CN102994089A - Preparation method of alkaline earth fluoride nanocrystal with ultra small core-shell structure - Google Patents
Preparation method of alkaline earth fluoride nanocrystal with ultra small core-shell structure Download PDFInfo
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Abstract
Disclosed is a preparation method of alkaline earth fluoride nanocrystal with ultra small core-shell structure. The method comprises steps of: using soluble barium salt and rare earth ion salt as raw materials; conducting a solvothermal reaction in a mixed solvent of ethanol and oleic acid at 160 DEG C for 12 h to obtain Yb / Tm: BaF2 nanoparticles of 3 nm; and then adding the synthesized nanoparticles, strontium trifluoroacetic acid, rare-earth trifluoroacetic acid salt to a mixed solvent of oleic acid and octadecene, and reacting for 1-6 h under protection of inert atmosphere at 260-310 DEG C to obtain nanocrystal with ultra small core-shell structure (7 nm) Yb / Tm: BaF2 @ Ln / Nd: SrF2. The obtained nanocrystal with core-shell structure has good dispersion, uniform shape, narrow size distribution, ultra small scale, and luminescence properties of near infrared-near infrared up-conversion and near infrared-near infrared down-transfer, and is hopefully to be widely used in the field of biomarkers.
Description
Technical field
The invention belongs to the inorganic materials preparing technical field, relate to a kind of nanocrystalline preparation method of extra small (～7 nanometer) nucleocapsid structure alkaline earth fluoride with near infrared-near infrared bimodulus characteristics of luminescence.
Technical background
In recent years, rare earth ion doped luminescence nanocrystalline is subject to showing great attention to of scientific circles owing to being with a wide range of applications in the biomarker field.The luminescence nanocrystalline in vivo complexity of metabolism is that can it as one of key index of biological labled material.Studies show that nanocrystalline ratio is easier to excrete when yardstick during less than 10 nanometer in organism.But yardstick is less, and nanocrystalline specific surface area is larger, and the rare earth ion of doping is higher at the probability on surface, causes its luminous intensity obviously to descend.In order to overcome surperficial cancellation, effectively one of means are the structure nano-crystal with core-shell structure, namely protect luminous in stratum nucleare of rare earth at the nuclear nanocrystal surface inertia shell of growing.In traditional luminous nano-crystal with core-shell structure synthetic method, generally be to realize controlledly synthesis to product by intense adjustment precursor amounts, reaction solvent, tensio-active agent, reaction times and temperature of reaction etc.This way is complexity but also loaded down with trivial details not only, and is difficult to realize the preparation less than the nano-crystal with core-shell structure of 10 nanometers.
The present invention proposes a kind of method of the nanocrystalline size of luminous nucleon shell structure alkaline earth fluoride being regulated and control by rare earth ion doped realization.In the shell process of growth, by mixing rare earth ion, can regulate and control the yardstick of alkaline earth fluoride shell thickness and the nano-crystal with core-shell structure that finally obtains of control, so obtain to have near infrared-near infrared shift luminous, the single dispersion of bimodulus under the conversion and near infrared-near infrared, extra small (～7 nanometer) nucleocapsid structure alkaline earth fluoride is nanocrystalline.
Summary of the invention
The present invention proposes a kind of method of the nanocrystalline yardstick of luminous nucleon shell structure alkaline earth fluoride being regulated and control by rare earth ion doped realization, and purpose is to prepare novel extra small (～7 nanometer) core-shell structured nanomaterials that has on efficient near infrared-near infrared conversion and the lower transfer bimodulus characteristics of luminescence.
Technical scheme of the present invention is as follows:
(1) 0.40 mmol barium ion salt, 0.09 mmol ytterbium ion salt and 0.01 mmol thulium ion salt (described ion salt is: nitrate, oxymuriate or acetate) are joined 10 mL deionized waters, after stirring the transparent settled solution of formation, dropwise join in the mixed solution of 10 mL ethanol, 10 mL oleic acid and 2.5 g sodium oleates, be moved in the 40 mL water heating kettles after fully stirring, be added dropwise to subsequently hydrofluoric acid aqueous solution 4 mL of 1.0 mol/L, carry out solvent thermal reaction at last under 160 ℃ of temperature, soaking time is 12 hours.After products therefrom usefulness ethanol and the washing of hexanaphthene mixed solution, after 40～80 ℃ of oven dry, obtain Yb/Tm:BaF
2Examine nanocrystalline.
