CN106957654B - It is a kind of to prepare 8 nanometers or less rare-earth doped beta-NaYF4The method of upper conversion nano crystalline substance - Google Patents
It is a kind of to prepare 8 nanometers or less rare-earth doped beta-NaYF4The method of upper conversion nano crystalline substance Download PDFInfo
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 43
- 239000000126 substance Substances 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 16
- 229910052761 rare earth metal Inorganic materials 0.000 title claims description 19
- 150000002910 rare earth metals Chemical class 0.000 title claims description 18
- 229910003366 β-NaYF4 Inorganic materials 0.000 claims abstract description 21
- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 13
- 229910052689 Holmium Inorganic materials 0.000 claims abstract description 13
- 229910052775 Thulium Inorganic materials 0.000 claims abstract description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 17
- 229910052786 argon Inorganic materials 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 12
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 7
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 6
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 6
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 6
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000005642 Oleic acid Substances 0.000 claims description 6
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 6
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 6
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000643 oven drying Methods 0.000 claims description 6
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 2
- -1 rare earth compound Chemical class 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 12
- 230000006911 nucleation Effects 0.000 abstract description 7
- 238000010899 nucleation Methods 0.000 abstract description 7
- 239000003446 ligand Substances 0.000 abstract description 6
- 230000035484 reaction time Effects 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 10
- 238000004020 luminiscence type Methods 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7772—Halogenides
- C09K11/7773—Halogenides with alkali or alkaline earth metal
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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Abstract
The present invention, which discloses, a kind of prepares 8 nanometers or less β-NaYF4:Yb3+,RE3+The method of conversion nano crystalline substance on (RE=Tm, Er, Ho) accelerates the nucleation rate of β phase by introducing enuatrol ligand during the preparation process and efficiently promotes ɑ-NaYF4To β-NaYF4Transformation, so as to be effectively reduced obtain pure phase β-NaYF4:Yb3+,RE3+The reaction time of conversion nano crystalline substance and reaction temperature on (RE=Tm, Er, Ho).β-NaYF prepared by this method4:Yb3+,RE3+Conversion nano crystalline substance size small (4-8nm), good dispersion on (RE=Tm, Er, Ho), without miscellaneous phase (ɑ-NaYF4), preparation method is simple and repeatability is high, have broad application prospects.
Description
Technical field
The present invention relates to the preparation of rear-earth-doped upper conversion nano crystalline substance, specially it is a kind of prepare 8 nanometers or less it is rear-earth-doped
β-NaYF4The method of upper conversion nano crystalline substance, especially a kind of scale are less than the β-NaYF of 8nm4:Yb3+, RE3+(RE=Tm, Er,
Ho the preparation method of conversion nano crystalline substance on).
Background technique
Up-conversion luminescence is the anti-Stokes process for absorbing multiple lower energy photons and emitting a high-energy photon, up-conversion luminescence
Material is a kind of luminescent material that near infrared light can be converted into visible light.Due to having very low phonon energy, β-
NaYF4It is widely regarded as can be realized one of most effective host material of efficient up-conversion luminescence.α-is free of in order to obtain
NaYF4Pure phase β-the NaYF of miscellaneous phase4, the preparation of sample needs higher reaction temperature and longer reaction time, or even needs
It is carried out under high pressure.These synthesis conditions necessarily will increase the reunion between the size of particle, or even aggravation particle, therefore at present
β-the NaYF having been reported that4The size of particle is mostly in 10nm or more.And upper conversion nano crystalline substance should be wanted in biologic medical field
It asks its size very small (< 10nm), is easier to be attached to targeted molecular or cell surface in this way, conducive to accurately detecting and being easier to
It excretes to reduce the damage to cell.Therefore, monodisperse and super-small β-NaYF how simply to be prepared4It is nanocrystalline to become
It is restricted in an important bottleneck of biological field application.
Super-small β-NaYF is prepared at present4Nanocrystalline there are two types of methods, one is increasing the nucleation rate of β phase seed.
If β phase seed amount increases, under conditions of certain presoma, the growth rate of core is limited, this
Sample is conducive to synthesize small size β-NaYF4It is nanocrystalline.Shao et al. and Haase et al. are respectively in a high proportion of oleic acid with before
Drive body and a high proportion of Na+And Y3+Under conditions of synthesized the β-NaYF of 11.86nm and 5nm4It is nanocrystalline, but α-simultaneously
NaYF4Particle also constantly can be nucleated and grow.The second is reducing ɑ phase transition is the energy barrier crossed over required for β phase.In such case
Under, β phase can be prepared in relatively lower temp and in short period under conditions of.Cohen et al. has found in preparation process
Middle a certain amount of oleyl amine of addition can also prepare super-small β-NaYF4:Yb3+,Er3+It is nanocrystalline, because it can not only promote
Into the transformation of the opposite β phase of ɑ, and nucleation rate can be promoted.But a small amount of α-NaYF is still had in final product4。
Therefore, small size (being less than 10nm) β-NaYF is synthesized at present4Nanocrystalline method all can not effectively avoid α-NaYF4The life of miscellaneous phase
At.
