CN116925762B - Mn-doped tunable wide rectangular red fluorescent material and preparation method thereof - Google Patents
Mn-doped tunable wide rectangular red fluorescent material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 20
- 235000015895 biscuits Nutrition 0.000 claims abstract description 16
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 11
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 10
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 10
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000009837 dry grinding Methods 0.000 claims abstract description 8
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 3
- 239000007790 solid phase Substances 0.000 claims abstract 3
- 238000001816 cooling Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims 1
- 238000001228 spectrum Methods 0.000 abstract description 10
- 230000005284 excitation Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 description 22
- 239000010431 corundum Substances 0.000 description 22
- 239000013078 crystal Substances 0.000 description 14
- 238000010438 heat treatment Methods 0.000 description 12
- 238000011049 filling Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000002189 fluorescence spectrum Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 238000000695 excitation spectrum Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229930002875 chlorophyll Natural products 0.000 description 1
- 235000019804 chlorophyll Nutrition 0.000 description 1
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000005274 electronic transitions Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008636 plant growth process Effects 0.000 description 1
- 238000005381 potential energy Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7701—Chalogenides
- C09K11/7703—Chalogenides with alkaline earth metals
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
- A01G7/00—Botany in general
- A01G7/04—Electric or magnetic or acoustic treatment of plants for promoting growth
- A01G7/045—Electric or magnetic or acoustic treatment of plants for promoting growth with electric lighting
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/14—Measures for saving energy, e.g. in green houses
Abstract
The invention discloses a novel Mn 4+ doped tunable wide rectangular red fluorescent material and a preparation method thereof, wherein the chemical formula of the novel Mn 4+ doped tunable wide rectangular red fluorescent material is xMn 4+:Li3LaMgTi(1‑x)O6 (0.2at% -x < 1at%), the fluorescent material is prepared by taking MnO 2、Li2CO3、La2O3, mgO and TiO 2 as raw materials, carrying out dry grinding in an agate mortar to obtain a biscuit, and carrying out high-temperature solid-phase sintering on the obtained biscuit. The red fluorescent material has the characteristics of wide rectangle and tunable fluorescence, can obtain a rectangle fluorescent spectrum with the FWHM width reaching 100nm under 358 nm LED excitation, can adjust the spectrum intensity according to actual needs, and has good application prospect in the field of plant cultivation.
Description
Technical Field
The invention belongs to the technical field of fluorescent material preparation, and particularly relates to a red fluorescent material xMn 4+:Li3LaMgTi(1-x)O6 (0.2at% -x < 1at%) with a wide rectangle and a tunable fluorescent spectrum and a preparation method thereof.
Background
In the plant growth process, chlorophyll ab has stronger absorption intensity in near infrared wave bands of 660nm, 680nm, 700-710nm, 730-750nm and the like. Therefore, research on fluorescent materials suitable for these bands is of great significance for large-scale popularization of plant factories. Mn 4+ has excellent luminescence properties in these bands and is considered as an active ion having good application in plant cultivation. In particular, in recent years, oxide-based fluorescent materials doped with Mn 4+ have attracted a lot of attention, such as SrKYTeO 6:Mn4+ phosphor 、Ba2SrWO6:Mn4+、CaMgAl10O17:Mn4+、CaMg2La2W2O12:Mn4+,, which have high quantum efficiency and thermal stability. However, the conventional spectrum width is usually 10-15nm, and the fluctuation is large, so that the spectrum range is narrow, the uniformity is poor, and the key link for restricting the application of the spectrum is provided. In order to improve the color gamut and line width of the fluorescence spectrum, a method of doping different ions in a matrix is generally used, such as MgAl2Si2O8:Mn4+、Pr3+、4+、Nd3+、Cr3+、Mn4+：La2ZnTiO6., although this method can widen the spectrum range, the uniformity of the line is still poor, and a fluorescence spectrum similar to a rectangular pulse waveform cannot be obtained yet.
Disclosure of Invention
The invention aims to provide a novel Mn 4+ doped tunable wide rectangular red fluorescent material and a preparation method thereof, and the material has the properties of wide rectangular and tunable fluorescent spectrum and is suitable for being applied to the field of plant cultivation.
In order to achieve the above purpose, the invention adopts the following technical scheme:
A Mn 4+ doped tunable broad rectangular red fluorescent material has a chemical formula of xMn 4+:Li3LaMgTi(1-x)O6 (wherein 0.2at% is less than or equal to x <1 at%).
