CN101210179A - Rare earth doping zinc oxide nano luminescent material and preparation method thereof - Google Patents
Rare earth doping zinc oxide nano luminescent material and preparation method thereof Download PDFInfo
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- CN101210179A CN101210179A CNA2006101353932A CN200610135393A CN101210179A CN 101210179 A CN101210179 A CN 101210179A CN A2006101353932 A CNA2006101353932 A CN A2006101353932A CN 200610135393 A CN200610135393 A CN 200610135393A CN 101210179 A CN101210179 A CN 101210179A
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Abstract
A rare-earth-doped ZnO nanometer luminescent material and a preparation method thereof relate to nanometer fluorescent materials. The ZnO nanocrystal prepared by the invention comprises xRe<3+>-(1-x)ZnO (wherein, Re=Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er, Yb, and Tm; and x=0.1 to 6mol%). A fluorescent spectrometer is used for measuring luminescence of a Eu<3+>:ZnO sample, and an emission peak with a width of 614.0-nm and an emission peak with a sharp of 616.6 nm of Eu<3+> can be obtained respectively at two different grid positions at 464.9 nm and 467.7 nm by selecting an excited wavelength.
Description
Technical field
The present invention relates to the nano fluorescent luminescent material, especially relate to a kind of rare earth doping zinc oxide nano luminescent material and preparation thereof.
Background technology
Rear-earth-doped nano semiconductor material is a kind of novel fluorescence luminescent material, at aspects such as opto-electronic device, liquid-crystal displays wide application prospect is arranged, and is subjected to the common concern of Chinese scholars.Wherein ZnO is a kind of wide bandgap semiconductor materials, and it has many excellent physical chemistry, is a kind of good luminous host.Because the radius ratio Zn of trivalent rare earth ions
2+Ion is much bigger, and both electric charges do not match, and rare earth ion generally is difficult to replace Zn
2+The form of lattice point position mix ZnO nanocrystalline in.Thereby that is reported all can only obtain rare earth at nanocrystal surface or nearly surperficial weak light, does not solve the effective doping of rare earth ion in ZnO.The method of the rear-earth-doped ZnO nano particle of preparation mainly contains sol-gel method and reverse micelle method etc. at present, wherein the maximum of usefulness are sol-gel method (Wang, X.et al.Luminescencespectroscopy and visible upconversion properties of Er3+in ZnO nanocrystals.Journal of Physical Chemistry B 108,18408-18413 (2004); Spanhel, L.﹠amp; Anderson, M.A.Semiconductor Clusters in the Sol-Gel Process-QuantizedAggregation, Gelation, and Crystal-Growth in Concentrated ZnO Colloids.Journal of the American Chemical Society 113,2826-2833 (1991)).The present invention has improved sol-gel technology, adopts the method for sol-gel co-precipitation, has solved rear-earth-doped problem effectively, has obtained strong luminous rear-earth-doped ZnO nano luminescent material.
Summary of the invention
The present invention proposes a kind of nanocrystalline preparation technology of rear-earth-doped ZnO of high luminous intensity.
The nanocrystalline component of ZnO of the present invention's preparation is: xRe
3+-(1-x) ZnO (Re=Pr wherein, Nd, Sm, Eu, Tb, Dy, Tm, Ho, Er, Yb; X=0.1-6mol%).
The present invention adopts and is prepared as follows technology: lanthanon acetate and zinc acetate is evenly mixed, 100-150 ℃ of drying to remove crystal water, cooling adds dehydrated alcohol, stirring makes it to mix, with said mixture 60-90 ℃ of stirring, the milkiness solution that forms is cooled to below 10 ℃, and the lithium hydroxide that adds capacity then stirs, and obtains gelatinous mixture; The capacity normal hexane is joined in the above-mentioned gelatinous mixture, make it precipitation, leave standstill supernatant liquid and precipitate and separate, with the precipitation absolute ethanol washing that obtains, 40-80 ℃ of drying, it is initial nanocrystalline to obtain Re:ZnO, and with initial nanocrystalline 100-600 ℃ of thermal treatment, it is nanocrystalline to obtain Re:ZnO.
