CN114437721B - Rare earth ion Tb 3+ Doped LiTaO 3 Multi-band emission pressure luminescent material and preparation method and application thereof - Google Patents
Rare earth ion Tb 3+ Doped LiTaO 3 Multi-band emission pressure luminescent material and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a rare earth ion Tb 3+ Doped LiTaO 3 Multiband emission pressure luminescent material, preparation method and application thereof, and rare earth ion Tb 3+ Doped LiTaO 3 The chemical general formula of the multiband emission pressure luminescent material is Li 1‑x TaO 3 :xTb 3+ Wherein x is more than or equal to 0.005 and less than or equal to 0.03.
Description
Technical Field
The invention relates to a rare earth ion Tb 3+ Doped LiTaO 3 A multiband emission pressure luminescent material, a preparation method and an application thereof belong to the technical field of optical functional materials and the field of stress luminescence.
Background
The stress luminescent material can release stored energy in a luminescent form under the action of external mechanical stress (such as friction, impact, compression, stretching, bending, twisting, scraping, grinding, cutting, cracking and the like), has wide application prospects in various fields of stress induction, mechanical force driven illumination and display, artificial intelligent skin, structural member safety, health diagnosis and the like, and has attracted extensive attention of researchers at home and abroad. The stress luminescence phenomenon was first discovered and recorded in the sugar crystal mass in 1605 years. In 1998, akiyama et al reported on Sr 3 Al 2 O 6 The green stress luminescence of Eu and Dy fluorescent powder is visible to naked eyes, and the luminescence intensity is close to 500 times of that of sugar crystal blocks (Applied Physics Letters,1998,3046 (73): 3046-3048). Xun superman et al reported orange stress luminescence in ZnS: mn nanoparticle films in 1999 (Journal of the American Ceramic Society,1999,82 (9): 2342-2344). Stress luminescence is subsequently reported in a number of materials in succession.
The currently available relatively efficient inorganic stress-luminescent substrate is strontium aluminate (SrAl) 2 O 4 ) Lithium niobate (LiNbO) 3 ) Zinc sulfide (ZnS) and calcium zinc oxysulfide (CaZnOS). The generation of stress luminescence depends on the host material and the choice of doped luminescent ion, e.g. in SrAl 2 O 4 Mainly by doping divalent europium ions (Eu) 2+ ) To realize green stress luminescence; in LiNbO 3 Mainly by doping with trivalent praseodymium ions (Pr) 3+ ) Red stress luminescence is realized; in ZnS, mainly by doping with transition metal ions (Mn) 2+ ，Cu 2+ ) Red and green stress luminescence is realized. However, the preparation of the above materials is still to be improved, and on the one hand, srAl 2 O 4 :Eu 2+ The synthesis conditions of CaZnOS are complex, atmosphere treatment is needed, the manufacturing cost is further improved, the commercial popularization and application are not facilitated, the waterproof performance of the synthesized product is poor, the optical performance can be greatly reduced by absorbing moisture in the air, and the practical application is limited; on the other hand, most of the existing stress luminescent materials emit light in a single waveband, and generally only show a single emission peak, and most of the materials disappear after a single application of pressure, and the stress luminescent properties can be recovered by using ultraviolet excitation again. Therefore, the development of the stress luminescent material which has high efficiency, stability and multiband emission and can continuously realize stress luminescence has important significance.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a rare earth ion Tb 3+ Doped LiTaO 3 A multiband pressure luminescent material, a preparation method and application thereof.
In one aspect, the invention provides a rare earth ion Tb 3+ Doped LiTaO 3 Multiband emission pressure luminescent material, the rare earth ion Tb 3+ Doped LiTaO 3 The chemical general formula of the multiband emission pressure luminescent material is Li 1-x TaO 3 :xTb 3+ Wherein x is more than or equal to 0.005 and less than or equal to 0.03.
In this disclosure, the doped trivalent rare earth ion Tb 3+ Into LiTaO 3 Substitution of monovalent Li in the host lattice + The ion lattice, which is an imbalance of valence states by valence substitution, results in localized energy states in the forbidden band, i.e., trap levels. The stress luminescence mechanism is electron excited transition after irradiation, and a carrier is captured by a trap energy level and is stably stored. When the applied stress is applied again, the stress,the trap energy level moves to the conduction band due to the distortion of the geometric structure, so that the current carrier can jump to the conduction band and finally return to the ground state to realize stress luminescence corresponding to Tb 3+ The astronomy of (a) inhibits the f-f transition characteristic emission of the ring.
