CN107338046A - A kind of near-infrared fluorescent powder and preparation method thereof - Google Patents
A kind of near-infrared fluorescent powder and preparation method thereof Download PDFInfo
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- CN107338046A CN107338046A CN201710648396.4A CN201710648396A CN107338046A CN 107338046 A CN107338046 A CN 107338046A CN 201710648396 A CN201710648396 A CN 201710648396A CN 107338046 A CN107338046 A CN 107338046A
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Abstract
The invention provides a kind of near-infrared fluorescent powder, has formula shown in formula (I)：MAl12O19:XTi formulas (I)；Wherein, M is selected from Ca or Sr；0.001≤x≤0.10.The present invention adulterates Ti using aluminate as matrix3+Ion obtains a kind of Ti3+The near-infrared fluorescent powder of activation.The cost of material of the fluorescent material is relatively low, and luminous intensity is relatively strong and luminous zone is broadband.Also, it prepares the product stability height that the prices of raw materials are cheap, and low for equipment requirements, preparation is simple, favorable repeatability, obtain, and is easy to large-scale promotion and production application.
Description
Technical field
The invention belongs to field of material technology, and in particular to a kind of near-infrared fluorescent powder and preparation method thereof.
Background technology
Near-infrared light-emitting material has the properties such as near infrared light penetration depth is big, intensity is high, absorbed light intensity is small
And in the application in the fields such as optical-fibre communications, lasing light emitter, biology sensor and fluoroimmunoassay, it has been similarly subjected to extensive concern.
Particularly in bioanalysis, field of medical examination huge dive is shown with more fluoroimmunoassay technical elements
Power.This is due to near-infrared light-emitting material using visible ray as excitation source, can avoid harm of the ultraviolet light to biosystem,
Improve security and realize Non-Destructive Testing, while biosystem, without lighting, will not produce spectra overlapping and do near infrared region
Disturb and realize highly sensitive detection.
The research of near-infrared light-emitting material focuses primarily upon the rare earths such as Bu Lin, terphenyl, fluorescein PAN both at home and abroad at present
Organic coordination compound and rare earth ion Er3+、Nd3+、Yb3+Deng doping inorganic compound two types.
Its near infrared luminous intensity of rare earth organic complex is weaker, less stable.This is due to rare earth organic complex
In contain O-H and C-H, both keys have dither, are easy to make excitation state is non-radiative to arrive ground state, cause luminescence queenching,
Greatly reduce near-infrared luminous efficiency.By contrast, though rear-earth-doped inorganic near-infrared light-emitting material avoid it is this sudden
Go out phenomenon, but the application in fields such as bioanalysis nevertheless suffers from very big limitation, because rear-earth-doped inorganic near-infrared
The luminous zone of luminescent material is arrowband, therefore application limitation, and luminous intensity does not reach using required ideal tensile strength.
The content of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of near-infrared fluorescent powder and preparation method thereof,
Near-infrared fluorescent powder provided by the invention is with Ti3+As Doped ions, cost of material is relatively low, and luminous intensity is relatively strong and luminous zone is
Broadband.
The invention provides a kind of near-infrared fluorescent powder, has formula shown in formula (I)：
MAl12O19:XTi formulas (I)；
Wherein, M is selected from Ca or Sr；X is Ti3+Doping mole, 0.001≤x≤0.10, preferably 0.005≤x≤
0.05, more preferably 0.01≤x≤0.02.
In the present invention, the near-infrared fluorescent powder is with Ti3+As the centre of luminescence and Doped ions, the near-infrared fluorescent
The emission wavelength of powder is located at 600nm~850nm, preferably 650~800nm, more preferably 7500~750nm；Emission peak is located at
750~770nm, preferably 755~765nm.
Present invention also offers a kind of preparation method of above-mentioned near-infrared fluorescent powder, by the compound containing M, the chemical combination containing Al
Thing and the compound mixing containing Ti, are sintered, obtain near-infrared fluorescent powder.
The present invention is not particularly limited to the source of the preparing raw material, is commercially available.The compound containing M
The oxide of carbonate and/or M selected from M, preferably M carbonate.The compound containing Ti is selected from Ti oxide, excellent
Elect TiO as2；The compound containing Al is selected from Al oxide, i.e. aluminum oxide.
Compound containing M, the compound containing Al and the compound containing Ti are mixed, obtain mixture.In the present invention, institute
Mixing is stated preferably to mix in mortar.