The Mn 4+ doped tunable wide rectangular red fluorescent material has the following synthetic reaction formula:
; the preparation method specifically comprises the following steps:
1) Putting MnO 2、Li2CO3、La2O3, mgO and TiO 2 into an agate mortar according to a proportion, dry-grinding for 2 hours, and uniformly mixing to obtain an xMn 4+:Li3LaMgTi(1-x)O6 biscuit;
2) And filling the obtained biscuit into a corundum crucible, placing the corundum crucible into a tube furnace, heating the corundum crucible to 900 ℃ from normal temperature, keeping the temperature for 3-5 hours, continuously heating to 1150 ℃, sintering at the constant temperature for 3-5 hours, and cooling the sample to room temperature to obtain the Mn 4+ -doped tunable wide rectangular red fluorescent material.
Further, the molar ratio of MnO 2、Li2CO3、La2O3、MgO、TiO2 used in step 1) is x:1.5:0.5:1 (1-x), wherein 0.2at% is less than or equal to x <1at%.
Further, the purity of MnO 2 used in step 1) is 99.995% and the fineness is 0.5-1. Mu.m; the purity of Li 2CO3 is 99.995% and the fineness is 0.1-0.3 μm; the purity of La 2O3 used is 99.99 percent and the fineness is 0.2 mu m; the purity of MgO is 99.99%, and the fineness is 0.1-0.2 μm; the purity of the TiO 2 used was 99.99% and the fineness was 0.1. Mu.m.
Compared with the Mn 4+ fluorescent material disclosed at present, the Mn 4+ doped tunable wide rectangular red fluorescent material provided by the invention adopts a gradient temperature region preparation technology, so that the prepared Li 3LaMgTiO6 material is layered, namely the bottom layer temperature is higher, the crystal structure of the Li 3LaMgTiO6 material is changed from a tetragonal phase to a cubic phase, and the lattice parameter of the cubic phase is enlarged, so that the potential energy field of the crystal where Mn is located is stronger, and more energy is required for electronic transition, thereby causing the blue shift phenomenon of the spectral line of the fluorescent peak of the material from 711nm to 680nm, and being suitable for plant cultivation.
The invention has the advantages that:
(1) Li 3LaMgTiO6 is inexpensive and has a low sintering temperature (< 1300 ℃) and can also provide many octahedral sites, facilitating substitution of Mn 4+ ions.
(2) In the research of Mn 4+：Li3LaMgTiO6 fluorescent materials, the crystal phase structure of the surface layer of the material can be changed by designing a proper sintering temperature, so that the blue shift phenomenon of the fluorescent spectrum is caused, and the tunable wide rectangular fluorescent spectrum is realized. Experimental results show that when the sintering temperature is 1150 ℃, rectangular emission spectra with full width at half maximum (FWHM) of up to 100nm and top width of up to 31nm can be obtained. In the existing rare earth or transition metal ion luminescent materials, a wide rectangular emission spectrum is difficult to obtain, and no wide rectangular red light emission peak with a peak width of up to 31nm is found.
(3) The Mn 4+ doped red fluorescent material has uniformity and wide color gamut, so that the Mn 4+ doped red fluorescent material is very beneficial to large-scale application in plant factories.
(4) The matrix material Li 3LaMgTiO6 used in the invention has not been reported before, the research work and the preparation technology related to the material xMn 4+: Li3LaMgTiO6 have not been reported, and the wide rectangular red fluorescence spectrum phenomenon with tunable characteristics has not been reported yet. Meanwhile, the obtained red fluorescent material is very suitable for plant cultivation because the obtained rectangular wide red light is 680-711nm, and has the advantages of more uniform color, wider application range and the like compared with the red fluorescent material prepared by doping the existing Mn ions.
Drawings
FIG. 1 shows a schematic crystal structure (a) and a schematic crystal lattice (b) abstracted from the schematic crystal structure (a) of the fluorescent material of the present invention.
FIG. 2 is a graph showing the conversion of the crystal structure of the fluorescent material of the present invention from tetrahedron to cube.
FIG. 3 is an XRD pattern of the fluorescent luminescent materials prepared at different sintering temperatures in examples 1 to 4.
FIG. 4 is a graph showing the absorption spectra of fluorescent materials prepared by exciting different sintering temperatures in examples 1-3 using 358nm LED light sources.
FIG. 5 is a graph of excitation spectra of fluorescent luminescent materials prepared by excitation of different sintering temperatures in examples 1-4 using 358nm LED light source.
