CN112980441A - Rare earth ion activated indium salt high-efficiency fluorescent material, preparation method and application thereof - Google Patents
Rare earth ion activated indium salt high-efficiency fluorescent material, preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a rare earth ion activated indium oxide high-efficiency fluorescent powder material, a preparation method and application thereof, wherein the fluorescent material has a chemical formula (A)1‑xB)InO4xRe, wherein x is more than or equal to 0.001 and less than or equal to 0.3, B is Ca, Sr and/or Ba, A is La, Y, Sc, Lu and/or Gd, and Re is Nd3+、Sm3+、Eu3+、Yb3+、Ho3+、Er3+、Tm3+、Tb3+、Dy3+And/or Pr3+. With oxide A2O3、Re2O3And carbonate BCO3Is prepared by a solid-phase reaction method; metal ion nitrate is used as a raw material, and a sol-gel method is adopted for preparation; rare earth ion oxide and divalent metal carbonate are used as raw materials and prepared by a sol-gel method. Ultraviolet light with the wavelength of 210-370 nm is used as a light source for excitation or light excitation with the characteristic wavelength corresponding to 4f electronic transition of trivalent rare earth ion activator is used in the wavelength range of 300-450 nm, so that the ultraviolet light can be excitedThe material can emit light efficiently.
Description
Technical Field
The invention relates to a rare earth ion activated indium salt high-efficiency fluorescent material, a preparation method and application thereof, belonging to the field of rare earth luminescent materials.
Background
The rare earth doped fluorescent material is one of the most important rare earth functional materials, is mainly applied to the fields of energy-saving lamps, semiconductor illumination, flat panel display and the like, has become one of the supporting materials in the fields of energy-saving illumination, information display, photoelectric detection and the like, and plays an increasingly important role in scientific and technological progress and social development.
The rare earth doped fluorescent material consists of a matrix and a rare earth ion activator doped into the matrix, the luminescence characteristic of the fluorescent material is mainly determined by the property of 4f shell electrons of rare earth ions, and the rare earth ions show different electron transition forms and extremely rich energy level transitions along with the change of the number of the 4f shell electrons. Thus, rare earth ions can emit light of various wavelengths from the ultraviolet to infrared regions to form a wide variety of light emitting materials. In recent thirty years, rare earth luminescent materials have been developed remarkably, and meanwhile, with the wide application of rare earth fluorescent materials in various fields, higher requirements on the luminescent properties of the materials are provided. Especially in the application of white light LED illumination and display, the research and industrial development of rare earth luminescent materials have resulted in subversive changes, such as: the CRT, PDP, FED and other displays quit the historical stage, the output and sales of the rare earth tricolor fluorescent powder for the lamp are sharply reduced, and the demand for the high-efficiency white light fluorescent powder is more urgent.
The factors influencing the luminous efficiency of the rare earth fluorescent material mainly comprise the following two aspects:
firstly, the energy transfer mode of rare earth ion luminescence and the probability of 4f electron transition of rare earth ion are induced, most of trivalent rare earth ion luminescence comes from electron transition of unfilled 4f shell layer (called f-f transition), and since 4f layer electrons are shielded by 8 electrons of 5s and 5p electron layers, the crystal field isThe influence on the position of a spectral line is small, so the energy level of 4f electrons in a crystal field is generally similar to the discrete energy level of free atoms, and the emission spectrum is a linear spectrum. For rare earth free ions, 4fnThe space names of various electronic states in the configuration are the same, the transition matrix element between the electronic states is zero, and the rare earth ions 4f are determined according to the space name selection rule of the rare earth electronic transitionnThe electric dipole transition between the energy levels in the configuration is forbidden and the magnetic dipole transition is allowed. In the condensed state, the order of 4f can be changed due to the effect of the odd term of the crystal fieldnConfiguration of inverse parity is mixed into 4fnIn a configuration such that 4fnThe state in the configuration is no longer a single state but a mixed state of two parity, and the electric dipole transition matrix element between the electronic states is not zero, so that 4fnElectric dipole transitions within the configuration are possible, so that 4f based transitions can be observednThe luminescence of the f-f transition in the configuration. However, the f-f transition probability is still small, so that the light absorption and light emission generated by the f-f transition probability are weak, which is one of the main factors influencing the luminous efficiency of the rare earth fluorescent material.
