CN103897696B - Nm near-infrared long-afterglow material of a kind of Cr doping and preparation method thereof - Google Patents
Nm near-infrared long-afterglow material of a kind of Cr doping and preparation method thereof Download PDFInfo
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- CN103897696B CN103897696B CN201410127225.3A CN201410127225A CN103897696B CN 103897696 B CN103897696 B CN 103897696B CN 201410127225 A CN201410127225 A CN 201410127225A CN 103897696 B CN103897696 B CN 103897696B
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Abstract
The nm near-infrared long-afterglow material that the invention discloses a kind of Cr doping, matrix material is Zn(2-x)Al2xSn(1-x)O4, 0≤x≤0.1; Doping ion Cr3+For active ions, wherein Cr3+Doping be 0.01mol%～0.05mol%. The invention also discloses the preparation method of the nm near-infrared long-afterglow material of above-mentioned Cr doping. Nm near-infrared long-afterglow material particle prepared by the present invention be less than 100 nanometers and monodispersity good, excellent in uniformity, particle is after high temperature 1000 is spent above high temperature sintering, still can not reunite, granule stability is good, and be greater than 150 hours persistence, can be good at being applied to bio-imaging field, and with low cost.
Description
Technical field
The present invention relates to infrared long-persistence nano material, particularly more than a kind of nm near-infrared length of Cr dopingBrightness material 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 researchPersonnel wish directly to observe at live body or the esoteric physiology biological process of toy. LightStudy picture using photon as information source, represented a field of extending fast and be applied directly to pharmacology,Molecular cytobiology and diagnostics. But still there are many limitation in this technology, especially in vivoWhat when illumination, produce organizes autofluorescence and weak tissue permeability under shortwave exciting light irradiates. In order to overcomeThese difficulties, scientist has studied a series of phosphors, and utilizing emitted light is near infrared region (NIR), molecular emission near infrared light (700～1000nm), can be for living body molecule targetSurvey because organism blood be organized in this wave-length coverage in relative transparent, thereby reduced in bodyThe difficult problem that ambient interferences causes. Therefore there are many researchers to propose to replace with near infrared long-afterglow materialGeneration common fluorescent material, excite in vitro thereby realize, be expelled in body after twilight sunset can be used for doing lifeThe fluorescence labeling of thing. And with respect to other imaging marker material, long-afterglow material is in order to glimmering as biologyThe unique advantage of signal material is can be in order to observe the diffusion of marker material, and this is other any marksNote material is not available. The near-infrared long-afterglow material of latest developments also only limits to high temperature solid-phase sintering,Be can be prepared into nano level long-afterglow material also inevitably will run into raw material costliness, be unfavorable for pushing awayExtensively, the more impossible problem that is applied to production practices. We also find existing preparation nanometer long afterglow simultaneouslyMaterial all inevitably will run into the problem that high temperature sintering causes nano particle to increase, and therefore wants furtherAdvance the application of near-infrared long-afterglow material in bio-imaging, be necessary very much to develop improved technology of preparingDevelop 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 Cr dopingNm near-infrared long-afterglow material, 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, and twilight sunsetTime is greater than 150 hours, can be good at being applied to bio-imaging field, and with low cost.
Another object of the present invention is to the preparation side of the nm near-infrared long-afterglow material that above-mentioned Cr doping is providedMethod.
Object of the present invention is achieved through the following technical solutions:
A nm near-infrared long-afterglow material for Cr doping, matrix material is Zn(2-x)Al2xSn(1-x)O4，0≤x≤0.1; Doping ion Cr3+For active ions, wherein Cr3+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, stannic chloride, chromic nitrate is raw material, takes raw material and adds water and wineIn the mixed solution of essence, at room temperature stir after 10～30 minutes and add acetylacetone,2,4-pentanedione, at room temperature stir 0.5～2Hour obtain mixed liquor, wherein the pH value of mixed liquor is controlled at 2～4;
(2) mixed liquor step (1) being obtained is put into the oven drying 24～48h of 70～90 DEG C, is wetGel;
(3) mixed solution of n-butanol and alcohol is joined in the wet gel that step (2) obtains, be put intoIn the oil bath pan of 60～80 DEG C, react 1～2h, be warmed up to subsequently 90～100 DEG C of reactions 1～2 hour, treat in beakerLiquid complete reaction after, by temperature increase to 120～150 DEG C reaction 5～20 minutes, obtain after dry dry solidifyingGlue;
(4) xerogel that step (3) obtains is transferred in crucible after grinding, 1200～1300 DEG C meltIn stove, burn 2～4h, obtain powder;
(5) powder step (4) being obtained packs centrifuge tube into, carries out centrifugal treating after ultrasonic processing,To the nm near-infrared long-afterglow material of Cr doping.
