CN113150781A - High-thermal-stability continuous phase-change solid solution mineral fluorescent powder and application thereof - Google Patents
High-thermal-stability continuous phase-change solid solution mineral fluorescent powder and application thereof Download PDFInfo
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Abstract
The invention discloses high-thermal stability continuous phase change solid solution mineral fluorescent powder and application thereof, wherein the fluorescent powder comprises beta-Ca 3(PO4)2The fluorescent powder is doped with rare earth ions, and the rare earth ions are Sr2+Ions, the phosphor makes Ca by a cation structure regulation method2+Ions and Sr2+The substitution ratio of the ions is 1:1 and is synthesized by a high-temperature solid-phase method. The invention is at Ca2+/Sr2+The PL intensity can be strongest at a ratio of 1:1, the thermal stability is improved at a phosphor operating temperature of 150 ℃, i.e., 419.2K, and TCP represented by x ═ 1.5: the PL intensity of the Ce phosphor decreased only to 87.92% of the initial emission intensity, the QY increased from a minimum of 38.81% to 49.99%, the initial intensity remained 81% after 60min of continuous electron irradiation, and the CL initial intensity remained 79% after 90 min.
Description
Technical Field
The invention belongs to the technical field of fluorescent powder optimization, and particularly relates to high-thermal-stability continuous phase change solid solution mineral fluorescent powder and application thereof.
Background
The rare earth ion doped phosphate luminescent material has the characteristics of low sintering temperature, good chemical stability, strong ultraviolet near-ultraviolet light region absorption and the like. The whitlockite and the apatite are representatives of phosphate mineral luminescent materials, but compared with the apatite, the whitlockite structure has lower synthesis temperature and richer and more adjustable crystallographic lattice. The whitlockite matrix has a rhombohedral structure and belongs to the R3c space group, Z being 21.
Due to much of Eu2+The emission color of the activated whitlockite phosphor can be tuned on a large scale by cation/anion substitution or solid solution methods. For example, Ce3+Ion pair Ca2+The isomorphic substitution of ions can realize tunable color emission in beta-TCP fluorescent powder and can adjust and optimize the luminous performance of the whitlockite fluorescent powder, but Sr is doped into the whitlockite fluorescent powder2+The research of (2) is rare. Therefore, a high thermal stability continuous phase change solid solution mineral phosphor and application thereof are needed.
Disclosure of Invention
The invention provides Ce3+The high-thermal stability continuous phase change solid solution mineral fluorescent powder with obviously improved multi-aspect luminescence performance and the application are realized.
The invention includes beta-Ca3(PO4)2The fluorescent powder is doped with rare earth ions, and is characterized in that the rare earth ions are Ca2+Ions and Sr2+Ions, the phosphor makes Ca by a cation structure regulation method2+Ions and Sr2+The substitution ratio of the ions is 1:1 and is synthesized by a high-temperature solid-phase method.
Further, the fluorescent powder satisfies the following formula and comprises Ca3-xSrx(PO4)2:0.07Ce3+(x＝0,0.5,1,1.5,2,2.5,3)。
Further, the structure of the fluorescent powder is a phase transition solid solution with space groups of R3c and R3 m.
Furthermore, the excitation spectrum of the fluorescent powder is short-wave ultraviolet light in the range of 240nm-330nm, and the emission peak position is 366 nm.
The invention has the beneficial effects that:
the invention is at Ca2+/Sr2+The PL intensity can be strongest at a ratio of 1:1, the thermal stability is improved at a phosphor operating temperature of 150 ℃, i.e., 419.2K, and TCP represented by x ═ 1.5: the PL intensity of the Ce phosphor decreased only to 87.92% of the initial emission intensity, the QY increased from a minimum of 38.81% to 49.99%, the initial intensity remained 81% after 60min of continuous electron irradiation, and the CL initial intensity remained 79% after 90 min. .
