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Optics Express

Optics Express

  • Editor: Andrew M. Weiner
  • Vol. 21, Iss. 21 — Oct. 21, 2013
  • pp: 24793–24798
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Stepwise synthesis of cubic Au-AgCdS core-shell nanostructures with tunable plasmon resonances and fluorescence

Xiao-Li Liu, Shan Liang, Fan Nan, Yue-Yue Pan, Jun-Jun Shi, Li Zhou, Shuang-Feng Jia, Jian-Bo Wang, Xue-Feng Yu, and Qu-Quan Wang  »View Author Affiliations


Optics Express, Vol. 21, Issue 21, pp. 24793-24798 (2013)
http://dx.doi.org/10.1364/OE.21.024793


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Abstract

Cubic Au-AgCdS core-shell nanostructures were synthesized through cation exchange method assisted by tributylphosphine (TBP) as a phase-transfer agent. Among intermediate products, Au-Ag core-shell nanocubes exhibited many high-order plasmon resonance modes related to the special cubic shape, and these plasmon bands red-shifted along with the increasing of particle size. The plasmon band of Au core first red-shifted and broadened at the step of Au-Ag2S and then blue-shifted and narrowed at the step of Au-AgCdS. Since TBP was very crucial for the efficient conversion from Ag2S to CdS, we found that both absorption and fluorescence of the final products could be controlled by TBP.

© 2013 Optical Society of America

1. Introduction

Metal-semiconductor hetero-nanostructures usually exhibit dramatically different properties than the individual ingredients [1

1. J. Zhang, Y. Tang, K. Lee, and M. Ouyang, “Tailoring light-matter-spin interactions in colloidal hetero-nanostructures,” Nature 466(7302), 91–95 (2010). [CrossRef] [PubMed]

,2

2. Y. Wang, T. Yang, M. T. Tuominen, and M. Achermann, “Radiative rate enhancements in ensembles of hybrid metal-semiconductor nanostructures,” Phys. Rev. Lett. 102(16), 163001 (2009). [CrossRef] [PubMed]

], due to the intense interaction between metal and semiconductor. Surface plasmon resonances (SPR) in metal can be modified by the semiconductor ingredient in hetero-structures. Through near-field interactions, energy could flow from the excited state of semiconductor to the plasmon, leading to the loss compensation and amplification of plasmon [3

3. B. Peng, Q. Zhang, X. Liu, Y. Ji, H. V. Demir, C. H. A. Huan, T. C. Sum, and Q. Xiong, “Fluorophore-doped core-multishell spherical plasmonic nanocavities: resonant energy transfer toward a loss compensation,” ACS Nano 6(7), 6250–6259 (2012). [CrossRef] [PubMed]

5

5. R. F. Oulton, V. J. Sorger, T. Zentgraf, R. M. Ma, C. Gladden, L. Dai, G. Bartal, and X. Zhang, “Plasmon lasers at deep subwavelength scale,” Nature 461(7264), 629–632 (2009). [CrossRef] [PubMed]

]. On the other side, plasmon-exciton interaction can also bring a strong modification of the radiative and nonradiative properties for semiconductor, altering the emission behaviors of semiconductor (enhancement or quenching) [6

6. H. Y. Lin, Y. F. Chen, J. G. Wu, D. I. Wang, and C. C. Chen, “Carrier transfer induced photoluminescence change in metal-semiconductor core-shell nanostructures,” Appl. Phys. Lett. 88(16), 161911 (2006). [CrossRef]

,7

7. H. M. Gong, L. Zhou, X. R. Su, S. Xiao, S. D. Liu, and Q. Q. Wang, “Illuminating dark plasmons of silver nanoantenna rings to enhance exciton–plasmon interactions,” Adv. Funct. Mater. 19(2), 298–303 (2009). [CrossRef]

]. With appropriate band structures, charge transfer process like photo-excited electrons in semiconductor transferring to metal could suppress the direct recombination of carriers and promote efficient charge separation, resulting in a significant enhancement in the photoelectric conversion efficiency in solar cell and photo-catalysis system [8

8. N. Zhang, S. Liu, and Y. J. Xu, “Recent progress on metal core@semiconductor shell nanocomposites as a promising type of photocatalyst,” Nanoscale 4(7), 2227–2238 (2012). [CrossRef] [PubMed]

,9

9. D. Seo, G. Park, and H. Song, “Plasmonic monitoring of catalytic hydrogen generation by a single nanoparticle probe,” J. Am. Chem. Soc. 134(2), 1221–1227 (2012). [CrossRef] [PubMed]

].

