CN101177611A - High luminous intensity up-conversion fluorescence nano-crystal oxide and preparation method thereof - Google Patents
High luminous intensity up-conversion fluorescence nano-crystal oxide and preparation method thereof Download PDFInfo
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- CN101177611A CN101177611A CNA2007101447737A CN200710144773A CN101177611A CN 101177611 A CN101177611 A CN 101177611A CN A2007101447737 A CNA2007101447737 A CN A2007101447737A CN 200710144773 A CN200710144773 A CN 200710144773A CN 101177611 A CN101177611 A CN 101177611A
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Abstract
The invention discloses up-conversion fluorescent nanometer crystal oxide with strong luminous intensity and the preparation method thereof, and relates to an up-conversion material and the preparation method thereof. The invention solves the problem of low up-conversion luminous efficiency of the existing rare earth up-conversion material. A product formulation of the invention is: M:RE<3+>, Li<+>; wherein, M is Y2O3, Gd2O3, ZnO, ZrO2 or SiO2 and RE is rare earth element. The molar ratio between metal element and RE in the M is 1: 0.005-0.3, and the molar ratio between the metal element and lithium element in the M is 1: 0.005-0.3. The rare earth element is Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er or Tm. The invention adopts wet-chemical methods to prepare up-conversion fluorescent nanometer crystal oxide with strong luminous intensity. The wet-chemical methods are sol-gel method, burning method, hydrothermal method or solvent-thermal method. The up-conversion fluorescent luminous efficiency of the invention can be improved 80 times by maximum. The invention can greatly prompt the application of the oxide up-conversion luminous materials in the fields of fluorescent mark, up-conversion ultraviolet laser, fiber amplifier, etc. The method of the invention has simple technique and convenient operation.
Description
Technical field
The present invention relates to a kind of up-conversion and preparation method thereof.
Background technology
The up-conversion luminescence of rare earth ion is to absorb two or more lower energy photons, the phenomenon of a high-energy photon of emission.Up-conversion luminescence has utilized the 4f-4f transition of rare earth ion, according to the transition selection rule, thisly belong to abstinence originally with the electric dipole transition between the parity, in fact can be observed this transition, this mainly is because 4f configuration configuration g or the d opposite with parity mixes, or symmetry departs from reactive center, and making former is that the f-f transition of abstinence becomes permission.In last conversion substrate material, the matrix of oxide chemical stability is good, and physical strength is big, at aspects such as development compact type short wavelength laser, fluorescence labeling material, display material, anti-fake mark material, infrared eyes, all has great application prospect.But the phonon energy of matrix of oxide is bigger, causes its up-conversion luminescence efficient very low, and this has greatly limited its application.Therefore, the up-conversion luminescence efficient of raising rare earth ion is significant.
At present, mainly from selecting the low substrate material of phonon energy for use, add sensitized ions, seeking the up-conversion luminescence efficient that best inventions such as ion doping concentration increase rare earth ion, though though these methods have increased up-conversion luminescence efficient to a certain extent, up-conversion luminescence efficient is still lower.
Summary of the invention
The objective of the invention is in order to solve the inefficient problem of up-conversion luminescence of existing rare earth up-conversion, and a kind of high luminous intensity up-conversion fluorescence nano-crystal oxide and preparation method thereof is provided.The present invention passes through Li doped
+Ion strengthens the up-conversion luminescence efficient of trivalent rare earth ions doping oxide.
The general formula of high luminous intensity up-conversion fluorescence nano-crystal oxide of the present invention is M:RE
3+, Li
+Wherein M is Y
2O
3, Gd
2O
3, ZnO, ZrO
2Or SiO
2, RE is a rare earth element, and metallic element among the M and the mol ratio of RE are 1: 0.005～0.3, and the metallic element among the M and the mol ratio of elemental lithium are 1: 0.005～0.3.The RE rare earth element is Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er or Tm element.
The above-mentioned method for preparing high luminous intensity up-conversion fluorescence nano-crystal oxide of the present invention is a wet chemical method.Described wet chemical method is sol-gel method, combustion method, hydrothermal method or solvent-thermal method.
Principle: according to quantum mechanics, the up-conversion luminescence of rare earth ion is relevant with the symmetry around the active ions, increases active ions asymmetry on every side, can strengthen the luminous efficiency that goes up conversion.Therefore the present invention passes through Li doped
+Reduce active ions symmetry on every side, strengthen the up-conversion luminescence efficient of rare earth ion.
The up-conversion luminescence efficient of high luminous intensity up-conversion fluorescence nano-crystal oxide of the present invention is maximum to increase by 80 times.The present invention will greatly promote the application of up-conversion fluorescence nano-crystal in organism fluorescent mark field, and significant to developing conversion ultraviolet laser and fiber amplifier.Method technology of the present invention is simple, is convenient to operation.