Summary of the invention
The present invention provides the β-NaYF that especially a kind of scale is less than 8nm4:Yb3+, RE3+Turn on (RE=Tm, Er, Ho)
The preparation method for changing luminescence nanocrystalline can accelerate β-NaYF by introducing enuatrol ligand (NaOA) during the preparation process4's
Nucleation rate is efficiently promoting ɑ-NaYF4To β-NaYF4Transformation, thus obtain scale be less than 8nm monodispersed pure phase β-
NaYF4:Yb3+,RE3+It is nanocrystalline.
The invention is realized by the following technical scheme:
It is proposed by the present invention a kind of to prepare 8 nanometers or less rare-earth doped beta-NaYF4The method of upper conversion nano crystalline substance, it is described dilute
Soil doping β-NaYF4Upper conversion nano crystalline substance is β-NaYF4: xYb3+,y RE3+Upper conversion nano is brilliant, and the RE is Tm, Er and Ho,
By mole meter, 0 < x≤30%, 0 < y≤10%, the specific steps are as follows:
(1) rare earth particle MCl is weighed in proportion3·6H2O, M (Ac)3·nH2O or M (CF3COO)3, (M=Y, Yb and RE),
Oleic acid and l- octadecene solution is added, under protection of argon gas, 100 ~ 160 DEG C are heated with stirring to, and keep the temperature 10 ~ 60min, to rare earth
After particle is completely dissolved, cooled to room temperature；
It (2) successively will be respectively dissolved with enuatrol and NH4The methanol solution of F is added dropwise to reaction system obtained by step (1)
In, 50 ~ 70 DEG C are heated with stirring to, and keep the temperature, until methanol completely removes；
(3) under protection of argon gas, step (2) acquired solution is heated with stirring to 240 ~ 300 DEG C, and keeps the temperature 0 ~ 120min,
Cooled to room temperature later；
(4) step (3) products therefrom is centrifuged using centrifuge, then clean repeatedly with hexamethylene-ethyl alcohol with
After centrifugation three times, be finally dispersed in hexamethylene or in an oven drying it is dry to get to 8 nanometers or less β-NaYF4:Yb3+,
RE3+Upper conversion nano is brilliant.
In the present invention, oleic acid functions as surfactant and high boiling solvent, and l- octadecylene functions as
High boiling solvent.
In the present invention, the effect of enuatrol is the nucleation rate for accelerating β phase, while can be efficiently promoting ɑ-NaYF4It arrives
β-NaYF4Transformation.
A kind of β-NaYF prepared less than 8nm of the present invention4:Yb3+, RE3+Conversion nano crystalline substance on (RE=Tm, Er, Ho)
Method introduces enuatrol ligand (NaOA) during the preparation process.Its role is to the presence of NaOA ligand to be not only able to accelerate
The nucleation rate of β phase, while ɑ-NaYF can be efficiently promoting4To β-NaYF4Transformation, thus be conducive to synthesize small size β-
NaYF4:Yb3+, RE3+Conversion nano is brilliant on (RE=Tm, Er, Ho).NaOH is used to obtain as the method in the source Na tradition
Obtain pure phase rare-earth doped beta-NaYF4It needs in 300 DEG C of reactions at least 30min, obtained rare-earth doped beta-NaYF4Nanocrystalline scale
Greater than 20nm.And the method for using this patent, when reaction temperature is 300 DEG C, the reaction time can foreshorten to from 30min
0min, the β-NaYF of acquisition4:Yb3+, RE3+(RE=Tm, Er, Ho) nanocrystalline scale is 7.0nm.
The present invention provides not only a kind of simple and quick monodispersed super-small pure phase β-NaYF of synthesis4:Yb3+, RE3+
The method of conversion nano crystalline substance on (RE=Tm, Er, Ho), it is often more important that realize upper conversion hair by preparing core-shell structure
The enhancing of light provides smaller size of possibility.Using the synthetic method of this patent, as β-NaYF4:Yb3+,Er3+@NaYF4Nucleocapsid
When the size of structure is 9nm, Up-conversion Intensity can achieve the β-using the size of conventional method acquisition for 23nm
NaYF4:Yb3+,Er3+Intensity.
