CN113817468B - Oxide near-infrared luminescent material, preparation method thereof and luminescent device - Google Patents
Oxide near-infrared luminescent material, preparation method thereof and luminescent device Download PDFInfo
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- CN113817468B CN113817468B CN202111139004.4A CN202111139004A CN113817468B CN 113817468 B CN113817468 B CN 113817468B CN 202111139004 A CN202111139004 A CN 202111139004A CN 113817468 B CN113817468 B CN 113817468B
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Abstract
The invention discloses an oxide near-infrared luminescent material, a preparation method thereof and a luminescent device; the near-infrared luminescent material contains an inorganic compoundThe chemical formula of the inorganic compound is A x B y C z O q D p (ii) a Wherein A is one or the combination of more than two of Mg, ca, sr, ba, lu, Y, gd or La elements; b is one or the combination of more than two of Sc, in, ga, mg, zr, ti, hf, sn, lu, Y, gd or La elements; c is one or the combination of more than two of Al, si or Ge elements; o is oxygen element; d is Cr element; x is more than or equal to 0.7 and less than or equal to 1.3, y is more than or equal to 0.7 and less than or equal to 1.3, Z is more than or equal to 1 and less than or equal to 3, q is more than or equal to 5 and less than or equal to 7<p is less than or equal to 0.3. The near-infrared luminescent material has the emission peak wavelength of about 930nm and the half-peak width of about 210nm, can be efficiently excited by blue light, and has good chemical stability and thermal stability.
Description
Technical Field
The invention belongs to the technical field of luminescent materials, and particularly relates to an oxide near-infrared luminescent material, a preparation method thereof and a luminescent device.
Background
In recent years, near-infrared light shows great application prospects in the fields of night vision illumination, security protection, remote sensing, optical fiber communication, plant growth, nondestructive detection, targeted therapy, iris recognition, food component analysis and the like, but the existing near-infrared light source still can not meet actual requirements in the aspects of luminous efficiency, emission bandwidth and the like, so that the development of a novel broadband near-infrared light source becomes a research hotspot of scholars at home and abroad. Among many design schemes, the near-infrared phosphor conversion LED has excellent emission peak position, bandwidth, luminous efficiency and thermal stability, and has the advantages of simple structure, adjustable spectrum, green and safe preparation method, low cost, easy realization of miniaturization, and is more expected to be used with portable devices such as mobile phones, etc., thereby being considered as the most reliable solution of the broadband near-infrared light source.
At present, the ions capable of generating near infrared emission in inorganic phosphors are mainly: pr (Pr) of 3+ ,Nd 3+ ,Tm 3+ , Eu 2 + ,Ce 3+ ,Yb 3+ ,Er 3+ ,Ho 3+ Plasma of rare earth ions and Cr 3+ ,Ni 2+ ,Mn 2+ And (3) waiting for transition metal ions. Wherein, pr 3+ ,Nd 3+ ,Tm 3+ ,Yb 3+ ,Er 3+ ,Ho 3+ Ions are emitted in sharp lines, so that the wide application of a near-infrared light source is difficult to meet; eu (Eu) 2+ ,Mn 2+ And Ce 3+ The near infrared luminescence of (2) has been reported in very few systems, and a considerable part of visible light still remains in the emission spectrum; ni 2+ Ions generally have dual-mode fluorescence in both visible and near infrared regions, but the efficiency of the latter is relatively low, which severely limits the feasibility of the ions as near infrared light sources; inverse Cr 3+ The ions not only have the broadband emission characteristic which is easy to realize, but also have higher luminous efficiency and adjustable emission spectrum, can be more directly and efficiently excited by a blue light LED, and have good research value and application prospect.
At present, cr 3+ The main emission peak of the ion-doped broadband near-infrared fluorescent powder is mostly before 900nm, the material is usually accompanied with a 'red storm' phenomenon in practical application, and a high-efficiency thermally-stable long-wave near-infrared emission material system is very deficient. For example, mg reported by Liuquanlin teacher of Beijing university of science and technology 2 GeO 4 :Cr 3+ And LiScGeO 4 :Cr 3+ Has broad band near infrared emission with main peaks at 940nm and 1110nm, respectively, but the luminous intensity at 100 ℃ is only about 30% at room temperature, which is far from the practical requirement (J. Mater. Chem.C,2021,9, 5469-5477). La reported by Liu such as xi et al 3 Ga 5 GeO 14 :Cr 3+ Although having ultra-wideband near-infrared emission of 650-1400nm and a half-peak width of 330nm, due to Cr 3+ Occupying different crystallographic lattice positions and having different luminescence thermal stability, finally causing the emission main peak of the phosphor to be blue-shifted from 950nm at room temperature to 830nm at 150 ℃, and the unstable emission spectrum brings challenges to practical application, as shown in fig. 1. Therefore, the research and development of novel long-wave near-infrared fluorescent powder with better thermal stability and capable of being excited by a blue light LED is an important subject faced by a fluorescent powder conversion type near-infrared LED luminescent material, and the development of related luminescent materials and luminescent devices has important significance for the development of near-infrared light sources.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides Cr 3+ Doped long-wave emitting near-infrared fluorescent powder and preparation method thereofA method and conversion type LED light emitting device. The preparation method is simple, easy to operate, low in equipment cost and free of pollution, and the fluorescent powder is stable in chemical performance, good in thermal stability and high in luminous efficiency and can be effectively excited by ultraviolet, blue light and red light LED chips.
