CN112662396A - Solid solution type red long-afterglow luminescent material and preparation method thereof - Google Patents
Solid solution type red long-afterglow luminescent material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a solid solution type red long afterglow luminescent material, the chemical formula of which is Ca2‑x‑ySrxSmySnO4X is 0.001 to 0.1, and y is 0.001 to 0.01. The series of solid solution type red long-afterglow luminescent materials can be prepared by changing the Sr content, multiple red long-afterglow luminescent materials can be simultaneously prepared in a single system, the series of long afterglow luminescent materials are prepared by a high temperature solid phase method, the preparation method is simple in process and high in material stability, and the series of solid solution type red long afterglow luminescent materials prepared at the same time are high in afterglow luminescent intensity and long in afterglow time and have wide application value.
Description
Technical Field
The invention relates to a solid solution type red long-afterglow luminescent material and a preparation method thereof, belonging to the technical field of rare earth luminescent materials.
Background
There is a material in the luminescent material which can continuously emit light for a certain period of time after stopping the excitation of the external light source, and we refer to as a long afterglow luminescent material. The long afterglow materials can still be used after repeated excitation, and are mostly non-toxic and harmless inorganic non-metallic materials, so the long afterglow materials have continuously paid attention to a plurality of fields. Long afterglow materials were first used for low illumination and night signs; with the research of the long afterglow materials, the long afterglow materials are also widely applied to the fields of radiation detection, optical storage media, biological imaging and medicine. The afterglow material which is used for commercial use at first is sulfide, which is also the long afterglow material with the longest research time, but is less used at present because the afterglow time is shorter and the chemical stability is poor, so the afterglow material is easy to generate pollution.
The long afterglow material is a multifunctional energy storage material, can store energy when irradiated by natural light or ultraviolet light, and can continuously emit light after the irradiation of an excitation source is stopped. Because of the unique optical characteristics, the long afterglow material is widely noticed as an energy-saving and environment-friendly material and is widely applied in actual life. The long afterglow material is ZnS and CaS for the first application, and then in 1993, the discovery of aluminate long afterglow replaces sulfide long afterglow and opens up a new era for the application of the long afterglow material. With the development of economic society, the market demand for the long afterglow materials is huge at present.
At present, the research on the long afterglow materials at home and abroad mainly focuses on the development of novel materials, especially the development and research on the red long afterglow materials. For example, the red long afterglow material prepared in application publication No. CN 101524189B has the characteristics of simple preparation process and long afterglow time. The novel red long afterglow material prepared in the application publication No. CN 01138881.1 has the characteristics of low synthesis temperature and high afterglow brightness. The Eu ion-doped red long-afterglow phosphor prepared in application publication No. CN 102148858.4 has the characteristics of ultra-wide emission and excellent afterglow performance. However, the red long afterglow materials researched at present are single materials mainly comprising sulfide, have narrow application range, are easy to counterfeit and are not environment-friendly. The development of a series of red long afterglow materials not only can broaden the variety of the red long afterglow materials, but also has better security performance.
Found in experiments that Ca2-x-ySrxSmySnO4Solid solution type red long afterglow luminescent materialsThe crystal shape is not uniform, and the afterglow time becomes short with the increase of the storage time.
Disclosure of Invention
The purpose of the invention is as follows: solve the problem of Ca2-x-ySrxSmySnO4The problem that the crystal shape of the solid solution type red long afterglow luminescent material is not single and the afterglow time is shortened along with the prolonging of the storage time is solved, and the stable solid solution type red long afterglow luminescent material is provided.
The applicant found that: the preparation of various solid solutions can be realized through ion substitution, the possibility of preparing series red long afterglow materials can be realized simultaneously by adopting the preparation method of the ion substituted solid solution in a single red long afterglow material, the ionic radii of Ca and Sr ions are similar, solid solution substitution can be realized in the high temperature solid phase method reaction, and finally the solid solution substituted red long afterglow material is prepared.
