CN105219392A - Nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride and its preparation method and application - Google Patents
Nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride and its preparation method and application Download PDFInfo
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Abstract
Open nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride of the present invention and its preparation method and application, first be the nanocrystalline superstructure of luminous Cadmium Sulfide/cadmium telluride of part synthesizing water-solubility with Thiovanic acid, by phase transition, the phase topological framework of superstructure is changed subsequently, the superstructure in last organic phase and poly-3-hexyl thiophene is blended prepares Organic-inorganic composite light-detecting device.Cadmium Sulfide/cadmium telluride nanocrystalline superstructure fluorescence efficiency of the organic phase obtained is higher, and spectrochemical property is stablized, the preparation for light-detecting device, photoswitch is significant, in addition, the present invention is easy to operate, the used time is short, productive rate is high, is suitable for scale operation.
Description
Technical field
The invention belongs to field of nano material preparation, more particularly, relate to a kind of phase transition and prepare the method for the nanocrystalline superstructure of Cadmium Sulfide/cadmium telluride and the application on light-detecting device thereof.
Background technology
Nanocrystalline (NCs) has electrical properties ([1] Alivisatos, A.P.Science1996,271,933-937. [2] Zhou, the Y. of very strong dimensional effect, special chemical constitution and excellence; Yang, M.; Sun, K.; Tang, Z.; Kotov, N.A.J.Am.Chem.Soc.2010,132,6006-6013.).But, single nanocrystalline between electronic mobility extremely low, and continuous print charge transport path can not be formed.Therefore, be nanocrystallinely assembled into required nanocrystalline superstructure (NCsS) by single and become current a major challenge.In nanocrystalline superstructure, electron coupling between nanocrystalline counteracts its quantum confined effect, the raising of carrier mobility can be caused simultaneously, this will be conducive to formation ([3] Vanmaekelbergh of current carrier continuative transport path, D.NanoToday2011,6,419-437.), for its this for significant ([4] Xue, the D.J. of the research of photovoltaic device; Wang, J.J.; Wang, Y.Q.; Xin, S.; Guo, Y.G.; Wan, L.J.Adv.Mater.2011,23,3704 – 3707. [5] Yang, H.Y.; Son, D.I.; Kim, T.W.; Lee, J.M.; Park, W.I.Org.Electron.2010,11,1313. [6] Gaponik, N.; Rogach, A.L.Phys.Chem.Chem.Phys.2010,12,8685-8693).Due to the great potential that nanocrystalline superstructure has on novel nano structure and nano-device preparation, therefore, nanocrystalline superstructure has attracted increasing concern ([7] Huynh, W.U.; Dittmer, J.J.; Alivisatos, A.P.Science2002,295,2425-2427. [8] Murray, C.B.; Norris, D.J.; Bawendi, M.G.J.Am.Chem.Soc.1993,115,8706-8715.).
At present, existing scientist has synthesized the nanocrystalline superstructure that some have special appearance, as ([9] Nozik, A.J. such as nano wire, nanometer sheet, micellas; Beard, M.C.; Luther, J.M.; Law, M.; Ellingson, R.J.; Johnson, J.C.Chem.Rev.2010,110,6873-6890. [10] Guo, C.X.; Yang, H.B.; Sheng, Z.M.; Lu, Z.S.; Song, Q.L.; LiC.M.Angew.Chem.Int.Ed.2010,49,3014-3017. [11] Nikolic, M.S.; Olsson, C.; Salcher, A.; Kornowski, A.; Rank, A.; Schubert, R.;
a.; Weller, H.;
s.Angew.Chem.Int.Ed.2009,48,2752-2754.).In numerous existing nanostructure structure, the people such as Kotov report a kind of nanocrystalline superstructure ([12] Srivastava, S. of band shape; Santos, A.; Critchley, K.; Kim, K.S.; Podsiadlo, P.; Sun, K.; Lee, J.; Xu, C.L.; Lilly, G.D.; Glotzer, S.C.; Kotov, N.A.Science2010,327,1355-1359.), if this nano belt will play huge effect ([13] Xia, Y. as the functional unit of linking up the fields such as electronics, photoelectricity, electrochemistry and nano-device; Yang, P.; Sun, Y.; Wu, Y.; Mayers, B.; Gates, B.; Yin, Y.; Kim, F.; Yan, H.Adv.Mater.2003,5,353-389.).But, the people such as Kotov prepare the nanocrystalline superstructure of this band shape in aqueous phase, be difficult to form with nonpolar organic polymer the mixture dissolved each other, thus effectively cannot realize exciton dissociation on NCsS/ polymer interface, which limits its application at photoelectric field.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of method being prepared Cadmium Sulfide/cadmium telluride (CdS/CdTe) nanocrystalline superstructure by phase transition is provided, and have studied its application at light-detecting device.In technical solution of the present invention, CdTeNCsS with polymer formation blend in organic phase, and then is effectively realized exciton dissociation, thus may be used for the preparation of light-detecting device after being changed by phase transition recurring structure on NCsS/ polymer interface.
