CN114015445A - Garnet-structure near-infrared fluorescent material and preparation method and application thereof - Google Patents
Garnet-structure near-infrared fluorescent material and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of luminescent materials, and discloses a garnet-structured near-infrared fluorescent material, and a preparation method and application thereof. The chemical formula of the material is represented as: m3In2‑a‑ bScaCrbGa3O12(ii) a Wherein M is selected from La, Gd, Y or Lu; a is more than or equal to 0 and less than or equal to 1; b is more than or equal to 0.001 and less than or equal to 0.3. The excitation peak wavelength of the fluorescent material is located in a 445-470 nm waveband, the emission peak wavelength is located in a 720-810 nm waveband, the emission peak wavelength can be continuously changed, the luminous efficiency is high, and the requirements of development of near-infrared LED devices can be met.
Description
Technical Field
The invention belongs to the technical field of luminescent materials, and particularly relates to a garnet-structure near-infrared fluorescent material, and a preparation method and application thereof.
Background
In recent years, near-infrared technologies and devices have been widely used in industrial production, medical imaging, food inspection, optical fiber communication, security monitoring, and other production and living based on good absorption, scattering, and penetration of near-infrared light. For example, the near-infrared light with the wavelength of 700-1300 nm not only does not damage biological tissues, but also has good penetrability, the penetration depth can reach several centimeters, and the near-infrared light has very important application in the medical detection and imaging fields of blood oxygen, blood sugar, tissue images and the like; near-infrared light with the wavelength of 900-1100 nm can be well matched with the photoresponse of the silicon-based photovoltaic cell, and the application of the near-infrared fluorescent powder with the wavelength range in the silicon-based solar cell has wide application prospect in improving the photovoltaic conversion performance of the solar cell; in addition, the near infrared light is also widely applied to the fields of face recognition, AR/VR technology and the like. Compared with the traditional near-infrared light source, the near-infrared light emitting diode (pc-NIR-LED) based on fluorescence conversion has the advantages of high efficiency, stable spectrum, small volume, low cost, easiness in regulation and control and the like, and becomes a first-choice near-infrared light source device.
With the increasing market demand and scientific research value of near infrared technology, exploring and developing more efficient and practical near infrared fluorescent materials becomes a key link for the development thereof. Cr (chromium) component3+The activated near-infrared wide-spectrum fluorescent material is widely researched due to the advantages of wide absorption spectrum, high luminous efficiency, low cost and the like. However, the material still has some problems in the aspect of luminescence property, and the luminescence intensity, the thermal stability and the quantum efficiency of the material are greatly different due to different structures, so that the development and the application development of the near-infrared fluorescence conversion material are seriously restricted by the problems. Therefore, the exploration and development of stable and high-efficiency near-infrared broad-spectrum materials are urgent intrinsic requirements for the development of near-infrared fluorescence conversion LED devices, and have great significance. Among them, a fluorescent material of a garnet structure has good luminous intensity, thermal stability, and high quantum efficiency and is widely researched and developed.
Disclosure of Invention
In order to solve the limitations of the related researches, the primary object of the present invention is to provide a garnet-structured near-infrared fluorescent material. The excitation peak wavelength of the fluorescent material is located in a 445-470 nm waveband, the emission peak wavelength is located in a 720-810 nm waveband, the emission peak wavelength can be continuously changed, the luminous efficiency is high, and the requirements of development of near-infrared LED devices can be met.
The invention also aims to provide a preparation method of the garnet-structured near-infrared fluorescent material.
The invention also aims to provide application of the garnet-structure near-infrared fluorescent material.
The purpose of the invention is realized by the following scheme:
a garnet-structured near-infrared fluorescent material, the chemical formula of which is: m3In2-a- bScaCrbGa3O12(ii) a Wherein M is selected from La, Gd, Y or Lu; a is more than or equal to 0 and less than or equal to 1; b is more than or equal to 0.001 and less than or equal to 0.3.
The preparation method of the garnet-structure near-infrared fluorescent material comprises the following specific steps:
s1, grinding an M compound, an In compound, a Sc compound, a Ga compound and a Cr compound, and uniformly mixing to obtain a mixture A;
s2, sintering the mixture A in the air at 1500-1650 ℃, and crushing and grinding the product to obtain the garnet-structure near-infrared fluorescent material.
Preferably, in step S1, the M compound is lanthanum oxide, lanthanum nitrate, gadolinium oxide, gadolinium nitrate, yttrium oxide, yttrium nitrate, lutetium oxide, and lutetium nitrate.
Preferably, the In compound In step S1 is indium oxide or indium hydroxide.
Preferably, the Sc compound in step S1 is scandium oxide or scandium nitrate.
