CN104671280A - Reversible phase transfer method of CdS nanoribbons in oil phase/water phase - Google Patents
Reversible phase transfer method of CdS nanoribbons in oil phase/water phase Download PDFInfo
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- CN104671280A CN104671280A CN201310636559.9A CN201310636559A CN104671280A CN 104671280 A CN104671280 A CN 104671280A CN 201310636559 A CN201310636559 A CN 201310636559A CN 104671280 A CN104671280 A CN 104671280A
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Abstract
The invention discloses a reversible phase transfer method of CdS nanoribbons in an oil phase/water phase, which comprises the following steps: preparing CdS nanoribbons in a water phase, adding cetyl trimethylammonium bromide into the water-phase CdS nanoribbons so that the CdS nanoribbons are transferred from the water solution into chloroform, and adding azobisformamide so that the CdS nanoribbons are water-soluble again, thereby completing one phase transfer cycle. The technical scheme disclosed by the invention can implement reversible phase transfer, and the intensity and wavelength of the emission peak do not obviously change before and after transfer, which indicates that the fluorescence property of the nanoribbons does not obviously change.
Description
Technical field
The invention belongs to field of nanometer technology, more particularly, relate to the method for a kind of CdS nano belt reversible phase transition in oil phase and aqueous phase.
Background technology
Monodimension nanometer material refers to the nano material having bidimensional to be in nanoscale scope (1-100nm) in three dimensions, mainly comprises nano wire, nanometer rod, nano belt and nanotube etc.Because they have unique application in mesoscopic physics and nano-device assembling etc., monodimension nanometer material receives extensive concern (the Wang ZL.Characterizing the structure and properties of individual wire-like nanoentities.Adv.Mater. of people, 2000,12 (17): 1295-1298).In addition, quantum confined effect has impact to the electron-transporting of material, heat conductivity and mechanical property, monodimension nanometer material is ideal system (the Xia YN studying this influence, Yang PD, Sun YG, et al.One-dimensional nanostructures:synthesis, characterization, and applications.Adv.Mater., 2003,15 (5): 353-389).As a kind of important monodimension nanometer material, semiconductor nano-strip can represent a large class and be used for " the nanometer building blocks " of assemble nanometer functional device (as chemical sensor, field-effect transistor etc.).It should be noted that, semiconductor nano-strip has the square-section of regular geometry and high degree of crystallinity, this makes them and nano wire and hollow nanotube have obvious difference (Gao T, Li QH, Wang TH.CdS nanobelts as photoconductors.Appl.Phys.Lett., 2005,86 (17): 173105).
CdS is a kind of important II-VI group semiconductor compound, and under normal temperature, (300K) its energy bandwidth be 2.4eV.CdS nano belt has unique application in mesoscopic physics and nano-device assembling etc., such as device for non-linear optical, flat-panel screens, photodiode, laser, logical gate and transistor etc.Simultaneously, CdS is also a kind of well optical wavelength material and electroluminescent laserable material, be widely used in fields such as telecommunications, data storage and near field optic photoetching (Zhai TY, Fang XS, Liang L, et al.One-dimensional CdS nanostructures:synthesis, properties, and applications.Nanoscale, 2010,2 (2): 168-187).
But CdS nano belt often will be dispersed in different solvents and just can apply.Such as, in biological imaging, nanocrystallinely need water-soluble, and in photovoltaic applications, nanocrystallinely should be dissolved in common organic solvents.The best approach addressed this problem is exactly make nanocrystallinely between polar solvent and non-polar solvent, to realize reversible phase transition, and do not change nanocrystalline fluorescent characteristic, and the key of phase transition be to nanocrystalline carry out surface-functionalized to regulate the water-soluble of nanocrystal surface part or oil soluble.Ligand exchange is the phase transfer method often used, use ligand exchange can realize multiple nanocrystalline (metal, semi-conductor etc.) transfer from aqueous phase to oil phase or from oil phase to aqueous phase (Dubertret B, SkouridesP, NorrisDJ, et al.In vivo imaging of quantum dots encapsulated in phospholipid micelles.Science, 2002,298 (5599): 1759-1762).But these methods, owing to carrying out irreversible surface-functionalized to nanocrystalline, can only realize nanocrystalline unidirectional transfer between aqueous phase and oil phase usually.Therefore, under the condition not changing CdS nano belt character, reversible phase transition is carried out to it and just seems particularly important.
