CN105802624A - Near-infrared light-emitting material and preparation method and application thereof - Google Patents
Near-infrared light-emitting material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a near-infrared light-emitting material. The general chemical formula of the light-emitting material is Li2Zn1-xMnxGe3O8, wherein x is greater than 0 and less than or equal to 0.20.Meanwhile, the invention further discloses a preparation method of the near-infrared light-emitting material. The preparation method comprises the following steps of 1, weighing oxide or carbonate containing the elements of Li, Zn, Mn and Ge according to the mole ratio of all elements in the general chemical formula of the light-emitting material Li2Zn1-xMnxGe3O8, and conducting mixing and grinding, so that a mixture is obtained; 2, heating the mixture and raising the temperature to 900-950 DEG C, and conducting sintering for 3-3.5 hours while the temperature is preserved, so that a sintered body is obtained; 3, cooling the sintered body to the room temperature, and then conducting grinding, so that the near-infrared light-emitting material is obtained. The light-emitting material can emit near-infrared light with the wavelength being 650-900 nm under excitation of the wavelength range of 250-650 nm, in particular, an obvious characteristic peak with the wavelength being 832 nm under excitation of the wavelength 475 nm, therefore, the near-infrared light-emitting material can be widely applied to the fields such as medical images, cancer therapy, pharmacology, molecular cell biology and diagnostics, and more choices are provided for the occasions where light-emitting materials are used, such as medical images and biological detection.
Description
Technical field
The present invention relates to luminescent material and its production and use, specifically a kind of near-infrared light-emitting material and its preparation method and application.
Background technology
Near infrared region is the non-visible region that people find the earliest.But owing to the material frequency multiplication in this spectrum district and sum of fundamental frequencies absorption signal are weak, bands of a spectrum are overlapping, resolve complexity, limited by technical merit at that time, and near infrared spectrum " has been sunk into sleep " nearly a century and a half.Until the sixties in 20th century, the extensive work done along with the appearance of commercialization instrument and Norris et al., the theory that the content different wavelength points absworption peak multiple near infrared region of material is linear is proposed, and utilize the compositions such as the moisture in NIR diffuse-reflectance technical measurement agricultural product, albumen, fat, just make near-infrared spectrum technique be widely used in agricultural byproducts analysis.To the middle and late stage sixties, appearance along with various new analytical technologies, in addition the weakness that sensitivity is low, anti-interference is poor that classical near-infrared spectral analysis technology exposes, this technology that made people indifferent application in analyzing test, hereafter, near-infrared spectrum technique enters again a reticent period.
The important component part multivariate calibration techniques of Chemical Measurement (Chemometrics) subject that the seventies produces successful Application in spectrum analysis, promotes the popularization of near-infrared spectrum technique.To the later stage eighties, along with developing rapidly of computer technology, the digitized of analytical tool and the development of Chemical Measurement are driven, in terms of solving withdrawing spectral information and ambient interferences, good result is achieved by chemometrics method, in addition the feature that near infrared spectrum is exclusive in test sample technology, making people re-recognize the value of near infrared spectrum, near infrared spectrum applied research in each field launches successively.
Along with the development of near infrared technology, near-infrared is extended to a lot of medical domain: pharmacology, molecular cytobiology and diagnostics etc..The hospital of the U.S. is try to use a kind of new instrument to help nurse to find the blood vessel on patient's arm, principle is made by harmless near infrared ray, detect the position of blood vessel, and the distributed image of blood vessel is projected on arm in real time, to allow medical personnel know where play pin, this perhaps can protect against the misery of " treating unjustly pin ".Near-infrared fluorescent labelling luminescence is positioned near infrared region, and biomolecule does not has luminescence in this district, does not has spectra overlapping to disturb, and near-infrared fluorescent labelling can use the excited by visible light of shorter wavelength, thus avoids dissipating property of exciting light to obtain higher sensitivity.Near-infrared penetration depth in biological vital tissue is big, can produce optical signal at deep tissues, have little to no effect tissue itself, be conducive to obtaining more Biont information.At present, developed in industry and the near-infrared light-emitting material of open report is less.Therefore, it is highly desirable in industry constantly study more near-infrared light-emitting material, and it is applied to the fields such as medical imaging, oncotherapy, pharmacology, molecular cytobiology and diagnostics, use luminescent material to provide more more options for medical image and Biological Detection etc..