Preferably, the Ga compound in step S1 is gallium oxide.
Preferably, the Cr compound in step S1 is chromium oxide or chromium nitrate.
Preferably, the sintering time in the step S2 is 4-48 h.
The near-infrared fluorescent material is applied to a light conversion device.
Preferably, the light conversion device is a near-infrared LED device.
The invention uses optical active element Cr3+Is dissolved in M3In2Ga3O12In the (M ═ La, Gd, Y or Lu) crystalline phase, a high luminous efficiency can be obtained with an excitation peak wavelength of 445 to 470nm and an emission peak wavelength of 720 to 810nmThe novel material system. Belongs to a new structure and a new component compound and has potential application value. The invention relates to Cr3+Doping M alone3In2Ga3O12(M ═ La, Gd, Y or Lu), or on the basis thereof, a fluorescent material of a new composition formed by changing the In/Sc composition, and a mixture containing the above components as main components, are included In the scope of the present invention.
Compared with the prior art, the invention has the following beneficial effects:
1. the excitation peak wavelength of the garnet-structure near-infrared fluorescent material is 445-470 nm, so that the garnet-structure near-infrared fluorescent material is suitable for commercial blue-light LED chips, and has strong practicability;
2. under the excitation of 460nm blue light, the garnet-structure near-infrared fluorescent material efficiently emits near-infrared light with the peak wavelength of 720-810 nm, the emission spectrum covers 650-1050 nm, the quantum efficiency is above 71%, and the garnet-structure near-infrared fluorescent material can be used as fluorescent powder for a near-infrared LED for fluorescence conversion;
3. the garnet-structure near-infrared fluorescent material provided by the invention has the advantages of cheap and easily-obtained raw materials, low synthesis temperature, simple preparation process, no need of special reaction equipment and convenience in industrial production.
Drawings
FIG. 1 is Gd in example 13In1.82Cr0.18Ga3O12X-powder diffraction pattern of (a).
FIG. 2 is Gd in example 13In1.82Cr0.18Ga3O12Excitation spectrum of (1).
FIG. 3 is Gd in example 13In1.82Cr0.18Ga3O12The emission spectrum of (a).
FIG. 4 shows Y in example 23In1.92Cr0.08Ga3O12Excitation spectrum of (1).
FIG. 5 shows Y in example 23In1.92Cr0.08Ga3O12The emission spectrum of (a).
FIG. 6 shows Y in example 33In0.98ScCr0.02Ga3O12Excitation spectrum of (1).
FIG. 7 shows Y in example 33In0.98ScCr0.02Ga3O12The emission spectrum of (a).
FIG. 8 shows Lu in example 43In1.9Cr0.1Ga3O12Excitation spectrum of (1).
FIG. 9 shows Lu in example 43In1.9Cr0.1Ga3O12The emission spectrum of (a).
Detailed Description
The following examples are intended to illustrate the technical solutions of the present invention more clearly and completely, but are not intended to limit the present invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. The reagents, methods and apparatus used in the present patent are conventional in the art unless otherwise indicated.
Example 1
According to the chemical formula Gd of the phosphor3In1.82Cr0.18Ga3O12Weighing 0.15mol of Gd2O3、0.091molIn2O3、0.15molGa2O3、0.009molCr2O3The raw materials are analytically pure, and are mixed and fully ground, and after being uniformly mixed, the mixture is put into an alumina crucible for roasting, and the roasting temperature is 1500 ℃ and the temperature is kept for 20 hours. Cooling to room temperature, crushing, grinding, washing and drying the product to obtain Gd with the chemical composition3In1.82Cr0.18Ga3O12The phosphor of (1), wherein the X-powder diffraction pattern (Cu target, λ. cndot. 0.15406nm) is represented by the formula3In2Ga3O12The standard card pair is shown in FIG. 1. As can be seen from FIG. 1, Gd was successfully produced in this example3In1.82Cr0.18Ga3O12. FIG. 2 is Gd in this example3In1.82Cr0.18Ga3O12As is clear from FIG. 2, the fluorescenceThe light powder can be effectively excited by blue light and red light within the range of 400-800 nm, and the main excitation peak is positioned at 470 nm. FIG. 3 is Gd in this example3In1.82Cr0.18Ga3O12As can be seen from FIG. 3, the emission spectrum of (A) is 650 to 1050nm, and the main emission peak is 780 nm. The quantum efficiency was 87% under excitation by 460nm blue light (see table 1).
