CN108467734A - Quickly prepare not jljl phase NaYF4The method and up-conversion of up-conversion - Google Patents
Quickly prepare not jljl phase NaYF4The method and up-conversion of up-conversion Download PDFInfo
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- 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
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Abstract
Quickly prepare not jljl phase NaYF4The method and up-conversion of up-conversion, belong to up-conversion technical field.Method includes：To dissolved with Y3+、Yb3+And Er3+Initial soln in be mixed into sodium citrate, obtain complex solution.It is mixed into ethanol amine into complex solution, obtains precursor solution.It is mixed into precursor solution containing F‑Salt, adjust pH value be 1 10, obtain colloidal solution.Colloidal solution is placed in autoclave, 40 60min are heated under the conditions of 160 180 DEG C.Simple for process, crystalline phase is controllably, repeatability is strong, the period is short, NaYF obtained4Up-conversion pattern is uniform, luminous intensity is high.NaYF4Up-conversion is made according to the above method, and pattern is uniform, and has high luminous intensity.
Description
Technical field
The present invention relates to up-conversion technical fields, and not jljl phase NaYF is quickly prepared in particular to a kind of4On
The method and up-conversion of transition material.
Background technology
Up-conversion luminescence is realized by absorbing two or more low energy near infrared light long wavelength photons
The anti-Stokes process of one short VISIBLE LIGHT EMISSION.It is proposed for the first time from nineteen fifty-nine Bloembergen N. notional infrared
Quantum counter device so far, up-conversion luminescent material sensor, optical dynamic therapy, solar cell, biomarker and at
The fields such as picture show potential application value.
Yttrium fluoride natrium (NaYF4) it is generally acknowledged at present one of the host material with efficient up-conversion luminescence, there are six sides
Phase and cubic phase two kinds of crystal forms, rear-earth-doped hexagonal phase NaYF4The luminous intensity of up-conversion is vertical higher than identical doping
Square phase NaYF4One to two orders of magnitude, therefore efficiently quickly control prepares not jljl phase NaYF4Up-conversion has important meaning
Justice.
In the prior art, NaYF4The preparation method of up-conversion mainly has：Organic thermal decomposition method, high temperature solid-state method, water
Hot method of hot solvent etc..Organic thermal decomposition method generally uses expensive organic metal salt and high boiling organic solvent and surface-active
It is reacted at relatively high temperatures in the protection of agent inert gas, the method reaction solution needs anhydrous and oxygen-free to pre-process, after product
Phase processing is cumbersome, and cost of material is higher.High temperature solid-state method is also commonly used to prepare rear-earth-doped NaYF4Upper conversion material
Material, but its material morphology prepared is uncontrollable and reaction temperature is high.Although the luminescent properties of its sample of hydro-thermal solvent-thermal method are good
It is good, but hydro-thermal reaction especially prepares hexagonal phase NaYF4The period of up-conversion is long.Therefore using straightforward procedure, ultrafast
Speed prepares not jljl and is mutually especially hexagonal phase NaYF4Up-conversion improves production efficiency, has important application value.
In view of this, special propose the application.
Invention content
Not jljl phase NaYF is quickly prepared the purpose of the present invention is to provide a kind of4The method of up-conversion, technique
Simply, crystalline phase is controllable, repeatability is strong, the period is short, NaYF obtained4Up-conversion pattern is uniform, luminous intensity is high.
Another object of the present invention is to provide a kind of NaYF4Up-conversion, pattern is uniform, and has light intensity occurred frequently
Degree.
What the embodiment of the present invention was realized in：
It is a kind of quickly to prepare not jljl phase NaYF4The method of up-conversion, including：To dissolved with Y3+、Yb3+And Er3+Just
It is mixed into sodium citrate in beginning solution, obtains complex solution；It is mixed into ethanol amine into complex solution, obtains precursor solution；To presoma
It is mixed into containing F in solution-Salt, adjusting pH value be 1-10, obtain colloidal solution；Colloidal solution is placed in autoclave, in
40-60min is heated under the conditions of 160-180 DEG C.