(2) with step (1) Yb/Tm:BaF that obtains
2Examine nanocrystalline, 0.40 mmol trifluoroacetic acid strontium Sr (CF
3COO)
2, 0.09 mmol trifluoroacetic acid rare earth compound Ln (CF
3COO)
3(wherein Ln can be any element among La, Ce, Pr, Sm, Eu, Gd, Y, Tb, Dy, Ho, Er, Tm, Yb or the Lu) and 0.01 mmol trifluoroacetic acid neodymium Nd (CF
3COO)
3Join in 10 mL oleic acid and the 10 mL octadecylenes; be moved in the 100 mL three-necked bottles after stirring the transparent settled solution of formation; under inertia (nitrogen or argon gas) atmosphere protection, be heated to subsequently 100 ℃ and be incubated the deoxygenation that dewaters in 30 minutes; under inertia (nitrogen or argon gas) atmosphere protection, continue to be heated to 260-310 ℃ at last, and be incubated 1-6 hour and react.After products therefrom usefulness ethanol and the washing of hexanaphthene mixed solution, after 40-80 ℃ of oven dry, obtain Yb/Tm:BaF
2@Ln/Nd:SrF
2Nano-crystal with core-shell structure.
Powder X-ray diffraction analysis transmission electron microscope observation shows: above-mentioned synthetic Yb/Tm:BaF
2Examining nanocrystalline is pure cubic structure phase, and its yardstick is about 3 nanometers, is shaped as spherical; With Yb/Tm:BaF
2Nanocrystalline for examining the Yb/Tm:BaF for preparing
2@Ln/Nd:SrF
2(Ln=La, Ce, Pr, Sm, Eu, Gd, Y, Tb, Dy, Ho, Er, Tm, Yb or Lu) nano-crystal with core-shell structure still is pure Emission in Cubic, and its yardstick is about 7 nanometers, is shaped as cubic block.The extra small nano-crystal with core-shell structure of gained can be realized up-conversion luminescence in 750-800 nano waveband scopes under the irradiation of 980 nanometer lasers, under 796 nanometer excitation light irradiations, shift luminous under can realizing in 920-1120 nano waveband scopes.
The present invention has that technology of preparing is simple, cost is low, productive rate is high, produces advantages such as being easy to amplification.Products therefrom good dispersity, shape homogeneous, narrow diameter distribution, yardstick are extra small, have near infrared-near infrared bimodulus characteristics of luminescence, are expected to be used widely in the biomarker field.
Description of drawings
Fig. 1 is Yb/Tm:BaF in the example 1
2Examine nanocrystalline transmission electron microscope bright field image;
Fig. 2 is Yb/Tm:BaF in the example 1
2@Gd/Nd:SrF
2The transmission electron microscope bright field image of nano-crystal with core-shell structure;
Fig. 3 is Yb/Tm:BaF in the example 1
2@Gd/Nd:SrF
2The up-conversion luminescence spectrum of nano-crystal with core-shell structure;
Fig. 4 is Yb/Tm:BaF in the example 1
2@Gd/Nd:SrF
2The lower transfer luminous spectrum of nano-crystal with core-shell structure.
Embodiment
Example 1: 0.40 mmol nitrate of baryta, 0.09 mmol ytterbium nitrate and 0.01 mmol thulium nitrate are joined 10 mL deionized waters, after stirring the transparent settled solution of formation, dropwise join in the mixed solution of 10 mL ethanol, 10 mL oleic acid and 2.5 g sodium oleates, be moved in the 40 mL water heating kettles after fully stirring, be added dropwise to subsequently hydrofluoric acid aqueous solution 4 mL of 1.0 mol/L, carry out solvent thermal reaction at last under 160 ℃ of temperature, soaking time is 12 hours.Gained is nanocrystalline with after ethanol and the washing of hexanaphthene mixed solution, after 60 ℃ of oven dry, obtain Yb/Tm:BaF
2Examine nanocrystalline.With the Yb/Tm:BaF that obtains
2Examine nanocrystalline, 0.40 mmol trifluoroacetic acid strontium Sr (CF
3COO)
2, 0.09 mmol trifluoroacetic acid gadolinium Gd (CF
3COO)
3With 0.01mmol trifluoroacetic acid neodymium Nd (CF
3COO)
3Join in 10 mL oleic acid and the 10 mL octadecylenes; be moved in the 100 mL three-necked bottles after stirring the transparent settled solution of formation; under nitrogen atmosphere protection, be heated to subsequently 100 ℃ and be incubated the deoxygenation that dewaters in 30 minutes, under the nitrogen atmosphere protection, continue to be heated to 260 ℃ at last, and be incubated 6 hours.After products therefrom usefulness ethanol and the washing of hexanaphthene mixed solution, after 60 ℃ of oven dry, obtain Yb/Tm:BaF
2@Gd/Nd:SrF
2Nano-crystal with core-shell structure.