Example 2
According to the chemical formula Y of the phosphor3In1.92Cr0.08Ga3O12Weighing 0.15molY2O3、0.096molIn2O3、0.15molGa2O3、0.004molCr2O3The raw materials are analytically pure, and are mixed and fully ground, and after being uniformly mixed, the mixture is put into an alumina crucible for roasting, and the roasting temperature is 1550 ℃ and the temperature is kept for 14 hours. Cooling to room temperature, crushing, grinding, washing and drying the product to obtain Y3In1.92Cr0.08Ga3O12The fluorescent powder of (1). FIG. 4 shows Y in this embodiment3In1.92Cr0.08Ga3O12As can be seen from FIG. 4, the phosphor can be effectively excited by blue light and red light within the range of 400-800 nm, and the main excitation peak is at 453 nm; FIG. 5 shows Y in this embodiment3In1.92Cr0.08Ga3O12As can be seen from FIG. 5, the emission spectrum of (A) is 650 to 1050nm, and the main emission peak is 740 nm. The quantum efficiency was 85% under excitation by 460nm blue light (see table 1).
Example 3
According to the chemical formula Y of the phosphor3In0.98ScCr0.02Ga3O12Weighing 0.15molY2O3、0.049molIn2O3、0.05molSc2O3、0.15molGa2O3、0.001molCr2O3The raw materials are analytically pure, and are mixed and fully ground, and after being uniformly mixed, the mixture is put into an alumina crucible for roasting, and the roasting temperature is 1650 ℃ and the temperature is kept for 48 hours. After cooling to room temperature, the mixture is cooledCrushing, grinding, washing and drying the product to obtain the product with the chemical composition of Y3In0.98ScCr0.02Ga3O12The fluorescent powder of (1). FIG. 6 shows Y in this embodiment3In0.98ScCr0.02Ga3O12As can be seen from FIG. 6, the phosphor can be effectively excited by blue light and red light within the range of 400-800 nm, and the main excitation peak is at 455 nm; FIG. 7 shows Y in this example3In0.98ScCr0.02Ga3O12As can be seen from FIG. 7, the emission spectrum of (A) is 650 to 1050nm, and the main emission peak is at 748 nm. The quantum efficiency was 81% under excitation by 460nm blue light (see table 1).
Example 4
According to the chemical formula Lu of the phosphor3In1.9Cr0.1Ga3O12Weighing 0.15mol Lu2O3、0.095molIn2O3、0.15molGa2O3、0.005molCr2O3The raw materials are analytically pure, and are mixed and fully ground, and after being uniformly mixed, the mixture is put into an alumina crucible for roasting, and the roasting temperature is 1550 ℃ and the temperature is kept for 4 hours. After the product is cooled to room temperature, the product is crushed, ground, washed and dried to obtain the Lu with the chemical composition3In1.9Cr0.1Ga3O12The fluorescent powder of (1). FIG. 8 shows Lu in example 43In1.9Cr0.1Ga3O12Excitation spectrum of (1). As can be seen from FIG. 8, the phosphor can be effectively excited by blue light and red light within the range of 400-800 nm, and the main excitation peak is located at 445 nm; FIG. 9 shows Lu in example 43In1.9Cr0.1Ga3O12The emission spectrum of (a). As can be seen from FIG. 9, under the excitation of 460nm blue light, the emission spectrum covers 650-1050 nm, the emission main peak is at 720nm, and the quantum efficiency is 95% (see Table 1).
Example 5
According to the chemical formula Lu of the phosphor2GdIn1.9Cr0.1Ga3O120.2molLu (NO) was weighed3)3、0.05molGd2O3、0.095molIn2O3、0.15molGa2O3、0.005molCr2O3The raw materials are analytically pure, and are mixed and fully ground, and after being uniformly mixed, the mixture is put into an alumina crucible for roasting, and the roasting temperature is 1500 ℃ and the temperature is kept for 10 hours. After the product is cooled to room temperature, the product is crushed, ground, washed and dried to obtain the Lu with the chemical composition2GdIn1.9Cr0.1Ga3O12The fluorescent powder of (1). The fluorescent powder can be effectively excited by blue light and red light within the range of 400-800 nm, and the main excitation peak is at 453 nm; under the excitation of 460nm blue light, the emission spectrum covers 650-1050 nm, the emission main peak is 760nm, and the quantum efficiency is 92% (see table 1).
Example 6
According to the chemical formula La of the phosphor3In1.94Cr0.06Ga3O12Weighing 0.15mol of La2O3、0.097molIn2O3、0.15molGa2O3、0.06molCr(NO3)3The raw materials are analytically pure, and are mixed and fully ground, and after being uniformly mixed, the mixture is put into an alumina crucible for roasting, and the roasting temperature is 1600 ℃ and the temperature is kept for 30 hours. Cooling to room temperature, crushing, grinding, washing and drying the product to obtain the product with the chemical composition of La3In1.94Cr0.06Ga3O12The fluorescent powder of (1). The fluorescent powder can be effectively excited by blue light and red light within the range of 400-800 nm, and the main excitation peak is positioned at 455 nm; under the excitation of 460nm blue light, the emission spectrum covers 650-1050 nm, the emission main peak is located at 801nm, and the quantum efficiency is 79% (see table 1).