Many studies have been devoted to preparing metal-semiconductor hybrids consisted of various metal nanostructures and semiconductor materials [10

10. Z. Sun, Z. Yang, J. Zhou, M. H. Yeung, W. Ni, H. Wu, and J. Wang, “A general approach to the synthesis of gold-metal sulfide core-shell and heterostructures,” Angew. Chem. Int. Ed. Engl. 48(16), 2881–2885 (2009). [CrossRef] [PubMed]

15

15. S. Liang, X. L. Liu, Y. Z. Yang, Y. L. Wang, J. H. Wang, Z. J. Yang, L. B. Wang, S. F. Jia, X. F. Yu, L. Zhou, J. B. Wang, J. Zeng, Q. Q. Wang, and Z. Zhang, “Symmetric and asymmetric Au-AgCdSe hybrid nanorods,” Nano Lett. 12(10), 5281–5286 (2012). [CrossRef] [PubMed]

]. For instance, Wang’s group proposed a general approach to synthesize gold-metal sulfide core-shell and heterostructures [10

10. Z. Sun, Z. Yang, J. Zhou, M. H. Yeung, W. Ni, H. Wu, and J. Wang, “A general approach to the synthesis of gold-metal sulfide core-shell and heterostructures,” Angew. Chem. Int. Ed. Engl. 48(16), 2881–2885 (2009). [CrossRef] [PubMed]

], and Hsu’s group developed a facile approach for preparing Au-CdS core-shell nanocrystals with controllable shell thickness [11

11. W. T. Chen, T. T. Yang, and Y. J. Hsu, “Au−CdS core−shell nanocrystals with controllable shell thickness and photoinduced charge separation property,” Chem. Mater. 20(23), 7204–7206 (2008). [CrossRef]

]. These methods prepared designated metal ion-molecule complex acting as precursor to bind on Au core for growth of semiconductor shell. Ouyang’s group established a nonepitaxial growth to synthesize spherical Au-CdS core-shell nanostructures with monocrystalline semiconductor shell through a cation exchange process, this method can overcome the constraint of lattice mismatches between two components and suit for growth of multiple type semiconductor shells (CdS, CdTe, ZnS, PbS, etc.) [14

14. J. Zhang, Y. Tang, K. Lee, and M. Ouyang, “Nonepitaxial growth of hybrid core-shell nanostructures with large lattice mismatches,” Science 327(5973), 1634–1638 (2010). [CrossRef] [PubMed]

]. Metal-semiconductor hetero-structures have tunable optical properties since the SPR properties are strongly dependent on the composition, dimension, and morphology of metal nanoparticles (NPs) [16

16. L. Zhou, X. F. Fu, L. Yu, X. Zhang, X. F. Yu, and Z. H. Hao, “Crystal structure and optical properties of silver nanorings,” Appl. Phys. Lett. 94(15), 153102 (2009). [CrossRef]

18

18. A. S. Kumbhar, M. K. Kinnan, and G. Chumanov, “Multipole plasmon resonances of submicron silver particles,” J. Am. Chem. Soc. 127(36), 12444–12445 (2005). [CrossRef] [PubMed]

]. Compared with the spherical NPs, metallic nanorods support both longitudinal and transverse SPRs, and metallic nanocubes possess sharp corners with strong local field enhancements and multi-high-order SPRs induced by the local field coupling of pairs of parallel surface [18

18. A. S. Kumbhar, M. K. Kinnan, and G. Chumanov, “Multipole plasmon resonances of submicron silver particles,” J. Am. Chem. Soc. 127(36), 12444–12445 (2005). [CrossRef] [PubMed]

20

20. M. Haggui, M. Dridi, J. Plain, S. Marguet, H. Perez, G. C. Schatz, G. P. Wiederrecht, S. K. Gray, and R. Bachelot, “Spatial confinement of electromagnetic hot and cold spots in gold nanocubes,” ACS Nano 6(2), 1299–1307 (2012). [CrossRef] [PubMed]

], which are very sensitive to the environment [21

21. Y. H. Lee, H. Chen, Q. H. Xu, and J. Wang, “Refractive index sensitivities of noble metal nanocrystals: the effects of multipolar plasmon resonances and the metal type,” J. Phys. Chem. C 115(16), 7997–8004 (2011). [CrossRef]

].

