CN112143495A - Self-activated luminous fluorescent powder and preparation method thereof - Google Patents
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Abstract
The invention discloses a self-activated luminous fluorescent powder and a preparation method thereof, the self-activated luminous fluorescent powder does not need to be doped with active ions such as rare earth ions, and the use of a large amount of rare earth metal elements is avoided, so that the production cost is lower; the precursor matrix of the self-activated luminescent phosphor is niobium tungstate oxide (Nb)2WO8) The precursor matrix contains two self-activated luminescence centers, namely NbO6Octahedron and WO6The crystal lattice of the precursor matrix is formed by connecting the two octahedrons together in a three-dimensional space, so that the crystal lattice of the precursor matrix has higher strength and is favorable for self-luminous thermal stability, and the self-activated luminous fluorescent powder has the characteristics of good luminous performance, stable light emission and high thermal stability; the preparation method of the self-activated luminescent fluorescent powder has the advantages of simple integral preparation process, easy operation and high implementation feasibility.
Description
Technical Field
The invention belongs to the technical field of inorganic luminescent materials, and particularly relates to self-activated luminescent fluorescent powder and a preparation method thereof.
Background
With the progress of modern science and technology and the rapid development of luminescent display, there is a great demand for various high-efficiency and stable luminescent materials. Most of the current commercial light sources use various phosphors for light conversion, and the phosphors are various in variety, but most of the phosphors adopt rare earth doped tricolor phosphors. The fluorescent powder is based on rare earth luminescence, so the manufacturing cost of the fluorescent powder is high, and the fluorescent powder using a plurality of rare earth materials as the matrix is required to be prepared in a reducing atmosphere, the preparation process is complex and is not easy to control, and the environmental protection is not facilitated. Therefore, a relatively inexpensive luminescent material is sought to replace, and for example, a self-activated phosphor which can emit light without doping rare earth ions is one of the potential alternative materials.
The luminescence center of the general self-activated phosphor is an intrinsic matrix ion or anion group, and because the luminescence center is regularly arranged in a three-dimensional space and has higher concentration relative to the activation center, the luminescence efficiency of the self-activated phosphor is generally lower, and how to improve the luminescence efficiency of the self-activated phosphor is one of the main problems.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the self-activated luminescent fluorescent powder and the preparation method thereof, the self-activated luminescent fluorescent powder does not need to be doped with active ions such as rare earth ions, and the use of a large amount of rare earth metal elements is avoided, so that the production cost is low; the precursor matrix of the self-activated luminescent phosphor is niobium tungstate oxide (Nb)2WO8) The precursor matrix contains two self-activated luminescence centers, namely NbO6Octahedron and WO6The crystal lattice of the precursor matrix is formed by connecting the two octahedrons together in a three-dimensional space, so that the crystal lattice of the precursor matrix has higher strength and is favorable for self-luminous thermal stability, and the self-activated luminous fluorescent powder has the characteristics of good luminous performance, stable light emission and high thermal stability; the preparation method of the self-activated luminescent fluorescent powder has the advantages of simple integral preparation process, easy operation and high implementation feasibility.
In order to achieve the purpose, the technical scheme of the invention is to design the self-activated luminescent fluorescent powder, and the chemical general formula of the self-activated luminescent fluorescent powder is Nb1.5Ta0.5WO8The emission wavelength of the material at room temperature covers a visible light region of 400-700 nm.
The preferred technical scheme is that the self-activated luminescence can be realized by doping Li+Ions and Na+The self-activated luminescent fluorescent powder is doped with Li+Ions and Na+The chemical general formula of the ion is Nb1.5Ta0.5WO8:xLi+:yNa+Wherein x is doped Li+The molar ratio of the ions to W, y being Na+Ion corresponds to the molar ratio of W, 0<x<0.05，0<y<0.05 and x + y is less than or equal to 0.05.