The technical scheme adopted by the invention is as follows:
a solid solution type red long-afterglow luminescent material with chemical formula of Ca2-x-ySrxSmySnO4Wherein x is 0.001 ≦ 0.1, and y is 0.001 ≦ 0.01.
Preferably, x of the solid solution type red long afterglow luminescent material of the present invention is any value of 0.005 to 0.08.
Preferably, y of the solid solution type red long afterglow luminescent material of the present invention is 0.005.
Preferably, x and y of the solid solution type red long afterglow phosphor of the present invention are respectively 0.005 ≦ x ≦ 0.08, and 0.004 ≦ y ≦ 0.008.
When the value of x is 0.001 to 0.01, the solid solution type red long afterglow luminescent material of the invention forms a series of solid solutions, and can realize the preparation of a series of materials.
When the y value of the solid solution type red long afterglow luminescent material is 0.005, the red long afterglow luminescent material has the optimal afterglow luminescent intensity and the optimal afterglow decay time.
When the red luminescent material is prepared, the Sm and Sr codoping method is adopted, so that the prepared red long afterglow luminescent material has better crystallinity, high afterglow luminescent intensity and longer afterglow attenuation.
The preparation method of the solid solution type red long afterglow luminescent material comprises the following steps:
step 2, pre-sintering: in an air atmosphere muffle furnace, heating to 800 ℃ for presintering, and keeping the temperature for 6 hours;
and 3, sintering: grinding the obtained materials, heating to 1200-1400 ℃ in a muffle furnace in air atmosphere, sintering, keeping the temperature for 6 hours, cooling to room temperature, and grinding to obtain the solid solution type red long-afterglow luminescent material.
In the preparation method, Sr and Sm are codoped in the step 1, and boric acid is used as a fluxing agent to reduce the material synthesis temperature.
According to the preparation method, the crystallinity of the material is improved through pre-sintering in the step 2.
Preferably, in the preparation method of the invention, in the step 1, the boric acid (H) with the mass percentage of 6.0 percent of the mixture of the above 4 materials is added3BO3) The crystal form is used as a fluxing agent and plays a decisive role in the singleness and stability of the crystal form.
Drawings
FIG. 1 is an emission spectrum of the red long-afterglow materials prepared in examples 1 to 5, which shows that the prepared red long-afterglow materials show red luminescence;
FIG. 2 is an XRD pattern of the red long afterglow materials prepared in examples 1-5, and the diffraction peak intensity at each angle is high, indicating that the crystallinity is good and a good single phase is formed; example 1 the XRD pattern of the sample was the same as that of example 2.
FIG. 3 is the data of XRD patterns of 45.4-47 deg. for the red long afterglow materials prepared in examples 1-5, compared with the standard card, the diffraction peak is shifted to a low angle, indicating the formation of solid solution; example 1 sample profile the same as example 2 samples.
FIG. 4 is an afterglow decay curve of the red long afterglow materials prepared in examples 1-5, which shows that the materials have excellent afterglow performance; the sample of example 1 has the same decay curve as the sample of example 2.
FIG. 5 is the emission spectrum of the red long afterglow materials prepared in examples 1-5, which shows that the prepared red long afterglow material shows red luminescence, and the emission spectrum of the sample of example 1 is the same as that of the sample of example 2.
FIG. 6 is an XRD of the red long afterglow phosphors prepared in comparative examples 1, 2 and 3, and a part of the impurity phase appears in all three comparative examples.
FIG. 7 is the long afterglow decay curves of the red long afterglow materials prepared in comparative examples 1, 2 and 3, wherein the afterglow performance of the three comparative examples is decreased.
Has the advantages that: the solid solution type red long afterglow luminescent material has the advantages of high afterglow luminescent intensity, long afterglow time and stability, and can realize the preparation of series red long afterglow luminescent materials. The solid solution type red long-afterglow luminescent material can be used as an anti-counterfeiting material.
