CN108467733B - Near-infrared fluorescent powder, preparation method thereof and light-emitting device containing fluorescent powder - Google Patents
Near-infrared fluorescent powder, preparation method thereof and light-emitting device containing fluorescent powder Download PDFInfo
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Abstract
The invention belongs to the technical field of fluorescent materials, and particularly relates to near-infrared fluorescent powder, and further discloses a preparation method of the near-infrared fluorescent powder and a light-emitting device containing the fluorescent powder. The near-infrared fluorescent powder comprises a composition formula AxRrQqZy: zD, the excitation wavelength of the compound is 200-700nm, and the emission main peak in the near infrared region is 700-1600nm broadband emission. The near-infrared fluorescent powder has wide excitation wavelength, can well absorb ultraviolet light, blue light and red light, and has stronger near-infrared luminescence compared with the near-infrared fluorescent powder of a Gd-free gallium germanate system.
Description
Technical Field
The invention belongs to the technical field of fluorescent materials, and particularly relates to near-infrared fluorescent powder, and further discloses a preparation method of the near-infrared fluorescent powder and a light-emitting device containing the fluorescent powder.
Background
With the rise and rapid development of the fields of modern internet of things, biometric identification and wearable devices, various sensors and image identification technologies become more important. Among these technologies, the infrared LED is an important auxiliary light source due to its wide application characteristics.
An infrared LED (light emitting diode) is a near-infrared light emitting device which converts electric energy into light energy, has a series of advantages of small volume, low power consumption, good directivity and the like, and is widely applied to systems such as remote control, remote measurement, optical isolation, optical switching, photoelectric control, target tracking and the like. The infrared LED can be applied to special required applications such as iris identification, face identification and the like by combining a sensing device and an identification technology; or the infrared LED technology is applied to the biosensor of the wearable device, so that the physiological state of the human body can be quantified, and the wearable device becomes a new tool for health management. Meanwhile, in view of the rapid increase of the permeability of smart phones, automobiles, monitoring systems and other infrared LEDs, the infrared LED technology is widely concerned.
Currently, infrared LEDs are mainly used in the fields of communications, security monitoring and sensors, and mainly used for infrared LEDs with wavelengths of 850nm and 940 nm. In addition, the short-wave infrared luminescent material (located at 1000-1400nm) penetrates into the human body to a deeper depth, so that the short-wave infrared luminescent material is a biological transparent window, and can be applied to the fields of deep biomedical imaging, night vision monitoring and the like. However, in some new applications, such as gas sensors or portable/integrated spectroscopy systems, long wavelength near infrared luminescent materials are required. Therefore, there is also a need to develop long-wavelength near-infrared luminescent materials excited by blue light, ultraviolet light or red light. For example, Chinese patent document CN103320126B discloses a class of matrix ZnZGaYGeXO(Z+1.5Y+2X)The wide band white light long afterglow material doped with 0-20mo 1% alkali metal or alkali earth metal element may be excited in the range of 200-350nm, and has light emitting range of 300-800nm and light emitting peak of 520 nm. Also disclosed in the prior art is a long afterglow up-conversion phosphor Zn3Ga2GeO8:Cr3+,Yb3+,Er3+The emission peak of the fluorescent powder is 700nm under the excitation of 980 nm.
The existing acquisition mode of near-infrared short-wave light mainly comprises an infrared chip, or an oxide of transition metal or rare earth metal of a halogen lamp subjected to light splitting or photoluminescence, or an electroluminescent organic complex. However, the existing near-infrared light-emitting device has the problems of low excitation efficiency, high cost and the like of the used infrared chip; the halogen lamp needs to be filtered, most of light is split, so that the use efficiency is low, and meanwhile, the heat generation quantity of the halogen lamp is large, so that the halogen lamp cannot be applied to small-sized equipment; the existing electroluminescent material device and the technology are not mature, and the problems of low luminous efficiency and poor stability of the infrared spectrum part exist, so that the development of the near-infrared short-wave light emitting device is seriously influenced.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to provide a near-infrared phosphor which can be excited by blue light, ultraviolet light, near-ultraviolet light or red light, and the problem of low luminous efficiency of the existing near-infrared luminescent material is solved;
the second technical problem to be solved by the present invention is to provide a light emitting device containing the near-infrared phosphor, which can realize high-efficiency near-infrared light emission under the excitation of blue light, ultraviolet light, near-ultraviolet light or red light, and solve the problem of low light emitting efficiency of the existing near-infrared light emitting device.