The beneficial effects of the present invention are:
The present invention provides the β-NaYF that a kind of quick and easy preparation is less than 8nm4:Yb3+, RE3+(RE=Tm, Er, Ho)
The method of upper conversion nano crystalline substance, i.e., introduce enuatrol ligand (NaOA) during the preparation process, and the effect of NaOA ligand is not only
It can speed up the nucleation rate of β phase, while ɑ-NaYF can be efficiently promoting4To β-NaYF4Transformation, thus can be lower
Pure phase β-the NaYF of small size is obtained in reaction temperature and shorter reaction time4:Yb3+, RE3+(RE=Tm, Er, Ho) nanometer
Crystalline substance, and preparation method repeatability is high.
Detailed description of the invention
Fig. 1 is the XRD diagram of 1 gained sample of the embodiment of the present invention.
Fig. 2 is that the TEM of 1 gained sample of the embodiment of the present invention schemes.
Fig. 3 is that the TEM of 2 gained sample of the embodiment of the present invention schemes.
Fig. 4 is that the TEM of 3 gained sample of the embodiment of the present invention schemes.
Fig. 5 is that the TEM of 4 gained sample of the embodiment of the present invention schemes.
Fig. 6 is up-conversion luminescence spectrogram of the 4 gained sample of the embodiment of the present invention under 980nm excitation.
Specific embodiment
The present invention will be further explained with reference to the examples below.
Embodiment 1:
(1) firstly, weighing rare earth 1mmol RECl3·6H26mL oleic acid is added in O (Y:Yb:Er=80:18:2, molar ratio)
In 15mLl- octadecene solution.Under protection of argon gas, 150 DEG C are heated with stirring to and keeps the temperature 30min, it is completely molten to rare earth particle
Xie Hou, cooled to room temperature.
It (2) then, successively will be respectively dissolved with 2.5mmol enuatrol and 4mmol NH4The 10mL methanol solution of F is added dropwise
Into reaction system, it is heated with stirring to 60 DEG C and keeps the temperature 60min.
(3) then, solution under protection of argon gas, is heated with stirring to 300 DEG C, and keeps the temperature 0min, is naturally cooled to later
Room temperature.
(4) it is centrifuged using centrifuge, then after being cleaned and be centrifuged three times repeatedly with hexamethylene-ethyl alcohol, finally divided
It is dispersed in hexamethylene or dries in an oven drying.
(5) this experiment condition can get the pure phase β-NaYF that evenly dispersed size is 7.0 nm4:Yb3+, Er3+Upper conversion
Luminescence nanocrystalline.
Embodiment 2:
(1) firstly, weighing rare earth 1mmol RE (Ac)3·nH26mL oil is added in O (Y:Yb:Tm=78:18:4, molar ratio)
In acid and 15mLl- octadecene solution.Under protection of argon gas, 140 DEG C are heated with stirring to and keeps the temperature 30min, it is complete to rare earth particle
After dissolution, cooled to room temperature.
It (2) then, successively will be respectively dissolved with 2.5mmol enuatrol and 4mmol NH4The 10mL methanol solution of F is added dropwise
Into reaction system, it is heated with stirring to 50 DEG C and keeps the temperature 60min.
(3) then, solution under protection of argon gas, is heated with stirring to 260 DEG C, and keeps the temperature 30min, is naturally cooled to later
Room temperature.
(4) it is centrifuged using centrifuge, then after being cleaned and be centrifuged three times repeatedly with hexamethylene-ethyl alcohol, finally divided
It is dispersed in hexamethylene or dries in an oven drying.
(5) this experiment condition can get the pure phase β-NaYF that evenly dispersed size is 5.1 nm4:Yb3+, Tm3+Upper conversion
Luminescence nanocrystalline.
Embodiment 3:
(1) firstly, weighing rare earth 1mmol RECl3·6H26mL oleic acid is added in O (Y:Yb:Ho=75:20:5, molar ratio)
In 15mLl- octadecene solution.Under protection of argon gas, 155 DEG C are heated with stirring to and keeps the temperature 30min, it is complete to rare earth particle
After dissolution, cooled to room temperature.
It (2) then, successively will be respectively dissolved with 2.5mmol enuatrol and 4mmol NH4The 10mL methanol solution of F is added dropwise
Into reaction system, it is heated with stirring to 60 DEG C and keeps the temperature 60min.