Summary of the invention
Technical purpose of the present invention is to overcome the deficiencies in the prior art, provides a kind of method that can allow CdS quantum dot assembly that reversible phase transition occurs in aqueous phase and oil phase.
Technical purpose of the present invention is achieved by following technical proposals:
A method for CdS nano belt reversible phase transition in oil phase and aqueous phase, carry out according to following step:
Step 1, prepares CdS nano belt in aqueous phase, specifically: by CdC1
22.5H
2o and TGA is dissolved in 100mL ultrapure water for 1:1.5 in molar ratio, and mixing solutions concentration is that to be adjusted to pH value be 11.5 to 1MNaOH, then pours in the there-necked flask of 100mL by gained solution, and logical argon gas 30min under stirring at room temperature, to remove the oxygen dissolved in solution.Under the condition of isolated air, by the KHS solution of 3mL, be injected into fast in there-necked flask.Then mixing solutions is heated to backflow, back flow reaction 8h under magnetic agitation, can obtain CdS nanoparticle.Gained quantum dot solution is mixed with 350mL ethanol, after leaving standstill, in solution, produces precipitation, then centrifugal, outwell supernatant liquor, retain precipitation, precipitation is dissolved in again in the NaOH aqueous solution, leave standstill, self-assembly is formed water miscible polycrystalline CdS nano belt by the nanoparticle in solution.
Step 2, cetyl trimethylammonium bromide (CTAB) is added in aqueous phase CdS nano belt, move on to chloroform (oil phase) to make CdS nano belt from Transfer in Aqueous Solution, namely after adding cetyl trimethylammonium bromide, CTAB molecular adsorption is to nano belt surface, long alkane chain makes nano belt have oil soluble, transfer in oil phase to realize nano belt, specifically: in a clean bottle, cetyl trimethylammonium bromide (CTAB) is dissolved in chloroformic solution, be configured to CTAB homogeneous solution, then in bottle, the CdS nano belt aqueous solution is added, to demixing phenomenon be there is in solution, layering solution is placed on lucifuge place, leave standstill 8-10h, water-soluble CdS nano belt can be transferred in chloroformic solution completely gradually and go.
Step 3, Cellmic C 121 is added in oil phase (chloroform) solution of CdS nano belt, CdS nano belt is had again water-soluble, realize the transfer to aqueous phase, namely because the amide group in Cellmic C 121 molecule is easier than CdS nano belt and CTAB molecule combines, so, CTAB molecule splits away off from nano belt surface and combines with Cellmic C 121 molecule, again recover water-soluble to make CdS nano belt, specifically: select mass ratio to be that the capric acid (DA) of 1:1 and Tetramethylammonium hydroxide (TMAH) are dissolved in 2mL methyl alcohol and form Cellmic C 121 (TMAD), as the transfer agent of aqueous phase countertransference, join in oil phase (chloroform) solution of CdS nano belt, mixing solutions is jiggled, then leave standstill, oil-soluble CdS nano belt can be transferred to gradually in aqueous phase in 90min.
Repeat above-mentioned steps 2-3 and can realize to the greatest extent the reversible phase transition of CdS nano belt in aqueous phase and oil phase, and keep substantially identical character, do not change.The scanning electronic microscope utilizing model to be S-4800 carries out morphology characterization, and the diameter analyzing known CdS nano belt nano belt in aqueous phase and oil phase is probably 100nm, and after transferring to oil phase, nano belt becomes soft.The fluorogram of the CdS nano belt using the fluorescence protractor that model is F-4600 to measure, in figure 1 be for transfer before the emission peak of aqueous phase CdS nano belt, 2 for transferring to the emission peak after oil phase, 3 for transfer to the emission peak after aqueous phase from oil phase, as can be seen from the figure, all there is not obvious change in intensity and the wavelength of transfer front and back emission peak, this illustrates that the photoluminescent property of nano belt too large change does not occur.Utilize technical scheme of the present invention to realize reversible phase transition, all there is not obvious change in intensity and the wavelength of transfer front and back emission peak, illustrates that the photoluminescent property of nano belt considerable change does not occur.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that CdS nano belt shifts from aqueous phase to oil phase.