Drawings
Fig. 1 shows a CMP with a standard PDF card attached: a schematic diagram of an XRD (X-ray diffraction) spectrum of Ce fluorescent powder;
fig. 2 is a TCP: the Rietveld structure diagram of xCe;
fig. 3 is a TCP: schematic representation of 31P solid state Magic Angle Spin Nuclear Magnetic Resonance (MASNMR) spectra of xCe;
fig. 4 is (a) TCP calculated from DFT: band structure and band state density spectrum of x Ce (x ═ 1.5). TCP: ce belongs to an indirect bandgap semiconductor with an energy band gap of 5.039eV, and is suitable as a host material of phosphor.
In fig. 5, (a) TCP: excitation spectrum (PL) diagram of xce;
(b) TCP: schematic of the emission spectrum (PLE) of x Ce;
in fig. 6, (a) TCP: 1.5 temperature dependent emission spectrum schematic of Ce;
(b) TCP: a schematic diagram of the temperature-dependent luminous intensity and CIE chromaticity coordinate of xCe phosphor;
(c) TCP monitored at 366nm (λ ex ═ 310 nm): schematic attenuation curves in xCe phosphor;
(d) TCP: schematic diagram of variation of quantum yield QY of xCe;
in fig. 7, (a) TCP: 1.5 SEM and CL map of Ce phosphor particles illustrates the schematic;
(b) TCP under continuous electron beam bombardment time at 8kV, 80 mA: 1.5 CL spectrum and CL intensity trend diagram of Ce;
(c) TCP: 1.5 CL intensity of Ce vs probe current (fixed acceleration voltage: 8 kV);
(d) TCP: 1.5Ce (fixed probe current: 60mA) in the CL intensity acceleration voltage.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
The invention includes beta-Ca3(PO4)2The fluorescent powder is doped with rare earth ions, and the rare earth ions are Ca2+Ions and Sr2+Ions, the phosphor makes Ca by a cation structure regulation method2+Ions and Sr2+The substitution ratio of the ions is 1:1 and is synthesized by a high-temperature solid-phase method. The raw material adopts CaCO3(≥99.9％)、SrCO3(≥99.9％)、(NH4)2HPO4(≥99.9％)、(99.9％)、CeO2(≥99.99％)，Ca2+Ions and Sr2+The substitution ratio of the ions was 1:1, weighed according to the stoichiometric ratio, mixed in an agate mortar, and ground thoroughly for 30 minutes. Placing the mixture in a corundum crucible, preheating at 850 deg.C for 1h, and releasing NH in a muffle furnace in air3、H2O and CO2. After regrinding, at 5% H2、95％N2Is placed in a tube furnace and sintered for 10 hours at 1250 ℃. After slowly cooling to room temperature, the product was ground into a fine powder for subsequent characterization. The obtained chemical formula is Ca3-xSrx(PO4)2:0.07Ce3+(x is 0,0.5,1,1.5,2,2.5,3), the structure of the phosphor is a phase transition intermediate solid solution with space groups of R3c and R3m, the phosphor can be well excited by short-wave ultraviolet light in the range of 240nm-330nm, and the emission peak position is about 366 nm. In Ca2+And Sr2+The PL intensity is optimized at a substitution ratio of 1: 1. The thermal stability is good, and the PL intensity is only reduced to 87.92 percent of the initial emission intensity at the working temperature of 150 ℃ of the LED. The high-strength high-.
The fluorescent powder can be placed under short-wave ultraviolet light to see remarkable blue-violet fluorescence, and can be applied to field emission display FED, anti-counterfeiting and encrypted patterns and preparation of near ultraviolet insect-expelling LED devices.
Fig. 1 shows a CMP with a standard PDF card attached: the XRD pattern of the Ce fluorescent powder proves that the fluorescent powder is a single-phase whitlockite type mineral, phase change is generated in the process of gradually increasing x (Sr), and five Ca sites, Ca, are arranged at the asymmetric part of a unit cell2+All sites of the ion are covered by Ca2+/Sr2+Ion occupancy. The fluorescent powder of the invention belongs to a continuous phase change solid solution. End part Ca3(PO4)2And Sr3(PO4)2Crystallized in the steric groups R3c and R3m, respectively. The structure is a phase transition intermediate solid solution with space groups of R3c and R3m, the excitation spectrum is short-wave ultraviolet light in the range of 240nm-330nm, and the emission peak position is 360nm-370 nm. In Ca2+And Sr2+The substitution ratio of (a) to (b) is 1: 1. Various cation sites can be occupied by rare earth ions, alkali metal ions, transition metal ions and the like, so that the luminous performance of the whitlockite fluorescent powder can be adjusted and optimized.
