CN107057692B - CaF with good light-emitting performance under high pressure2:Tb3+Nano material and preparation method thereof - Google Patents
CaF with good light-emitting performance under high pressure2:Tb3+Nano material and preparation method thereof Download PDFInfo
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- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7743—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing terbium
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Abstract
The invention discloses CaF with good light-emitting performance under high pressure2:Tb3+A nano material and a preparation method thereof belong to the technical field of nano material preparation. Provides a method for synthesizing CaF in one step by using a solvothermal method2:Tb3+Green chemical method of nano material with Ca (NO)3)2And Tb (NO)3)3The precursor reactant is NaF as a fluorine source, and HF regulates the pH value of the solution. Using ethanol as a solvent, and carrying out a solvothermal reaction at 135-145 ℃ for 15-17 h to obtain a cubic fluorite structure CaF with a crystal grain size of 25nm2:Tb3+And (3) nano materials. The method has the advantages of simple preparation process, low cost, low energy consumption, environmental protection, nontoxicity, high repeatability and the like. Preparation of the resulting CaF2：Tb3+The nano material has excellent green fluorescence characteristic and can still keep good luminescence performance under the action of pressure. The luminescent material capable of overcoming the limit condition has wide prospect in the aspects of display devices, biological probes, fluorescent labels and the like.
Description
Technical Field
The present invention belongs to the field of nanometer luminescent material and its technology.
Background
The rare earth doped nano luminescent material has the characteristics of large specific surface area, high surface energy, small size and the like, and shows many characteristics of improved quantum confinement effect, red shift or blue shift phenomenon of spectrum, widened absorption band, enhanced luminous intensity and the like compared with a bulk material. Due to these unique and excellent optical properties, rare earth doped nano-luminescent materials have been widely used in light emitting devices, optical imaging and optoelectronic devices.
The rare earth doped nano luminescent material has a wide variety, and the host material is one of the important factors influencing the rare earth doped luminescent property. The choice of matrix depends mainly on the stability of the material and the size of the phonon energy, the lower phonon energy in the matrix being an important factor for the high emission efficiency of the activated ions. With CaF2The luminescent material as the substrate has high chemical stability, low phonon energy, good solubility and no toxicity, and thus has important application in the fields of display devices, biological probes, fluorescent labels and the like, and is receiving more and more attention. With CaF2The application of the luminescent material as the substrate is more and more extensive in a plurality of fields, the requirement on the luminescent performance of the material is more and more high, and particularly, the excellent luminescent material which still keeps good optical performance under the limit condition attracts the wide research interest of the researchers.
In recent years, CaF has been doped with rare earths2The preparation and luminescent properties of nanomaterials are studied in great numbers, but the focus is mainly on Yb3+/Er3+、Yb3+/Tm3+Isocodoped upconversion CaF2Nano luminescent material, and Tb3+Singly doped CaF2The preparation and optical performance research of the nano green fluorescent material are few, and especially the luminous performance stability research of the material under high pressure is not reported yet. Existing synthetic methods for preparing CaF2：Tb3+Nanomaterials have some disadvantages. Such as: CaF prepared by simple one-step hydrothermal synthesis method2：Tb3+The nano material has larger grain size, and can not realize the preparation of nano grains below 50 nm. To make a desire toPreparing CaF with smaller grain size2：Tb3+The nano material usually needs to be assisted by oleylamine and oleic acid serving as ligands or by adding a surfactant and the like, so that the preparation process is complex and the cost is high; the preparation process of oleylamine and oleic acid also needs to use a large amount of toxic organic solvent, and the production process has serious influence on the environment.
Disclosure of Invention
Aiming at the problems, the CaF with small crystal grain size and stable luminous performance under extreme conditions is synthesized by a simple and environment-friendly green method2:Tb3+Nanomaterials are very necessary. Therefore, the invention provides CaF with good light-emitting performance under high pressure2:Tb3+A nano material and a preparation method thereof.
The technical scheme adopted by the invention is as follows:
1) ca (NO) is added3)2And Tb (NO)3)3Dissolving in 10mL of deionized water to obtain a mixed solution, wherein Tb3+The metal cation accounts for 10 mol percent of the metal cation, and the concentration of the metal cation in the mixed solution is 0.0120-0.0130 mol/L;
2) adding NaF into the mixed solution, stirring to ensure that the molar ratio of the metal cations to the fluorine ions is 1:2,
3) adding hydrofluoric acid into the mixed solution to adjust the pH value to 1, fully mixing and stirring, transferring into a reaction kettle, sealing,
4) preparation of CaF by solvothermal reaction2:Tb3+The solvent is ethanol, the filling degree of the reaction kettle is 80-90%, the temperature is 135-145 ℃, the reaction is carried out for 15-17 h, and the reaction product is taken out after furnace cooling.