The purpose of the invention is realized by at least one of the following technical solutions.
An oxide near-infrared luminescent material, which comprises an inorganic compound, wherein the chemical formula of the inorganic compound is A x B y C z O q D p ；
Wherein A is one or the combination of more than two of Mg, ca, sr, ba, lu, Y, gd or La elements;
b is one or the combination of more than two of Sc, in, ga, mg, zr, ti, hf, sn, lu, Y, gd or La elements;
c is one or the combination of more than two of Al, si or Ge elements;
o is oxygen element;
d is Cr element;
0.7≤x≤1.3,0.7≤y≤1.3,1≤Z≤3,5≤q≤7,0<p≤0.3。
preferably, x is 0.8, 0.9, 1.0, y is 0.85, 0.95, 1.0, Z is 1.8, 2.0, 2.5, q is 5.8, 6.0, 6.2, p is 0.01, 0.03, 0.08, 0.12, 0.15.
Preferably, the B at least contains Sc or In;
preferably, C is Al and Si, and z =2.
Preferably, the luminescent material and CaScAlSiO 6 Have the same crystal structure.
Preferably, the wavelength range of the near infrared light emitted by the luminescent material is 700-1300nm.
Preferably, the inorganic compound has the chemical formula of Cr 0.01 CaSc 0.84 Al 1.15 SiO 6 The emission wavelength range of the blue light excited by 460nm is 700-1300nm, the peak value is 930nm, and the half-peak width can reach 210nm; the luminescence intensity at 100 ℃ was 69% of that at room temperature.
Preferably, the luminescent material is one or a combination of two or more of single crystal, powder crystal, glass or ceramic.
The preparation method of the oxide near-infrared luminescent material comprises the following steps:
1) According to the general formula A x B y C z O q D p Weighing the raw materials according to the stoichiometric ratio, grinding and uniformly mixing to obtain a raw material mixture;
2) Calcining the mixture obtained in the step 1) at high temperature to obtain a sintered body;
3) Grinding the sintered body obtained in the step 2) into powder to obtain the oxide near-infrared luminescent material.
Preferably, in step 1), the raw material is a simple substance, an oxide, a halide, a sulfide, a carbonate, a borate, a sulfate, a phosphate or a nitrate of magnesium, calcium, strontium, barium, lutetium, yttrium, gadolinium, lanthanum, indium, scandium, gallium, aluminum, zirconium, titanium, hafnium, tin, germanium and chromium;
preferably, in the step 3), the grinding time is 3-60min.
Preferably, in the step 2), the high-temperature calcination is sintered in an oxidation, reduction, air and inert gas environment;
preferably, in the step 2), the calcining temperature is 1250-1550 ℃ and the calcining time is 3-48h.
A conversion type LED light-emitting device comprises a packaging substrate, an LED chip and the oxide near-infrared light-emitting material, wherein the light-emitting material can absorb light emitted by the LED chip and emit near-infrared light.
Preferably, the light-emitting wavelength of the LED chip is between 400 and 800 nm;
further preferably, the LED chip is an InGaN or GaN blue semiconductor chip.
Preferably, the conversion-type LED lighting device further includes a curing adhesive.
The preparation process of the LED light-emitting device comprises the following steps of fixing the near-infrared light-emitting material with broadband emission characteristics on an LED chip, and lighting the chip to obtain the near-infrared LED light-emitting device.
Compared with the prior art, the invention has the following advantages:
1) The near-infrared luminescent material has high luminescent efficiency (18 percent of absolute internal quantum efficiency), good thermal stability and wider excitation and emission range, wherein the excitation spectrum covers all visible light regions, can be used as a light conversion material of a near-ultraviolet-near-infrared LED chip, and is particularly well matched with a commercial most-efficient blue light chip.
