CN107118770B - Near-infrared fluorescent powder and preparation method thereof - Google Patents
Near-infrared fluorescent powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses near-infrared fluorescent powder, which has a chemical general formula as follows: ca3Ga1.95‑2xIn2xCr0.05Ge4O14Wherein x is more than or equal to 0 and less than or equal to 0.975. Also discloses a preparation method thereof: a) according to the chemical general formula Ca of the fluorescent powder3Ga1.95‑2xIn2xCr0.05Ge4O14Weighing oxides or carbonates containing Ca, Ga, In, Cr and Ge elements according to the molar ratio of the elements, mixing and grinding to obtain a mixture, wherein x is more than or equal to 0 and less than or equal to 0.975 In the chemical general formula; b) heating the mixture to 1100-1300 ℃ and roasting for 3-4h to obtain a sintered body; c) and cooling the obtained sintered body to room temperature, and fully grinding to obtain the near-infrared fluorescent powder. The near-infrared fluorescent powder prepared by the invention has the advantages of wide excitation wavelength range, high luminous intensity and high stability, and the adopted high-temperature solid-phase preparation method has the advantages of simple process, easy operation and control, high safety, short preparation time, high production efficiency and greatly reduced production cost compared with the prior art, and is suitable for industrial large-scale production and popularization and application.
Description
Technical Field
The invention relates to a luminescent material and a preparation method thereof, in particular to near-infrared fluorescent powder and a preparation method thereof.
Background
The near-infrared light region is a non-visible light region discovered earlier by people, and due to the fact that the early technical level is not high, spectrum overlapping and analysis are complex due to the influence of frequency doubling and frequency combination, and research and application of near-infrared light are limited to a certain extent. Until the 60 s in the 20 th century, the appearance of commercial instruments and a great deal of work done by Norris and other people put forward the theory that the content of substances and absorption peaks of a plurality of different wavelength points in a near infrared region are in a linear relationship, and the NIR diffuse reflection technology is utilized to measure components such as moisture, protein, fat and the like in agricultural products, so that the near infrared spectrum technology is widely applied to agricultural and sideline product analysis. In the middle and later period of the 60 s, with the appearance of various new analysis technologies and the weaknesses of low sensitivity and poor anti-interference performance exposed by the classical near infrared spectrum analysis technology, people are indifferent to the application of the technology in analysis and test, and then near infrared spectrum enters a silent period.
The successful application of multivariate calibration technology, an important component of Chemometrics (Chemometrics) disciplines generated in the 70 s, in spectral analysis promoted the popularization of near infrared spectroscopy. In the later 80 s, along with the rapid development of computer technology, the digitization of analytical instruments and the development of chemometrics are driven, good effects on the aspects of spectral information extraction and background interference are achieved through a chemometrics method, and the special characteristics of near infrared spectrum on a sample measuring technology are added, so that people know the value of the near infrared spectrum again, and the application research of the near infrared spectrum in various fields is continuously developed.
With the further development of near infrared technology, near infrared is extended to many medical fields such as pharmacology, molecular cell biology, diagnostics, and the like. Hospitals in the united states are trying to use a new instrument to help nurses find blood vessels on the arms of patients by detecting the location of blood vessels by means of near infrared rays harmless to the human body and projecting the distribution image of blood vessels on the arms in real time so as to let medical staff know where to put the needles, which may be free from suffering from "unnecessary needles". The near-infrared fluorescence mark emits light in a near-infrared region, biomolecules do not emit light in the near-infrared region and have no spectrum overlapping interference, and the near-infrared fluorescence mark can be excited by visible light with shorter wavelength, so that the excitation light dispersibility is avoided, and higher sensitivity is obtained. Besides, the near infrared light can be applied to biometric identification such as fingerprint identification, iris identification, face identification, etc., which is applied to the LED. A novel broadband infrared LED derived from an Oselan photoelectric semiconductor is applied to an infrared emitter by a fluorescent powder technology for the first time, and as a result, the LED capable of emitting broadband infrared light with a wavelength range of 650nm to 1050nm is successfully created, an infrared spectrum technology suitable for the consumer product market is created, and the LED is applied to the food industry, the agriculture and other industries to measure the moisture, fat, carbohydrate, sugar content or protein content in food. Therefore, research and development of the near-infrared fluorescent powder become the subject of active research of research and development personnel in the current industry, so as to provide more choices for the demands of the near-infrared material market.