In order to ensure the smooth preparation of the self-activated luminescent phosphor, a method for preparing a self-activated luminescent phosphor is proposed, which comprises the following steps:
s1: according to the chemical formula Nb1.5Ta0.5WO8The stoichiometric ratio of each element in the alloy is measured to respectively contain Nb5+Ionic compound containing Ta5+Ionic compound containing W6+Ionic compounds, or, according to the general chemical formula Nb1.5Ta0.5WO8:xLi+:yNa+The stoichiometric ratio of each element in the alloy is measured to respectively contain Nb5+Ionic compound containing Ta5+Ionic compound containing W6+Ionic compound containing Li+Ionic compound containing Na+Ionic compounds, and then uniformly mixing and grinding the weighed compounds to obtain a raw material mixture;
s2: pre-calcining the raw material mixture obtained in the step S1 for several times in an air atmosphere, wherein the pre-calcining temperature is 500-950 ℃, and the pre-calcining time is 1-10 hours, so as to obtain a pre-calcined mixture;
s3: and (4) calcining the pre-calcined mixture obtained in the step (S2) for several times in the air atmosphere at the calcining temperature of 950-1100 ℃ for 1-10 hours, and naturally cooling to room temperature to obtain the self-activated luminescent phosphor.
Preferably, the Nb content5+The ionic compound is niobium pentoxide, the compound contains Ta5+The ionic compound is tantalum pentoxide, and the W-containing compound6+The ionic compound is ammonium tungstate, and the compound contains Li+Of ionsThe compound is lithium carbonate, and the Na-containing compound+The ionic compound is sodium carbonate.
The invention has the advantages and beneficial effects that:
1. the self-activated luminescent fluorescent powder does not need to be doped with active ions such as rare earth ions, and the use of a large amount of rare earth metal elements is avoided, so that the production cost is low.
2. The precursor matrix of the self-activated luminescent phosphor is niobium tungstate oxide (Nb)2WO8) The precursor matrix contains two self-activated luminescence centers, namely NbO6Octahedron and WO6The crystal lattice of the precursor matrix is formed by connecting the two octahedrons together in a three-dimensional space, so that the crystal lattice of the precursor matrix has higher strength and is favorable for self-luminous thermal stability, and the self-activated luminous fluorescent powder has the characteristics of good luminous performance, stable light emission and high thermal stability.
3. The preparation method of the self-activated luminescent fluorescent powder has the advantages of simple integral preparation process, easy operation and high implementation feasibility: the addition of the monovalent alkali metal ions enables the sintering temperature of the self-activated luminescent fluorescent powder during preparation to be far lower than that of the fluorescent powder of the same type, thereby saving energy and reducing production cost; the self-activated luminescent fluorescent powder does not need protection of inert gas or reducing atmosphere in the preparation process, so that the preparation method of the self-activated luminescent fluorescent powder has far lower requirements on equipment than those of the similar fluorescent powder, and further reduces the production cost and the production difficulty of the self-activated luminescent fluorescent powder.
Drawings
FIG. 1 shows the X-ray powder diffraction pattern of the samples prepared in examples 1 to 5 and PDF #20-1318 (Nb)2WO8) Wherein the chemical formula of sample 1 in example 1 is Nb1.5Ta0.5WO8(ii) a Sample 2 of example 2 has the chemical formula Nb1.5Ta0.5WO8:0.01Li+:0.04Na+(ii) a ExamplesSample 3 of 3 has the chemical formula Nb1.5Ta0.5WO8:0.04Li+:0.01Na+(ii) a Sample 4 of example 4 has the chemical formula Nb1.5Ta0.5WO8:0.02Li+:0.025Na+(ii) a Sample 5 of example 5 has a chemical formula of Nb1.5Ta0.5WO8:0.025Li+:0.025Na+；
FIG. 2 is an SEM photograph of sample 1 prepared in example 1;
FIG. 3 is a luminescence spectrum at an excitation wavelength of 254nm of samples prepared in examples 1 to 5, wherein the chemical formula of sample 1 in example 1 is Nb1.5Ta0.5WO8(ii) a Sample 2 of example 2 has the chemical formula Nb1.5Ta0.5WO8:0.01Li+:0.04Na+(ii) a Sample 3 of example 3 has a chemical formula of Nb1.5Ta0.5WO8:0.04Li+:0.01Na+(ii) a Sample 4 of example 4 has the chemical formula Nb1.5Ta0.5WO8:0.02Li+:0.025Na+(ii) a Sample 5 of example 5 has a chemical formula of Nb1.5Ta0.5WO8:0.025Li+:0.025Na+。
Detailed Description
The following description of the embodiments of the present invention will be made with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Example 1
Sample 1, a chemical formula of which is Nb, was prepared according to the method for preparing a self-activated luminescent phosphor of the present invention1.5Ta0.5WO8The method comprises the following specific operations:
according to the chemical formula Nb1.5Ta0.5WO82.99 g of niobium pentoxide, 1.657 g of tantalum pentoxide and 3.802 g of ammonium tungstate are weighed according to the stoichiometric ratio of the elements; grinding and uniformly mixing the samples, pre-calcining for the first time in an air atmosphere at 500 ℃ for 3 hours, and then coolingCooling to room temperature; taking out the first pre-calcined sample, fully mixing and grinding the samples uniformly, carrying out second pre-calcination in an air atmosphere, cooling the mixture to room temperature to obtain a powdery pre-calcined mixture, wherein the pre-calcination temperature is 850 ℃ and the calcination time is 4 hours; and calcining the pre-calcined mixture for the third time in an air atmosphere at the calcining temperature of 1100 ℃ for 5 hours, and naturally cooling to room temperature to obtain the self-activated luminescent phosphor powder, namely the sample 1.
