CN103194229A - Near-infrared long-afterglow florescent powder and preparation method thereof - Google Patents
Near-infrared long-afterglow florescent powder and preparation method thereof Download PDFInfo
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- CN103194229A CN103194229A CN2013101096079A CN201310109607A CN103194229A CN 103194229 A CN103194229 A CN 103194229A CN 2013101096079 A CN2013101096079 A CN 2013101096079A CN 201310109607 A CN201310109607 A CN 201310109607A CN 103194229 A CN103194229 A CN 103194229A
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Abstract
The invention discloses a near-infrared long-afterglow florescent powder. A substrate material of the near-infrared long-afterglow florescent powder is ZnZA1YSiXO(Z+1.5Y+2X) or ZnZA1YGeXO (Z+1.5y+2X) or ZnZGaYSiXO(Z+1.5Y+2X), wherein X is more than or equal to 1 and less than or equal to 5, Y is more than or equal to 1 and less than or equal to 5, and Z is more than or equal to 1 and less than or equal to 5; and the substrate material is doped with 0.001-5mol% of Cr<3+> and 0.001-20mol% of M, wherein M is one or two of an alkali metal element, an alkaline-earth metal element and a rare-earth element. The invention further discloses a preparation method of the near-infrared long-afterglow florescent powder. The near-infrared long-afterglow florescent powder prepared by using the method can be excited under visible light; in addition, the afterglow time of the near-infrared long-afterglow florescent powder is longer than 120h; and furthermore, the near-infrared long-afterglow florescent powder has an optical-excitation luminescence property and can be well used for bioimaging.
Description
Technical field
The present invention relates to fluorescent material, particularly a kind of near infrared long persistence luminescent powder and preparation method
Background technology
Optical imagery, has represented a field of extending fast and has been applied directly to pharmacology, molecular cytobiology and diagnostics as information source with photon.But still there are many limitation in this technology, and what produce during illumination especially in vivo organizes autofluorescence and the weak tissue permeability under the shortwave excitation light irradiation.In order to overcome these difficulties, scientist has studied a series of phosphors, emission is only near infrared region (NIR), molecular emission near infrared light (700～1000nm), can be used for the detection of living body molecule target, because organism blood is relative transparent with being organized in this wavelength region interior, thereby has reduced the difficult problem that background interference causes in the body.But because the exciting light of many fluorescent materials all is to be positioned at the short wavelength zone, so just both be not easy to excitation fluorescent material, more be not easy to observe phenomena.Therefore there are many researchists to propose to substitute common fluorescent material with near infrared long-afterglow material, thereby are implemented in external exciting, be expelled to the twilight sunset that still exists afterwards in the body and still can be used for doing biological fluorescent mark.The near-infrared fluorescent marker is because its luminous near-infrared region that is positioned at, and biomolecules does not have luminous in this light district, the interference that does not have spectra overlapping to cause, detection background is lower, the near-infrared fluorescent marker can use visible light or the near ultraviolet excitation of shorter wavelength, the Stokes shift of spectrum is big, thereby this influence that helps avoid the exciting light scattering obtains higher sensitivity, in addition, composition in the biological vital tissue to nearly outer photoabsorption seldom, near infrared light penetration depth in biological tissue is big, can produce optical signal at deep tissues, and to organizing almost not influence itself, this helps to obtain the information of more organisms, therefore, the near-infrared fluorescent marker becomes when previous research focus.Long-afterglow material can well be removed at the bottom of the special next back of the body of non-specific imaging as imaging.Long-afterglow material in the past mainly concentrates on the visible region, as the night vision material.The long-afterglow material development of near infrared region and slow, and then limited the application of long-afterglow material aspect bio-imaging.Therefore greatly develop the development that the near infrared long-afterglow material could further promote medical imaging, oncotherapy etc.
Summary of the invention
For the above-mentioned shortcoming and deficiency that overcome prior art, one of purpose of the present invention is to provide a kind of near infrared long persistence luminescent powder.This fluorescent material can excite under visible light, launches the near infrared light of 700nm, and the sunset glow time is greater than 120h.And this material possesses the optical stimulated luminescence characteristic simultaneously, can well be used for bio-imaging.