A kind of NaYF4Up-conversion, according to above-mentioned quick preparation not jljl phase NaYF4The method system of up-conversion
.
The advantageous effect of the embodiment of the present invention is：
Quick preparation provided by the invention not jljl phase NaYF4The method of up-conversion passes through hydro-thermal normal direction NaYF4In
Adulterate yttrium, ytterbium and erbium, obtained NaYF4Up-conversion pattern is uniform, luminescent properties are good.This method does not need atmosphere guarantor
Shield, it is simple for process；By state modulators crystalline phases such as the pH that simply adjusts colloidal solution, repeatability is strong.Add in precursor solution
There is ethanol amine, contributes to form a kind of similar to NaYF4Cubic phase intermediate product makes rapid reaction carry out in 40-60min i.e.
It can complete, it is with short production cycle.Suitable for large-scale production.
Phase NaYF provided by the invention4Up-conversion, according to above-mentioned quick preparation not jljl phase NaYF4Upper conversion material
The method of material is made, and it is uniform to have a pattern, and has the advantages that high luminous intensity.
Description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is NaYF made from the embodiment of the present invention 14The scanning electron microscope diagram of up-conversion；
Fig. 2 is NaYF made from the embodiment of the present invention 14Upper conversion hair of the up-conversion under the excitation of 980 nanometer lasers
Light spectrogram；
Fig. 3 is NaYF made from the embodiment of the present invention 14The XRD spectrum of up-conversion；
Fig. 4 is NaYF made from the embodiment of the present invention 24The scanning electron microscope diagram of up-conversion；
Fig. 5 is NaYF made from the embodiment of the present invention 24Upper conversion hair of the up-conversion under the excitation of 980 nanometer lasers
Light spectrogram；
Fig. 6 is NaYF made from the embodiment of the present invention 34The scanning electron microscope diagram of up-conversion；
Fig. 7 is NaYF made from the embodiment of the present invention 34The XRD spectrum of up-conversion.
Specific implementation mode
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Prepared by not jljl phase NaYF to the quick of the embodiment of the present invention below4The method and up-conversion of up-conversion
It is specifically described.
The present invention provides one kind and quickly preparing not jljl phase NaYF4The method of up-conversion, including：To dissolved with Y3+、Yb3+
And Er3+Initial soln in be mixed into sodium citrate, obtain complex solution；It is mixed into ethanol amine into complex solution, obtains precursor solution；
It is mixed into precursor solution containing F-Salt, adjusting pH value be 1-10, obtain colloidal solution；Colloidal solution is placed in autoclave
In, 40-60min is heated under the conditions of 160-180 DEG C.
In this method, pass through hydro-thermal normal direction NaYF4Middle doping yttrium, ytterbium and erbium, so as to get NaYF4Up-conversion pattern
It is uniform, luminescent properties are good.
In some specific embodiments of the invention, Y3+It is provided by ytterbium nitrate, Yb3+It is provided by yttrium nitrate, Er3+By nitre
Sour erbium provides.When initial soln configures, a certain amount of yttrium nitrate, ytterbium nitrate and erbium nitrate are dissolved in the water.
In other embodiments of the invention, Y3+、Yb3+And Er3+It can also be provided respectively by respective chloride.Specifically
Ground is Y3+By ytterbium chloride offer soluble in water, Yb3+By yttrium chloride offer soluble in water, Er3+By erbium chloride offer soluble in water.
Further, in order to make NaYF4Up-conversion has preferably optical property, Y3+、Yb3+And Er3+Molar ratio
For 78-88:10-20:2, such as 78:20:2、82:16:2、85:13:2、88:10:2 etc..Preferably, it is 78:20:2.
