CN117229776A - Rare earth doped magnesium tantalate UVA luminescent fluorescent powder - Google Patents
Rare earth doped magnesium tantalate UVA luminescent fluorescent powder Download PDFInfo
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- CN117229776A CN117229776A CN202311185730.9A CN202311185730A CN117229776A CN 117229776 A CN117229776 A CN 117229776A CN 202311185730 A CN202311185730 A CN 202311185730A CN 117229776 A CN117229776 A CN 117229776A
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- 239000000843 powder Substances 0.000 title claims abstract description 37
- CJXLIMFTIKVMQN-UHFFFAOYSA-N dimagnesium;oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Mg+2].[Mg+2].[Ta+5].[Ta+5] CJXLIMFTIKVMQN-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 10
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 8
- 239000011777 magnesium Substances 0.000 claims abstract description 80
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 5
- 238000003746 solid phase reaction Methods 0.000 claims abstract description 3
- 238000004020 luminiscence type Methods 0.000 claims description 59
- 150000001875 compounds Chemical class 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 6
- -1 magnesium tantalate compound Chemical class 0.000 claims description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 5
- 238000001514 detection method Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 241000238631 Hexapoda Species 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 2
- 238000001308 synthesis method Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 230000005284 excitation Effects 0.000 description 37
- 238000010521 absorption reaction Methods 0.000 description 34
- 238000002441 X-ray diffraction Methods 0.000 description 18
- 238000000862 absorption spectrum Methods 0.000 description 18
- 238000000695 excitation spectrum Methods 0.000 description 18
- 238000001748 luminescence spectrum Methods 0.000 description 18
- 238000002360 preparation method Methods 0.000 description 18
- 238000002835 absorbance Methods 0.000 description 17
- 239000012071 phase Substances 0.000 description 17
- 230000009286 beneficial effect Effects 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 238000007689 inspection Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 6
- 230000006378 damage Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000010431 corundum Substances 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 1
- 229910017493 Nd 2 O 3 Inorganic materials 0.000 description 1
- 208000019155 Radiation injury Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses rare earth doped magnesium tantalate UVA luminescent fluorescent powder. The chemical composition expression of the UVA fluorescent powder is Mg 4 Ta 2 O 9 0.25at% RE, wherein RE is La 3+ 、Ce 3+ 、Pr 3+ 、Nd 3+ 、Sm 3+ 、Eu 3+ 、Gd 3+ 、Tb 3+ 、Dy 3+ 、Ho 3+ 、Er 3+ 、Tm 3+ 、Yb 3+ 、Lu 3+ 、Y 3+ And Sc (Sc) 3+ At least one of them. The UVA fluorescent powder is synthesized by adopting a high-temperature solid-phase reaction method, stably exists in the air, and has safe and simple process and easy control. The emission wavelength of the vacuum ultraviolet excited UVA fluorescent powder is adjustable within the range of 360-392 nm, and the luminous peak intensity is commercial blue fluorescent powder BaMgAl 10 O 17 :Eu 2+ (BAM) 1.275-4.575 times.
Description
Technical Field
The invention relates to rare earth doped magnesium tantalate UVA luminescent fluorescent powder, and belongs to the technical field of vacuum ultraviolet luminescent materials.
Background
According to different biological effects, ultraviolet rays are divided into four wave bands according to wavelengths: long wave UVA, medium wave UVB, short wave UVC, and vacuum wave UVD. The longer the wavelength, the more transmissive. The long wave UVA has a wavelength of 320-400 nm, has strong penetrating power, can penetrate glass, even 9 feet of water, can be coated on the inner wall of a glass lampshade by virtue of the band luminescent material, can be used for manufacturing trap lamps, nondestructive inspection lamps, fluorescent leakage detection lamps, degreasing cleaning lamps, criminal and forensic inspection lamps, laboratory inspection lamps and the like according to different emission wavelengths, and can also be used for ore identification, anti-counterfeiting verification, banknote inspection, element solidification and the like. Currently, development of UVA phosphors that are environmentally friendly and tunable in the emission wavelength range to be suitable for different applications is of great importance in production and life.
Mg 4 Ta 2 O 9 Is a novel vacuum ultraviolet excited UVA luminescent material with the density of 6.2g/cm 3 The effective atomic number is 59.6g/mol, the decay time is 4.5 mu s, the thermal stability is good, the radiation damage resistance threshold is high, the vacuum ultraviolet region has a strong excitation peak at about 160nm and a strong emission peak at 366nm, and the luminous intensity is greatly improved by doping rare earth ions and adjusting the luminous wavelength of UVA, so that the doped magnesium tantalate becomes a potential novel vacuum ultraviolet excited UVA luminous material similar to the application of mercury-free fluorescent lamps.
