CN110055068B - Visible-near infrared luminescent material and preparation method thereof - Google Patents

Visible-near infrared luminescent material and preparation method thereof Download PDF

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CN110055068B
CN110055068B CN201910441199.4A CN201910441199A CN110055068B CN 110055068 B CN110055068 B CN 110055068B CN 201910441199 A CN201910441199 A CN 201910441199A CN 110055068 B CN110055068 B CN 110055068B
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解荣军
毛敏倩
曾华涛
周天亮
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Xiamen University
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Abstract

A visible-near infrared luminescent material and a preparation method thereof relate to luminescent materials. The visible-near infrared luminescent material consists of Y3Al2‑xCrx(AlO4)3With Ca3Al2‑yCry(SiO4)3Solid solution is formed according to the molar ratio M: 1. During preparation, a Y precursor, an Al precursor and a Cr precursor are mixed and subjected to high-temperature solid-phase reaction in a reducing atmosphere to obtain Y3Al2‑xCrx(AlO4)3(ii) a Mixing the Ca precursor, the Al precursor, the Cr precursor and the Si precursor, and carrying out high-temperature solid-phase reaction in a reducing atmosphere to obtain Ca3Al2‑yCry(SiO4)3(ii) a Will Y3Al2‑ xCrx(AlO4)3And Ca3Al2‑yCry(SiO4)3Mixing according to the molar ratio M: 1, and carrying out high-temperature solid-phase reaction in a reducing atmosphere to obtain the visible-near infrared luminescent material.

Description

Visible-near infrared luminescent material and preparation method thereof
Technical Field
The invention relates to a luminescent material, in particular to a visible-near infrared luminescent material and a preparation method thereof.
Background
First, the visible-near infrared analysis technique is a highly new analysis technique rapidly developed in the field of analytical chemistry, and has attracted more and more attention from analytical experts at home and abroad. Compared with the traditional analysis technology, the near infrared spectrum analysis technology has a plurality of advantages, and can complete the measurement of a plurality of performance indexes of a sample to be measured only by completing the acquisition and measurement of visible-near infrared spectrum once for the sample to be measured within a few minutes. The analysis sample does not need to be pretreated during spectral measurement; other materials are not consumed or a sample is not damaged in the analysis process; the analysis reproducibility is good, and the cost is low.
Secondly, the visible-near infrared analysis technology is realized on the premise of a proper visible-near infrared spectrum light source, and the wider the spectrum in the visible-near infrared range of the light source, the better the efficiency. The traditional visible-near infrared light source, such as a xenon lamp, has large volume, high heat generation and short service life. The visible-near infrared LED chip has the advantages of firm structure, small volume, energy conservation and the like, overcomes the defects of a xenon lamp to a certain extent, but has a narrow spectrum range, a plurality of chips with different light-emitting wave bands are needed to be spliced to obtain a wider spectrum, but the aging rates of the chips of different types are different, so that the stability of the visible-near infrared LED light source spectrum of the whole chip is poor. The visible-near infrared LED light source based on the blue light chip to excite the visible-near infrared luminescent material has visible-near infrared spectrum all derived from the luminescence of the luminescent material, and the manufacturing of satisfactory visible-near infrared light source becomes possible as long as the performance of the luminescent material is ensured to be stable enough and the spectrum is wide enough.
Again, some luminescent materials with emission spectra in the visible-near infrared region, such as BaAl, are reported in the present disclosure2O4:Cr3+(1、Singh V.，Chakradhar R.P.S.，Rao J.L.，et al，Studies on red-emitting Cr3+A polypeptide phosphate-associated by combustion process, Materials Chemistry and Physics, 2008, 111: 143-; such as Sr2Si5N8:Nd3+/Eu2+(2、
Figure BDA0002072067730000011
S., Katelnikovas A., Haase M., et al, New NIR emitting phosphor for blue leds with stable light output up to 180 ℃, Journal of Luminescence, 2016,172: 185-. However, the full width at half maximum of the emission spectrum of the luminescent materials is only tens of nanometers and is relatively narrow, so that the application requirement of a visible-near infrared spectrum light source cannot be met.
Finally, in general, if the a and B species have the same crystal structure and similar chemical formula, a solid solution can often be formed. Whereas if A and B are exactly luminescent materials, the solid solution formed by A and B is luminescentThe light should be between a and B. This phenomenon has been demonstrated in a variety of luminescent material systems that can form solid solutions. Such as Ca3Al2O6:Eu2+Has a main peak of the emission spectrum of about 650nm, Sr3Al2O6:Eu2+Has the same crystal structure and similar chemical formula and can form a solid solution Ca near 605nm3-xSrxAl2O6:Eu2+(0 ≦ x ≦ 3) having an emission spectrum with a main peak between 650 and 605nm varying with the value of x (3, Tianliang Zhou, Zhen Song, Liu Bian, et al, Synthesis and luminescence properties of Escherichia coli activated Ca)3Al2O6-Sr3Al2O6System, Journal of Rare Earth, 2012, 30(7):632-636), similar phenomena in other systems, such as Ca2- xSrxSi5N8:Eu2+(4、Van den Eeckhout K，Smet P，Poelman D，Luminescent afterglow behavior in the M2Si5N8:Eu family(M＝Ca，Sr，B1)，Materials，2011，4(6):980-990)、Sr1-xCaxAlSiN3:Eu2+The same applies to (5, Peter Schmidt, Thomas J ü stel, Walter Mayr, et al, Light-emitting device comprising an Eu (II) -activated phosphor, US7061024B2, 2006).
Y3Al2(AlO4)3:Cr3+And Ca3Al2(SiO4)3:Cr3+With the same crystal structure and similar chemical formula, a solid solution can be formed, the main peaks of the emission spectra of the solid solution and the solid solution are respectively positioned at 705nm and 700nm, and the full width at half maximum of the emission spectra is about 45 nm. Obviously, Y3Al2(AlO4)3:Cr3+And Ca3Al2(SiO4)3:Cr3+If a solid solution is formed, the luminescence properties (main peak of emission spectrum) should be in between.
