CN101787284A - Upconversion luminescent hollow sphere using yttrium fluoride as ground substance and preparation method thereof - Google Patents
Upconversion luminescent hollow sphere using yttrium fluoride as ground substance and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an upconversion luminescent hollow sphere using yttrium fluoride as a ground substance and a preparation method thereof and belongs to the technical field of preparation of rare earth doped luminescent materials. The chemical formula of the upconversion luminescent hollow sphere is Y1-x-yYbxLnyF3, wherein Ln is Er or Tm, x is not less than 0.05 and not more than 0.2, and y is not less than 0.01 and not more than 0.1. The preparation method comprises the following steps of: (1) proportionally mixing rare earth compound ions with arginine and fluorides to obtain a mixed solution; (2) carrying out hydrothermal reaction at different temperatures for different time periods to obtain a precursor; and (3) and carrying out heat treatment on the precursor at different temperatures to obtain the fluoride hollow luminescent sphere. The method has the advantages of simple synthesis process, low cost, environmental protection, strong practicability and easy mass production. When excited by a 980nm laser, the prepared fluoride upconversion hollow luminescent sphere can emit stronger red and green light.
Description
Technical field
The present invention relates to a kind of is the up-conversion luminescence hollow material and preparation method thereof of matrix with the yttrium fluoride, belongs to the rear-earth-doped luminous material preparing technical field.
Background technology
Up-conversion luminescent material is the important rare earth luminescent material of a class, it can convert the low frequency exciting light to high frequency emission light by multi-photon mechanism, in fields such as solid statelaser, transmitter, solar cell, anti-counterfeit recognition, infrared acquisition, biological detection important use is arranged all.Rare earth fluorine has low phonon vibration energy, and rare earth ion excited state quencher degree is little, and high heat and environmental stability have become the good matrix of up-conversion luminescent material.
The preparation method who with the fluorochemical is the last conversion nano luminescent material of matrix mainly contains hydrothermal method, solvent-thermal method, microemulsion method etc.The converting luminescent material of fluoride of these preparation method's preparations is solid material, yet there are no the report of the hollow up-conversion luminescent material of preparation.And be in the patent of 200810155960.X in the patent No., Wang Zhilin has proposed a kind of method for preparing the composite rare-earth fluoride hollow ball, be that compound rare-earth metal ion and ethylenediamine tetraacetic acid (EDTA) effect are formed title complex, add fluorochemical again, in the mixing solutions of organic solvent and water, react and obtain the composite rare-earth fluoride hollow ball.Also do not adopt the arginine auxiliary law to prepare the report of conversion hollow luminous ball on the fluorochemical of nanometer rod assembling at present both at home and abroad.
Amino acid can use as tensio-active agent as a kind of important biomolecules, and the auxiliary synthesis method of amino acid attracts biologist and chemist more and more to pay close attention to just gradually in recent years.Arginine is an amino acid a kind of simple in structure, cheap, is that tensio-active agent assists hollow rare earth luminous nanometer ball of synthesis of nano rod assembling to have that method is simple, economical, free of contamination advantage with it.Hollow luminous nanometer ball has low density, specific surface area is big, perviousness is high characteristics, thereby is being widely used aspect the slowly-releasing of molecular fluorescence probe, medicine and conveying material and the light filler.
Summary of the invention
The purpose of this invention is to provide a kind of is the up-conversion luminescence hollow ball and preparation method thereof of matrix with the yttrium fluoride, and this luminescent ball is to be assembled by nanometer rod.
The chemical expression of the up-conversion luminescent material that the present invention is prepared is: Y
1-x-yYb
xLn
yF
3
Wherein: Ln is Er or Tm; X=0.05～0.2; Y=0.01～0.1
Preparation nanometer rod provided by the present invention assembling be that the method that goes up the conversion hollow luminous ball of matrix is that rare earth ion forms mixing solutions with arginine earlier with the yttrium fluoride, add ammonium fluoride solution again, under differing temps and time, carry out hydro-thermal reaction, can obtain changing hollow luminous ball on the yttrium fluoride of described nanometer rod assembling.
The employed raw material of preparation method of the present invention is that purity is 99.99% Y
2O
3, Yb
2O
3, Tm
2O
3, Er
2O
3, and analytically pure NH
4F, solvent are water, HNO
3Be used for the dissolved oxygen thing, tensio-active agent is analytically pure arginine.