Disclosure of Invention
The invention solves the technical problems that: how to improve Mg 4 Ta 2 O 9 The luminous intensity of the fluorescent material.
To solve the aboveThe technical problem is that the invention provides an application of a vacuum ultraviolet excited rare earth doped magnesium tantalate compound as UVA fluorescent powder, wherein the chemical composition expression of the magnesium tantalate niobate compound is Mg 4 Ta 2 O 9 0.25at% RE, wherein RE is La 3+ 、Ce 3+ 、Pr 3+ 、Nd 3+ 、Sm 3+ 、Eu 3+ 、Gd 3+ 、Tb 3+ 、Dy 3+ 、Ho 3+ 、Er 3+ 、Tm 3+ 、Yb 3+ 、Lu 3+ 、Y 3+ And Sc (Sc) 3+ At least one of them.
Preferably, the emission wavelength of the magnesium tantalate niobate compound is 360-392 nm, the magnesium tantalate niobate compound is in a UVA region, and the luminous peak intensity is commercial blue fluorescent powder BaMgAl 10 O 17 :Eu 2+ (BAM) 1.275-4.575 times.
Preferably, the application of the rare earth doped magnesium tantalate compound as UVA fluorescent powder comprises the following steps: the lamp is applied to insect guiding lamps, black light lamps and flaw detection lamps.
Preferably, the magnesium tantalate niobate compound is synthesized by adopting a high-temperature solid phase reaction method, and the specific synthesis method comprises the following steps:
weighing MgO and Ta as raw materials according to stoichiometric ratio according to chemical composition expression 2 O 5 And trivalent rare earth oxide, grinding and mixing uniformly; and then the obtained mixture is orderly presintered and calcined in air atmosphere, naturally cooled to room temperature and ground.
Preferably, the MgO is added in an excess of 3at% relative to the standard stoichiometric ratio;
and/or, the presintering temperature is 1250 ℃ and the presintering time is 12 hours;
and/or the calcination temperature is 1350 ℃ for 24 hours.
The invention uses Mg 4 Ta 2 O 9 As a matrix, different trivalent rare earth ions with concentration of 0.25at% are doped, and Mg is prepared by a high-temperature solid-phase synthesis method 4 Ta 2 O 9 RE 0.25at%, adjustable emission wavelength in 360-392 nm, light emitting band in UVA area (320-400 nm) and highest light emitting intensityTo Mg (Mg) 4 Ta 2 O 9 3.588 times BAM, and is resistant to thermal injury and radiation injury. Thus, the UVA fluorescent powder Mg 4 Ta 2 O 9 RE is used as UVA luminescent material excited by vacuum ultraviolet, has the advantages of heat damage resistance and radiation damage resistance, is coated on the inner wall of a glass lampshade, can be used for manufacturing trap lamps, nondestructive inspection lamps, fluorescent leakage detection lamps, degreasing cleaning lamps, criminal and forensic inspection lamps, laboratory inspection lamps and the like according to different emission wavelengths, and can also be used for ore identification, anti-counterfeiting verification, banknote inspection, element solidification and the like.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention provides Mg 4 Ta 2 O 9 RE is used as UVA fluorescent powder, and has the advantages of thermal degradation resistance, radiation damage resistance and stable luminescence property;
(2) The luminous intensity of the vacuum ultraviolet excited UVA fluorescent powder is the comparative sample BaMgAl 10 O 17 :Eu 2+ 1.275-4.575 times of (BAM) blue fluorescent powder, wherein (Mg 0.9975 Ho 0.0025 ) 4 Ta 2 O 9 The highest luminous intensity of the (B) is that of a comparative sample BaMgAl 10 O 17 :Eu 2+ (BAM) 4.575 times; the emission wavelength of the UVA fluorescent powder is adjustable within the range of 360-392 nm, and the UVA fluorescent powder has wide application prospect in the fields of trap lamps, nondestructive inspection lamps, black light lamps and the like;
(3) The preparation method is simple, the preparation and use conditions are simple, and the mass industrialized production is easy to realize.