Disclosure of Invention
The first purpose of the invention is to provideWith Cr3+The material is an activator, can generate visible-near infrared emission under the excitation of blue light, has low cost of raw materials and relatively low synthesis temperature, and can be applied to a visible-near infrared luminescent material of a visible-near infrared LED device.
The second purpose of the invention is to provide a preparation method of the visible-near infrared luminescent material.
The visible-near infrared luminescent material consists of Y3Al2-xCrx(AlO4)3With Ca3Al2-yCry(SiO4)3Solid solution is formed according to the molar ratio M: 1, wherein M is more than 0.5 and less than 11, x is more than 0 and less than 1.5, and y is more than 0 and less than 1.5; preferably, M is 2 and x ═ y ═ 0.6.
The preparation method of the visible-near infrared luminescent material comprises the following steps:
1) mixing a Y precursor, an Al precursor and a Cr precursor, and carrying out high-temperature solid-phase reaction in a reducing atmosphere to obtain Y3Al2-xCrx(AlO4)3；
2) Mixing the Ca precursor, the Al precursor, the Cr precursor and the Si precursor, and carrying out high-temperature solid-phase reaction in a reducing atmosphere to obtain Ca3Al2-yCry(SiO4)3；
3) Will Y3Al2-xCrx(AlO4)3And Ca3Al2-yCry(SiO4)3Mixing according to the molar ratio M: 1, and carrying out high-temperature solid-phase reaction in a reducing atmosphere to obtain the visible-near infrared luminescent material.
In the step 1), the molar ratio of Y, Al and Cr in the Y precursor, the Al precursor and the Cr precursor can be 3: 5-x: x, wherein x is more than 0 and less than 1.5; the Y precursor can be at least one selected from carbonate of Y, oxide of Y, oxalate of Y, nitrate of Y and the like; the Al precursor can be selected from at least one of Al carbonate, Al oxide, Al oxalate, Al nitrate and the like; the Cr precursor can be selected from at least one of Cr carbonate, Cr oxide, Cr oxalate, Cr nitrate and the like; the purities of the Y precursor, the Al precursor and the Cr precursor are not lower than 99.5%; the reducing atmosphere can be ammonia gas or nitrogen-hydrogen mixed gas, the temperature of the high-temperature solid-phase reaction can be 1550-1650 ℃, and the time of the high-temperature solid-phase reaction can be 4-10 h.
In the step 2), the molar ratio of Ca, Al, Cr and Si in the Ca precursor, the Al precursor, the Cr precursor and the Si precursor can be 3: 2-y: 3, wherein y is more than 0 and less than 1.5; the Ca precursor may be at least one selected from the group consisting of Ca carbonate, Ca oxide, Ca oxalate, Ca nitrate, and the like; the Al precursor can be selected from at least one of Al carbonate, Al oxide, Al oxalate, Al nitrate and the like; the Cr precursor can be selected from at least one of Cr carbonate, Cr oxide, Cr oxalate, Cr nitrate and the like; the Si precursor can be silicon dioxide and the like; the purity of the Ca precursor, the Al precursor, the Cr precursor and the Si precursor is not lower than 99.5%; the reducing atmosphere can be ammonia gas or nitrogen-hydrogen mixed gas; the temperature of the high-temperature solid-phase reaction can be 1250-1350 ℃, and the time of the high-temperature solid-phase reaction can be 4-10 h.
In step 3), the Y3Al2-xCrx(AlO4)3And Ca3Al2-yCry(SiO4)3Mixing at a molar ratio of M: 1, wherein M is more than 0.5 and less than 11. The reducing atmosphere can be ammonia gas or nitrogen-hydrogen mixed gas; the temperature of the high-temperature solid-phase reaction can be 1450-1550 ℃, and the time of the high-temperature solid-phase reaction can be 4-10 h.
Compared with the prior art, the visible-near infrared luminescent material prepared according to the invention has luminescent properties completely different from those of the traditional knowledge. The material is made of Cr3+As an activator, under the excitation of blue light, the main peak of the emission spectrum is positioned near 744nm, and the full width at half maximum of the emission spectrum exceeds 170 nm. The raw materials for synthesizing the material have low cost and relatively low synthesis temperature, so that the luminescent material can be applied to visible-near infrared LED devices.
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FIG. 1 is a graph showing an emission spectrum of a luminescent material obtained in comparative example 1 of the present invention.
FIG. 2 is a graph showing an emission spectrum of a luminescent material obtained in comparative example 2 of the present invention.
FIG. 3 is a graph showing an emission spectrum of a luminescent material obtained in comparative example 3 of the present invention.
FIG. 4 is a graph showing an emission spectrum of a luminescent material obtained in comparative example 4 of the present invention.
FIG. 5 is a graph showing an emission spectrum of a luminescent material obtained in comparative example 5 of the present invention.
FIG. 6 is a graph showing an emission spectrum of a visible-near infrared luminescent material obtained in example 1 of the present invention.
FIG. 7 is a graph showing an emission spectrum of a visible-near infrared luminescent material obtained in example 2 of the present invention.
FIG. 8 is a graph showing an emission spectrum of a visible-near infrared luminescent material obtained in example 3 of the present invention.
FIG. 9 is a graph showing an emission spectrum of a visible-near infrared luminescent material obtained in example 4 of the present invention.
Detailed Description
The following examples will further illustrate the present invention with reference to the accompanying drawings.
The visible-near infrared luminescent material is prepared from Y3Al2-xCrx(AlO4)3With Ca3Al2-yCry(SiO4)3The solid solution is formed according to the molar ratio M: 1, wherein M is more than 0.5 and less than 11, x is more than 0 and less than 1.5, and y is more than 0 and less than 1.5.
