conclusion, but did not give an intuitive and effective image on the characterization of the formation of the embedding structure; in 2002, Professor M.Morita also used the sol-gel method to prepare silica-embedded organic rare earth complexes, this time they Expand the types of rare earths to four elements of cerium, samarium, europium and terbium, and mainly study the influence of temperature and annealing on the fluorescence properties of rare earth complexes

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  • Preparation method of fluorescent hybrid nanoparticles
  • Preparation method of fluorescent hybrid nanoparticles

Examples

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Embodiment 1

[0023] A method for preparing fluorescent nano-hybrid particles, comprising the following steps:

[0024] (1) Weigh and record the mass of a 25ml round bottom flask, the mass of a 0.5cm spindle-shaped rotor, weigh 0.125g of europium trioxide white powder into the round bottom flask, add 1ml of deionized water, stir, and make the white powder into a paste Put it in a 50°C water bath and add an aqueous solution of hydrochloric acid dropwise under the condition of magnetic stirring until the white paste turns into a transparent and clear solution.

[0025] (2) Utilize the rotary evaporator to steam the excess water of the obtained clear solution, and fully volatilize the excess hydrochloric acid, and then dry in a constant temperature drying oven to obtain colorless and transparent europium chloride crystals, calculated to be 0.0008mol.

[0026] (3) Measure 8ml of absolute ethanol, dissolve colorless and transparent europium chloride crystals, and obtain a 0.1 mol / l ethanol solut...

Embodiment 2

[0034] A method for preparing fluorescent nano-hybrid particles, comprising the following steps:

[0035] (1) Preparation of organic rare earth complexes: as in Example 1, configure the ethanol solution of 0.1mol / l europium chloride, the ethanol solution of 0.3mol / l α-thiophenoyl trifluoroacetone, 0.1mol / l The ethanol solution of o-phenanthroline, the three were stirred and reacted for 2 hours according to the molar ratio of 1:1:1, 13 drops of aqueous sodium hydroxide solution was added dropwise, pH=9, and a ternary complex of europium was generated, 8000 rpm Minutes of centrifugation, alcohol wash each time, the obtained product was dissolved with 2ml of acetone until clear and transparent.

[0036] (2) Preparation of nano silica gel: mix 33.35ml ethanol and 13.5ml triple distilled water in a glass container, then add 0.7ml concentrated ammonia water and 2.45ml tetraethyl orthosilicate respectively to prepare gained nano silica The particle size is 150±60nm.

[0037] (3) Ad...

Embodiment 3

[0041] A method for preparing fluorescent nano-hybrid particles, comprising the following steps:

[0042] (1) Preparation of organic rare earth complexes: as in Example 1, configure the ethanol solution of 0.1mol / l europium chloride, the ethanol solution of 0.3mol / l α-thiophenoyl trifluoroacetone, 0.1mol / l The ethanol solution of o-phenanthroline, the three were stirred and reacted for 2 hours according to the molar ratio of 1:1:1, 15 drops of aqueous sodium hydroxide solution was added dropwise, pH=11, and a ternary complex of europium was generated, 8000 rpm Minutes of centrifugation, alcohol wash each once, the product obtained was dissolved with 4ml of acetone until clear and transparent.

[0043](2) Preparation of nano silica gel: mix 33.35ml ethanol and 13.5ml triple distilled water in a glass container, then add 0.7ml concentrated ammonia water and 2.45ml tetraethyl orthosilicate respectively to prepare gained nano silica The particle size is 130±60nm.

[0044] (3) Ad...

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Abstract

The invention discloses a preparation method of fluorescent hybrid nanoparticles. The preparation method includes: preparing ternary complexes of rare-earth europium under the alkaline condition (adjustment with a water solution of sodium hydroxide) prior to dispersing via an alkaline solution (adjustment with ammonium hydroxide); subjecting the alkaline solution to further hybrid reaction with silica gel; on the premises of reducing particle size of silicon dioxide, enabling dispersibility of the ternary complexes of the rare-earth europium in silicon dioxide nanoparticles to be improved. The obtained fluorescent hybrid nanoparticles are obviously improved in fluorescence property, fluorescence strength is doubled that of a pure complex, fluorescence decay trend is alleviated, fluorescence life is prolonged, and raw materials good in fluorescence property are provided for photoluminescence materials.

Description

technical field [0001] The invention relates to the technical field of fluorescent materials, in particular to a method for preparing fluorescent nano-hybrid particles. Background technique [0002] The reason why rare earths have excellent luminescent properties is that they have a special energy conversion function (that is, the transition of electrons between different energy levels to generate energy) and a special 4f electron layer structure. However, the light absorption coefficient ε of rare earth ions in the near ultraviolet region is very small, so the luminous efficiency is low. In the 1960s, Weissman discovered the "Antenna Effect", a theory that improves the luminous efficiency of rare earth ions. However, after further research, it was found that the organic complexes of rare earth ions have poor thermal stability, concentration self-quenching phenomenon is prone to occur at high concentrations, and the compatibility mismatch between the preparation method and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/02C09K11/06B82Y20/00
CPCB82Y20/00C09K11/02C09K11/06C09K2211/182
Inventor 王彦欣唐建国黄林军王瑶刘继宪
Owner QINGDAO UNIV
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