Drawings
FIG. 1 is a commercially available BaMgAl 10 O 17 :Eu 2+ (BAM) X-ray diffraction (XRD) pattern of blue fluorescent powder, diffraction peak and standard card (PDF # 26-0163) are in one-to-one correspondence;
FIG. 2 shows Mg prepared in each example 4 Ta 2 O 9 X-ray diffraction (XRD) pattern of 0.25at% RE, wherein RE is La 3+ 、Ce 3+ 、Pr 3+ 、Nd 3+ 、Sm 3+ 、Eu 3+ 、Gd 3+ 、Tb 3+ 、Dy 3+ 、Ho 3+ 、Er 3+ 、Tm 3+ 、Yb 3+ 、Lu 3+ 、Y 3+ And Sc (Sc) 3+ ;
FIGS. 3a-f are Mg prepared in various examples 4 Ta 2 O 9 0.25at% RE and commercial blue phosphor BaMgAl for comparison 10 O 17 :Eu 2+ Vacuum ultraviolet excitation spectrum and corresponding luminescence spectrum of (BAM);
FIGS. 4a-r are Mg prepared in various examples 4 Ta 2 O 9 0.25at% RE and commercial blue phosphor BaMgAl for comparison 10 O 17 :Eu 2+ An absorption spectrum of the UV-Vis Band of (BAM).
Detailed Description
In order to make the invention more comprehensible, preferred embodiments accompanied with figures are described in detail below.
In the following examples, commercial blue phosphor BaMgAl was used for comparison of luminescence properties 10 O 17 :Eu 2+ (BAM)。
Example 1
MgO and Ta are respectively weighed according to the stoichiometric ratio of 4.12:1.00 2 O 5 Grinding the raw materials in an agate mortar, adding absolute ethyl alcohol as a dispersing agent, uniformly grinding, loading into a corundum crucible, presintering for 12 hours at 1250 ℃ in an air atmosphere, naturally cooling to room temperature, pouring the raw materials into the agate mortar, continuously and fully grinding, loading into the corundum crucible, sintering for 24 hours at 1350 ℃ in the air atmosphere, naturally cooling to room temperature, and uniformly grinding to obtain the product.
The X-ray diffraction pattern of the product is shown in FIG. 2, and all diffraction peaks correspond to standard diffraction peaks (PDF#38-1458), indicating that single-phase Mg is synthesized 4 Ta 2 O 9 Fluorescent powder. Vacuum ultraviolet excitation spectrum and corresponding luminescence spectrum of the product are shown in figure 3a, mg 4 Ta 2 O 9 Vacuum ultraviolet excitation peak is 160nm, the excitation peak covers 130-170 nm wave band, and the corresponding luminescence peak positionAt 364nm, the emission peak covers a wave band of 300-500 nm, and the intensity of the emission peak is that of a comparative sample BaMgAl 10 O 17 :Eu 2+ (BAM) 1.275 times. The strong excitation band of the commercial BAM fluorescent powder covers 120-175 nm, 147nm excitation is adopted, the emission peak is positioned at 450nm, and the band of 400-525 nm is covered. The absorption spectrum of the UV-Vis band (220-800 nm) of the product is shown in FIG. 4b, mg 4 Ta 2 O 9 The absorbance near 364nm of the luminescence peak is very low, and the absorption cut-off edge is positioned at 337nm, thereby being beneficial to avoiding the self absorption of luminescence photons.
Example 2
MgO, ta are respectively weighed according to the stoichiometric ratio of 4.110:1.000:0.005 2 O 5 ,La 2 O 3 Product (Mg) 0.9975 La 0.0025 ) 4 Ta 2 O 9 The preparation method is the same as in example 1.
The X-ray diffraction pattern of the product is shown in FIG. 2, and all diffraction peaks correspond to standard diffraction peaks (PDF#38-1458), indicating a synthetic single phase (Mg 0.9975 La 0.0025 ) 4 Ta 2 O 9 Fluorescent powder. The vacuum ultraviolet excitation spectrum and the corresponding luminescence spectrum of the product are shown in figure 3d, (Mg) 0.9975 La 0.0025 ) 4 Ta 2 O 9 The vacuum ultraviolet excitation peak is 160nm, the excitation peak covers 130-170 nm wave band, the corresponding luminescence peak is 360nm, the emission peak covers 300-500 nm wave band, and the luminescence peak intensity is the comparison sample BaMgAl 10 O 17 :Eu 2+ (BAM) 2.450 times. The absorption spectrum of the UV-Vis band (220-800 nm) of the product is shown in FIG. 4k, (Mg) 0.9975 La 0.0025 ) 4 Ta 2 O 9 The absorbance near 360nm of the luminescence peak is very low, and the absorption cut-off edge is positioned at 322nm, thereby being beneficial to avoiding the self absorption of luminescence photons.
Example 3
MgO, ta are respectively weighed according to the stoichiometric ratio of 4.110:1.000:0.005 2 O 5 ,Ce 2 O 3 Product (Mg) 0.9975 Ce 0.0025 ) 4 Ta 2 O 9 The preparation method is the same as in example 1.
