CN103897696A - Cr-doped nano near infrared long-persistence material and preparation method thereof - Google Patents
Cr-doped nano near infrared long-persistence material and preparation method thereof Download PDFInfo
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- CN103897696A CN103897696A CN201410127225.3A CN201410127225A CN103897696A CN 103897696 A CN103897696 A CN 103897696A CN 201410127225 A CN201410127225 A CN 201410127225A CN 103897696 A CN103897696 A CN 103897696A
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Abstract
The invention discloses a Cr-doped nano near infrared long-persistence material. A base material is Zn(2-x)Al2xSn(1-x)O4, wherein x is more than or equal to 0 and less than or equal to 1, the doped ion Cr<3+> is an active ion, and the doping amount of the Cr<3+> is 0.01-0.05mol%. The invention also discloses a method for preparing the Cr-doped nano near infrared long-persistence material. The nano near infrared long-persistence material prepared by the invention has the particle size being less than 100nm and is high in monodispersity and excellent in uniformity, the particles are not aggregated after being sintered at a high temperature of over 1000 DEG C, the stability of the particles is high, the persistence time is more than 150 hours, and the Cr-doped nano near infrared long-persistence material can be well applied to the field of bioimaging and is low in cost.
Description
Technical field
The present invention relates to infrared long-persistence nano material, particularly nm near-infrared long-afterglow material of a kind of Cr doping and preparation method thereof.
Background technology
Along with the development of biomedical research, also more and more higher to the requirement of research object, biomedical scientific research personnel wishes directly to observe at live body or the esoteric physiology biological procedures of animalcule.Optical imagery, using photon as information source, has represented a field of extending fast and has been applied directly to pharmacology, molecular cytobiology and diagnostics.But this technology still exists many limitation, what produce when illumination especially in vivo organizes autofluorescence and weak tissue permeability under shortwave excitation light irradiation.In order to overcome these difficulties, scientist has studied a series of phosphors, utilizing emitted light is near infrared region (NIR), molecular emission near infrared light (700～1000nm), can be for the detection of living body molecule target, because organism blood be organized in this wavelength region in relative transparent, thereby reduced the difficult problem that in body, background interference causes.Therefore there are many researchists to propose to substitute common fluorescent material with near infrared long-afterglow material, excite in vitro thereby realize, be expelled to the interior twilight sunset afterwards of body and can be used for doing biological fluorescent mark.And with respect to other imaging marker material, long-afterglow material is in order to be can be in order to observe the diffusion of marker material as the unique advantage of biological fluorescent labelling material, this is that other any marker materials are not available.The near infrared long-afterglow material of latest developments also only limits to high temperature solid-phase sintering, also inevitably will run into raw material costliness even if can be prepared into nano level long-afterglow material, is unfavorable for promoting the more impossible problem that is applied to production practice.We also find that existing preparation nanometer long-afterglow material all inevitably will run into the problem that high temperature sintering causes nano particle to increase simultaneously, therefore want further to advance the application of near infrared long-afterglow material in bio-imaging, be necessary very much to develop improved technology of preparing and develop nm near-infrared long-afterglow material cheaply.
Summary of the invention
In order to overcome the above-mentioned shortcoming and deficiency of prior art, the object of the present invention is to provide a kind of nm near-infrared long-afterglow material of Cr doping, particle be less than 100 nanometers and monodispersity good, excellent in uniformity, particle, after high temperature 1000 is spent above high temperature sintering, still can not be reunited, granule stability is good, and be greater than 150 hours time of persistence, can be good at being applied to bio-imaging field, and with low cost.
Another object of the present invention is to the preparation method of the nm near-infrared long-afterglow material that above-mentioned Cr doping is provided.
Object of the present invention is achieved through the following technical solutions:
A nm near-infrared long-afterglow material for Cr doping, body material is Zn
(2-x)al
2xsn
(1-x)o
4, 0≤x≤0.1; Dopant ion Cr
3+for active ions, wherein Cr
3+doping be 0.01mol%～0.05mol%.
