CN109097044A - A kind of small size erbium and ytterbium double doping lithium niobate fluorescent powder and its preparation method and application - Google Patents
A kind of small size erbium and ytterbium double doping lithium niobate fluorescent powder and its preparation method and application Download PDFInfo
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- CN109097044A CN109097044A CN201811076429.3A CN201811076429A CN109097044A CN 109097044 A CN109097044 A CN 109097044A CN 201811076429 A CN201811076429 A CN 201811076429A CN 109097044 A CN109097044 A CN 109097044A
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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
The present invention relates to a kind of small size erbiums and ytterbium double doping lithium niobate fluorescent powder and its preparation method and application.The preparation method includes the following steps: S1: dissolving erbium source, ytterbium source, niobium source and lithium source to obtain mixed solution；S2: the mixed solution reacts 12 ~ 48h at 260 ~ 270 DEG C, cooling, is centrifuged, washing, obtains sediment after dry；S3: the sediment is calcined into 5 ~ 120min at 900 ~ 1050 DEG C, grinding obtains erbium and ytterbium double doping lithium niobate fluorescent powder.Preparation method provided by the invention is high temperature hydro-thermal method, and preparation process is simple；The erbium and ytterbium double doping lithium niobate fluorescent powder being prepared are micron order small size fine granularity, and 980nm wavelength near-infrared laser can be converted to visible green and feux rouges, 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 a kind of small size erbium and ytterbium double doping lithium niobate fluorescent powder
Body and its preparation method and application.
Background technique
Upper conversion process is that long-wave radiation is converted to the process of shortwave radiation by the level structure of rare earth ion.It is upper to turn
Conversion materials are made of rare earth doped and host material, and rare earth doped type has been fixed, and then there are many kinds of selections for host material.
As the host material of up-conversion, lower phonon energy is needed.Lithium niobate is a kind of to collect a variety of optical properties in one
The material of body, with piezoelectricity, acousto-optic, electric light, Preset grating and the effects such as non-linear.The highest phonon energy of lithium niobate is about
880cm-1, belong to reduced levels, this also illustrates that lithium niobate has the ability as upper conversion host material.Lithium niobate is as upper turn
Conversion materials have both a variety of optical properties, will greatly widen the range of its application.Currently, lithium niobate up-conversion is mostly big
Block monocrystal, and preparation process is cumbersome, limits the application range of lithium niobate up-conversion.
Therefore it provides a kind of small size lithium niobate fluorescent powder 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, limit its scope of application
Defect and deficiency provide the preparation method of a kind of small size erbium and ytterbium double doping lithium niobate fluorescent powder.System provided by the invention
Preparation Method is high temperature hydro-thermal method, and preparation process is simple；The erbium and ytterbium double doping lithium niobate fluorescent powder being prepared are micron order
Small size fine granularity, and 980nm wavelength near infrared light can be converted into visible green and feux rouges, extension lithium niobate will be expected to
Application range.
The small size erbium and ytterbium codope niobic acid being prepared another object of the present invention is to provide above-mentioned preparation method
Lithium fluorescent powder.
Another object of the present invention is to provide above-mentioned small size erbiums and ytterbium double doping lithium niobate fluorescent powder to lead in optics
Application in domain.
For achieving the above object, the present invention adopts the following technical scheme:
A kind of preparation method of small size erbium and ytterbium double doping lithium niobate fluorescent powder, includes the following steps:
S1: it dissolves erbium source, ytterbium source, niobium source and lithium source to obtain mixed solution；Mole in the erbium source, ytterbium source, niobium source and lithium source
Than for 1.13 ~ 2.18:3.38 ~ 4.37:50.0 ~ 60.0:150 ~ 160；
S2: the mixed solution reacts 12 ~ 48h at 260 ~ 270 DEG C, cooling, is centrifuged, washing, obtains sediment after dry；
S3: the sediment is calcined into 5 ~ 120min at 900 ~ 1050 DEG C, grinding obtains small size erbium and ytterbium codope niobium
Sour lithium fluorescent powder.
For the present invention using high temperature hydro-thermal method preparation small size erbium and ytterbium double doping lithium niobate fluorescent powder, particle size can
Reach micron order, and can launch conversion visible green and feux rouges under the excitation of 980nm near-infrared laser, will be expected to widen
The application range of lithium niobate.
Existing conventional erbium source, ytterbium source, niobium source and lithium source are used equally in the present invention.
Preferably, the erbium source is one or more of five water erbium nitrates or four water acetic acid erbiums.
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 erbium source, ytterbium source, niobium source and lithium source is 1.13:3.38:60:160.
Preferably, it is dissolved in the water to obtain mixed solution in S1.
Preferably, the temperature reacted in S2 is 270 DEG C, time 48h.
Preferably, the rate being centrifuged in S2 is 8000rpm, time 3min.
Preferably, temperature dry in S2 is 70 DEG C, time 12h.
Preferably, the temperature calcined in S3 is 1050 DEG C, time 2h.
Preferably, the time ground in S3 is 1 ~ 5min.
