CN109233825A - A kind of small size thulium and ytterbium double doping lithium niobate up-conversion and its preparation method and application - Google Patents
A kind of small size thulium and ytterbium double doping lithium niobate up-conversion and its preparation method and application Download PDFInfo
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- CN109233825A CN109233825A CN201811076432.5A CN201811076432A CN109233825A CN 109233825 A CN109233825 A CN 109233825A CN 201811076432 A CN201811076432 A CN 201811076432A CN 109233825 A CN109233825 A CN 109233825A
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Abstract
The present invention relates to a kind of small size thuliums and ytterbium double doping lithium niobate up-conversion and its preparation method and application.The preparation method includes the following steps: S1: dissolving thulium source, ytterbium source, niobium source and lithium source to obtain mixed solution；S2: the mixed solution reacts at least 48h at 260 ~ 280 DEG C, cooling, is centrifuged, washing, obtains sediment after dry；S3: the sediment is calcined into 0.5 ~ 2h at 500 ~ 650 DEG C, grinding obtains small size thulium and ytterbium double doping lithium niobate up-conversion.Preparation method provided by the invention is high temperature hydro-thermal method, can also successfully be entered thulium ion and ytterbium ion doping in lithium niobate lattice without 800 DEG C and the above high-temperature calcination, simple process；The partial size of the small size thulium and ytterbium double doping lithium niobate up-conversion that are prepared is Nano grade (250 ~ 500nm), and under 980nm laser excitation, converting blue light in sending will be expected to the application range of extension lithium niobate.
Description
Technical field
The invention belongs to optical material technical fields, and in particular to convert on a kind of small size thulium and ytterbium double doping lithium niobate
Material and its preparation method and application.
Background technique
Rare earth thulium ion (Tm3+) using upper switch technology near infrared light effectively can be converted into visible blue, in light
It learns data storage, colored display, optical anti-counterfeiting and biomedical diagnostics etc. and presents broad application prospect, becoming most has
One of rare earth ion of researching value.Under the excitation of 980nm wavelength near infrared light, using ytterbium (Yb3+) ion as sensitizer increase
The luminous efficiency of strong upper converting blue light.This is because Yb3+Ion not only has very big absorption cross section in the near infrared region, and
And it can be efficiently by the energy transmission of absorption to Tm3+Ion.Small size rare earth thulium ion doped lithium columbate up-conversion
(Tm:LiNbO3) be hopeful LiNbO3Electric light, acousto-optic, ferroelectricity, piezoelectricity and the nonlinear optics and rare earth Tm of host material3+From
Converting blue light collection creates adequate condition for the research and development of integration and micro devices, has important research together in one on son
Value.
Therefore it provides a kind of lithium niobate up-conversion of small size has important research significance and application value.
Summary of the invention
It is an object of the invention to overcome in the prior art lithium niobate be mostly large size single crystal, in biomedical imaging and
The application defect and deficiency that are restricted of solar battery etc. are provided on a kind of small size thulium and ytterbium double doping lithium niobate
The preparation method of transition material.Preparation method provided by the invention is high temperature hydro-thermal method, without (800 DEG C or more) of high temperature calcinings
It can be obtained thulium/ytterbium ion doping lithium niobate up-conversion and effective visible blue；The thulium being prepared and ytterbium codope
The partial size of lithium niobate up-conversion is Nano grade, under 980nm laser excitation, issues blue light, will be expected to extension lithium niobate
Application range.
The small size thulium and ytterbium codope niobic acid being prepared another object of the present invention is to provide above-mentioned preparation method
Lithium up-conversion.
For achieving the above object, the present invention adopts the following technical scheme:
A kind of preparation method of small size thulium and ytterbium double doping lithium niobate up-conversion, includes the following steps:
S1: it dissolves thulium source, ytterbium source, niobium source and lithium source to obtain mixed solution；Mole in the thulium source, ytterbium source, niobium source and lithium source
Than for 1 ~ 10.97:10.97 ~ 50:254.7 ~ 309.8:662.2 ~ 805.23；
S2: the mixed solution reacts at least 48h at 260 ~ 280 DEG C, cooling, is centrifuged, washing, obtains sediment after dry；
S3: the sediment is calcined into 0.5 ~ 2h at 500 ~ 650 DEG C, grinding obtains small size thulium and ytterbium double doping lithium niobate
Up-conversion.
