CN108531175B - Near-infrared fluorescent powder and preparation method and application thereof - Google Patents
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Abstract
The invention discloses near-infrared fluorescent powder, which has a chemical general formula as follows: mg (magnesium)3‑xGa2CrxGeO8Wherein x is more than 0 and less than or equal to 0.1, and discloses a preparation method of the near-infrared fluorescent powder, which comprises the following steps: according to the chemical general formula Mg of the fluorescent powder3‑xGa2CrxGeO8Weighing oxides or carbonates containing Mg, Ga, Cr and Ge elements according to the molar ratio of the elements, mixing and grinding to obtain a mixture; heating the mixture to 1200-1300 ℃ and roasting for 3-4h to obtain a sintered body; and cooling the obtained sintered body to room temperature, and fully grinding to obtain the near-infrared fluorescent powder. Also discloses the application of the near-infrared fluorescent powder. The near-infrared fluorescent powder provided by the invention has longer excitation wavelength, is not easy to be absorbed by organisms, has wide spectrum emission, high luminous intensity and high stability, can cover a part of a first window and a second window of a biological window of a body by covering the wavelength of 700-1200nm, has simple preparation process, is easy to operate and control, has high safety and short preparation time, and is convenient for large-scale production, popularization and application.
Description
Technical Field
The invention relates to a luminescent material, a preparation method and application thereof, in particular to near-infrared fluorescent powder, and a preparation method and application 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 relation, 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 the analysis of agricultural and sideline products. 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 gradually neglect the application of the technology in analysis and test, and then the 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 development of near infrared technology, near infrared is extended to many medical fields: 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 biological recognition, such as fingerprint recognition, iris recognition, face recognition, and the like, and can also be applied to the LED. For example, a new broadband infrared LED derived from an Oselan photoelectric semiconductor firstly applies a fluorescent powder technology to an infrared emitter, develops an infrared spectrum technology suitable for the consumer product market, and is applied to the food industry, the agriculture and other industries to measure the moisture, fat, carbohydrate, sugar content or protein content and the like in food; however, the technology relies on near-infrared fluorescent powder capable of emitting a wide spectrum, and most of the existing near-infrared fluorescent powder cannot meet the use requirements, so research and development personnel in the industry need to research and develop more near-infrared fluorescent powder with wide emission spectrum, more material choices are provided for the near-infrared fluorescent powder required by the Osram lamp bead, and more choices are provided for the near-infrared fluorescent powder used in food detection, biological detection and organism imaging.
Disclosure of Invention
The invention aims to provide near-infrared fluorescent powder, a preparation method and application thereof, so as to provide a near-infrared luminescent material with wide emission spectrum and good luminous intensity, and provide more material choices for the near-infrared fluorescent powder which needs to use the wide emission spectrum, such as Oselta lamp beads, biological monitoring and the like.
The purpose of the invention is realized by the following technical scheme: a near-infrared phosphor has a chemical formula: mg (magnesium)3-xGa2CrxGeO8Wherein x is more than 0 and less than or equal to 0.1.
Preferably, x is more than or equal to 0.01 and less than or equal to 0.01 in the chemical general formula; more preferably, x is 0.01 ≦ x ≦ 0.07 in the chemical formula; the near infrared phosphor in the more preferred range has a relatively stronger luminous intensity.
Most preferably, the phosphor has the strongest emission intensity when x =0.03 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 Mg of the fluorescent powder3-xGa2CrxGeO8Weighing oxides or carbonates containing Mg, Ga, Cr and Ge elements according to the molar ratio of the elements, mixing and grinding to obtain a mixture; x is more than 0 and less than or equal to 0.1 in the chemical general formula;
(b) heating the mixture to 1200-1300 ℃ 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.
In step (a), it is preferred that 0.01. ltoreq. x.ltoreq.0.01 in the general chemical formula; more preferably, x is 0.03 ≦ x ≦ 0.07 in the chemical formula; the luminous intensity of the prepared near-infrared fluorescent powder in a more preferable range is relatively stronger; most preferably, the phosphor prepared has the strongest luminous intensity when x =0.03 in the chemical formula.
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 1200 ℃ and 1300 ℃ for roasting for 4 h.