Summary of the invention
It is an object of the invention to provide a kind of near-infrared light-emitting material and its preparation method and application, to provide the near-infrared light-emitting material that a kind of purity is high, luminescent properties is good, provide more luminescent materials to select for medical image and Biological Detection.
It is an object of the invention to be achieved through the following technical solutions: a kind of near-infrared light-emitting material, the chemical general formula of this luminescent material is Li2Zn1-xMnxGe3O8, wherein 0 ＜ x≤0.20；The near infrared light of 650-900nm launched under the exciting that wavelength is 250-650nm by this material, especially, produces 832nm more significantly characteristic peak under the exciting that wavelength is 475nm.
Preferably, the chemical general formula of this luminescent material is Li2Zn1-xMnxGe3O8, wherein 0 ＜ x≤0.10；Under this optimum condition, the intensity of emission peak is higher.
Present invention also offers the preparation method of a kind of near-infrared light-emitting material, comprise the following steps:
A () is according to the chemical general formula Li of luminescent material2Zn1-xMnxGe3O8In the mol ratio of each element weigh the oxide containing Li, Zn, Mn, Ge element or carbonate, mixing, grind, obtain mixture, 0 ＜ x≤0.20 in described chemical general formula；
B described mixture is heated to 900-950 DEG C by (), heat preservation sintering 3-3.5h, obtains sintered body；
C () grinds after described sintered body is cooled to room temperature, obtain near-infrared light-emitting material.
In the preparation method of the near-infrared light-emitting material that the present invention provides, step (a) weighs the oxide containing Li, Zn, Mn, Ge element or carbonate is preferably Li2CO3(A.R.)、ZnO (A.R.)、GeO2(99.999%) and MnCO3(A.R.).
0 ＜ x≤0.10 of step (a) in the preparation method of the near-infrared light-emitting material that the present invention provides；Under this optimum condition, the intensity of emission peak is higher.
In the preparation method of the near-infrared light-emitting material that the present invention provides, the described milling time of step (a) is 15-30min.
In the preparation method of the near-infrared light-emitting material that the present invention provides, the described heating ramp rate of step (b) is 5-10 DEG C/min.
When being heated to 900 DEG C described in step (b) in the preparation method of the near-infrared light-emitting material that the present invention provides, during heat preservation sintering 3h, preferably 0.05≤x≤0.2 in chemical general formula, so it is easier to prepare pure phase product.
In the preparation method of the near-infrared light-emitting material that the present invention provides, step (b) is preferably heated to 950 DEG C, and heat preservation sintering 3h, under this optimum condition, it is easier to prepare pure phase product.
The preferred 5-10min of step (c) milling time in the preparation method of the near-infrared light-emitting material that the present invention provides.
The present invention is based on lower transfer principle, with Li2ZnGe3O8For substrate, it is doped with a certain proportion of Mn2+, by specific preparation technology, synthesized and a kind of can launch the near infrared light of 650-900nm under the exciting of wave-length coverage 250-650nm, under the exciting that wavelength is 475nm, especially produce the advanced luminescent material of 832nm more significantly characteristic peak.Detected by experiment, luminescent material purity prepared by the present invention is high, good luminous performance, it characteristics of luminescence possessed can make it be applied in fields such as medical image, oncotherapy, pharmacology, molecular cytobiology and diagnosticss, uses luminescent material to provide more more options for the field such as medical image and Biological Detection；And its preparation method is simple, safe, easily operated control, it is simple to large-scale production and popularization and application.
Accompanying drawing explanation
Fig. 1 is the luminescent ceramic matrix Li of embodiment 3 preparation2ZnGe3O8Emission spectrum figure.
Fig. 2 is the X ray diffracting spectrum of luminescent material prepared by embodiment 4-8.
Fig. 3 is the X ray diffracting spectrum of luminescent material prepared by embodiment 10-14.
Fig. 4 is absorption spectrum and the emission spectrum figure of the luminescent material of embodiment 10 preparation.