In order to solve the technical problem, the near-infrared phosphor comprises a composition formula AxRrQqZy: an inorganic compound of zD; wherein the content of the first and second substances,
the element A is Gd element, and one of La, Lu or Y element is selectively added;
the R element is Ga element and/or Al element;
the Q element is Ge element and/or Si element;
the element Z is O, and is selectively added with F;
the D element is one or two of Cr, Er, Yb, Ni, Nd, Zn, Li, Na or K;
and the parameters x, r, q, y and z satisfy the following conditions: x is more than or equal to 2 and less than or equal to 4, r is more than or equal to 3 and less than or equal to 7, q is more than or equal to 0.8 and less than or equal to 1.2, y is more than or equal to 11 and less than or equal to 17, and z is more than or equal to 0.0001 and less than or equal to 0.5.
Preferably, the inorganic compound has a structure similar to that of the compound La3Ga5GeO14The same crystal structure.
Preferably, the parameters x, r, q, y and z satisfy the following conditions: x is 3, r + z is 5, q is 1, and y is 14.
Specifically, the R element is a combination of Al element and Ga element, the Al element accounts for the mole percentage i of the R element, and i is more than or equal to 1% and less than or equal to 20%.
The element Z is the combination of an element O and an element F, the element F accounts for j in the molar percentage of the element Z, and j is more than or equal to 80% and less than or equal to 100%.
The D element is the combination of Cr element and Zn element.
The phosphor further includes a second inorganic compound selected from the group consisting of LiF, LiCl, NaF, KF, BaF2At least one of (1).
The invention also discloses a method for preparing the near-infrared fluorescent powder, which comprises the following steps:
(1) uniformly mixing oxides, carbonates or nitrates corresponding to selected A, R, Q, Z and D elements and a fluxing agent serving as raw materials according to a selected stoichiometric ratio to obtain a mixture;
(2) placing the mixture in a crucible, and sintering at the temperature of 1200-1500 ℃ in air or protective atmosphere for 2-10h to obtain a roasted product;
(3) and crushing, grinding, grading and screening the obtained roasted product to obtain the required near-infrared fluorescent powder.
The invention also discloses a light-emitting device which comprises a light source and a light-emitting material, wherein the light-emitting material comprises the near-infrared fluorescent powder.
Preferably, the light source is a semiconductor chip with an emission peak wavelength range of 200-750nm, and preferably a semiconductor chip with an emission wavelength of 200-500 nm.
More preferably, the light emitting device includes a semiconductor chip, a light conversion portion i and a light conversion portion ii, the light conversion portion i absorbs the primary light emitted by the semiconductor chip and converts the primary light into secondary light with a higher wavelength, the light conversion portion ii absorbs the primary light emitted by the semiconductor chip and the secondary light emitted by the light conversion portion i and converts the primary light and the secondary light into tertiary light with a higher wavelength, wherein the emission peak wavelength range of the semiconductor chip is 200-500nm, the light conversion portion i at least includes a light emitting material emitting light with a peak wavelength of 600-660nm, and the light conversion portion ii at least includes the near-infrared phosphor.
The light-emitting material contained in the light conversion part I is CaAlSiN3Or Sr2Si5N8Crystal modification ofAnd (5) structure.
The near-infrared fluorescent powder can realize more efficient near-infrared emission by substituting Gd element for La element in gallium germanate matrix, because Gd element in the matrix3+Excited state of ion and luminescence center Cr3+With crossing of the absorption bands, the formation of Gd from the matrix is achieved3+To luminescence center Cr3+Thereby achieving significant light efficiency enhancement. Therefore, the Gd-gallium-germanate-containing fluorescent powder in the matrix has strong broadband absorption peaks in the range of purple light, blue light and red light, and can obtain high-efficiency near-infrared light emission particularly under the excitation of blue light. Compared with the fluorescent powder with the gallium germanate component reported in the prior art, the near infrared emission performance of ultraviolet light and red light laser is stronger, and especially the near infrared emission performance under the excitation of blue light is more efficient.