Detailed Description
The preparation method of the Mn 4+ doped tunable wide rectangular red fluorescent material comprises the following steps:
1) Putting MnO 2、Li2CO3、La2O3, mgO and TiO 2 into an agate mortar according to the molar ratio of x to 1.5 to 0.5 to 1 (1-x), dry-grinding for 2 hours, and uniformly mixing to obtain an xMn 4+:Li3LaMgTi(1-x)O6 biscuit; wherein x is more than or equal to 0.2at% and less than 1at%;
2) And filling the obtained biscuit into a corundum crucible, placing the corundum crucible into a tube furnace, heating the corundum crucible to 900 ℃ from normal temperature, keeping the temperature for 3-5 hours, continuously heating to 1150 ℃, sintering at the constant temperature for 3-5 hours, and cooling the sample to room temperature to obtain the Mn 4+ -doped tunable wide rectangular red fluorescent material.
FIG. 1 shows a schematic crystal structure (a) and a schematic crystal lattice (b) abstracted from the schematic crystal structure (a) of the fluorescent material of the present invention.
FIG. 2 is a graph showing the conversion of the crystal structure of the fluorescent material of the present invention from tetrahedron to cube. As can be seen from the figure, the lattice constant expands with increasing temperature due to the different temperatures of the different regions of the crystal, and is limited by the layered structure, so that the expansion rate in the horizontal direction is faster than in the vertical direction (a); the position of the regular octahedron changes after expansion of the crystal structure (b).
In order to make the contents of the present invention more easily understood, the technical scheme of the present invention will be further described with reference to the specific embodiments, but the present invention is not limited thereto.
The purity of MnO 2 is 99.995% and the fineness is 0.5-1 μm; the purity of Li 2CO3 is 99.995% and the fineness is 0.1-0.3 μm; the purity of La 2O3 used is 99.99 percent and the fineness is 0.2 mu m; the purity of MgO is 99.99%, and the fineness is 0.1-0.2 μm; the purity of the TiO 2 used was 99.99% and the fineness was 0.1. Mu.m.
Example 1
A0.2 Mn 4+:Li3LaMgTi0.8O6 fluorescent luminescent material, the preparation method comprises the following steps:
1) Selecting MnO 2,Li2CO3,La2O3, mgO and TiO 2 with high purity and close size uniformity, putting the mixture into an agate mortar according to the mol ratio of 0.2:1.5:0.5:1:0.8, dry-grinding for 2 hours, and uniformly mixing to obtain a 0.2Mn 4+:Li3LaMgTi0.8O6 biscuit
2) And filling the obtained biscuit into a corundum crucible, placing the corundum crucible into a tube furnace, heating the corundum crucible to 900 ℃ from normal temperature, keeping the temperature for 3 hours, continuously heating to 900 ℃, sintering the corundum crucible at the constant temperature for 3 hours, and cooling the sample to the room temperature to obtain the powdery 0.2Mn 4+:Li3LaMgTi0.8O6 fluorescent powder.
Example 2
A0.2 Mn 4+:Li3LaMgTi0.8O6 fluorescent luminescent material, the preparation method comprises the following steps:
1) Selecting MnO 2,Li2CO3,La2O3, mgO and TiO 2 with high purity and close size uniformity, putting the mixture into an agate mortar according to the molar ratio of 0.2:1.5:0.5:1:0.8, dry-grinding for 2 hours, and uniformly mixing to obtain a 0.2Mn 4+:Li3LaMgTi0.8O6 biscuit;
2) And filling the obtained biscuit into a corundum crucible, placing the corundum crucible into a tube furnace, heating the corundum crucible to 900 ℃ from normal temperature, keeping the constant temperature for h, continuously heating to 1000 ℃, sintering the corundum crucible at the constant temperature for 3h, and cooling the sample to the room temperature to obtain the powdery 0.2Mn 4+:Li3LaMgTi0.8O6 fluorescent powder.
Example 3
A0.2 Mn 4+:Li3LaMgTi0.8O6 fluorescent luminescent material, the preparation method comprises the following steps:
1) Selecting MnO 2,Li2CO3,La2O3, mgO and TiO 2 with high purity and close size uniformity, putting the mixture into an agate mortar according to the molar ratio of 0.2:1.5:0.5:1:0.8, dry-grinding for 2 hours, and uniformly mixing to obtain a 0.2Mn 4+:Li3LaMgTi0.8O6 biscuit;
2) And filling the obtained biscuit into a corundum crucible, placing the corundum crucible into a tube furnace, heating the corundum crucible to 900 ℃ from normal temperature, keeping the temperature for 3 hours, continuously heating to 1100 ℃, sintering the corundum crucible at the constant temperature for 3 hours, and cooling the sample to the room temperature to obtain the powdery 0.2Mn 4+:Li3LaMgTi0.8O6 fluorescent powder.