The present invention obtains small size thulium ion and ytterbium ion doping lithium niobate up-conversion using high temperature hydro-thermal method.Water
Thermal method is using water as reaction medium, to generate hyperbaric environment by heating in the reaction kettle of sealing, so that some water that are insoluble in
Substance can dissolve a kind of preparation method of concurrent biochemical reaction.The simple process of hydro-thermal method, the product of production have preferably
The process of high-temperature calcination is omitted in crystallinity.The present inventor through a large number of experiments as a result, it has been found that, hydrothermal temperature is too
It is low, thulium ion doped lithium columbate up-conversion cannot be formed.The present invention passes through the control to hydrothermal temperature and time, system
The standby other thulium ion doped lithium columbate up-conversion of nanoscale out, needing not move through 800 DEG C and the above high-temperature calcination can also be at
Near infrared light is converted to upper conversion visible blue by function, will be expected to the application range of extension lithium niobate.
Existing conventional thulium source, ytterbium source, niobium source and lithium source are used equally in the present invention.
Preferably, the thulium source is one or more of five water thulium nitrates or acetic acid thulium.
Preferably, the ytterbium source is one or more of five water ytterbium nitrates or acetic acid ytterbium.
Preferably, the niobium source is niobium pentaoxide.
Preferably, the lithium source is one or more of Lithium hydroxide monohydrate or lithium hydroxide.
Preferably, the molar ratio of the thulium source, ytterbium source, niobium source and lithium source is 4.332:21.66:293.6:763.2.
Preferably, it is dissolved in the water to obtain mixed solution in S1.
Preferably, the temperature reacted in S2 is 270 DEG C, time 72h.
Preferably, the rate being centrifuged in S2 is 8000rpm, time 5min.
Preferably, the process washed in S2 are as follows: benefit is washed with deionized 2 times.
Preferably, temperature dry in S2 is 80 DEG C, time 8h.
Preferably, the temperature calcined in S3 is 500 DEG C, time 2h.
Preferably, the time ground in S3 is at least 2min.
A kind of small size thulium and ytterbium double doping lithium niobate up-conversion, are prepared by above-mentioned preparation method.
Preferably, the partial size of the small size thulium and ytterbium double doping lithium niobate up-conversion is 250 ~ 500nm.
The application of above-mentioned small size thulium and ytterbium double doping lithium niobate up-conversion in optical field is also of the invention
In protection scope.
Preferably, the small size thulium and ytterbium double doping lithium niobate up-conversion are in biomedical imaging or solar-electricity
Application in pond.
Compared with prior art, the invention has the following beneficial effects:
Preparation method provided by the invention is high temperature hydro-thermal method, can also be successfully by thulium ion without 800 DEG C and the above high-temperature calcination
Enter in lithium niobate lattice with ytterbium ion doping, simple process；It is converted on the small size thulium and ytterbium double doping lithium niobate being prepared
The partial size of material is Nano grade (250 ~ 500nm), under 980nm laser excitation, issues visible blue, will be expected to extension niobic acid
The application range of lithium.
Detailed description of the invention
Fig. 1 is the SEM figure of the small size thulium that embodiment 1 provides and ytterbium double doping lithium niobate up-conversion；
Fig. 2 is the fluorescence spectra of the small size thulium that embodiment 1 provides and ytterbium double doping lithium niobate up-conversion；
Fig. 3 is the XRD diagram of the small size thulium that embodiment 1 provides and ytterbium double doping lithium niobate up-conversion.