5) Washing with deionized water and absolute ethyl alcohol to remove impurities, and drying to obtain CaF2:Tb3+And (3) nano materials.
The CaF thus obtained2:Tb3+The nano material is a fluorite cubic phase structure, the particle size is 25nm, and the luminous intensity of the strongest green light luminous peak under the pressure of 8.9GPa is increased by 216 percent when compared with 0 GPa.
The invention has the beneficial effects that:
1. the invention discloses a methodTb with small grain size and uniform appearance is synthesized by one step by adopting solvothermal method3+Doped CaF2The nano fluorescent material has the advantages of simple operation, low energy consumption, environmental protection, high repeatability and the like;
2. tb of the invention3+Doped CaF2The nanometer material has excellent fluorescence characteristic. The luminous performance of the sample under high pressure is measured in situ by adopting a diamond anvil cell press, and the sample still keeps good luminous characteristic under the high pressure of 8.9 GPa. With large-scale production of CaF suitable for use in extreme conditions2：Tb3+The potential of nanomaterials.
3. The luminescent material capable of overcoming the limit condition has wide prospect in the aspects of display devices, biological probes, fluorescent labels and the like.
Drawings
FIG. 1 is CaF2：Tb3+Transmission electron microscopy of nanocrystalline grains.
FIG. 2 is CaF2：Tb3+X-ray diffraction pattern of the nano-crystalline grains.
FIG. 3 is CaF2：Tb3+Photoluminescence spectra of nanocrystals at atmospheric pressure.
FIG. 4 is CaF2：Tb3+Photoluminescence spectra of nanocrystals at high pressure.
Detailed Description
The technical solution of the present invention is further explained and illustrated by the following examples, wherein all reagents are commercially available products and are used without further purification unless otherwise specified.
① Ca (NO) is selected3)2、Tb(NO3)3NaF is used as a precursor reactant, and 0.01125mol/L of Ca (NO)3)2And 0.00125mol/L of Tb (NO)3)3Adding the mixture into 10mL of deionized water together for dissolving; adding 0.025mol/L NaF into the mixed solution, stirring on a magnetic stirrer, simultaneously dropwise adding 5 drops (about 0.05mL of each drop) of hydrofluoric acid with the concentration of 40%, adjusting the pH value to 1, fully stirring for 60min, transferring into a 40mL reaction kettle, sealing, using ethanol as a solvent, and ensuring the filling degree to be 85%. At 140 DEG CAnd performing heat treatment for 16 hours, cooling along with the furnace, and taking out. And ultrasonically and centrifugally washing the taken product for 2 times by using deionized water, and ultrasonically and centrifugally washing for 3 times by using absolute ethyl alcohol. Drying the sample at 80 ℃ for 10h to obtain cubic phase Tb3+Doped CaF2Nanocrystalline grain starting samples.
It can be seen from FIG. 1 that the samples prepared were uniform in size and narrow in particle size distribution with an average size of 25 nm. FIG. 2 is Tb3+Doped CaF2The XRD spectrogram of the nano crystal grain shows that the prepared sample is a fluorite cubic phase structure without impurity diffraction peaks, which indicates that Tb is doped3+Without changing the crystal structure of the matrix thereafter. FIG. 3 is Tb3+Doped CaF2The photoluminescence spectrum of the nano crystal grains shows that the prepared sample has good fluorescence characteristics, wherein the strongest luminescence peak is a green luminescence peak, and the nano crystal grain is a green fluorescent material with a prospect.
②CaF2:Tb3+The high-pressure luminous performance research is carried out in a symmetrical diamond anvil cell, the symmetrical diamond anvil cell is pressurized, the size of the diamond anvil cell surface is 400 microns, a sealing gasket is made of a T301 stainless steel sheet, the prepressing thickness is 60 microns, a small hole with the diameter of 120 microns is drilled in the prepressed gasket to serve as a high-pressure sample cavity, silicon oil is selected as a pressure transmission medium, the pressure calibration is carried out by adopting a standard ruby fluorescence pressing technology, the CaF prepared in the step ① is subjected to pressure measurement, and the high-pressure sample cavity is formed by adopting a standard ruby fluorescence pressing technology2:Tb3+And putting the nano crystal grains into a diamond anvil cell press, pressurizing the sample to the maximum pressure of 8.9GPa, and measuring the wavelength of the laser used for the high-pressure luminescence test to 325 nm. As can be seen from fig. 4, the luminescence intensity gradually increased with the increase of the pressure during the sample pressurization. Wherein, the luminous intensity of the strongest green light luminous peak at 545nm at 0GPa is increased by 216 percent when the pressure is added to 8.9GPa, which indicates that the sample has good optical performance and still has stable luminous characteristics under the condition of high pressure limit.