The mol ratio of the metal ion total amount in the described acetylacetone,2,4-pentanedione of step (1) and mixed liquor is 1:1.
In the mixed solution of the described water of step (1) and alcohol, the volume ratio of water and alcohol is=1:0.5～1:1.
In the mixed solution of the described n-butanol of step (3) and alcohol, the volume ratio of n-butanol and alcohol is2:8～3:7。
Step (5) centrifugal treating, is specially: taking rotating speed as 6000 revs/min, and centrifugal 7～12min, alcoholWash 3～5 times, wash 3～5 times, afterwards leave standstill after 48～72 hours taking rotating speed as 10000 revs/min centrifugal10～20min。
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) invention adopts zinc acetate, aluminum nitrate, stannic chloride, chromic nitrate, acetylacetone,2,4-pentanedione, alcohol, n-butanolFor raw material, with low cost, be easy to megatechnics and promote.
(2) the nm near-infrared long-afterglow material that the present invention prepares, particle is less than 100 nanometers and listFavorable dispersibility, excellent in uniformity, particle, after high temperature 1000 is spent above high temperature sintering, still can not be reunited,Granule stability is good, excellent in uniformity, and this is a kind of huge dashing forward in the preparation of long-persistence nano materialBroken, and be greater than 150 hours persistence, can be good at being applied to bio-imaging field.
Brief description of the drawings
Fig. 1 is the fluorescence spectrum of the nm near-infrared long-afterglow material prepared of embodiments of the invention 1 and excitesSpectrum.
Fig. 2 is the long-persistence luminous decay of the nm near-infrared long-afterglow material prepared of embodiments of the invention 1Spectrum.
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 of the nm near-infrared long-afterglow material prepared of embodiments of the invention 2Spectrum.
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 of the nm near-infrared long-afterglow material prepared of embodiments of the invention 3Spectrum.
Fig. 7 is the scanning electron microscope (SEM) photograph of the nm near-infrared long-afterglow material prepared of embodiments of the invention 3.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are notBe limited to this.
Embodiment 1
The nm near-infrared long-afterglow material of the Cr doping of the present embodiment, matrix material isZn(2-x)Al2xSn(1-x)O4, x=0.01; Doping ion Cr3+For active ions, wherein Cr3+Doping be0.01mol%。
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, stannic chloride, chromic nitrate is raw material, takes raw material and adds 20g waterIn the mixed solution of alcohol, at room temperature stir after 30 minutes and add acetylacetone,2,4-pentanedione, at room temperature stir 1Hour obtain mixed liquor, wherein the pH value of mixed liquor is controlled at 2; Wherein, in acetylacetone,2,4-pentanedione and mixed liquorThe mol ratio of metal ion total amount be 1:1; In the mixed solution of described water and alcohol, the volume of water and alcoholThan being=1:1;
(2) mixed solution step (1) being obtained is put into the oven drying 24h of 80 DEG C, obtains wet gel;
(3) mixed solution of 20g n-butanol 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, treat that the liquid in beaker is completeAfter full response, by temperature increase to 150 DEG C reaction 5～20 minutes, after being dried, obtain xerogel; Described positive fourthIn the mixed solution of alcohol and alcohol, the volume ratio of n-butanol and alcohol is 3:7;
(4) xerogel that step (3) obtains is transferred in crucible after grinding, in the smelting furnace of 1200 DEG CBurn 2h, obtain powder;
(5) powder step (4) being obtained packs centrifuge tube into, and by ultrasonic 30min, 6000 leave the heart10min, alcohol is washed 3 times, wash 3 times, afterwards leave standstill after 48 hours taking rotating speed as 10000 revs/min centrifugal10min separates bulky grain with granule, can obtain particle and be less than 100 nanometers, single good dispersionNano particle.