The mol ratio of the compound containing M, the compound containing Ti and the compound containing Al is preferably 1000:6000:1~
10:60:1。
The temperature of the sintering is 1400~1600 DEG C, preferably 1450~1550 DEG C；The time of the sintering be 4~
8h, preferably 5~7h.The atmosphere of the sintering is the mixed atmosphere of nitrogen and hydrogen.Wherein, the volume of the nitrogen and hydrogen
Than for 1:10~1:20, preferably 1:14~1:16.
In the present invention, the sintering uses high temperature process furnances, and the high temperature process furnances are preferably Muffle furnace.
Compared with prior art, the invention provides a kind of near-infrared fluorescent powder, there is formula shown in formula (I)：
MAl12O19:XTi formulas (I)；Wherein, M is selected from Ca or Sr；0.001≤x≤0.10.The present invention adulterates Ti using aluminate as matrix3+
Ion obtains a kind of Ti3+The near-infrared fluorescent powder of activation.The cost of material of the fluorescent material is relatively low, and luminous intensity is relatively strong and luminous zone
For broadband.Also, its preparation prices of raw materials is cheap, and low for equipment requirements, preparation is simple, favorable repeatability, obtains
The product stability arrived is high, is easy to large-scale promotion and production application.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram of fluorescent material prepared in embodiment 1；
Fig. 2 is the diffusing reflectance spectra of fluorescent material prepared in embodiment 1；
Fig. 3 is the excitation spectrum of fluorescent material prepared in embodiment 1；
Fig. 4 is the emission spectrum of fluorescent material prepared in embodiment 1；
Fig. 5 is the diffusing reflectance spectra of fluorescent material prepared in embodiment 2；
Fig. 6 is the excitation spectrum of fluorescent material prepared in embodiment 2；
Fig. 7 is the emission spectrum of fluorescent material prepared in embodiment 2；
Fig. 8 is the excitation spectrum of fluorescent material prepared in embodiment 3；
Fig. 9 is the emission spectrum of fluorescent material prepared in embodiment 3.
Embodiment
For a further understanding of the present invention, with reference to embodiment to near-infrared fluorescent powder provided by the invention and its preparation
Method is illustrated, and protection scope of the present invention is not limited by the following examples.
The X-ray diffraction detection of testing sample uses the general analysis XD-2X x ray diffractometer xs in Beijing in following examples；Exciting light
Spectrum detection uses Edinburg FLS-980 XRFs；Diffusing reflection spectrum detection is divided using Evolution-220 UV, visible lights
Photometer；Excitation spectrum detection uses Edinburg FLS-980 XRFs.
Embodiment 1
According to the chemical composition of fluorescent material：SrAl12O19:0.001Ti3+, Al is weighed respectively2O3、SrCO3And TiO2, it rubs
Your ratio is 6:1:0.001, it is sufficiently mixed and puts high temperature process furnances into after being ground uniformly in mortar and be sintered, at 1600 DEG C
Lower nitrogen is 1 with hydrogen volume ratio:4h is fired in 10 environment, obtains the fluorescent material.
The fluorescent material obtained in the present embodiment is analyzed, as a result as shown in Figure 1 to 4.Fig. 1 is institute in embodiment 1
The X-ray diffractogram of the fluorescent material of preparation；Fig. 2 is the diffusing reflectance spectra of fluorescent material prepared in embodiment 1, in wherein Fig. 2
Less figure is the partial enlarged drawing at 300~800nm in big figure；Fig. 3 is the exciting light of fluorescent material prepared in embodiment 1
Spectrum；Fig. 4 is the emission spectrum of fluorescent material prepared in embodiment 1.Fig. 1 X-ray diffractogram proves to obtain SrAl12O19It is pure
Phase；There is obvious absworption peak at 400~600nm in Fig. 2 spectrogram that diffuses, illustrate that prepared fluorescent material can quilt
Wavelength effectively excites in the range of this；Fig. 3 is the excitation spectrum of gained under 730nm wavelength detectings, is gone out in figure in 400~600nm
Now obvious excitation peak, belongs to Ti3+Feature excitation peak, illustrate that the fluorescent material can be by excited by visible light；Fig. 4 is in 500nm wavelength
Under excite the emission spectrum of gained, show obvious emission peak at 730nm wavelength, belong to Ti3+Characteristic emission peak, illustrate this
Fluorescent material can launch near infrared light.