Preferably, x is more than or equal to 0.005 and less than or equal to 0.02, and the stress luminous intensity is firstly enhanced and then weakened, and the best effect is achieved when x =0.01.
Preferably, the rare earth ion Tb 3+ Doped LiTaO 3 The pressure light emission spectrum of the multiband emission pressure light-emitting material is multiband emission from blue light to orange light, the emission center wavelengths are 487nm,541nm,583nm and 618nm respectively and correspond to Tb respectively 3+ Is 5 D 4 → 7 F 6 、 7 F 5 、 7 F 4 And 7 F 3 and (4) transition. Furthermore, the rare earth ions Tb obtained in the invention 3+ Doped LiTaO 3 The multiband emission pressure luminescent material still has excellent luminescent performance after pressure is applied for multiple cycles between 0N and 2000N, and has the advantages of high luminescent intensity, high sensitivity, recoverability and the like (namely, excellent pressure luminescent cycle stability is achieved).
In another aspect, the present invention provides a rare earth ion Tb as described above 3+ Doped LiTaO 3 The preparation method of the pressure luminescent material comprises the following steps:
(1) The lithium source, the tantalum source and the terbium source are Li: ta: tb =1-x: 1;
(2) Calcining the obtained pre-sintering powder at 1000-1400 ℃ in air atmosphere to obtain the rare earth ion Tb 3+ Doped LiTaO 3 A pressure luminescent material.
In the present invention, the lithium source, the tantalum source, and the terbium source are mixed and then subjected to calcination for the purpose of promoting diffusion. Then calcining to make it produce solid-phase reaction so as to obtain rare earth ion Tb 3+ Doped LiTaO 3 A pressure luminescent material.
Preferably, the lithium source is a lithium-containing compound, preferably at least one of lithium oxide, lithium carbonate, lithium nitride and lithium carbide.
Preferably, the tantalum source is a tantalum-containing compound, preferably at least one of tantalum pentoxide and tantalum powder.
Preferably, the terbium source is a terbium-containing compound, preferably at least one of terbium heptaoxide, terbium acetate, terbium sulfate, terbium fluoride and terbium powder.
Preferably, the temperature rise rate of the pre-sintering is 3-10 ℃/min.
Preferably, the pre-sintering time is 2 to 8 hours.
Preferably, the heating rate of the calcination is 2-10 ℃/min.
Preferably, the calcination time is 5 to 15 hours.
In another aspect, the present invention provides a rare earth ion Tb as described above 3+ Doped LiTaO 3 The pressure luminescent material is applied to stress distribution monitoring and failure early warning of organisms, mechanical parts and buildings, stress sensors, stress displays and ultra-precise devices.
Has the beneficial effects that:
the invention provides a novel multiband emission pressure luminescent material and a preparation method thereof, namely trivalent rare earth ions Tb 3+ Doped LiTaO 3 The two-step heat treatment solid phase synthesis method is adopted, the preparation process is simple, no atmosphere treatment is needed, and the preparation condition is easy to control;
in the present invention, liTaO is Tb 3+ The pressure luminescent material has a luminescent spectrum covering multiband emission from blue light to orange light (487nm, 541nm,583nm and 618 nm), still has a luminescent property after pressure is applied for multiple cycles of 0-2000N, and has the advantages of high luminescent intensity, high sensitivity, recoverability and the like.
Drawings
FIG. 1 shows the different doped Tb's obtained in examples 1-4 3+ Concentration of Li 1-x TaO 3 :xTb 3+ (X =0.005, 0.01, 0.015, and 0.02) X-ray diffraction pattern (XRD) of a pressure-emitting material in which LiTaO is inserted at the lowermost side 3 Standard X-ray diffraction spectra of the phases;
FIG. 2 shows the doping of different Tb's obtained in examples 1-4 3+ Concentration of Li 1-x TaO 3 :xTb 3+ (x =0.005, 0.01, 0.015, and 0.02) luminescence spectrum of the stressor phosphor at 2000N pressure;
FIG. 3 shows Li obtained in example 1 0.995 TaO 3 :0.005Tb 3+ (x = 0.005) a luminescence intensity chart of the pressure luminescent material under a cyclic external pressure of 0 to 2000N;
FIG. 4 shows Li obtained in example 2 0.995 TaO 3 :0.01Tb 3+ (x = 0.01) luminescence intensity diagram of the pressure luminescent material under a cyclic external pressure of 0 to 2000N;
FIG. 5 shows Li prepared in example 3 0.995 TaO 3 :0.015Tb 3+ (x = 0.015) luminescence intensity plot of pressure luminescent materials under cyclic external pressure of 0-2000N;
FIG. 6 shows Li obtained in example 4 0.995 TaO 3 :0.02Tb 3+ (x = 0.02) luminescence intensity of the pressure luminescent material under a cyclic external pressure of 0 to 2000N.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
In this disclosure, the rare earth ion Tb 3+ Doped LiTaO 3 The chemical general formula of the multiband emission pressure luminescent material can be Li 1-x TaO 3 :xTb 3+ Wherein the rare earth ion Tb 3+ The value of the mole number x is 0.005-0.03, preferably 0.005-0.02, more preferably 0.0075-0.015, and most preferably x =0.01.