Description of drawings
Fig. 1 is Gd under the laser excitation of 970nm infrared diode
2O
3: Er
3+1% and Gd
2O
3: Er
3+1%, Li
+5% nanocrystalline last convert light spectrogram, 1 expression Gd among the figure
2O
3: Er
3+1%, Li
+5% nanocrystalline last inversion spectrum curve, 2 expression Gd
2O
3: Er
3+1% nanocrystalline last inversion spectrum curve.Fig. 2 is ZnO:Er under the laser excitation of 970nm infrared diode
3+1% and ZnO:Er
3+1%, Li
+5% nanocrystalline last convert light spectrogram, 3 expression ZnO:Er among the figure
3+1%, Li
+5% nanocrystalline last inversion spectrum curve, 4 expression ZnO:Er
3+1% nanocrystalline last inversion spectrum curve.Fig. 3 is Y under the laser excitation of 970nm infrared diode
2O
3: Er
3+1% and Y
2O
3: Er
3+1%, Li
+5% nanocrystalline last convert light spectrogram, 5 expression Y among the figure
2O
3: Er
3+1%, Li
+5% nanocrystalline last inversion spectrum curve, 6 expression Y
2O
3: Er
3+1% nanocrystalline last inversion spectrum curve.
Embodiment
Embodiment one: the general formula of the high luminous intensity up-conversion fluorescence nano-crystal oxide of present embodiment is M:RE
3+, Li
+Wherein M is Y
2O
3, Gd
2O
3, ZnO, ZrO
2Or SiO
2, RE is a rare earth element, and metallic element among the M and the mol ratio of RE are 1: 0.005～0.3, and the metallic element among the M and the mol ratio of elemental lithium are 1: 0.005～0.3.
Embodiment two: what present embodiment and embodiment one were different is that M is Y
2O
3, Gd
2O
3, or ZrO
2Other is identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is that RE is Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er or Tm element.Other is identical with embodiment one.
Embodiment four: what present embodiment and embodiment one were different is that RE is Pr, Sm, Eu, Dy or Er.Other is identical with embodiment one.
Embodiment five: what present embodiment and embodiment one were different is that RE is Pr or Er.Other is identical with embodiment one.
Embodiment six: what present embodiment and embodiment one were different is that RE is Er.Other is identical with embodiment one.
Embodiment seven: present embodiment and embodiment one are different is that metallic element among the M and the mol ratio of RE are 1: 0.01～0.07.Other is identical with embodiment one.
Embodiment eight: present embodiment and embodiment one are different is that metallic element among the M and the mol ratio of RE are 1: 0.06.Other is identical with embodiment one.
Embodiment nine: present embodiment and embodiment one are different is that the metallic element among the M and the mol ratio of elemental lithium are 1: 0.03～0.12.Other is identical with embodiment one.
Embodiment ten: present embodiment and embodiment one are different is that the metallic element among the M and the mol ratio of elemental lithium are 1: 0.05～0.10.Other is identical with embodiment one.
Embodiment ten: present embodiment and embodiment one are different is that the metallic element among the M and the mol ratio of elemental lithium are 1: 0.07.Other is identical with embodiment one.
Embodiment 11: the high luminous intensity up-conversion fluorescence nano-crystal oxide of present embodiment is Y
2O
3: Er
3+, Li
+, ZrO
2: Er
3+, Li
+, Gd
2O
3: Er
3+, Li
+Or ZnO:Er
3+, Li
+Other is identical with embodiment one.
Embodiment 12: the method for the high luminous intensity up-conversion fluorescence nano-crystal oxide of preparation embodiment one is for adopting wet chemical method in the present embodiment.Described wet chemical method is sol-gel method, combustion method, hydrothermal method.
Embodiment 13: present embodiment adopts the Prepared by Sol Gel Method high luminous intensity up-conversion fluorescence nano-crystal oxide, its preparation method is realized by following step: one, rare earths salt and lithium salt solution are joined in the solution of M and be stirred to evenly, wherein the mol ratio of metallic element among the M and RE is 1: 0.005～0.3, metallic element among the M and the mol ratio of elemental lithium 1: 0.005～0.3; Two, add citric acid (making sequestrant) in the mixed solution after step 1 is handled, be stirred to evenly, wherein citric acid is 3～5: 1 with the mol ratio of whole metallic cations; Three, dropping ammonia in the mixed solution after step 2 is handled is regulated pH value to 5～7; Four, down the mixed solution after step 3 is handled is dried at 130 ℃-150 ℃, obtain black puffy solid; Five, with black puffy solid at 800 ℃ of following constant temperature 2h, naturally cool to room temperature, promptly obtain high luminous intensity up-conversion fluorescence nano-crystal oxide.It is white powder that present embodiment makes product, and its particle diameter is 30～40nm.
Embodiment 14: present embodiment adopts combustion method to prepare high luminous intensity up-conversion fluorescence nano-crystal oxide, its preparation method is realized by following step: one, rare earths salt and lithium salt solution are joined in the solution of M and be stirred to evenly, wherein the mol ratio of metallic element among the M and RE is 1: 0.005～0.3, metallic element among the M and the mol ratio of elemental lithium 1: 0.005～0.3; Two, the amount carbohydrate gum solution that in the mixed solution after step 1 is handled, adds, wherein carbohydrate gum is 1～4: 1 with the mol ratio of whole metallic cations, obtains presoma; Three, the presoma that obtains through step 2 of heating evaporates fully until moisture, continues elevated temperature, reach the mixture burning-point after, take fire, burning is finished and is obtained high luminous intensity up-conversion fluorescence nano-crystal oxide.It is white powder that present embodiment makes product, and its particle diameter is 30～60nm.