X of the productThe ray diffraction pattern is shown in FIG. 2, and all diffraction peaks correspond to standard diffraction peaks (PDF#38-1458), indicating a synthetic single phase (Mg 0.9975 Ce 0.0025 ) 4 Ta 2 O 9 Fluorescent powder. The vacuum ultraviolet excitation spectrum and the corresponding luminescence spectrum of the product are shown in figure 3d, (Mg) 0.9975 Ce 0.0025 ) 4 Ta 2 O 9 The vacuum ultraviolet excitation peak is 160nm, the excitation peak covers 130-170 nm wave band, the corresponding luminescence peak is 390nm, the emission peak covers 300-550 nm wave band, the luminescence peak intensity is the comparison sample BaMgAl 10 O 17 :Eu 2+ (BAM) 2.913 times. The absorption spectrum of the UV-Vis band (220-800 nm) of the product is shown in FIG. 4l, (Mg) 0.9975 Ce 0.0025 ) 4 Ta 2 O 9 The absorbance near 390nm of the luminescence peak of (C) is very low, and the absorption cut-off edge is positioned at 403nm, thereby being beneficial to avoiding the self absorption of luminescence photons.
Example 4
MgO, ta are respectively weighed according to the stoichiometric ratio of 4.110:1.000:0.005 2 O 5 ,Pr 2 O 3 Product (Mg) 0.9975 Pr 0.0025 ) 4 Ta 2 O 9 The preparation method is the same as in example 1.
The X-ray diffraction pattern of the product is shown in FIG. 2, and all diffraction peaks correspond to standard diffraction peaks (PDF#38-1458), indicating a synthetic single phase (Mg 0.9975 Pr 0.0025 ) 4 Ta 2 O 9 Fluorescent powder. The vacuum ultraviolet excitation spectrum and the corresponding luminescence spectrum of the product are shown in figure 3a, (Mg) 0.9975 Pr 0.0025 ) 4 Ta 2 O 9 The vacuum ultraviolet excitation peak is 160nm, the excitation peak covers 130-170 nm wave band, the corresponding luminescence peak is 372nm, the emission peak covers 300-500 nm wave band, and the luminescence peak intensity is the comparison sample BaMgAl 10 O 17 :Eu 2+ (BAM) 2.488 times. The absorption spectrum of the UV-Vis band (220-800 nm) of the product is shown in FIG. 4m, (Mg) 0.9975 Pr 0.0025 ) 4 Ta 2 O 9 The absorbance near 372nm of the luminescence peak is very low, and the absorption cut-off edge is positioned at 332nm, which is favorable for avoiding luminescence lightAnd (5) sub-self-absorption.
Example 5
MgO, ta are respectively weighed according to the stoichiometric ratio of 4.110:1.000:0.005 2 O 5 ,Nd 2 O 3 Product (Mg) 0.9975 Nd 0.0025 ) 4 Ta 2 O 9 The preparation method is the same as in example 1.
The X-ray diffraction pattern of the product is shown in FIG. 2, and all diffraction peaks correspond to standard diffraction peaks (PDF#38-1458), indicating a synthetic single phase (Mg 0.9975 Nd 0.0025 ) 4 Ta 2 O 9 Fluorescent powder. The vacuum ultraviolet excitation spectrum and the corresponding luminescence spectrum of the product are shown in figure 3f, (Mg) 0.9975 Nd 0.0025 ) 4 Ta 2 O 9 Vacuum ultraviolet excitation peak is 160nm, excitation peak covers 130-170 nm wave band, corresponding luminescence peak is 386nm, emission peak covers 300-500 nm wave band, and luminescence peak intensity is comparative sample BaMgAl 10 O 17 :Eu 2+ 3.613 times (BAM). The absorption spectrum of the UV-Vis band (220-800 nm) of the product is shown in FIG. 4n, (Mg) 0.9975 Nd 0.0025 ) 4 Ta 2 O 9 The absorbance near 386nm of the luminescence peak is very low, and the absorption cut-off edge is positioned at 321nm, thereby being beneficial to avoiding the self absorption of luminescence photons.
Example 6
MgO, ta are respectively weighed according to the stoichiometric ratio of 4.110:1.000:0.005 2 O 5 ,Sm 2 O 3 Product (Mg) 0.9975 Sm 0.0025 ) 4 Ta 2 O 9 The preparation method is the same as in example 1.