Detailed description of the invention
Example below is used for further describing the present invention, but the present invention is not limited in any form by embodiment.Unless stated otherwise, the present invention uses reagent, method and apparatus are the art conventional reagent, method and apparatus.But limit the present invention the most in any form.
Embodiment 1
Weigh lithium carbonate (Li respectively2CO3) 0.3079g, zinc oxide (ZnO) 0.3391g, germanium oxide (GeO2) 1.3080g, it being placed in agate mortar and be fully ground and after mix homogeneously, the powder after grinding is placed in little dry pot roasting 3h under 900 DEG C of stoves of high temperature, naturally cools to room temperature, is taken out by sample and grinds, obtains substrate Li2ZnGe3O8。
Embodiment 2
Weigh lithium carbonate 0.3079g, zinc oxide 0.3391g, germanium oxide 1.3080g respectively, being placed in agate mortar and be fully ground and after mix homogeneously, the powder after grinding is placed in little dry pot roasting 3h under 925 DEG C of stoves of high temperature, naturally cools to room temperature, sample is taken out and grinds, obtain substrate Li2ZnGe3O8。
Embodiment 3
Weigh lithium carbonate 0.3079g, zinc oxide 0.3391g, germanium oxide 1.3080g respectively, being placed in agate mortar and be fully ground and after mix homogeneously, the powder after grinding is placed in little dry pot roasting 3h under 950 DEG C of stoves of high temperature, naturally cools to room temperature, sample is taken out and grinds, obtain substrate Li2ZnGe3O8。
Embodiment 4
Weigh lithium carbonate 0.5172g, zinc oxide 0.5669g, germanium oxide 2.1974g, manganese carbonate 0.0040g, it is placed in agate mortar after mix homogeneously, grind 15min, powder after grinding is placed in little dry pot, it is warming up to 900 DEG C with the heating rate of 10 DEG C/min, heat preservation sintering 3h, sinter is naturally cooled to room temperature (25 DEG C), sample is taken out and grinds 10min, obtain Li2Zn0.995Mn0.005Ge3O8。
Embodiment 5
Weigh lithium carbonate 0.5172g, zinc oxide 0.5640g, germanium oxide 2.1974g, manganese carbonate 0.0080g, it is placed in agate mortar after mix homogeneously, grind 30min, powder after grinding is placed in little dry pot, it is warming up to 900 DEG C with the heating rate of 8 DEG C/min, heat preservation sintering 3h, sinter is naturally cooled to room temperature (25 DEG C), sample is taken out and grinds 5min, obtain Li2Zn0.99Mn0.01Ge3O8。
Embodiment 6
Weigh lithium carbonate 0.5172g, zinc oxide 0.5526g, germanium oxide 2.1974g, manganese carbonate 0.0241g, it is placed in agate mortar after mix homogeneously, grind 20min, powder after grinding is placed in little dry pot, it is warming up to 900 DEG C with the heating rate of 5 DEG C/min, heat preservation sintering 3h, sinter is naturally cooled to room temperature (25 DEG C), sample is taken out and grinds 8min, obtain Li2Zn0.97Mn0.03Ge3O8。
Embodiment 7
Weigh lithium carbonate 0.5172g, zinc oxide 0.5412g, germanium oxide 2.1974g, manganese carbonate 0.0402g, it is placed in agate mortar after mix homogeneously, grind 30min, powder after grinding is placed in little dry pot, it is warming up to 900 DEG C with the heating rate of 10 DEG C/min, heat preservation sintering 3h, sinter is naturally cooled to room temperature (25 DEG C), sample is taken out and grinds 10min, obtain Li2Zn0.95Mn0.05Ge3O8。
Embodiment 8
Weigh lithium carbonate 0.5172g, zinc oxide 0.5128g, germanium oxide 2.1974g, manganese carbonate 0.0805g, it is placed in agate mortar after mix homogeneously, grind 15min, powder after grinding is placed in little dry pot, it is warming up to 900 DEG C with the heating rate of 10 DEG C/min, heat preservation sintering 3h, sinter is naturally cooled to room temperature (25 DEG C), sample is taken out and grinds 8min, obtain Li2Zn0.9Mn0.1Ge3O8。