The solid solution type red long afterglow luminescent material has the following advantages:
the red long afterglow substrate used in the patent technology of the invention is Ca2SnO4It has the advantages of high temperature resistance, stable chemical property, no toxicity, etc. On the basis of doping red luminescence center Sm, a series of red long afterglow materials can be simultaneously prepared by adopting a method of substituting Ca by Sr, and the materials have similar chemical and physical properties and can be better applied to actual production.
Detailed Description
The present invention is further illustrated by the following specific examples, all of which use high purity chemical materials as raw materials.
Example 1
Weighing CaCO3(4N)2mol,SnO2(4N)1mol,Sm2O3 0.0025mol,SrCO30.006mol, adding boric acid (4N) with the mass percentage of the mixture of the 4 materials being 6 percent; the raw materials are uniformly mixed in air and then are put into an alumina crucible, the mixture is heated to 800 ℃ in an air atmosphere muffle furnace for presintering, the heat preservation time is 6 hours, the mixture is naturally cooled to room temperature, the obtained material is uniformly ground and then is put into the alumina crucible, the mixture is heated to 1200 ℃ to 1400 ℃ in the air atmosphere furnace for sintering, the heat preservation time is 6 hours, the obtained material is ground, and then the red long afterglow material can be prepared, the excitation emission spectrum of the red long afterglow material is shown in figure 1, and the red long afterglow material can show red luminescence.
Example 2
Weighing CaCO3(4N)2mol,SnO2(4N)1mol,Sm2O3 0.0005mol,SrCO30.001mol, and adding boric acid (4N) with the mass percentage of the mixture of the 4 materials being 6%; the raw materials are uniformly mixed in air and then are put into an alumina crucible, the mixture is heated to 800 ℃ in an air atmosphere muffle furnace for presintering, the heat preservation time is 6 hours, the mixture is naturally cooled to room temperature, the obtained material is uniformly ground and then is put into the alumina crucible, the mixture is heated to 1200 ℃ to 1400 ℃ in the air atmosphere furnace for sintering, the heat preservation time is 6 hours, the obtained material is ground, and then the red long afterglow material can be prepared, the XRD pattern of the embodiment 2 is shown in figure 2, and as can be seen from figure 2, the red long afterglow material has no impure phase, better crystallinity and good single phase formation; the XRD pattern data is shown in figure 3 at 45.4-47 degrees, and the XRD diffraction peak is shifted to the left relative to the standard card, which shows that the good solid solution is obtained in the embodiment; the long afterglow decay curve is shown in figure 4, and the long afterglow luminescence property is excellent; the emission spectrum is shown in fig. 5, from which it can be seen that red luminescence appears.
Example 3
Weighing CaCO3(4N)2mol,SnO2(4N)1mol,Sm2O3 0.0025mol,SrCO30.005mol, adding boric acid (4N) with the mass percentage of the mixture of the 4 materials being 6 percent; the raw materials are evenly mixed in the air and then put into an alumina crucible, the mixture is pre-sintered in an air atmosphere muffle furnace after being heated to 800 ℃, the heat preservation time is 6 hours,naturally cooling to room temperature, uniformly grinding the obtained materials, putting the materials into an alumina crucible, heating to 1200-1400 ℃ in an air atmosphere furnace for sintering, preserving heat for 6 hours, grinding the obtained materials to obtain the red long afterglow material, wherein an XRD (X-ray diffraction) spectrum of the red long afterglow material is shown in figure 2, and the red long afterglow material has no impurity phase, has good crystallinity and forms a good single phase as can be seen from figure 2; the XRD pattern data is shown in figure 3 at 45.4-47 degrees, and the XRD diffraction peak is shifted to the left relative to the standard card, which shows that the good solid solution is obtained in the embodiment; the long afterglow decay curve is shown in figure 4, and the long afterglow luminescence property is excellent; the emission spectrum is shown in fig. 5, from which it can be seen that red luminescence appears.