In one embodiment of the present invention, M is preferably 0.6, x is preferably 0.01, and y is preferably 0.01; in one embodiment of the present invention, M is preferably 1, x is preferably 0.1, and y is preferably 0.1; in one embodiment of the present invention, M is preferably 2, x is preferably 0.2, and y is preferably 0.2; in one embodiment of the present invention, M is preferably 2, x is preferably 0.6, and y is preferably 0.6; in one embodiment of the present invention, M is preferably 2, x is preferably 1, and y is preferably 1; in one embodiment of the present invention, M is preferably 4, x is preferably 0.04, and y is preferably 1.2; in one embodiment of the present invention, M is preferably 6, x is preferably 0.4, and y is preferably 1; in one embodiment of the present invention, M is preferably 8, x is preferably 1.2, and y is preferably 1; in another embodiment of the present invention, M is preferably 10, x is preferably 0.01, and y is preferably 1.4.
The embodiment of the preparation method of the visible-near infrared luminescent material comprises the following steps:
1) mixing a Y precursor, an Al precursor and a Cr precursor, and carrying out high-temperature solid-phase reaction in a reducing atmosphere to obtain Y3Al2-xCrx(AlO4)3；
2) Mixing the Ca precursor, the Al precursor, the Cr precursor and the Si precursor, and carrying out high-temperature solid-phase reaction in a reducing atmosphere to obtain Ca3Al2-yCry(SiO4)3；
3) Will Y3Al2-xCrx(AlO4)3And Ca3Al2-yCry(SiO4)3Mixing according to a molar ratio M: 1, and carrying out high-temperature solid-phase reaction in a reducing atmosphere to obtain the visible-near infrared luminescent material.
In the step 1), the molar ratio of Y, Al to Cr in the Y precursor, the Al precursor and the Cr precursor is 3: 5-x: x, wherein x is more than 0 and less than 1.5.
In the step 1), the Y precursor is a compound containing Y, which is well known in the art, and is not particularly limited, and in the present invention, the Y precursor is preferably one or more selected from the group consisting of a carbonate of Y, an oxide of Y, an oxalate of Y, and a nitrate of Y, and more preferably an oxide of Y, that is, yttrium oxide; the Al precursor can be selected from one or more of Al carbonate, Al oxide, Al oxalate and Al nitrate, and is more preferably Al oxide, namely alumina; the Cr precursor may be selected from one or more of a carbonate of Cr, an oxide of Cr, an oxalate of Cr, and a nitrate of Cr, and more preferably is an oxide of Cr, i.e., chromium sesquioxide.
In the step 2), the molar ratio of Ca, Al, Cr and Si in the Ca precursor, the Al precursor, the Cr precursor and the Si precursor is 3: 2-y: 3, wherein y is more than 0 and less than 1.5.
In the step 2), the Ca precursor may be a compound containing Ca, which is well known in the art, and is not particularly limited, and in the present invention, the Ca precursor is preferably one or more selected from the group consisting of a carbonate of Ca, an oxide of Ca, an oxalate of Ca, and a nitrate of Ca, and more preferably a carbonate of Ca, i.e., calcium carbonate; the Al precursor is selected from one or more of Al carbonate, Al oxide, Al oxalate and Al nitrate, and is more preferably Al oxide, namely alumina; the Cr precursor is selected from one or more of Cr carbonate, Cr oxide, Cr oxalate and Cr nitrate, and is more preferably Cr oxide, namely chromic oxide; the Si precursor is selected from silicon dioxide.
In the above step 3), Y3Al2-xCrx(AlO4)3And Ca3Al2-yCry(SiO4)3Mixing at a molar ratio of M: 1, wherein M is more than 0.5 and less than 11.
The purity of the Y precursor, the Ca precursor, the Al precursor, the Cr precursor and the Si precursor is not lower than 99.5%, and the higher the purity is, the less impurities are in the obtained luminescent material.
In the step 1), the temperature of the high-temperature solid-phase reaction is 1550-1650 ℃, the reducing atmosphere is ammonia gas or mixed gas of nitrogen and hydrogen, and the time of the high-temperature solid-phase reaction is 4-10 hours.
In the step 2), the temperature of the high-temperature solid-phase reaction is 1250-1350 ℃, the reducing atmosphere is ammonia gas or mixed gas of nitrogen and hydrogen, and the time of the high-temperature solid-phase reaction is 4-10 hours.
In the step 3), the temperature of the high-temperature solid-phase reaction is 1450-1550 ℃, the reducing atmosphere is ammonia gas or mixed gas of nitrogen and hydrogen, and the time of the high-temperature solid-phase reaction is 4-10 hours.
The temperature of the high-temperature solid phase in the step 1) is preferably 1550-1650 ℃, and the reducing atmosphere is ammonia gas or nitrogen-hydrogen mixed gas; in some embodiments provided herein, the temperature of the high temperature solid phase is preferably 1600 ℃.
The time for high-temperature solid phase in the step 1) is preferably 4-10 h, and more preferably 5-8 h; in some embodiments provided herein, the time for the high temperature solid phase is preferably 6 hours.
The reducing atmosphere in the step 1) is not particularly limited as long as it is a dry atmosphere known to those skilled in the art, and ammonia gas is preferable in the present invention.
The temperature of the high-temperature solid phase in the step 2) is preferably 1250-1350 ℃, and the reducing atmosphere is ammonia gas or nitrogen-hydrogen mixed gas; in some embodiments provided herein, the temperature of the high temperature solid phase is preferably 1300 ℃.
The time for high-temperature solid phase in the step 2) is preferably 4-10 h, and more preferably 5-8 h; in some embodiments provided herein, the time for the high temperature solid phase is preferably 6 hours.
The reducing atmosphere in the step 2) is not particularly limited as long as it is a dry atmosphere known to those skilled in the art, and ammonia gas is preferable in the present invention.
The temperature of the high-temperature solid phase in the step 3) is preferably 1450-1550 ℃, and the reducing atmosphere is ammonia gas or nitrogen-hydrogen mixed gas; in some embodiments provided herein, the temperature of the high temperature solid phase is preferably 1500 ℃.
The time for high-temperature solid phase in the step 3) is preferably 4-10 h, and more preferably 5-8 h; in some embodiments provided herein, the time for the high temperature solid phase is preferably 6 hours.
