Orange-red light-emitting fluorescent material and preparation method thereof

Abstract

The application discloses an orange-red light emitting fluorescent material and a preparation method thereof, and belongs to the technical field of photoluminescence fluorescence. 1‑x TaO4:xTb 3+ , 0 < x < 0.005. The Al 1‑x TaO4:xTb 3+ fluorescent material prepared by the solid phase method has multiple light emitting peaks at 400-700 nm, and the proportion determines that the material has orange-red light emitting characteristics.

Description

Technical Field

[0001] This invention belongs to the field of photoluminescence and fluorescence technology, specifically relating to a fluorescent material that emits orange-red light and its preparation method. Background Technology

[0002] Metal oxides, as a new generation of luminescent materials, possess advantages such as high efficiency, high stability, wide emission spectrum, tunability, and broad application areas, making them an ideal choice for various optoelectronic and optical applications. Terbium, an important activator and favorable emission center in solids, exhibits high luminescent efficiency. 3+ The emission can range from blue to green across a large color area, depending on... 5 D3 or 5 D4 energy level. Tb 3+ The ions contain many absorption bands caused by 4f-4f transitions from the near-ultraviolet (UV) to the visible region. Doped Tb 3+ Luminescent materials have been extensively studied. In many hosts, such as phosphates, aluminates, and borates, energy transfer from the host to the activator is efficient, and Tb is induced upon UV excitation. 3+ A powerful launch, but currently there is very little information about Tb. 3+ Reports on the emission of orange-red light by ions. Summary of the Invention

[0003] To address the shortcomings of the existing technologies, this invention proposes a fluorescent material that emits orange-red light and its preparation method.

[0004] To achieve the above objectives, the technical solution adopted by the present invention is as follows: a fluorescent material emitting orange-red light with the chemical formula Al 1-x TaO4: xTb 3+ , 0 < x ≤ 0.005.

[0005] The present invention also claims a method for preparing the orange-red light-emitting fluorescent material comprising: weighing and mixing Al2O3, Ta2O5 and Tb4O7 according to the stoichiometric ratio of the chemical formula, adding anhydrous ethanol and grinding, and then calcining to obtain the orange-red light-emitting fluorescent material.

[0006] In a preferred embodiment of the present invention, the molar ratio of Al2O3, Ta2O5, and Tb4O7 is according to Al 1-x TaO4: xTb 3 + Calculation of stoichiometric ratios for 0 < x ≤ 0.005.

[0007] In a preferred embodiment of the present invention, the total mass of Al2O3, Ta2O5 and Tb4O7 to the volume ratio of anhydrous ethanol is 1 g / (4-7) ml.

[0008] In a preferred embodiment of the present invention, the calcination temperature is 1300-1700℃, the time is 1-10h, and the heating rate is 5℃ / min.

[0009] In a preferred embodiment of the present invention, the grinding time is 20-60 minutes.

[0010] Compared with the prior art, the beneficial effects of the present invention are as follows: The Al described in the present invention 1-x TaO4: xTb 3+ Each Tb in the AlTaO4 matrix of the fluorescent material 3+ It is independent, an independent Tb 3+ The center, under ultraviolet light irradiation, causes the Al 1-x TaO4: xTb 3+ Fluorescent materials have multiple emission peaks in the 400-700 nm range, thus exhibiting orange-red luminescence properties. Attached Figure Description

[0011] Figure 1 The emission spectrum of the orange-red light-emitting fluorescent material prepared in Example 1 of this invention after being excited by a xenon lamp with a wavelength of 302 nm at room temperature.

[0012] Figure 2 The excitation spectrum of the orange-red light-emitting fluorescent material prepared in Example 1 of this invention is shown. Detailed Implementation

[0013] To better illustrate the purpose, technical solution, and advantages of the present invention, the present invention will be further described below in conjunction with specific embodiments.

[0014] In the examples and comparative examples, the purity of Al2O3, Ta2O5, and Tb4O7 was 99.99%.