The fluorescent powder provided by the invention can be applied to preparation of Oselta lamp beads and also can be applied to food detection, biological detection and organism imaging because the fluorescent powder has an emission spectrum of 700-1200nm by detection.
The invention utilizes Cr3+Doped in Mg3Ga2GeO8In the method, positive ion Mg is regulated and controlled, so that the near-infrared fluorescent powder with high-intensity emission in the wavelength range of 700nm-1200nm is obtained. The invention has the creativity that: the near-infrared fluorescent powder has longer excitation wavelength and is less prone to be absorbed by organisms, the emission spectrum is broad spectrum emission, the wavelength covers 700-1200nm, the first window and the second window of a body biological window can be covered, the luminous intensity is high, the stability is high, the near-infrared fluorescent powder is applied to the Oselta lamp beads, and the near-infrared fluorescent powder can be well applied to biological detection, organism imaging and food detection. Further, the present invention adoptsThe high-temperature solid phase preparation method has the advantages of simple preparation process, easy operation and control, high safety, short preparation time and convenient large-scale production, popularization and application.
Drawings
FIG. 1 is a comparison of XRD patterns and standard patterns of phosphors prepared in examples 2, 4, 5, and 6.
FIG. 2 shows excitation and emission spectra of the phosphor prepared in example 3.
FIG. 3 shows the luminous intensities of the phosphors prepared in examples 1 to 5 of the present invention.
FIG. 4 shows the excitation spectra of the phosphors prepared in examples 1-5 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: 0.8047g of magnesium oxide (MgO) and Ga oxide (Ga) were weighed out respectively2O3) 1.2496g, chromium oxide (Cr)2O3) 0.0025g and germanium oxide (Ge)2O3) 0.6976g, 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 1260 ℃ 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 fully grinding to obtain the sintered body with the chemical formula of Mg2.995Ga2Cr0.005GeO8The near-infrared fluorescent powder.
Example 2
(1) Weighing the following raw materials in parts by weight: weighing magnesium oxide (MgO) 0.8033g and gallium oxide (Ga) respectively2O3) 1.2496g, chromium oxide (Cr)2O3) 0.0051G and germanium oxide (G)e2O3) 0.6976g, 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 1260 ℃ 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 fully grinding to obtain the sintered body with the chemical formula of Mg2.99Ga2Cr0.01GeO8The near-infrared fluorescent powder.
Example 3
(1) Weighing the following raw materials in parts by weight: 0.7979g of magnesium oxide (MgO) and Ga oxide (Ga) were weighed out respectively2O3) 1.2496g, chromium oxide (Cr)2O3) 0.0152g and germanium oxide (Ge)2O3) 0.6976g, 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 1260 ℃ 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 fully grinding to obtain the sintered body with the chemical formula of Mg2.97Ga2Cr0.03GeO8The near-infrared fluorescent powder.
Example 4
(1) Weighing the following raw materials in parts by weight: 0.7926g of magnesium oxide (MgO) and Ga oxide (Ga) were weighed out respectively2O3) 1.2496g, chromium oxide (Cr)2O3) 0.0253g and germanium oxide (Ge)2O3) 0.6976g, 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 1260 ℃ 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 fully grinding to obtain the sintered body with the chemical formula of Mg2.95Ga2Cr0.05GeO8The near-infrared fluorescent powder.
Example 5
(1) Weighing the following raw materials in parts by weight: respectively weighing 0.7872g of magnesium oxide (MgO), 1.2496g of gallium oxide (Ga 2O 3), 0.0355g of chromium trioxide (Cr 2O 3) and 0.6976g of germanium oxide (Ge 2O 3), uniformly mixing, and fully grinding in an agate mortar for 30min to obtain a mixture;
(2) placing the ground mixture powder in a small crucible, heating to 1260 ℃ 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 fully grinding to obtain the sintered body with the chemical formula of Mg2.93Ga2Cr0.07GeO8The near-infrared fluorescent powder.
Example 6
(1) Weighing the following raw materials in parts by weight: 0.7791g of magnesium oxide (MgO) and Ga oxide (Ga) were weighed out respectively2O3) 1.2496g, chromium oxide (Cr)2O3) 0.0507g and germanium oxide (Ge)2O3) 0.6976g, 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 1260 ℃ 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 fully grinding to obtain the sintered body with the chemical formula of Mg2.9Ga2Cr0.1GeO8The near-infrared fluorescent powder.