Disclosure of Invention
The invention aims to provide a near-infrared fluorescent powder and a preparation method thereof, and provides more choices for the market demand of near-infrared materials.
The purpose of the invention is realized by the following technical scheme: a near-infrared fluorescent powder has a chemical general formula as follows: ca3Ga1.95-2xIn2xCr0.05Ge4O14Wherein x is more than or equal to 0 and less than or equal to 0.975.
Preferably, x is more than or equal to 0.1 and less than or equal to 0.975 in the chemical general formula; more preferably, x is more than or equal to 0.3 and less than or equal to 0.975 in the chemical general formula, and the luminous intensity of the near-infrared fluorescent powder in the preferred range is relatively strong; more preferably, x is more than or equal to 0.5 and less than or equal to 0.9 in the chemical general formula, and the luminous intensity of the near-infrared fluorescent powder in a more preferable range is relatively stronger; most preferably, the phosphor has the strongest emission intensity when x =0.7 in the chemical formula.
The invention also provides a preparation method of the near-infrared fluorescent powder, which comprises the following steps:
(a) according to the chemical general formula Ca of the fluorescent powder3Ga1.95-2xIn2xCr0.05Ge4O14Weighing oxides or carbonates containing Ca, Ga, In, Cr and Ge elements according to the molar ratio of the elements, mixing and grinding to obtain a mixture, wherein x is more than or equal to 0 and less than or equal to 0.975 In the chemical general formula;
(b) heating the mixture to 1100-1300 ℃ and roasting for 3-4h to obtain a sintered body;
(c) and cooling the obtained sintered body to room temperature, and fully grinding to obtain the near-infrared fluorescent powder.
The grinding time of the step (a) is 15-30 min.
The temperature rise rate in the step (b) is 5-10 ℃/min.
Heating to 1100-1300 ℃ for roasting for 4 h.
Heating to 1200 ℃ and roasting for 4 h.
In the preparation method of the near-infrared fluorescent powder provided by the invention, In the step (a), oxides or carbonates containing Ca, Ga, In, Cr and Ge elements are weighed, preferably CaCO3（A.R.）、Ga2O3（99.99%）、In2O3（A.R.）、Cr2O3(99.99%) and Ge2O3（A.R.）。
The invention utilizes Cr3+In Ca3Ga2Ge4O14And on the basis of medium doping, regulating and controlling cations Ga and In so as to obtain the near-infrared fluorescent powder with high-intensity emission In the wavelength range of 675-900 nm. The near-infrared fluorescent powder prepared by the invention has wide range of excitation wavelength, high luminous intensity and good stability, and the Cr adopted by the invention3+The ion-doped novel near-infrared fluorescent material is synthesized by changing the proportion of the matrix cations, and the adopted high-temperature solid-phase preparation method has the advantages of simple preparation process, easy operation and control, high safety, short preparation time, high production efficiency and greatly reduced production cost compared with the prior art, and is suitable for industrial large-scale production and popularization and application.
Drawings
FIG. 1 is a comparison of the standard pattern and XRD patterns of phosphors prepared in examples 2, 4, 5, and 6.
FIG. 2 shows excitation and emission spectra of the phosphor prepared in example 5.
FIG. 3 shows the luminous intensities of the phosphors prepared in examples 1 to 7 of the present invention.
Detailed Description
The following examples are intended to illustrate the present invention in further detail, but the present invention is not limited thereto in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated. But are not intended to limit the invention in any manner.
Example 1
(1) Weighing the following raw materials in parts by weight: separately weighing calcium carbonate (CaCO)3) 1.0009g gallium oxide (Ga)2O3) 0.6092g, chromium oxide (Cr)2O3) 0.0127g and germanium oxide (Ge)2O3) 1.3952g, mixing uniformly, and placing in an agate mortar for fully grinding for 30min to obtain a mixture;
(2) placing the ground mixture powder in a small crucible, heating to 1200 ℃ at a heating rate of 5 ℃/min, sintering for 4h at the temperature, and naturally cooling to room temperature to obtain a sintered body;
(3) cooling the obtained sintered body to room temperature, and grinding to obtain Ca3Ga1.95Cr0.05Ge4O14The near-infrared fluorescent powder.
