CN103848404A - Method for preparing monolayer self-assembling structure of nanorods - Google Patents
Method for preparing monolayer self-assembling structure of nanorods Download PDFInfo
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- CN103848404A CN103848404A CN201410020328.XA CN201410020328A CN103848404A CN 103848404 A CN103848404 A CN 103848404A CN 201410020328 A CN201410020328 A CN 201410020328A CN 103848404 A CN103848404 A CN 103848404A
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Abstract
The invention relates to a method for preparing monolayer self-assembling structure of nanorods, and in particular relates to a method for preparing a monolayer self-assembling structure of CdSe@Cds nanorods. The method comprises the following steps: smearing a CdSe@Cds nanorod solution onto a copper screen which is wrapped with a carbon film and used for a transmission electron microscopy for observation through a dripping and smearing method; and then performing the self-assembling of the CdSe@Cds nanorods on a carbon film substrate by a thermal annealing technology. Compared with the other self-assembling methods, the self-assembling method in a thermal annealing manner is simple in process and does not require complicated supplementary instruments such as a template and the like, thereby being suitable for large-scale preparation of superlattice structures; and more importantly, the method can be used for partially removing organic insulating molecules wrapping the surfaces of the nanorods so as to improve the electric conductivity of the nanorods. The method has the advantages that the method is novel, simple, low in cost and simple to operate; and the defect in the prior art that the large-scale preparation of the nanorods with self-assembled monolayers is not realized is overcome, so that the method has a good application prospect in the field of nanocrystalline photoelectric devices.
Description
Technical field
The invention belongs to the technical field of novel nano-material self-assembling method, relate in particular to the construction process of monodimension nanometer material self-assembled structures.
Background technology
Nano material, with its distinctive volume effect, surface effects, quantum size effect and tunnel effect, makes nano material have potential using value in fields such as optics, electricity, materialogy and biomedicines.Along with the development of nanoscale science and technology and the continuous crossing research of utilisation technology, nano material is assembled into have the superlattice of ad hoc structure or realize it with certain form and is specifically orientated, thereby realize the control of size to nano material, size-grade distribution, assembling dimension, effective means are provided for promoting nano material in the application aspect photoelectric device, self-assembling technique becomes the problem of the primary study developing in current nanosecond science and technology field, is also dominating in following nano materials research field.
Wherein, become one of the study hotspot in this field in recent years for the implementation method of the controlled self-assembly of monodimension nano stick, more common self-assembling method has the slow method of evaporation of solvent (Nano.Lett.2006,6,2066; Nano.Lett.2006,6,1479); Electric field revulsion (Nano.Lett.2007,7,2480; J.Am.Chem.Soc.2004,126,12984); Template (J.Am.Chem.Soc.2006,128,3898; Appl.Phy.Lett.2004,84,3376); Langmuir-Blodgett method (Acc.Chem.Res.2008,41,1662; Nature.Nanotech.2010,5,15) and solubleness adjustment method (Nano.Lett.2009,9,3077) etc.
Although these methods have its advantage, these self-assembling techniques need auxiliary instrument and technology, preparation process complexity conventionally, are difficult to be widely used in the application that requires low cost, efficient nano photoelectric device; In addition, these methods can not be removed and cover nanocrystal organic coordination molecule around, even can in the process of self-assembly, introduce more organic coordination molecule.As everyone knows, the insulation characterisitic of such organic coordination molecule has seriously hindered the electric charge transmission of current carrier, has limited the application of nanocrystalline material in photoelectric device.
Therefore, the challenge of the photovoltaic device based on nanocrystal will be removed these organic insulation molecules exactly, further shortens the distance between nanometer rod.The method of exploring the new relatively easy nanometer rod self-assembly of development is still necessary.The present invention adopts comparatively easy self-assembling technique, can not need step and supplementary instrument complicated in other self-assembling method, thereby further simplify operation steps, the present invention has simple and practical feature, for preparing fast, efficiently, at low cost nanocrystalline functional device provides new scheme on a large scale, fill up the sky of this area certainly.
Summary of the invention
The object of the invention is to overcome deficiency of the prior art, provide a kind of fast, program is easy, preparation cost is low, can prepare on a large scale the method for CdSe@CdS nanometer rod individual layer self-assembled structures.