The preparation method of the nm near-infrared long-afterglow material of above-mentioned Cr doping, comprises the following steps:
(1) with zinc acetate, aluminum nitrate, tin chloride, chromium nitrate is raw material, take raw material and add water and the mixing solutions of alcohol in, at room temperature stir after 10～30 minutes and add methyl ethyl diketone, at room temperature stir and within 0.5～2 hour, obtain mixed solution, wherein the pH value of mixed solution is controlled at 2～4;
(2) mixed solution step (1) being obtained is put into the oven drying 24～48h of 70～90 DEG C, obtains wet gel;
(3) mixing solutions of propyl carbinol and alcohol is joined in the wet gel that step (2) obtains, be put in the oil bath pan of 60～80 DEG C and react 1～2h, be warmed up to subsequently 90～100 DEG C of reactions 1～2 hour, after the liquid complete reaction in beaker, by temperature increase to 120～150 DEG C reaction 5～20 minutes, after being dried, obtain xerogel;
(4) xerogel that step (3) obtains is transferred in crucible after grinding, and in the smelting furnace of 1200～1300 DEG C, burns 2～4h, obtains powder;
(5) powder step (4) being obtained packs centrifuge tube into, carries out centrifugal treating after supersound process, obtains the nm near-infrared long-afterglow material of Cr doping.
The mol ratio of the metal ion total amount in the described methyl ethyl diketone of step (1) and mixed solution is 1:1.
In the mixing solutions of the described water of step (1) and alcohol, the volume ratio of water and alcohol is=1:0.5～1:1.
In the mixing solutions of the described propyl carbinol of step (3) and alcohol, the volume ratio of propyl carbinol and alcohol is 2:8～3:7.
Step (5) centrifugal treating, is specially: taking rotating speed as 6000 revs/min, and centrifugal 7～12min, alcohol is washed 3～5 times, washes 3～5 times, leaves standstill after 48～72 hours taking rotating speed as 10000 revs/min of centrifugal 10～20min afterwards.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) invention adopts zinc acetate, aluminum nitrate, and tin chloride, chromium nitrate, methyl ethyl diketone, alcohol, propyl carbinol is raw material, with low cost, is easy to megatechnics and promotes.
(2) the nm near-infrared long-afterglow material that the present invention prepares, particle be less than 100 nanometers and monodispersity good, excellent in uniformity, particle, after high temperature 1000 is spent above high temperature sintering, still can not be reunited, and granule stability is good, excellent in uniformity, this is a kind of huge breakthrough in the preparation of long-persistence nano material, and is greater than 150 hours time of persistence, can be good at being applied to bio-imaging field.
Brief description of the drawings
Fig. 1 is fluorescence spectrum and the excitation spectrum of the nm near-infrared long-afterglow material prepared of embodiments of the invention 1.
Fig. 2 is the long-persistence luminous decay spectrum of the nm near-infrared long-afterglow material prepared of embodiments of the invention 1.
Fig. 3 is the scanning electron microscope (SEM) photograph of the nm near-infrared long-afterglow material prepared of embodiments of the invention 1.
Fig. 4 is the long-persistence luminous decay spectrum of the nm near-infrared long-afterglow material prepared of embodiments of the invention 2.
Fig. 5 is the scanning electron microscope (SEM) photograph of the nm near-infrared long-afterglow material prepared of embodiments of the invention 2.
Fig. 6 is the long-persistence luminous decay spectrum of the nm near-infrared long-afterglow material prepared of embodiments of the invention 3.
Fig. 7 is the scanning electron microscope (SEM) photograph of the nm near-infrared long-afterglow material prepared of embodiments of the invention 3.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
The nm near-infrared long-afterglow material of the Cr doping of the present embodiment, body material is Zn
(2-x)al
2xsn
(1-x)o
4, x=0.01; Dopant ion Cr
3+for active ions, wherein Cr
3+doping be 0.01mol%.