The Re:ZnO for preparing is nanocrystalline to be pure wurtzite structure.XRD powder art diffraction and transmission electron microscope show that what obtain is nanocrystalline small-particle near the single 3-50 of dispersion nanometer.By the selective exitation wavelength, can obtain strong, sharp-pointed rare earth luminescence, show rare earth ion can effectively be doped to ZnO nanocrystalline in, be a kind of good fluorescence luminescent material.
Material preparation process of the present invention is simple, cost is low, good reproducibility, can produce in enormous quantities.The present invention and nanocrystalline the comparing of Re:ZnO for preparing both at home and abroad at present, rare earth ion can be doped to the nanocrystalline middle Zn of ZnO effectively
2+The lattice point position, can obtain very strong rare earth luminescence by selective exitation, be a kind of good advanced luminescent material.
Description of drawings
Fig. 1: different levels of doping Eu
3+: 30 minutes (a) 0.5at% of the initial nanocrystalline 400 ℃ of thermal treatments of ZnO, (b) 1at%, (c) 2at% and (d) Eu
3+: the initial nanocrystalline XRD diffraction pattern of ZnO (1at%);
Fig. 2 mixes Eu
3+The ZnO of 2at% is initial nanocrystalline at the transmission electron microscope picture of 400 ℃ of thermal treatments after 30 minutes;
Fig. 3: mix Eu
3+The ZnO of 1at% is initial nanocrystalline at the selective excitation emmission spectrum of 400 ℃ of thermal treatments after 30 minutes, and excitation wavelength is 464.9nm and 467.7nm.
Embodiment
Example 1: in round-bottomed flask with 0.022g acetic acid europium (Eu (CH
3COO)
36H
2O) and 2.195g zinc acetate (Zn (CH
3OO)
22H
2O) evenly mixed, drying is 60 minutes in 120 ℃ baking oven, cools off a little back and adds 100 milliliters of dehydrated alcohols, stirs to make it to mix.Heated and stirred refluxed 3 hours in 80 ℃ of water-baths then, obtained emulsion, the emulsion that obtains is transferred to be as cold as 0 ℃ in the beaker rapidly, and ultrasonic agitation is 30 minutes in 0 ℃ ice-water bath, added 0.8 gram, one hydronium(ion) oxidation lithium (LiOHH simultaneously
2O) make it complete hydrolysis and obtain gelatinous mixture.250 ml n-hexanes are joined in the above-mentioned gelatinous mixture, make it rapid precipitation, left standstill 30 minutes,, the precipitation that obtains with absolute ethanol washing six times, 60 ℃ of dryings 14 hours, is obtained Eu supernatant liquid and precipitate and separate
3+: ZnO (0.5at%) wurtzite is initial nanocrystalline, particle diameter 3-5 nanometer, and agglomeration is arranged.With initial nanocrystalline, obtain monodispersed Eu 400 ℃ of thermal treatments 30 minutes
3+: the fine ore deposit of ZnO (0.5at%) is nanocrystalline, particle diameter 11-15 nanometer.Luminous with fluorescence spectrophotometer test sample product has the strong emission peak of broadening initial exciting at 614.0nm with 465nm in nanocrystalline; Nanocrystallinely after 30 minutes, can obtain two different lattice points position Eu respectively at 464.9nm and 467.7nm with initial by the selective exitation wavelength 400 ℃ of thermal treatments
3+At the strong emission peak of 614.0nm broadening and at the sharp-pointed strong emission peak of 616.8nm.
