CN103756677A - Synthesis and preparation method for novel hollow luminescence rare earth micron structure - Google Patents

Synthesis and preparation method for novel hollow luminescence rare earth micron structure Download PDF

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Publication number
CN103756677A
CN103756677A CN201310410428.9A CN201310410428A CN103756677A CN 103756677 A CN103756677 A CN 103756677A CN 201310410428 A CN201310410428 A CN 201310410428A CN 103756677 A CN103756677 A CN 103756677A
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China
Prior art keywords
rare earth
hollow
micron structure
preparation
novel hollow
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Pending
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CN201310410428.9A
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李玉丹
王金
赫川
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TIANJIN JIAOQIANG TECHNOLOGY Co Ltd
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TIANJIN JIAOQIANG TECHNOLOGY Co Ltd
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Publication of CN103756677A publication Critical patent/CN103756677A/en
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Abstract

The invention relates to a synthesis and preparation method for a novel hollow luminescence rare earth nano-micron structure, wherein the method comprises a Y2O3:Ln<3+>(Ln<3+>=Eu<3+>, Nd<3+>) hollow micron structure synthesis process. According to the present invention, the method has characteristics of easy operation, easily-understood principle, easily-available product and surfactant use saving; during the novel hollow luminescence rare earth nano-micron structure process, the template is not required to be modified, and is not required to be removed after completing the reaction; and the obtained hollow micron structure Y2O3:Ln<3+>(Ln<3+>=Eu<3+>, Nd<3+>) with characteristics of uniform dispersion, uniform size and similar shape respectively emits red light and purplish red light under ultraviolet light and low-voltage electron beam excitation, and is a valuable and potential luminescence material.