Meanwhile, through experimental tests on water resistance and thermal stability, the performance of the fluorescent powder prepared by the invention is not obviously changed or reduced, which shows that the near-infrared fluorescent powder prepared by the invention has better water resistance and thermal stability and better product performance.
The near-infrared fluorescent powder can be used for preparing a light-emitting device, the light-emitting device can obtain near-infrared light under excitation of different blue light, ultraviolet light, near-ultraviolet light or red light, can avoid the defects of other infrared light obtaining modes, has the advantage of high light-emitting efficiency, can be applied to the fields of night vision monitoring, near-infrared short-band detection, medical treatment and the like, and can be applied to various types of equipment. In the light-emitting device, on the basis of matching with the near-infrared fluorescent powder, the light-emitting material emitting light with the peak wavelength of 600-660nm is simultaneously used, so that the light-emitting device has stronger near-infrared emission and unique application, and the application field of the light-emitting device is further widened.
Drawings
In order that the present disclosure may be more readily and clearly understood, the following detailed description of the present disclosure is provided in connection with specific embodiments thereof and the accompanying drawings, in which,
FIG. 1 is a graph showing an excitation spectrum at a monitoring wavelength of 750nm of a near-infrared phosphor sample prepared in example 1;
FIG. 2 is a graph showing the 460nm excitation emission spectrum of a near-infrared phosphor sample prepared in example 1;
FIG. 3 is a schematic view of a light-emitting device according to the present invention;
the reference numbers in the figures denote: 1-light conversion part I, 2-semiconductor chip, 3-pin, 4-heat sink, 5-base, 6-light conversion part II, 7-plastic lens.
Detailed Description
Example 1
The near-infrared phosphor of this embodiment comprises a compound having a formula of LaGd2Ga4.82GeO13.97：0.12Cr,0.06Zn。
According to the formula LaGd2Ga4.82GeO13.97: the stoichiometric ratio of 0.12Cr and 0.06Zn, and the La is accurately weighed2O3、Ga2O3、Gd2O3、GeO2And Cr2O3Mixing with ZnO to obtain a mixture; grinding and uniformly mixing the mixture, calcining at 1300 ℃ for 5h, and cooling to obtain a roasted product; and carrying out post-treatment such as crushing, grinding, grading, screening and washing on the obtained roasted product to obtain a near-infrared fluorescent powder sample.
The obtained near-infrared fluorescent powder sample is subjected to excitation test, and excitation and emission spectrograms of the obtained sample are shown in attached figures 1 and 2. The results in the figure show that the near-infrared phosphor sample can be effectively excited in the ranges of 200-.
Example 2
The near-infrared phosphor described in this embodiment contains a compound with a composition formula of La1.5Gd1.5Ga4GeO11：0.5Cr。
According to the formula La1.5Gd1.5Ga4GeO11: 0.5Cr, and accurately weighing La2O3、Gd2O3、Ga2O3、GeO2And Cr2O3Mixing to obtain a mixture; grinding and uniformly mixing the mixture, calcining at 1200 ℃ for 5h, and cooling to obtain a roasted product; and carrying out post-treatment such as crushing, grinding, grading, screening and washing on the obtained roasted product to obtain a near-infrared fluorescent powder sample.
And (3) carrying out excitation test on the obtained near-infrared fluorescent powder sample, wherein the result shows that the emission peak position of the near-infrared fluorescent powder sample is 780nm under the excitation of 460 nm.
Example 3
The near-infrared phosphor of this embodiment contains a compound having a composition formula of Gd3Ga4Al0.5GeO14：0.5Cr。
The preparation method of the near-infrared phosphor described in this example is the same as that of example 2, and the difference is that a compound with a proper amount is selected according to the chemical formula of the target compound, and the mixture is mixed, ground and calcined to obtain the desired near-infrared phosphor material.
Example 4
The near-infrared phosphor described in this embodiment contains a compound with a composition formula of La2.9Gd0.1Ga4.96GeO13.99：0.02Cr,0.02Zn。
The preparation method of the near-infrared phosphor described in this example is the same as that of example 2, and the difference is that a compound with a proper amount is selected according to the chemical formula of the target compound, and the mixture is mixed, ground and calcined to obtain the desired near-infrared phosphor material.