Example 7 detection of optical properties of the phosphors prepared in the examples.
The experimental method comprises the following steps:
1. detection of Mg in the phosphors prepared in examples 2, 3, 4 and 62.99Ga2Cr0.01GeO8、Mg2.97Ga2Cr0.03GeO8、Mg2.93Ga2Cr0.07GeO8、Mg2.9Ga2Cr0.1GeO8And an X-ray diffraction pattern of the standard sample, as shown in fig. 1.
2. Detection of Mg prepared in example 32.97Ga2Cr0.03GeO8The emission spectrum is obtained as shown in FIG. 2, in which the excitation wavelength λ isex＝600nm。
3. Detection of Mg in the phosphors prepared in examples 1 to 52.995Ga2Cr0.005GeO8、Mg2.99Ga2Cr0.01GeO8、Mg2.97Ga2Cr0.03GeO8、Mg2.95Ga2Cr0.05GeO8、Mg2.93Ga2Cr0.07GeO8The result of the emission intensity of (2) is shown in FIG. 3. The figure shows that: when x =0.005, the red shift phenomenon starts to occur and the emission intensity increases; when x =0.01, the first emission peak continues to be enhanced to the maximum, the second emission peak still has enhanced intensity, and the wavelength is also red-shifted; when x =0.03, the first emission peak begins to decrease in intensity and the second emission peak continues to increase in intensity, but the wavelength continues to be red-shifted; when x =0.05, the intensity of the first emission peak continues to decrease, the intensity of the second emission peak continues to increase, but the wavelength is still red-shifted; when x =0.07, the intensity of the first emission peak continues to decrease and the intensity of the second emission peak continues to increase, when the wavelength reaches the maximum red-shift position, the emission peak position is red-shifted from 720nm to 780 nm. It can be seen from the figure that the intensity of the first emission peak reaches the strongest at x =0.03 and the emission peak position is red-shifted from the first 720nm to 780 nm.
4. The excitation spectra of the phosphors prepared in examples 1-5 were examined.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above 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 construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. AThe near-infrared fluorescent powder is characterized in that the chemical general formula of the fluorescent powder is as follows: mg (magnesium)3-xGa2CrxGeO8Wherein x is more than 0 and less than or equal to 0.1;
the preparation method of the near-infrared fluorescent powder comprises the following steps:
(a) according to the chemical general formula Mg of the fluorescent powder3-xGa2CrxGeO8Weighing oxides or carbonates containing Mg, Ga, Cr and Ge elements according to the molar ratio of the elements, mixing and grinding to obtain a mixture;
(b) heating the mixture to 1200-1300 ℃ 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.
2. The near-infrared phosphor of claim 1, wherein x is 0.01. ltoreq. x.ltoreq.0.1 in the chemical formula.
3. The near-infrared phosphor of claim 2, wherein x is 0.01. ltoreq. x.ltoreq.0.07 in the chemical formula.
4. The near-infrared phosphor of claim 3, wherein x =0.03 in the chemical formula.
5. The near-infrared phosphor of claim 1, wherein the milling time of step (a) is 15-30 min.
6. The near-infrared phosphor of claim 1, wherein the temperature increase rate of step (b) is 5-10 ℃/min.
7. The near-infrared phosphor as claimed in claim 1, wherein the heating in step (b) is carried out at 1300 ℃ for 4 h.
8. The use of the near-infrared phosphor of claim 1 in the preparation of an osram bead.
9. Use of the near-infrared phosphor of claim 1 in food detection, biological detection and imaging of organisms; applications in biological detection and in biological imaging are for non-disease diagnostic purposes.
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| High Efficiency and Broad-Band Near-Infrared Ca2LuZr2Al3O12:Cr3+ Garnet Phosphor for Blue LED Chip;Liangliang Zhang et al.;《Journal of Materials Chemistry C》;20180418;第6卷;第4867-4976页 * |
| Rare-Earth-Free High-Efficiency Narrow-Band Red-Emitting Mg3Ga2GeO8:Mn4+ Phosphor Excited by Near-UV Light for White-Light-Emitting Diodes;Xin Ding et al.;《Inorganic Chemistry》;20151231;第55卷;第154-162页 * |
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