CN103965898A - Novel fluorescent magnetic nanotube material and preparation method thereof - Google Patents
Novel fluorescent magnetic nanotube material and preparation method thereof Download PDFInfo
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- CN103965898A CN103965898A CN201410185776.5A CN201410185776A CN103965898A CN 103965898 A CN103965898 A CN 103965898A CN 201410185776 A CN201410185776 A CN 201410185776A CN 103965898 A CN103965898 A CN 103965898A
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Abstract
The invention discloses a novel fluorescent magnetic nanotube-ferroferric oxide/polyaniline/carbon quantum dot nanotube and a preparation method thereof. The preparation method comprises the following steps: preparing a ferroferric oxide/polyaniline nanotube in an anodic aluminum oxide template, mixing carton quantum dots with the ferroferric oxide/polyaniline nanotube, and performing heating reflux to obtain the ferroferric oxide/polyaniline/carbon quantum dot nanotube. The novel fluorescent magnetic nanotube synthesized by the method can emit blue, green and red light under the excitation of ultraviolet, blue and green light, is good in multi-color light emission performance, and can be used in the fields of external living cell development, bio-labeling, cell cellular immunity magnetic separation, bio-sensing and the like.
Description
Technical field
The present invention relates to a kind of novel fluorescence magnetic nanotube and preparation method thereof, belong to preparation and the Application Areas thereof of nano composite material.
Background technology
Quantum dot can be described as again semiconductor nanocrystals body, and due to its quantum size effect, particle diameter difference or composition material difference can be launched the fluorescence of different colours, and studying at present more is CdX(X=S, Se, Te).As document S. Tamil Selvan, Pranab K. Patra. et al. Synthesis of Silica-Coated Semiconductor and Magnetic Quantum Dotsand Their Use in the Imaging of Live Cells. Angew. Chem. 2007, the application of the magnetic CdS quantum dot of reporting in 119,2500-2504. in cell developing.In addition, application number is the preparation that 201210125567.2 patent of invention discloses a kind of magnetic fluorescence composite Nano ball, first prepared CdSe quantum dot, then prepared Z 250@silica nanosphere, by Z 250@silica nanosphere is carried out to surface amino groups modification, CdSe quantum dot is loaded to nano grain surface, magnetic fluorescence composite Nano ball has very strong magnetic and excellent fluorescence property, can be used for carrying out organism interior orientation medicament transport and organism fluorescence imaging.What at present research was more is, and that magnetic nanoparticle and CdX quantum dot (X=S, Se, Te) carry out is compound, but the research of not also being combined with carbon quantum dot about magnetic ferroferric oxide nanometer pipe is reported.
Due to the defect on carbon quantum dot surface and the difference of size, along with radiative variation, variation can be sent the light of different colours to exciting light, this be other can only be under specific wavelength the not available advantage of fluorescigenic dyestuff.If carbon quantum dot is combined with organism, can utilize the stability of photoluminescence of carbon quantum dot and wavelength tuning effect to carry out mark to organism.Fluorescent carbon quantum dot is because it has unique luminosity, hypotoxicity, well the feature such as fluorescence lifetime can be used for the aspects such as optical electron device, biomarker, biological developing and enjoy people's concern.Simultaneously magnetic ferroferric oxide has that bio-compatibility is good, saturation magnetization high, is widely used in the aspect such as biomarker, drug targeting.Carbon quantum dot is combined with magnetic Nano material and prepare carbon quantum dot magnetic nanometer composite material, utilize the good biocompatibility of magnetic Nano material and good magnetic property to realize the magnetic induction of carbon quantum dot, capable of circulation, separation and purification etc., also by more extensive the application that makes carbon quantum dot in biomarker imaging, cellular immunization magnetic separate.
Summary of the invention
The invention provides a kind of novel fluorescence magnetic nanotube and preparation method thereof, and the fluorescence magnetic nanotube of preparation has a good multicolor luminous performance.