Embodiment 15: Hydrothermal Preparation high luminous intensity up-conversion fluorescence nano-crystal oxide in the present embodiment, its preparation method is realized by following step: one, rare earths salt and lithium salt solution are joined in the salts solution of M and be stirred to evenly, wherein the mol ratio of metallic element among the M and RE is 1: 0.005～0.3, metallic element among the M and the mol ratio of elemental lithium 1: 0.005～0.3; Two, with ammoniacal liquor the pH value of step 1 mixed solution is adjusted to 6.5, obtains gelatinous precipitate; Three, the gelatinous precipitate that obtains is put into autoclave, sealing was 160 ℃ of constant temperature three days; Naturally cool to room temperature then, the gained throw out is centrifugal, with washed with de-ionized water 5 times (removing the foreign ion in the product), again 200 ℃ of oven dry down; Four, step 4 is obtained product and rise to 500 ℃ gradually, and keep 4h, promptly get high luminous intensity up-conversion fluorescence nano-crystal oxide.It is spherical that present embodiment makes shape of product, and particle diameter is 70～110nm.
Claims (10)
1. high luminous intensity up-conversion fluorescence nano-crystal oxide, the general formula that it is characterized in that high luminous intensity up-conversion fluorescence nano-crystal oxide is M:RE
3+, Li
+Wherein M is Y
2O
3, Gd
2O
3, ZnO, ZrO
2Or SiO
2, RE is a rare earth element, metallic element among the M and the mol ratio of RE are 1: 0.005～0.3, metallic element among the M and the mol ratio of elemental lithium 1: 0.005～0.3.
2. high luminous intensity up-conversion fluorescence nano-crystal oxide according to claim 1 is characterized in that M is Y
2O
3, Gd
2O
3Or ZrO
2
3. high luminous intensity up-conversion fluorescence nano-crystal oxide according to claim 1 is characterized in that RE is Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er or Tm element.
4. high luminous intensity up-conversion fluorescence nano-crystal oxide according to claim 1 is characterized in that metallic element among the M and the mol ratio of RE are 1: 0.01～0.07.
5. high luminous intensity up-conversion fluorescence nano-crystal oxide according to claim 1 is characterized in that metallic element among the M and the mol ratio of RE are 1: 0.06.
6. high luminous intensity up-conversion fluorescence nano-crystal oxide according to claim 1 is characterized in that the metallic element among the M and the mol ratio of elemental lithium are 1: 0.03～0.12.
7. high luminous intensity up-conversion fluorescence nano-crystal oxide according to claim 1 is characterized in that the metallic element among the M and the mol ratio of elemental lithium are 1: 0.07.
8. high luminous intensity up-conversion fluorescence nano-crystal oxide according to claim 1 is characterized in that high luminous intensity up-conversion fluorescence nano-crystal oxide is Y
2O
3: Er
3+, Li
+, ZrO
2: Er
3+, Li
+, Gd
2O
3: Er
3+, Li
+Or ZnO:Er
3+, Li
+
9. the method for preparing the described high luminous intensity up-conversion fluorescence nano-crystal oxide of claim 1 is characterized in that the preparation method of high luminous intensity up-conversion fluorescence nano-crystal oxide is wet chemical method.
10. the preparation method of high luminous intensity up-conversion fluorescence nano-crystal oxide according to claim 9 is characterized in that described wet chemical method is sol-gel method, combustion method, hydrothermal method.
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| CN102660273A (en) * | 2012-04-26 | 2012-09-12 | 哈尔滨工程大学 | Preparation method of rare earth doped nano zirconia up-conversion phosphor powder |
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| CN102952543A (en) * | 2011-08-25 | 2013-03-06 | 海洋王照明科技股份有限公司 | Thulium-holmium co-doped zirconia upconversion phosphor and preparation method thereof |
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| CN102952544A (en) * | 2011-08-25 | 2013-03-06 | 海洋王照明科技股份有限公司 | Erbium-ytterbium co-doped zirconia luminescent film, preparation method and organic electroluminescent device |
| CN102952543B (en) * | 2011-08-25 | 2015-05-06 | 海洋王照明科技股份有限公司 | Thulium-holmium co-doped zirconia upconversion phosphor and preparation method thereof |
| CN102952544B (en) * | 2011-08-25 | 2015-02-11 | 海洋王照明科技股份有限公司 | Erbium-ytterbium co-doped zirconia luminescent film, preparation method and organic electroluminescent device |
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| CN102660273A (en) * | 2012-04-26 | 2012-09-12 | 哈尔滨工程大学 | Preparation method of rare earth doped nano zirconia up-conversion phosphor powder |
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Open date: 20080514 |