CN112480918A - Manganese-doped deep red light fluorescent powder material and preparation method thereof - Google Patents

Manganese-doped deep red light fluorescent powder material and preparation method thereof Download PDF

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CN112480918A
CN112480918A CN202011409127.0A CN202011409127A CN112480918A CN 112480918 A CN112480918 A CN 112480918A CN 202011409127 A CN202011409127 A CN 202011409127A CN 112480918 A CN112480918 A CN 112480918A
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manganese
powder
deep red
double perovskite
doped double
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CN112480918B (en
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李涓
李冠威
车声雷
郑精武
乔梁
应耀
李旺昌
余靓
蔡伟
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Zhejiang University of Technology ZJUT
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    • 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
    • C09K11/7708—Vanadates; Chromates; Molybdates; Tungstates
    • H—ELECTRICITY
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    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/50—Wavelength conversion elements
    • H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
    • H01L33/502—Wavelength conversion materials
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Abstract

The invention discloses a manganese-doped deep red light fluorescent powder material and a preparation method thereof, wherein the chemical general formula of the manganese-doped deep red light fluorescent powder material is as follows: a. the2‑2xCaB’1‑xO6:2xR3+,xMn4+Wherein: a is one of Sr and Ba; b' is one of Mo and W; r is one of La, Gd, Eu, Y, Sm, Nd and Dy; the value range of x is more than or equal to 0.001 and less than or equal to 0.130. The method adopts a solid-phase reaction method, takes carbonate and oxide corresponding to related elements as raw materials, utilizes trivalent rare earth ions to balance charges, effectively improves the fluorescence intensity of the material, prepares the deep red fluorescent powder which can be excited by a commercial LED chip, and can be used in the field of LED illumination and artificial light sources for assisting plant growth as the fluorescent powder for lamps. The trivalent rare earth ions are used for balancing the charges, so that the fluorescence intensity of the material can be effectively improved.

Description

Manganese-doped deep red light fluorescent powder material and preparation method thereof
Technical Field
The invention relates to the technical field of fluorescent powder preparation, in particular to a preparation method of manganese-doped double perovskite deep red fluorescent powder.
Background
In recent decades, White Light Emitting Diodes (WLEDs) have attracted the interest of researchers and have been developed in large quantities due to their advantages of low power consumption, reliable performance, environmental protection, etc. At present, the commercial white light LED mainly uses Y3Al5O12:Ce3+The white fluorescent powder with low cost and simple process is produced by the method of combining (YAG: Ce) yellow fluorescent powder and blue light emitting diode (GaN). However, the white LED lamp lacking the red phosphor may cause a change in color temperature and a deviation in color rendering index, and thus the white LED phosphor composed of three-color phosphors becomes one of hot spots for research and development. The method can solve the problems of poor color rendering property and the like of a blue light excitation type and has the advantages of high color rendering property, no change of light color along with current and adjustable light temperature. Meanwhile, the near ultraviolet LED chip shows less current attenuation and higher external quantum yield than the blue chip, thereby achieving better luminous efficiency.
Mn4+As a non-rare earth ion activator, belongs to 3d3Transition metal ions in electronic configuration. Mn4+By substitution of octahedral central ions in the matrix lattice, e.g. Al3+、Ti4+、Ge4+、Mo6+、W6+And (5) carrying out plasma to form a stable octahedral structure. In octahedron, Mn4+Is a ground state of4A2The lowest activation state is2E。Mn4+The doped fluorescent powder has low cost and excitation bandwidth, and gradually becomes a material for WLEDNovel red fluorescent powder. The excitation broadband mainly belongs to Mn4+Is/are as follows4A2→2T2,4A2→4T1And4A2→4T2the simultaneous emission spectra are usually narrow-band emissions, and belong to spin-forbidden2E→4A2And (4) transition.