The invention provides a kind of novel fluorescence magnetic nano-tube material, it is to be coated with load carbon quantum dot on the ferriferrous oxide nano pipe of polyaniline in periphery, thereby the Z 250/polyaniline/carbon quantum dot nano tubular structure material that forms external diameter 150-200 nm, it can send respectively blue light, green glow and ruddiness under the exciting of UV-light, blue light and green glow.
The present invention also provides the preparation method of this novel fluorescence magnetic nano-tube material, and it comprises the steps:
(1) preparation of magnetic ferroferric oxide nanometer pipe: add successively citric acid, urea in iron salt solutions, the pH value of regulator solution is 7.5-8.5, then wide aperture periodicity anodic oxidation aluminium formwork is immersed in above-mentioned solution, under nitrogen protection, be heated to 85-95 degree Celsius and keep 1-3 hour, take out template dry, anneal under argon shield;
(2) preparation of Z 250/polyaniline nanotube: the template after annealing is placed in to the single port flask that fills aniline monomer, vacuumize maintain 20-40 minute after take out, immediately template is put into the ammonium persulphate-aqueous hydrochloric acid of preparation, at 0-1 degree Celsius of lower standing and reacting 1.5-2.5 hour, under normal temperature, continue again reaction 20-30 hour, the template finally obtaining is dissolved to 8-15 minute in NaOH solution, and magnetic separates and obtains Z 250/polyaniline nanotube;
(3) preparation of Z 250/polyaniline/carbon quantum dot nano pipe: get carbon quantum dot powder and be scattered in deionized water; ultrasonic; Z 250/polyaniline nano pipe powder of getting above-mentioned preparation is scattered in solution; under nitrogen protection, be heated to 85-95 degree Celsius of backflow 3-5 hour, magnetic separates and obtains Z 250/polyaniline/carbon quantum dot nano pipe.
Preferably, in the described iron salt solutions of step (1), the mol ratio of divalent iron salt and trivalent iron salt is 1:2, and the mol ratio of molysite and citric acid is 1:1, and the mol ratio of molysite and urea is 1:10.
As preferably, the condition of the described anneal of step (1) is 550 degrees Celsius, 10 hours.
Preferably, the described ammonium persulphate-aqueous hydrochloric acid of step (2) is the mixing solutions of the hydrochloric acid of 3 milligrams every milliliter of the ammonium persulfate solution of 9 milligrams every milliliter of concentration and concentration, and the volume ratio of described ammonium persulfate solution and hydrochloric acid is 1:1.
As preferably, the amount ratio of the described carbon quantum dot of step (3) and Z 250/polyaniline nanotube is 1:10.
The described wide aperture of step (1) the periodically preparation of anodic oxidation aluminium formwork can adopt following method: taking oxalic acid-ethanol system as electrolytic solution, taking high-purity aluminium flake as anode, taking stainless steel plate as negative electrode, depress oxidation in subzero 8 to subzero 4 degrees Celsius, 110-130 voltaism and prepare with aluminium base anodic oxidation aluminium formwork for 4-6 hour, then use saturated SnCl
4-HCl solution is removed the aluminum base layer at the anodic oxidation aluminium formwork back side, removes blocking layer reaming with phosphoric acid solution, obtains the periodically anodic oxidation aluminium formwork of wide aperture of bilateral.
As preferably, above-mentioned wide aperture is periodically in the preparation of anodic oxidation aluminium formwork, and described oxalic acid-ethanol system is oxalic acid solution and the mixing of ethanol, and oxalic acid solution concentration used is 0.3 mole every liter, and the volume ratio of oxalic acid solution and ethanol is 2-4:1; The massfraction of described phosphoric acid solution is 5%-7%, removes the condition on blocking layer and be 65-75 degree Celsius, 6-10 minute for good; Described high-purity aluminium flake is first with high temperature annealing, then is good through chemical rightenning; In electrolytic oxidation reaction, first depress reaction 10 minutes with 40 voltaisms, and then according to the rate of pressure rise of 20 volts of per minutes, voltage is raised to 110-130 voltaism and depresses oxidation 4-6 hour for good.