Example 5
The near-infrared phosphor described in this embodiment contains a compound with a composition formula of La2.9Gd0.1Ga4.88GeO13.99：0.1Cr,0.02Zn。
The preparation method of the near-infrared phosphor described in this example is the same as that of example 2, and the difference is that a compound with a proper amount is selected according to the chemical formula of the target compound, and the mixture is mixed, ground and calcined to obtain the desired near-infrared phosphor material.
Example 6
The near-infrared phosphor described in this embodiment contains a compound with a composition formula of La2.9Gd0.1Ga4.78GeO14.03：0.2Cr,0.06Zn。
The preparation method of the near-infrared phosphor described in this example is the same as that of example 2, and the difference is that a compound with a proper amount is selected according to the chemical formula of the target compound, and the mixture is mixed, ground and calcined to obtain the desired near-infrared phosphor material.
Example 7
The near-infrared phosphor of this embodiment comprises a compound having a formula of LaGd1.94Ga4.88GeO14：0.12Cr,0.06Nd。
The preparation method of the near-infrared phosphor described in this example is the same as that of example 2, and the difference is that a compound with a proper amount is selected according to the chemical formula of the target compound, and the mixture is mixed, ground and calcined to obtain the desired near-infrared phosphor material.
Example 8
The near-infrared phosphor described in this embodiment contains a compound with a composition formula of La0.5Gd2.44Ga4.88GeO14：0.12Cr,0.06Er。
The preparation method of the near-infrared phosphor described in this example is the same as that of example 2, and the difference is that a compound with a proper amount is selected according to the chemical formula of the target compound, and the mixture is mixed, ground and calcined to obtain the desired near-infrared phosphor material.
Example 9
The near-infrared phosphor described in this embodiment contains a compound with a composition formula of La0.2Gd2.78Ga4.82GeO13.96：0.12Cr,0.06Zn,0.02Li。
The preparation method of the near-infrared phosphor described in this example is the same as that of example 2, and the difference is that a compound with a proper amount is selected according to the chemical formula of the target compound, and the mixture is mixed, ground and calcined to obtain the desired near-infrared phosphor material.
Example 10
The near-infrared phosphor of this embodiment comprises a compound with a composition formula of Lu2.9Gd0.1Ga4.86GeO13.99：0.12Cr,0.02Zn。
The preparation method of the near-infrared phosphor described in this example is the same as that of example 2, and the difference is that a compound with a proper amount is selected according to the chemical formula of the target compound, and the mixture is mixed, ground and calcined to obtain the desired near-infrared phosphor material.
Example 11
The near-infrared phosphor of this embodiment contains a compound with a composition formula of Y2.9Gd0.1Ga4.82GeO13.97：0.12Cr,0.06Zn。
The preparation method of the near-infrared phosphor described in this example is the same as that of example 2, and the difference is that a compound with a proper amount is selected according to the chemical formula of the target compound, and the mixture is mixed, ground and calcined to obtain the desired near-infrared phosphor material.
Example 12
The near-infrared phosphor of this embodiment contains a compound having a composition formula of Gd3Ga4.82GeO13.97：0.12Cr,0.06Zn。
The preparation method of the near-infrared phosphor described in this example is the same as that of example 2, and the difference is that a compound with a proper amount is selected according to the chemical formula of the target compound, and the mixture is mixed, ground and calcined to obtain the desired near-infrared phosphor material.
Example 13
The near-infrared phosphor of this embodiment contains a compound having a composition formula of Gd3Al4.88GeO14：0.12Cr。
The preparation method of the near-infrared phosphor described in this example is the same as that of example 2, and the difference is that a compound with a proper amount is selected according to the chemical formula of the target compound, and the mixture is mixed, ground and calcined to obtain the desired near-infrared phosphor material.
Example 14
This implementationThe near-infrared fluorescent powder comprises a compound with the composition formula of Gd3Ga4.82SiO13.97：0.12Cr,0.06Zn。
The preparation method of the near-infrared phosphor described in this example is the same as that of example 2, and the difference is that a compound with a proper amount is selected according to the chemical formula of the target compound, and the mixture is mixed, ground and calcined to obtain the desired near-infrared phosphor material.
Example 15
The near-infrared phosphor of this embodiment contains a compound having a composition formula of Gd3Ga4.82Ge0.5Si0.5O13.97：0.12Cr,0.06Zn。
The preparation method of the near-infrared phosphor described in this example is the same as that of example 2, and the difference is that a compound with a proper amount is selected according to the chemical formula of the target compound, and the mixture is mixed, ground and calcined to obtain the desired near-infrared phosphor material.