In this paper, we chose Au nanocubes as core to synthesize Au-AgCdS core-shell nanostructures through a stepwise method, including growth of cubic Ag on core, sulfuration of Ag shells, and cation exchange process (with tributylphosphine, TBP) from Ag2S to CdS. We observed five SPR bands and their unique evolution in the intermediate product of cubic Au-Ag NPs and found that both resonant absorption and fluorescence (FL) behavior of the final products were controlled by TBP.

2. Experimental section

Au nanocubes were prepared using a seed-mediated growth as reported previously [19

19. X. Wu, T. Ming, X. Wang, P. Wang, J. Wang, and J. Chen, “High-photoluminescence-yield gold nanocubes: for cell imaging and photothermal therapy,” ACS Nano 4(1), 113–120 (2010). [CrossRef] [PubMed]

,22

22. X. L. Liu, S. Liang, F. Nan, Z. J. Yang, X. F. Yu, L. Zhou, Z. H. Hao, and Q. Q. Wang, “Solution-dispersible Au nanocube dimers with greatly enhanced two-photon luminescence and SERS,” Nanoscale 5(12), 5368–5374 (2013). [CrossRef] [PubMed]

], and centrifuged and re-dispersed in water for future used. For growth of Au-Ag nanocubes, Au nanocubes (0.5 mL) and cetyltrimethylammoniumchloride (CTAC, 20 mM, 4.5 mL) were mixed and heated at 60 °C under magnetic stirring. After 20 mins, AgNO3 solution (2 mM, 2 mL) and 2 mL of mixture solution containing ascorbic acid (50 mM) and CTAC (40 mM) were simultaneously injected drop by drop, and the mixture was stirred for 4 hrs [23

23. Y. Ma, W. Li, E. C. Cho, Z. Li, T. Yu, J. Zeng, Z. Xie, and Y. Xia, “Au@Ag core-shell nanocubes with finely tuned and well-controlled sizes, shell thicknesses, and optical properties,” ACS Nano 4(11), 6725–6734 (2010). [CrossRef] [PubMed]

]. The Au-Ag nanocubes (1 mL) and NaHS solution (50 mM, 10 μL) were mixed and reacted for 20 mins at room temperature under magnetic stirring. The Au-Ag2S nanocubes were obtained by centrifugation (7600 rpm for 10 mins) and washed with water once. Au-AgCdS(II) core-shell NPs were synthesized as following procedure: Au-Ag2S nanocubes (1 mL) and CTAC (0.2 M, 1 mL) were mixed together and heated at 60 °C under magnetic stirring, then Cd(NO3)2 solution (50 mM, 10 μL) and TBP (10 μL) were added into the mixture. After 6 hrs, the final products were collected by centrifugation (7600 rpm for 10 mins). Au-AgCdS(I) were obtained through the same procedure but without adding TBP.

The transmission electron microscope (TEM) images were performed with a JEOL 2010 HT transmission electron microscope operated at 200 kV. Energy-dispersive X-ray Spectrum (EDX) analysis was performed on an EDAX instrument incorporated in the HRTEM. The absorption spectra were measured using a TU-1810 UV-vis spectrophotometer. For fluorescence measurements, the excitation source was a mode-locked Ti:sapphire laser (Mira 900, Coherent) with a pulse width of around 3 ps and a repetition rate of 76 MHz. The FL spectra were recorded by a spectrometer (Spectrapro 2500i, Acton) with a liquid-nitrogen cooled CCD (SPEC-10: 100B, Princeton).

3. Results and discussion

EDX analyses were carried out to confirm the conversion from Ag2S to CdS. Figure 2(a)
Fig. 2 (a) EDX elemental maps of Au, Ag, Cd, and S in a Au-AgCdS(II) nanocube. (b) Line profile of Au(II), Ag(II), and Cd(II) in the same Au-AgCdS(II) nanocube. All lines are normalized and the maximum intensity of Au is set to 1. Cd(I) line profile of a Au-AgCdS(I) nanocube (red) is also shown for comparison, which is normalized by it’s own Au distribution.
shows the EDX elemental maps of Au, Ag, Cd, and S in a Au-AgCdS(II) nanocube. The data suggest that the shell is composed of Ag, Cd, and S. The distributions of Au, Ag, and Cd are also displayed by line-scan EDX spectra in Fig. 2(b). The intensity of Cd distribution in Au-AgCdS(II) is stronger than that in Au-AgCdS(I), which manifests that the conversion from Ag2S to CdS is more effective with the assistance of TBP.