Having a2BB’O6The double perovskite has stronger physical and chemical stability and becomes a good substrate material of the red fluorescent powder for WLED. In double perovskite A2CaB’O6(A＝Sr2+,Ba2+；B’＝W6+,Mo6+) In the molybdate structure, [ B' O ]6]Octahedron being Mn4+Providing an occupiable lattice site. However, due to Mn4+Occupies B'6+Causes charge imbalance and the appearance of oxygen vacancies, which are responsible for Mn4+The luminous intensity of (a) is harmful. In order to prevent the occurrence of oxygen vacancy, the invention creatively selects trivalent rare earth ion Re3+As charge compensators substituted for A2+To balance the charge and eliminate the influence of oxygen vacancies.
Disclosure of Invention
The invention aims to provide manganese-doped double perovskite deep red fluorescent powder aiming at the defects of the prior art. The chemical general formula is as follows: a. the2-2xCaB’1-xO6:2xR3+,xMn4+Wherein: a is one of Sr and Ba; b' is one of Mo and W; r is one of La, Gd, Eu, Y, Sm, Nd and Dy; the value range of x is more than or equal to 0.001 and less than or equal to 0.130.
The invention also aims to provide a preparation method of the manganese-doped double perovskite crimson fluorescent powder, which adopts a solid phase reaction method, takes carbonate and oxide corresponding to related elements as raw materials, utilizes trivalent rare earth ions to balance charges, effectively improves the fluorescent intensity of the materials, prepares the crimson fluorescent powder which can be excited by commercial LED chips, and can be used in the field of LED illumination and artificial light sources for assisting plant growth as the fluorescent powder for lamps. The trivalent rare earth ions are used for balancing the charges, so that the fluorescence intensity of the material can be effectively improved.
The invention adopts the following basic steps:
step (1) according to A2-2xCaB’1-xO6:2xR3+,xMn4+Preparing compounds containing relevant elements according to a stoichiometric ratio, mixing and grinding for 1.5-2h, fully vibrating the mixed powder, putting the powder into a high-temperature muffle furnace, heating the powder from room temperature to 800 ℃, preserving the heat for 1-2 h, continuing heating the powder to 1050-1150 ℃, preserving the heat for 2-3 h, and naturally cooling the powder to room temperature;
step (2), grinding the sample cooled to room temperature in the step (1) into powder again, and mixing uniformly;
and (3) putting the powder in the step (2) into a high-temperature muffle furnace, heating the muffle furnace from room temperature to 1200-1400 ℃, preserving the heat for 4-12 hours, then cooling the muffle furnace to 900 ℃ from the room temperature, naturally cooling the muffle furnace to the room temperature, and grinding the muffle furnace to obtain the manganese-doped double perovskite red fluorescent powder.
Further, the compound containing the relevant element is carbonate or oxide containing the relevant element;
further, manganese ion Mn is contained4+The compound of (A) is MnO2、MnCO3One or more of; containing strontium ions Sr2+The compound of (A) is SrCO3(ii) a Barium ion Ba2+The compound of (A) is BaCO3(ii) a Ca ion containing calcium2+The compound of (A) is CaCO3(ii) a Containing tungsten ions W6 +The compound of (A) is WO3(ii) a Molybdenum ion Mo6+The compound of (A) is MoO3(ii) a Containing rare earth ions R3+The compounds of (b) are the respective corresponding trivalent oxides.
Further, the heating rate and the cooling rate in the step (1) and the step (3) are 5-10 ℃/min.
Further, the calcination temperature in the step (3) is 1300 ℃, and the heat preservation time is 4 hours.
The invention has the following beneficial effects:
(1) the preparation method of the manganese-doped double perovskite deep red fluorescent powder has the advantages of simple process, convenient operation, low cost and high production efficiency, and is suitable for industrial large-scale production.
(2) A of the invention2-2xCaB’1-xO6:2xR3+,xMn4+The deep red fluorescent powder has a wide excitation band, and can be excited by a commercial LED blue light chip (460nm) and an ultraviolet chip (380nm) at the same time.
(3) According to the invention, rare earth ions are used as charge compensation agents, so that charges are balanced, and the fluorescence property of a sample is improved.