Example 4
Weighing CaCO3(4N)2mol,SnO2(4N)1mol,Sm2O3 0.0025mol,SrCO30.01mol, adding boric acid (4N) with the mass percentage of the mixture of the 4 materials being 6 percent; uniformly mixing the raw materials in air, putting the mixture into an alumina crucible, heating the mixture to 800 ℃ in an air atmosphere muffle furnace for presintering, preserving the heat for 6 hours, naturally cooling the mixture to room temperature, uniformly grinding the obtained material, putting the ground material into the alumina crucible, heating the mixture to 1200-1400 ℃ in the air atmosphere muffle furnace for sintering, preserving the heat for 6 hours, grinding the obtained material to obtain a red long afterglow material, wherein an XRD (X-ray diffraction) spectrum of the red long afterglow material is shown in figure 2, and as can be seen from figure 2, the red long afterglow material has no impurity phase, good crystallinity and good single phase formation; the XRD pattern data is shown in figure 3 at 45.4-47 degrees, and the XRD diffraction peak is shifted to the left relative to the standard card, which indicates that a good solid solution is obtained; the long afterglow decay curve is shown in figure 4, the long afterglow luminescence property is excellent, the emission spectrum is shown in figure 5, and the red luminescence is shown in the figure.
Example 5
Weighing CaCO3(4N)2mol,SnO2(4N)1mol,Sm2O3 0.005mol,SrCO30.01mol, adding boric acid (4N) with the mass percentage of the mixture of the 4 materials being 6 percent; the raw materials are evenly mixed in the air and then are put into an alumina crucible, in an air atmosphere muffle furnace,heating to 800 ℃ for presintering, keeping the temperature for 6h, naturally cooling to room temperature, uniformly grinding the obtained material, putting the ground material into an alumina crucible, heating to 1200-1400 ℃ in an air atmosphere furnace for sintering, keeping the temperature for 6h, and grinding the obtained material to obtain a red long afterglow material; the XRD spectrum is shown in figure 2, and as can be seen from figure 2, no impurity phase appears, the crystal property is better, and a good single phase is formed; the XRD pattern data of the product of the embodiment is 45.4-47 degrees as shown in figure 3, and the XRD diffraction peak is shifted to the left relative to the standard card, which shows that a good solid solution is obtained; the long afterglow decay curve is shown in figure 4, and the long afterglow luminescent material has excellent long afterglow luminescent performance; the emission spectrum is shown in fig. 5, where it can be seen that red luminescence appears.
Comparative example 1 reference is made to example 3.
Weighing CaCO3(4N)2mol,SnO2(4N)1mol,Sm2O3 0.0025mol,SrCO30.005mol, adding boric acid with the mass percentage of 4.5 percent of the mixture of the above 4 materials; the raw materials are uniformly mixed in air and then are put into an alumina crucible, the temperature is raised to 800 ℃ in an air atmosphere muffle furnace for presintering, the heat preservation time is 6 hours, the mixture is naturally cooled to room temperature, the obtained material is uniformly ground and then is put into the alumina crucible, the temperature is raised to 1200 ℃ to 1400 ℃ in the air atmosphere furnace for sintering, the heat preservation time is 6 hours, the obtained material is ground, the red long afterglow material is obtained, the XRD pattern of the red long afterglow material is shown in figure 6, and partial impurity phases appear. The long afterglow decay curve is shown in figure 7, and the afterglow performance is reduced.
Comparative example 2 reference is made to example 3.
Weighing CaCO3(4N)2mol,SnO2(4N)1mol,Sm2O3 0.0025mol,SrCO30.005mol, adding boric acid with the mass percent of the mixture of the 4 materials being 8 percent; uniformly mixing the raw materials in air, putting the mixture into an alumina crucible, heating the mixture to 800 ℃ in an air atmosphere muffle furnace for presintering, preserving the heat for 6 hours, naturally cooling the mixture to room temperature, uniformly grinding the obtained material, putting the ground material into the alumina crucible, heating the ground material to 1200-1400 ℃ in the air atmosphere furnace for sintering, preserving the heat for 6 hours, and obtaining the productGrinding the materials to obtain the red long afterglow material, wherein the XRD pattern is shown in figure 6, and partial impure phases appear. The long afterglow decay curve is shown in figure 7, and the afterglow performance is reduced.