The fluorescence spectrum of the nm near-infrared long-afterglow material of Cr doping prepared by the present embodiment is aobvious as shown in Figure 1Show, under 280nm excites, sent the luminous of 698nm, the luminous correspondence of 698nm 4 excitation peaks,Respectively 290nm, 320nm, 400nm, 515nm. Fig. 2 has shown Cr doping prepared by the present embodimentNm near-infrared long-afterglow material irradiates after 10 minutes under sunshine, and stop exciting latter 150 hours more thanBrightness attenuation. Fig. 3 is the ESEM of the nm near-infrared long-afterglow material of the Cr doping prepared of the present inventionFigure, has shown that the nm near-infrared long-afterglow material particle of Cr doping prepared by the present invention is less than 100 nanometers,And favorable dispersibility, the pattern of single nano particle is visible, although passed through the high temperature burning of 1200 degrees CelsiusKnot, but dispersed well nano particle still can be obtained, make this material can be good at applicationIn bio-imaging.
Embodiment 2
The nm near-infrared long-afterglow material of the Cr doping of the present embodiment, matrix material isZn(2-x)Al2xSn(1-x)O4, x=0.1; Doping ion Cr3+For active ions, wherein Cr3+Doping be0.05mol%。
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, stannic chloride, chromic nitrate is raw material, takes raw material and adds 20g waterIn the mixed solution of alcohol, at room temperature stir after 10 minutes and add acetylacetone,2,4-pentanedione, at room temperature stir 1Hour obtain mixed liquor, wherein the pH value of mixed liquor is controlled at 4; Wherein, in acetylacetone,2,4-pentanedione and mixed liquorThe mol ratio of metal ion total amount be 1:1; In the mixed solution of described water and alcohol, the volume of water and alcoholThan being=1:0.5;
(2) mixed solution step (1) being obtained is put into the oven drying 24h of 70 DEG C, obtains wet gel;
(3) mixed solution of 20g n-butanol 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, treat that the liquid in beaker is completeAfter full response, by temperature increase to 120 DEG C reaction 20 minutes, obtain after being put into 150 DEG C of oven drying 24hXerogel; In the mixed solution of described n-butanol and alcohol, the volume ratio of n-butanol and alcohol is 2:8;
(4) xerogel that step (3) obtains is transferred in crucible after grinding, in the smelting furnace of 1300 DEG CBurn 2h, obtain powder;
(5) powder step (4) being obtained packs centrifuge tube into, and by ultrasonic 30min, 6000 leave the heart10min, alcohol is washed 3 times, wash 3 times, afterwards leave standstill after 48 hours taking rotating speed as 10000 revs/min centrifugal10min separates bulky grain with granule, can obtain particle and be less than 100 nanometers, single good dispersionNano particle.
Fig. 4 has shown that the nm near-infrared long-afterglow material of Cr doping prepared by the present embodiment shines under sunshinePenetrate after 10 minutes, and stop exciting the decay of afterglow situation of latter 150 hours. Fig. 5 is Cr prepared by the present inventionThe scanning electron microscope (SEM) photograph of nm near-infrared long-afterglow material of doping, has shown receiving of Cr doping prepared by the present inventionRice near-infrared long-afterglow material particle is less than 100 nanometers, and favorable dispersibility, the shape of single nano particleLooks are visible, although passed through the high temperature sintering of 1300 degrees Celsius, still can obtain well dispersedNano particle, makes 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, matrix material isZn(2-x)Al2xSn(1-x)O4, x=0; Doping ion Cr3+For active ions, wherein Cr3+Doping be0.01mol%。
The nm near-infrared long-afterglow material preparation method of the Cr doping of the present embodiment is as follows:
(1) with zinc acetate, stannic chloride, chromic nitrate is raw material, takes raw material and adds 20g water and alcoholIn mixed solution, at room temperature stir after 30 minutes and add acetylacetone,2,4-pentanedione, at room temperature stir and obtain for 1 hourMixed liquor, wherein the pH value of mixed liquor is controlled at 4; Wherein, the metal in acetylacetone,2,4-pentanedione and mixed liquor fromThe mol ratio of sub-total amount is 1:1; In the mixed solution of described water and alcohol, the volume ratio of water and alcohol is=1:1;
(2) mixed solution step (1) being obtained is put into the oven drying 24h of 90 DEG C, obtains wet gel;
(3) mixed solution of 20g n-butanol 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, treat the liquid in beakerAfter complete reaction, by temperature increase to 150 DEG C reaction 5 minutes, after being dried, obtain xerogel; Described n-butanolIn the mixed solution of alcohol, the volume ratio of n-butanol and alcohol is 2:8;
(4) xerogel that step (3) obtains is transferred in crucible after grinding, in the smelting furnace of 1200 DEG CBurn 4h, obtain powder;
(5) powder step (4) being obtained packs centrifuge tube into, and by ultrasonic 30min, 6000 leave the heart10min, alcohol is washed 5 times, wash 5 times, afterwards leave standstill after 72 hours taking rotating speed as 10000 revs/min centrifugal20min separates bulky grain with granule, can obtain particle and be less than 100 nanometers, single good dispersionNano particle.