Fig. 2 is that CdS nano belt transfers to the schematic diagram of aqueous phase from oil phase.
Fig. 3 is the fluorogram of CdS nano belt, in figure 1 be for transfer before the emission peak of aqueous phase CdS nano belt, 2 for transferring to the emission peak of CdS nano belt after oil phase, and 3 is the emission peak of CdS nano belt after transferring to aqueous phase from oil phase.
Fig. 4 is the stereoscan photograph of CdS nano belt in aqueous phase (SEM).
Fig. 5 is the stereoscan photograph of CdS nano belt in oil phase (SEM).
Embodiment
Technical scheme of the present invention is further illustrated below in conjunction with specific embodiment.
CdS nano belt is prepared, specifically: by CdC1 in aqueous phase
22.5H
2o and TGA is dissolved in 100mL ultrapure water for 1:1.5 in molar ratio, and mixing solutions concentration is that to be adjusted to pH value be 11.5 to 1MNaOH, then pours in the there-necked flask of 100mL by gained solution, and logical argon gas 30min under stirring at room temperature, to remove the oxygen dissolved in solution.Under the condition of isolated air, by the KHS solution of 3mL, be injected into fast in there-necked flask.Then mixing solutions is heated to backflow, back flow reaction 8h under magnetic agitation, can obtain CdS nanoparticle.Gained quantum dot solution is mixed with 350mL ethanol, after leaving standstill, in solution, produces precipitation, then centrifugal, outwell supernatant liquor, retain precipitation, precipitation is dissolved in again in the NaOH aqueous solution, leave standstill, self-assembly is formed water miscible polycrystalline CdS nano belt by the nanoparticle in solution.
Embodiment 1
In a clean bottle, 10mg cetyl trimethylammonium bromide (CTAB) is dissolved in the chloroformic solution of 4mL, be configured to CTAB homogeneous solution, then in bottle, the 2mLCdS nano belt aqueous solution is added, to demixing phenomenon be there is in solution, layering solution is placed on lucifuge place, leave standstill 8-10h, water-soluble CdS nano belt can be transferred in chloroformic solution completely gradually and go.By 34mgDA with 34mg(Tetramethylammonium hydroxide) TMAH is dissolved in shape (4 bromide) in 2mL methyl alcohol and becomes TMAD, as the transfer agent of aqueous phase countertransference, 2mL water and 1mLTMAD solution is added in the bottle that oil soluble CdS nano belt is housed, mixing solutions is jiggled, then leave standstill, oil-soluble CdS nano belt can be transferred to gradually in aqueous phase in 90min.
Embodiment 2
In a clean bottle, 12mgCTAB is dissolved in the chloroformic solution of 4mL, be configured to CTAB homogeneous solution, then in bottle, the 2.5mLCdS nano belt aqueous solution is added, to demixing phenomenon be there is in solution, layering solution is placed on lucifuge place, leave standstill 8-10h, water-soluble CdS nano belt can be transferred in chloroformic solution completely gradually and go.34mgDA and 34mgTMAH is dissolved in 2mL methyl alcohol and forms TMAD, as the transfer agent of aqueous phase countertransference, 2mL water and 1mLTMAD solution is added in the bottle that oil soluble CdS nano belt is housed, mixing solutions is jiggled, then leave standstill, oil-soluble CdS nano belt can be transferred to gradually in aqueous phase in 90min.
Embodiment 3
In a clean bottle, 8.5mgCTAB is dissolved in the chloroformic solution of 4mL, be configured to CTAB homogeneous solution, then in bottle, the 3mLCdS nano belt aqueous solution is added, to demixing phenomenon be there is in solution, layering solution is placed on lucifuge place, leave standstill 8-10h, water-soluble CdS nano belt can be transferred in chloroformic solution completely gradually and go.28mgDA and 28mgTMAH is dissolved in 2mL methyl alcohol and forms TMAD, as the transfer agent of aqueous phase countertransference, 2mL water and 1mLTMAD solution is added in the bottle that oil soluble CdS nano belt is housed, mixing solutions is jiggled, then leave standstill, oil-soluble CdS nano belt can be transferred to gradually in aqueous phase in 90min.