To further prove the confidence of the conclusions, the patent uses the Vienna simulation package (VASP) code to calculate the TCP based on the Density Functional Theory (DFT): lattice structure and electronic structure of x Ce (x ═ 1.5). In order to determine the optimum, a formula is used to calculate the formation energy E for different doping conditions.
0.5-3mol
E＝E(Final)-E(Origin)-μCe+μSr (1)
As shown in table 1, where e (final) and e (origin) are the total energy of the doped crystal and the perfect crystal, respectively. μ Ce and μ Sr are the chemical potentials of the added atoms Ce and Sr. The calculation results show that the energy difference of formation of 5 cation positions is not large, and all the positions are probably determined according to Ce3+The reasonableness of occupation.
TABLE 1 DFT calculation of 5 Ce' s3+A formation energy E occupying a different crystal position.
For TCP: xCe series of phosphors, terminal Ca3(PO4)2And Sr3(PO4)2Crystallized in the steric groups R3c and R3m, respectively. Therefore, it is speculated that samples of composition between the two end members would prefer to form a partial solid solution rather than a complete solid solution. These two crystal structures differ from each other in several respects. The R3c structure has no inversion center, but exists at R-3 m. Furthermore, the cell volume of the R3c phase is much larger than that of the R-3m phase, which means that the number of different positions of Sr/Ca ions in the unit cell independent portion of the R3c phase is larger than that of the R-3m phase. Furthermore, this refinement indicates that there is a difference in anionic polyhedra between them: the composition of R3c contains three kinds of [ PO ]4]Groups, and only one [ PO ] is present in the composition in R-3m4]A group.
Shown in fig. 2 is TCP: a refined view of the Rietveld structure of xCe: (a) x is 0.5; (b) x is 1; (c) x is 1.5; (d) x is 2; (e) x is 2.5; (f) the method comprises the following steps Unit cell volume v (x) is linearly dependent. V (x) increases linearly with increasing x (Sr), and Sr2+Ion greater than Ca2+The fact of ions is very consistent, and the linear trend proves that the real chemical composition of the fluorescent powder obtained by the patent is close to a theoretical value.
To observe the difference, proceed31P solid state Magic Angle Spin Nuclear Magnetic Resonance (MASNMR) studies. In Ca3(PO4)2Multiple peaks can be obviously observed, and multiple [ PO ] exists in the structure of R-3c4]The groups are identical. However, as Sr concentration increased, these peaks gradually blurred and completely transformed into a sharp peak at x ═ 3, indicating the presence of only one P position in the R-3m structure, sufficiently suggesting that the initial Ca was present3(PO4)2The structure is transformed. Thus, Ca3(PO4)2Should be structurally different from Sr3(PO4)2A new phase (solid solution) of (1). In addition, the chemical shift of P and the increase in Sr content exhibited almost continuous changes, and were completely transformed in Sr3(PO4)2, forming two types of crystal structures. Based on this, it is presumed that the solid solubility limit under the synthesis conditions is aboutx > 2.5 and confirms the credibility of the current conclusion.
Calculating the band structure and the band state density of the matrix material according to DFT, wherein TCP: ce belongs to an indirect bandgap semiconductor, and the energy band gap is 5.039eV, which is close to the practical value calculated by DRS test. The valence band top is mainly formed by Op, and the conduction band bottom is mainly formed by Cad, so that photoluminescence generated by electron transition can be well matched. The results show that the material is suitable as a matrix material of the fluorescent powder.
Shown in fig. 3 is TCP: of xCe31P solid state Magic Angle Spin Nuclear Magnetic Resonance (MASNMR) spectra. The chemical shift of P and the increase of Sr content show almost continuous change, and the Sr content is increased3(PO4)2The two types of crystal structures are formed by complete transformation, and the structure of the series of fluorescent powder is proved to be a continuous phase change solid solution.