The intensity and wavelength of the near-infrared phosphor prepared in this example were controlled at an emission wavelength of 745 nm.
Example 2
(1) Weighing the following raw materials in parts by weight: separately weighing calcium carbonate (CaCO)3) 1.0009g gallium oxide (Ga)2O3) 0.5467g indium oxide (In)2O3) 0.0925g of chromium oxide (Cr)2O3) 0.0127g and germanium oxide (Ge)2O3) 1.3952g, mixing uniformly, and placing in an agate mortar for fully grinding for 30min to obtain a mixture;
(2) placing the ground mixture powder in a small crucible, heating to 1200 ℃ at a heating rate of 5 ℃/min, sintering for 4h at the temperature, and naturally cooling to room temperature to obtain a sintered body;
(3) cooling the obtained sintered body to room temperature, and grinding to obtain Ca3Ga1.75In0.2Cr0.05Ge4O14The near-infrared fluorescent powder.
The phosphor prepared in this example began to exhibit a red-shift phenomenon and enhanced emission intensity, with the greatest degree of red-shift.
Example 3
(1) Weighing the following raw materials in parts by weight: separately weighing calcium carbonate (CaCO)3) 1.0009g gallium oxide (Ga)2O3) 0.4217g indium oxide (In)2O3) 0.2776g, chromium oxide (Cr)2O3) 0.0127g and germanium oxide (Ge)2O3) 1.3952g, mixing uniformly, and placing in an agate mortar for fully grinding for 30min to obtain a mixture;
(2) placing the ground mixture powder in a small crucible, heating to 1200 ℃ at a heating rate of 5 ℃/min, sintering for 4h at the temperature, and naturally cooling to room temperature to obtain a sintered body;
(3) cooling the obtained sintered body to room temperature, and grinding to obtain Ca3Ga1.35In0.6Cr0.05Ge4O14The near-infrared fluorescent powder.
The wavelength intensity of the near-infrared phosphor prepared in this example is continuously enhanced, and the wavelength is also red-shifted
Example 4
(1) Weighing the following raw materials in parts by weight: separately weighing calcium carbonate (CaCO)3) 1.0009g gallium oxide (Ga)2O3) 0.2968g indium oxide (In)2O3) 0.4627g, chromium oxide (Cr)2O3) 0.0127g and germanium oxide (Ge)2O3) 1.3952g, mixing uniformly, and placing in an agate mortar for fully grinding for 30min to obtain a mixture;
(2) placing the ground mixture powder in a small crucible, heating to 1200 ℃ at a heating rate of 5 ℃/min, sintering for 4h at the temperature, and naturally cooling to room temperature to obtain a sintered body;
(3) cooling the obtained sintered body to room temperature, and grinding to obtain Ca3Ga0.95InCr0.05Ge4O14The near-infrared fluorescent powder.
The wavelength intensity of the phosphor prepared in this example continues to increase, and the wavelength is also red-shifted.
Example 5
(1) Weighing the following components in parts by weightRaw materials: separately weighing calcium carbonate (CaCO)3) 1.0009g gallium oxide (Ga)2O3) 0.1718g indium oxide (In)2O3) 0.6478g, chromium oxide (Cr)2O3) 0.0127g and germanium oxide (Ge)2O3) 1.3952g, mixing uniformly, and placing in an agate mortar for fully grinding for 30min to obtain a mixture;
(2) placing the ground mixture powder in a small crucible, heating to 1200 ℃ at a heating rate of 5 ℃/min, sintering for 4h at the temperature, and naturally cooling to room temperature to obtain a sintered body;
(3) cooling the obtained sintered body to room temperature, and grinding to obtain Ca3Ga0.55In1.4Cr0.05Ge4O14The near-infrared fluorescent powder.
The phosphor prepared in this example has the strongest intensity, which is about the phosphor (Ca) prepared in example 13Ga1.95Cr0.05Ge4O14) The wavelength is also approximately in the maximum red-shift range to 778nm (only 2nm from the farthest wavelength) 17 times the light intensity. Because the substrate is prepared into the near-infrared fluorescent powder in a down-conversion luminescence mode, the luminous efficiency is higher than that of the up-conversion infrared fluorescent powder.