(3) then, solution under protection of argon gas, is heated with stirring to 290 DEG C, and keeps the temperature 5min, is naturally cooled to later
Room temperature.
(4) it is centrifuged using centrifuge, then after being cleaned and be centrifuged three times repeatedly with hexamethylene-ethyl alcohol, finally divided
It is dispersed in hexamethylene or dries in an oven drying.
(5) this experiment condition can get the pure phase β-NaYF that evenly dispersed size is 7.8nm4:Yb3+, Ho3+Upper conversion
Luminescence nanocrystalline.
Embodiment 4:
(1) firstly, weighing rare earth 1mmol RECl3·6H26mL oleic acid is added in O (Y:Yb:Er=78:18:4, molar ratio)
In 15mLl- octadecene solution.Under protection of argon gas, 145 DEG C are heated with stirring to and keeps the temperature 30min, it is complete to rare earth particle
After dissolution, cooled to room temperature.
It (2) then, successively will be respectively dissolved with 2.5mmol enuatrol and 4mmol NH4The 10mL methanol solution of F is added dropwise
Into reaction system, it is heated with stirring to 60 DEG C and keeps the temperature 60min.
(3) then, solution under protection of argon gas, is heated with stirring to 240 DEG C, and keeps the temperature 120min, later natural cooling
To room temperature.
(4) it is centrifuged using centrifuge, then after being cleaned and be centrifuged three times repeatedly with hexamethylene-ethyl alcohol, finally divided
It is dispersed in hexamethylene or dries in an oven drying.
(5) this experiment condition can get the pure phase β-NaYF that evenly dispersed size is 6.6nm4:Yb3+, Er3+Upper conversion
Luminescence nanocrystalline.
Claims (1)
1. a kind of prepare 8 nanometers or less rare-earth doped beta-NaYF4The method of upper conversion nano crystalline substance, it is characterised in that the rare earth is mixed
Miscellaneous β-NaYF4Upper conversion nano crystalline substance is β-NaYF4: xYb3+,y RE3+Upper conversion nano is brilliant, and the RE is Tm, Er and Ho, massage
That percentages, 0 < x≤30%, 0 < y≤10%, the specific steps are as follows:
(1) rare earth compound MCl is weighed in proportion3·6H2O, M (Ac)3·nH2O or M (CF3COO)3, M Y, Yb and RE add
Enter oleic acid and l- octadecene solution, under protection of argon gas, 100 ~ 160 DEG C is heated with stirring to, and keep the temperature 10 ~ 60min, to rare earth
After grain is completely dissolved, cooled to room temperature；
It (2) successively will be respectively dissolved with enuatrol and NH4The methanol solution of F is added dropwise in reaction system obtained by step (1), is stirred
It mixes and is heated to 50 ~ 70 DEG C, and keep the temperature, until methanol completely removes；
(3) under protection of argon gas, step (2) acquired solution is heated with stirring to 240 ~ 300 DEG C, and keeps the temperature 0 ~ 120min, later
Cooled to room temperature；
(4) step (3) products therefrom is centrifuged using centrifuge, then is cleaned and be centrifuged repeatedly with hexamethylene-ethyl alcohol
After three times, be finally dispersed in hexamethylene or in an oven drying it is dry to get to 8 nanometers or less β-NaYF4:Yb3+, RE3+On
Conversion nano is brilliant.
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| CN110408377B (en) * | 2018-04-27 | 2021-07-20 | 中国科学院福建物质结构研究所 | Rare earth doped NaCeF4Near-infrared fluorescent nano probe and preparation method and biological application thereof |
| CN108557861A (en) * | 2018-05-28 | 2018-09-21 | 合肥国轩高科动力能源有限公司 | NaYF is converted in one kind4The preparation method of nano-powder self-assembled film |
| CN108982440A (en) * | 2018-06-10 | 2018-12-11 | 福建医科大学 | The upper building for converting faint photodetector and its detection for glutathione |
| CN111117617B (en) * | 2019-12-31 | 2021-07-06 | 同济大学 | Tungstate-based up-conversion luminescence temperature sensing material and preparation method thereof |
| CN111747652B (en) * | 2020-03-27 | 2021-05-11 | 同济大学 | Mesoporous bioactive glass composite material with up-conversion luminescence property and preparation method thereof |
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Non-Patent Citations (1)
| Title |
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| Bright dual-mode green emission from selective set of dopant ions in β-Na(Y,Gd)F4:Yb,Er/β-NaGdF4:Ce,Tb core/shell nanocrystals;Ho Seong Jang等;《OPTICS EXPRESS》;20120712;第20卷(第15期);17107-17118 * |
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