CN116925762A - 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 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 20
- 235000015895 biscuits Nutrition 0.000 claims abstract description 16
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims abstract description 11
- 229910010413 TiO 2 Inorganic materials 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
- 238000000034 method Methods 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 3
- 239000007790 solid phase Substances 0.000 claims abstract 3
- 238000002156 mixing Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- 238000001228 spectrum Methods 0.000 abstract description 8
- 230000005284 excitation Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 description 28
- 239000010431 corundum Substances 0.000 description 28
- 239000013078 crystal Substances 0.000 description 14
- 238000010438 heat treatment Methods 0.000 description 12
- 239000000203 mixture Substances 0.000 description 12
- 239000000843 powder Substances 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 4
- 238000002189 fluorescence spectrum Methods 0.000 description 3
- 230000003595 spectral effect Effects 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
- 238000006243 chemical reaction 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
- 229910020068 MgAl Inorganic materials 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
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
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- 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
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- 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
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Abstract
The invention discloses a novel Mn 4+ Doped tunable wide rectangular red fluorescent material and preparation method thereof, and chemical formula of doped tunable wide rectangular red fluorescent material is xMn 4+ :Li 3 LaMgTi (1‑x) O 6 (0.2at%≤x<1 at%) of the fluorescent material is MnO 2 、Li 2 CO 3 、La 2 O 3 MgO and TiO 2 The method comprises the steps of taking the 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 the excitation of 358nm LEDs, can be regulated 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 with a wide rectangle and a tunable fluorescence spectrum 4+ :Li 3 LaMgTi (1-x) O 6 （0.2at%≤x<1 at%) 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 (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, mn is doped 4+ Is attracting a great deal of attention, such as SrKYTEO 6 :Mn 4+ Phosphor, ba 2 SrWO 6 :Mn 4+ 、CaMgAl 10 O 17 :Mn 4+ 、CaMg 2 La 2 W 2 O 12 :Mn 4+ These fluorescent materials 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. To improve the color gamut and linewidth of fluorescence spectra, methods of doping different ions into the matrix, such as MgAl, are generally used 2 Si 2 O 8 :Mn 4+ 、Pr 3+、4+ 、Nd 3+ 、Cr 3+ 、Mn 4+ ：La 2 ZnTiO 6 . Although this approach can broaden the spectral range, the spectral line uniformity is stillPoor, and a fluorescence spectrum similar to a rectangular pulse waveform has not been obtained yet.
Disclosure of Invention
The invention aims to provide a novel Mn 4+ The doped tunable wide rectangular red fluorescent 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:
mn (Mn) 4+ Doped tunable broad rectangular red fluorescent material with chemical formula of xMn 4+ :Li 3 LaMgTi (1-x) O 6 (wherein 0.2at% is less than or equal to x)<1at%）。
The Mn of 4+ The synthesis reaction formula of the doped tunable broad rectangular red fluorescent material is as follows:
the method comprises the steps of carrying out a first treatment on the surface of the The preparation method specifically comprises the following steps:
1) Mixing MnO according to a proportion 2 、Li 2 CO 3 、La 2 O 3 MgO and TiO 2 Dry grinding in agate mortar for 2 hr and mixing to obtain xMn 4+ :Li 3 LaMgTi (1-x) O 6 A biscuit;
2) Putting 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 ℃ and sintering the corundum crucible at the constant temperature for 3-5 hours, and cooling a sample to room temperature to obtain the Mn 4+ Doped tunable broad rectangular red fluorescent material.
Further, mnO used in step 1) 2 、Li 2 CO 3 、La 2 O 3 、MgO、TiO 2 The mol ratio of (2) is x, 1.5:0.5:1 (1-x), wherein 0.2at% is less than or equal to x<1at%。
Further, mnO used in step 1) 2 The purity of (2) is 99.995%, and the fineness is 0.5-1 mu m; li used 2 CO 3 The purity of (2) is 99.995%, and the fineness is 0.1-0.3 μm; by a means ofBy La 2 O 3 The purity of (2) is 99.99%, and the fineness is 0.2 μm; the purity of MgO is 99.99%, and the fineness is 0.1-0.2 μm; tiO used 2 The purity of (2) was 99.99% and the fineness was 0.1. Mu.m.