Two of purpose of the present invention is the preparation method for above-mentioned a kind of near infrared long persistence luminescent powder.
Purpose of the present invention is achieved through the following technical solutions:
A kind of near infrared long persistence luminescent powder, its body material are Zn
ZAl
YSi
XO
(Z+1.5Y+2X)Or Zn
ZAl
YGe
XO
(Z+1.5Y+2X)Or Zn
ZGa
YSi
XO
(Z+1.5Y+2X), wherein, 1≤X≤5,1≤Y≤5,1≤Z≤5; The Cr of 0.001～5mol% mixes in the body material
3+With the M of 0.001～20mol%, wherein M is a kind of in alkali metal, alkali earth metal, the rare earth element or two kinds.
With Zn
ZAl
YSi
XO
(Z+1.5Y+2X)For the preparation method of the near infrared long persistence luminescent powder of body material as follows:
(1) weighing material: take by weighing the compound that contains zinc, aluminium, silicon, chromium respectively; From the compound of alkali metal containing element, alkali earth metal, rare earth element, choose a kind of or two kinds for raw material, and weighing;
(2) material takes out after 1～3 hour 900～1000 ℃ of pre-burnings after grinding mixing, behind the regrinding, fires 2～5 hours in 1250～1450 ℃.
With Zn
ZAl
YGe
XO
(Z+1.5Y+2X)For the preparation method of the near infrared long persistence luminescent powder of body material as follows:
(1) weighing material: take by weighing the compound that contains zinc, aluminium, germanium, chromium respectively; From the compound of alkali metal containing element, alkali earth metal, rare earth element, choose a kind of or two kinds for raw material, and weighing;
(2) material takes out after 1～3 hour 900～1000 ℃ of pre-burnings after grinding mixing, behind the regrinding, fires 2～5 hours in 1150～1250 ℃.
With Zn
ZGa
YSi
XO
(Z+1.5Y+2X)For the preparation method of the near infrared long persistence luminescent powder of body material as follows:
(1) weighing material: take by weighing the compound that contains zinc, gallium, silicon, chromium respectively; From the compound of alkali metal containing element, alkali earth metal, rare earth element, choose a kind of or two kinds for raw material, and weighing;
(2) material takes out after 1～3 hour 900～1000 ℃ of pre-burnings after grinding mixing, behind the regrinding, fires 2～5 hours in 1250～1450 ℃.
Compared with prior art, the present invention has the following advantages and beneficial effect:
A kind of near infrared long persistence luminescent powder of the present invention can excite under visible light, launches the near infrared light of 700nm, and the sunset glow time greater than 120h, and this material possesses the optical stimulated luminescence characteristic simultaneously, can well be used for bio-imaging.
Description of drawings
Fig. 1 is fluorescence spectrum and the excitation spectrum of the sample of embodiments of the invention 1 preparation.
Fig. 2 is the long-persistence luminous decay spectrum of the sample of embodiments of the invention 1 preparation.
Fig. 3 places ten minutes afterglow luminescence image for sample dark place after exciting of embodiments of the invention 1 preparation.
Fig. 4 places one hour afterglow luminescence image for sample dark place after exciting of embodiments of the invention 1 preparation.
Fig. 5 places 12 hours afterglow luminescence image for sample dark place after exciting of embodiments of the invention 1 preparation.
Fig. 6 places the afterglow luminescence image of twenty four hours for sample dark place after exciting of embodiments of the invention 1 preparation.
Fig. 7 places 48 hours afterglow luminescence image for sample dark place after exciting of embodiments of the invention 1 preparation.
Fig. 8 places 120 hours afterglow luminescence image for sample dark place after exciting of embodiments of the invention 1 preparation.
Fig. 9 is the steady persistence excitation spectrum of the sample of embodiments of the invention 1 preparation.