Example 6
(1) Weighing the following raw materials in parts by weight: separately weighing calcium carbonate (CaCO)3) 1.0009g gallium oxide (Ga)2O3) 0.0469g of indium oxide (In)2O3) 0.8329g, chromium oxide (Cr)2O3) 0.0127g and germanium oxide (Ge)2O3) 1.3952g, mixing uniformly, and placing in an agate mortar for fully grinding for 30min to obtain a mixture;
(2) placing the ground mixture powder in a small crucible, heating to 1200 ℃ at a heating rate of 5 ℃/min, sintering for 4h at the temperature, and naturally cooling to room temperature to obtain a sintered body;
(3) cooling the obtained sintered body to room temperature, and grinding to obtain Ca3Ga0.15In1.8Cr0.05Ge4O14The near-infrared fluorescent powder.
The light intensity of the phosphor prepared in this example is reduced, but a 2nm red shift still occurs, reaching the farthest wavelength.
Example 7
(1) Weighing the following raw materials in parts by weight: separately weighing calcium carbonate (CaCO)3) 1.0009g gallium oxide (Ga)2O3) 0g of indium oxide (In)2O3) 0.9023g, chromium oxide (Cr)2O3) 0.0127g and germanium oxide (Ge)2O3) 1.3952g, mixing uniformly, and placing in an agate mortar for fully grinding for 30min to obtain a mixture;
(2) placing the ground mixture powder in a small crucible, heating to 1200 ℃ at a heating rate of 5 ℃/min, sintering for 4h at the temperature, and naturally cooling to room temperature to obtain a sintered body;
(3) cooling the obtained sintered body to room temperature, and grinding to obtain Ca3In1.95Cr0.05Ge4O14The near-infrared fluorescent powder.
In the phosphor prepared In this example, the matrix is completely controlled from Ga to In, and the wavelength position is substantially unchanged but the intensity is reduced.
Example 8
(1) Weighing the following raw materials in parts by weight: separately weighing calcium carbonate (CaCO)3) 1.0009g gallium oxide (Ga)2O3) 0.1718g indium oxide (In)2O3) 0.6478g, chromium oxide (Cr)2O3) 0.0127g and germanium oxide (Ge)2O3) 1.3952g, mixing uniformly, and placing in an agate mortar for full grinding for 15min to obtain a mixture;
(2) placing the ground mixture powder in a small crucible, heating to 1100 ℃ at a heating rate of 10 ℃/min, sintering for 4h at the temperature, and naturally cooling to room temperature to obtain a sintered body;
(3) cooling the obtained sintered body to room temperature, and grinding to obtain Ca3Ga0.55In1.4Cr0.05Ge4O14The near-infrared fluorescent powder.
Example 9
(1) Weighing the following raw materials in parts by weight: separately weighing calcium carbonate (CaCO)3) 1.0009g gallium oxide (Ga)2O3) 0.1718g indium oxide (In)2O3) 0.6478g, chromium oxide (Cr)2O3) 0.0127g and germanium oxide (Ge)2O3) 1.3952g, mixing uniformly, and placing in an agate mortar for full grinding for 20min to obtain a mixture;
(2) placing the ground mixture powder into a small crucible, heating to 1300 ℃ at a heating rate of 8 ℃/min, sintering for 3h at the temperature, and naturally cooling to room temperature to obtain a sintered body;
(3) cooling the obtained sintered body to room temperature, and grinding to obtain Ca3Ga0.55In1.4Cr0.05Ge4O14The near-infrared fluorescent powder.
Example 10 the properties of the phosphors prepared in the examples were examined.
The experimental method comprises the following steps:
detection of the phosphors Ca prepared in examples 2, 4, 5 and 63Ga1.75In0.2Cr0.05Ge4O14（x=0.1）、Ca3Ga0.95InCr0.05Ge4O14（x=0.5）、Ca3Ga0.55In1.4Cr0.05Ge4O14(x = 0.7) and Ca3Ga0.15In1.8Cr0.05Ge4O14(X = 0.9) and the X-ray diffraction pattern of the standard sample, as shown in fig. 1.