The invention provides a kind of novel fluorescence magnetic nanotube is Z 250/polyaniline/carbon quantum dot nano pipe and preparation method thereof.First in anodic oxidation aluminium formwork, prepare Z 250/polyaniline nanotube, by carbon quantum dot and the blend of Z 250/polyaniline nanotube, reflux makes Z 250/polyaniline/carbon quantum dot nano pipe (as Fig. 1) on this basis.The novel fluorescence magnetic nanotube that the present invention synthesizes can send respectively blue light, green glow and ruddiness under the exciting of UV-light, blue light and green glow, there is good multicolor luminous performance, can be used for the fields such as external viable cell development, biomarker, the separation of cellular immunization magnetic, bio-sensing.
Brief description of the drawings
Fig. 1 is the side electron scanning micrograph of the fluorescence magnetic nanotube of preparation, and magnification is 30,000 times.In figure, in the upper right corner, illustration is the electron scanning micrograph of the fluorescence magnetic nanotube mouth of pipe of preparation.
Embodiment
Following embodiment is further illustrating using the explaination as to the technology of the present invention content for content of the present invention; but flesh and blood of the present invention is not limited in described in following embodiment, those of ordinary skill in the art can and should know any simple change or replacement based on connotation of the present invention all should belong to protection domain of the presently claimed invention.
embodiment 1
(1) first high-purity aluminium flake is annealed 10 hours under 535 degrees Celsius, then the phosphoric acid that is 85% with massfraction and massfraction are the mixed acid solution (phosphoric acid of 65% nitric acid, concentrated nitric acid, the volume ratio 8:1:1 of distilled water) chemical rightenning 3 minutes under 80 degrees Celsius of water-baths, then taking aluminium flake as anode, stainless steel plate is negative electrode, at subzero 6 degrees Celsius, in the electrolytic solution of 0.3 mole of every liter of oxalic acid solution and ethanol 3:1 preparation by volume, depress reaction 10 minutes at 40 voltaisms, then according to the rate of pressure rise of 20 volts of per minutes, voltage is raised to 120 volts, sustained reaction 5 hours.And then use saturated SnCl
4-HCl solution is removed the aluminum base layer at the porous anodic alumina template back side, and the phosphoric acid solution that is 6% with massfraction, in 70 degrees Celsius of 8 minutes removal blocking layers reaming, obtains the periodically anodic oxidation aluminium formwork of wide aperture of bilateral;
(2) trivalent iron salt of the divalent iron salt of 0.01 mole and 0.02 mole is dissolved in the there-necked flask that fills 40 ml distilled waters, add again the citric acid of 0.03 mole, after dissolving with the pH value of ammoniacal liquor regulator solution to 8.0 left and right, then add the urea of 0.3 mole, abundant stirring and dissolving;
(3) alumina formwork of preparation in (1) is immersed in the solution of (2) preparation, the high pure nitrogen that first passes into 10 minutes is got rid of the air in there-necked flask, and then oil bath is heated to 90 degrees Celsius of maintenances 2 hours.After taking out template, naturally dry, under argon gas atmosphere, anneal 10 hours in 550 degrees Celsius;
(4) template after annealing is placed in to the single port flask that fills aniline monomer, with rotary-vane vaccum pump vacuumize maintain 30 minutes after take out, put into immediately 10 milliliters of ammonium persulphates (concentration is 9 milligrams every milliliter) and 10 milliliters of hydrochloric acid (concentration is 3 milligrams every milliliter) mixed aqueous solution, standing and reacting 2 hours under 0-1 degrees celsius, then under normal temperature, continue reaction 24 hours.The template finally obtaining ultrasonic dissolution 10 minutes in the sodium hydroxide solution of 0.5 mole every liter, the sample that magnetic is separated is dried;
(5) taking the carbon quantum dot powder of 1 milligram is scattered in 50 ml deionized water; after ultrasonic 1 hour; taking dry sample powder in 10 milligrams (4) is scattered in solution again; 90 degrees Celsius of backflows of oil bath heating 4 hours under the protection of nitrogen atmosphere; carry out again magnetic separating treatment, obtain Z 250/polyaniline/carbon quantum dot nano tube material of black powder state.