Example 16
The near-infrared phosphor described in this embodiment contains a compound with a composition formula of La2Gd2Ga2.88Ge1.2O12.9：0.12Cr。
The preparation method of the near-infrared phosphor described in this example is the same as that of example 2, and the difference is that a compound with a proper amount is selected according to the chemical formula of the target compound, and the mixture is mixed, ground and calcined to obtain the desired near-infrared phosphor material.
Example 17
The near-infrared phosphor described in this embodiment contains a compound with a composition formula of La2Gd2Ga5.84GeO17：0.12Cr,0.06Zn。
The preparation method of the near-infrared phosphor described in this example is the same as that of example 2, and the difference is that a compound with a proper amount is selected according to the chemical formula of the target compound, and the mixture is mixed, ground and calcined to obtain the desired near-infrared phosphor material.
Example 18
This example illustratesThe near-infrared fluorescent powder contains a compound with the composition formula of La2.5Gd0.5Ga4.82GeO14：0.12Cr,0.06Yb。
The preparation method of the near-infrared phosphor described in this example is the same as that of example 2, and the difference is that a compound with a proper amount is selected according to the chemical formula of the target compound, and the mixture is mixed, ground and calcined to obtain the desired near-infrared phosphor material.
Comparative example 1
The near-infrared phosphor described in this embodiment contains a compound with a composition formula of La3Ga4.88GeO14：0.12Cr。
According to the formula La3Ga4.88GeO14:0.12Cr stoichiometric ratio, La was accurately weighed2O3、Gd2O3、Ga2O3、GeO2And Cr2O3And a flux NH4Grinding and uniformly mixing Cl to obtain a mixture; calcining the obtained mixture at 1300 ℃ for 5h, and cooling to obtain a calcined product; and (3) carrying out crushing, grinding, grading, screening and washing post-treatment on the obtained roasted product to obtain the required infrared fluorescent powder sample.
The near-infrared phosphors prepared in examples 1 to 18 and comparative example 1 were respectively subjected to an excitation test, and the peak wavelength and the relative luminous intensity under the excitation of 460nm wavelength were measured, and the results are shown in table 1 below.
TABLE 1 Peak wavelength and relative luminous intensity of near-infrared phosphor excited at 460nm wavelength
| Numbering | Molecular formula | Emission peak/nm | Relative luminous intensity% |
| Example 1 | LaGd2Ga4.82GeO13.97:0.12Cr,0.06Zn | 745 | 135 |
| Example 2 | La1.5Gd1.5Ga4GeO11:0.5Cr | 780 | 138 |
| Example 3 | Gd3Ga4Al0.5GeO14:0.5Cr | 740 | 143 |
| Example 4 | La2.9Gd0.1Ga4.96GeO13.99:0.02Cr,0.02Zn | 896 | 109 |
| Example 5 | La2.9Gd0.1Ga4.88GeO13.99:0.1Cr,0.02Zn | 896 | 118 |
| Example 6 | La2.9Gd0.1Ga4.78GeO14.03:0.2Cr,0.06Zn | 920 | 122 |
| Example 7 | LaGd1.94Ga4.88GeO14:0.12Cr,0.06Nd | 1066 | 143 |
| Example 8 | La0.5Gd2.44Ga4.88GeO14:0.12Cr,0.06Er | 1534 | 125 |
| Example 9 | La0.2Gd2.78Ga4.82GeO13.96:0.12Cr,0.06Zn,0.02Li | 770 | 142 |
| Example 10 | Lu2.9Gd0.1Ga4.86GeO13.99:0.12Cr,0.02Zn | 780 | 136 |
| Example 11 | Y2.9Gd0.1Ga4.82GeO13.97:0.12Cr,0.06Zn | 778 | 138 |
| Example 12 | Gd3Ga4.82GeO13.97:0.12Cr，0.06Zn | 758 | 152 |
| Example 13 | Gd3Al4.88GeO14:0.12Cr | 768 | 148 |
| Example 14 | Gd3Ga4.82SiO13.97:0.12Cr,0.06Zn | 760 | 134 |
| Example 15 | Gd3Ga4.82Ge0.5Si0.5O13.97:0.12Cr,0.06Zn | 756 | 140 |
| Example 16 | La2Gd2Ga2.88Ge1.2O12.9:0.12Cr | 780 | 135 |
| Example 17 | La2Gd2Ga5.84GeO17:0.12Cr,0.06Zn | 786 | 130 |
| Example 18 | La2.5Gd0.5Ga4.82GeO14:0.12Cr,0.06Yb | 980 | 160 |
| Comparative example 1 | La3Ga4.88GeO14:0.12Cr | 930 | 100 |
As can be seen from the data in the table above, the near-infrared fluorescent powder of the invention emits broadband emission with a main emission peak in a near-infrared region of 700-1600nm, has a wide excitation wavelength, can well absorb ultraviolet light, blue light and red light, and is relatively higher than that of La without Gd3Ga4.88GeO140.12Cr fluorescent powder, the near-infrared fluorescent powder has stronger near-infrared luminous performance.