Referring to FIG. 1, the curve labeled sample 1 is the X-ray powder diffraction pattern of sample 1 prepared in example 1, which is in complete agreement with standard card PDF #20-1318, and shows that sample 1 is a single phase;
referring to the attached figure 2, the SEM test of the sample 1 prepared in the embodiment 1 of the invention shows that the particle size is more than 10-30 μm, and the crystallization is good;
referring to fig. 3, the curve labeled as sample 1 is the luminescence spectrum of sample 1 prepared in example 1 of the present invention, and the result shows that sample 1 emits a broadband spectrum of 400-700 nm at room temperature under the excitation of 254nm ultraviolet light, and the main peak is located at about 505 nm.
Example 2
Sample 2, a chemical formula of which is Nb, was prepared according to the method for preparing self-activated luminescent phosphor of the present invention1.5Ta0.5WO8:0.01Li+:0.04Na+The method comprises the following specific operations:
according to the chemical formula Nb1.5Ta0.5WO8:0.01Li+:0.04Na+Weighing 6.18 g of niobium pentoxide, 3.424 g of tantalum pentoxide, 7.858 g of ammonium tungstate, 0.012 g of lithium carbonate and 0.066 g of sodium carbonate according to the stoichiometric ratio of the elements; grinding and uniformly mixing the samples, then carrying out primary pre-calcination in an air atmosphere, wherein the pre-calcination temperature is 500 ℃, the pre-calcination time is 1 hour, and then cooling to room temperature; taking out the first pre-calcined sample, fully mixing and grinding the samples uniformly, carrying out second pre-calcination in an air atmosphere, cooling the mixture to room temperature to obtain a powdery pre-calcined mixture, wherein the pre-calcination temperature is 850 ℃ and the pre-calcination time is 3 hours; the precalcined mixture is calcined for a third time in an air atmosphere,the calcining temperature is 1050 ℃, the calcining time is 5 hours, and the self-activated luminescent phosphor powder, namely the sample 2, is obtained after natural cooling to the room temperature.
Referring to FIG. 1, the curve labeled sample 2 is the X-ray powder diffraction pattern of sample 2 prepared in example 2, which is in complete agreement with standard card PDF #20-1318, and shows that sample 2 is prepared as a single phase;
referring to fig. 3, the curve labeled as sample 2 is the luminescence spectrum of sample 2 prepared in example 2 of the present invention, and the result shows that under the excitation of 254nm ultraviolet light, sample 2 emits a broadband spectrum of 400-700 nm at room temperature, the main peak is located at about 505nm, and the luminescence intensity of sample 2 is enhanced to a certain extent compared with the curve of sample 1.
Example 3
Sample 3, a chemical formula of which is Nb, was prepared according to the method for preparing self-activated luminescent phosphor of the present invention1.5Ta0.5WO8:0.04Li+:0.01Na+The method comprises the following specific operations:
according to the chemical formula Nb1.5Ta0.5WO8:0.04Li+:0.01Na+5.382 g of niobium pentoxide, 2.983 g of tantalum pentoxide, 6.844 g of ammonium tungstate, 0.04 g of lithium carbonate and 0.014 g of sodium carbonate are weighed respectively according to the stoichiometric ratio of the elements; grinding and uniformly mixing the samples, then carrying out primary pre-calcination in an air atmosphere, wherein the pre-calcination temperature is 550 ℃, the pre-calcination time is 1 hour, and then cooling to room temperature; taking out the first pre-calcined sample, fully mixing and grinding the samples uniformly, carrying out second pre-calcination in an air atmosphere, cooling the mixture to room temperature to obtain a powdery pre-calcined mixture, wherein the pre-calcination temperature is 850 ℃ and the pre-calcination time is 3 hours; and calcining the pre-calcined mixture for the third time in an air atmosphere at 1050 ℃ for 5 hours, and naturally cooling to room temperature to obtain the self-activated luminescent phosphor powder, namely the sample 3.