(4) The manganese-doped double perovskite deep red fluorescent powder prepared by the invention has good stability and long fluorescent life.
Drawings
FIG. 1 is an X-ray diffraction pattern of phosphor samples prepared according to example 1, example 2, example 3 (a is example 1, b is example 2, c is example 3);
FIG. 2 is a graph of the emission spectrum of a phosphor sample prepared in example 1 at 493nm excitation and the excitation spectrum monitored at 683 nm.
FIG. 3 is a graph of the emission spectrum at 493nm and the excitation spectrum at 683nm for the phosphor samples prepared in example 2 and the phosphor samples without the addition of a charge compensation agent.
FIG. 4 is a plot of the emission spectrum of the phosphor sample prepared in example 3 at 416nm excitation and the excitation spectrum monitored at 695 nm.
Detailed Description
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:
the preparation method of the manganese-doped double perovskite dark red fluorescent powder comprises the following specific steps:
step (1) according to A2-2xCaB’1-xO6:2xR3+,xMn4+Preparing compounds containing relevant elements according to a stoichiometric ratio, mixing and grinding for 1.5-2h, fully vibrating the mixed powder, putting the powder into a high-temperature muffle furnace, heating the powder from room temperature to 800 ℃, preserving the heat for 1-2 h, continuing heating the powder to 1050-1150 ℃, preserving the heat for 2-3 h, and naturally cooling the powder to room temperature;
step (2), grinding the sample cooled to room temperature in the step (1) into powder again, and mixing uniformly;
and (3) putting the powder in the step (2) into a high-temperature muffle furnace, heating the muffle furnace from room temperature to 1200-1400 ℃, preserving the heat for 4-12 hours, then cooling the muffle furnace to 700-900 ℃, naturally cooling the muffle furnace to room temperature, and grinding the muffle furnace to obtain the manganese-doped double perovskite crimson fluorescent powder.
Further, the compound containing the relevant element is carbonate or oxide containing the relevant element;
further, manganese ion Mn is contained4+The compound of (A) is MnO2、MnCO3One or more of; containing strontium ions Sr2+The compound of (A) is SrCO3(ii) a Barium ion Ba2+The compound of (A) is BaCO3(ii) a Ca ion containing calcium2+The compound of (A) is CaCO3(ii) a Containing tungsten ions W6 +The compound of (A) is WO3(ii) a Molybdenum ion Mo6+The compound of (A) is MoO3(ii) a Containing rare earth ions R3+The compounds of (b) are the respective corresponding trivalent oxides.
Further, the heating rate and the cooling rate in the step (1) and the step (3) are 5-10 ℃/min.
Further, the calcination temperature in the step (3) is 1300 ℃, and the heat preservation time is 4 hours.
The method adopts a solid-phase reaction method, takes carbonate and oxide corresponding to related elements as raw materials, utilizes trivalent rare earth ions to balance charges, effectively improves the fluorescence intensity of the material, prepares the deep red fluorescent powder which can be excited by a commercial LED chip, and can be used in the field of LED illumination and artificial light sources for assisting plant growth as the fluorescent powder for lamps. The trivalent rare earth ions are used for balancing the charges, so that the fluorescence intensity of the material can be effectively improved.
Example 1
2.8064g of SrCO were weighed3(0.019mol), 0.1629g of La2O3(0.0005mol)，1.0010gCaCO3(0.01mol)，1.3688gMoO3(0.0095mol)，0.0435gMnO2(0.0005mol) the powder was mixed in an agate mortar and ground for 2 h. Weighing 1g of mixed powder, putting the mixed powder into a crucible, fully compacting the mixed powder, putting the compacted mixed powder into a high-temperature muffle furnace, heating the mixed powder from room temperature to 700 ℃, keeping the temperature for 1 hour, and then continuously rising the temperatureHeating to 1050 ℃, preserving heat for 2 hours, naturally cooling to room temperature, grinding the sample again for 10 minutes to powder, mixing uniformly, putting the mixture into the crucible again, fully compacting the mixture, putting the mixture into a high-temperature muffle furnace, heating from room temperature to 1300 ℃, preserving heat for 4 hours, then cooling to 900 ℃, ending the procedure, naturally cooling to room temperature, grinding the sample cooled to room temperature to powder to obtain Sr1.9La0.1CaMo0.95Mn0.05O6The manganese-doped double perovskite deep red fluorescent powder.