Example 2: in round-bottomed flask with 0.0442g acetic acid europium (Eu (CH
3COO)
36H
2O) and 2.195g zinc acetate (Zn (CH
3OO)
22H
2O) evenly mixed, drying is 60 minutes in 120 ℃ baking oven, cools off a little back and adds 100 milliliters of dehydrated alcohols, stirs to make it to mix.Heated and stirred refluxed 3 hours in 80 ℃ of water-baths then, obtained emulsion, the emulsion that obtains is transferred to be as cold as 0 ℃ in the beaker rapidly, and ultrasonic agitation is 30 minutes in 0 ℃ ice-water bath, added 0.8 gram, one hydronium(ion) oxidation lithium (LiOHH simultaneously
2O) make it complete hydrolysis and obtain gelatinous mixture.250 ml n-hexanes are joined in the above-mentioned gelatinous mixture, make it rapid precipitation, left standstill 30 minutes,, the precipitation that obtains with absolute ethanol washing six times, 40-60 ℃ of drying 14 hours, is obtained Eu supernatant liquid and precipitate and separate
3+: ZnO (1at%) wurtzite is initial nanocrystalline, particle diameter 3-5 nanometer, and agglomeration is arranged.With initial nanocrystalline, obtain monodispersed Eu 400 ℃ of thermal treatments 30 minutes
3+: ZnO (1at%) wurtzite is nanocrystalline, particle diameter 9-14 nanometer.Luminous with fluorescence spectrophotometer test sample product has the strong emission peak of broadening initial exciting at 614.0nm with 465nm in nanocrystalline; Nanocrystallinely after 30 minutes, can obtain two different lattice points position Eu respectively at 464.9nm and 467.7nm with initial by the selective exitation wavelength 400 ℃ of thermal treatments
3+At the strong emission peak of 614.0nm broadening and at the sharp-pointed strong emission peak of 616.8nm.
Example 3: in round-bottomed flask with 0.0892g acetic acid europium (Eu (CH
3COO)
36H
2O) and 2.195g zinc acetate (Zn (CH
3OO)
22H
2O) evenly mixed, drying is 60 minutes in 120 ℃ baking oven, cools off a little back and adds 100 milliliters of dehydrated alcohols, stirs to make it to mix.Heated and stirred refluxed 3 hours in 80 ℃ of water-baths then, obtained emulsion, the emulsion that obtains is transferred to be as cold as 0 ℃ in the beaker rapidly, and ultrasonic agitation is 30 minutes in 0 ℃ ice-water bath, added a hydronium(ion) oxidation lithium (LiOHH of 0.8 gram simultaneously
2O) make it complete hydrolysis and obtain gelatinous mixture.250 ml n-hexanes are joined in the above-mentioned gelatinous mixture, make it rapid precipitation, left standstill 30 minutes,, the precipitation that obtains with absolute ethanol washing six times, 60 ℃ of dryings 14 hours, is obtained Eu supernatant liquid and precipitate and separate
3+: ZnO (2at%) wurtzite is initial nanocrystalline, particle diameter 3-5 nanometer, and agglomeration is arranged.With initial nanocrystalline, obtain monodispersed Eu 400 ℃ of thermal treatments 30 minutes
3+: ZnO (2at%) wurtzite is nanocrystalline, particle diameter 8-11 nanometer.Luminous with fluorescence spectrophotometer test sample product has the strong emission peak of broadening initial exciting at 614.0nm with 465nm in nanocrystalline; Nanocrystallinely after 30 minutes, can obtain two different lattice points position Eu respectively at 464.9nm and 467.7nm with initial by the selective exitation wavelength 400 ℃ of thermal treatments
3+At the strong emission peak of 614.0nm broadening and at the sharp-pointed strong emission peak of 616.8nm.