Referring to FIG. 1, the curve labeled sample 3 is the X-ray powder diffraction pattern of sample 3 prepared in example 3, which is in complete agreement with standard card PDF #20-1318, and shows that sample 3 is prepared as a single phase;
referring to fig. 3, the curve labeled as sample 3 is the luminescence spectrum of sample 3 prepared in example 3 of the present invention, and the result shows that under the excitation of 254nm ultraviolet light, sample 3 emits a broadband spectrum of 400 to 700nm at room temperature, the main peak is located at about 505nm, the luminescence intensity of sample 3 is enhanced to a certain extent compared with the curve of sample 1, and the luminescence intensity of sample 3 is greater than that of sample 2.
Example 4
Sample 4, whose chemical formula is Nb, was prepared according to the method for preparing self-activated luminescent phosphor of the present invention1.5Ta0.5WO8:0.02Li+:0.025Na+The method comprises the following specific operations:
according to the chemical formula Nb1.5Ta0.5WO8:0.02Li+:0.025Na+5.781 g of niobium pentoxide, 3.203 g of tantalum pentoxide, 7.351 g of ammonium tungstate, 0.022 g of lithium carbonate and 0.031 g of sodium carbonate are weighed according to the stoichiometric ratio of the elements; grinding and uniformly mixing the samples, then carrying out primary pre-calcination in an air atmosphere, wherein the pre-calcination temperature is 600 ℃, the pre-calcination time is 3 hours, and then cooling to room temperature; taking out the first pre-calcined sample, fully mixing and grinding the samples uniformly, carrying out second pre-calcination in an air atmosphere, cooling the mixture to room temperature to obtain a powdery pre-calcined mixture, wherein the pre-calcination temperature is 950 ℃ and the pre-calcination time is 7 hours; and calcining the pre-calcined mixture for the third time in the air atmosphere at the calcining temperature of 950 ℃ for 6 hours, and naturally cooling to room temperature to obtain the self-activated luminescent phosphor powder, namely the sample 4.
Referring to FIG. 1, the curve labeled sample 4 is the X-ray powder diffraction pattern of sample 4 prepared in example 4, which is in complete agreement with standard card PDF #20-1318, and shows that sample 4 is prepared as a single phase;
referring to fig. 3, the curve labeled as sample 4 is the luminescence spectrum of sample 4 prepared in example 4 of the present invention, and the result shows that under the excitation of 254nm ultraviolet light, sample 4 emits a broadband spectrum of 400 to 700nm at room temperature, the main peak is located at about 505nm, the luminescence intensity of sample 4 is enhanced to a certain extent compared with the curve of sample 1, and the luminescence intensity of sample 4 is greater than that of sample 3.
Example 5
Sample 5, a chemical formula of which is Nb, was prepared according to the method for preparing self-activated luminescent phosphor of the present invention1.5Ta0.5WO8:0.025Li+:0.025Na+The method comprises the following specific operations:
according to the chemical formula Nb1.5Ta0.5WO8:0.025Li+:0.025Na+4.186 g of niobium pentoxide, 2.321 g of tantalum pentoxide, 5.232 g of ammonium tungstate, 0.021 g of lithium carbonate and 0.028 g of sodium carbonate are respectively weighed according to the stoichiometric ratio of the elements; grinding and uniformly mixing the samples, then carrying out primary pre-calcination in an air atmosphere, wherein the pre-calcination temperature is 600 ℃, the pre-calcination time is 3 hours, and then cooling to room temperature; taking out the first pre-calcined sample, fully mixing and grinding the samples uniformly, carrying out second pre-calcination in an air atmosphere, cooling the mixture to room temperature to obtain a powdery pre-calcined mixture, wherein the pre-calcination temperature is 950 ℃ and the pre-calcination time is 7 hours; and calcining the pre-calcined mixture for the third time in the air atmosphere at the calcining temperature of 950 ℃ for 6 hours, and naturally cooling to room temperature to obtain the self-activated luminescent phosphor powder, namely the sample 5.