For achieving the above object, the preparation method of described CdSe@CdS nanometer rod individual layer self-assembly realizes by following steps: the preparation of (1) CdSe@CdS nanometer rod; (2) cleaning of CdSe@CdS nanometer rod solution and concentration regulation and control; (3) preparation of CdSe@CdS nano-rod film; (4) preparation of CdSe@CdS nanometer rod self-assembled structures.
(1) preparation of CdSe@CdS nanometer rod: the synthetic of CdSe@CdS nanometer rod is to adopt document (Nano.Lett.2007,7,2951; Nano.Lett.2007,7,2942) described seed mediated growth method.Adopt trioctylphosphine oxide (TOPO) (TOPO) and tri octyl phosphine (TOP) as solvent, take octyl phosphonic acid (ODPA) and hexyl phosphonic acids (HPA) as part.First will fill TOPO, the there-necked flask of ODPA and Cadmium oxide is heated to Cadmium oxide at 320 ℃ and is dissolved completely, then under the condition of 120 ℃, take out the vacuum of 2 hours, then under nitrogen protection and magnetic agitation, be heated to 370 ℃, with syringe fast by selenium: TOP injection of solution is in flask, at this temperature, react after 3 minutes and stop heating, after solution is cooled to room temperature, by adding quantitative anhydrous methanol to make the synthetic CdSe seed precipitation obtaining, after 3 eccentric cleaning, CdSe seed is dissolved in TOP, and CdSe seed concentration is adjusted to 400 μ M, stand-by.
By quantitative TOPO, ODPA, HPA and Cadmium oxide are contained in flask, under nitrogen protection, temperature are increased to 320 ℃ of complete dissolved oxygen cadmiums, solution are cooled to thereupon] 20 ℃ and take out the vacuum of 2 hours; Then solution is heated to 350 ℃, now by sulphur: the CdSe seed of preparation in TOP solution and step (1): TOP solution is injected into rapidly in flask stopped heating, the synthetic CdSe@CdS nanometer rod that obtains after 8 minutes.
Length and the diameter of described CdSe@CdS nanometer rod are respectively 50 nanometers and 5 nanometers.
(2) cleaning of CdSe@CdS nanometer rod solution and concentration regulation and control: by repeated precipitation eccentric cleaning in mixture of toluene/methanol 3 times, each cleaning 5 minutes, remove remaining TOPO, again precipitation is dissolved in appropriate toluene solvant again, forms the dispersion soln of finite concentration CdSe@CdS nanometer rod;
The concentration of described CdSe@CdS nanometer rod is 0.01 μ M;
(3) preparation of CdSe@CdS nano-rod film: carbon film is placed in watch-glass, is then placed on together on hot-plate; The CdSe@CdS nanometer rod solution of 0.5 μ l is dropped in to the central authorities of carbon film, form CdSe@CdS nano-rod film, then leave standstill and treat solvent evaporates 3 minutes.
(4) preparation of CdSe@CdS nanometer rod self-assembled structures: under the environment of nitrogen, above-mentioned CdSe@CdS nano-rod film is carried out to anneal;
In step (4), the temperature of annealing is 200 ℃, and the time of annealing is 0.5 hour.
After annealing, obtain the structure of described individual layer CdSe@CdS nanometer rod self-assembly.From Fig. 1 and Fig. 2, can find out, the construction process of the one dimension Nano structure that the embodiment of the present invention provides can be realized the individual layer self-assembly of CdSe@CdS nanometer rod in solid substrate.
The preliminary study of the formation mechanism by the CdSe@CdS one dimension self-assembled structures to prepared in the present invention, think that the coated part surface organic molecule of CdSe@CdS nanorod surfaces is removed in this annealing process, enough space and degree of freedom are provided to like this self assembling process of CdSe@CdS nanometer rod, thereby have realized CdS@CdS nanometer rod in the suprabasil individual layer self-assembly of carbon film.
The feature that the surperficial organic molecule that the present invention mainly utilizes CdSe@CdS nanorod surfaces to be coated can be removed in annealing process, has realized the self-assembly of CdSe@CdS nanometer rod individual layer in carbon film substrate.The inventive method wants novel simple than the existing method that other prepares individual layer nanometer rod self-assembled structures, and each step process is simple, without complicated instrument and template, thereby has good application and development prospect.Prepared CdSe@CdS nanometer rod individual layer self-assembled structures is expected to obtain application in fields such as novel nano photoelectric devices.