Specific embodiment
Below with reference to embodiment, the present invention is further explained.These embodiments are merely to illustrate the present invention rather than limitation
The scope of the present invention.Test method without specific conditions in lower example embodiment usually according to this field normal condition or is pressed
The condition suggested according to manufacturer；Used raw material, reagent etc., unless otherwise specified, being can be from the business such as conventional market
The raw materials and reagents that approach obtains.The variation for any unsubstantiality that those skilled in the art is done on the basis of the present invention
And replacement belongs to scope of the present invention.
Embodiment 1
The present embodiment provides a kind of small size thuliums and ytterbium double doping lithium niobate up-conversion, are prepared via a method which to obtain.
1. measuring 80mL deionized water, 0.5263g Lithium hydroxide monohydrate, 1.2822g niobium pentaoxide, 0.1598g are weighed
Five water ytterbium nitrates and five water thulium nitrate of 0.0317g are added in deionized water, stir evenly.
2. the mixed liquor stirred evenly is moved in reaction kettle, as 270 DEG C of hydro-thermal reaction 72h in baking oven.
3. taking out reaction kettle, 8000rpm is centrifuged 5min and collects precipitating, and precipitating is washed with deionized 2 times.
4. by the precipitating washed as 80 DEG C in drying box dry 8h after, be placed in Muffle furnace 500 DEG C of calcining 2h, it is cold
But small size thulium and ytterbium double doping lithium niobate up-conversion are prepared into room temperature.
Fig. 1 is the SEM figure of small size thulium prepared by the present embodiment 1 and ytterbium double doping lithium niobate up-conversion.From figure
In as can be seen that prepared that sample is bulk, size is between 250 ~ 500nm.
Fig. 2 is the fluorescence spectra of small size thulium prepared by the present embodiment 1 and ytterbium double doping lithium niobate up-conversion.
It can be seen from the figure that prepared sample issues the visible blue light of 477nm wavelength, source under the excitation of 980nm wavelength laser
In thulium ion1G4→3H6Radiation transistion.
Fig. 3 is the XRD diagram of small size thulium prepared by the present embodiment 1 and ytterbium double doping lithium niobate up-conversion.A belongs to
Lithium niobate standard card, b are sample prepared by the present embodiment.It can be seen from the figure that prepared sample and standard card are complete
It is complete consistent, illustrate that the sample of preparation is lithium niobate.
Embodiment 2
The present embodiment provides a kind of small size thulium and ytterbium double doping lithium niobate up-conversion, preparation method is substantially and embodiment
Method in 1 is consistent, and difference is: the Lithium hydroxide monohydrate in step 1 is 0.5328g, niobium pentaoxide 1.2979g, five
Water ytterbium nitrate is 0.1613g and five water thulium nitrates are 0.008g.The small size thulium and ytterbium codope niobic acid that this method is prepared
Lithium up-conversion structure, pattern and optical property are similar to Example 1.
Embodiment 3
The present embodiment provides a kind of small size thuliums and ytterbium double doping lithium niobate up-conversion for it.Preparation method substantially with implementation
Method in example 1 is consistent, and difference is: the Lithium hydroxide monohydrate in step 1 is 0.5554g, niobium pentaoxide 1.3531g,
Five water ytterbium nitrates are 0.0832g and five water thulium nitrates are 0.0082g.The small size thulium and ytterbium codope niobium that this method is prepared
The structure of sour lithium up-conversion, pattern and optical property are similar to Example 1.
Embodiment 4
Its present embodiment provides a kind of small size thulium and ytterbium double doping lithium niobate up-conversion, preparation method substantially with implementation
Method in example 1 is consistent, and difference is: the Lithium hydroxide monohydrate in step 1 is 0.5485g, niobium pentaoxide 1.3363g,
Five water ytterbium nitrates are 0.0824g and five water thulium nitrates are 0.0327g.The small size thulium and ytterbium codope niobium that this method is prepared
The structure of sour lithium up-conversion, pattern and optical property are similar to Example 1.
Embodiment 5
The present embodiment provides a kind of small size thuliums and ytterbium double doping lithium niobate up-conversion.It is prepared via a method which to obtain.