Technical purpose of the present invention is achieved by following technical proposals:
Nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride and preparation method thereof, carry out according to following step:
The nanocrystalline superstructure of phase sulfur cadmium/cadmium telluride taking Thiovanic acid as part is joined in the chloroformic solution of cetyl trimethylammonium bromide (CTAB), the nanocrystalline superstructure of Cadmium Sulfide/cadmium telluride after leaving standstill in aqueous phase is transferred in chloroform, namely obtains the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride.
In above-mentioned preparation process, the CdS/CdTeNCsS in the aqueous phase of upper strata is transferred in lower floor's chloroformic solution, uses separating funnel to collect the chloroformic solution of lower floor, obtains a kind of CdS/CdTeNCsS had in novel nano structure organic phase.
In above-mentioned preparation process, select 3.0-4.0g cetyl trimethylammonium bromide to be dissolved in 100mL chloroform, form the chloroformic solution of cetyl trimethylammonium bromide.
In above-mentioned preparation process, select time of repose at least 4h, preferably 4-8h.
The application of the nanocrystalline superstructure of above-mentioned organic phase Cadmium Sulfide/cadmium telluride in light-detecting device.
In above-mentioned application scheme, the nanocrystalline superstructure of described organic phase Cadmium Sulfide/cadmium telluride and the mixing of poly-3-hexyl thiophene to obtain homogeneous solution, then with solution spin coating to obtain composite membrane, are selected to carry out composite membrane spin coating on the microelectrode of laser ablation.
In above-mentioned application scheme, the nanocrystalline superstructure of described organic phase Cadmium Sulfide/cadmium telluride is prepare according to preparation method of the present invention, through shifting the nanocrystalline superstructure of Cadmium Sulfide/cadmium telluride be dispersed in chloroform obtained.
In above-mentioned application scheme, the mass ratio of described poly-3-hexyl thiophene (P3HT), the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride is (1-2): (3-4), preferably (1.2-1.5): (3.5-3.8).Select both to be uniformly dissolved in dispersion in chloroform solvent, or be uniformly dissolved respectively and be dispersed in chloroform, then chloroform is mixed.
As shown in Figure 1, there is the schematic diagram changed in the banded NCsS of luminous CdS/CdTe its topological framework in phase transition behavior, makes stiff NCsS structure originally become submissive and loose, finally obtain the organic phase NCsS that can be used for preparing light-detecting device.As shown in accompanying drawing 2-5, NCsS is pencil superstructure and chloroform middle pencil superstructure mutually in aqueous phase respectively, NCs forms pencil NCsS in self assembling process as we can see from the figure, can become submissive and loose structure (i.e. the NCsS of the organic phase of phase in version acquisition is formed by many nano belt structures) after being transferred to organic phase.Through fluorometric investigation (photoluminescence of the NCsS namely in aqueous phase and organic phase), in aqueous phase, fluorescence obviously weakens, and chloroform mutually in have obvious Fluorescence Increasing, show NCsS be successfully transferred to chloroform mutually in.Utilize EDS to detect the composition of organic phase NCsS nanometer bundle sample, the atom content per-cent of Cd, Te, S is 48.7:1.7:49.6, shows that sulfonium ion that Thiovanic acid discharges instead of the Te element in CdTe.As can be seen from Fig. 6-8, light-detecting device based on organic phase NCsS shows larger on-off ratio (100) and photosensitivity, simultaneously, this device all has good responsiveness under different light intensity, and (photoswitch preparation is see document: BeatrizH, ChristianK, HorstW, Quantumdotattachmentandmorphologycontrolbycarbonnanotube s, nanoletters, 2007,7 (12): 3564-3568).
In technical solution of the present invention, first with the banded NCsS of luminous CdS/CdTe that Thiovanic acid (TGA) is part synthesizing water-solubility, the phase topological framework of NCsS is made to change (originally stiff NCsS structure become soft and loosen) by phase transition subsequently, the NCsS in last organic phase and poly-3-hexyl thiophene (P3HT) is blended prepares Organic-inorganic composite light-detecting device.The CdS/CdTeNCsS fluorescence efficiency of the organic phase obtained is higher, and spectrochemical property is stablized, and the preparation for light-detecting device, photoswitch is significant, and in addition, the present invention is easy to operate, the used time is short, productive rate is high, is suitable for scale operation.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that NCsS its topological framework in phase transition behavior occurs to change.