The nm near-infrared long-afterglow material preparation method of the Cr doping of the present embodiment is as follows:
(1) with zinc acetate, aluminum nitrate, tin chloride, chromium nitrate is raw material, takes raw material and adds in the mixing solutions of 20g water and alcohol, at room temperature stirs after 30 minutes and adds methyl ethyl diketone, at room temperature stir and within 1 hour, obtain mixed solution, wherein the pH value of mixed solution is controlled at 2; Wherein, the mol ratio of the metal ion total amount in methyl ethyl diketone and mixed solution is 1:1; In the mixing solutions of described water and alcohol, the volume ratio of water and alcohol is=1:1;
(2) mixing solutions step (1) being obtained is put into the oven drying 24h of 80 DEG C, obtains wet gel;
(3) mixing solutions of 20g propyl carbinol and alcohol is joined in the wet gel that step (2) obtains, be put in the oil bath pan of 70 DEG C and react 1h, be warmed up to subsequently 98 DEG C of reactions 1 hour, after the liquid complete reaction in beaker, by temperature increase to 150 DEG C reaction 5～20 minutes, after being dried, obtain xerogel; In the mixing solutions of described propyl carbinol and alcohol, the volume ratio of propyl carbinol and alcohol is 3:7;
(4) xerogel that step (3) obtains is transferred in crucible after grinding, and in the smelting furnace of 1200 DEG C, burns 2h, obtains powder;
(5) powder step (4) being obtained packs centrifuge tube into, by ultrasonic 30min, 6000 leave heart 10min, alcohol is washed 3 times, wash 3 times, leave standstill afterwards after 48 hours taking rotating speed as 10000 revs/min of centrifugal 10min separate macrobead with small-particle, can obtain particle and be less than 100 nanometers, single finely disseminated nanoparticle.
The fluorescence spectrum of the nm near-infrared long-afterglow material of Cr prepared by the present embodiment doping shows as shown in Figure 1, and under 280nm excites, sent the luminous of 698nm, the luminous correspondence of 698nm 4 excitation peaks, is respectively 290nm, 320nm, 400nm, 515nm.Fig. 2 has shown that the nm near-infrared long-afterglow material of Cr doping prepared by the present embodiment irradiates after 10 minutes under sunlight, and stops exciting the decay of afterglow situation of latter 150 hours.Fig. 3 is the scanning electron microscope (SEM) photograph of the nm near-infrared long-afterglow material of the Cr doping prepared of the present invention, the nm near-infrared long-afterglow material particle that has shown Cr doping prepared by the present invention is less than 100 nanometers, and favorable dispersity, the pattern of single nanoparticle is visible, although passed through the high temperature sintering of 1200 degrees Celsius, but still can obtain dispersed well nanoparticle, make this material can be good at being applied in bio-imaging.
Embodiment 2
The nm near-infrared long-afterglow material of the Cr doping of the present embodiment, body material is Zn
(2-x)al
2xsn
(1-x)o
4, x=0.1; Dopant ion Cr
3+for active ions, wherein Cr
3+doping be 0.05mol%.
The nm near-infrared long-afterglow material preparation method of the Cr doping of the present embodiment is as follows:
(1) with zinc acetate, aluminum nitrate, tin chloride, chromium nitrate is raw material, takes raw material and adds in the mixing solutions of 20g water and alcohol, at room temperature stirs after 10 minutes and adds methyl ethyl diketone, at room temperature stir and within 1 hour, obtain mixed solution, wherein the pH value of mixed solution is controlled at 4; Wherein, the mol ratio of the metal ion total amount in methyl ethyl diketone and mixed solution is 1:1; In the mixing solutions of described water and alcohol, the volume ratio of water and alcohol is=1:0.5;
(2) mixing solutions step (1) being obtained is put into the oven drying 24h of 70 DEG C, obtains wet gel;
(3) mixing solutions of 20g propyl carbinol and alcohol is joined in the wet gel that step (2) obtains, be put in the oil bath pan of 60 DEG C and react 1h, be warmed up to subsequently 90 DEG C of reactions 1 hour, after the liquid complete reaction in beaker, by temperature increase to 120 DEG C reaction 20 minutes, obtain xerogel after being put into 150 DEG C of oven drying 24h; In the mixing solutions of described propyl carbinol and alcohol, the volume ratio of propyl carbinol and alcohol is 2:8;
(4) xerogel that step (3) obtains is transferred in crucible after grinding, and in the smelting furnace of 1300 DEG C, burns 2h, obtains powder;
(5) powder step (4) being obtained packs centrifuge tube into, by ultrasonic 30min, 6000 leave heart 10min, alcohol is washed 3 times, wash 3 times, leave standstill afterwards after 48 hours taking rotating speed as 10000 revs/min of centrifugal 10min separate macrobead with small-particle, can obtain particle and be less than 100 nanometers, single finely disseminated nanoparticle.