Preferably, in the initial soln, Y3+、Yb3+And Er3+Total mol concentration be 0.1-0.2mol/L, such as
0.1mol/L, 0.12mol/L, 0.14mol/L, 0.16mol/L, 0.18mol/L, 0.2mol/L etc..Preferably, it is 0.1mol/
L。
Sodium citrate is mixed into initial soln, is on the one hand NaYF4The synthesis of up-conversion provides sodium source, on the other hand with
Y3+、Yb3+And Er3+Coordination.
In order to make sodium citrate be fully complexed with initial soln, in operating process, in the magnetic agitation of 600-1500r/min
It is lower that sodium citrate is added into the initial soln, stir substantially 5min.
Further, initial concentration when sodium citrate is dissolved in initial soln is preferably 0.1-0.2mol/L, such as
0.1mol/L, 0.12mol/L, 0.14mol/L, 0.16mol/L, 0.18mol/L, 0.2mol/L etc., it is therefore preferable to 0.1mol/L.
The mole of the sodium citrate：Y3+、Yb3+And Er3+Moles total number be 1-2:1-2.
Through inventor the study found that being mixed into ethanol amine into complex solution, contribute to form a kind of similar to NaYF4Cube
Phase intermediate product makes rapid reaction progress can be completed in 40-60min, significantly shortens the production cycle.
The volume ratio of complex solution and ethanol amine is preferably 5-10:1, such as 5:1、6:1、7:1、8:1、9:1、10:1 etc..
In the operating process that the precursor solution is prepared, under the magnetic agitation of 600-1500r/min, in proportion by ethyl alcohol
Amine is added in complex solution, reacts 1-5min.
Containing F-Salt be NaYF4The synthesis of up-conversion provides Fluorine source, in some preferred embodiments of the invention, contains
There is F-Salt selection ammonium fluoride, sodium fluoride etc..
Further, contain F-Salt in F-Mole：Y3+、Yb3+And Er3+Moles total number be preferably 12-24:1, such as
12:1、14:1、16:1、18:1、20:1、22:1、24:1 etc..
In order to make to contain F-Salt be sufficiently mixed and react with precursor solution, in operating process, in the magnetic of 600-1500r/min
Under power stirring, F will be contained in proportion-Salt be added precursor solution in, react 1-5min.
It is added in precursor solution and contains F-Salt after, as needed adjust pH value be 1-10, obtain the NaYF of different crystalline phases4
Up-conversion.
Method provided by the invention does not need atmosphere protection, simple for process；By the pH etc. for simply adjusting colloidal solution
State modulator crystalline phase, repeatability are strong.Reaction can be completed in 40-60min, with short production cycle.Suitable for large-scale production.
In preferred embodiments of the present invention, the adjusting of colloidal solution pH value is carried out using hydrochloric acid.Due to being added in reaction
Ethanol amine adjusts the process for avoiding ethanol amine from being influenced reaction by oxidation using hydrochloric acid.
Obtained product is washed after the completion of hydro-thermal reaction, is specifically included：After reaction kettle is cooled to room temperature, centrifugation
Separation will centrifuge obtained product absolute ethyl alcohol and be dried under the conditions of water supersound washing 3 times, 80 DEG C, obtains NaYF4Upper conversion
Material.
The present invention also provides a kind of NaYF4Up-conversion, according to the above method be made, have production it is simple and quick can
Control, pattern is uniform, has the advantages that high luminous intensity.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
It is a kind of quickly to prepare not jljl phase NaYF4The method of up-conversion, including：
By Y3+:Yb3+:Er3+Molar ratio be 78:20:2 yttrium nitrates, ytterbium nitrate, erbium nitrate for weighing 1mmol are dissolved in
Initial soln is formed in 10mL water.1mmol sodium citrates, stirring is added into initial soln under the magnetic agitation of 600r/min
5min forms complex solution.Complex solution adds 2mL ethanol amines under the magnetic agitation of 600r/min, and it is molten that reaction 1min obtains forerunner
Liquid.Under the magnetic agitation of 600r/min, 12mmol ammonium fluorides are added in precursor solution and react 1min, into reaction solution
Concentrated hydrochloric acid adjusting pH value is added and obtains colloidal solution for 10.Colloidal solution is added in autoclave, in 180 DEG C of baking ovens
Heat 40min.After reaction kettle is cooled to room temperature, centrifuge, with absolute ethyl alcohol and water supersound washing 3 times, after 80 DEG C of drying
The NaYF Yellow luminous to column hexagonal phase4:20%Yb3+/ 2%Er3+Upper conversion micron is brilliant.