The rare earth ion Tb provided by the present invention is exemplarily illustrated below 3+ Doped LiTaO 3 A method for preparing a multiband emission pressure luminescent material.
Selecting raw materials. A compound containing lithium, tantalum and terbium is selected as a raw material. The lithium-containing compound may be any one of lithium oxide, lithium carbonate, lithium nitride, and lithium carbide. The tantalum-containing compound raw material is any one of tantalum pentoxide and tantalum powder. The terbium-containing compound raw material is any one of terbium heptaoxide, terbium acetate, terbium sulfate, terbium fluoride and terbium powder.
And (4) batching. Weighing and mixing compound raw materials containing lithium, tantalum and terbium according to a molar ratio of 1-x:1, wherein x is not less than 0.005 and not more than 0.03, and uniformly mixing to obtain mixed powder.
And (6) pre-burning. And pre-sintering the mixed powder at 500-900 ℃ in an air atmosphere to obtain the pre-sintered powder. Preferably, after the completion of the calcination, the slurry is cooled and then taken out and polished again. As an example of pre-sintering, raw materials are strictly weighed according to a molar ratio, are uniformly mixed, are put into a muffle furnace to be heated from room temperature to 500-900 ℃ at a heating rate of 3-10 ℃/min, are pre-treated for 2-8 hours in an air atmosphere, and are cooled to obtain pre-sintered powder.
And (4) calcining. Calcining the pre-sintered powder in air atmosphere at the temperature of 1000-1400 ℃; and finally, cooling to room temperature along with the furnace. And grinding the pre-sintered powder again, putting the ground powder into a muffle furnace, heating the ground powder to the calcining temperature of 1000-1500 ℃ from room temperature according to the heating rate of 2-10 ℃/min, and calcining the ground powder for 5-15 hours in the air atmosphere.
In the present invention, liTaO is obtained 3 :Tb 3+ The pressure luminescence spectrum covers multiband emission from blue light to orange light (487 nm,541nm,583nm and 618 nm), still has luminescence performance after pressure is applied for 0-2000N multiple cycles, has the advantages of high luminescence intensity, high sensitivity, restorability and the like, and has important practical application value in application scenes of stress distribution monitoring and failure early warning of organisms, mechanical parts and buildings, stress sensors, stress displays, ultra-precision device processing and the like. Meanwhile, the preparation condition of the invention is mild, the operation is simple, and the scale production is easy to realize.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that insubstantial modifications and adaptations of the invention by those skilled in the art based on the foregoing description are intended to be included within the scope of the invention. The specific process parameters and the like of the following examples are also merely one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1
According to the molar ratio of Li to Ta to Tb =0.995 to 0.005 (equivalent to Tb doping amount x = 0.005), selecting lithium carbonate, tantalum oxide and terbium tetraoxide as raw materials, and respectively weighing the raw materials as 0.3676g, 2.2097g and 0.0094g. Fully grinding the mixture in an agate mortar for 1 hour, and uniformly mixing the mixture to obtain mixed powder. And (3) putting the mixed powder into a muffle furnace, heating from room temperature to 600 ℃ at a heating rate of 5 ℃/min, pretreating for 2 hours in an air atmosphere, and cooling to obtain the pre-sintered powder. Grinding the pre-sintered powder again, putting the powder into a muffle furnace, heating the powder from room temperature to the calcining temperature of 1100 ℃ at the heating rate of 3 ℃/min, calcining the powder for 5 hours in the air atmosphere, and cooling the powder to the room temperature along with the furnace to obtain Li 0.995 TaO 3 :0.005Tb 3+ (x = 0.005) pressure phosphor. The crystallinity of the synthesized powder is high, and the XRD diffraction phase analysis result is shown in figure 1. The detection shows that the pressure luminescent material prepared in this embodiment has a linear light emission peak under a pressure of 2000N, and has a blue light emission at 487nm, a green light emission at 541nm, a yellow light emission at 583nm, and an orange light emission at 618nm, as shown in the analysis result of the pressure emission spectrum shown in fig. 2.