Based on this, Ca is selected3(PO4)2(when x is 0,2.5]) And Sr3(PO4)2(when x ═ 3) was used as the parent phase as the initial model for Rietveld structure refinement, which was performed using TOPAS 4.2. TCP: the xCe crystal structure diagram shows that there are five Ca sites in the asymmetric part of the unit cell, Ca2+All sites of the ion are covered by Ca2+/Sr2+Ion occupancy. Overall, the progressive substitution of Ca by Sr results in a diffraction peak moving towards a smaller 2 θ angle, with a significant phase change from R-3c to R-3m with x ═ 3, and v (x) increasing linearly with increasing x (Sr), which is in contrast to Sr2+Ion greater than Ca2+The fact of ions is very consistent, and the linear trend proves that the real chemical composition of the fluorescent powder obtained by the patent is close to a theoretical value. When x is from 0 to 2.5, all peaks are indexed by rhomboidal cells (R3c), the parameters corresponding to Ca3(PO4)2(PDF #09-0169) except that the diffraction peaks were found to shift to smaller 2 θ angles. However, when the cation sites are all occupied by Sr (x ═ 3), a significant phase transition occurs, where the parameters correspond to Sr3(PO4)2And can be well fitted by diamond shaped cells in the spatial population R-3 m.
Shown in fig. 4 are (a) TCP calculated from DFT: band structure and band state density spectrum of x Ce (x ═ 1.5). TCP: ce belongs to an indirect bandgap semiconductor with an energy band gap of 5.039eV, and is suitable as a host material of phosphor.
TCP: ce phosphor exhibited broadband excitation (PLE) spectra, demonstrating that all TCPs: the Ce fluorescent powder can be well excited by short-wave ultraviolet light in the range of 240nm-330nm, the emission (PL) peak position is about 366nm, the Ce fluorescent powder belongs to near ultraviolet excited purple light emission, and the Ce fluorescent powder has application prospects as fluorescent powder and anti-counterfeiting materials. It is noteworthy that for x ≦ 1, there are three excitation peaks, and for 1 < x ≦ 2.5, there are two significant excitation peaks, with relatively weak excitation peak intensity at 260nm and slightly higher excitation peak intensity at 310 nm. When x is 3, there is only one significant excitation peak, which again verifies that structural changes cause changes in the photoexcitation peak. Furthermore, the emission spectrum shows that as the Sr/Ca ratio increases, the total excitation band intensity increases first and then decreases. When x is 1.5, the sample yields the highest PL intensity, determined at Ce3+When the doping concentration of the ions is 0.07mol, the optimal substitution ratio of Ca2+ and Sr2+ is 1: 1.
In general, the temperature dependence of the phosphors is important because the emission intensity of most phosphors decreases if the operating temperature exceeds a certain value due to the temperature quenching effect. The phosphor prepared for the LED must maintain stable emission efficiency for a long period of time at a temperature of about 150 ℃. Thus, testing of TCP: the trend of the temperature-dependent emission spectrum and the CIE chromaticity coordinates of the Ce samples between 77.2K and 500K. At 310nm excitation, the emission spectrum intensities of all 7 samples show a tendency of gradual blue shift in the position of the strongest peak with a slow decrease in temperature from room temperature. Represented by x ═ 1.5, TCP: the emission spectrum intensity of the Ce fluorescent powder is slowly reduced along with the increase of the temperature. TCP represented by x ═ 1.5 at the higher temperature of 150 ℃, i.e., 419.2K, at which the LED operates: the PL intensity of the Ce phosphor decreased only to 87.92% of the initial emission intensity. Clearly, good color stability and emission intensity stability indicate that TCP: the Ce fluorescent powder has good thermal stability to temperature quenching effect.
It was determined that the fluorescence lifetime of Sr-substituted samples with different ratios also showed a tendency to increase and then decrease, and 29, 30, 32, 31, 22ns respectively correspond to x being 0,0.5,1,1.5,2,2.5,3, and it is reasonable that the decay time varies with the variation of the luminous intensity. Next, the quantum yield QY gradually increased with Sr substitution from 38.90% (x ═ 0, 0.5), to 44.18% (x ═ 1), 49.99% (x ═ 1.5), then gradually decreased to 38.81% (x ═ 2), 37.52% (x ═ 2.5), 30.37% (x ═ 3). From the above results, it can be concluded that the cation substitution structure control method is optimal in the light emitting property at a Ca/Sr ratio of 1:1, in consideration of the comprehensive light emitting intensity, thermal stability, fluorescence lifetime, and quantum efficiency.