The reducing atmosphere in the step 3) is not particularly limited as long as it is a dry atmosphere known to those skilled in the art, and ammonia gas is preferable in the present invention.
The high-temperature solid-phase reaction phase is preferably carried out in a high-temperature furnace; after the reaction of the steps 1) to 3) is carried out, the visible-near infrared luminescent material can be obtained after the reaction is cooled to room temperature along with the furnace.
The embodiment of the invention successfully prepares the visible-near infrared luminescent material by adopting high-temperature solid-phase reaction.
In order to further illustrate the present invention, a visible-near infrared light emitting material and a method for preparing the same according to the present invention are described in detail below with reference to examples.
The reagents used in the following comparative examples and examples are all commercially available.
Comparative example 1
The raw material is Y2O3(analytical grade), Al2O3(analytically pure) and Cr2O3(analytically pure) with a molar ratio of 1.5: 2.2: 0.3, grinding and uniformly mixing the raw materials, putting the mixture into a crucible, sintering the mixture at 1600 ℃ for 6 hours in a high-temperature furnace in an ammonia reduction atmosphere, and cooling the mixture to room temperature along with the furnace to obtain the theoretical chemical component Y3Al1.4Cr0.6(AlO4)3The light-emitting material of (1).
The luminescent material obtained in comparative example 1 was analyzed by a fluorescence spectrometer to obtain an emission spectrum thereof, as shown in fig. 1. It can be seen that the material can be excited by blue light, the main peak of the emission spectrum is located near 705nm, and the highest intensity of the spectral luminescence peak and the full width at half maximum of the emission spectrum under the excitation of the blue light are shown in table 1. It can be seen that comparative example 1 corresponds to the luminescent material having a low luminous intensity and a narrow half-height width of less than 45 nm.
Comparative example 2
The raw material is CaCO3(analytical grade), Al2O3(analytically pure) Cr2O3(analytically pure) and SiO2(analytically pure) at a molar ratio of 3: 0.7: 0.3: 3, grinding and mixing the above raw materials, placing into a crucible, sintering at 1300 deg.C for 6h in a high temperature furnace under an ammonia reducing atmosphere, and cooling to room temperature to obtain Ca as a theoretical chemical component3Al1.4Cr0.6(SiO4)3The light-emitting material of (1).
The luminescent material obtained in comparative example 2 was analyzed by a fluorescence spectrometer to obtain an emission spectrum thereof, as shown in fig. 2. It can be seen that the material can be excited by blue light, the main peak of the emission spectrum is located near 700nm, and the highest intensity of the spectral luminescence peak and the full width at half maximum of the emission spectrum under the excitation of the blue light are shown in table 1. It can be seen that comparative example 2 has a lower luminescence intensity and a narrower half-height width, which is less than 45 nm.
Comparative example 3
Step 1), the raw material is Y2O3(analytical grade), Al2O3(analytically pure) and Cr2O3(analytically pure) at a molar ratio of 1.5: 2.2: 0.3, grinding and uniformly mixing the raw materials, putting the mixture into a crucible, reducing the mixture in an ammonia reducing atmosphere,sintering the mixture for 6 hours at 1600 ℃ in a high-temperature furnace, and cooling the sintered mixture to room temperature along with the furnace to obtain the material with the theoretical chemical component of Y3Al1.4Cr0.6(AlO4)3The light-emitting material of (1).
Step 2), the raw material is CaCO3(analytical grade), Al2O3(analytically pure) Cr2O3(analytically pure) and SiO2(analytically pure) at a molar ratio of 3: 0.7: 0.3: 3, grinding and mixing the above raw materials, placing into a crucible, sintering at 1300 deg.C for 6h in a high temperature furnace under an ammonia reducing atmosphere, and cooling to room temperature to obtain Ca as a theoretical chemical component3Al1.4Cr0.6(SiO4)3The light-emitting material of (1).
Step 3), mixing Y3Al1.4Cr0.6(AlO4)3And Ca3Al1.4Cr0.6(SiO4)3Mixing at a molar ratio of 0.4: 1, placing into a crucible, sintering at 1500 deg.C for 6 hr in a high temperature furnace under ammonia reducing atmosphere, and cooling to room temperature to obtain a product with theoretical chemical composition of 0.4Y3Al1.4Cr0.6(AlO4)3·Ca3Al1.4Cr0.6(SiO4)3The material of (1).
The material obtained in comparative example 3 was analyzed by a fluorescence spectrometer to obtain an emission spectrum thereof, as shown in fig. 3. It can be seen that the material hardly emits light under excitation of blue light.
Comparative example 4
Step 1), the raw material is Y2O3(analytical grade), Al2O3(analytically pure) and Cr2O3(analytically pure) with a molar ratio of 1.5: 2.2: 0.3, grinding and uniformly mixing the raw materials, putting the mixture into a crucible, sintering the mixture at 1600 ℃ for 6 hours in a high-temperature furnace in an ammonia reduction atmosphere, and cooling the mixture to room temperature along with the furnace to obtain the theoretical chemical component Y3Al1.4Cr0.6(AlO4)3The light-emitting material of (1).
Step 2), the raw material is CaCO3(analytical grade), Al2O3(analytically pure) Cr2O3(minute)Purity) and SiO2(analytically pure) at a molar ratio of 3: 0.7: 0.3: 3, grinding and mixing the above raw materials, placing into a crucible, sintering at 1300 deg.C for 6h in a high temperature furnace under an ammonia reducing atmosphere, and cooling to room temperature to obtain Ca as a theoretical chemical component3Al1.4Cr0.6(SiO4)3The light-emitting material of (1).
Step 3), mixing Y3Al1.4Cr0.6(AlO4)3And Ca3Al1.4Cr0.6(SiO4)3According to a molar ratio of 12: 1, mixing, placing into a crucible, sintering at 1500 ℃ for 6h in a high-temperature furnace under the reducing atmosphere of ammonia gas, and cooling to room temperature along with the furnace to obtain the material with the theoretical chemical composition of 12Y3Al1.4Cr0.6(AlO4)3·Ca3Al1.4Cr0.6(SiO4)3The material of (1).