Embodiment 2
It is a kind of quickly to prepare not jljl phase NaYF4The method of up-conversion, including：
By Y3+:Yb3+:Er3+Molar ratio be 78:20:2 yttrium nitrates, ytterbium nitrate, erbium nitrate for weighing 1mmol are dissolved in
Initial soln is formed in 10mL water.1mmol sodium citrates, stirring is added into initial soln under the magnetic agitation of 600r/min
5min forms complex solution.Complex solution adds 2mL ethanol amines under the magnetic agitation of 600r/min, and it is molten that reaction 1min obtains forerunner
Liquid.Under the magnetic agitation of 600r/min, 12mmol ammonium fluorides are added in precursor solution and react 1min, into reaction solution
Concentrated hydrochloric acid adjusting pH value is added and obtains colloidal solution for 4.Colloidal solution is added in autoclave, in 180 DEG C of baking ovens
Heat 40min.After reaction kettle is cooled to room temperature, centrifuge, with absolute ethyl alcohol and water supersound washing 3 times, after 80 DEG C of drying
To Yellow luminous column hexagonal phase NaYF4:20%Yb3+/ 2%Er3+Upper conversion micron is brilliant.
Embodiment 3
It is a kind of quickly to prepare not jljl phase NaYF4The method of up-conversion, including：
By Y3+:Yb3+:Er3+Molar ratio be 78:20:2 yttrium nitrates, ytterbium nitrate, erbium nitrate for weighing 1mmol are dissolved in
Initial soln is formed in 10mL water.1mmol sodium citrates, stirring is added into initial soln under the magnetic agitation of 600r/min
5min forms complex solution.Complex solution adds 2mL ethanol amines under the magnetic agitation of 600r/min, and it is molten that reaction 1min obtains forerunner
Liquid.Under the magnetic agitation of 600r/min, 12mmol ammonium fluorides are added in precursor solution and react 1min, into reaction solution
It is 1 that concentrated hydrochloric acid, which is added, and adjusts pH value, obtains colloidal solution.Colloidal solution is added in autoclave, in 180 DEG C of baking ovens
Heat 40min.After reaction kettle is cooled to room temperature, centrifuge, with absolute ethyl alcohol and water supersound washing 3 times, after 80 DEG C of drying
To octahedral shape cubic phase NaYF4:20%Yb3+/ 2%Er3+Upper conversion micron is brilliant.
Embodiment 4
It is a kind of quickly to prepare not jljl phase NaYF4The method of up-conversion, including：
By Y3+:Yb3+:Er3+Molar ratio be 78:20:2 yttrium nitrates, ytterbium nitrate, erbium nitrate for weighing 1mmol are dissolved in
Initial soln is formed in 10mL water.1mmol sodium citrates, stirring is added into initial soln under the magnetic agitation of 600r/min
5min forms complex solution.Complex solution adds 1mL ethanol amines under the magnetic agitation of 600r/min, and it is molten that reaction 1min obtains forerunner
Liquid.Under the magnetic agitation of 600r/min, 12mmol ammonium fluorides are added in precursor solution and react 1min, into reaction solution
Concentrated hydrochloric acid adjusting pH value is added and obtains colloidal solution for 10.Colloidal solution is added in autoclave, in 160 DEG C of baking ovens
Heat 60min.After reaction kettle is cooled to room temperature, centrifuge, with absolute ethyl alcohol and water supersound washing 3 times, after 80 DEG C of drying
To Yellow luminous column hexagonal phase NaYF4:20%Yb3+/ 2%Er3+Upper conversion micron is brilliant.