Fig. 5 shows (a) TCP: excitation spectrum (PL) of xce; (b) TCP: emission spectrum (PLE) of Ce. All the TCPs: the Ce fluorescent powder can be well excited by short-wave ultraviolet light in the range of 240nm-330nm, the emission (PL) peak position is about 366nm, the Ce fluorescent powder belongs to near ultraviolet excited purple light emission, and the Ce fluorescent powder has application prospects as fluorescent powder and anti-counterfeiting materials.
In order to try the multifunctional use of the mineral phosphors, the cathodoluminescent properties of the phosphors were also tested, TCP: SEM and corresponding CL mapping images of Ce (x ═ 1.5) samples were observed, the samples showed uniform emission, and again the Ce was confirmed3+The ions are uniformly distributed in the sample. The degradation performance of the phosphor in FED applications is of critical importance.
And testing TCP: and the decay behavior of xCe (x ═ 1.5) fluorescent powder under the condition of continuous electronic bombardment of I ═ 80mA, Va ═ 8 kV. Obviously, the CL intensity of the phosphor gradually decreased with increasing bombardment time, but due to its dense and stable crystal structure, it maintained 81% of the initial intensity after 60min of continuous electron irradiation and 79% of the initial intensity after 90 min. The decrease in CL intensity is primarily due to the accumulation of surface carbon during electron beam bombardment. It is well known that graphitic carbon build-up occurs during electron beam irradiation at high current densities, which reduces the number of excited electrons reaching the phosphor particles and also increases the conductivity of the sample surface, thereby severely affecting the CL intensity of the phosphor. Obviously, experiments at appropriate times (90min) showed that TCP: the xCe fluorescent powder has good stability in CL intensity under the bombardment of low-voltage electron beams, and shows potential advantages in FED application.
Fig. 6 shows (a) TCP: 1.5 temperature dependent emission spectrum of Ce; (b) TCP: the temperature-dependent luminous intensity and CIE chromaticity coordinate of the xCe fluorescent powder; (c) TCP monitored at 366nm (λ ex ═ 310 nm): attenuation curves and calculated lifetimes in xCe phosphors; (d) TCP: change in quantum yield QY of xCe. It shows that at the higher operating temperature of the LED, i.e. 419.2K, TCP, represented by x ═ 1.5: the PL intensity of the Ce phosphor decreased only to 87.92% of the initial emission intensity. Good color stability and emission intensity stability indicate that TCP: the Ce fluorescent powder has good thermal stability to temperature quenching effect. The quantum yield QY increases optimally from 38.90% (x ═ 0, 0.5) to 49.99% (x ═ 1.5) with Sr substitution.
And testing TCP: the CL intensity of Ce (x ═ 1.5) varied with the acceleration voltage (fixed probe current: 60mA) and probe current (fixed acceleration voltage: 8 kV). The CL intensity gradually increased with increasing probe current and accelerating voltage, but the spectral shape and peak position did not change significantly, both showing two broad bands at 370nm and 700nm, with the strongest emission peak of 370 nm. Furthermore, no saturation effect was detected when the probe current was increased at a fixed applied voltage. It is well known that decay time is a key parameter in determining whether a phosphor has a saturation effect. The shorter the decay time of the activated ions, the more excitation/emission cycles within the pulsed electron beam time, the less likely saturation effects will occur. TCP: the attenuation curve of xCe is plotted in logarithmic form, which fits well to a second order exponential function, with a mean lifetime calculated as 32ns, which is small compared to some reported phosphors (several to several hundred microseconds), etc. Therefore, due to Ce3+Decay time is very short, TCP: there is no saturation effect in Ce phosphor, indicating that it is more effective for the application of FEDs.