The luminescent material obtained in comparative example 4 was analyzed by a fluorescence spectrometer to obtain an emission spectrum thereof, as shown in fig. 4. It can be seen that the material can be excited by blue light, the main peak of the emission spectrum is located near 705nm, and the highest intensity of the spectral luminescence peak and the full width at half maximum of the emission spectrum under the excitation of the blue light are shown in table 1. It can be seen that comparative example 4 corresponds to the luminescent material having a low luminous intensity and a narrow half-height width of less than 45 nm.
Comparative example 5
The raw material is Y2O3(analytically pure), CaCO3(analytical grade), Al2O3(analytically pure) Cr2O3(analytically pure) and SiO2(analytically pure) at a molar ratio of 1: 0.7: 0.3: 3, grinding and mixing the above raw materials, placing into a crucible, sintering at 1500 deg.C for 6h in an ammonia reducing atmosphere, furnace cooling to room temperature to obtain 2Y chemical component3Al1.4Cr0.6(AlO4)3·Ca3Al1.4Cr0.6(SiO4)3The light-emitting material of (1).
The luminescent material obtained in comparative example 5 was analyzed by a fluorescence spectrometer to obtain an emission spectrum thereof, as shown in fig. 5. The material can be excited by blue light, the main peak of the emission spectrum is located near 744nm, and the highest intensity of the spectral luminescence peak and the full width at half maximum of the emission spectrum under the excitation of the blue light are shown in table 1. It can be seen that comparative example 5 (without the multi-step synthesis) corresponds to a luminescent material with a lower luminescence intensity and a wider full width at half maximum of about 160 nm.
Example 1
Step 1), the raw material is Y2O3(analytical grade), Al2O3(analytically pure) and Cr2O3(analytically pure) with a molar ratio of 1.5: 2.495: 0.005, grinding and mixing the above raw materials, placing into a crucible, sintering at 1600 deg.C for 6h in a high temperature furnace under an ammonia reducing atmosphere, and cooling to room temperature to obtain the theoretical chemical component Y3Al1.99Cr0.01(AlO4)3The light-emitting material of (1).
Step 2), the raw material is CaCO3(analytical grade), Al2O3(analytically pure) Cr2O3(analytically pure) and SiO2(analytically pure) at a molar ratio of 3: 0.995: 0.005: 3, grinding and mixing the above raw materials, placing into a crucible, sintering at 1300 deg.C for 6h in a high temperature furnace under an ammonia reducing atmosphere, and furnace-cooling to room temperature to obtain Ca as a theoretical chemical component3Al1.99Cr0.01(SiO4)3The light-emitting material of (1).
Step 3), mixing Y3Al1.99Cr0.01(AlO4)3And Ca3Al1.99Cr0.01(SiO4)3Mixing at a molar ratio of 0.6: 1, placing into a crucible, sintering at 1500 deg.C for 6 hr in a high temperature furnace under ammonia reducing atmosphere, and cooling to room temperature to obtain a powder with theoretical chemical composition of 0.6Y3Al1.99Cr0.01(AlO4)3·Ca3Al1.99Cr0.01(SiO4)3The material of (1).
The fluorescent material obtained in example 1 was analyzed by a fluorescence spectrometer to obtain an emission spectrum thereof, as shown in fig. 6. The material can be excited by blue light, the main peak of the emission spectrum is located near 744nm, and the highest intensity of the spectral luminescence peak and the full width at half maximum of the emission spectrum under the excitation of the blue light are shown in table 1. It can be seen that the luminescent material of example 1 has a high luminous intensity, a wide full width at half maximum of about 171 nm.
Example 2
Step 1), the raw material is Y2O3(analytical grade), Al2O3(analytically pure) and Cr2O3(analytically pure) with a molar ratio of 1.5: 2.45: 0.05, grinding and mixing the above raw materials, placing into a crucible, sintering at 1600 deg.C for 6h in a high temperature furnace under an ammonia reducing atmosphere, and cooling to room temperature to obtain the theoretical chemical component Y3Al1.9Cr0.1(AlO4)3The light-emitting material of (1).
Step 2), the raw material is CaCO3(analytical grade), Al2O3(analytically pure) Cr2O3(analytically pure) and SiO2(analytically pure) at a molar ratio of 3: 0.95: 0.05: 3, grinding and mixing the above raw materials, placing into a crucible, sintering at 1300 deg.C for 6h in a high temperature furnace under an ammonia reducing atmosphere, and cooling to room temperature to obtain Ca as a theoretical chemical component3Al1.9Cr0.1(SiO4)3The light-emitting material of (1).
Step 3), mixing Y3Al1.9Cr0.1(AlO4)3And Ca3Al1.9Cr0.1(SiO4)3Mixing at a molar ratio of 1:1, placing into a crucible, sintering at 1500 deg.C for 6h in a high temperature furnace under ammonia reducing atmosphere, and cooling to room temperature to obtain a product with theoretical chemical component Y3Al1.9Cr0.1(AlO4)3·Ca3Al1.9Cr0.1(SiO4)3The material of (1).
The fluorescent material obtained in example 2 was analyzed by a fluorescence spectrometer to obtain an emission spectrum thereof, as shown in fig. 7. It can be seen that the material can be excited by blue light, the main peak of the emission spectrum is located near 746nm, and the highest intensity of the spectral luminescence peak and the full width at half maximum of the emission spectrum under the excitation of the blue light are shown in table 1. It can be seen that the luminescent material of example 2 has a high luminous intensity, a wide full width at half maximum, about 172 nm.
Example 3
Step 1), the raw material is Y2O3(analytical grade), Al2O3(analytically pure) and Cr2O3(analytically pure) with a molar ratio of 1.5: 2.4: 0.1, grinding and uniformly mixing the raw materials, putting the mixture into a crucible, sintering the mixture at 1600 ℃ for 6 hours in a high-temperature furnace in an ammonia reduction atmosphere, and cooling the mixture to room temperature along with the furnace to obtain the theoretical chemical component Y3Al1.8Cr0.2(AlO4)3The light-emitting material of (1).