2) The near-infrared luminescent material has an emission band in a range of 700-1300nm under the excitation of blue light, a main peak is about 930nm, the half-peak width can reach 210nm, and the red storm phenomenon does not exist, so that the performance of the near-infrared luminescent material is superior to that of most near-infrared fluorescent powder, and the near-infrared luminescent material can be applied to the fields of night vision monitoring, medical treatment, food analysis and the like.
3) The preparation method is simple, easy to operate, low in equipment cost, free of pollution and suitable for popularization and use; the method is expected to be widely applied to the fields of optical fiber communication, component analysis, biological imaging, solar cells, iris recognition, night vision illumination and the like.
4) The near-infrared luminescent material of the invention is prepared by Cr 3+ The ion doping is realized, so that more people are encouraged to explore Cr 3 + Doped near-infrared phosphor.
Drawings
FIG. 1 is comparative example 1Cr 0.12 La 3 Ga 4.88 GeO 14 Thermal stability test result graph of (1);
FIG. 2 is comparative example 1Cr 0.12 La 3 Ga 4.88 GeO 14 With example 2Cr 0.01 CaSc 0.84 Al 1.15 SiO 6 Comparing the absolute quantum efficiency test results;
FIG. 3 is a graph comparing XRD of near infrared fluorescent materials prepared in examples 1,8,12,14 and 16 with standard cards;
FIG. 4 shows the near infrared fluorescent material Cr prepared in example 1 0.03 CaSc 0.97 AlSiO 6 A fluorescence spectrum of (a);
FIG. 5 shows a near-infrared fluorescent material Cr prepared in example 2 0.01 CaSc 0.84 Al 1.15 SiO 6 Fluorescent thermal stability test pattern of (1);
FIG. 6 is a graph showing the thermal stability characteristics of the near infrared fluorescent materials prepared in examples 4,5,7,14 and 16;
FIG. 7 shows the near infrared fluorescent material Cr prepared in example 2 0.01 CaSc 0.84 Al 1.15 SiO 6 And packaging the obtained product on a 460nm blue chip to obtain an emission spectrum of the near-infrared LED light-emitting device.
Detailed Description
The present invention is specifically described below with reference to examples, but the embodiments and the scope of the present invention are not limited to the following examples.
Example 1
The chemical composition formula of the near-infrared phosphor of this example is Cr x CaSc 1-x AlSiO 6 Wherein x =0.03. Accurately weighing Li according to the stoichiometric ratio of each element in the chemical formula 2 CO 3 ,CaCO 3 ,Sc 2 O 3 ,Al 2 O 3 , SiO 2 ,Cr 2 O 3 And (3) putting the high-purity powder raw material into an agate mortar for grinding for about 30 minutes, so that the raw materials are fully and uniformly mixed. Transferring the mixed raw materials into an alumina crucible, adding a lid, and placing at 20% H 2 +80％N 2 Sintering the mixture for 8 hours at 1500 ℃ in an atmosphere high-temperature reaction furnace, naturally cooling the mixture, taking the mixture out, and grinding the mixture for about 10 minutes to obtain Cr 0.03 CaSc 0.97 AlSiO 6 The XRD and the fluorescence spectrum of the fluorescent powder are respectively shown in figures 3 and 4, and it can be known from figure 3 that the fluorescent powder is a single phase, and it can be known from figure 4 that the fluorescent powder can be perfectly matched with a 460nm blue light chip and emits near infrared light of 700-1300nm, the main emission peak is about 930nm, and the half-peak width can reach 210 nm.
Comparative example 1
La was synthesized according to the method of example 1 3 Ga 5 GeO 14 Near-infrared fluorescent powder La with crystal structure 3 Ga 4.88 GeO 14 0.12Cr, and the thermal stability thereof was measured as shown in FIG. 1: it can be seen from the graph that the luminous intensities at 100 ℃ and 150 ℃ are 57% and 36% at room temperature, respectively; the fluorescent powder is prepared under high temperatureThe emission peak is blue shifted from 950nm at room temperature to 830nm at 150 ℃ and its thermal stability is poor. La at room temperature 3 Ga 4.88 GeO 14 0.12Cr and Cr 0.01 CaSc 0.84 Al 1.15 SiO 6 The results of the quantum efficiency test under 460nm excitation are shown in FIG. 2, from which it can be seen that Cr 0.01 CaSc 0.84 Al 1.15 SiO 6 The quantum efficiency of (2) is higher.