The PL strength can be strongest at a Ca/Sr ratio of 1:1, the thermal stability is improved at a phosphor operating temperature of 150 ℃, i.e., 419.2K, and TCP represented by x ═ 1.5: the PL intensity of the Ce phosphor decreased only to 87.92% of the initial emission intensity, and QY increased from a minimum of 38.81% to 49.99%. After 60min of continuous electron irradiation, 81% of the initial intensity was maintained, and after 90min, 79% of the initial intensity of CL was maintained. In addition, due to Ce3+Decay time is very short, TCP: the Ce fluorescent powder has no saturation effect, which shows that the Ce fluorescent powder is more effective for the application of FEDs and shows potential advantages in field emission displays. The enhancement of the luminous intensity, QY and thermal stability and good CL performance prove the effectiveness of the method and have the potential of being applied to other white apatite phosphors.
Fig. 7 shows (a) TCP: 1.5 SEM and CL map of Ce phosphor particles; (b) TCP under continuous electron beam bombardment time at 8kV, 80 mA: 1.5 the CL spectrum and CL intensity variation trend of Ce; TCP: the CL intensity of 1.5Ce varies with (c) the probe current (fixed acceleration voltage: 8kV) and (d) the acceleration voltage (fixed probe current: 60 mA). The inset shows the change in CL intensity with increasing filament current and accelerating voltage, respectively. After 60min of continuous electron irradiation, 81% of the initial intensity was maintained, and after 90min, 79% of the initial intensity of CL was maintained. In addition, since Ce3+ has a very short decay time, TCP: the Ce fluorescent powder has no saturation effect, which shows that the Ce fluorescent powder is more effective for the application of FEDs and shows potential advantages in field emission displays. In addition, due to Ce3+Extremely short decay time, TCP: the absence of CL saturation effect in Ce phosphor indicates that it is more effective for FEDs applications, showing potential advantages in field emission displays. The enhancement of the luminous intensity, QY and thermal stability and good CL performance prove the effectiveness of the method and have the potential of being applied to other white apatite phosphors.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (4)
1. A high-thermal stability continuous phase-change solid solution mineral fluorescent powder contains beta-Ca3(PO4)2The fluorescent powder is doped with rare earth ions, and is characterized in that the rare earth ions are Sr2+Ion(s)The phosphor enables Ca to be generated by a cation structure regulation method2+Ions and Sr2+The substitution ratio of the ions is 1:1 and is synthesized by a high-temperature solid-phase method.
2. The mineral phosphor of claim 1, wherein the phosphor satisfies the following formula and contains Ca3-xSrx(PO4)2:0.07Ce3+(x＝0,0.5,1,1.5,2,2.5,3)。
3. The high thermal stability continuous phase transition solid solution mineral phosphor of claim 1, wherein the structure of the phosphor is an intercrystalline solid solution with space groups R3c and R3 m.
4. The mineral phosphor powder with high thermal stability and continuous phase transition solid solution in the claim 1, is characterized in that the excitation spectrum of the phosphor powder is short-wave ultraviolet light in the range of 240nm to 330nm, and the emission peak position is 366 nm.
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| CN111978961A (en) * | 2020-09-10 | 2020-11-24 | 山东大学 | Preparation method of phosphate luminescent material with adjustable luminescent color and luminescent material prepared by method |
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| CN111978961A (en) * | 2020-09-10 | 2020-11-24 | 山东大学 | Preparation method of phosphate luminescent material with adjustable luminescent color and luminescent material prepared by method |
Non-Patent Citations (3)
| Title |
|---|
| HAIPENG JI等: "Cation Substitution Dependent Bimodal Photoluminescence in Whitlockite Structural Ca3–xSrx(PO4)2:Eu2+ (0 ≤ x ≤ 2) Solid Solution Phosphors", 《INORG. CHEM.》 * |
| HAIPENG JI等: "Discovery of New Solid Solution Phosphors via Cation Substitution- Dependent Phase Transition in M3(PO4)2:Eu2+ (M = Ca/Sr/Ba) Quasi-Binary Sets", 《J. PHYS. CHEM. C》 * |
| YULI YUAN等: "A novel blue-purple Ce3þ doped whitlockite phosphor:Synthesis, crystal structure, and photoluminescence properties", 《JOURNAL OF RARE EARTHS》 * |
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