Accompanying drawing explanation
Fig. 1 be the CdSe@CdS nanometer rod individual layer self-assembled structures for preparing of the method that provides according to the invention process low power transmission electron microscope photo (scale be 0.2 μ m).
Fig. 2 is the high power transmission electron microscope photo (scale is 100nm) of the CdSe@CdS nanometer rod individual layer self-assembled structures for preparing of the method that provides according to the invention process.
Embodiment
Below in conjunction with accompanying drawing, enforcement of the present invention is elaborated: under being originally implemented in take technical scheme of the present invention as prerequisite, implement; be used for illustrating the present invention; provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following enforcement.
M in described embodiment is mol/L.
In the present invention, described CdSe@CdS nanometer rod is to adopt seed growth method synthetic, and concrete synthesis step is as follows;
Synthetic and the solubility configuration of CdSe seed: by 3.O gram of TOPO, 0.28 gram of ODPA and 0.06 gram of Cadmium oxide are contained in the there-necked flask of 50 milliliters, under the condition of vacuum and 150 ℃, heat 1 hour, by solution 320 ℃ of complete dissolved oxygen cadmiums of heating, until become optically transparent solution.Under the condition of 120 ℃, take out the vacuum of 2 hours thereupon, then under nitrogen protection and magnetic agitation, be heated to 370 ℃, the TOP injection of solution of 1.5 grams in flask, treat that temperature heating returns to 370 ℃, now fast selenium solution (0.058 gram of selenium is dissolved in 0.360 gram of TOP) is expelled in flask with syringe, at this temperature, react after 3 minutes and stop heating, after solution is cooled to room temperature, add quantitative anhydrous methanol to make CdSe seed precipitation, after 3 eccentric cleaning, CdSe seed is dissolved in TOP, and CdSe seed concentration is adjusted to 400 μ M, stand-by.
The preparation of CdSe@CdS nanometer rod: by TOPO (3.0 grams); ODPA (0.29 gram); HPA (0.08 gram) and Cadmium oxide (0.09 gram) are contained in the there-necked flask of 50 milliliters; under the environment of nitrogen protection; under the condition of 150 ℃, heat 1 hour; then temperature is increased to 320 ℃, and dissolved oxygen cadmium completely, until become optically transparent solution.Solution is cooled to 120 ℃ and take out the vacuum of 2 hours thereupon; Then solution is heated to 350 ℃, the TOP injection of solution of 1.5 grams in flask, treat that temperature heating returns to 350 ℃, the CdSe seed of now being prepared by the previous step of sulphur solution (0.12 gram of sulphur is dissolved in 1.5 grams of TOP) and 200 μ L: TOP solution is injected into rapidly in flask, after 8 minutes, stop heating, the CdSe@CdS nanometer rod solution after synthetic is cooled to room temperature.
The cleaning of CdSe@CdS nanometer rod and concentration regulation and control: by repeated precipitation in mixture of toluene/methanol, adopt the method for eccentric cleaning to clean 3 times CdSe@CdS nanometer rod solution, each scavenging period is 5 minutes, finally precipitation is dissolved in appropriate toluene solvant again, forming concentration is the dispersion soln of the CdSe@CdS nanometer rod of 0.01 μ M;
The preparation of CdSe@CdS nano-rod film: the copper mesh of the coated carbon film that a slice transmission electron microscopy observation is used is placed in watch-glass, is then placed on hot-plate together; The above-mentioned CdSe@CdS nanometer rod solution of 0.5 μ l is dropped in to the central authorities of carbon film, form CdSe@CdS nano-rod film, then leave standstill and treat solvent evaporates 3 minutes.
The preparation of CdSe@CdS nanometer rod self-assembled structures: under the environment of nitrogen, to above-mentioned CdSe@CdS nano-rod film heating, be progressively increased to 200 ℃ (approximately 3 minutes) from room temperature; Then under the condition of 200 ℃, heat 0.5 hour, finally stop heating and be cooled to room temperature (approximately 10 minutes), just obtain the structure of described individual layer CdSe@CdS nanometer rod self-assembly.