Claims (10)
1. a novel fluorescence magnetic nano-tube material, it is to be coated with load carbon quantum dot on the ferriferrous oxide nano pipe of polyaniline in periphery, thereby the Z 250/polyaniline/carbon quantum dot nano tubular structure material that forms external diameter 150-200 nm, it can send respectively blue light, green glow and ruddiness under the exciting of UV-light, blue light and green glow.
2. a preparation method for novel fluorescence magnetic nano-tube material described in claim 1, comprises the steps:
(1) preparation of magnetic ferroferric oxide nanometer pipe: add successively citric acid, urea in iron salt solutions, the pH value of regulator solution is 7.5-8.5, then wide aperture periodicity anodic oxidation aluminium formwork is immersed in above-mentioned solution, under nitrogen protection, be heated to 85-95 degree Celsius and keep 1-3 hour, take out template dry, anneal under argon shield;
(2) preparation of Z 250/polyaniline nanotube: the template after annealing is placed in to the single port flask that fills aniline monomer, vacuumize maintain 20-40 minute after take out, immediately template is taken out to ammonium persulphate-aqueous hydrochloric acid of putting into preparation, at 0-1 degree Celsius of lower standing and reacting 1.5-2.5 hour, under normal temperature, continue again reaction 20-30 hour, the template finally obtaining is dissolved to 8-15 minute in sodium hydroxide solution, and magnetic separates and obtains polyaniline/ferriferrous oxide nano pipe;
(3) preparation of Z 250/polyaniline/carbon quantum dot nano pipe: get carbon quantum dot powder and be scattered in deionized water; ultrasonic; Z 250/polyaniline nano pipe powder of getting above-mentioned preparation is scattered in above-mentioned solution; under nitrogen protection, be heated to 85-95 degree Celsius of backflow 3-5 hour, magnetic separates and obtains Z 250/polyaniline/carbon quantum dot nano pipe.
3. the preparation method of novel fluorescence magnetic nano-tube material as claimed in claim 2, it is characterized in that, in the described iron salt solutions of step (1), the mol ratio of divalent iron salt and trivalent iron salt is 1:2, the mol ratio of molysite and citric acid is 1:1, and the mol ratio of molysite and urea is 1:10.
4. the preparation method of novel fluorescence magnetic nano-tube material as claimed in claim 2, is characterized in that, the condition of the described anneal of step (1) is 500-600 degree Celsius, 8-12 hour.
5. the preparation method of novel fluorescence magnetic nano-tube material as claimed in claim 2, it is characterized in that, described ammonium persulphate-the aqueous hydrochloric acid of step (2) is the mixing solutions of the hydrochloric acid of 3 milligrams every milliliter of the ammonium persulfate solution of 9 milligrams every milliliter of concentration and concentration, and the volume ratio of described ammonium persulfate solution and hydrochloric acid is 1:1.
6. the preparation method of novel fluorescence magnetic nano-tube material as claimed in claim 2, is characterized in that, the amount ratio of the described carbon quantum dot of step (3) and Z 250/polyaniline nanotube is 1:10.
7. the preparation method of novel fluorescence magnetic nano-tube material as claimed in claim 2, it is characterized in that, the described wide aperture of step (1) periodically anodic oxidation aluminium formwork is taking oxalic acid-ethanol system as electrolytic solution, taking high-purity aluminium flake as anode, taking stainless steel plate as negative electrode, depress oxidation in subzero 8 to subzero 4 degrees Celsius, 110-130 voltaism and prepare with aluminium base anodic oxidation aluminium formwork for 4-6 hour, then use saturated SnCl
4-HCl solution is removed the aluminum base layer at the anodic oxidation aluminium formwork back side, removes blocking layer reaming with phosphoric acid solution, obtains the periodically anodic oxidation aluminium formwork of wide aperture of bilateral.
8. the preparation method of novel fluorescence magnetic nano-tube material as claimed in claim 7, it is characterized in that, described oxalic acid-ethanol system is oxalic acid solution and the mixing of ethanol, and oxalic acid solution concentration used is 0.3 mole every liter, and the volume ratio of oxalic acid solution and ethanol is 2-4:1.