Example 4: in round-bottomed flask with 0.0457g acetic acid erbium (Er (CH
3COO)
36H
2O) and 2.195g zinc acetate (Zn (CH
3OO)
22H
2O) evenly mixed, drying is 60 minutes in 120 ℃ baking oven, cools off a little back and adds 100 milliliters of dehydrated alcohols, stirs to make it to mix.Heated and stirred refluxed 3 hours in 80 ℃ of water-baths then, obtained emulsion, the emulsion that obtains is transferred to be as cold as 0 ℃ in the beaker rapidly, and ultrasonic agitation is 30 minutes in 0 ℃ ice-water bath, added 0.8 gram, one hydronium(ion) oxidation lithium (LiOHH simultaneously
2O) make it complete hydrolysis and obtain gelatinous mixture.250 ml n-hexanes are joined in the above-mentioned gelatinous mixture, make it rapid precipitation, left standstill 30 minutes,, the precipitation that obtains with absolute ethanol washing six times, 40-60 ℃ of drying 14 hours, is obtained Er supernatant liquid and precipitate and separate
3+: ZnO (1at%) wurtzite is initial nanocrystalline, particle diameter 3-5 nanometer, and agglomeration is arranged.With initial nanocrystalline, obtain monodispersed Er 400 ℃ of thermal treatments 30 minutes
3+: ZnO (1at%) wurtzite is nanocrystalline, particle diameter 9-13 nanometer.
Example 5: in round-bottomed flask with 0.0449g acetic acid terbium (Tb (CH
3COO)
36H
2O) and 2.195g zinc acetate (Zn (CH
3OO)
22H
2O) evenly mixed, drying is 60 minutes in 120 ℃ baking oven, cools off a little back and adds 100 milliliters of dehydrated alcohols, stirs to make it to mix.Heated and stirred refluxed 3 hours in 80 ℃ of water-baths then, obtained emulsion, the emulsion that obtains is transferred to be as cold as 0 ℃ in the beaker rapidly, and ultrasonic agitation is 30 minutes in 0 ℃ ice-water bath, added 0.8 gram, one hydronium(ion) oxidation lithium (LiOHH simultaneously
2O) make it complete hydrolysis and obtain gelatinous mixture.250 ml n-hexanes are joined in the above-mentioned gelatinous mixture, make it rapid precipitation, left standstill 30 minutes,, the precipitation that obtains with absolute ethanol washing six times, 40-60 ℃ of drying 14 hours, is obtained Tb supernatant liquid and precipitate and separate
3+: ZnO (1at%) wurtzite is initial nanocrystalline, particle diameter 3-5 nanometer, and agglomeration is arranged.With initial nanocrystalline, obtain monodispersed Tb 400 ℃ of thermal treatments 30 minutes
3+: ZnO (1at%) wurtzite is nanocrystalline, particle diameter 9-14 nanometer.
Example 6: in round-bottomed flask with 0.0434g acetic acid neodymium (Nd (CH
3COO)
36H
2O) and 2.195g zinc acetate (Zn (CH
3OO)
22H
2O) evenly mixed, drying is 60 minutes in 120 ℃ baking oven, cools off a little back and adds 100 milliliters of dehydrated alcohols, stirs to make it to mix.Heated and stirred refluxed 3 hours in 80 ℃ of water-baths then, obtained emulsion, the emulsion that obtains is transferred to be as cold as 0 ℃ in the beaker rapidly, and ultrasonic agitation is 30 minutes in 0 ℃ ice-water bath, added 0.8 gram, one hydronium(ion) oxidation lithium (LiOHH simultaneously
2O) make it complete hydrolysis and obtain gelatinous mixture.250 ml n-hexanes are joined in the above-mentioned gelatinous mixture, make it rapid precipitation, left standstill 30 minutes,, the precipitation that obtains with absolute ethanol washing six times, 40-60 ℃ of drying 14 hours, is obtained Nd supernatant liquid and precipitate and separate
3+: ZnO (1at%) wurtzite is initial nanocrystalline, particle diameter 3-5 nanometer, and agglomeration is arranged.With initial nanocrystalline, obtain monodispersed Nd 400 ℃ of thermal treatments 30 minutes
3+: ZnO (1at%) wurtzite is nanocrystalline, particle diameter 9-14 nanometer.