Secondly, the concentration of rare earth ions that can efficiently emit light, after the luminescence center of the rare earth ion in the host lattice absorbs energy to reach an excited state, the energy can be transferred to another center in the host in some form, in addition to being returned to the ground state by its own radiative transition or non-radiative transition, and the process of this transfer is called energy transfer. Because the rare earth ions have rich energy levels, when the energy difference of two energy levels of one rare earth ion is equal to the energy difference of two energy levels of another ion, energy resonance transfer is carried out, and the radiation and non-radiation processes between the two ions are easy to occur. According to the theory of Dexter, the resonance energy transfer efficiency is inversely proportional to the square of the distance between two ions, which means that the energy transfer efficiency increases rapidly with the increase of the doping concentration of rare earth ions in the matrix lattice, and particularly between the same kind of rare earth ions, concentration quenching easily occurs through cross relaxation due to the perfect matching of the energy difference between the two energy levels, so that few rare earth ions can efficiently emit photons despite the high concentration of rare earth ions doped in the matrix.
It is obvious that both the probability of 4f electron transition of rare earth ions and the energy transfer for inducing the luminescence of the rare earth ions are related to the substrate providing the luminescent environment for the rare earth ions, and therefore, to realize more efficient luminescence of rare earth fluorescence, the design and preparation of rare earth fluorescent materials based on novel substrates are required.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, improve the luminous efficiency of rare earth ions by effectively reducing non-radiative energy loss ways caused by cross relaxation among the rare earth ions, and finally provide a fluorescent material of rare earth ion activated indate oxide capable of efficiently emitting light and a preparation method of the fluorescent material.
The technical scheme of the invention is as follows:
a rare-earth ion activated efficient luminescent material of indium oxide is prepared from rare-earth ion Re3+Activator doping to InAlate oxide (AB) InO4A substrate having a 214-layered perovskite structure formed in the A site of the lattice and having a chemical formula of (A)1-xB)InO4xRe; wherein, 0.001<x<0.3, B is one or more of divalent metal ions such as Ca, Sr, Ba and the like, A is one or more of La, Y, Sc, Lu and Gd photo-inert metal ions, and Re is Nd3+、Sm3+、Eu3+、Yb3+、Ho3+、Er3 +、Tm3+、Tb3+、Dy3+、Pr3+One or more trivalent rare earth ion activators.
Preferably, the chemical formula of the fluorescent material is (La0.91Sr) InO4:0.09 Eu.
Preferably, the fluorescent material has a chemical formula of (La)0.79Sr)InO4:0.21Eu。
Preferably, the fluorescent material has a chemical formula of (La)0.90Sr)InO4:(0.04Eu,0.06Tb)。
Preferably, the fluorescent material has a chemical formula of (Y)0.81Sr0.5Ba0.5)InO4:0.09Dy。
The preparation method of the fluorescent material comprises the following steps:
the chemical formula is (A) prepared by adopting a solid-phase reaction method1-xB)InO4xRe the rare earth ion activated indium oxide high efficiency fluorescent material comprises the following steps:
with oxide A2O3、Re2O3And carbonate BCO of divalent metal B3The method is characterized in that the carbonate raw material of the divalent metal needs to be pre-sintered for 3 hours at 500 ℃, and the rare earth oxide raw material needs to be thermally insulated for 2 hours at 800 ℃ to remove impurities. Firstly, the desired oxide A is weighed according to the stoichiometry2O3、Re2O3And carbonate BCO of divalent metal B3Fully grinding, reacting at 1100-1300 ℃ for 4-8 hours after uniformly mixing, naturally cooling to room temperature, ball-milling for 4 hours, drying, placing in a muffle furnace again, reacting at 1300-1500 ℃ for 6-16 hours, cooling to room temperature, grinding, analyzing the phase and crystal structure of the material by adopting X-ray diffraction, and confirming that the (A) with the layered perovskite structure is obtained1-xB)InO4xRe indium oxide phosphor.