FIG. 2 is a graph of the emission spectrum of a phosphor sample prepared in example 1 at 493nm excitation and the excitation spectrum monitored at 683 nm.
Example 2
2.6882g of SrCO were weighed3(0.0182mol), 0.3291g of Gd2O3，1.0010gCaCO3(0.01mol)，1.3111gMoO3(0.0091mol)，0.0783gMnO2(0.0009mol) the mixed powder was ground in an agate mortar for 2 h. Weighing 1g of mixed powder, placing the mixed powder into a crucible, fully vibrating the mixed powder, placing the mixed powder into a high-temperature muffle furnace, heating the mixed powder from room temperature to 700 ℃, keeping the temperature for 1 hour, continuing to heat the mixed powder to 1050 ℃, keeping the temperature for 2 hours, naturally cooling the mixed powder to room temperature, grinding the sample for 10 minutes again to form powder, uniformly mixing the powder, placing the mixed powder into the crucible again, fully vibrating the mixed powder, placing the mixed powder into the high-temperature muffle furnace, heating the mixed powder to 1300 ℃ from the room temperature, keeping the temperature for 4 hours, cooling the mixed powder to 900 ℃, ending the procedure, naturally cooling the mixed powder to the room temperature, grinding the sample cooled1.82La0.18CaMo0.91Mn0.09O6The manganese-doped double perovskite deep red fluorescent powder.
FIG. 3 is a graph of the emission spectrum at 493nm and the excitation spectrum at 683nm for the phosphor samples prepared in example 2 and the phosphor samples without the addition of a charge compensation agent.
Example 3
3.6723g of BaCO were weighed out3(0.0186mol), 0.2281g of La2O3(0.0007mol)，1.0010gCaCO3(0.01mol)，1.3400gMoO3(0.0093mol)，0.0609gMnO2(0.0007mol) mixing the powders in an agate mortarAnd (5) grinding for 2 h. Weighing 1g of mixed powder, placing the mixed powder into a crucible, fully vibrating the mixed powder, placing the mixed powder into a high-temperature muffle furnace, heating the mixed powder from room temperature to 700 ℃, keeping the temperature for 1 hour, continuing to heat the mixed powder to 1050 ℃, keeping the temperature for 2 hours, naturally cooling the mixed powder to the room temperature, grinding the sample for 10 minutes again to form powder, uniformly mixing the powder, placing the mixed powder into the crucible again, fully vibrating the mixed powder, placing the mixed powder into the high-temperature muffle furnace, heating the mixed powder to 1300 ℃ from the room temperature, keeping the temperature for 4 hours, cooling the mixed powder to 900 ℃, naturally cooling the mixed powder to the room temperature, grinding the sample cooled to the room1.86La0.14CaMo0.93Mn0.07O6The manganese-doped double perovskite deep red fluorescent powder.
FIG. 1 is an X-ray diffraction pattern of phosphor samples prepared according to example 1, example 2, example 3 (a is example 1, b is example 2, c is example 3);
FIG. 4 is a plot of the emission spectrum of the phosphor sample prepared in example 3 at 416nm excitation and the excitation spectrum monitored at 695 nm.