Embodiment 5
It is a kind of quickly to prepare not jljl phase NaYF4The method of up-conversion, including：
By Y3+:Yb3+:Er3+Molar ratio be 78:20:2 yttrium nitrates, ytterbium nitrate, erbium nitrate for weighing 1mmol are dissolved in
Initial soln is formed in 10mL water.1mmol sodium citrates, stirring is added into initial soln under the magnetic agitation of 600r/min
5min forms complex solution.Complex solution adds 2mL ethanol amines under the magnetic agitation of 600r/min, and it is molten that reaction 1min obtains forerunner
Liquid.Under the magnetic agitation of 600r/min, 24mmol ammonium fluorides are added in precursor solution and react 1min, into reaction solution
Concentrated hydrochloric acid adjusting pH value is added and obtains colloidal solution for 4.Colloidal solution is added in autoclave, in 180 DEG C of baking ovens
Heat 60min.After reaction kettle is cooled to room temperature, centrifuge, with absolute ethyl alcohol and water supersound washing 3 times, after 80 DEG C of drying
To the column hexagonal phase NaYF of green emitting4:20%Yb3+/ 2%Er3+Upper conversion micron is brilliant.
Embodiment 6
It is a kind of quickly to prepare not jljl phase NaYF4The method of up-conversion, including：
By Y3+:Yb3+:Er3+Molar ratio be 78:20:2 yttrium nitrates, ytterbium nitrate, erbium nitrate for weighing 1mmol are dissolved in
Initial soln is formed in 10mL water.1mmol sodium citrates, stirring is added into initial soln under the magnetic agitation of 600r/min
5min forms complex solution.Complex solution adds 2mL ethanol amines under the magnetic agitation of 600r/min, and it is molten that reaction 1min obtains forerunner
Liquid.Under the magnetic agitation of 600r/min, 24mmol ammonium fluorides are added in precursor solution and react 1min, into reaction solution
Concentrated hydrochloric acid adjusting pH value is added and obtains colloidal solution for 1.Colloidal solution is added in autoclave, in 180 DEG C of baking ovens
Heat 60min.After reaction kettle is cooled to room temperature, centrifuge, with absolute ethyl alcohol and water supersound washing 3 times, after 80 DEG C of drying
To a cube square phase NaYF4:20%Yb3+/ 2%Er3+Upper conversion micron is brilliant.
Fig. 1 is NaYF made from embodiment 14The scanning electron microscope diagram of up-conversion, Fig. 2 are made for embodiment 1
NaYF4Up-conversion luminescence spectrogram of the up-conversion under the excitation of 980 nanometer lasers, Fig. 3 are NaYF made from embodiment 14
The XRD spectrum of up-conversion.
By Fig. 1, Fig. 2 and Fig. 3 it is found that 1 preparation-obtained micron crystalline substance of embodiment has uniform monodispersed six sides rib
Column structure is the hexagonal phase NaYF of high-purity4Material, and show the hexagonal phase NaYF of high intensity4:20%Yb3+/ 2%
Er3+Yellow up-conversion luminescence feature.
Fig. 4 is NaYF made from embodiment 24The scanning electron microscope diagram of up-conversion, Fig. 5 are made for embodiment 2
NaYF4Up-conversion luminescence spectrogram of the up-conversion under the excitation of 980 nanometer lasers.
By Fig. 4 and Fig. 5 it is found that 2 preparation-obtained micron crystalline substance of embodiment has uniform monodisperse hexagonal prism shape
Structure is the hexagonal phase NaYF of high-purity4Material, and show the hexagonal phase NaYF of high luminous intensity intensity4:20%Yb3+/
2%Er3+Converting characteristic in green.
Fig. 6 is NaYF made from embodiment 34The scanning electron microscope diagram of up-conversion, Fig. 7 are made for embodiment 3
NaYF4The XRD spectrum of up-conversion.