The method of conversion hollow luminous ball comprises the steps: on the fluorochemical of preparation nanometer rod assembling
Step 1. with the rare earth oxide nitric acid dissolve, adds the mixing solutions that entry forms rare earth ion under the condition of room temperature or heating, add arginine solution again and mix, use magnetic stirrer 30 minutes under the room temperature, add ammonium fluoride solution again, continue to stir 30 minutes, obtain mixing solutions; Wherein rare earth ion total amount and fluorion (F
-) the ratio of amount of substance be 1: 3～5; The rare earth ion total amount is 1: 2.5～3.5 with the ratio of arginic amount of substance;
Step 2. moves into reactor with step 1 gained mixing solutions, respectively at reacting under 160～200 ℃ the condition 24～48 hours, takes out reactor, room temperature to be naturally cooled to, and centrifugation, washing after the drying, obtains precursor samples for several times;
Step 3. in 450～600 ℃ of following calcinations 4～8 hours, obtains the precursor samples of step 2 gained to change hollow luminous ball on the yttrium fluoride of nanometer rod assembling.
The present invention is raw material with the rare-earth oxide, under the condition that arginine exists, through different hydrothermal temperatures, differential responses time and thermal treatment subsequently, can obtain changing hollow luminous ball on the yttrium fluoride of nanometer rod assembling.The present invention is tensio-active agent with the arginine, and entire reaction is carried out in the aqueous solution, without any organic solvent, and economic environmental protection, practical, be with a wide range of applications.
Description of drawings
Fig. 1 is the prepared Y of embodiment 1
0.9Yb
0.09Er
0.01F
3The SEM photo of hollow luminous ball; This figure double as is a Figure of abstract;
Fig. 2 is the prepared Y of embodiment 1
0.9Yb
0.09Er
0.01F
3The XRD spectra of hollow luminous ball;
Fig. 3 is the prepared Y of embodiment 1
0.9Yb
0.09Er
0.01F
3The last switching emission spectrogram of hollow luminous ball;
Embodiment
Embodiment 1: take by weighing 257mg Y
2O
3, 44.8mg Yb
2O
3With 4.83mg Er
2O
3In beaker, add the rare nitric acid of 5mL (nitric acid and deionized water volume ratio are 1: 1) dissolving, the cooling back adds the 21mL deionized water and forms rare-earth ion solution; Take by weighing the 1.32g arginine and join in the 9mL deionized water, after treating to dissolve fully, two solution are mixed, under the room temperature with obtaining rare earth ion and arginic mixing solutions behind the magnetic stirrer 30min; Taking by weighing the 280mg Neutral ammonium fluoride is dissolved in the 5mL deionized water and obtains ammonium fluoride solution; Ammonium fluoride solution is dropwise joined in rare earth ion and the arginic mixing solutions, continue to stir 30min under the room temperature and get mixing solutions, it is transferred in the reactor of 50mL, behind 200 ℃ of reaction 24h, take out reactor, naturally cool to room temperature, centrifugation, after the washing drying, obtain precursor samples; Precursor samples is put into the temperature programming stove, with 3 ℃/min temperature rise rate thermal treatment temp is risen to 450 ℃, constant temperature 4h under this temperature can obtain the Y that nanometer rod is assembled
0.9Yb
0.09Er
0.01F
3Last conversion hollow luminous ball.Fig. 1 is the synthetic Y of institute
0.9Yb
0.09Er
0.01F
3The stereoscan photograph of the hollow luminous nanometer ball of last conversion shows that synthetic product diameter is about the hollow ball-shape structure of 700nm, and this structure is to be about 80～100nm by diameter, and the nanometer rod self-assembly that length is about 300～500nm forms; Fig. 2 is the x-ray diffraction pattern of product, illustrates that product is the YF of pure phase
3, belong to rhombic system.Fig. 3 is the last switching emission spectrum of product, and interpret sample has the emission of stronger redness and green up-conversion fluorescence under the exciting of 980nm laser.