Example 2
On the basis of the embodiment 1, tb is increased 3+ And (4) doping amount. According to the molar ratio of Li to Ta to Tb =0.99 (equivalent to Tb doping amount x = 0.01), selecting lithium carbonate, tantalum oxide and terbium heptaoxide as raw materials, respectively weighing 0.3621g, 2.2097g and 0.0187g, and fully grinding in an agate mortar for 1 hour to uniformly mix the raw materials to obtain a mixed powder. And putting the mixed powder into a muffle furnace, heating from room temperature to 600 ℃ at the heating rate of 5 ℃/min, pretreating for 2h in the air atmosphere, and cooling to obtain the pre-sintered powder. Grinding the pre-sintered powder again, putting the powder into a muffle furnace, heating the powder from room temperature to the calcining temperature of 1100 ℃ at the heating rate of 3 ℃/min, calcining the powder for 5 hours in the air atmosphere, and cooling the powder to the room temperature along with the furnace to obtain Li 0.990 TaO 3 :0.01Tb 3+ (x = 0.01) pressure luminescent powder.The crystallinity of the synthesized powder is high, and shown as the result of XRD diffraction phase analysis shown in figure 1. The detection shows that the pressure luminescent material prepared in this embodiment has a linear light emission peak under a pressure of 2000N, and has a blue light emission at 487nm, a green light emission at 541nm, a yellow light emission at 583nm, and an orange light emission at 618nm, as shown in the analysis result of the pressure emission spectrum shown in fig. 2. And the pressure luminescence intensity is remarkably enhanced compared with that of the embodiment 1.
Example 3
Rare earth ion Tb in this example 3 3+ Doped LiTaO 3 The preparation process of the multiband emission pressure luminescent material is as shown in example 2, and the difference is that: x =0.015. See the XRD diffraction phase analysis results shown in fig. 1. It was detected that the pressure luminescent material prepared in this example 3 has a linear spectrum of the emission peak at 2000N, and has a blue light emission at 487nm, a green light emission at 541nm, a yellow light emission at 583nm, and an orange light emission at 618nm, as shown in the analysis result of the pressure emission spectrum shown in fig. 2.
Example 4
On the basis of the embodiment 2, tb is further increased 3+ And (4) doping amount. According to the molar ratio of Li to Ta to Tb =0.9801 (equivalent to Tb doping amount x = 0.02), lithium carbonate, tantalum oxide and terbium heptaoxide are selected as raw materials, the raw materials are respectively weighed as 0.3584g, 2.2097g and 0.0374g, and fully ground in an agate mortar for 1 hour to be uniformly mixed to obtain mixed powder. And (3) putting the mixed powder into a muffle furnace, heating from room temperature to 600 ℃ at a heating rate of 5 ℃/min, pretreating for 2 hours in an air atmosphere, and cooling to obtain the pre-sintered powder. Grinding the pre-sintered powder again, putting the powder into a muffle furnace, heating the powder from room temperature to the calcining temperature of 1100 ℃ at the heating rate of 3 ℃/min, calcining the powder for 5 hours in the air atmosphere, and cooling the powder to the room temperature along with the furnace to obtain Li 0.980 TaO 3 :0.02Tb 3+ (x = 0.02) pressure luminescent powder. See XRD diffraction phase analysis results shown in FIG. 1. The detection shows that the pressure luminescent material prepared in the embodiment has a linear light spectrum as the luminescent emission peak under the pressure of 2000N, and has blue light emission at 487nm, green light emission at 541nm, yellow light emission at 583nm and orange light emission at 618nmSee the pressure emission spectroscopy results shown in fig. 2.
FIG. 1 shows the doping of different Tb's obtained in examples 1-4 3+ Concentration of Li 1-x TaO 3 :xTb 3+ (X =0.005, 0.01, 0.015, 0.02) X-ray diffraction pattern (XRD) of a pressure luminescent material in which LiTaO is inserted at the lowermost part 3 The standard X-ray diffraction spectrum of the phase shows that the diffraction peak of the synthesized sample corresponds well to the standard card, i.e. the synthesized sample is a pure phase.