Embodiment 9
Weigh lithium carbonate 0.5172g, zinc oxide 0.4558g, germanium oxide 2.1974g, manganese carbonate 0.1609g, it is placed in agate mortar after mix homogeneously, grind 30min, powder after grinding is placed in little dry pot, it is warming up to 900 DEG C with the heating rate of 10 DEG C/min, heat preservation sintering 3.5h, sinter is naturally cooled to room temperature (25 DEG C), sample is taken out and grinds 10min, obtain Li2Zn0.8Mn0.2Ge3O8。
Embodiment 10
Weigh lithium carbonate 0.5172g, zinc oxide 0.5669g, germanium oxide 2.1974g, manganese carbonate 0.0040g, it is placed in agate mortar after mix homogeneously, grind 30min, powder after grinding is placed in little dry pot, it is warming up to 950 DEG C with the heating rate of 10 DEG C/min, heat preservation sintering 3h, sinter is naturally cooled to room temperature (25 DEG C), sample is taken out and grinds 8min, obtain Li2Zn0.995Mn0.005Ge3O8。
Embodiment 11
Weigh lithium carbonate 0.5172g, zinc oxide 0.5640g, germanium oxide 2.1974g, manganese carbonate 0.0080g, it is placed in agate mortar after mix homogeneously, grind 30min, powder after grinding is placed in little dry pot, it is warming up to 950 DEG C with the heating rate of 8 DEG C/min, heat preservation sintering 3h, sinter is naturally cooled to room temperature (25 DEG C), sample is taken out and grinds 10min, obtain Li2Zn0.99Mn0.01Ge3O8。
Embodiment 12
Weigh lithium carbonate 0.5172g, zinc oxide 0.5526g, germanium oxide 2.1974g, manganese carbonate 0.0241g, it is placed in agate mortar after mix homogeneously, grind 20min, powder after grinding is placed in little dry pot, it is warming up to 950 DEG C with the heating rate of 5 DEG C/min, heat preservation sintering 3h, sinter is naturally cooled to room temperature (25 DEG C), sample is taken out and grinds 5min, obtain Li2Zn0.97Mn0.03Ge3O8。
Embodiment 13
Weigh lithium carbonate 0.5172g, zinc oxide 0.5412g, germanium oxide 2.1974g, manganese carbonate 0.0402g, it is placed in agate mortar after mix homogeneously, grind 30min, powder after grinding is placed in little dry pot, it is warming up to 950 DEG C with the heating rate of 10 DEG C/min, heat preservation sintering 3h, sinter is naturally cooled to room temperature (25 DEG C), sample is taken out and grinds 10min, obtain Li2Zn0.95Mn0.05Ge3O8。
Embodiment 14
Weigh lithium carbonate 0.5172g, zinc oxide 0.5128g, germanium oxide 2.1974g, manganese carbonate 0.0805g, it is placed in agate mortar after mix homogeneously, grind 15min, powder after grinding is placed in little dry pot, it is warming up to 950 DEG C with the heating rate of 10 DEG C/min, heat preservation sintering 3h, sinter is naturally cooled to room temperature (25 DEG C), sample is taken out and grinds 5min, obtain Li2Zn0.9Mn0.1Ge3O8。
Embodiment 15
Weigh lithium carbonate 0.5172g, zinc oxide 0.4558g, germanium oxide 2.1974g, manganese carbonate 0.1609g, it is placed in agate mortar after mix homogeneously, grind 30min, powder after grinding is placed in little dry pot, it is warming up to 950 DEG C with the heating rate of 10 DEG C/min, heat preservation sintering 3.5h, sinter is naturally cooled to room temperature (25 DEG C), sample is taken out and grinds 10min, obtain Li2Zn0.8Mn0.2Ge3O8。
Embodiment 16
Weigh lithium carbonate 0.5172g, zinc oxide 0.5526g, germanium oxide 2.1974g, manganese carbonate 0.0241g, it is placed in agate mortar after mix homogeneously, grind 25min, powder after grinding is placed in little dry pot, it is warming up to 925 DEG C with the heating rate of 5 DEG C/min, heat preservation sintering 3h, sinter is naturally cooled to room temperature (25 DEG C), sample is taken out and grinds 8min, obtain Li2Zn0.97Mn0.03Ge3O8。
Embodiment 17 detects the optical property detection of the luminescent material prepared by embodiment.