Example 4
A0.2 Mn 4+:Li3LaMgTi0.8O6 fluorescent luminescent material, the preparation method comprises the following steps:
1) Selecting MnO 2,Li2CO3,La2O3, mgO and TiO 2 with high purity and close size uniformity, putting the mixture into an agate mortar according to the molar ratio of 0.2:1.5:0.5:1:0.8, dry-grinding for 2 hours, and uniformly mixing to obtain a 0.2Mn 4+:Li3LaMgTi0.8O6 biscuit;
2) And filling the obtained biscuit into a corundum crucible, placing the corundum crucible into a tube furnace, heating the corundum crucible to 900 ℃ from normal temperature, keeping the temperature for 3 hours, continuously heating to 1150 ℃, sintering the corundum crucible at the constant temperature for 3 hours, and cooling the sample to the room temperature to obtain the powdery 0.2Mn 4+:Li3LaMgTi0.8O6 fluorescent powder.
FIG. 3 is an XRD pattern of the fluorescent luminescent materials prepared at different sintering temperatures in examples 1 to 4. From the figure, it can be seen that, starting from 1000 °, the diffraction peaks of the cubic phase are increased in the powder diffraction pattern, which proves that the crystal structure is transformed.
FIG. 4 is a graph showing the absorption spectra of fluorescent materials prepared by exciting different sintering temperatures in examples 1-3 using 358nm LED light sources. As can be seen from the figure, the fluorescent luminescent materials prepared at different sintering temperatures mainly comprise three absorption bands, namely 264-280nm,331-375nm and 490nm.
FIG. 5 is a graph of excitation spectra of fluorescent luminescent materials prepared by excitation of different sintering temperatures in examples 1-4 using 358nm LED light source. As can be seen from the graph, the blue shift phenomenon occurs at the fluorescence peak position along with the different preparation temperatures, and when the temperature is 1150 ℃, a rectangular red light emission peak with the peak width of 31nm can be obtained.
The foregoing description is only of the preferred embodiments of the invention, and all changes and modifications that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (6)
1. An Mn 4+ doped tunable broad rectangular red fluorescent material, which is characterized in that: the chemical formula of the catalyst is xMn 4+:Li3LaMgTi(1-x)O6, wherein x is more than or equal to 0.2at% and less than or equal to 1at%.
2. A method for preparing the Mn 4+ doped tunable broad rectangular red fluorescent material of claim 1, wherein: the method comprises the following steps:
1) Putting MnO 2、Li2CO3、La2O3, mgO and TiO 2 into an agate mortar according to a proportion, dry-grinding and uniformly mixing to obtain an xMn 4+:Li3LaMgTi(1-x)O6 biscuit;
2) And (3) carrying out high-temperature solid-phase sintering on the obtained biscuit, and then cooling the sample to room temperature to obtain the finished product.
3. The method for preparing the Mn 4+ doped tunable broad rectangular red fluorescent material according to claim 2, characterized in that: the molar ratio of MnO 2、Li2CO3、La2O3、MgO、TiO2 used in step 1) is x:1.5:0.5:1 (1-x), wherein 0.2at% is less than or equal to x <1at%.
4. A method for preparing a tunable broad rectangular red fluorescent material doped with Mn 4+ according to claim 2 or 3, wherein: the purity of MnO 2 used in step 1) is 99.995% and the fineness is 0.5-1 μm; the purity of Li 2CO3 is 99.995% and the fineness is 0.1-0.3 μm; the purity of La 2O3 used is 99.99 percent and the fineness is 0.2 mu m; the purity of MgO is 99.99%, and the fineness is 0.1-0.2 μm; the purity of the TiO 2 used was 99.99% and the fineness was 0.1. Mu.m.
5. The method for preparing the Mn 4+ doped tunable broad rectangular red fluorescent material according to claim 2, characterized in that: and 2) the high-temperature solid-phase sintering is carried out by raising the temperature from normal temperature to 900 ℃, keeping the temperature for 3-5 hours, and then continuously raising the temperature to 1150 ℃ and carrying out constant-temperature sintering for 3-5 hours.
6. Use of a tunable broad rectangular red fluorescent material doped with Mn 4+ according to claim 1 in plant cultivation.
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