Embodiment 2: take by weighing 158mgY
2O
3, 78.8mg Yb
2O
3With 38.3mg Er
2O
3In beaker, add the rare nitric acid of 5mL (nitric acid and deionized water volume ratio are 1: 1) dissolving, the cooling back adds the 21mL deionized water and forms rare-earth ion solution; Take by weighing the 1.05g arginine and join in the 9mL deionized water, after treating to dissolve fully, two solution are mixed, under the room temperature with obtaining rare earth ion and arginic mixing solutions behind the magnetic stirrer 30min.Taking by weighing the 222mg Neutral ammonium fluoride is dissolved in the 5mL deionized water and obtains ammonium fluoride solution; Ammonium fluoride solution is dropwise joined in rare earth ion and the arginic mixing solutions, continue to stir 30min under the room temperature and get mixing solutions, it is transferred in the reactor of 50mL, in 160 ℃ of reaction 24h, take out reactor, room temperature to be naturally cooled to, centrifugation, after the washing drying, obtain precursor samples, precursor samples is put into the temperature programming stove, thermal treatment temp is risen to 450 ℃ with 3 ℃/min temperature rise rate, constant temperature 4h under this temperature can obtain the Y that nanometer rod is assembled
0.7Yb
0.2Er
0.1F
3Last conversion hollow luminous ball.Under the exciting of 980nm laser, launch stronger redness and green up-conversion fluorescence.
Embodiment 3: take by weighing 213mgY
2O
3, 20.7mg Yb
2O
3With 20.1mg Er
2O
3In beaker, add the rare nitric acid of 5mL (nitric acid and deionized water volume ratio are 1: 1) dissolving, the cooling back adds the 21mL deionized water and forms rare-earth ion solution; Take by weighing the 1.22g arginine and join in the 9mL deionized water, after treating to dissolve fully, two solution are mixed, under the room temperature with obtaining rare earth ion and arginic mixing solutions behind the magnetic stirrer 30min.Taking by weighing the 312mg Neutral ammonium fluoride is dissolved in the 5mL deionized water and obtains ammonium fluoride solution; Ammonium fluoride solution is dropwise joined in rare earth ion and the arginic mixing solutions, under room temperature, continue to stir 30min and get mixing solutions, it is transferred in the reactor of 50mL, in 200 ℃ of reaction 48h, take out reactor, room temperature to be naturally cooled to, centrifugation, after the washing drying, obtain precursor samples, precursor samples is put into the temperature programming stove, thermal treatment temp is risen to 500 ℃ with 3 ℃/min temperature rise rate, constant temperature 6h under this temperature can obtain the Y that nanometer rod is assembled
0.9Yb
0.05Er
0.05F
3Last conversion hollow luminous ball.Under the exciting of 980nm laser, launch stronger redness and green up-conversion fluorescence.
Embodiment 4: take by weighing 203mgY
2O
3, 35.5mg Yb
2O
3With 3.86mg Tm
2O
3In beaker, add the rare nitric acid of 5mL (nitric acid and deionized water volume ratio are 1: 1) dissolving, the cooling back adds the 21mL deionized water and forms rare-earth ion solution; Take by weighing the 1.22g arginine and join in the 9mL deionized water, after treating to dissolve fully, two solution are mixed, under the room temperature with obtaining rare earth ion and arginic mixing solutions behind the magnetic stirrer 30min.Taking by weighing the 222mg Neutral ammonium fluoride is dissolved in the 5mL deionized water and obtains ammonium fluoride solution; Ammonium fluoride solution is dropwise joined in rare earth ion and the arginic mixing solutions, under room temperature, continue to stir 30min and get mixing solutions, it is transferred in the reactor of 50mL, in 180 ℃ of reaction 48h, take out reactor, room temperature to be naturally cooled to, centrifugation, after the washing drying, obtain precursor samples, precursor samples is put into the temperature programming stove, thermal treatment temp is risen to 450 ℃ with 3 ℃/min temperature rise rate, constant temperature 4h under this temperature can obtain the Y that nanometer rod is assembled
0.9Yb
0.09Tm
0.01F
3Last conversion hollow luminous ball.Under the exciting of 980nm laser, launch stronger redness and green up-conversion fluorescence.