Fig. 2 is transmission electron microscope (TEM) photo of NCsS in aqueous phase.
Fig. 3 is scanning electronic microscope (SEM) photo of NCsS in aqueous phase.
Fig. 4 be chloroform mutually in transmission electron microscope (TEM) photo of NCsS.
Fig. 5 be chloroform mutually in scanning electronic microscope (SEM) photo of NCsS.
Fig. 6 utilizes the electric current time history plot of light-detecting device under light source on/off switch condition of the nanocrystalline superstructure of organic phase of the present invention Cadmium Sulfide/cadmium telluride (incident light density is 5.51mWcm
-2, bias voltage is 1V).
Fig. 7 is the electric current of light-detecting device under different light intensity (I)-voltage (V) graphic representation utilizing the nanocrystalline superstructure of organic phase of the present invention Cadmium Sulfide/cadmium telluride.
Fig. 8 utilizes the light-detecting device of the nanocrystalline superstructure of organic phase of the present invention Cadmium Sulfide/cadmium telluride when bias voltage is for 1V, the function curve of photoelectric current and incident light density.
Embodiment
Technical scheme of the present invention is further illustrated below in conjunction with specific embodiment.
First, (its synthetic method refers to: [15] Tang, B. to synthesize sodium hydrogen telluride (NaHTe); Yang, F.; Lin, Y.; Zhuo, L.H.; Ge, J.C.; Cao, L.H.Chem.Mater.2007,19,1212 – 1214.).By 102.8mgNaBH
4, 5mL ultrapure water and 109.5mg tellurium powder put into a little flask, then reaction system put into ice bath cooling under ar gas environment.Between the reaction period, for keeping pressure equilibrium, go out by the hydrogen discharge of conduit by argon gas and generation.After reacting about 8h, the tellurium powder of black disappears, and produces the sodium tetraborate precipitation (Na of white at drag
2b
4o
7), gained solution is NaHTe solution.The NaHTe clear liquid of generation is left standstill 30h, synthesized NaHTe solution as raw material, in a particular embodiment for the preparation of CdS/CdTe quantum dot.
Secondly, the nanocrystalline superstructure of aqueous phase CdS/CdTe (NCsS) is prepared, according to reference (Shen, Y.T.; Lei, D.; Feng, W.J.Mater.Chem.C2013,1,1926-1932) guidance synthesize: by 0.4mmolCdCl
2the solution of 100mL is mixed with 0.6mmol Thiovanic acid (TGA), under the condition stirred, dropwise add 1.0MNaOH solution and the pH value of solution is adjusted to 11.8, at room temperature solution is transferred in the there-necked flask of 250mL subsequently, logical argon gas emptying air.Opening under the state stirred, the NaHTe solution (0.3mmol, 1.7mL) prepared with syringe holder joins in above-mentioned solution, cools at 100 DEG C after reflux 8h.After reaction terminates, in the CdTe quantum aqueous solution, add methyl alcohol, centrifugal after leaving standstill 48h.Precipitation again dissolved in deionized water, be adjusted to pH=9 with NaOH, in the middle of this process, quantum dot is assembled into nanocrystalline superstructure (CdS/CdTeNCsS), i.e. the nanocrystalline superstructure of Cadmium Sulfide/cadmium telluride.
When preparing light-detecting device, see document Holdcroft, S.Macromolecules1991,24,4834-4838, Ju á rez, B.H.; Klinke, C.; Kornowski, A.; Weller, H.NanoLett.2007,7,3564 – 3568.
Embodiment 1
Being dissolved in by 3.6gCTAB in 100mL chloroform, is that the NCsS solution of part adds in the chloroformic solution of 4mLCTAB with TGA by 4mL, standing mixt.After 8h, collect chloroform mutually in solution, obtain softness and loose organic phase NCsS structure; 30mgP3HT is dissolved in 3mL chloroform.The chloroformic solution of 100 μ LNCsS and 200 μ LP3HT solution are mixed to obtain final solution.Be spun on (2000rpm) on prewashed gold electrode, obtained light-detecting device, wherein the mass ratio of poly-3-hexyl thiophene (P3HT), the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride is 1.2:3.8.