Step 2), the raw material is CaCO3(analytical grade), Al2O3(analytically pure) Cr2O3(analytically pure) and SiO2(analytically pure) at a molar ratio of 3: 0.9: 0.1: 3, grinding and mixing the above raw materials, placing into a crucible, sintering at 1300 deg.C for 6h in a high temperature furnace under an ammonia reducing atmosphere, and cooling to room temperature to obtain Ca as a theoretical chemical component3Al1.8Cr0.2(SiO4)3The light-emitting material of (1).
Step 3), mixing Y3Al1.8Cr0.2(AlO4)3And Ca3Al1.8Cr0.2(SiO4)3Mixing at a molar ratio of 2:1, placing into a crucible, sintering at 1500 deg.C for 6 hr in a high temperature furnace under ammonia reducing atmosphere, and cooling to room temperature to obtain 2Y theoretical chemical component3Al1.8Cr0.2(AlO4)3·Ca3Al1.8Cr0.2(SiO4)3The material of (1).
The fluorescent material obtained in example 3 was analyzed by a fluorescence spectrometer to obtain an emission spectrum thereof, as shown in fig. 8. It can be seen that the material can be excited by blue light, the main peak of the emission spectrum is located near 748nm, and the highest intensity of the spectral luminescence peak and the full width at half maximum of the emission spectrum under the excitation of the blue light are shown in table 1. It can be seen that the luminescent material of example 3 has a high luminous intensity, a wide full width at half maximum, about 177 nm.
Example 4
Step (ii) of1) The raw material is Y2O3(analytical grade), Al2O3(analytically pure) and Cr2O3(analytically pure) with a molar ratio of 1.5: 2.2: 0.3, grinding and uniformly mixing the raw materials, putting the mixture into a crucible, sintering the mixture at 1600 ℃ for 6 hours in a high-temperature furnace in an ammonia reduction atmosphere, and cooling the mixture to room temperature along with the furnace to obtain the theoretical chemical component Y3Al1.4Cr0.6(AlO4)3The light-emitting material of (1).
Step 2), the raw material is CaCO3(analytical grade), Al2O3(analytically pure) Cr2O3(analytically pure) and SiO2(analytically pure) at a molar ratio of 3: 0.7: 0.3: 3, grinding and mixing the above raw materials, placing into a crucible, sintering at 1300 deg.C for 6h in a high temperature furnace under an ammonia reducing atmosphere, and cooling to room temperature to obtain Ca as a theoretical chemical component3Al1.4Cr0.6(SiO4)3The light-emitting material of (1).
Step 3), mixing Y3Al1.4Cr0.6(AlO4)3And Ca3Al1.4Cr0.6(SiO4)3Mixing at a molar ratio of 2:1, placing into a crucible, sintering at 1500 deg.C for 6 hr in a high temperature furnace under ammonia reducing atmosphere, and cooling to room temperature to obtain 2Y theoretical chemical component3Al1.4Cr0.6(AlO4)3·Ca3Al1.4Cr0.6(SiO4)3The material of (1).
The fluorescent material obtained in example 4 was analyzed by a fluorescence spectrometer to obtain an emission spectrum thereof, as shown in fig. 9. The material can be excited by blue light, the main peak of the emission spectrum is located near 744nm, and the highest intensity of the spectral luminescence peak and the full width at half maximum of the emission spectrum under the excitation of the blue light are shown in table 1. It can be seen that example 4 corresponds to the luminescent material having higher luminous intensity and wider full width at half maximum of about 175 nm.
Example 5
Step 1), the raw material is Y2O3(analytical grade), Al2O3(analytically pure) and Cr2O3(analytically pure),grinding the above raw materials at a molar ratio of 1.5: 2: 0.5, mixing, placing into a crucible, sintering at 1600 deg.C for 6 hr in a high temperature furnace under ammonia reducing atmosphere, and cooling to room temperature to obtain the product with theoretical chemical component of Y3AlCr(AlO4)3The light-emitting material of (1).
Step 2), the raw material is CaCO3(analytical grade), Al2O3(analytically pure) Cr2O3(analytically pure) and SiO2(analytically pure) at a molar ratio of 3: 0.5: 3, grinding and mixing the above raw materials, placing into a crucible, sintering at 1300 deg.C for 6h in a high temperature furnace under an ammonia reducing atmosphere, and cooling to room temperature to obtain Ca as a theoretical chemical component3AlCr(SiO4)3The light-emitting material of (1).
Step 3), mixing Y3AlCr(AlO4)3And Ca3AlCr(SiO4)3Mixing at a molar ratio of 2:1, placing into a crucible, sintering at 1500 deg.C for 6 hr in a high temperature furnace under ammonia reducing atmosphere, and cooling to room temperature to obtain 2Y theoretical chemical component3AlCr(AlO4)3·Ca3AlCr(SiO4)3The material of (1).
The fluorescent material obtained in example 5 was analyzed by a fluorescence spectrometer. It can be seen that the material can be excited by blue light, the main peak of the emission spectrum is located near 746nm, and the highest intensity of the spectral luminescence peak and the full width at half maximum of the emission spectrum under the excitation of the blue light are shown in table 1. It can be seen that the luminescent material of example 5 has a high luminous intensity, a wide full width at half maximum, and about 177 nm.
Example 6
Step 1), the raw material is Y2O3(analytical grade), Al2O3(analytically pure) and Cr2O3(analytically pure) with a molar ratio of 1.5: 2.48: 0.02, grinding and uniformly mixing the raw materials, putting the mixture into a crucible, sintering the mixture at 1600 ℃ for 6 hours in a high-temperature furnace in an ammonia reduction atmosphere, and cooling the mixture to room temperature along with the furnace to obtain the theoretical chemical component Y3Al1.96Cr0.04(AlO4)3The light-emitting material of (1).