Compared with the Mn disclosed at present 4+ Fluorescent material, mn provided by the invention 4+ The doped tunable wide rectangular red fluorescent material adopts a gradient temperature zone preparation technology to prepare Li 3 LaMgTiO 6 The material is layered, namely the bottom layer temperature is higher, the crystal structure of the material is changed from tetragonal phase to cubic phase, and the lattice parameter of the cubic phase is increased, 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 spectral line of blue shift of fluorescence peak of the material from 711nm to 680nm, and the material is suitable for plant cultivation.
The invention has the advantages that:
（1）Li 3 LaMgTiO 6 low price and low sintering temperature<1300 ℃) and can also provide a number of octahedral sites favoring Mn 4+ Substitution of ions.
(2) In the pair Mn 4+ ：Li 3 LaMgTiO 6 In the research of fluorescent materials, it is found that 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 a 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) Mn obtained by the invention 4+ The uniformity and wide color gamut of the doped red fluorescent material make it very advantageous for large-scale application in plant factories.
(4) Matrix material Li used in the present invention 3 LaMgTiO 6 Has not been reported before, and relates to the material xMn 4+ : Li 3 LaMgTiO 6 The research work and the preparation technology of the fluorescent powder have not been reported, and the phenomenon of a broad rectangular red fluorescent spectrum with tunable characteristics has not been reported. 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
Mn (Mn) 4+ The preparation of the doped tunable wide rectangular red fluorescent material comprises the following steps:
1) MnO is added according to the mol ratio of x to 1.5:0.5:1 (1-x) 2 、Li 2 CO 3 、La 2 O 3 MgO and TiO 2 Dry grinding in agate mortar for 2 hr and mixing to obtain xMn 4+ :Li 3 LaMgTi (1-x) O 6 A biscuit; wherein x is 0.2at% or less<1at%；
2) Putting 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 ℃ and sintering the corundum crucible at the constant temperature for 3-5 hours, and cooling a sample to room temperature to obtain Mn 4+ Doped tunable broad 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.
MnO used 2 The purity of (2) is 99.995%, and the fineness is 0.5-1 mu m; li used 2 CO 3 The purity of (2) is 99.995%, and the fineness is 0.1-0.3 μm; la used 2 O 3 The purity of (2) is 99.99%, and the fineness is 0.2 μm; the purity of MgO is 99.99%, and the fineness is 0.1-0.2 μm; tiO used 2 The purity of (2) was 99.99% and the fineness was 0.1. Mu.m.
Example 1
0.2Mn 4+ :Li 3 LaMgTi 0.8 O 6 The preparation method of the fluorescent luminescent material comprises the following steps:
1) MnO with high purity and close size uniformity is selected 2 ，Li 2 CO 3 ，La 2 O 3 MgO and TiO 2 Putting the mixture into an agate mortar according to the molar ratio of 0.2:1.5:0.5:1:0.8, dry-grinding the mixture for 2 hours, and uniformly mixing the mixture to obtain 0.2Mn 4+ :Li 3 LaMgTi 0.8 O 6 Biscuit
2) Putting 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 the corundum crucible to 900 ℃, sintering the corundum crucible at the constant temperature for 3 hours, and cooling a sample to the room temperature to obtain powdery 0.2Mn 4+ :Li 3 LaMgTi 0.8 O 6 Fluorescent powder.
Example 2
0.2Mn 4+ :Li 3 LaMgTi 0.8 O 6 Fluorescent luminescent material, its preparation method comprises the following stepsThe steps are as follows:
1) MnO with high purity and close size uniformity is selected 2 ，Li 2 CO 3 ，La 2 O 3 MgO and TiO 2 Putting the mixture into an agate mortar according to the molar ratio of 0.2:1.5:0.5:1:0.8, dry-grinding the mixture for 2 hours, and uniformly mixing the mixture to obtain 0.2Mn 4+ :Li 3 LaMgTi 0.8 O 6 A biscuit;
2) Putting the obtained biscuit into a corundum crucible, placing the corundum crucible into a tube furnace, heating the corundum crucible from normal temperature to 900 ℃, keeping the temperature constant for h, continuously heating the corundum crucible to 1000 ℃, sintering the corundum crucible at the constant temperature for 3h, and cooling a sample to the room temperature to obtain powdery 0.2Mn 4+ :Li 3 LaMgTi 0.8 O 6 Fluorescent powder.