The X-ray diffraction pattern of the product is shown in FIG. 2, and all diffraction peaks correspond to standard diffraction peaks (PDF#38-1458), indicating a synthetic single phase (Mg 0.9975 Sm 0.0025 ) 4 Ta 2 O 9 Fluorescent powder. The vacuum ultraviolet excitation spectrum and the corresponding luminescence spectrum of the product are shown in figure 3b, (Mg) 0.9975 Sm 0.0025 ) 4 Ta 2 O 9 Vacuum ultraviolet excitation peak is 160nm, excitation peak covers 130-170 nm wave band, corresponding luminescence peak is 364nm, emission peakCovering the wave band of 300-550 nm, the luminous peak intensity is the comparative sample BaMgAl 10 O 17 :Eu 2+ 2.925 times (BAM). The absorption spectrum of the UV-Vis band (220-800 nm) of the product is shown in FIG. 4o, (Mg) 0.9975 Sm 0.0025 ) 4 Ta 2 O 9 The absorbance near 364nm of the luminescence peak is very low, and the absorption cut-off edge is positioned at 403nm, so that the self-absorption of luminescence photons is avoided.
Example 7
MgO, ta are respectively weighed according to the stoichiometric ratio of 4.110:1.000:0.005 2 O 5 ,Eu 2 O 3 Product (Mg) 0.9975 Eu 0.0025 ) 4 Ta 2 O 9 The preparation method is the same as in example 1.
The X-ray diffraction pattern of the product is shown in FIG. 2, and all diffraction peaks correspond to standard diffraction peaks (PDF#38-1458), indicating a synthetic single phase (Mg 0.9975 Eu 0.0025 ) 4 Ta 2 O 9 Fluorescent powder. The vacuum ultraviolet excitation spectrum and the corresponding luminescence spectrum of the product are shown in figure 3d, (Mg) 0.9975 Eu 0.0025 ) 4 Ta 2 O 9 The vacuum ultraviolet excitation peak is 160nm, the excitation peak covers 130-170 nm wave band, the corresponding light-emitting peak is 364nm, the emission peak covers 300-500 nm wave band, and the light-emitting peak intensity is the comparative sample BaMgAl 10 O 17 :Eu 2+ (BAM) 2.313 times. The absorption spectrum of the UV-Vis band (220-800 nm) of the product is shown in FIG. 4p, (Mg) 0.9975 Eu 0.0025 ) 4 Ta 2 O 9 The absorbance near 364nm of the luminescence peak is very low, and the absorption cut-off edge is positioned at 332nm, so that the self-absorption of luminescence photons is avoided.
Example 8
MgO, ta are respectively weighed according to the stoichiometric ratio of 4.110:1.000:0.005 2 O 5 ,Gd 2 O 3 Product (Mg) 0.9975 Gd 0.0025 ) 4 Ta 2 O 9 The preparation method is the same as in example 1.
The X-ray diffraction pattern of the product is shown in FIG. 2, and all diffraction peaks correspond to standard diffraction peaks (PDF#38-1458), indicating coincidenceInto a single phase (Mg) 0.9975 Gd 0.0025 ) 4 Ta 2 O 9 Fluorescent powder. The vacuum ultraviolet excitation spectrum and the corresponding luminescence spectrum of the product are shown in figure 3c, (Mg) 0.9975 Gd 0.0025 ) 4 Ta 2 O 9 The vacuum ultraviolet excitation peak is 160nm, the excitation peak covers 130-170 nm wave band, the corresponding light-emitting peak is 364nm, the emission peak covers 300-500 nm wave band, and the light-emitting peak intensity is the comparative sample BaMgAl 10 O 17 :Eu 2+ 2.513 times (BAM). The absorption spectrum of the UV-Vis band (220-800 nm) of the product is shown in FIG. 4q, (Mg) 0.9975 Gd 0.0025 ) 4 Ta 2 O 9 The absorbance near 364nm of the luminescence peak is very low, and the absorption cut-off edge is positioned at 380nm, so that the self-absorption of luminescence photons is avoided.
Example 9
MgO, ta are respectively weighed according to the stoichiometric ratio of 4.110:1.000:0.005 2 O 5 ,Tb 2 O 3 Product (Mg) 0.9975 Tb 0.0025 ) 4 Ta 2 O 9 The preparation method is the same as in example 1.
The X-ray diffraction pattern of the product is shown in FIG. 2, and all diffraction peaks correspond to standard diffraction peaks (PDF#38-1458), indicating a synthetic single phase (Mg 0.9975 Tb 0.0025 ) 4 Ta 2 O 9 Fluorescent powder. The vacuum ultraviolet excitation spectrum and the corresponding luminescence spectrum of the product are shown in figure 3c, (Mg) 0.9975 Tb 0.0025 ) 4 Ta 2 O 9 The vacuum ultraviolet excitation peak is 160nm, the excitation peak covers 130-170 nm wave band, the corresponding luminescence peak is 362nm, the emission peak covers 300-500 nm wave band, and the luminescence peak intensity is the comparison sample BaMgAl 10 O 17 :Eu 2+ (BAM) 2.100 times. The absorption spectrum of the UV-Vis band (220-800 nm) of the product is shown in FIG. 4r, (Mg) 0.9975 Tb 0.0025 ) 4 Ta 2 O 9 The absorbance near 362nm of the luminescence peak is very low, and the absorption cut-off edge is positioned at 331nm, thereby being beneficial to avoiding the self absorption of luminescence photons.