Examples 2 to 20
The chemical composition formulas, calcination temperatures, times, and milling times of examples 2-20 are shown in Table 1; the preparation method refers to example 1.
A comparison of XRD of the near infrared fluorescent materials prepared in examples 1,8,12,14 and 16 with that of the standard card is shown in FIG. 3, from which it can be seen that the prepared phosphor is a single phase, and the phosphors obtained in other examples are also single phases;
example 2Cr produced 0.01 CaSc 0.84 Al 1.15 SiO 6 The fluorescence thermal stability test chart of (1) is shown in figure 5, and the stability of the fluorescent powder is good, wherein the luminous intensity at 100 ℃ and 150 ℃ is 69% and 44% respectively at room temperature;
the thermal stability of the near-infrared fluorescent materials prepared in examples 4,5,7,14 and 16 is shown in fig. 6, and it can be seen from the figure that the control of the chemical composition has a certain effect on the thermal stability of the fluorescent powder.
TABLE 1
In Table 1, X is the ratio of the luminous intensity at 100 ℃ to the luminous intensity at room temperature.
Example 21
A near-infrared LED light-emitting device. The near-infrared LED light-emitting device of the present invention was prepared as follows. The near infrared rayThe LED light-emitting device comprises a packaging substrate, an LED chip and fluorescent powder capable of effectively absorbing the light emitted by the LED chip and releasing near infrared light; wherein the near-infrared phosphor is the near-infrared phosphor of embodiment 20, and the chemical composition formula thereof is Cr 0.01 CaSc 0.84 Al 1.15 SiO 6 . The LED chip is a blue InGaN semiconductor chip, and the light-emitting peak wavelength of the LED chip is 460nm. And (3) uniformly dispersing the near-infrared fluorescent powder in the silica gel, covering the silica gel on the chip in a coating or dispensing manner, and welding a circuit to obtain the near-infrared LED light-emitting device.
The spectrogram of the near-infrared LED light-emitting device prepared in example 21 is shown in fig. 7, and it can be seen from the spectrogram that the device can be well excited by a 460nm chip and emits a strong near-infrared spectrum.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall fall within the protection scope of the present invention.
Claims (9)
1. An oxide near-infrared luminescent material, which is characterized by comprising an inorganic compound, wherein the chemical formula of the inorganic compound is Cr 0.01 CaSc 0.84 Al 1.15 SiO 6 、Cr 0.01 SrSc 0.99 AlSiO 6 Or Cr 0.01 CaSc 0.89 Al 1.1 SiO 6 。
2. The oxide near-infrared luminescent material as claimed in claim 1, wherein the luminescent material is CaScAlSiO 6 Have the same crystal structure.
3. The oxide near-infrared luminescent material as claimed in claim 1, wherein the inorganic compound has a chemical formula of Cr 0.01 CaSc 0.84 Al 1.15 SiO 6 Its emission wavelength range under excitation of 460nm blue lightThe circumference is 700-1300nm, the peak value is 930nm, and the half-peak width can reach 210nm; at 100 o The emission intensity at C was 69% of that at room temperature.
4. The oxide near-infrared luminescent material according to claim 1, wherein the luminescent material is one or a combination of two or more of a single crystal, a powder crystal, glass, or ceramic.
5. The method for preparing the oxide near-infrared luminescent material according to any one of claims 1 to 4, characterized by comprising the steps of:
1) Weighing raw materials according to the stoichiometric ratio of the chemical formula, and grinding and uniformly mixing to obtain a raw material mixture;
2) Calcining the mixture obtained in the step 1) at high temperature to obtain a sintered body;
3) Grinding the sintered body obtained in the step 2) into powder to obtain the oxide near-infrared luminescent material.
6. The method according to claim 5, wherein the raw material in step 1) is SiO 2 Elemental, oxide, halide, sulfide, carbonate, borate, sulfate, phosphate, or nitrate salts of calcium, strontium, scandium, aluminum, and chromium;
in the step 3), the grinding time is 3-60min.
7. The method according to claim 5, wherein in step 2), the high-temperature calcination is performed in an oxidizing, reducing, air, inert gas environment;
in the step 2), the calcining temperature is 1250-1550 ℃, and the calcining time is 3-48h.
8. A conversion-type LED light-emitting device comprising a package substrate, an LED chip, and the oxide near-infrared light-emitting material according to any one of claims 1 to 4, wherein the light-emitting material is capable of absorbing light emitted from the LED chip and emitting near-infrared light.
9. The converted LED lighting device according to claim 8, wherein the LED chip has a light emission wavelength between 400nm and 800 nm; the LED chip is an InGaN or GaN blue light semiconductor chip.
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