The chemical formula is (A) prepared by using metal ion nitrate as a raw material and adopting a sol-gel method1-xB)InO4xRe the layered perovskite type indate nano fluorescent powder comprises the following process steps: the nitrate of the desired metal ions was weighed out stoichiometrically, dissolved in 250ml of a 10% strength citric acid solution and a few drops of nitric acid were added dropwise to the solution to prevent hydrolysis of the metal ions. The mixed solution is put in a water bath at 70-90 ℃, the solvent is slowly evaporated while stirring to form sol, the gel is dried for 8-16 hours at 120 ℃ after gelation to form dry gel, the dry gel is decomposed for 2-4 hours at 600 ℃, heat treatment is carried out for 2-4 hours at 800 ℃, and finally the gel reacts for 6-18 hours at the high temperature of 950-1350 ℃ to prepare the (A) with the layered perovskite structure1-xB)InO4xRe indium acid salt phosphor, and the grain size is 50-500 nm.
The chemical is prepared by taking rare earth ion oxide and divalent metal carbonate as raw materials and adopting a sol-gel methodIs of the formula (A)1-xB)InO4xRe the layered perovskite type indate nano fluorescent powder comprises the following process steps: weighing the required rare earth ion oxide and divalent metal carbonate according to the stoichiometric proportion, and respectively dissolving the rare earth ion oxide and the divalent metal carbonate into the dilute HNO3The solution was heated while stirring until a uniform and stable nitrate solution was formed, and these nitrate solutions were mixed, and citric acid and polyvinyl alcohol (PVA, molecular weight: 10000) were added thereto and dissolved by stirring. Wherein the molar ratio of citric acid to polyvinyl alcohol is 2-4: 1, the mixed solution is placed in a 70-90 ℃ water bath, the solvent is slowly evaporated while stirring to form sol, the gel is dried at 120 ℃ for 8-16 hours to form dry gel after gelation, the dry gel is decomposed at 600 ℃ for 2-4 hours after grinding, heat treated at 800 ℃ for 2-4 hours, and finally reacted at 950-1350 ℃ for 6-18 hours to obtain the layered perovskite type indate (A), namely the layered perovskite type indate1-xB)InO4xRe nm oxide phosphor with a grain size of 50-500 nm.
Compared with the prior art, the invention has the beneficial effects that:
the invention proposes the use of an indate oxide (AB) InO having a 214-layered perovskite structure4As a matrix, is a rare earth ion Re3+The activator provides a luminescent environment at (A)1-xB)InO4xRe wherein the rare earth ions are distributed in the AO layer and the AO layer, the BO layer and the InO layer are alternated to form the structural feature of AO-InO-BO-InO-AO, so that the rare earth ions Re3+The activators are effectively separated, so that non-radiative energy loss caused by cross relaxation among rare earth ions can be effectively reduced, and the luminous efficiency of the rare earth ions is improved.
The fluorescent material can excite the rare earth ion activator to emit light by two modes of matrix sensitization and 4f electron transition absorption, has high luminous efficiency, can be widely applied to the fields of LED illumination, various displays and the like, has simple preparation method and process, and is suitable for large-scale production.
Drawings
FIG. 1 is a view of a layered perovskite type indate salt (La)0.91Sr)InO4XRD pattern and crystal structure of 0.09Eu fluorescent powderSchematic representation.
FIG. 2 (La)0.91Sr)InO40.09Eu phosphor and (La)0.79Sr)InO40.21Eu phosphor emits light at 613 nm.