Fig. 6 has shown that the nm near-infrared long-afterglow material of Cr doping prepared by the present embodiment shines under sunshinePenetrate after 10 minutes, and stop exciting the decay of afterglow situation of latter 150 hours. Fig. 7 is Cr prepared by the present inventionThe scanning electron microscope (SEM) photograph of nm near-infrared long-afterglow material of doping, has shown that material granule prepared by the present invention is littleIn 100 nanometers, and favorable dispersibility, the pattern of single nano particle is visible, takes the photograph although passed through 1200The high temperature sintering of family name's degree, but dispersed well nano particle still can be obtained, make this material energyEnough being well applied in bio-imaging.
Above-described embodiment is preferably embodiment of the present invention, but embodiments of the present invention are not subject to described realityExecute routine restriction, other any do not deviate from the change done under Spirit Essence of the present invention and principle, modification,Substitute, combine, 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, matrix material isZn(2-x)Al2xSn(1-x)O4, 0≤x≤0.1; Doping ion Cr3+For active ions, wherein Cr3+Doping be0.01mol％～0.05mol％。
2. the preparation method of the nm near-infrared long-afterglow material of Cr doping described in claim 1, its featureBe, comprise the following steps:
(1) with zinc acetate, aluminum nitrate, stannic chloride, chromic nitrate is raw material, takes raw material and adds water and wineIn the mixed solution of essence, at room temperature stir after 10～30 minutes and add acetylacetone,2,4-pentanedione, at room temperature stir 0.5～2Hour obtain mixed liquor, wherein the pH value of mixed liquor is controlled at 2～4;
(2) mixed liquor step (1) being obtained is put into the oven drying 24～48h of 70～90 DEG C, is wetGel;
(3) mixed solution of n-butanol and alcohol is joined in the wet gel that step (2) obtains, be put intoIn the oil bath pan of 60～80 DEG C, react 1～2h, be warmed up to subsequently 90～100 DEG C of reactions 1～2 hour, treat in beakerLiquid complete reaction after, by temperature increase to 120～150 DEG C reaction 5～20 minutes, obtain after dry dry solidifyingGlue;
(4) xerogel that step (3) obtains is transferred in crucible after grinding, 1200～1300 DEG C meltIn stove, burn 2～4h, obtain powder;
(5) powder step (4) being obtained packs centrifuge tube into, carries out centrifugal treating after ultrasonic processing,To 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,It is characterized in that, the mol ratio of the metal ion total amount in the described acetylacetone,2,4-pentanedione of step (1) and mixed liquor is 1:1.
4. the preparation method of the nm near-infrared long-afterglow material of Cr doping according to claim 2,It is characterized in that, in the mixed solution of the described water of step (1) and alcohol, the volume ratio of water and alcohol is1:0.5～1:1。
5. the preparation method of the nm near-infrared long-afterglow material of Cr doping according to claim 2,It is characterized in that, in the mixed solution of the described n-butanol of step (3) and alcohol, the volume of n-butanol and alcoholThan being 2:8～3:7.
6. the preparation method of the nm near-infrared long-afterglow material of Cr doping according to claim 2,It 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 Zhi Houjing 3～5 timesPut after 48～72 hours taking rotating speed as 10000 revs/min of centrifugal 10～20min.
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| 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 |
| CN107945690B (en) * | 2017-11-29 | 2020-03-06 | 四川三盛恒业科技有限公司 | Long-afterglow self-luminous public signboard and manufacturing method thereof |
| 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 |
| 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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