1. measuring 80mL deionized water, 0.342g lithium hydroxide, 1.459g niobium pentaoxide, 0.1709g acetic acid are weighed
Ytterbium and 0.028g acetic acid thulium are added in deionized water, stir evenly.
2. the mixed liquor stirred evenly is moved in reaction kettle, as 260 DEG C of hydro-thermal reaction 72h in baking oven.
3. taking out reaction kettle, 8000rpm is centrifuged 5min and collects precipitating, and precipitating is washed with deionized 2 times.
4. by the precipitating washed as 80 DEG C in drying box dry 8h after, be placed in 650 DEG C of calcining 0.5h in Muffle furnace,
It is cooled to room temperature and is prepared into small size thulium and ytterbium double doping lithium niobate up-conversion.Small size thulium that this method is prepared and
The structure of ytterbium double doping lithium niobate up-conversion, pattern and optical property are similar to Example 1.
Embodiment 6
The present embodiment provides a kind of small size thuliums and ytterbium double doping lithium niobate up-conversion, are prepared via a method which to obtain.
1. measuring 80mL deionized water, 0.5263g Lithium hydroxide monohydrate, 1.2822g niobium pentaoxide, 0.1598g are weighed
Five water ytterbium nitrates and five water thulium nitrate of 0.0317g are added in deionized water, stir evenly.
2. the mixed liquor stirred evenly is moved in reaction kettle, as 280 DEG C of hydro-thermal reaction 48h in baking oven.
3. taking out reaction kettle, 8000rpm is centrifuged 5min and collects precipitating, and precipitating is washed with deionized 2 times.
4. by the precipitating washed as 80 DEG C in drying box dry 8h after, be placed in Muffle furnace 600 DEG C of calcining 1h, it is cold
But thulium and ytterbium double doping lithium niobate up-conversion are prepared into room temperature.The small size thulium and ytterbium codope that this method is prepared
The structure of lithium niobate up-conversion, pattern and optical property are similar to Example 1.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. the preparation method of a kind of small size thulium and ytterbium double doping lithium niobate up-conversion, which is characterized in that including walking as follows
It is rapid:
S1: it dissolves thulium source, ytterbium source, niobium source and lithium source to obtain mixed solution；Mole in the thulium source, ytterbium source, niobium source and lithium source
Than for 1 ~ 10.97:10.97 ~ 50:254.7 ~ 309.8:662.2 ~ 805.23；
S2: the mixed solution reacts at least 48h at 260 ~ 280 DEG C, cooling, is centrifuged, washing, obtains sediment after dry；
S3: the sediment is calcined into 0.5 ~ 2h at 500 ~ 650 DEG C, grinding obtains small size thulium and ytterbium double doping lithium niobate
Up-conversion.
2. preparation method according to claim 1, which is characterized in that the thulium source is one in five water thulium nitrates or acetic acid thulium
Kind is several.
3. preparation method according to claim 1, which is characterized in that the ytterbium source is in five water ytterbium nitrates or acetic acid ytterbium
It is one or more of.
4. preparation method according to claim 1, which is characterized in that the niobium source is niobium pentaoxide.
5. preparation method according to claim 1, which is characterized in that the lithium source is in Lithium hydroxide monohydrate or lithium hydroxide
One or more.
6. preparation method according to claim 1, which is characterized in that the thulium source, ytterbium source, niobium source and lithium source molar ratio be
4.332: 21.66: 293.2:763.2。
7. preparation method according to claim 1, which is characterized in that the temperature reacted in S2 is 270 DEG C, time 72h.
8. preparation method according to claim 1, which is characterized in that the temperature calcined in S3 is 500 DEG C, time 2h.
9. a kind of small size thulium and ytterbium double doping lithium niobate up-conversion, which is characterized in that pass through any institute of claim 1 ~ 8
Preparation method is stated to be prepared.
10. the application of small size thulium described in claim 9 and ytterbium double doping lithium niobate up-conversion in optical field.
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Cited By (1)
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Application publication date: 20190118 |