Embodiment 2
According to the chemical composition of fluorescent material：SrAl12O19:0.10Ti3+, Al is weighed respectively2O3、SrCO3And TiO2, its mole
Ratio is 6:1:0.10, it is sufficiently mixed and puts high temperature process furnances into after being ground uniformly in mortar and be sintered, at 1400 DEG C
Nitrogen is 1 with hydrogen volume ratio:8h is fired in 10 environment, obtains the fluorescent material.
The fluorescent material obtained in the present embodiment is analyzed, as a result as shown in Fig. 5~Fig. 7.Fig. 5 is institute in embodiment 2
Less figure in the diffusing reflectance spectra of the fluorescent material of preparation, wherein Fig. 5 is the partial enlarged drawing in big figure at 300~800nm；Figure
6 be the excitation spectrum of fluorescent material prepared in embodiment 2；Fig. 7 is the emission spectrum of fluorescent material prepared in embodiment 2.
There is obvious absworption peak at 400~600nm in Fig. 5 spectrogram that diffuses, illustrate that prepared fluorescent material can be by this
In the range of wavelength effectively excite；Fig. 6 is the excitation spectrum of gained under 770nm wavelength monitorings, is occurred in figure in 400~600nm
Obvious excitation peak, belongs to Ti3+Feature excitation peak, illustrate that the fluorescent material can be by excited by visible light；Fig. 7 is under 500nm wavelength
The emission spectrum of gained is excited, obvious emission peak is shown at 770nm wavelength, belongs to Ti3+Characteristic emission peak, illustrate that this is glimmering
Light powder can launch near infrared light.
Embodiment 3
According to the chemical composition of fluorescent material：CaAl12O19:0.01Ti3+, Al is weighed respectively2O3、CaCO3And TiO2, its mole
Ratio is 6:1:0.01, it is sufficiently mixed and puts high temperature process furnances into after being ground uniformly in mortar and be sintered, at 1600 DEG C
Nitrogen is 1 with hydrogen volume ratio:4h is fired in 20 environment, obtains the fluorescent material.
The fluorescent material obtained in the present embodiment is analyzed, as a result as shown in Fig. 8~Fig. 9, Fig. 8 is institute in embodiment 3
The excitation spectrum of the fluorescent material of preparation；Fig. 9 is the emission spectrum of fluorescent material prepared in embodiment 3.Fig. 8 is 770nm wavelength
The excitation spectrum of lower gained is detected, occurs obvious excitation peak in 400~600nm in figure, belongs to Ti3+Feature excitation peak, say
The bright fluorescent material can be by excited by visible light；Fig. 9 is the emission spectrum that gained is excited under 500nm wavelength, belongs to Ti3+Feature hair
Peak is penetrated, obvious emission peak is shown at 770nm wavelength, illustrates that the fluorescent material can launch near infrared light.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of near-infrared fluorescent powder, it is characterised in that there is formula shown in formula (I)：
MAl12O19:XTi formulas (I)；
Wherein, M is selected from Ca or Sr；0.001≤x≤0.10.
2. near-infrared fluorescent powder according to claim 1, it is characterised in that the emission wavelength position of the near-infrared fluorescent powder
In 600nm~850nm, emission peak is located at 750~770nm.
3. a kind of preparation method of near-infrared fluorescent powder as claimed in claim 1, it is characterised in that by the compound containing M, contain
Al compound and the compound mixing containing Ti, are sintered, obtain near-infrared fluorescent powder.
4. preparation method according to claim 3, it is characterised in that the compound containing M be selected from M carbonate and/
Or M oxide.
5. preparation method according to claim 3, it is characterised in that the compound containing Ti is selected from Ti oxide.
6. preparation method according to claim 3, it is characterised in that the compound containing Al is selected from Al oxide.
7. preparation method according to claim 3, it is characterised in that the temperature of the sintering is 1400~1600 DEG C, institute
The time for stating sintering is 4~8h.
8. preparation method according to claim 3, it is characterised in that the atmosphere of the sintering is the mixing of nitrogen and hydrogen
Atmosphere.
9. preparation method according to claim 8, it is characterised in that the volume ratio of the nitrogen and hydrogen is 1:10~1:
20。
10. preparation method according to claim 3, it is characterised in that the compound containing M, the compound containing Ti and
The mol ratio of compound containing Al is 1000:6000:1~10:60:1.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015131036A1 (en) * | 2014-02-28 | 2015-09-03 | Oregon State University | Compounds comprising a hibonite structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015131036A1 (en) * | 2014-02-28 | 2015-09-03 | Oregon State University | Compounds comprising a hibonite structure |
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