Embodiment 5: take by weighing 242mgY
2O
3, 49.8mg Yb
2O
3With 24.4mg Tm
2O
3In beaker, add the rare nitric acid of 5mL (nitric acid and deionized water volume ratio are 1: 1) dissolving, the cooling back adds the 21mL deionized water and forms rare-earth ion solution; Take by weighing the 1.54g arginine and join in the 9mL deionized water, after treating to dissolve fully, two solution are mixed, under the room temperature with obtaining rare earth ion and arginic mixing solutions behind the magnetic stirrer 30min.Taking by weighing the 467mg Neutral ammonium fluoride is dissolved in the 5mL deionized water and obtains ammonium fluoride solution; Ammonium fluoride solution is dropwise joined in rare earth ion and the arginic mixing solutions, under room temperature, continue to stir 30min and get mixing solutions, it is transferred in the reactor of 50mL, in 180 ℃ of reaction 24h, take out reactor, room temperature to be naturally cooled to, centrifugation, after the washing drying, obtain precursor samples, precursor samples is put into the temperature programming stove, thermal treatment temp is risen to 450 ℃ with 3 ℃/min temperature rise rate, constant temperature 4h under this temperature can obtain the Y that nanometer rod is assembled
0.85Yb
0.1Tm
0.05F
3Last conversion hollow luminous ball.Under the exciting of 980nm laser, launch stronger redness and green up-conversion fluorescence.
Embodiment 6: take by weighing 247mgY
2O
3, 48.5mg Yb
2O
3With 4.75mg Tm
2O
3In beaker, add the rare nitric acid of 5mL (nitric acid and deionized water volume ratio are 1: 1) dissolving, the cooling back adds the 21mL deionized water and forms rare-earth ion solution; Take by weighing the 1.50g arginine and join in the 9mL deionized water, after treating to dissolve fully, two solution are mixed, under the room temperature with obtaining rare earth ion and arginic mixing solutions behind the magnetic stirrer 30min.Taking by weighing the 455mg Neutral ammonium fluoride is dissolved in the 5mL deionized water and obtains ammonium fluoride solution; Ammonium fluoride solution is dropwise joined in rare earth ion and the arginic mixing solutions, under room temperature, continue to stir 30min and get mixing solutions, it is transferred in the reactor of 50mL, in 160 ℃ of reaction 48h, take out reactor, room temperature to be naturally cooled to, centrifugation, after the washing drying, obtain precursor samples, precursor samples is put into the temperature programming stove, thermal treatment temp is risen to 450 ℃ with 3 ℃/min temperature rise rate, constant temperature 6h under this temperature can obtain the Y that nanometer rod is assembled
0.89Yb
0.1Tm
0.01F
3Last conversion hollow luminous ball.Under the exciting of 980nm laser, launch stronger redness and green up-conversion fluorescence.
Embodiment 7: take by weighing 267mgY
2O
3, 124mg Yb
2O
3With 30.1mg Er
2O
3In beaker, add the rare nitric acid of 5mL (nitric acid and deionized water volume ratio are 1: 1) dissolving, the cooling back adds the 21mL deionized water and forms rare-earth ion solution; Take by weighing the 1.25g arginine and join in the 9mL deionized water, after treating to dissolve fully, two solution are mixed, under the room temperature with obtaining rare earth ion and arginic mixing solutions behind the magnetic stirrer 30min.Taking by weighing the 533mg Neutral ammonium fluoride is dissolved in the 5mL deionized water and obtains ammonium fluoride solution; Ammonium fluoride solution is dropwise joined in rare earth ion and the arginic mixing solutions, under room temperature, continue to stir 30min and get mixing solutions, it is transferred in the reactor of 50mL, in 160 ℃ of reaction 24h, take out reactor, room temperature to be naturally cooled to, centrifugation, after the washing drying, obtain precursor samples, precursor samples is put into the temperature programming stove, thermal treatment temp is risen to 600 ℃ with 3 ℃/min temperature rise rate, constant temperature 8h under this temperature can obtain the Y that nanometer rod is assembled
0.75Yb
0.2Er
0.05F
3Last conversion hollow luminous ball.Under the exciting of 980nm laser, launch stronger redness and green up-conversion fluorescence.
Claims (2)
1. one kind is the up-conversion luminescence hollow ball of matrix with the yttrium fluoride, it is characterized in that, described is that the up-conversion luminescence hollow ball of matrix is to be assembled by nanometer rod with the yttrium fluoride; Described is that the chemical formula formula of the up-conversion luminescence hollow ball of matrix is Y with the yttrium fluoride
1-x-yYb
xLn
yF
3, wherein: Ln is Er or Tm; X=0.05～0.2; Y=0.01～0.1.