FIG. 3 uses light excitation (La) of different wavelengths in the range of 210 nm-370 nm0.91Sr)InO40.09Eu phosphor.
Detailed Description
Example 1: prepared by adopting a solid-phase reaction method (La)0.91Sr)InO4:0.09Eu
With La2O3、SrCO3、In2O3、Eu2O3As a raw material, wherein SrCO is required3Presintering at 500 ℃ for 3 hours, La2O3、Eu2O3And In2O3Presintering at 800 deg.C for 2 hr. Firstly, weighing 0.0091mol of La according to the stoichiometric proportion2O30.0009mol of Eu2O30.02mol of SrCO3And 0.01mol of In2O3Fully grinding, reacting at 1200 ℃ for 4 hours after uniformly mixing, naturally cooling to room temperature, ball-milling for 4 hours, then placing in a muffle furnace for reacting at 1350 ℃ for 12 hours, cooling to room temperature, analyzing the phase and crystal structure of the material by X-ray diffraction after grinding, and as shown in figure 1, proving that the pure phase (La) with 214-layer type layered perovskite structure prepared by the method (La-Ti-0.91Sr)InO40.09Eu fluorescent powder.
Example 2: prepared by adopting a solid-phase reaction method (La)0.79Sr)InO4:0.21Eu
With La2O3、SrCO3、In2O3、Eu2O3As a raw material, wherein SrCO is required3Presintering at 500 ℃ for 3 hours, La2O3、Eu2O3And In2O3Presintering at 800 deg.C for 2 hr. Firstly, 0.0079mol of La is weighed according to the stoichiometric proportion2O30.0021mol of Eu2O3Taking 0.02mol of SrCO3And 0.01mol of In is taken2O3Fully grinding, reacting at 1200 ℃ for 4 hours after uniformly mixing, naturally cooling to room temperature, ball-milling for 4 hours, then placing in a muffle furnace for reacting at 1350 ℃ for 12 hours, cooling to room temperature, grinding to obtain pure phase (La) with layered perovskite structure0.79Sr)InO40.21Eu fluorescent powder.
Example 3: prepared by adopting a solid-phase reaction method (La)0.90Sr)InO4:(0.04Eu,0.06Tb)
With La2O3、SrCO3、In2O3、Eu2O3、Tb2O3As a raw material, wherein SrCO is required3Presintering at 500 ℃ for 3 hours, La2O3、Eu2O3、Tb2O3And In2O3Presintering at 800 deg.C for 2 hr. Firstly, 0.009mol of La is weighed according to the stoichiometry2O30.02mol of SrCO30.01mol of In2O30.0004mol of Eu2O30.0006mol of Tb2O3Fully grinding, reacting at 1200 ℃ for 4 hours after uniformly mixing, naturally cooling to room temperature, ball-milling for 4 hours, then placing in a muffle furnace for reacting at 1350 ℃ for 12 hours, cooling to room temperature, grinding to obtain pure phase (La) with layered perovskite structure0.90Sr)InO4Fluorescent powder (0.04Eu,0.06 Tb).
Example 4: prepared by a sol-gel method (Y)0.81Sr0.5Ba0.5)InO4:0.09Dy
0.01mol of Sr (NO) is weighed according to the stoichiometric proportion3)20.01mol of Ba (NO)3)2And 0.0162mol of Y (NO)3)3·6H2O, 0.0018mol Dy (NO)3)3·6H2O and 0.02mol of In (NO)3)3·9H2O raw material, dissolving it into 250ml of citric acid solution with the concentration of 10%, and dripping a few drops of nitric acid into the solution to prevent the metal ions from hydrolyzing. Then the mixed solution is put in 70 ℃ water bath, the solvent is slowly evaporated while stirring to form sol, and the gel is gelatedDrying at 120 deg.C for 12 hr to form xerogel, grinding, calcining at 600 deg.C for 2 hr, calcining at 800 deg.C for 3 hr, and reacting at 1000 deg.C for 12 hr to obtain layered perovskite type indate oxide (Y)0.81Sr0.5Ba0.5)InO40.09Dy nano fluorescent powder, the grain size of which is 50-200 nm.