A kind of small size erbium and ytterbium double doping lithium niobate fluorescent powder, are prepared by above-mentioned preparation method.
Preferably, the partial size of the small size erbium and ytterbium double doping lithium niobate fluorescent powder is 1 ~ 2 μm.
The application of above-mentioned small size erbium and ytterbium double doping lithium niobate fluorescent powder in optical field is also in guarantor of the invention
It protects in range.
Compared with prior art, the invention has the following beneficial effects:
Preparation method provided by the invention is high temperature hydro-thermal method, and preparation process is simple；The small size erbium and ytterbium being prepared are double-doped
Miscellaneous lithium niobate fluorescent powder is micron particles shape, under 980nm laser excitation, can launch conversion visible green and red
Light will be expected to the application range of broadening lithium niobate.
Detailed description of the invention
Fig. 1 is the XRD spectra of the small size erbium that embodiment 1 provides and ytterbium double doping lithium niobate fluorescent powder；
Fig. 2 is the upconversion emission figure of the small size erbium that embodiment 1 provides and ytterbium double doping lithium niobate fluorescent powder；
Fig. 3 is the SEM figure of the small size erbium that embodiment 1 provides and ytterbium double doping lithium niobate fluorescent powder.
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 erbiums and ytterbium double doping lithium niobate fluorescent powder.It is prepared via a method which to obtain.
1. measure 80mL deionized water, be added 0.0128mol Lithium hydroxide monohydrate, 0.0049mol niobium pentaoxide,
Five water ytterbium nitrate of five water erbium nitrate of 0.0901mmol and 0.2702mmol, and stir evenly.
2. the mixed liquor after stirring is transferred in reaction kettle, 48h is reacted at 270 DEG C.
3. being cooled to room temperature to reaction kettle, mixed liquor is taken out, 8000rpm revolving speed is centrifuged 3min, removes supernatant.
4. a centrifugation gained is deposited in 70 DEG C of dry 12h in drying box.
It is calcined 5. the sample after drying is placed in Muffle furnace, calcination temperature is 1050 DEG C, calcination time 2h.
6. calcined sample is placed in grinding alms bowl and grinds 5min, gained powder is erbium and ytterbium double doping lithium niobate
Fluorescent powder.
Fig. 1 is the XRD diagram of small size erbium prepared by the present embodiment 1 and ytterbium double doping lithium niobate fluorescent powder.Wherein, a
It is small size erbium prepared by the present invention and ytterbium double doping lithium niobate fluorescent powder for lithium niobate standard card PDF#78-0250, b.
Pass through the comparison of a and b, it can be seen that prepared small size erbium and ytterbium double doping lithium niobate fluorescent powder and standard card are complete
Entirely always, only there are two minimum miscellaneous peaks, thus may determine that sample prepared by the present invention is lithium niobate.
Fig. 2 is the upconversion emission figure of small size erbium prepared by the present embodiment 1 and ytterbium double doping lithium niobate fluorescent powder.
Under 980nm laser excitation, observes that 515 ~ 575nm wave band is very upper by force and convert green light peak, found in 640 ~ 680nm wave band weaker
Upper conversion visible red.
Fig. 1 is the SEM figure of small size erbium prepared by the present embodiment 1 and ytterbium double doping lithium niobate fluorescent powder.As schemed
Show, the granular size of prepared lithium niobate fluorescent powder is about 1 ~ 2 μm, and partial particulate is reunited.
Embodiment 2
The present embodiment provides a kind of small size erbiums and ytterbium double doping lithium niobate fluorescent powder.Preparation method substantially with embodiment 1
In method it is consistent, difference is: Lithium hydroxide monohydrate total amount in step 1 is 0.0132mol, and niobium pentaoxide total amount is
0.0051mol, five water erbium nitrate total amounts are 0.0164mmol, and five water ytterbium nitrate total amounts are 0.183mmol.This method is prepared
Small size erbium and ytterbium double doping lithium niobate fluorescent powder performance it is similar to Example 1.
Embodiment 3
The present embodiment provides a kind of small size erbiums and ytterbium double doping lithium niobate fluorescent powder.Preparation method substantially with embodiment 1
In method it is consistent, difference is: Lithium hydroxide monohydrate total amount in step 1 is 0.0111mol, and niobium pentaoxide total amount is
0.0043mol, five water erbium nitrate total amounts are 0.0915mmol, and five water ytterbium nitrate total amounts are 0.8215mmol.This method is prepared into
The performance of the small size erbium and ytterbium double doping lithium niobate fluorescent powder that arrive is similar to Example 1.
Embodiment 4
The present embodiment provides a kind of small size erbiums and ytterbium double doping lithium niobate fluorescent powder for it.Preparation method is substantially and embodiment
Method in 1 is consistent, and difference is: reaction temperature is 260 DEG C in step 2, time 12h.The small ruler that this method is prepared
The performance of very little erbium and ytterbium double doping lithium niobate fluorescent powder is similar to Example 1.