Example 3
0.2Mn 4+ :Li 3 LaMgTi 0.8 O 6 The preparation method of the fluorescent luminescent material comprises the following steps:
1) MnO with high purity and close size uniformity is selected 2 ，Li 2 CO 3 ，La 2 O 3 MgO and TiO 2 Putting the mixture into an agate mortar according to the molar ratio of 0.2:1.5:0.5:1:0.8, dry-grinding the mixture for 2 hours, and uniformly mixing the mixture to obtain 0.2Mn 4+ :Li 3 LaMgTi 0.8 O 6 A biscuit;
2) Putting 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 the corundum crucible to 1100 ℃, sintering the corundum crucible at the constant temperature for 3 hours, and cooling a sample to the room temperature to obtain powdery 0.2Mn 4+ :Li 3 LaMgTi 0.8 O 6 Fluorescent powder.
Example 4
0.2Mn 4+ :Li 3 LaMgTi 0.8 O 6 The preparation method of the fluorescent luminescent material comprises the following steps:
1) MnO with high purity and close size uniformity is selected 2 ，Li 2 CO 3 ，La 2 O 3 MgO and TiO 2 Putting the mixture into an agate mortar according to the molar ratio of 0.2:1.5:0.5:1:0.8, dry-grinding the mixture for 2 hours, and uniformly mixing the mixture to obtain 0.2Mn 4+ :Li 3 LaMgTi 0.8 O 6 A biscuit;
2) Putting 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 the corundum crucible to 1150 ℃ and sintering the corundum crucible at the constant temperature for 3 hours, and cooling a sample to the room temperature to obtain powdery 0.2Mn 4+ :Li 3 LaMgTi 0.8 O 6 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. Mn (Mn) 4+ A doped tunable broad rectangular red phosphor characterized by: the chemical formula is xMn 4+ :Li 3 LaMgTi (1-x) O 6 Wherein x is 0.2at% or less<1at%。
2. Mn as claimed in claim 1 4+ The preparation method of the doped tunable wide rectangular red fluorescent material is characterized by comprising the following steps of: the method comprises the following steps:
1) Mixing MnO according to a proportion 2 、Li 2 CO 3 、La 2 O 3 MgO and TiO 2 Dry grinding in agate mortar and mixing to obtain xMn 4+ :Li 3 LaMgTi (1-x) O 6 A 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. Mn according to claim 2 4+ The preparation method of the doped tunable wide rectangular red fluorescent material is characterized by comprising the following steps of: mnO used in step 1) 2 、Li 2 CO 3 、La 2 O 3 、MgO、TiO 2 The mol ratio of (2) is x, 1.5:0.5:1 (1-x), wherein 0.2at% is less than or equal to x<1at%。
4. A Mn according to claim 2 or 3 4+ The preparation method of the doped tunable wide rectangular red fluorescent material is characterized by comprising the following steps of: mnO used in step 1) 2 The purity of (2) is 99.995%, and the fineness is 0.5-1 mu m; li used 2 CO 3 The purity of (2) is 99.995%, and the fineness is 0.1-0.3 μm; la used 2 O 3 The purity of (2) is 99.99%, and the fineness is 0.2 μm; the purity of MgO is 99.99%, and the fineness is 0.1-0.2 μm; tiO used 2 The purity of (2) was 99.99% and the fineness was 0.1. Mu.m.
5. Mn according to claim 2 4+ The preparation method of the doped tunable wide rectangular red fluorescent material is characterized by comprising the following steps of: 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. Mn as claimed in claim 1 4+ The application of the doped tunable wide rectangular red fluorescent material in plant cultivation.
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