Step 2), the raw material is CaCO3(analytical grade), Al2O3(analytically pure) Cr2O3(analytically pure) and SiO2(analytically pure) at a molar ratio of 3: 0.4: 0.6: 3, grinding and mixing the above raw materials, placing into a crucible, sintering at 1300 deg.C for 6h in a high temperature furnace under an ammonia reducing atmosphere, and cooling to room temperature to obtain Ca as a theoretical chemical component3Al0.8Cr1.2(SiO4)3The light-emitting material of (1).
Step 3), mixing Y3Al1.96Cr0.04(AlO4)3And Ca3Al0.8Cr1.2(SiO4)3Mixing at a molar ratio of 4: 1, placing into a crucible, sintering at 1500 deg.C for 6 hr in a high temperature furnace under ammonia reducing atmosphere, and cooling to room temperature to obtain a product with theoretical chemical composition of 4Y3Al1.96Cr0.04(AlO4)3·Ca3Al0.8Cr1.2(SiO4)3The material of (1).
The fluorescent material obtained in example 6 was analyzed by a fluorescence spectrometer. It can be seen that the material can be excited by blue light, the main peak of the emission spectrum is located near 745nm, and the highest intensity of the spectral luminescence peak and the full width at half maximum of the emission spectrum under the excitation of the blue light are shown in table 1. It can be seen that example 6 corresponds to the luminescent material having higher luminous intensity and wider full width at half maximum, which is about 173 nm.
Example 7
Step 1), the raw material is Y2O3(analytical grade), Al2O3(analytically pure) and Cr2O3(analytically pure) with a molar ratio of 1.5: 2.3: 0.2, grinding and uniformly mixing the raw materials, putting the mixture into a crucible, sintering the mixture at 1600 ℃ for 6 hours in a high-temperature furnace in an ammonia reduction atmosphere, and cooling the mixture to room temperature along with the furnace to obtain the theoretical chemical component Y3Al1.6Cr0.4(AlO4)3The light-emitting material of (1).
Step 2), the raw material is CaCO3(analytical grade), Al2O3(analytically pure) Cr2O3(analytically pure) and SiO2(analytically pure) at a molar ratio of 3: 0.5: 3, and mixingGrinding the raw materials, uniformly mixing, placing into a crucible, sintering at 1300 ℃ for 6h in a high-temperature furnace under the reducing atmosphere of ammonia gas, and cooling to room temperature along with the furnace to obtain Ca as a theoretical chemical component3AlCr(SiO4)3The light-emitting material of (1).
Step 3), mixing Y3Al1.6Cr0.4(AlO4)3And Ca3AlCr(SiO4)3Mixing at a molar ratio of 6: 1, placing into a crucible, sintering at 1500 deg.C for 6h in a high temperature furnace under ammonia reducing atmosphere, and cooling to room temperature to obtain a theoretical chemical component of 6Y3Al1.6Cr0.4(AlO4)3·Ca3AlCr(SiO4)3The material of (1).
The fluorescent material obtained in example 7 was analyzed by a fluorescence spectrometer. It can be seen that the material can be excited by blue light, the main peak of the emission spectrum is located near 745nm, and the highest intensity of the spectral luminescence peak and the full width at half maximum of the emission spectrum under the excitation of the blue light are shown in table 1. It can be seen that example 7 corresponds to the luminescent material having a higher luminous intensity and a wider half width of about 175 nm.
Example 8
Step 1), the raw material is Y2O3(analytical grade), Al2O3(analytically pure) and Cr2O3(analytically pure) with a molar ratio of 1.5: 0.95: 0.05, grinding and uniformly mixing the raw materials, putting the mixture into a crucible, sintering the mixture at 1600 ℃ for 6h in a high-temperature furnace in an ammonia reduction atmosphere, and cooling the mixture to room temperature along with the furnace to obtain the theoretical chemical component Y3Al0.8Cr1.2(AlO4)3The light-emitting material of (1).
Step 2), the raw material is CaCO3(analytical grade), Al2O3(analytically pure) Cr2O3(analytically pure) and SiO2(analytically pure) at a molar ratio of 3: 0.5: 3, grinding and mixing the above raw materials, placing into a crucible, sintering at 1300 deg.C for 6h in a high temperature furnace under an ammonia reducing atmosphere, and cooling to room temperature to obtain Ca as a theoretical chemical component3AlCr(SiO4)3The light-emitting material of (1).
Step (ii) of3) Is a reaction of Y3Al0.8Cr1.2(AlO4)3And Ca3AlCr(SiO4)3Mixing at a molar ratio of 8: 1, placing into a crucible, sintering at 1500 deg.C for 6 hr in a high temperature furnace under ammonia reducing atmosphere, and cooling to room temperature to obtain 8Y3Al0.8Cr1.2(AlO4)3·Ca3AlCr(SiO4)3The material of (1).
The fluorescent material obtained in example 8 was analyzed by a fluorescence spectrometer. The material can be excited by blue light, the main peak of the emission spectrum is located near 744nm, and the highest intensity of the spectral luminescence peak and the full width at half maximum of the emission spectrum under the excitation of the blue light are shown in table 1. It can be seen that the luminescent material of example 8 has a high luminous intensity, a wide full width at half maximum, and about 177 nm.
Example 9
Step 1), the raw material is Y2O3(analytical grade), Al2O3(analytically pure) and Cr2O3(analytically pure) with a molar ratio of 1.5: 2.495: 0.005, grinding and mixing the above raw materials, placing into a crucible, sintering at 1600 deg.C for 6h in a high temperature furnace under an ammonia reducing atmosphere, and cooling to room temperature to obtain the theoretical chemical component Y3Al1.99Cr0.01(AlO4)3The light-emitting material of (1).
Step 2), the raw material is CaCO3(analytical grade), Al2O3(analytically pure) Cr2O3(analytically pure) and SiO2(analytically pure) at a molar ratio of 3: 0.3: 0.7: 3, grinding and mixing the above raw materials, placing into a crucible, sintering at 1300 deg.C for 6h in a high temperature furnace under an ammonia reducing atmosphere, and cooling to room temperature to obtain Ca as a theoretical chemical component3Al0.6Cr1.4(SiO4)3The light-emitting material of (1).