2. a method for preparing with the yttrium fluoride up-conversion luminescence hollow ball that is matrix is characterized in that, selects for use arginine as tensio-active agent, and by the hydro-thermal synthetic technology, the preparation product is to change hollow luminous ball on the fluorochemical of nanometer rod assembling, the steps include:
Step 1. with the rare earth oxide nitric acid dissolve, adds entry and forms mixing solutions under the condition of room temperature or heating, add arginine solution again and mix, use magnetic stirrer 30 minutes under the room temperature, add ammonium fluoride solution again, continue to stir described rare earth ion total amount and F 30 minutes
-The ratio of amount of substance be 1: 3～5; The rare earth ion total amount is 1: 2.5～3.5 with the ratio of arginic amount of substance,
Step 2. moves into reactor with step 1 gained mixing solutions, respectively at reacting under 160～200 ℃ the condition 24～48 hours, takes out reactor, room temperature to be naturally cooled to, and centrifugation, washing after the drying, obtains precursor samples for several times,
Step 3. in 450～600 ℃ of following calcinations 4～8 hours, obtains YF with the precursor samples of step 2 gained
3: Eu
3+The hollow luminous ball of nanometer rod assembling.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102942926A (en) * | 2012-11-09 | 2013-02-27 | 沈阳化工大学 | Preparation method of hollow light-emitting rare-earth microsphere |
| CN104087301A (en) * | 2014-07-03 | 2014-10-08 | 上海交通大学 | Preparation method of general porous rare-earth-doped up-conversion nanomaterial |
| CN104357056A (en) * | 2014-11-13 | 2015-02-18 | 南京信息工程大学 | Preparation method of europium-doped sodium gadolinium fluoride red light-emitting porous nanocrystal material |
| CN104371729A (en) * | 2014-12-03 | 2015-02-25 | 南京邮电大学 | Fluorescent powder and preparation method thereof |
| CN105586039A (en) * | 2016-03-11 | 2016-05-18 | 扬州大学 | Hollow-structure CeO2:Er3+/Yb3+ up-conversion luminescent material and application thereof |
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| WO1997046488A1 (en) * | 1996-06-05 | 1997-12-11 | Sarnoff Corporation | Method for preparing small particle size fluoride up-converting phosphors |
| CN1185475A (en) * | 1996-12-17 | 1998-06-24 | 中国科学院长春物理研究所 | Up-conversion luminous material and preparation method thereof |
| US5891361A (en) * | 1997-05-02 | 1999-04-06 | Sarnoff Corporation | Method for preparing small particle size fluoride up-converting phosphors |
| JP2008266628A (en) * | 2007-03-27 | 2008-11-06 | Dainippon Printing Co Ltd | Phosphor particle dispersion, and three-dimentional display device and two-dimentional display device using the same |
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2010
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| WO1997046488A1 (en) * | 1996-06-05 | 1997-12-11 | Sarnoff Corporation | Method for preparing small particle size fluoride up-converting phosphors |
| CN1185475A (en) * | 1996-12-17 | 1998-06-24 | 中国科学院长春物理研究所 | Up-conversion luminous material and preparation method thereof |
| US5891361A (en) * | 1997-05-02 | 1999-04-06 | Sarnoff Corporation | Method for preparing small particle size fluoride up-converting phosphors |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102942926A (en) * | 2012-11-09 | 2013-02-27 | 沈阳化工大学 | Preparation method of hollow light-emitting rare-earth microsphere |
| CN104087301A (en) * | 2014-07-03 | 2014-10-08 | 上海交通大学 | Preparation method of general porous rare-earth-doped up-conversion nanomaterial |
| CN104087301B (en) * | 2014-07-03 | 2016-08-24 | 上海交通大学 | A kind of preparation method of general porous rare earth doping up-conversion nano material |
| CN104357056A (en) * | 2014-11-13 | 2015-02-18 | 南京信息工程大学 | Preparation method of europium-doped sodium gadolinium fluoride red light-emitting porous nanocrystal material |
| CN104357056B (en) * | 2014-11-13 | 2017-02-22 | 南京信息工程大学 | Preparation method of europium-doped sodium gadolinium fluoride red light-emitting porous nanocrystal material |
| CN104371729A (en) * | 2014-12-03 | 2015-02-25 | 南京邮电大学 | Fluorescent powder and preparation method thereof |
| CN105586039A (en) * | 2016-03-11 | 2016-05-18 | 扬州大学 | Hollow-structure CeO2:Er3+/Yb3+ up-conversion luminescent material and application thereof |
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