Description

A kind of synthetic and preparation method of novel hollow luminescence rare earth micrometer structure
Technical field
The present invention relates to the synthetic and preparation method of rare earth nano material, particularly relate to a kind of synthetic and preparation method of novel hollow luminescence rare earth micrometer structure,, belong to luminescent material technical field.
Background technology
In recent years, rare earth nano material is produced and is produced apparent impact human sciences's technology, life as a critical material.Rare earth ion is as the luminescence center of luminescent material, by inorganic and organic materials investigator extensive concern.Some title complexs have the phenomenon of photoluminescence.The electronic structure of rare earth ion uniqueness with become to build feature, make luminescent properties can by change part form to regulate and control, there is unique luminescent properties.Rare earth metal is playing a significant role aspect the functional materialss such as luminescent material, catalytic material, magnetoopticmemory material, hydrogen storage material.Therefore the preparation of nano material is also the emphasis that people pay close attention to.The micrometer structure of its hollow core due to its special character (as large in specific surface area, relative density is little, refractive index and thermal expansivity low etc.) caused social extensive concern, and be widely used at aspects such as the encapsulation of slowly-releasing, sensor and the active material of medicine and optical crystals.Up to now, developed the method for a variety of synthetic hollow structures.But these methods have certain defect.Therefore, must find a kind of suitable structure, it can have stronger receptivity, and the energy efficient absorbing can be passed to the excited state of rare earth metal and causes luminous.So develop a kind of novel simple, stable and practical synthetic method that obtains, prepare profile, big or small similar and composition inorganic novel hollow luminous structured material uniformly, meet social demand.
Summary of the invention
The present invention be directed to the less stable of original synthetic hollow micron rare earth structure, method complexity, in order to overcome the above problems, the object of the present invention is to provide a kind of synthetic and preparation method of novel hollow luminescence rare earth micrometer structure.Present method, take PS structure as template, first by coordination, adopts the mode of grinding to add organic ligand between PS structure, then carries out the synthetic Y of surperficial modification 2o 3: Ln 3+(Ln 3+=Eu 3+, Nd 3+) novel hollow luminescence rare earth nano-micrometre structure, there is unified, uniform profile, and do not need the use of tensio-active agent, be a kind of valuable luminescent material.
The object of the invention is to be achieved through the following technical solutions:
A preparation method for novel hollow luminescence rare earth nano-micrometre structure, described method comprises Y 2o 3: Ln 3+(Ln 3+=Eu 3+, Nd 3+) building-up process of novel hollow micrometer structure:
By Y 2o 3first by reaction, obtain Ln with the oxide compound of rare earth 3+(Ln 3+=Eu 3+, Nd 3+) exchange structure, in mortar fully grind, make it to mix, again abrasive material is dissolved in to nitric acid, regulates pH value, add distilled water, be uniformly dissolved, add PS structure, stir 0.5h, gained solution supersound process, add modifier again, then heat with oil bath, centrifuge washing three times, dry in baking oven, and then at high temperature process, novel hollow luminescence rare earth nano-micrometre structure obtained.
In the present invention, the oxide compound of the rare earth described in step is europium sesquioxide and Neodymium trioxide.
In the present invention, the modifier described in step is carbon four silicon.
Advantage of the present invention and effect are:
1, easy to operate, principle is simple, and product easily obtains.
The use of 2, having omitted tensio-active agent in synthetic process.
3, in building-up process, neither need self form to modify, also do not need reaction to finish rear removal template.
4, the Y with unified big or small, dispersed and appearance similar obtaining 2o 3: Ln 3+(Ln 3+=Eu 3+, Nd 3+) hollow micron structure, under UV-light and denoted low voltage electron beam excite, send respectively red and red-purple is luminous.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
The present invention, take polystyrene (PS) as template, first by coordination, adopts the mode of grinding to add organic ligand between PS structure, then it is carried out to surperficial modification and synthesized Y 2o 3: Ln 3+(Ln 3+=Eu 3+, Nd 3+) novel hollow micrometer structure.A synthetic Y has been proposed 2o 3: Ln 3+(Ln 3+=Eu 3+, Nd 3+) inorganic mechanism that novel hollow micrometer structure is new, and at rare earth ion (Eu 3+, Nd 3+) doping Y 2o 3the process of novel hollow micrometer structure synthetic product in, embodied fully Y 2o 3: Ln 3+(Ln 3+=Eu 3+, Nd 3+) luminosity.
The present invention adopts PS structure as self form, can control better and prepare the hollow structure of this product, first by coordination, adopt the mode of grinding to add organic ligand between PS structure, again it is carried out to surperficial modification, synthesized the Y of dispersed, unified profile 2o 3: Ln 3+(Ln3+=Eu 3+, Nd 3+) novel hollow micrometer structure.Prepared Y 2o 3: Ln 3+(Ln 3+=Eu 3+, Nd 3+) at room temperature, by exciting of denoted low voltage electron beam and UV-light, the feature that presents respectively the luminous rare earth element of emitting red light and red-purple is luminous.
Embodiment:
By Y 2o 3(0.4mmol) first by reaction, obtain Ln with the oxide compound (0.02mmol) of rare earth 3+(Ln 3+=Eu 3+, Nd 3+) exchange structure, then in mortar fully grind, make it to mix, again abrasive material is dissolved in to nitric acid (2mol/L), regulates pH value approximately 3 left and right, add the distilled water of 30mL, be uniformly dissolved, add 100mgPS structure, stir 0.5h, ultrasonic 2h, add modifier, with 80 ℃ of oil bath heating 4h, water and ethanol centrifuge washing 3 times, dry at 60 ℃, and then under 850 ℃ of left and right, process and within 4 hours, obtain product.

Claims (1)

1. a synthetic and preparation method for novel hollow luminescence rare earth nano-micrometre structure, is characterized in that, described method comprises Y 2o 3: Ln 3+(Ln 3+=Eu 3+, Nd 3+) building-up process of hollow micron structure: Y 2o 3first by reaction, make it to obtain Ln with the oxide compound of rare earth 3+(Ln 3+=Eu 3+, Nd 3+) exchange structure, in mortar fully grind, make it to mix, again abrasive material is dissolved in to nitric acid, regulates pH value, add distilled water, be uniformly dissolved, add PS structure, coordination, stir, supersound process, adds modifier, with oil bath heating, centrifuge washing, is dried again, and then at high temperature process, obtain this product; Described Y 2o 3with the mol ratio of oxide compound of the rare earth of doping be 15~20:1; Described water bath heating temperature is 80~90 ℃.
CN201310410428.9A 2013-09-10 2013-09-10 Synthesis and preparation method for novel hollow luminescence rare earth micron structure Pending CN103756677A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113214833A (en) * 2021-04-28 2021-08-06 华南理工大学 Europium-doped porous metal oxide and halide perovskite color-changing luminescent composite material and preparation method and application thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113214833A (en) * 2021-04-28 2021-08-06 华南理工大学 Europium-doped porous metal oxide and halide perovskite color-changing luminescent composite material and preparation method and application thereof

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Application publication date: 20140430