Figure 10 is the optical stimulated luminescence spectrum (sample was placed after 10 hours, excitation wavelength 980nm, power 1.2W) of the sample of embodiments of the invention 1 preparation.
Figure 11 is the optical stimulated luminescence decay spectrum (sample was placed after 10 hours, monitoring wavelength 698nm, excitation wavelength 980nm, power 1.2W) of the sample of embodiments of the invention 1 preparation.
Figure 12 is the optical stimulated luminescence spectrum (sample was placed after 10 hours, excitation wavelength 808nm, power 0.5W) of the sample of embodiments of the invention 1 preparation.
Figure 13 is the optical stimulated luminescence decay spectrum (sample was placed after 10 hours, monitoring wavelength 698nm, excitation wavelength 808nm, power 0.5W) of the sample of embodiments of the invention 1 preparation.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
The preparation method of the near infrared long persistence luminescent powder of present embodiment:
According to following composition: matrix is Zn
ZGa
YSi
XO
(Z+1.5Y+2X)Wherein, x=1, Y=2, Z=3, doped element is Sr and Cr; Sr
2+Doping be 5mol%, Cr
3+The doping of ion is 0.1mol%; Take by weighing zinc oxide, gallium oxide, silicon oxide, chromic oxide respectively, Strontium carbonate powder takes out after 2 hours 1000 ℃ of pre-burnings after grinding mixing, behind the regrinding, fires 3 hours in 1350 ℃.
The fluorescence spectrum of the near infrared long persistence luminescent powder of present embodiment preparation has sent the luminous of 698nm as shown in Figure 1 under 290nm excites, the luminous correspondence of 698nm 4 excitation peaks, is respectively 290nm, 320nm, 400nm, 515nm.Fig. 2 has shown that the sample of present embodiment preparation shines after 10 minutes under sunlight, and stops to excite back one hour decay of afterglow situation, the curve display of exponential attenuation the seizure mechanism of trap.
The near infrared long persistence luminescent powder that takes by weighing the present embodiment preparation of 1.5g is pressed into the disk of diameter 1cm, disk is placed in the imaging device observes.Fig. 3-Fig. 8 has shown that the wafer sample of the present invention's preparation is after sunlight excites 10 minutes, place ten minutes, one hour, 12 hours, twenty four hours, 48 hours, 120 hours afterglow luminescence image respectively at the dark place, shown that this kind material has good long afterglow property.Fig. 9 is the steady persistence excitation spectrum of wafer sample of the present invention, has shown that this kind material can produce steady persistence through excited by visible light.
Figure 10 has shown through after 10 hours, and the optical stimulated luminescence spectrum of the near infrared long persistence luminescent powder of present embodiment preparation has obtained being positioned at the optical stimulated luminescence peak of 698nm under 980nm laser excitation.Figure 11 has shown the optical stimulated luminescence decay spectrum that obtains behind the near infrared long persistence luminescent powder for preparing with 980nm laser radiation present embodiment, and at first sample is luminous very weak, and On represents the moment that laser apparatus is opened, and off represents the moment that laser apparatus cuts out; The luminous reproduction of 698nm, intensity is bigger, but along with the growth of irradiation time, decay is also than comparatively fast, close excitation light source this moment after, showed that the luminous intensity during than 0s is big, but the little twilight sunset of intensity during than laser radiation.Figure 12 has shown through after 10 hours, and the optical stimulated luminescence spectrum of the near infrared long persistence luminescent powder of present embodiment has obtained being positioned at the optical stimulated luminescence peak of 698nm under 808nm laser excitation.Figure 13 has shown the optical stimulated luminescence decay spectrum that obtains behind the near infrared long persistence luminescent powder with 808nm laser radiation present embodiment, and at first sample is luminous very weak, and On represents the moment that laser apparatus is opened, and off represents the moment that laser apparatus cuts out; The luminous reproduction of 698nm, intensity is bigger, but along with the growth of irradiation time, decay is also than comparatively fast, but through back intensity after a while in decline, but remain on a stable intensity, shown that this long-afterglow material has a large amount of deep traps.