The near-infrared phosphors prepared in the above examples 1 to 18 were respectively soaked in water, and an acid solution was simultaneously added for ball milling treatment. Through detection, the performance of the near-infrared fluorescent powder prepared by the invention is not obviously changed after the treatment, which shows that the fluorescent powder prepared by the invention has good water resistance.
The near-infrared phosphors prepared in the above examples 1 to 18 were respectively baked at a high temperature, and the performance of the phosphors was not significantly reduced by the detection, indicating that the phosphors prepared by the present invention have a very good thermal stability.
The following examples 19 to 24 are light emitting devices using the near-infrared phosphor of the present invention as a near-infrared light emitting material, that is, a structure of a light emitting device known in the prior art is taken as an example, the structure is shown in fig. 3, the light emitting device includes a base 5, and is provided with a heat sink 4 and a pin 3, a light source of the light emitting device is a semiconductor chip 2, an optical material portion of the light emitting device includes a light conversion portion i and a light conversion portion ii, and an outer layer thereof is provided with a plastic lens 7. The light conversion part I absorbs the primary light emitted by the semiconductor chip 2 and converts the primary light into secondary light with higher wavelength, and the light conversion part II absorbs the primary light emitted by the semiconductor chip 2 and the secondary light emitted by the light conversion part I and converts the primary light and the secondary light into tertiary light with higher wavelength.
The light-emitting devices described in examples 19 to 24 below were provided with the light-converting part II alone or with the light-converting parts I and II. Wherein, the light conversion part I at least comprises a luminescent material emitting light with the peak wavelength of 600-660nm, and the light conversion part II 6 at least comprises the near-infrared fluorescent powder.
The light emitting devices in examples 19 to 24 described below were compared with a light emitting device containing the fluorescent material in comparative example 1 as a light emitting material. The contrast light-emitting device takes a semiconductor chip with the peak wavelength of 460nm as a light source, only comprises a light conversion part II, the light conversion part II comprises the near-infrared fluorescent powder of the comparative example 1, the fluorescent powder absorbs blue light of the light source, the emission peak wavelength of 930nm near-infrared light is set, and the luminous efficiency of the fluorescent powder is set to be 100.
Example 19
The light emitting device of this embodiment uses a semiconductor chip with a peak wavelength of 640nm as a light source, and the light emitting device of this embodiment only contains the light conversion part ii, and the light conversion part ii contains the near-infrared phosphor of embodiment 1, and the phosphor absorbs red light of the light source and emits near-infrared light with a peak wavelength of 745 nm.
Through detection, the near-infrared luminous efficiency of the light-emitting device of the embodiment is improved by 50% compared with that of the contrast light-emitting device.
Example 20
The light emitting device of this embodiment uses a semiconductor chip with a peak wavelength of 460nm as a light source, and the light emitting device of this embodiment only contains a light conversion part ii, and the light conversion part ii contains the near-infrared phosphor of embodiment 1, and the near-infrared phosphor absorbs blue light of the light source and emits near-infrared light with a peak wavelength of 745 nm.
Through detection, the near-infrared luminous efficiency of the light-emitting device of the embodiment is improved by 35% compared with that of the contrast light-emitting device.