Comparative example 3 reference example 3 no pre-sintering procedure.
Weighing CaCO3(4N)2mol,SnO2(4N)1mol,Sm2O3 0.0025mol,SrCO30.005mol, adding boric acid (4N) with the mass percentage of the mixture of the 4 materials being 6 percent; the raw materials are evenly mixed in air and then put into an alumina crucible, the mixture is heated to 1200 ℃ to 1400 ℃ in a muffle furnace with air atmosphere for sintering, the temperature is kept for 6 hours, the obtained materials are ground, the red long afterglow material is obtained, the XRD pattern of the red long afterglow material is shown in figure 6, and partial impure phases appear. The long afterglow decay curve is shown in figure 7, and the afterglow performance is reduced.
Test example:
20g of the products obtained in examples 1 to 5 and comparative examples 1 to 3 were spread on an open petri dish, and then stored in a constant temperature and humidity cabinet at a temperature of 30 ℃ and a relative humidity of 65%. The afterglow time was measured after the end of month 8, and the results are shown in Table 1.
The afterglow time is measured by using a Hitachi F-4600 fluorescence spectrophotometer, exciting for 10min at 250nm and observing the afterglow condition at 580 nm.
TABLE 1
| Afterglow time of 0 day, hour | Afterglow time at end of month 8, h | |
| Example 1 product | 7.2 | 7.3 |
| EXAMPLE 2 product | 7.1 | 7.2 |
| EXAMPLE 3 product | 7.6 | 7.5 |
| EXAMPLE 4 product | 7.8 | 7.7 |
| EXAMPLE 5 product | 7.0 | 7.0 |
| Comparative example 1 product | 5.0 | 3.5 |
| Comparative example 2 product | 6.6 | 4.2 |
| Comparative example 3 product | 5.4 | 3.8 |
Claims (6)
1. A solid solution type red long afterglow luminescent material is characterized in that the chemical formula is as follows: ca2-x-ySrxSmySnO4Wherein x is 0.001 ≦ 0.1, and y is 0.001 ≦ 0.01.
2. The solid solution type red long afterglow luminescent material of claim 1, wherein x is any value of 0.005 to 0.08.
3. The solid solution type red long afterglow luminescent material of claim 1, wherein y is 0.005.
4. The solid solution-type long red afterglow phosphor of claim 1, wherein x and y are in the range of 0.005 ≦ x ≦ 0.08, and 0.004 ≦ y ≦ 0.008, respectively.
5. The method for preparing a solid solution type red long afterglow luminescent material of any one of claims 1 to 5, comprising the steps of:
step 1, weighing: with CaCO3、SnO2、SrCO3And Sm2O3Weighing raw materials according to the composition of a chemical structural formula and a stoichiometric ratio, mixing, adding H with the mass percentage of 6% in the mixture of the 4 materials3BO3Making fluxing agent, and grinding uniformly in air;
step 2, pre-burning: in an air atmosphere muffle furnace, heating to 800 ℃ for presintering, and keeping the temperature for 6 hours;
and 3, sintering: grinding the obtained materials, heating to 1200-1400 ℃ in a muffle furnace in air atmosphere, sintering, keeping the temperature for 6 hours, cooling to room temperature, and grinding to obtain the solid solution type red long-afterglow luminescent material.
6. The method of claim 5, wherein: in the step 1, Sr and Sm are co-doped.
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| CN104774613A (en) * | 2015-03-17 | 2015-07-15 | 同济大学 | Stannate based elastic stress luminescent material, preparation method, and applications thereof |
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| CN101565614A (en) * | 2009-04-30 | 2009-10-28 | 兰州大学 | Orange-red long afterglow Luminescent Material |
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