Claims (2)
1. the preparation method of a rare earth doping zinc oxide nano luminescent material, it is characterized in that: lanthanon acetate and zinc acetate is evenly mixed, 100-150 ℃ of drying to remove crystal water, cooling adds dehydrated alcohol, stirring makes it to mix, and said mixture 60-90 ℃ of stirring, is cooled to the milkiness solution that forms below 10 ℃, the lithium hydroxide that adds capacity then stirs, and obtains gelatinous mixture; The capacity normal hexane is joined in the above-mentioned gelatinous mixture, make it precipitation, leave standstill supernatant liquid and precipitate and separate, with the precipitation absolute ethanol washing that obtains, 40-80 ℃ of drying, it is initial nanocrystalline to obtain Re:ZnO, and with initial nanocrystalline 100-600 ℃ of thermal treatment, it is nanocrystalline to obtain Re:ZnO.
2. rare earth doping zinc oxide nano luminescent material that adopts the preparation of the described method of claim 1, its component is: xRe
3+-(1-x) ZnO, Re=Pr wherein, Nd, Sm, Eu, Tb, Dy, Tm, Ho, Er, Yb; X=0.1-6mol%.
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| WO2010099667A1 (en) * | 2009-03-06 | 2010-09-10 | 海洋王照明科技股份有限公司 | ZnO GREEN LUMINESCENT MATERIAL AND ITS PREPARATION |
| CN101993692A (en) * | 2009-08-30 | 2011-03-30 | 中国科学院合肥物质科学研究院 | Method for doping earth ions in zinc oxide nano crystal |
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| WO2010099667A1 (en) * | 2009-03-06 | 2010-09-10 | 海洋王照明科技股份有限公司 | ZnO GREEN LUMINESCENT MATERIAL AND ITS PREPARATION |
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| CN101993692A (en) * | 2009-08-30 | 2011-03-30 | 中国科学院合肥物质科学研究院 | Method for doping earth ions in zinc oxide nano crystal |
| CN101993692B (en) * | 2009-08-30 | 2013-01-02 | 中国科学院合肥物质科学研究院 | Method for doping earth ions in zinc oxide nano crystal |
| CN103384931A (en) * | 2010-12-23 | 2013-11-06 | 野猫技术开发公司 | Lithium-ion battery materials with improved properties |
| CN102719797A (en) * | 2012-05-08 | 2012-10-10 | 常州天合光能有限公司 | Zinc oxide based transparent conductive membrane having up-conversion function and method for preparing same |
| CN103396799A (en) * | 2013-07-25 | 2013-11-20 | 惠州市西顿工业发展有限公司 | LED (light-emitting diode) lamp as well as preparation method of red emitting inorganic luminescent material used in LED lamp |
| CN105176525A (en) * | 2013-07-25 | 2015-12-23 | 惠州市西顿工业发展有限公司 | LED lamp and preparation method of red-emitting inorganic luminescent material adopted by same |
| CN103627396A (en) * | 2013-12-09 | 2014-03-12 | 广西师范学院 | Method for synthesizing rare earth Ho-doped CdTe:Ho quantum dot by hydrothermal method |
| CN105295902A (en) * | 2015-10-22 | 2016-02-03 | 大连民族大学 | Rare-earth-doped ZnO nanocrystal temperature and humidity sensing material and preparation method thereof |
| CN108484926A (en) * | 2018-04-17 | 2018-09-04 | 南昌大学 | A kind of preparation method and application of the double transmitting fluorescence probes of cerium-quantum dot coordination polymer |
| WO2021129706A1 (en) * | 2019-12-27 | 2021-07-01 | Tcl科技集团股份有限公司 | Nanomaterial and preparation method therefor, quantum dot light-emitting diode and preparation method therefor |
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Application publication date: 20080702 |