Example 5: prepared by a sol-gel method (La)0.92Ba)InO4:0.08Tm
Weighing 0.0092mol of La according to the stoichiometric proportion2O30.02mol of BaCO30.01mol of In2O30.0008mol of Tm2O3And dissolving them in diluted HNO3In the solution, the solution was stirred while heating until a uniform and stable nitrate solution was formed, the above nitrate solutions were mixed, 0.12mol of citric acid and 0.04mol of polyvinyl alcohol (PVA, molecular weight: 10000) were added thereto, and dissolved by stirring. The mixed solution is put in a water bath at 70-90 ℃, the solvent is slowly evaporated while stirring to form sol, the gel is dried for 8-16 hours at 120 ℃ after gelation to form dry gel, the dry gel is ground, decomposed for 2 hours at 600 ℃, thermally treated for 3 hours at 800 ℃, and finally reacted for 12 hours at the high temperature of 1000 ℃ to obtain the layered perovskite type indate (La < Sc >)0.92Ba)InO40.08Tm nano oxide fluorescent powder, the grain size of which is 50 to 500 nm.
Example 6: (La)0.91Sr)InO40.09Eu test for luminescence property
First detecting hypersensitive transitions (e.g. Eu) causing rare earth ions3+Is/are as follows5D2—7F0Transition) as shown in fig. 2, it can be observed that ultraviolet light with a wavelength in the range of 250nm to 350nm is used as a light source to excite the indium oxide fluorescent powder (La)0.91Sr)InO4:0.09Eu3+Or (La)0.79Sr)InO4:0.21Eu3+The material can efficiently emit light by matrix sensitization. It is also observed that at a wavelength range of 350nm to 450nm, the use of Eu corresponds to3+The characteristic wavelength of the 4f electron transition of (a) is: 363nm and 394nm light as light sourceThe fluorescent material can be excited to emit light efficiently. Based on (La)0.91Sr)InO40.09Eu and (La)0.79Sr)InO4The 0.21Eu phosphor emits light at 613nm, ultraviolet light with wavelengths of 305nm, 363nm and 394nm is selected as excitation light source to excite (La0.91Sr)InO40.09Eu phosphor, and the emission spectrum of the detected material is shown in FIG. 3, which shows that (La)0.91Sr)InO40.09Eu is a high-efficiency fluorescent powder material.
Claims (11)
1. A rare earth ion activated indium oxide high-efficiency fluorescent material is characterized in that:
the fluorescent material is prepared by mixing rare earth ions Re3+Activator doping to InAlate oxide (AB) InO4A substrate having a 214-layered perovskite structure formed in the A site of the lattice and having a chemical formula of (A)1-xB)InO4:xRe；
Wherein, 0.001<x<0.3, B is one or more of Ca, Sr and Ba divalent metal ions, A is one or more of La, Y, Sc, Lu and Gd photo-inert metal ions, and Re is Nd3+、Sm3+、Eu3+、Yb3+、Ho3+、Er3+、Tm3+、Tb3+、Dy3+、Pr3+One or more trivalent rare earth ion activators.