Detection of Ca prepared in example 53Ga0.55In1.4Cr0.05Ge4O14The excitation and emission spectra are obtained as shown in FIG. 2, in which the excitation wavelength λ isex470nm, emission wavelength λem＝778nm。
Detection of the phosphors Ca prepared in examples 1 to 73Ga1.95Cr0.05Ge4O14（x=0）、Ca3Ga1.75In0.2Cr0.05Ge4O14（x=0.1）、Ca3Ga1.35In0.6Cr0.05Ge4O14（x=0.3）Ca3Ga0.95InCr0.05Ge4O14（x=0.5）、Ca3Ga0.55In1.4Cr0.05Ge4O14（x=0.7）、Ca3Ga0.15In1.8Cr0.05Ge4O14（x=0.9）、Ca3In1.95Cr0.05Ge4O14(x = 0.975) as shown in fig. 3; it can be seen from the graph that the near-infrared phosphors prepared in examples 3-7 have relatively strong luminous intensities; the near-infrared phosphors prepared in examples 4 to 6 have relatively higher luminous intensities; especially, the phosphor prepared in example 5 has the strongest luminous intensity.
Claims (8)
1. A near-infrared phosphor is characterized in that the chemical general formula is as follows: ca3Ga1.95-2xIn2xCr0.05Ge4O14Wherein x is more than or equal to 0.3 and less than or equal to 0.975.
2. The near-infrared phosphor of claim 1, wherein x is 0.5. ltoreq. x.ltoreq.0.9 in the chemical formula.
3. The near-infrared phosphor of claim 2, wherein x =0.7 in the chemical formula.
4. A preparation method of near-infrared fluorescent powder is characterized by comprising the following steps: (a) according to the chemical general formula Ca of the fluorescent powder3Ga1.95-2xIn2xCr0.05Ge4O14Weighing oxides or carbonates containing Ca, Ga, In, Cr and Ge elements according to the molar ratio of the elements, mixing and grinding to obtain a mixture, wherein x is more than or equal to 0.3 and less than or equal to 0.975 In the chemical general formula; (b) mixing the mixtureHeating to 1100-1300 ℃ and roasting for 3-4h to obtain a sintered body; and (c) cooling the obtained sintered body to room temperature, and fully grinding to obtain the near-infrared fluorescent powder.
5. The method of claim 4, wherein the grinding time in step (a) is 15-30 min.
6. The method of claim 4, wherein the temperature increase rate in step (b) is 5-10 ℃/min.
7. The method as claimed in claim 4, wherein the heating in step (b) is carried out at 1100 ℃ and 1300 ℃ for 4 h.
8. The method of claim 7, wherein the heating of step (b) is carried out to 1200 ℃ for 4 h.
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| US10808171B2 (en) | 2018-01-30 | 2020-10-20 | Lextar Electronics Corporation | Infrared emitting fluoride phosphor and infrared light emitting device |
| CN108531175B (en) * | 2018-06-01 | 2020-11-24 | 河北大学 | Near-infrared fluorescent powder and preparation method and application thereof |
| KR102391310B1 (en) * | 2018-08-23 | 2022-04-26 | 그리렘 어드밴스드 머티리얼스 캄파니 리미티드 | Near-infrared fluorescent powder and light-emitting device containing the fluorescent powder |
| CN111171811A (en) * | 2018-11-12 | 2020-05-19 | 厦门稀土材料研究所 | Near-infrared luminescent material, preparation method thereof and LED device thereof |
| EP3795655B1 (en) * | 2019-07-09 | 2022-11-23 | Grirem Advanced Materials Co., Ltd. | Red and near-infrared light-emitting material and light-emitting device |
| CN110444651B (en) * | 2019-07-09 | 2021-02-26 | 有研稀土新材料股份有限公司 | Optical device |
| KR102554970B1 (en) * | 2019-07-09 | 2023-07-11 | 그리렘 어드밴스드 머티리얼스 캄파니 리미티드 | Red light and near-infrared light emitting materials and light emitting devices |
| CN111647404A (en) * | 2020-07-25 | 2020-09-11 | 陕西师范大学 | Cr (chromium)3+Activated broadband near-infrared fluorescent powder and preparation method thereof |
| CN114672310A (en) * | 2020-12-24 | 2022-06-28 | 中国科学院宁波材料技术与工程研究所 | Pyrophosphate near-infrared fluorescent powder and preparation method and application thereof |
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