Fig. 4 has shown that the nm near-infrared long-afterglow material of Cr doping prepared by the present embodiment irradiates after 10 minutes under sunlight, and stops exciting the decay of afterglow situation of latter 150 hours.Fig. 5 is the scanning electron microscope (SEM) photograph of the nm near-infrared long-afterglow material of the Cr doping prepared of the present invention, the nm near-infrared long-afterglow material particle that has shown Cr doping prepared by the present invention is less than 100 nanometers, and favorable dispersity, the pattern of single nanoparticle is visible, although passed through the high temperature sintering of 1300 degrees Celsius, but still can obtain dispersed well nanoparticle, make this material can be good at being applied in bio-imaging.
Embodiment 3
The nm near-infrared long-afterglow material of the Cr doping of the present embodiment, body material is Zn
(2-x)al
2xsn
(1-x)o
4, x=0; Dopant ion Cr
3+for active ions, wherein Cr
3+doping be 0.01mol%.
The nm near-infrared long-afterglow material preparation method of the Cr doping of the present embodiment is as follows:
(1) with zinc acetate, tin chloride, chromium nitrate is raw material, takes raw material and adds in the mixing solutions of 20g water and alcohol, at room temperature stirs after 30 minutes and adds methyl ethyl diketone, at room temperature stirs and within 1 hour, obtains mixed solution, wherein the pH value of mixed solution is controlled at 4; Wherein, the mol ratio of the metal ion total amount in methyl ethyl diketone and mixed solution is 1:1; In the mixing solutions of described water and alcohol, the volume ratio of water and alcohol is=1:1;
(2) mixing solutions step (1) being obtained is put into the oven drying 24h of 90 DEG C, obtains wet gel;
(3) mixing solutions of 20g propyl carbinol and alcohol is joined in the wet gel that step (2) obtains, be put in the oil bath pan of 80 DEG C and react 2h, be warmed up to subsequently 100 DEG C of reactions 2 hours, after the liquid complete reaction in beaker, by temperature increase to 150 DEG C reaction 5 minutes, after being dried, obtain xerogel; In the mixing solutions of described propyl carbinol and alcohol, the volume ratio of propyl carbinol and alcohol is 2:8;
(4) xerogel that step (3) obtains is transferred in crucible after grinding, and in the smelting furnace of 1200 DEG C, burns 4h, obtains powder;
(5) powder step (4) being obtained packs centrifuge tube into, by ultrasonic 30min, 6000 leave heart 10min, alcohol is washed 5 times, wash 5 times, leave standstill afterwards after 72 hours taking rotating speed as 10000 revs/min of centrifugal 20min separate macrobead with small-particle, can obtain particle and be less than 100 nanometers, single finely disseminated nanoparticle.
Fig. 6 has shown that the nm near-infrared long-afterglow material of Cr doping prepared by the present embodiment irradiates after 10 minutes under sunlight, and stops exciting the decay of afterglow situation of latter 150 hours.Fig. 7 is the scanning electron microscope (SEM) photograph of the nm near-infrared long-afterglow material of the Cr doping prepared of the present invention, show that material granule prepared by the present invention is less than 100 nanometers, and favorable dispersity, the pattern of single nanoparticle is visible, although passed through the high temperature sintering of 1200 degrees Celsius, but still can obtain dispersed well nanoparticle, make this material can be good at being applied in bio-imaging.
Above-described embodiment is preferably embodiment 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 principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (6)
1. a nm near-infrared long-afterglow material for Cr doping, is characterized in that, body material is Zn
(2-x)al
2xsn
(1-x)o
4, 0≤x≤0.1; Dopant ion Cr
3+for active ions, wherein Cr
3+doping be 0.01mol%～0.05mol%.