Embodiment 2
The preparation method of the near infrared long persistence luminescent powder of present embodiment:
According to following composition: matrix is Zn
ZGa
YSi
XO
(Z+1.5Y+2X)Wherein, x=1, Y=2, Z=5, doped element is Yb and Cr; Yb
3+Doping be 20mol%, Cr
3+The doping of ion is 2mol%; Take by weighing zinc oxide, gallium oxide, silicon oxide, chromic oxide respectively, ytterbium oxide takes out after 3 hours 900 ℃ of pre-burnings after grinding mixing, behind the regrinding, fires 3 hours in 1250 ℃.Its luminescent spectrum after tested, emission peak is positioned at 698nm, and excitation peak is positioned at 320nm, 417nm, 571nm, and the 698nm steady persistence time is 120h.
Embodiment 3
According to following composition: matrix is Zn
ZGa
YSi
XO
(Z+1.5Y+2X)Wherein, x=5, Y=5, Z=1, doped element is Ca and Cr; Ca
2+Doping be 0.001mol%, Cr
3+The doping of ion is 5mol%; Take by weighing zinc oxide, gallium oxide, silicon oxide, chromic oxide respectively, calcium carbonate takes out after 1 hour 1000 ℃ of pre-burnings after grinding mixing, behind the regrinding, fires 1 hour in 1450 ℃.Its luminescent spectrum after tested, emission peak is positioned at 698nm, and excitation peak is positioned at 320nm, 415nm, 580nm, and the 698nm steady persistence time is 180h.
Embodiment 4
The preparation method of the near infrared long persistence luminescent powder of present embodiment:
According to following composition: Zn
ZAl
YSi
XO
(Z+1.5Y+2X)Wherein, x=1, Y=2, Z=5, doped element is Er, Li and Cr; Er
3+Doping be 10mol%, Li
+Doping be 10mol%; Cr
3+The doping of ion is 2mol%; Take by weighing zinc oxide, aluminum oxide, silicon oxide, chromic oxide respectively, Erbium trioxide, Quilonum Retard take out after 3 hours 900 ℃ of pre-burnings after grinding mixing, behind the regrinding, fire 3 hours in 1250 ℃.Its luminescent spectrum after tested, emission peak is positioned at 698nm, and excitation peak is positioned at 318nm, 420nm, 575nm, and the 698nm steady persistence time is 120h.
Embodiment 5
The preparation method of the near infrared long persistence luminescent powder of present embodiment:
According to following composition: Zn
ZAl
YSi
XO
(Z+1.5Y+2X)Wherein, x=5, Y=5, Z=1, doped element is Ca and Cr; Ca
2+Doping be 0.001mol%, Cr
3+The doping of ion is 5mol%; Take by weighing zinc oxide, aluminum oxide, silicon oxide, chromic oxide respectively, calcium carbonate takes out after 1 hour 1000 ℃ of pre-burnings after grinding mixing, behind the regrinding, fires 1 hour in 1450 ℃.Its luminescent spectrum after tested, emission peak is positioned at 698nm, and excitation peak is positioned at 318nm, 421nm, 585nm, and the 698nm steady persistence time is 150h.
Embodiment 6
The preparation method of the near infrared long persistence luminescent powder of present embodiment:
According to following composition: Zn
ZAl
YSi
XO
(Z+1.5Y+2X)Wherein, x=2, Y=5, Z=1, doped element is Er and Cr; Er
3+Doping be 8mol%, Cr
3+The doping of ion is 3mol%; Take by weighing zinc oxide, aluminum oxide, silicon oxide, chromic oxide respectively, Erbium trioxide takes out after 2 hours 1000 ℃ of pre-burnings after grinding mixing, behind the regrinding, fires 3 hours in 1350 ℃.Its luminescent spectrum after tested, emission peak is positioned at 698nm, and excitation peak is positioned at 317nm, 425nm, 580nm, and the 698nm steady persistence time is 140h.