Transmission electron microscope observation shows: above-mentioned synthetic Yb/Tm:BaF
2Examining nanocrystalline is 3 nanometer left and right sides spherical particles (Fig. 1); With Yb/Tm:BaF
2Nanometer ball is nuclear, the Yb/Tm:BaF that is synthesized
2@Gd/Nd:SrF
2Nano-crystal with core-shell structure 7 nanometer left and right sides cubic blocks (Fig. 2).Spectrum test shows: the extra small nano-crystal with core-shell structure of gained is under the irradiation of 980 nanometer lasers, can in 750-800 nano waveband scopes, realize up-conversion luminescence (Fig. 3), under the irradiation of 796 nanometer lasers, shift under can in 920-1120 nano waveband scopes, realizing luminous (Fig. 4).
Example 2: 0.40 mmol nitrate of baryta, 0.09 mmol ytterbium nitrate and 0.01 mmol thulium nitrate are joined 10 mL deionized waters, after stirring the transparent settled solution of formation, dropwise join in the mixed solution of 10 mL ethanol, 10 mL oleic acid and 2.5 g sodium oleates, be moved in the 40 mL water heating kettles after fully stirring, be added dropwise to subsequently hydrofluoric acid aqueous solution 4 mL of 1.0 mol/L, carry out solvent thermal reaction at last under 160 ℃ of temperature, soaking time is 12 hours.Gained is nanocrystalline with after ethanol and the washing of hexanaphthene mixed solution, after 60 ℃ of oven dry, obtain Yb/Tm:BaF
2Examine nanocrystalline.With the Yb/Tm:BaF that obtains
2Examine nanocrystalline, 0.40 mmol trifluoroacetic acid strontium Sr (CF
3COO)
2, 0.09 mmol trifluoroacetic acid gadolinium Gd (CF
3COO)
3With 0.01mmol trifluoroacetic acid neodymium Nd (CF
3COO)
3Join in 10 mL oleic acid and the 10 mL octadecylenes; be moved in the 100 mL three-necked bottles after stirring the transparent settled solution of formation; under nitrogen atmosphere protection, be heated to subsequently 100 ℃ and be incubated the deoxygenation that dewaters in 30 minutes, under the nitrogen atmosphere protection, continue to be heated to 280 ℃ at last, and be incubated 3 hours.After products therefrom usefulness ethanol and the washing of hexanaphthene mixed solution, after 60 ℃ of oven dry, obtain extra small (～7 nanometer) Yb/Tm:BaF
2@Gd/Nd:SrF
2Nano-crystal with core-shell structure.Spectrum test shows that institute obtains that nanocrystalline to produce near infrared-near infrared bimodulus luminous.
Example 3: 0.40 mmol nitrate of baryta, 0.09 mmol ytterbium nitrate and 0.01 mmol thulium nitrate are joined 10 mL deionized waters, after stirring the transparent settled solution of formation, dropwise join in the mixed solution of 10 mL ethanol, 10 mL oleic acid and 2.5 g sodium oleates, be moved in the 40 mL water heating kettles after fully stirring, be added dropwise to subsequently hydrofluoric acid aqueous solution 4 mL of 1.0 mol/L, carry out solvent thermal reaction at last under 160 ℃ of temperature, soaking time is 12 hours.Gained is nanocrystalline with after ethanol and the washing of hexanaphthene mixed solution, after 60 ℃ of oven dry, obtain Yb/Tm:BaF
2Examine nanocrystalline.With the Yb/Tm:BaF that obtains
2Examine nanocrystalline, 0.40 mmol trifluoroacetic acid strontium Sr (CF
3COO)
2, 0.09 mmol trifluoroacetic acid gadolinium Gd (CF
3COO)
3With 0.01mmol trifluoroacetic acid neodymium Nd (CF
3COO)
3Join in 10 mL oleic acid and the 10 mL octadecylenes; be moved in the 100 mL three-necked bottles after stirring the transparent settled solution of formation; under nitrogen atmosphere protection, be heated to subsequently 100 ℃ and be incubated the deoxygenation that dewaters in 30 minutes, under the nitrogen atmosphere protection, continue to be heated to 310 ℃ at last, and be incubated 1 hour.After products therefrom usefulness ethanol and the washing of hexanaphthene mixed solution, after 60 ℃ of oven dry, obtain extra small (～7 nanometer) Yb/Tm:BaF
2@Gd/Nd:SrF
2Nano-crystal with core-shell structure.Spectrum test shows that institute obtains that nanocrystalline to produce near infrared-near infrared bimodulus luminous.