2. the preparation method of the nm near-infrared long-afterglow material of Cr doping described in claim 1, is characterized in that, comprises the following steps:
(1) with zinc acetate, aluminum nitrate, tin chloride, chromium nitrate is raw material, take raw material and add water and the mixing solutions of alcohol in, at room temperature stir after 10～30 minutes and add methyl ethyl diketone, at room temperature stir and within 0.5～2 hour, obtain mixed solution, wherein the pH value of mixed solution is controlled at 2～4;
(2) mixed solution step (1) being obtained is put into the oven drying 24～48h of 70～90 DEG C, obtains wet gel;
(3) mixing solutions of propyl carbinol and alcohol is joined in the wet gel that step (2) obtains, be put in the oil bath pan of 60～80 DEG C and react 1～2h, be warmed up to subsequently 90～100 DEG C of reactions 1～2 hour, after the liquid complete reaction in beaker, by temperature increase to 120～150 DEG C reaction 5～20 minutes, after being dried, obtain xerogel;
(4) xerogel that step (3) obtains is transferred in crucible after grinding, and in the smelting furnace of 1200～1300 DEG C, burns 2～4h, obtains powder;
(5) powder step (4) being obtained packs centrifuge tube into, carries out centrifugal treating after supersound process, obtains the nm near-infrared long-afterglow material of Cr doping.
3. the preparation method of the nm near-infrared long-afterglow material of Cr doping according to claim 2, is characterized in that, the mol ratio of the metal ion total amount in the described methyl ethyl diketone of step (1) and mixed solution is 1:1.
4. the preparation method of the nm near-infrared long-afterglow material of Cr doping according to claim 2, is characterized in that, in the mixing solutions of the described water of step (1) and alcohol, the volume ratio of water and alcohol is=1:0.5～1:1.
5. the preparation method of the nm near-infrared long-afterglow material of Cr doping according to claim 2, is characterized in that, in the mixing solutions of the described propyl carbinol of step (3) and alcohol, the volume ratio of propyl carbinol and alcohol is 2:8～3:7.
6. the preparation method of the nm near-infrared long-afterglow material of Cr doping according to claim 2, is characterized in that, step (5) centrifugal treating, is specially:
Taking rotating speed as 6000 revs/min, centrifugal 7～12min, alcohol is washed 3～5 times, washes 3～5 times, leaves standstill after 48～72 hours taking rotating speed as 10000 revs/min of centrifugal 10～20min afterwards.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104861970A (en) * | 2015-04-03 | 2015-08-26 | 华南理工大学 | Cr-doped near-infrared long-afterglow luminescent material with perovskite structure and preparation method thereof |
| CN107945690A (en) * | 2017-11-29 | 2018-04-20 | 四川三盛恒业科技有限公司 | A kind of long afterglow self-luminescence public identifier board and preparation method thereof |
| CN108130079A (en) * | 2018-01-24 | 2018-06-08 | 南开大学 | Batch synthetic water disperses the method for small particle overlength near-infrared twilight sunset nano-particle |
| 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 |
| CN108998018A (en) * | 2018-07-16 | 2018-12-14 | 浙江工业大学 | A kind of Cr3+The stanniferous mixing spinelle near-infrared long after glow luminous material and preparation method thereof of doping |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104861970A (en) * | 2015-04-03 | 2015-08-26 | 华南理工大学 | Cr-doped near-infrared long-afterglow luminescent material with perovskite structure and preparation method thereof |
| CN104861970B (en) * | 2015-04-03 | 2016-07-06 | 华南理工大学 | The near-infrared long after glow luminous material of the perovskite structure of a kind of Cr doping and preparation method |
| CN107945690A (en) * | 2017-11-29 | 2018-04-20 | 四川三盛恒业科技有限公司 | A kind of long afterglow self-luminescence public identifier board and preparation method thereof |
| CN108130079A (en) * | 2018-01-24 | 2018-06-08 | 南开大学 | Batch synthetic water disperses the method for small particle overlength near-infrared twilight sunset nano-particle |
| CN108130079B (en) * | 2018-01-24 | 2020-11-06 | 南开大学 | Method for synthesizing water-dispersed small-particle-size ultra-long near-infrared afterglow nanoparticles in batches |
| 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 |
| CN108998018A (en) * | 2018-07-16 | 2018-12-14 | 浙江工业大学 | A kind of Cr3+The stanniferous mixing spinelle near-infrared long after glow luminous material and preparation method thereof of doping |
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|---|---|
| CN103897696B (en) | 2016-05-04 |
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