9. the preparation method of novel fluorescence magnetic nano-tube material as claimed in claim 7, is characterized in that, the massfraction of described phosphoric acid solution is 5%-7%, and the condition of removing blocking layer is 65-75 degree Celsius, 6-10 minute.
10. the preparation method of novel fluorescence magnetic nano-tube material as claimed in claim 7, is characterized in that, described high-purity aluminium flake is first with high temperature annealing, then through chemical rightenning.
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Cited By (6)
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| CN104120481A (en) * | 2014-08-08 | 2014-10-29 | 武汉科技大学 | Pure iron based surface Fe3O4 nano-column array and preparation method thereof |
| CN105860063A (en) * | 2016-05-11 | 2016-08-17 | 安徽大学 | Carbon quantum dot/polyaniline composite nano-tube with super-large aspect ratio and synthesis method thereof |
| CN106350852A (en) * | 2016-09-22 | 2017-01-25 | 宇龙计算机通信科技(深圳)有限公司 | Magnetic aluminum alloy battery cover, processing method and equipment |
| CN107688011A (en) * | 2017-06-28 | 2018-02-13 | 昆明理工大学 | Ofloxacin method in magnetic SPME combination carbon quantum dot fluorescence sensitivity detection milk |
| CN108083344A (en) * | 2017-12-25 | 2018-05-29 | 浙江工业大学 | The method that template-hydro-thermal method prepares ferriferrous oxide nano line |
| CN115569632A (en) * | 2022-09-28 | 2023-01-06 | 扬州工业职业技术学院 | Magnetic activated carbon fiber adsorbent and preparation method thereof |
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| CN102153862A (en) * | 2011-03-14 | 2011-08-17 | 安徽大学 | Preparation method of polyaniline/carbon nano tube compound electromagnetic shielding material |
| EP2584623A2 (en) * | 2011-10-21 | 2013-04-24 | Samsung Electronics Co., Ltd | Semiconductor nanocrystal-polymer composite, method of preparing the same, and composite film and optoelectronic device including the same |
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| CN101723311A (en) * | 2009-11-06 | 2010-06-09 | 武汉理工大学 | Magnetic flourescent nano material for magnetic-photo sensor and preparation method thereof |
| CN102153862A (en) * | 2011-03-14 | 2011-08-17 | 安徽大学 | Preparation method of polyaniline/carbon nano tube compound electromagnetic shielding material |
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| CN104120481A (en) * | 2014-08-08 | 2014-10-29 | 武汉科技大学 | Pure iron based surface Fe3O4 nano-column array and preparation method thereof |
| CN105860063A (en) * | 2016-05-11 | 2016-08-17 | 安徽大学 | Carbon quantum dot/polyaniline composite nano-tube with super-large aspect ratio and synthesis method thereof |
| CN105860063B (en) * | 2016-05-11 | 2018-06-29 | 安徽大学 | Carbon quantum dot/the polyaniline composite nanometer tube and its synthetic method of a kind of super large draw ratio |
| CN106350852A (en) * | 2016-09-22 | 2017-01-25 | 宇龙计算机通信科技(深圳)有限公司 | Magnetic aluminum alloy battery cover, processing method and equipment |
| CN107688011A (en) * | 2017-06-28 | 2018-02-13 | 昆明理工大学 | Ofloxacin method in magnetic SPME combination carbon quantum dot fluorescence sensitivity detection milk |
| CN108083344A (en) * | 2017-12-25 | 2018-05-29 | 浙江工业大学 | The method that template-hydro-thermal method prepares ferriferrous oxide nano line |
| CN115569632A (en) * | 2022-09-28 | 2023-01-06 | 扬州工业职业技术学院 | Magnetic activated carbon fiber adsorbent and preparation method thereof |
| CN115569632B (en) * | 2022-09-28 | 2023-08-25 | 扬州工业职业技术学院 | Magnetic activated carbon fiber adsorbent and preparation method thereof |
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