Example 21
The light emitting device structure described in this embodiment includes a semiconductor chip with a peak wavelength of 460nm, and a light conversion portion i and a light conversion portion ii, where the light conversion portion i absorbs blue primary light emitted from the semiconductor chip and converts the blue primary light into red secondary light with a higher wavelength, and the light conversion portion ii absorbs primary light emitted from the semiconductor chip and red secondary light emitted from the light conversion portion i and converts the red secondary light into near-infrared emitted tertiary light with a higher wavelength.
The light conversion part I contains Ca as a component0.04Sr0.95AlSiN30.01Eu luminescent material, which absorbs blue light emitted by a blue light chip and emits red light with the peak wavelength of 600nm, wherein the light conversion part II contains the near-infrared fluorescent powder of the embodiment 2, which absorbs the blue light of the blue light chip and the red light of the light conversion part II and efficiently emits the near-infrared light with the peak wavelength of 780 nm.
Through detection, the near-infrared luminous efficiency of the light-emitting device of the embodiment is improved by 70% compared with that of the contrast light-emitting device.
Example 22
The light emitting device structure described in this embodiment includes a semiconductor chip with a peak wavelength of 460nm, and a light conversion portion i and a light conversion portion ii, where the light conversion portion i absorbs blue primary light emitted from the semiconductor chip and converts the blue primary light into red secondary light with a higher wavelength, and the light conversion portion ii absorbs primary light emitted from the semiconductor chip and red secondary light emitted from the light conversion portion i and converts the red secondary light into near-infrared emitted tertiary light with a higher wavelength.
The light conversion part I contains Ca as a component0.4Sr0.5AlSiN 3: 0.01Eu, which absorbs blue light emitted by the blue chip and emits red light with a peak wavelength of 640nm, and the light conversion part II contains the near-infrared phosphor of the invention in the embodiment 3, which absorbs blue light of the blue chip and red light of the light conversion part II and efficiently emits near-infrared light with a peak wavelength of 740 nm.
Through detection, the near-infrared luminous efficiency of the light-emitting device of the embodiment is improved by 75% compared with that of the contrast light-emitting device.
Example 23
The light emitting device structure described in this embodiment includes a semiconductor chip with a peak wavelength of 460nm, and a light conversion portion i and a light conversion portion ii, where the light conversion portion i absorbs blue primary light emitted from the semiconductor chip and converts the blue primary light into red secondary light with a higher wavelength, and the light conversion portion ii absorbs primary light emitted from the semiconductor chip and red secondary light emitted from the light conversion portion i and converts the red secondary light into near-infrared emitted tertiary light with a higher wavelength.
The light conversion part I contains Ca as a component0.992AlSiN3: 0.008Eu luminescent material which absorbs blue light emitted by the blue light chip and emits red light with peak wavelength of 660nm, and the light conversion part II contains the near-infrared fluorescent powder of the embodiment 4 of the invention, which absorbs blue light of the blue light chip and red light of the light conversion part II and efficiently emits near-infrared light with peak wavelength of 896 nm.
Through detection, the near-infrared luminous efficiency of the light-emitting device of the embodiment is improved by 25% compared with that of the contrast light-emitting device.
Example 24
The light emitting device structure described in this embodiment includes a semiconductor chip with a peak wavelength of 460nm, and a light conversion portion i and a light conversion portion ii, where the light conversion portion i absorbs blue primary light emitted from the semiconductor chip and converts the blue primary light into red secondary light with a higher wavelength, and the light conversion portion ii absorbs primary light emitted from the semiconductor chip and red secondary light emitted from the light conversion portion i and converts the red secondary light into near-infrared emitted tertiary light with a higher wavelength.
The light conversion part I contains Sr as a component1.97Si5N8: 0.03Eu luminescent material, which absorbs blue light emitted by the blue light chip and emits red light with peak wavelength of 628nm, and the light conversion part II contains the near-infrared fluorescent powder of the embodiment 5, which absorbs blue light of the blue light chip and red light of the light conversion part II and efficiently emits near-infrared light with peak wavelength of 896 nm.
Through detection, the near-infrared luminous efficiency of the light-emitting device of the embodiment is improved by 65% compared with that of the contrast light-emitting device.
The results of measuring the luminous efficacy of the light-emitting devices obtained in the above examples 19 to 24 are shown in table 2 below.