Claims (5)
1. CaF with good light-emitting performance under high pressure2:Tb3+The nano material is characterized in that the fluorite has a cubic phase structure, the grain size is 25nm, Tb3+The doping proportion of (A) is 10%, the luminous intensity of the strongest green light luminous peak is increased by 216% when compared with 0GPa under the pressure of 8.9GPa, and the preparation steps are as follows:
1) ca (NO) is added3)2And Tb (NO)3)3Dissolving in 10mL of deionized water to obtain a mixed solution, wherein Tb3+The metal cation accounts for 10 mol percent of the metal cation, and the concentration of the metal cation in the mixed solution is 0.0120-0.0130 mol/L;
2) adding NaF into the mixed solution, and stirring to ensure that the molar ratio of the metal cations to the fluorine ions is 1: 2;
3) adding hydrofluoric acid into the mixed solution to adjust the pH value to 1, fully mixing and stirring, and then transferring into a reaction kettle for sealing;
4) preparation of CaF by solvothermal reaction2:Tb3+The solvent is ethanol, the filling degree of the reaction kettle is 80-90%, the temperature is 135-145 ℃, the reaction is carried out for 15-17 h, and the reaction product is taken out after furnace cooling.
5) Washing with deionized water and absolute ethyl alcohol to remove impurities, and drying to obtain CaF2:Tb3+And (3) nano materials.
2. CaF with good light-emitting properties under high pressure according to claim 12:Tb3+The preparation method of the nano material comprises the following specific steps:
1) ca (NO) is added3)2And Tb (NO)3)3Dissolving in 10mL of deionized water to obtain a mixed solution, wherein Tb3+The metal cation accounts for 10 mol percent of the metal cation, and the concentration of the metal cation in the mixed solution is 0.0120-0.0130 mol/L;
2) adding NaF into the mixed solution, and stirring to ensure that the molar ratio of the metal cations to the fluorine ions is 1: 2;
3) adding hydrofluoric acid into the mixed solution to adjust the pH value to be below 1, fully mixing and stirring, and then transferring into a reaction kettle for sealing;
4) preparation of CaF by solvothermal reaction2:Tb3+The solvent is ethanol, the filling degree of the reaction kettle is 80-90%, the temperature is 135-145 ℃, the reaction is carried out for 15-17 h, and the reaction product is taken out after furnace cooling.
3. CaF with good light emission properties under high pressure according to claim 22:Tb3+The preparation method of the nano material is characterized in that the concentration of metal cations in the mixed solution in the step 1) is 0.0125 mol/L.
4. CaF with good light emission properties under high pressure according to claim 22:Tb3+The preparation method of the nano material is characterized in that the filling degree of the reaction kettle in the step 4) is 85 percent.
5. CaF with good light emission properties under high pressure according to claim 22:Tb3+The preparation method of the nano material is characterized in that the reaction is carried out for 16 hours at the temperature of 140 ℃.
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| CN1880406A (en) * | 2005-06-03 | 2006-12-20 | 纳幕尔杜邦公司 | Method for preparing rare-earth doped fluoride nanoparticles |
| CN105295905A (en) * | 2015-11-18 | 2016-02-03 | 湖北工业大学 | Preparation method of water-soluble Eu<3+>-doped calcium fluoride nano particles |
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| CN1880406A (en) * | 2005-06-03 | 2006-12-20 | 纳幕尔杜邦公司 | Method for preparing rare-earth doped fluoride nanoparticles |
| CN105295905A (en) * | 2015-11-18 | 2016-02-03 | 湖北工业大学 | Preparation method of water-soluble Eu<3+>-doped calcium fluoride nano particles |
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| 廖金生等.铽掺杂氟化钙绿色荧光粉的合成及发光性能.《光学学报》.2014, * |
| 铽掺杂氟化钙绿色荧光粉的合成及发光性能;廖金生等;《光学学报》;20140510;0516002/1-0516002/6 * |
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