Referring to FIG. 1, the curve labeled sample 5 is the X-ray powder diffraction pattern of sample 5 prepared in example 5, which is in complete agreement with standard card PDF #20-1318, and shows that sample 5 is prepared as a single phase;
referring to fig. 3, the curve labeled as sample 5 is the luminescence spectrum of sample 5 prepared in example 5 of the present invention, and the result shows that under the excitation of 254nm ultraviolet light, sample 4 emits a broadband spectrum of 400-700 nm at room temperature, the main peak is located at about 505nm, the luminescence intensity of sample 5 is enhanced to a certain extent compared with the curve of sample 1, and the luminescence intensity of sample 5 is greater than that of sample 4.
The theoretical basis of the self-activated luminescent fluorescent powder of the invention is as follows:
firstly, the precursor matrix is niobium tungstate oxide (Nb)2WO8) The precursor matrix contains two self-activated luminescent materialsCore, i.e. NbO6Octahedron and WO6The structure is easy to transfer energy and disperse energy between each luminescence center by excitation energy under the excitation of external energy, and then luminescence quenching is caused. To prevent this loss of energy, Ta is added to the precursor matrix structure5+Ion substitution of part of Nb5+Ions; similarly, in order to further block energy transfer and enhance self-activated luminescence, the addition of monovalent Li in the gaps of crystal lattice is designed+Ions and Na+Experiments prove that the self-activated luminescence of the fluorescent powder can be observed at room temperature by the design and the modification of the structures, and the self-activated luminescence of the fluorescent powder is enhanced by the doping of the univalent ions.
Next, the precursor matrix (Nb)2WO8) The crystal lattice has higher strength, is favorable for self-luminous thermal stability, and is suitable for being used as a matrix material of rare earth ions.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the technical principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (4)
1. The self-activated luminescent fluorescent powder is characterized in that the chemical general formula of the self-activated luminescent fluorescent powder is Nb1.5Ta0.5WO8The emission wavelength of the material at room temperature covers a visible light region of 400-700 nm.
2. The self-activated light-emitting phosphor of claim 1, wherein the self-activated light emission is capable of being doped with Li+Ions and Na+The self-activated luminescent fluorescent powder is doped with Li+Ions and Na+The chemical general formula of the ion is Nb1.5Ta0.5WO8:xLi+:yNa+Wherein x is doped Li+The molar ratio of the ions to W, y being Na+Ion corresponds to the molar ratio of W, 0<x<0.05，0<y<0.05 and x + y is less than or equal to 0.05.
3. A method for preparing the self-activated luminescent phosphor of any one of claims 1 to 2, comprising the steps of:
s1: according to the chemical formula Nb1.5Ta0.5WO8The stoichiometric ratio of each element in the alloy is measured to respectively contain Nb5+Ionic compound containing Ta5+Ionic compound containing W6+Ionic compounds, or, according to the general chemical formula Nb1.5Ta0.5WO8:xLi+:yNa+The stoichiometric ratio of each element in the alloy is measured to respectively contain Nb5+Ionic compound containing Ta5+Ionic compound containing W6+Ionic compound containing Li+Ionic compound containing Na+Ionic compounds, and then uniformly mixing and grinding the weighed compounds to obtain a raw material mixture;
s2: pre-calcining the raw material mixture obtained in the step S1 for several times in an air atmosphere, wherein the pre-calcining temperature is 500-950 ℃, and the pre-calcining time is 1-10 hours, so as to obtain a pre-calcined mixture;
s3: and (4) calcining the pre-calcined mixture obtained in the step (S2) for several times in the air atmosphere at the calcining temperature of 950-1100 ℃ for 1-10 hours, and naturally cooling to room temperature to obtain the self-activated luminescent phosphor.
4. The method of claim 3 wherein said Nb-containing phosphor is5+The ionic compound is niobium pentoxide, the compound contains Ta5+The ionic compound is tantalum pentoxide, and the W-containing compound6+The ionic compound is ammonium tungstate, and the compound contains Li+The ionic compound is lithium carbonate, and the Na-containing compound+The ionic compound is sodium carbonate.
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