Table 2 structural information and relative luminous efficacy of the light emitting device of the present invention
According to the data in the table, the light-emitting device prepared by the near-infrared fluorescent powder has higher light-emitting efficiency.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (8)
1. A near-infrared phosphor is characterized by comprising a composition formula A x R r Q q Z y : an inorganic compound of zD; wherein the content of the first and second substances,
the element A is Gd element, or the element A is Gd element and is added with one of La, Lu or Y element;
the R element is Ga element and/or Al element;
the Q element is Ge element and/or Si element;
the element Z is an element O;
the D element is Cr element, or the D element is Cr element and is added with one or two of Er, Yb, Nd, Zn, Li, Na or K element;
and saidx、r、q、yAndzthe following conditions are satisfied: 2 is less than or equal tox≤4，3≤r≤7，0.8≤q≤1.2，11≤y≤17，0.0001≤z≤0.5；
The inorganic compound has a structure similar to that of the compound La3Ga5GeO14The same crystal structure.
2. The near-infrared phosphor of claim 1, wherein the R element is a combination of Al element and Ga element, and the Al element accounts for i in the molar percentage of the R element, and i is 1% to 20%.
3. The near-infrared phosphor of claim 1 or 2, wherein the D element is a combination of Cr element and Zn element.
4. A method for preparing the near-infrared phosphor of any one of claims 1 to 3, comprising the steps of:
(1) uniformly mixing oxides, carbonates or nitrates corresponding to selected A, R, Q, Z and D elements and a fluxing agent serving as raw materials according to a selected stoichiometric ratio to obtain a mixture;
(2) placing the mixture in a crucible, and sintering at the temperature of 1200-1500 ℃ in air or protective atmosphere for 2-10h to obtain a roasted product;
(3) and crushing, grinding, grading and screening the obtained roasted product to obtain the required near-infrared fluorescent powder.
5. A light-emitting device comprising a light source and a luminescent material, wherein the luminescent material comprises the near-infrared phosphor of any one of claims 1 to 3.
6. The light-emitting device according to claim 5, wherein the light source is a semiconductor chip having an emission peak wavelength range of 200-500 nm.
7. The light-emitting device according to claim 5 or 6, wherein the light-emitting device comprises a semiconductor chip, a light-converting part I and a light-converting part II, the light-converting part I absorbs the primary light emitted by the semiconductor chip and converts the primary light into the secondary light with a higher wavelength, the light-converting part II absorbs the primary light emitted by the semiconductor chip and the secondary light emitted by the light-converting part I and converts the primary light and the secondary light into the tertiary light with a higher wavelength, wherein the emission peak wavelength range of the semiconductor chip is 200-500nm, the light-converting part I at least comprises a luminescent material emitting light with a peak wavelength of 600-660nm, and the light-converting part II at least comprises the near-infrared phosphor as set forth in any one of claims 1-3.
8. The light-emitting device according to claim 7, wherein the light-emitting material contained in the light-converting region I has CaAlSiN3Or Sr2Si5N8The crystal structure of (1).
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| US11898080B2 (en) | 2019-04-03 | 2024-02-13 | National Institute For Materials Science | Phosphor, method for producing same and light emitting element |
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| JP7231660B2 (en) * | 2019-07-09 | 2023-03-01 | 有研稀土新材料股▲フン▼有限公司 | Near-infrared light-emitting materials and light-emitting devices |
| CN112342021A (en) * | 2019-08-07 | 2021-02-09 | 厦门稀土材料研究所 | Near-infrared broadband emission luminescent material, preparation method thereof and luminescent device comprising material |
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| CN112011332B (en) * | 2020-09-11 | 2022-05-06 | 有研稀土新材料股份有限公司 | Far-red fluorescent powder and light-emitting device comprising same |
| CN114644923B (en) * | 2020-12-17 | 2023-06-02 | 中国科学院江西稀土研究院 | Near infrared luminescent material and preparation method and application thereof |
| WO2022137847A1 (en) * | 2020-12-24 | 2022-06-30 | 日亜化学工業株式会社 | Oxide phosphor, light emitting device, and method for producing oxide phosphor |
| CN117480231A (en) * | 2021-06-28 | 2024-01-30 | 松下知识产权经营株式会社 | Phosphor, light emitting device, light source for sensor system, and illumination system for sensor system |
| CN113652230A (en) * | 2021-07-15 | 2021-11-16 | 厦门大学 | Near-infrared luminescent material and luminescent device containing same |
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