Example 4: 0.40 mmol nitrate of baryta, 0.09 mmol ytterbium nitrate and 0.01 mmol thulium nitrate are joined 10 mL deionized waters, after stirring the transparent settled solution of formation, dropwise join in the mixed solution of 10 mL ethanol, 10 mL oleic acid and 2.5 g sodium oleates, be moved in the 40 mL water heating kettles after fully stirring, be added dropwise to subsequently hydrofluoric acid aqueous solution 4 mL of 1.0 mol/L, carry out solvent thermal reaction at last under 160 ℃ of temperature, soaking time is 12 hours.Gained is nanocrystalline with after ethanol and the washing of hexanaphthene mixed solution, after 60 ℃ of oven dry, obtain Yb/Tm:BaF
2Examine nanocrystalline.With the Yb/Tm:BaF that obtains
2Examine nanocrystalline, 0.40 mmol trifluoroacetic acid strontium Sr (CF
3COO)
2, 0.09 mmol trifluoroacetic acid lanthanum La (CF
3COO)
3With 0.01mmol trifluoroacetic acid neodymium Nd (CF
3COO)
3Join in 10 mL oleic acid and the 10 mL octadecylenes; be moved in the 100 mL three-necked bottles after stirring the transparent settled solution of formation; under nitrogen atmosphere protection, be heated to subsequently 100 ℃ and be incubated the deoxygenation that dewaters in 30 minutes, under the nitrogen atmosphere protection, continue to be heated to 280 ℃ at last, and be incubated 3 hours.After products therefrom usefulness ethanol and the washing of hexanaphthene mixed solution, after 60 ℃ of oven dry, obtain extra small (～7 nanometer) Yb/Tm:BaF
2@La/Nd:SrF
2Nano-crystal with core-shell structure.Spectrum test shows that institute obtains that nanocrystalline to produce near infrared-near infrared bimodulus luminous.
Example 5: 0.40 mmol nitrate of baryta, 0.09 mmol ytterbium nitrate and 0.01 mmol thulium nitrate are joined 10 mL deionized waters, after stirring the transparent settled solution of formation, dropwise join in the mixed solution of 10 mL ethanol, 10 mL oleic acid and 2.5 g sodium oleates, be moved in the 40 mL water heating kettles after fully stirring, be added dropwise to subsequently hydrofluoric acid aqueous solution 4 mL of 1.0 mol/L, carry out solvent thermal reaction at last under 160 ℃ of temperature, soaking time is 12 hours.Gained is nanocrystalline with after ethanol and the washing of hexanaphthene mixed solution, after 60 ℃ of oven dry, obtain Yb/Tm:BaF
2Examine nanocrystalline.With the Yb/Tm:BaF that obtains
2Examine nanocrystalline, 0.40 mmol trifluoroacetic acid strontium Sr (CF
3COO)
2, 0.09 mmol trifluoroacetic acid lutetium Lu (CF
3COO)
3With 0.01mmol trifluoroacetic acid neodymium Nd (CF
3COO)
3Join in 10 mL oleic acid and the 10 mL octadecylenes; be moved in the 100 mL three-necked bottles after stirring the transparent settled solution of formation; under nitrogen atmosphere protection, be heated to subsequently 100 ℃ and be incubated the deoxygenation that dewaters in 30 minutes, under the nitrogen atmosphere protection, continue to be heated to 280 ℃ at last, and be incubated 3 hours.After products therefrom usefulness ethanol and the washing of hexanaphthene mixed solution, after 60 ℃ of oven dry, obtain extra small (～7 nanometer) Yb/Tm:BaF
2@Lu/Nd:SrF
2Nano-crystal with core-shell structure.Spectrum test shows that institute obtains that nanocrystalline to produce near infrared-near infrared bimodulus luminous.