FIG. 2 shows the different doped Tb's obtained in examples 1-4 3+ Concentration of Li 1-x TaO 3 :xTb 3+ (x =0.005, 0.01, 0.0015 and 0.02) the luminescence spectrum of the luminescent material under 2000N pressure is linear, and the luminescence emission peak is blue light emission at 487nm, green light emission at 541nm, yellow light emission at 583nm and orange light emission at 618nm, and the four peaks respectively correspond to Tb 3+ The characteristic emission of the ions, and the luminous intensity has a tendency of rising first and falling second along with the doping concentration.
FIGS. 3, 4, 5 and 6 show different doped Tb compounds obtained in examples 1-4 3+ Concentration of Li 1-x TaO 3 :xTb 3+ (x =0.005, 0.01, 0.015, and 0.02) luminescence intensity of a phosphor under a pressure of 10 cycles of 0 to 2000N, from which it is known that stress luminescence is strongest at the first application of a load and then gradually decreases as the number of times of application of the load increases, but still has a certain emission intensity. The material can emit strong pressure luminescence under the action of stress, and still has certain luminescence intensity after ten-cycle compression, namely the pressure luminescence intensity can be recovered, and the material has excellent luminescence recoverability. Meanwhile, after the application of the large stress is finished, the afterglow of the pressure luminescence is quickly attenuated, and the timeliness is realized. By contrast, li 1-x TaO 3 :xTb 3+ (x = 0.01) has an optimum cycling performance, with the highest luminous intensity after 10 applications of pressure.
Finally, it must be said here that: the above embodiments are only used for further detailed description of the technical solutions of the present invention, and should not be understood as limiting the scope of the present invention, and the insubstantial modifications and adaptations made by those skilled in the art according to the above descriptions of the present invention are within the scope of the present invention.
Claims (12)
1. Rare earth ion Tb 3+ Doped LiTaO 3 The multi-band emission pressure luminescent material is characterized in that the rare earth ions Tb 3+ Doped LiTaO 3 The chemical general formula of the multiband emission pressure luminescent material is Li 1-x TaO 3 :xTb 3+ Wherein x is more than or equal to 0.005 and less than or equal to 0.02; the rare earth ion Tb 3+ Doped LiTaO 3 The pressure light emission spectrum of the multiband emission pressure light-emitting material is multiband emission from blue light to orange light, and the emission center wavelengths are 487nm,541nm,583nm and 618nm respectively.
2. Rare earth ion Tb according to claim 1 3+ Doped LiTaO 3 A multiband emission pressure luminescent material, characterized in that x =0.01.
3. A rare earth ion Tb as claimed in claim 1 or 2 3+ Doped LiTaO 3 The preparation method of the pressure luminescent material is characterized by comprising the following steps:
(1) The lithium source, the tantalum source and the terbium source are Li: ta: tb =1-x: 1;
(2) Calcining the obtained pre-sintering powder at 1000-1400 ℃ in air atmosphere to obtain the rare earth ion Tb 3+ Doped LiTaO 3 A pressure luminescent material.
4. The method of claim 3, wherein the lithium source is a lithium-containing compound.
5. The production method according to claim 4, wherein the lithium source is at least one of lithium oxide, lithium carbonate, lithium nitride, and lithium carbide.
6. The method of claim 3, wherein the tantalum source is a tantalum-containing compound.
7. The method of claim 6, wherein the tantalum source is at least one of tantalum pentoxide and tantalum powder.
8. The method of claim 6, wherein the terbium source is a terbium-containing compound.
9. The method of claim 8, wherein the terbium source is at least one of terbium heptaoxide, terbium acetate, terbium sulfate, terbium fluoride and terbium powder.
10. The production method according to claim 3, wherein the temperature increase rate of the pre-firing is 3 to 10 ℃/min; the pre-sintering time is 2-8 hours.
11. The production method according to any one of claims 3 to 10, wherein the temperature increase rate of the calcination is 2 to 10 ℃/min; the calcination time is 5 to 15 hours.
12. A rare earth ion Tb as claimed in claim 1 or 2 3+ Doped LiTaO 3 The pressure luminescent material is applied to stress distribution monitoring and failure early warning of organisms, mechanical parts and buildings, stress sensors, stress displays and ultra-precise devices.
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| CN109135741A (en) * | 2018-07-20 | 2019-01-04 | 同济大学 | A kind of tantalic acid alkali elastic stress luminescent material and preparation method thereof |
| CN110511754A (en) * | 2019-08-23 | 2019-11-29 | 同济大学 | A kind of tantalic acid alkali photostimulated phosphor and preparation method thereof |
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