Step 3), mixing Y3Al1.99Cr0.01(AlO4)3And Ca3Al0.6Cr1.4(SiO4)3Mixing at a molar ratio of 10: 1, loading into a crucible, and reducing with ammonia gasThen sintering the mixture for 6 hours at 1500 ℃ in a high-temperature furnace, and cooling the mixture to room temperature along with the furnace to obtain the material with the theoretical chemical composition of 10Y3Al1.99Cr0.01(AlO4)3·Ca3Al0.6Cr1.4(SiO4)3The material of (1).
The fluorescent material obtained in example 9 was analyzed by a fluorescence spectrometer. The material can be excited by blue light, the main peak of the emission spectrum is positioned near 747nm, and the highest intensity of the spectral luminescence peak and the full width at half maximum of the emission spectrum under the excitation of the blue light are shown in table 1. It can be seen that the luminescent material of example 9 has a high luminous intensity, a wide full width at half maximum, and a wavelength of about 173 nm.
TABLE 1
Figure BDA0002072067730000121
The above examples are only for illustrating the embodiments of the present invention and illustrating the technical features of the present invention, and are not intended to limit the scope of the present invention. Any modification or equivalent arrangement which can be easily implemented by a person skilled in the art is intended to be within the scope of the present invention, which is defined by the following claims.

Claims (4)

1. A method for preparing a visible-near infrared luminescent material is characterized in that the visible-near infrared luminescent material is prepared from Y3Al2-xCrx(AlO4)3With Ca3Al2-yCry(SiO4)3Solid solution is formed according to the molar ratio M: 1, wherein M is more than 0.5 and less than 11, x is more than 0 and less than 1.5, and y is more than 0 and less than 1.5;
the preparation method of the visible-near infrared luminescent material comprises the following steps:
1) mixing a Y precursor, an Al precursor and a Cr precursor, and carrying out high-temperature solid-phase reaction in a reducing atmosphere to obtain Y3Al2-xCrx(AlO4)3(ii) a The molar ratio of Y, Al to Cr in the Y precursor, Al precursor and Cr precursor is 3: 5X, wherein x is more than 0 and less than 1.5; the Y precursor is at least one selected from carbonate of Y, oxide of Y, oxalate of Y and nitrate of Y; the Al precursor is selected from at least one of Al carbonate, Al oxide, Al oxalate and Al nitrate; the Cr precursor is selected from at least one of Cr carbonate, Cr oxide, Cr oxalate and Cr nitrate; the purities of the Y precursor, the Al precursor and the Cr precursor are not lower than 99.5%;
2) mixing the Ca precursor, the Al precursor, the Cr precursor and the Si precursor, and carrying out high-temperature solid-phase reaction in a reducing atmosphere to obtain Ca3Al2-yCry(SiO4)3(ii) a The molar ratio of Ca, Al, Cr and Si in the Ca precursor, the Al precursor, the Cr precursor and the Si precursor is 3: 2-y: 3, wherein y is more than 0 and less than 1.5; the Ca precursor is at least one of Ca carbonate, Ca oxide, Ca oxalate and Ca nitrate; the Al precursor is selected from at least one of Al carbonate, Al oxide, Al oxalate and Al nitrate; the Cr precursor is selected from at least one of Cr carbonate, Cr oxide, Cr oxalate and Cr nitrate; the Si precursor is silicon dioxide; the purity of the Ca precursor, the Al precursor, the Cr precursor and the Si precursor is not lower than 99.5%; the temperature of the high-temperature solid-phase reaction is 1250-1350 ℃, and the time of the high-temperature solid-phase reaction is 4-10 h;
3) will Y3Al2-xCrx(AlO4)3And Ca3Al2-yCry(SiO4)3Mixing according to the molar ratio M: 1, and carrying out high-temperature solid-phase reaction in a reducing atmosphere to obtain the visible-near infrared luminescent material.
2. The method for preparing the visible-near infrared luminescent material according to claim 1, wherein in the step 1), the temperature of the high-temperature solid-phase reaction is 1550 to 1650 ℃, and the time of the high-temperature solid-phase reaction is 4 to 10 hours.
3. The see-near of claim 1The preparation method of the infrared luminescent material is characterized in that in the step 3), Y is3Al2-xCrx(AlO4)3And Ca3Al2-yCry(SiO4)3Mixing at a molar ratio of M: 1, wherein M is more than 0.5 and less than 11; the temperature of the high-temperature solid-phase reaction is 1450-1550 ℃, and the time of the high-temperature solid-phase reaction is 4-10 hours.
4. The method for preparing the visible-near infrared luminescent material of claim 1, wherein in the steps 1) to 3), the reducing atmosphere is ammonia gas or a mixed gas of nitrogen and hydrogen.
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Citations (1)

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Publication number Priority date Publication date Assignee Title
CN105860975A (en) * 2016-04-13 2016-08-17 厦门大学 Down-conversion green phosphor and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN105860975A (en) * 2016-04-13 2016-08-17 厦门大学 Down-conversion green phosphor and preparation method thereof

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A RIETVELD STUDY OF THE CATION SUBSTITUTION BETWEEN UVAROVITE AND YTTRIUM-ALUMINUM SYNTHETIC GARNETS, OBTAINED BY SOL-GEL METHOD;CARDA, J; TENA, MA; MONROS, G; 等;《CRYSTAL RESEARCH AND TECHNOLOGY》;19941231;第29卷(第3期);387-391 *
CARDA, J;TENA, MA;MONROS, G;等.A RIETVELD STUDY OF THE CATION SUBSTITUTION BETWEEN UVAROVITE AND YTTRIUM-ALUMINUM SYNTHETIC GARNETS, OBTAINED BY SOL-GEL METHOD.《CRYSTAL RESEARCH AND TECHNOLOGY》.1994,第29卷(第3期),第387-391页. *
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