Claims (1)
1. nanocrystalline preparation method of extra small nucleocapsid structure alkaline earth fluoride with near infrared-near infrared bimodulus characteristics of luminescence, the method comprises the steps:
(1) 0.40 mmol barium ion salt, 0.09 mmol ytterbium ion salt and 0.01 mmol thulium ion salt are joined 10 mL deionized waters, after stirring the transparent settled solution of formation, dropwise join in the mixed solution of 10 mL ethanol, 10 mL oleic acid and 2.5 g sodium oleates, be moved in the 40 mL water heating kettles after fully stirring, be added dropwise to subsequently hydrofluoric acid aqueous solution 4 mL of 1.0 mol/L, carry out solvent thermal reaction at last under 160 ℃ of temperature, the reaction times is 12 hours.After products therefrom usefulness ethanol and the washing of hexanaphthene mixed solution, after 40-80 ℃ of oven dry, obtain examining nanocrystalline.
(2) with step (1) Yb/Tm:BaF that obtains
2Examine nanocrystalline, 0.40 mmol Sr (CF
3COO)
2, 0.09 mmol Ln (CF
3COO)
3(wherein Ln can be any element among La, Ce, Pr, Sm, Eu, Gd, Y, Tb, Dy, Ho, Er, Tm, Yb or the Lu) and 0.01 mmol Nd (CF
3COO)
3Join in 10 mL oleic acid and the 10 mL octadecylenes; be moved in the 100 mL three-necked bottles after stirring the transparent settled solution of formation; under inert atmosphere protection, be heated to subsequently 100 ℃ and be incubated the deoxygenation that dewaters in 30 minutes; under inert atmosphere protection, continue to be heated to 260-310 ℃ at last, and be incubated 1-6 hour and react.After products therefrom usefulness ethanol and the washing of hexanaphthene mixed solution, after 40-80 ℃ of oven dry, obtain nano-crystal with core-shell structure.
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| CN103224787A (en) * | 2013-04-19 | 2013-07-31 | 中国科学院福建物质结构研究所 | Rare earth-doped alkaline earth metal fluoride nano material, and preparation method and application thereof |
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| CN103224787A (en) * | 2013-04-19 | 2013-07-31 | 中国科学院福建物质结构研究所 | Rare earth-doped alkaline earth metal fluoride nano material, and preparation method and application thereof |
| CN103224787B (en) * | 2013-04-19 | 2017-12-12 | 中国科学院福建物质结构研究所 | Rear-earth-doped alkali earth metal fluoride nano material and its preparation and application |
| CN103305222A (en) * | 2013-06-18 | 2013-09-18 | 南京大学 | KSc2F7: yb, preparation method and application of Er up-conversion fluorescent nanorods |
| CN103305222B (en) * | 2013-06-18 | 2014-11-26 | 南京大学 | KSc2F7: yb, preparation method and application of Er up-conversion fluorescent nanorods |
| CN104250554A (en) * | 2013-06-28 | 2014-12-31 | 长春理工大学 | Neodymium-doped barium fluoride nano powder luminescent material |
| CN104250553A (en) * | 2013-06-28 | 2014-12-31 | 长春理工大学 | Preparation method for neodymium-doped barium fluoride nano-material |
| CN104109531A (en) * | 2014-06-23 | 2014-10-22 | 北京大学 | Core-shell structure rare earth light-emitting nano material and preparation method |
| CN105802627A (en) * | 2016-04-29 | 2016-07-27 | 华南师范大学 | Composite nano material capable of exciting upconversion steady persistence through near-infrared light and preparation thereof |
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| CN107903899A (en) * | 2017-12-21 | 2018-04-13 | 内蒙古师范大学 | A kind of ytterbium erbium is co-doped with KGdF4The synthetic method of nano particle and nanobelt |
| CN112457849A (en) * | 2020-12-15 | 2021-03-09 | 中国计量大学 | Near-infrared fluoride core-shell nanocrystalline scintillator |
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