Embodiment 5
The present embodiment provides a kind of small size erbiums and ytterbium double doping lithium niobate fluorescent powder.Preparation method substantially with embodiment 1
In method it is consistent, difference is: in step 5 calcination temperature be 900 DEG C, time 5min.The small ruler that this method is prepared
The performance of very little erbium and ytterbium double doping lithium niobate fluorescent powder is similar to Example 1.
Embodiment 6
The present embodiment provides a kind of small size erbiums and ytterbium double doping lithium niobate fluorescent powder.It is prepared via a method which to obtain.
1. measure 80mL deionized water, be added 0.0145mol lithium hydroxide, 0.0056mol niobium pentaoxide,
Tetra- water acetic acid erbium of 0.102mmol and 0.307mmol acetic acid ytterbium, and stir evenly.
2. the mixed liquor after stirring is transferred in reaction kettle, 48h is reacted at 270 DEG C.
3. being cooled to room temperature to reaction kettle, mixed liquor is taken out, 8000rpm revolving speed is centrifuged 3min, removes supernatant.
4. a centrifugation gained is deposited in 70 DEG C of dry 12h in drying box.
It is calcined 5. the sample after drying is placed in Muffle furnace, calcination temperature is 1050 DEG C, calcination time 2h.
6. calcined sample is placed in grinding alms bowl and grinds 5min, gained powder is erbium and ytterbium double doping lithium niobate
Fluorescent powder.
The performance of small size erbium and ytterbium double doping lithium niobate fluorescent powder that this method is prepared is 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 erbium and ytterbium double doping lithium niobate fluorescent powder, which comprises the steps of:
S1: it dissolves erbium source, ytterbium source, niobium source and lithium source to obtain mixed solution；Mole in the erbium source, ytterbium source, niobium source and lithium source
Than for 1.13 ~ 2.18:3.38 ~ 4.37:50.0 ~ 60.0:150 ~ 160；
S2: the mixed solution reacts 12 ~ 48h at 260 ~ 270 DEG C, cooling, is centrifuged, washing, obtains sediment after dry；
S3: the sediment is calcined into 5min ~ 120min at 900 ~ 1050 DEG C, grinding obtains small size erbium and ytterbium codope
Lithium niobate fluorescent powder.
2. preparation method according to claim 1, which is characterized in that the erbium source is in five water erbium nitrates or four water acetic acid erbiums
One or more.
3. preparation method according to claim 1, which is characterized in that the ytterbium source is one in five water ytterbium nitrates or acetic acid ytterbium
Kind is several.
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 erbium source, ytterbium source, niobium source and lithium source molar ratio be
1.13:3.38: 60:160。
7. preparation method according to claim 1, which is characterized in that the temperature reacted in S2 is 270 DEG C, time 48h.
8. preparation method according to claim 1, which is characterized in that the temperature calcined in S3 is 1050 DEG C, time 2h.
9. a kind of small size erbium and ytterbium double doping lithium niobate fluorescent powder, which is characterized in that any described by claim 1 ~ 8
Preparation method is prepared.
10. the application of small size erbium described in claim 9 and ytterbium double doping lithium niobate fluorescent powder in optical field.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102162133A (en) * | 2011-03-25 | 2011-08-24 | 哈尔滨工业大学 | Zirconium, erbium and ytterbium-doped lithium niobate crystal and preparation method thereof |
| CN102797038A (en) * | 2012-08-10 | 2012-11-28 | 中国科学院上海光学精密机械研究所 | Mg-Yb-Er doped lithium niobate laser crystals and preparation method thereof |
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2018
- 2018-09-14 CN CN201811076429.3A patent/CN109097044A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102162133A (en) * | 2011-03-25 | 2011-08-24 | 哈尔滨工业大学 | Zirconium, erbium and ytterbium-doped lithium niobate crystal and preparation method thereof |
| CN102797038A (en) * | 2012-08-10 | 2012-11-28 | 中国科学院上海光学精密机械研究所 | Mg-Yb-Er doped lithium niobate laser crystals and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| FULEI WANG ET AL.: "Yb Sensitized Near-Stoichiometric Er:LiNbO3 Single Crystal: A Matrix for Optical Communication and Upconversion Emission", 《CRYST. GROWTH DES.》 * |
| PREPARATION OF CUBE MICROMETER POTASSIUM NIOBATE (KNBO3) BY HYDR: "Preparation of cube micrometer potassium niobate (KNbO3) by hydrothermal method and sonocatalytic degradation of organic dye", 《ULTRASONICS SONOCHEMISTRY》 * |
| YANNAN QIAN ET AL.: "Optical characteristics of Er3+ ion in Er/Yb:LiNbO3 crystal: Comparison with the dissimilar effect of anti-photorefractive ions Zn2+, In3+ and Zr4+", 《JOURNAL OF QUANTITATIVE SPECTROSCOPY & RADIATIVE TRANSFER》 * |
| 赵丹: "《新型磷酸盐晶体材料的合成与发光性能研究》", 31 December 2017, 西安交通大学出版社 * |
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Application publication date: 20181228 |