Embodiment 7
The preparation method of the near infrared long persistence luminescent powder of present embodiment:
According to following composition: Zn
ZAl
YGe
XO
(Z+1.5Y+2X)Wherein, x=1, Y=2, Z=5, doped element is Yb, Li and Cr; Yb
3+Doping be 10mol%, Li
+Doping be 10mol%; Cr
3+The doping of ion is 2mol%; Take by weighing zinc oxide, aluminum oxide, germanium oxide, chromic oxide respectively, ytterbium oxide, Quilonum Retard take out after 3 hours 900 ℃ of pre-burnings after grinding mixing, behind the regrinding, fire 5 hours in 1150 ℃.Its luminescent spectrum after tested, emission peak is positioned at 700nm, and excitation peak is positioned at 315nm, 418nm, 594nm, and the 700nm steady persistence time is 120h.
Embodiment 8
The preparation method of the near infrared long persistence luminescent powder of present embodiment:
According to following composition: Zn
ZAl
YGe
XO
(Z+1.5Y+2X)Wherein, x=5, Y=5, Z=1, doped element is Er and Cr; Er
3+Doping be 0.001mol%, Cr
3+The doping of ion is 5mol%; Take by weighing zinc oxide, aluminum oxide, silicon oxide, chromic oxide, Erbium trioxide respectively, after grinding mixing, take out after 1 hour 1000 ℃ of pre-burnings, behind the regrinding, fired 2 hours in 1250 ℃.Its luminescent spectrum after tested, emission peak is positioned at 700nm, and excitation peak is positioned at 318nm, 427nm, 589nm, and the 700nm steady persistence time is 130h.
Embodiment 9
The preparation method of the near infrared long persistence luminescent powder of present embodiment:
According to following composition: Zn
ZAl
YGe
XO
(Z+1.5Y+2X)Wherein, x=2, Y=5, Z=1, doped element is Sr and Cr; Sr
2+Doping be 8mol%, Cr
3+The doping of ion is 3mol%; Take by weighing zinc oxide, aluminum oxide, silicon oxide, chromic oxide respectively, Strontium carbonate powder takes out after 2 hours 1000 ℃ of pre-burnings after grinding mixing, behind the regrinding, fires 3 hours in 1200 ℃.Its luminescent spectrum after tested, emission peak is positioned at 700nm, and excitation peak is positioned at 315nm, 425nm, 595nm, and the 700nm steady persistence time is 120h.
Above-described embodiment is preferred implementation of the present invention; but embodiments of the present invention are not limited by the examples; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (4)
1. a near infrared long persistence luminescent powder is characterized in that, its body material is Zn
ZAl
YSi
XO
(Z+1.5Y+2X)Or Zn
ZAl
YGe
XO
(Z+1.5Y+2X)Or Zn
ZGa
YSi
XO
(Z+1.5Y+2X), wherein, 1≤X≤5,1≤Y≤5,1≤Z≤5; The Cr of 0.001～5mol% mixes in the body material
3+With the M of 0.001～20mol%, wherein M is a kind of in alkali metal, alkali earth metal, the rare earth element or two kinds.
2. the preparation method of the described near infrared long persistence luminescent powder of claim 1 is characterized in that, with Zn
ZAl
YSi
XO
(Z+1.5Y+2X)For the preparation method of the near infrared long persistence luminescent powder of body material as follows:
(1) weighing material: take by weighing the compound that contains zinc, aluminium, silicon, chromium respectively; From the compound of alkali metal containing element, alkali earth metal, rare earth element, choose a kind of or two kinds for raw material, and weighing;
(2) material takes out after 1～3 hour 900～1000 ℃ of pre-burnings after grinding mixing, behind the regrinding, fires 2～5 hours in 1250～1450 ℃.
3. the preparation method of the described near infrared long persistence luminescent powder of claim 1 is characterized in that, with Zn
ZAl
YGe
XO
(Z+1.5Y+2X)For the preparation method of the near infrared long persistence luminescent powder of body material as follows:
(1) weighing material: take by weighing the compound that contains zinc, aluminium, germanium, chromium respectively; From the compound of alkali metal containing element, alkali earth metal, rare earth element, choose a kind of or two kinds for raw material, and weighing;
(2) material takes out after 1～3 hour 900～1000 ℃ of pre-burnings after grinding mixing, behind the regrinding, fires 2～5 hours in 1150～1250 ℃.