Example 10
MgO, ta are respectively weighed according to the stoichiometric ratio of 4.110:1.000:0.005 2 O 5 And Dy 2 O 3 Product (Mg) 0.9975 Dy 0.0025 ) 4 Ta 2 O 9 The preparation method is the same as in example 1.
The X-ray diffraction pattern of the product is shown in FIG. 2, and all diffraction peaks correspond to standard diffraction peaks (PDF#38-1458), indicating a synthetic single phase (Mg 0.9975 Dy 0.0025 ) 4 Ta 2 O 9 Fluorescent powder. The vacuum ultraviolet excitation spectrum and the corresponding luminescence spectrum of the product are shown in figure 3e, (Mg) 0.9975 Dy 0.0025 ) 4 Ta 2 O 9 The vacuum ultraviolet excitation peak is 160nm, the excitation peak covers 130-170 nm wave band, the corresponding luminescence peak is 368nm, the emission peak covers 300-500 nm wave band, and the luminescence peak intensity is the comparison sample BaMgAl 10 O 17 :Eu 2+ (BAM) 1.975 times. The absorption spectrum of the UV-Vis band (220-800 nm) of the product is shown in FIG. 4c, (Mg) 0.9975 Dy 0.0025 ) 4 Ta 2 O 9 The absorbance near 368nm of the luminescence peak is very low, and the absorption cut-off edge is positioned at 400nm, so that the self-absorption of luminescence photons is avoided.
Example 11
MgO, ta are respectively weighed according to the stoichiometric ratio of 4.110:1.000:0.005 2 O 5 ,Ho 2 O 3 Product (Mg) 0.9975 Ho 0.0025 ) 4 Ta 2 O 9 The preparation method is the same as in example 1.
The X-ray diffraction pattern of the product is shown in FIG. 2, and all diffraction peaks correspond to standard diffraction peaks (PDF#38-1458), indicating a synthetic single phase (Mg 0.9975 Ho 0.0025 ) 4 Ta 2 O 9 Fluorescent powder. The vacuum ultraviolet excitation spectrum and the corresponding luminescence spectrum of the product are shown in figure 3f, (Mg) 0.9975 Ho 0.0025 ) 4 Ta 2 O 9 The vacuum ultraviolet excitation peak is 160nm, the excitation peak covers 130-170 nm wave band, the corresponding light-emitting peak is 392nm, the emission peak covers 300-550 nm wave band, and the light-emitting peak intensity is the comparative sample BaMgAl 10 O 17 :Eu 2+ (BAM) 4.575 times. The absorption spectrum of the UV-Vis band (220-800 nm) of the product is shown in FIG. 4d, (Mg) 0.9975 Ho 0.0025 ) 4 Ta 2 O 9 The absorbance near 392nm of the luminescence peak is very low, and the absorption cut-off edge is positioned at 324nm, thereby being beneficial to avoiding the self absorption of luminescence photons.
Example 12
MgO, ta are respectively weighed according to the stoichiometric ratio of 4.110:1.000:0.005 2 O 5 ,Er 2 O 3 Product (Mg) 0.9975 Er 0.0025 ) 4 Ta 2 O 9 The preparation method is the same as in example 1.
The X-ray diffraction pattern of the product is shown in FIG. 2, and all diffraction peaks correspond to standard diffraction peaks (PDF#38-1458), indicating a synthetic single phase (Mg 0.9975 Er 0.0025 ) 4 Ta 2 O 9 Fluorescent powder. The vacuum ultraviolet excitation spectrum and the corresponding luminescence spectrum of the product are shown in figure 3e, (Mg) 0.9975 Er 0.0025 ) 4 Ta 2 O 9 The vacuum ultraviolet excitation peak is 160nm, the excitation peak covers 130-170 nm wave band, the corresponding luminescence peak is 358nm, the emission peak covers 300-520 nm wave band, and the luminescence peak intensity is the comparison sample BaMgAl 10 O 17 :Eu 2+ 2.513 times (BAM). The absorption spectrum of the UV-Vis band (220-800 nm) of the product is shown in FIG. 4e, (Mg) 0.9975 Er 0.0025 ) 4 Ta 2 O 9 The absorbance near 358nm of the luminescence peak of (C) is very low, and the absorption cut-off edge is positioned at 363nm, thereby being beneficial to avoiding the self absorption of luminescence photons.