2. The indate oxide high efficiency fluorescent material of claim 1, wherein:
the chemical formula of the fluorescent material is (La)0.91Sr)InO4:0.09Eu。
3. The indate oxide high efficiency fluorescent material of claim 1, wherein:
the chemical formula of the fluorescent material is (La)0.79Sr)InO4:0.21Eu。
4. The indate oxide high efficiency fluorescent material of claim 1, wherein:
the chemical formula of the fluorescent material is (La)0.90Sr)InO4:(0.04Eu,0.06Tb)。
5. The indate oxide high efficiency fluorescent material of claim 1, wherein:
the chemical formula of the fluorescent material is (Y)0.81Sr0.5Ba0.5)InO4:0.09Dy。
6. The method for preparing the indate oxide high-efficiency fluorescent material according to any one of claims 1 to 5, wherein:
with oxide A2O3、Re2O3And carbonate BCO of divalent metal B3The preparation method of the fluorescent material by adopting a solid-phase reaction method as a raw material comprises the following process steps:
step 1, pre-burning a divalent metal carbonate raw material at 500 ℃ for 3 hours in a heat preservation way, and removing impurities from a rare earth oxide raw material at 800 ℃ for 2 hours;
step 2, weighing the required oxide A according to the stoichiometric proportion2O3、Re2O3And carbonate BCO of divalent metal B3Fully grinding, uniformly mixing, and reacting at 1100-1300 ℃ for 4-8 hours;
and 3, naturally cooling to room temperature, performing ball milling for 4 hours, drying, placing in a muffle furnace again, reacting for 6-16 hours at the high temperature of 1300-1500 ℃, cooling to room temperature, and grinding to obtain the fluorescent powder of the fluorescent material.
7. The method for preparing the indate oxide high-efficiency fluorescent material according to any one of claims 1 to 5, wherein:
the method for preparing the fluorescent material by using metal ion nitrate as a raw material and adopting a sol-gel method comprises the following process steps:
step 1, weighing nitrate of required metal ions according to the stoichiometric amount, dissolving the nitrate into 250ml of citric acid solution with the concentration of 10%, and dropwise adding a few drops of nitric acid into the solution to prevent the metal ions from being hydrolyzed;
step 2, placing the mixed solution in a water bath at 70-90 ℃, slowly evaporating the solvent while stirring to form sol, drying the gel at 120 ℃ for 8-16 hours after gelation to form dry gel, decomposing the gel at 600 ℃ for 2-4 hours after grinding, and performing heat treatment at 800 ℃ for 2-4 hours;
and 3, finally reacting for 6-18 hours at the high temperature of 950-1350 ℃ to prepare the fluorescent powder of the fluorescent material.
8. The method for preparing the indate oxide high-efficiency fluorescent material according to any one of claims 1 to 5, wherein:
the preparation method of the fluorescent material by using rare earth ion oxide and divalent metal carbonate as raw materials and adopting a sol-gel method comprises the following process steps:
step 1, weighing required rare earth ion oxide and divalent metal carbonate according to stoichiometric amount, and respectively dissolving the rare earth ion oxide and the divalent metal carbonate into dilute HNO3In the solution, heating and stirring are carried out simultaneously until uniform and stable nitrate solutions are formed, the nitrate solutions are mixed, citric acid and polyvinyl alcohol are added, the molar ratio of the citric acid to the polyvinyl alcohol is 2-4: 1, and the mixture is stirred and dissolved to obtain a mixed solution;
step 2, placing the mixed solution in a water bath at 70-90 ℃, slowly evaporating the solvent while stirring to form sol, drying the gel at 120 ℃ for 8-16 hours after gelation to form dry gel, decomposing the gel at 600 ℃ for 2-4 hours after grinding, and performing heat treatment at 800 ℃ for 2-4 hours;
and 3, finally reacting for 6-18 hours at the high temperature of 950-1350 ℃ to obtain the fluorescent powder of the fluorescent material.
9. Use of the indate oxide high efficiency fluorescent material according to any one of claims 1 to 5 in LED lighting, displays.
10. Use of the indate oxide high efficiency fluorescent material according to claim 9, characterized in that:
ultraviolet light with the wavelength ranging from 210nm to 370nm is used as a light source to excite the fluorescent material to emit light efficiently.
11. Use of the indate oxide high efficiency fluorescent material according to claim 9, characterized in that:
in the wavelength range of 300 nm-450 nm, light with characteristic wavelength corresponding to 4f electronic transition of the trivalent rare earth ion activator is used as a light source to excite the fluorescent material to emit light efficiently.
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