[0015] Example 1

[0016] A method for preparing an orange-red emitting fluorescent material includes: weighing Al2O3: 49.75 mol, Ta2O5: 50 mol, and Tb4O7: 0.125 mol according to the following ratio, mixing the powder, placing it in an agate mortar, adding anhydrous ethanol dropwise, and grinding for 30 min (the mass ratio of the mixed powder to the volume of anhydrous ethanol is 1 g: 4 mL) until the material is in powder form, then transferring the material to a corundum crucible, placing it in a box furnace at 1600℃ for high-temperature sintering for 4 h, with a heating rate of 5℃ / min, and finally allowing it to cool naturally to room temperature to obtain the orange-red emitting fluorescent material Al2O3. 0.995 TaO4: 0.005Tb 3+ .

[0017] The emission spectrum of the orange-red emitting fluorescent material prepared in Example 1 was measured at room temperature using an F7000 fluorescence spectrophotometer. A xenon lamp source of 302 nm was selected. The results are shown in [Figure number missing]. Figure 1 ,from Figure 1 It can be seen that after 1 minute of excitation by a 302nm xenon lamp, the material has multiple emission peaks in the 400-750nm region, and the proportion of these peaks determines the orange-red color of the sample's emission.

[0018] Further, by detecting at a wavelength of 850 nm, the excitation spectrum (PLE) of the fluorescent material emitting orange-red light can be measured, and the results are shown in [Figure number missing]. Figure 2 As can be seen, there are multiple excitation peaks, which correspond to Tb respectively. 3+ The characteristic excitation peak.

[0019] Comparative Example 1

[0020] A method for preparing a fluorescent material includes: weighing Al2O3:50mol and Ta2O5:50mol according to the following ratio, mixing the mixed powder, placing it in an agate mortar, adding anhydrous ethanol dropwise, and grinding for 30min (the mass ratio of the mixed powder to the volume of anhydrous ethanol is 1g:4mL) until the material is in powder form, then transferring the material to a corundum crucible, placing it in a box furnace at 1600℃ for high-temperature sintering for 4h, with a heating rate of 5℃ / min, and finally allowing it to cool naturally to room temperature to obtain the fluorescent material AlTaO4.

[0021] The fluorescent material AlTaO4 prepared in Comparative Example 1 was excited by a 254nm xenon lamp, thus emitting ultraviolet light.

[0022] Comparative Example 2

[0023] A method for preparing a fluorescent material includes: weighing Al2O3:45mol, Ta2O5:50mol, and Tb4O7:2.5mol according to the following ratio, mixing the powder, placing it in an agate mortar, adding anhydrous ethanol dropwise, and grinding for 30 min (the mass ratio of the mixed powder to the volume of anhydrous ethanol is 1g:7mL) until the material is in powder form, then transferring the material to a corundum crucible, placing it in a box furnace at 1300℃ for high-temperature sintering for 10 h, with a heating rate of 5℃ / min, and finally allowing it to cool naturally to room temperature to obtain the fluorescent material Al2O3. 0.99 TaO4: 0.01Tb 3+ .

[0024] The fluorescent material prepared in Comparative Example 2, when excited by a 302 nm xenon lamp, exhibits high fluorescence intensity due to Tb. 3+ Green emission occurs through cross-relaxation interactions between them.

[0025] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A method for preparing an orange-red light-emitting fluorescent material, characterized in that, include: Al₂O₃, Ta₂O₅, and Tb₄O₇ were weighed and mixed according to their stoichiometric ratios, then anhydrous ethanol was added, and the mixture was ground before calcination to obtain an orange-red emitting fluorescent material. The stoichiometric ratio of the chemical formulas is Al 3+ Ta 5+ :Tb 3+ The molar ratio is (1-x):1:x, where 0 < x ≤ 0.

005.

2. The method for preparing the orange-red light-emitting fluorescent material as described in claim 1, characterized in that, The total mass of Al2O3, Ta2O5 and Tb4O7 to the volume ratio of anhydrous ethanol is 1 g / (4-7) ml.

3. The method for preparing the orange-red light-emitting fluorescent material as described in claim 1, characterized in that, The calcination temperature is 1300-1700℃, the time is 1-10h, and the heating rate is 5℃ / min.

4. The method for preparing the orange-red light-emitting fluorescent material as described in claim 1, characterized in that, The grinding time is 20-60 minutes.

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