Example 13
MgO, ta are respectively weighed according to the stoichiometric ratio of 4.110:1.000:0.005 2 O 5 ,Tm 2 O 3 Product (Mg) 0.9975 Tm 0.0025 ) 4 Ta 2 O 9 The preparation method is the same as in example 1.
The X-ray diffraction pattern of the product is shown in FIG. 2, and all diffraction peaks correspond to standard diffraction peaks (PDF#38-1458), indicating that the synthesized single phase (Mg 0.9975 Tm 0.0025 ) 4 Ta 2 O 9 FluorescenceAnd (5) powder. The vacuum ultraviolet excitation spectrum and the corresponding luminescence spectrum of the product are shown in figure 3f, (Mg) 0.9975 Tm 0.0025 ) 4 Ta 2 O 9 The vacuum ultraviolet excitation peak is 160nm, the excitation peak covers 130-170 nm wave band, the corresponding luminescence peak is 358nm, the emission peak covers 300-550 nm wave band, and the luminescence peak intensity is the comparison sample BaMgAl 10 O 17 :Eu 2+ (BAM) 1.788 times. The absorption spectrum of the UV-Vis band (220-800 nm) of the product is shown in FIG. 4f, (Mg) 0.9975 Tm 0.0025 ) 4 Ta 2 O 9 The absorbance near 358nm of the luminescence peak is very low, and the absorption cut-off edge is positioned at 323nm, which is beneficial to avoiding the self absorption of luminescence photons.
Example 14
MgO, ta are respectively weighed according to the stoichiometric ratio of 4.110:1.000:0.005 2 O 5 ,Yb 2 O 3 Product (Mg) 0.9975 Yb 0.0025 ) 4 Ta 2 O 9 The preparation method is the same as in example 1.
The X-ray diffraction pattern of the product is shown in FIG. 2, and all diffraction peaks correspond to standard diffraction peaks (PDF#38-1458), indicating a synthetic single phase (Mg 0.9975 Yb 0.0025 ) 4 Ta 2 O 9 Fluorescent powder. The vacuum ultraviolet excitation spectrum and the corresponding luminescence spectrum of the product are shown in figure 3f, (Mg) 0.9975 Yb 0.0025 ) 4 Ta 2 O 9 The vacuum ultraviolet excitation peak is 160nm, the excitation peak covers 130-170 nm wave band, the corresponding luminescence peak is 362nm, the emission peak covers 300-500 nm wave band, and the luminescence peak intensity is the comparison sample BaMgAl 10 O 17 :Eu 2+ (BAM) 2.650 times. The absorption spectrum of the UV-Vis band (220-800 nm) of the product is shown in FIG. 4g, (Mg) 0.9975 Yb 0.0025 ) 4 Ta 2 O 9 The absorbance near 362nm of the luminescence peak is very low, and the absorption cut-off edge is positioned at 324nm, which is beneficial to avoiding the self absorption of luminescence photons.
Example 15
MgO, ta are respectively weighed according to the stoichiometric ratio of 4.110:1.000:0.005 2 O 5 ,Lu 2 O 3 Product (Mg) 0.9975 Lu 0.0025 ) 4 Ta 2 O 9 The preparation method is the same as in example 1.
The X-ray diffraction pattern of the product is shown in FIG. 2, and all diffraction peaks correspond to standard diffraction peaks (PDF#38-1458), indicating a synthetic single phase (Mg 0.9975 Lu 0.0025 ) 4 Ta 2 O 9 Fluorescent powder. The vacuum ultraviolet excitation spectrum and the corresponding luminescence spectrum of the product are shown in figure 3c, (Mg) 0.9975 Lu 0.0025 ) 4 Ta 2 O 9 The vacuum ultraviolet excitation peak is 160nm, the excitation peak covers 130-170 nm wave band, the corresponding luminescence peak is 366nm, the emission peak covers 300-550 nm wave band, and the luminescence peak intensity is the comparison sample BaMgAl 10 O 17 :Eu 2+ (BAM) 2.863 times. The absorption spectrum of the UV-Vis band (300-800 nm) of the product is shown in FIG. 4h, (Mg) 0.9975 Lu 0.0025 ) 4 Ta 2 O 9 The absorbance near 366nm of the luminescence peak is very low, and the absorption cut-off edge is positioned at 342nm, thereby being beneficial to avoiding the self absorption of luminescence photons.