By Fig. 6 and Fig. 7 it is found that the micron crystalline substance that embodiment 3 is prepared has the micron of uniform octahedral structure brilliant, it is
The cubic phase NaYF of high-purity4Material.
To sum up, quick preparation provided by the invention not jljl phase NaYF4The method of up-conversion passes through hydro-thermal normal direction
NaYF4Middle doping yttrium, ytterbium and erbium, obtained NaYF4Up-conversion pattern is uniform, luminescent properties are good.This method does not need gas
Atmosphere is protected, simple for process；By state modulators crystalline phases such as the pH that simply adjusts colloidal solution, repeatability is strong.Precursor solution
In added with ethanol amine, contribute to form and a kind of being similar to NaYF4Cubic phase intermediate product makes rapid reaction carry out in 40-60min
Inside it can be completed, it is with short production cycle.Suitable for large-scale production.
Phase NaYF provided by the invention4Up-conversion, according to above-mentioned quick preparation not jljl phase NaYF4Upper conversion material
The method of material is made, and it is uniform to have a pattern, and has the advantages that high luminous intensity.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of quickly preparing not jljl phase NaYF4The method of up-conversion, which is characterized in that including：To dissolved with Y3+、Yb3+
And Er3+Initial soln in be mixed into sodium citrate, obtain complex solution；It is mixed into ethanol amine into the complex solution, obtains presoma
Solution；It is mixed into the precursor solution containing F-Salt, adjusting pH value be 1-10, obtain colloidal solution；By the colloidal solution
It is placed in autoclave, 40-60min is heated under the conditions of 160-180 DEG C.
2. according to the method described in claim 1, it is characterized in that, in the initial soln, the Y3+, the Yb3+And it is described
Er3+Molar ratio be 78-88:10-20:2；Preferably, it is 78:20:2.
3. according to the method described in claim 2, it is characterized in that, in the initial soln, the Y3+, the Yb3+And it is described
Er3+Total mol concentration be 0.1-0.2mol/L.
4. according to claim 1-3 any one of them methods, which is characterized in that in the initial soln, the Y3+, it is described
Yb3+And the Er3+It is provided respectively by corresponding nitrate.
5. according to claim 1-3 any one of them methods, which is characterized in that the mole of the sodium citrate：The Y3+、
The Yb3+And the Er3+Moles total number be 1-2:1-2.
6. according to claim 1-3 any one of them methods, which is characterized in that the body of the complex solution and the ethanol amine
Product is than being 5-10:1.
7. according to claim 1-3 any one of them methods, which is characterized in that described to contain F-Salt in F-Mole：It is described
Y3+, the Yb3+And the Er3+Moles total number be 12-24:1.
8. the method according to the description of claim 7 is characterized in that described contain F-Salt be ammonium fluoride.
9. according to the method described in claim 1, being carried out using hydrochloric acid it is characterized in that, adjusting the operation that pH value is 1-10.
10. according to NaYF made from claim 1-9 any one of them methods4Up-conversion.
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| CN112625685A (en) * | 2020-12-11 | 2021-04-09 | 湖北文理学院 | Spherical hexagonal NaYF4Upconverting material and method for the production thereof |
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| CN112574749A (en) * | 2020-12-11 | 2021-03-30 | 湖北文理学院 | Three-dimensional NaYF4Up-conversion luminous micro-flower and preparation method thereof |
| CN112625685A (en) * | 2020-12-11 | 2021-04-09 | 湖北文理学院 | Spherical hexagonal NaYF4Upconverting material and method for the production thereof |
| CN112574749B (en) * | 2020-12-11 | 2022-07-08 | 湖北文理学院 | Three-dimensional NaYF4Up-conversion luminous micro-flower and preparation method thereof |
| CN112625685B (en) * | 2020-12-11 | 2022-08-30 | 湖北文理学院 | Spherical hexagonal NaYF 4 Upconverting material and method for the production thereof |
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