As a example by embodiment 3, detection substrate Li prepared by embodiment 32ZnGe3O8Emission spectrum as shown in Figure 1.Showing in Fig. 1, this substrate is to have two obvious emission peaks of 414nm and 548nm under 254nm excites at wavelength.
Luminescent material prepared by Example 4-8, detects the X ray diffracting spectrum of each luminescent material as shown in Figure 2.Showing in Fig. 2, the luminescent material that embodiment 7,8 is prepared compared with embodiment 4,5,6 is almost without miscellaneous peak, and the purity of its product is higher.
Luminescent material prepared by Example 10-14, detects the X ray diffracting spectrum of each luminescent material as shown in Figure 3.Showing in Fig. 3, luminescent material prepared by embodiment 10-14 is almost without miscellaneous peak, and the purity of its product is higher.Finding from the contrast of embodiment 4-8 and the X ray diffracting spectrum of embodiment 10-14, in preparing luminescent material, adulterate in substrate the most a small amount of Mn2+(0 < x <
0.05), time, the sintering process of 950 DEG C of heat preservation sintering 3h of its temperature is even more ideal compared with 900 DEG C of heat preservation sintering 3h, it is easier to obtain the pure phase of near-infrared light-emitting material.
As a example by the material of embodiment 10 preparation, the excitation spectrum of the luminescent material of embodiment 10 preparation that detection obtains and emission spectrum are as shown in Figure 4.Fig. 4 shows under the exciting of wavelength 475nm, the obvious characteristic peak of 832nm can be produced.Thus illustrating, material prepared by the present invention can launch near infrared light under specific wavelength excites, and has broad application prospects.
Above-described embodiment is the present invention preferably embodiment; but embodiments of the present invention are also not restricted by the embodiments; the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify; all should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (8)
1. a near-infrared light-emitting material, it is characterised in that the chemical general formula of this luminescent material is Li2Zn1-xMnxGe3O8, wherein 0 ＜ x≤0.20.
Near-infrared light-emitting material the most according to claim 1, it is characterised in that described 0 ＜ x≤0.10.
3. the preparation method of a near-infrared light-emitting material, it is characterised in that comprise the following steps:
A () is according to the chemical general formula Li of luminescent material2Zn1-xMnxGe3O8In the mol ratio of each element weigh the oxide containing Li, Zn, Mn, Ge element or carbonate, mixing, grind, obtain mixture, 0 ＜ x≤0.20 in described chemical general formula；
B described mixture is heated to 900-950 DEG C by (), heat preservation sintering 3-3.5h, obtains sintered body；
C () grinds after described sintered body is cooled to room temperature, obtain near-infrared light-emitting material.
The preparation method of near-infrared light-emitting material the most according to claim 3, it is characterised in that 0 ＜ x≤0.10 described in described step (a).
The preparation method of near-infrared light-emitting material the most according to claim 3, it is characterised in that described step (a) milling time is 15-30min.
The preparation method of near-infrared light-emitting material the most according to claim 3, it is characterised in that the described heating ramp rate of described step (b) is 5-10 DEG C/min.
7. according to the preparation method of the near-infrared light-emitting material described in claim 3,4,5 or 6, it is characterised in that be heated to 950 DEG C described in described step (b), heat preservation sintering 3h.
8. the transmitting near infrared light application in medical image, oncotherapy, pharmacology, molecular cytobiology or diagnostics under the exciting that wavelength is 250-650nm of the near-infrared light-emitting material described in a claim 1.
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| JP2009021033A (en) * | 2007-07-10 | 2009-01-29 | Hitachi Ltd | Image display device |
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| PENGFEI LI ET AL.: "Red to near infrared ultralong lasting luminescence from Mn2+-doped sodium gallium aluminum germanate glasses and (Al,Ga)-albite glass-ceramics", 《J. MATER. CHEM. C》 * |
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