Example 4
3.5144g of BaCO were weighed out3(0.0178mol), 0.3584g of La2O3(0.0011mol)，1.0010gCaCO3(0.01mol)，1.2823gMoO3(0.0089mol)，0.0957gMnO2(0.0011mol) the mixed powder was ground in an agate mortar for 2 hours. Weighing 1g of mixed powder, placing the mixed powder into a crucible, fully vibrating the mixed powder, placing the mixed powder into a high-temperature muffle furnace, heating the mixed powder from room temperature to 700 ℃, keeping the temperature for 1 hour, continuing to heat the mixed powder to 1050 ℃, keeping the temperature for 2 hours, naturally cooling the mixed powder to the room temperature, grinding the sample again for 10 minutes to obtain a powder, uniformly mixing the powder, placing the mixed powder into the crucible again, fully vibrating the mixed powder, placing the mixed powder into the high-temperature muffle furnace, heating the mixed powder to 1350 ℃ from the room temperature, keeping the temperature for 4 hours, cooling the mixed powder to 700 ℃, naturally cooling the mixed powder to the room temperature, grinding the sample cooled to the1.78La0.22CaMo0.89Mn0.11O6The manganese-doped double perovskite deep red fluorescent powder.

Claims (10)

1. A manganese-doped double perovskite deep red fluorescent powder is characterized in that:
the chemical general formula is as follows: a. the2-2xCaB’1-xO6:2xR3+,xMn4+；
Wherein: a is one of Sr and Ba;
b' is one of Mo and W;
r is one of La, Gd, Eu, Y, Sm, Nd and Dy;
the value range of x is more than or equal to 0.001 and less than or equal to 0.130.
2. A preparation method of manganese-doped double perovskite dark red fluorescent powder is characterized by comprising the following steps:
step (1) according to A2-2xCaB’1-xO6:2xR3+,xMn4+Preparing compounds containing relevant elements according to a stoichiometric ratio, mixing and grinding for 1.5-2h, fully vibrating the mixed powder, putting the powder into a high-temperature muffle furnace, heating the powder from room temperature to 800 ℃, preserving the heat for 1-2 h, continuing heating the powder to 1050-1150 ℃, preserving the heat for 2-3 h, and naturally cooling the powder to room temperature;
step (2), grinding the sample cooled to room temperature in the step (1) into powder again, and mixing uniformly;
and (3) putting the powder in the step (2) into a high-temperature muffle furnace, heating the muffle furnace from room temperature to 1200-1400 ℃, preserving the heat for 4-12 hours, then cooling the muffle furnace to 900 ℃ from the room temperature, naturally cooling the muffle furnace to the room temperature, and grinding the muffle furnace to obtain the manganese-doped double perovskite red fluorescent powder.
3. The method for preparing manganese-doped double perovskite deep red phosphor according to claim 2, wherein A is2-2xCaB’1-xO6:2xR3+,xMn4+The compound containing the relevant element is carbonate or oxide containing the relevant element.
4. The method for preparing manganese-doped double perovskite deep red phosphor according to claim 2, wherein the manganese-doped double perovskite deep red phosphor is characterized by containing manganese ions Mn4+The compound of (A) is MnO2、MnCO3One or more of (a).
5. The method for preparing manganese-doped double perovskite deep red phosphor according to claim 2, wherein the strontium ion Sr is contained2+The compound of (A) is SrCO3(ii) a Barium ion Ba2+The compound of (A) is BaCO3。
6. The method for preparing manganese-doped double perovskite deep red phosphor according to claim 2, wherein the phosphor contains Ca ions2+The compound of (A) is CaCO3(ii) a Containing tungsten ions W6+The compound of (A) is WO3。
7. The method for preparing manganese-doped double perovskite deep red phosphor according to claim 2, wherein the molybdenum ion Mo is contained6+The compound of (A) is MoO3。
8. The method for preparing manganese-doped double perovskite deep red phosphor according to claim 2, wherein R is rare earth ion3+The compounds of (b) are the respective corresponding trivalent oxides.
9. The method for preparing manganese-doped double perovskite deep red phosphor according to claim 2, wherein the temperature rise rate and the temperature drop rate in the steps (1) and (3) are 5-10 ℃/min.
10. The method for preparing manganese-doped double perovskite deep red phosphor according to claim 2, wherein the calcination temperature in the step (3) is 1300 ℃ and the holding time is 4 hours.
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