Example 16
MgO, ta are respectively weighed according to the stoichiometric ratio of 4.110:1.000:0.005 2 O 5 ,Y 2 O 3 Product (Mg) 0.9975 Y 0.0025 ) 4 Ta 2 O 9 The preparation method is the same as in example 1.
The X-ray diffraction pattern of the product is shown in FIG. 2, and all diffraction peaks correspond to standard diffraction peaks (PDF#38-1458), indicating a synthetic single phase (Mg 0.9975 Y 0.0025 ) 4 Ta 2 O 9 Fluorescent powder. The vacuum ultraviolet excitation spectrum and the corresponding luminescence spectrum of the product are shown in figure 3e, (Mg) 0.9975 Y 0.0025 ) 4 Ta 2 O 9 The vacuum ultraviolet excitation peak is 160nm, the excitation peak covers 130-170 nm wave band, the corresponding light-emitting peak is 364nm, the emission peak covers 300-550 nm wave band, and the light-emitting peak intensity is the comparative sample BaMgAl 10 O 17 :Eu 2+ (BAM) 1.675 times. The absorption spectrum of the UV-Vis band (220-800 nm) of the product is shown in FIG. 4i,(Mg 0.9975 Y 0.0025 ) 4 Ta 2 O 9 the absorbance near 364nm of the luminescence peak is very low, and the absorption cut-off edge is positioned at 318nm, so that the self-absorption of luminescence photons is avoided.
Example 17
MgO, ta are respectively weighed according to the stoichiometric ratio of 4.110:1.000:0.005 2 O 5 ,Sc 2 O 3 Product (Mg) 0.9975 Sc 0.0025 ) 4 Ta 2 O 9 The preparation method is the same as in example 1.
The X-ray diffraction pattern of the product is shown in FIG. 2, and all diffraction peaks correspond to standard diffraction peaks (PDF#38-1458), indicating a synthetic single phase (Mg 0.9975 Sc 0.0025 ) 4 Ta 2 O 9 Fluorescent powder. The vacuum ultraviolet excitation spectrum and the corresponding luminescence spectrum of the product are shown in figure 3e, (Mg) 0.9975 Sc 0.0025 ) 4 Ta 2 O 9 The vacuum ultraviolet excitation peak is 160nm, the excitation peak covers 130-170 nm wave band, the corresponding light-emitting peak is 364nm, the emission peak covers 300-550 nm wave band, and the light-emitting peak intensity is the comparative sample BaMgAl 10 O 17 :Eu 2+ 2.925 times (BAM). The UV-Vis band (300-800 nm) absorption spectrum of the product is shown in FIG. 4j, (Mg) 0.9975 Sc 0.0025 ) 4 Ta 2 O 9 The absorbance near 364nm of the luminescence peak is very low, and the absorption cut-off edge is positioned at 324nm, so that the self-absorption of luminescence photons is avoided.
While the invention has been described with respect to preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (5)
1. The application of the vacuum ultraviolet excited rare earth doped magnesium tantalate compound as UVA fluorescent powder is characterized in that the chemical composition expression of the magnesium tantalate niobate compound is Mg 4 Ta 2 O 9 :0.25at% RE, wherein RE is La 3+ 、Ce 3+ 、Pr 3+ 、Nd 3+ 、Sm 3+ 、Eu 3+ 、Gd 3+ 、Tb 3+ 、Dy 3+ 、Ho 3+ 、Er 3+ 、Tm 3+ 、Yb 3+ 、Lu 3+ 、Y 3+ And Sc (Sc) 3+ At least one of them.
2. The use according to claim 1, wherein the magnesium tantalate niobate compound has an emission wavelength of 360-392 nm, is in the UVA region, and has a luminescence peak intensity of commercial blue phosphor BaMgAl 10 O 17 :Eu 2+ (BAM) 1.275-4.575 times.
3. The use of claim 1, wherein the use of the rare earth doped magnesium tantalate compound as UVA phosphor comprises: the lamp is applied to insect guiding lamps, black light lamps and flaw detection lamps.
4. The use according to claim 1, wherein the magnesium tantalate niobate compound is synthesized by a high temperature solid phase reaction method, and the specific synthesis method comprises:
weighing MgO and Ta as raw materials according to stoichiometric ratio according to chemical composition expression 2 O 5 And trivalent rare earth oxide, grinding and mixing uniformly; and then the obtained mixture is orderly presintered and calcined in air atmosphere, naturally cooled to room temperature and ground.
5. The use according to claim 4, wherein the MgO is added in an excess of 3at% with respect to the standard stoichiometric ratio;
and/or, the presintering temperature is 1250 ℃ and the presintering time is 12 hours;
and/or the calcination temperature is 1350 ℃ for 24 hours.
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