4. the preparation method of the described near infrared long persistence luminescent powder of claim 1 is characterized in that, with Zn
ZGa
YSi
XO
(Z+1.5Y+2X)For the preparation method of the near infrared long persistence luminescent powder of body material as follows:
(1) weighing material: take by weighing the compound that contains zinc, gallium, silicon, chromium respectively; From the compound of alkali metal containing element, alkali earth metal, rare earth element, choose a kind of or two kinds for raw material, and weighing;
(2) material takes out after 1～3 hour 900～1000 ℃ of pre-burnings after grinding mixing, behind the regrinding, fires 2～5 hours in 1250～1450 ℃.
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Cited By (6)
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| CN104560034A (en) * | 2014-12-18 | 2015-04-29 | 华南理工大学 | Near-infrared long-persistence luminescent material capable of energy transmission, and preparation method and application thereof |
| CN105199732A (en) * | 2015-08-27 | 2015-12-30 | 华南理工大学 | Near-infrared long-afterglow material with dual functions of bioimaging and photo-thermal treating and preparation method of near-infrared long-afterglow material |
| CN108148583A (en) * | 2018-02-05 | 2018-06-12 | 韩山师范学院 | A kind of near-infrared long after glow luminous material of aluminate-base and preparation method thereof |
| CN111621294A (en) * | 2020-03-24 | 2020-09-04 | 中国科学院上海微系统与信息技术研究所 | Aluminosilicate-based complex phase luminescent material and preparation method and application thereof |
| WO2021243521A1 (en) * | 2020-06-01 | 2021-12-09 | 苏州君诺新材科技有限公司 | Oxynitride fluorescent powder with transition metal as light-emitting center, and preparation method therefor |
| CN114540007A (en) * | 2021-11-18 | 2022-05-27 | 国网浙江省电力有限公司湖州供电公司 | Yellow-green long-afterglow fluorescent powder, preparation method and long-acting fluorescent coating |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104560034A (en) * | 2014-12-18 | 2015-04-29 | 华南理工大学 | Near-infrared long-persistence luminescent material capable of energy transmission, and preparation method and application thereof |
| CN105199732A (en) * | 2015-08-27 | 2015-12-30 | 华南理工大学 | Near-infrared long-afterglow material with dual functions of bioimaging and photo-thermal treating and preparation method of near-infrared long-afterglow material |
| CN108148583A (en) * | 2018-02-05 | 2018-06-12 | 韩山师范学院 | A kind of near-infrared long after glow luminous material of aluminate-base and preparation method thereof |
| CN108148583B (en) * | 2018-02-05 | 2021-08-31 | 韩山师范学院 | Aluminate-based near-infrared long-afterglow luminescent material and preparation method thereof |
| CN111621294A (en) * | 2020-03-24 | 2020-09-04 | 中国科学院上海微系统与信息技术研究所 | Aluminosilicate-based complex phase luminescent material and preparation method and application thereof |
| CN111621294B (en) * | 2020-03-24 | 2023-03-31 | 中国科学院上海微系统与信息技术研究所 | Aluminosilicate-based complex phase luminescent material and preparation method and application thereof |
| WO2021243521A1 (en) * | 2020-06-01 | 2021-12-09 | 苏州君诺新材科技有限公司 | Oxynitride fluorescent powder with transition metal as light-emitting center, and preparation method therefor |
| CN114540007A (en) * | 2021-11-18 | 2022-05-27 | 国网浙江省电力有限公司湖州供电公司 | Yellow-green long-afterglow fluorescent powder, preparation method and long-acting fluorescent coating |
| CN114540007B (en) * | 2021-11-18 | 2023-06-02 | 国网浙江省电力有限公司湖州供电公司 | Yellow-green long-afterglow fluorescent powder, preparation method and long-acting fluorescent coating |
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