Example 7
The phosphor prepared according to the method of example 6 has the formula: la3In1.7Sc0.25Cr0.05Ga3O12The emission peak wavelength and quantum efficiency of the obtained phosphor are shown in table 1.
Example 8
The phosphor prepared according to the method of example 6 has the formula: la3In0.9999ScCr0.001Ga3O12The emission peak wavelength and quantum efficiency of the obtained phosphor are shown in table 1.
Example 9
The phosphor prepared according to the method of example 6 has the formula: gd (Gd)3In1.42Sc0.5Cr0.08Ga3O12The emission peak wavelength and quantum efficiency of the obtained phosphor are shown in table 1.
Example 10
The phosphor prepared according to the method of example 6 has the formula: gd (Gd)3In0.7ScCr0.3Ga3O12The emission peak wavelength and quantum efficiency of the obtained phosphor are shown in table 1.
Example 11
The phosphor prepared according to the method of example 6 has the formula: lu (Lu)3In0.85ScCr0.15Ga3O12The emission peak wavelength and quantum efficiency of the obtained phosphor are shown in table 1.
Example 12
The phosphor prepared according to the method of example 6 has the formula: lu (Lu)3In0.94Sc0.25Cr0.06Ga3O12The emission peak wavelength and quantum efficiency of the obtained phosphor are shown in table 1.
TABLE 1 emission peak position and quantum efficiency of the phosphors of examples 1-12 under 460nm blue excitation
The above-mentioned embodiments are only preferred embodiments of the present invention and are only used for illustrating the technical solutions of the present invention, but the embodiments of the present invention are not limited by the above-mentioned embodiments, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be regarded as equivalent replacements within the protection scope of the present invention.
Claims (10)
1. A garnet-structured near-infrared fluorescent material, characterized in that the chemical formula of the material is as follows: m3In2-a- bScaCrbGa3O12(ii) a Wherein M is selected from La, Gd, Y or Lu; a is more than or equal to 0 and less than or equal to 1; b is more than or equal to 0.001 and less than or equal to 0.3.
2. The preparation method of the garnet-structure near-infrared fluorescent material according to claim 1, comprising the following steps:
s1, grinding an M compound, an In compound, a Sc compound, a Ga compound and a Cr compound, and uniformly mixing to obtain a mixture A;
s2, sintering the mixture A in the air at 1500-1650 ℃, and crushing and grinding the product to obtain the garnet-structure near-infrared fluorescent material.
3. The method of claim 2, wherein the M compound in step S1 is lanthanum oxide, lanthanum nitrate, gadolinium oxide, gadolinium nitrate, yttrium oxide, yttrium nitrate, lutetium oxide, or lutetium nitrate.
4. The method of claim 2, wherein the In compound is indium oxide or indium hydroxide In step S1.
5. The method of claim 2, wherein the Sc compound is scandium oxide or scandium nitrate in step S1.
6. The method of claim 2, wherein the Ga compound is gallium oxide in step S1.
7. The method of claim 2, wherein the Cr compound is chromium oxide or chromium nitrate in step S1.
8. The method for preparing a garnet-structure near-infrared fluorescent material as set forth in claim 2, wherein the sintering time in step S2 is 4-48 hours.
9. Use of the near-infrared fluorescent material according to claim 1 in a light conversion device.
10. Use according to claim 9, wherein the light conversion device is a near-infrared LED device.
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| CN115287068A (en) * | 2022-08-30 | 2022-11-04 | 广东省科学院资源利用与稀土开发研究所 | Sodium yttrium gallium germanium garnet-based near-infrared light fluorescent powder and preparation method thereof |
| CN117363355A (en) * | 2023-09-27 | 2024-01-09 | 广东省科学院资源利用与稀土开发研究所 | Calcium europium gallium germanium garnet-based deep red fluorescent powder and preparation method thereof |
| CN115872445B (en) * | 2022-12-16 | 2024-04-19 | 广东工业大学 | Garnet type luminescent material and preparation method and application thereof |
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| CN115872445B (en) * | 2022-12-16 | 2024-04-19 | 广东工业大学 | Garnet type luminescent material and preparation method and application thereof |
| CN117363355A (en) * | 2023-09-27 | 2024-01-09 | 广东省科学院资源利用与稀土开发研究所 | Calcium europium gallium germanium garnet-based deep red fluorescent powder and preparation method thereof |
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