Embodiment 2
Being dissolved in by 4.0gCTAB in 100mL chloroform, is that the NCsS solution of part adds in the chloroformic solution of 4mLCTAB with TGA by 4mL, standing mixt.After 8h, collect chloroform mutually in solution, obtain softness and loose organic phase NCsS structure; 40.0mgP3HT is dissolved in 3mL chloroform.The chloroformic solution of 100 μ LNCsS and 200 μ LP3HT solution are mixed to obtain final solution.Be spun on (2000rpm) on prewashed gold electrode, obtained light-detecting device, wherein the mass ratio of poly-3-hexyl thiophene (P3HT), the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride is 2:4.
Embodiment 3
Being dissolved in by 3gCTAB in 100mL chloroform, is that the NRsS solution of part adds in the chloroformic solution of 4mLCTAB with TGA by 4mL, standing mixt.After 8h, collect chloroform mutually in solution, obtain softness and loose organic phase NCsS structure; 30.0mgP3HT is dissolved in 3mL chloroform.The chloroformic solution of 100 μ LNCsS and 200 μ LP3HT solution are mixed to obtain final solution.Be spun on (2000rpm) on prewashed gold electrode, obtained light-detecting device, wherein the mass ratio of poly-3-hexyl thiophene (P3HT), the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride is 1:3.5.
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 (10)
1. the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride, it is characterized in that, carry out according to following step: the nanocrystalline superstructure of phase sulfur cadmium/cadmium telluride taking Thiovanic acid as part is joined in the chloroformic solution of cetyl trimethylammonium bromide, the nanocrystalline superstructure of Cadmium Sulfide/cadmium telluride after leaving standstill in aqueous phase is transferred in chloroform, namely obtains the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride.
2. the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride according to claim 1, is characterized in that, selects 3.0-4.0g cetyl trimethylammonium bromide to be dissolved in 100mL chloroform, forms the chloroformic solution of cetyl trimethylammonium bromide.
3. the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride according to claim 1, is characterized in that, selects time of repose at least 4h, preferably 4-8h.
4. the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride according to claim 1, it is characterized in that, the nanocrystalline superstructure of Cadmium Sulfide/cadmium telluride in the aqueous phase of upper strata is transferred in lower floor's chloroformic solution, use separating funnel to collect the chloroformic solution of lower floor, namely obtain the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride.
5. the preparation method of the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride, it is characterized in that, carry out according to following step: the nanocrystalline superstructure of phase sulfur cadmium/cadmium telluride taking Thiovanic acid as part is joined in the chloroformic solution of cetyl trimethylammonium bromide, the nanocrystalline superstructure of Cadmium Sulfide/cadmium telluride after leaving standstill in aqueous phase is transferred in chloroform, namely obtains the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride.
6. the preparation method of the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride according to claim 5, it is characterized in that, select 3.0-4.0g cetyl trimethylammonium bromide to be dissolved in 100mL chloroform, form the chloroformic solution of cetyl trimethylammonium bromide.
7. the preparation method of the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride according to claim 5, is characterized in that, selects time of repose at least 4h, preferably 4-8h.
8. the preparation method of the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride according to claim 5, it is characterized in that, the nanocrystalline superstructure of Cadmium Sulfide/cadmium telluride in the aqueous phase of upper strata is transferred in lower floor's chloroformic solution, use separating funnel to collect the chloroformic solution of lower floor, namely obtain the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride.
9. the application of the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride in light-detecting device as described in one of claim 1-4, it is characterized in that, the nanocrystalline superstructure of described organic phase Cadmium Sulfide/cadmium telluride and the mixing of poly-3-hexyl thiophene are to obtain homogeneous solution, again with solution spin coating to obtain composite membrane, the mass ratio of described poly-3-hexyl thiophene, the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride is (1-2): (3-4).
10. the application of the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride according to claim 9 in light-detecting device, it is characterized in that, the mass ratio of described poly-3-hexyl thiophene, the nanocrystalline superstructure of organic phase Cadmium Sulfide/cadmium telluride is (1.2-1.5): (3.5-3.8); Select both to be uniformly dissolved in dispersion in chloroform solvent, or be uniformly dissolved respectively and be dispersed in chloroform, then chloroform is mixed.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20110091925A1 (en) * | 2009-10-05 | 2011-04-21 | Ryan Kevin M | Processing of nanoparticles |
| 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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| LEI DA等: "Recent progress in the fields of tuning the band gap of", 《SCIENCE CHINA TECHNOLOGICAL SCIENCES》 * |
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