Above to invention has been exemplary description; should be noted that; when not departing from core of the present invention, any simple distortion, amendment or other those skilled in the art can not spend the equivalent replacement of creative work all to fall into protection scope of the present invention.
Claims (5)
1. the method for CdS nano belt reversible phase transition in oil phase and aqueous phase, it is characterized in that, carry out according to following step: in aqueous phase CdS nano belt, add cetyl trimethylammonium bromide, move on to oil phase to make CdS nano belt from Transfer in Aqueous Solution, Cellmic C 121 is added in the oil-phase solution of CdS nano belt, CdS nano belt is had again water-soluble, realize the transfer to aqueous phase.
2. the method for a kind of CdS nano belt according to claim 1 reversible phase transition in oil phase and aqueous phase, is characterized in that, described oil phase is chloroform.
3. the method for a kind of CdS nano belt according to claim 1 reversible phase transition in oil phase and aqueous phase, it is characterized in that, mass ratio is selected to be that the capric acid of 1:1 and Tetramethylammonium hydroxide are dissolved in methyl alcohol and form Cellmic C 121, as the transfer agent of aqueous phase countertransference, join in the oil-phase solution of CdS nano belt.
4. the method for a kind of CdS nano belt according to claim 1 reversible phase transition in oil phase and aqueous phase, is characterized in that, prepare CdS nano belt, by CdC1 in aqueous phase
22.5H
2o and TGA is dissolved in 100mL ultrapure water for 1:1.5 in molar ratio, and mixing solutions concentration is that to be adjusted to pH value be 11.5 to 1MNaOH, then pours in the there-necked flask of 100mL by gained solution, and logical argon gas 30min under stirring at room temperature, to remove the oxygen dissolved in solution.Under the condition of isolated air, by the KHS solution of 3mL, be injected into fast in there-necked flask.Then mixing solutions is heated to backflow, back flow reaction 8h under magnetic agitation, can obtain CdS nanoparticle.Gained quantum dot solution is mixed with 350mL ethanol, after leaving standstill, in solution, produces precipitation, then centrifugal, outwell supernatant liquor, retain precipitation, precipitation is dissolved in again in the NaOH aqueous solution, leave standstill, self-assembly is formed water miscible polycrystalline CdS nano belt by the nanoparticle in solution.
5. the method for a kind of CdS nano belt according to claim 1 reversible phase transition in oil phase and aqueous phase, it is characterized in that, repeat in aqueous phase, to add cetyl trimethylammonium bromide, in oil phase, add the step of Cellmic C 121, realize the repeatedly reversible phase transition in oil phase and aqueous phase of CdS nano belt, and CdS nano belt character remains unchanged substantially.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105602544A (en) * | 2015-12-24 | 2016-05-25 | 北京北达聚邦科技有限公司 | Preparation method for converting aqueous phase quantum dots into oil phase quantum dots |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7824653B2 (en) * | 2004-05-24 | 2010-11-02 | Drexel University | Water soluble quantum dots |
| CN102557113A (en) * | 2011-12-21 | 2012-07-11 | 天津大学 | Water-soluble CdS one-dimensional semiconductor nanobelt and preparation method of water-soluble CdS one-dimensional semiconductor nanobelt |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7824653B2 (en) * | 2004-05-24 | 2010-11-02 | Drexel University | Water soluble quantum dots |
| CN102557113A (en) * | 2011-12-21 | 2012-07-11 | 天津大学 | Water-soluble CdS one-dimensional semiconductor nanobelt and preparation method of water-soluble CdS one-dimensional semiconductor nanobelt |
Non-Patent Citations (1)
| Title |
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| YIFENG WEI ET AL.: ""Reversible phase transfer of quantum dots and metal nanoparticles"", 《THE ROYAL SOCIETY OF CHEMISTRY 2010》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105602544A (en) * | 2015-12-24 | 2016-05-25 | 北京北达聚邦科技有限公司 | Preparation method for converting aqueous phase quantum dots into oil phase quantum dots |
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Application publication date: 20150603 |