In sum, above use generality illustrates, the present invention is described in detail for embodiment, but on basis of the present invention, not departing from modifications or improvements on basis of the present invention, all belongs to the scope that patent of the present invention contains.
Claims (9)
1. prepare a method for CdSe CdS nanometer rod individual layer self-assembly, it is characterized in that it realizes by following step:
One, adopt the synthetic CdSe@CdS nanometer rod of preparing specific dimensions of seed mediated growth method, and be dispersed in toluene solvant; Two, after methyl alcohol and eccentric cleaning processing, CdSe@CdS nanometer rod is fully disperseed in toluene solvant, avoid reuniting, form the dispersion soln of finite concentration CdSe@CdS nanometer rod; Three, by dripping the method being coated with, the dispersion soln of the CdSe@CdS nanometer rod of certain capacity is coated onto in solid substrate, realizes the deposition of CdSe@CdS nano-rod film; The temperature and time of four, annealing by regulation and control, realizes controlled nanometer stick array and self-assembles in solid substrate.
2. the preparation method of CdSe@CdS nanometer rod individual layer according to claim 1 self-assembly, it is characterized in that in step 1, the diameter of described CdSe CdS nanometer rod is that～5 nanometers, length are～50 nanometers, is good list and divides state in bulk in toluene solvant.
3. method according to claim 1, is characterized in that in step 2, and the eccentric cleaning number of times of described CdSe@CdS nanometer rod is 3 times, cleans 5 minutes, to remove remaining TOPO at every turn.
4. method according to claim 1, is characterized in that in step 2, and the concentration of described CdSe@CdS nanometer rod dispersion soln is 0.01 μ M.
5. method according to claim 1, is characterized in that in step 3, and the capacity of described CdSe@CdS nanometer rod is 0.5 μ l.
6. method according to claim 1, is characterized in that in step 4, and described anneal environment is to anneal 0.5 hour under the condition of 200 ℃ of nitrogen atmosphere and temperature.
7. the preparation method of CdSe@CdS nanometer rod individual layer according to claim 1 self-assembly, is characterized in that described solid substrate is the copper mesh of the coated carbon film of 400 order used of transmission electron microscopy observation.
8. the preparation method of CdSe@CdS nanometer rod individual layer according to claim 1 self-assembly, it is characterized in that described self-assembling method refers to that the surperficial organic molecule being coated by CdSe@CdS nanorod surfaces removes in this annealing process, thereby realized CdSe@CdS nanometer rod in the suprabasil self-assembly of carbon film.
9. the preparation method of CdSe@CdS nanometer rod individual layer according to claim 1 self-assembly, is characterized in that described nano-bar material can also be CdS, the CdSe with the synthetic preparation of seed mediated growth method.
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| CN104409558A (en) * | 2014-12-21 | 2015-03-11 | 浙江理工大学 | Manufacturing method of nano-photoelectric device based on CdS (Cadmium Sulfide) nano-rods |
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| CN102163486A (en) * | 2010-12-30 | 2011-08-24 | 陕西科技大学 | Photoethcing self assembly preparation method of patterned BiFeO3 film |
| CN102173406A (en) * | 2010-12-24 | 2011-09-07 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method for carbon nano tube or graphene extra-thin film |
| CN103021503A (en) * | 2011-09-26 | 2013-04-03 | 国家纳米科学中心 | Graphene-carbon nano composite transparent conducting thin film and preparation method thereof |
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| CN102173406A (en) * | 2010-12-24 | 2011-09-07 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method for carbon nano tube or graphene extra-thin film |
| CN102163486A (en) * | 2010-12-30 | 2011-08-24 | 陕西科技大学 | Photoethcing self assembly preparation method of patterned BiFeO3 film |
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| ANNA PERSANO 等: "Photoconduction Properties in Aligned Assemblies of Colloidal CdSe/CdS Nanorods", 《ACS NANO》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104409558A (en) * | 2014-12-21 | 2015-03-11 | 浙江理工大学 | Manufacturing method of nano-photoelectric device based on CdS (Cadmium Sulfide) nano-rods |
| CN104409558B (en) * | 2014-12-21 | 2017-02-22 | 浙江理工大学 | Manufacturing method of nano-photoelectric device based on CdS (Cadmium Sulfide) nano-rods |
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