The absorption spectral evolution reflects the distinctive SPR properties of metal NPs determined by composition, size, and shape. The spectral responses dependent on the thickness of Ag shells in Au-Ag core-shell nanocubes are shown in Fig. 3(a)
Fig. 3 (a) Absorption spectra of Au and Au-Ag nanocubes with different particle size. dAu and dAg represent the side length of Au nanocubes and the thickness of silver shell, respectively. (b) Multiple plasmon resonance modes vary with the size of the Au-Ag nanocubes. (c, d) Absorption spectra of Au-Ag2S NPs (0 hr), Au-AgCdS(II) and Au-AgCdS(I) NPs synthesized at different exchange reaction time T (T = 1, 2, 4 and 6 hrs).
. The Au nanocubes with side length of 43 ± 3 nm have a plasmon band at ~545 nm due to the dipole resonance. As a thin Ag shell (~9 nm) is deposited on Au nanocubes, the dipole resonance of Au-Ag core-shell nanocubes blue-shifts to ~527 nm. Due to the dielectric function of Ag is different from Au, the blue-shift originates from the altering of effective dielectric function by Ag coating [27

27. S. Link, Z. L. Wang, and M. A. El-Sayed, “Alloy formation of gold-silver nanoparticles and the dependence of the plasmon absorption on their composition,” J. Phys. Chem. B 103(18), 3529–3533 (1999). [CrossRef]

,28

28. M. Liu and P. Guyot-Sionnest, “Synthesis and optical characterization of Au/Ag core/shell nanorods,” J. Phys. Chem. B 108(19), 5882–5888 (2004). [CrossRef]

]. When the Ag thickness further increases, the dipole plasmon band (band B5) begins to red-shift because the size of whole particle increases. This band progressively red-shifts to ~617 nm when Au-Ag nanocubes grow to 111 ± 13 nm.

At the same time, multiple plasmon resonance absorption peaks gradually emerge in the range between 300 nm and 500 nm, and these new plasmon bands are very sensitive to the shape and size of Au-Ag nanocubes. The plasmon band near 340 nm (band B1) usually appeared when Ag NPs are cube shape, which may be derived from the octupole or dipole [21

21. Y. H. Lee, H. Chen, Q. H. Xu, and J. Wang, “Refractive index sensitivities of noble metal nanocrystals: the effects of multipolar plasmon resonances and the metal type,” J. Phys. Chem. C 115(16), 7997–8004 (2011). [CrossRef]

,29

29. F. Zhou, Z. Y. Li, Y. Liu, and Y. Xia, “Quantitative analysis of dipole and quadrupole excitation in the surface plasmon resonance of metal nanoparticles,” J. Phys. Chem. C 112(51), 20233–20240 (2008). [CrossRef]

]. As the edge length of Au-Ag nanocubes increases to 75 ± 9 nm, a plasmon band attributed to the quadrupole resonance appears at ~461 nm (band B4). The band B3 near 410 nm is a mix of quadrupole and dipole plasmon resonance [29

29. F. Zhou, Z. Y. Li, Y. Liu, and Y. Xia, “Quantitative analysis of dipole and quadrupole excitation in the surface plasmon resonance of metal nanoparticles,” J. Phys. Chem. C 112(51), 20233–20240 (2008). [CrossRef]

]. The band B2 arises and presents clearly as Au-Ag nanocubes grow large, which has been reported before when Ag nanocubes have a big size [30

30. X. Xia, J. Zeng, L. K. Oetjen, Q. Li, and Y. Xia, “Quantitative analysis of the role played by poly(vinylpyrrolidone) in seed-mediated growth of Ag nanocrystals,” J. Am. Chem. Soc. 134(3), 1793–1801 (2012). [CrossRef] [PubMed]

,31

31. Q. Zhang, W. Li, C. Moran, J. Zeng, J. Chen, L. P. Wen, and Y. Xia, “Seed-mediated synthesis of Ag nanocubes with controllable edge lengths in the range of 30-200 nm and comparison of their optical properties,” J. Am. Chem. Soc. 132(32), 11372–11378 (2010). [CrossRef] [PubMed]

]. As shown in Fig. 3(b), these plasmon bands display a continuous red-shift with the increasing of size. An interesting phenomenon is that, although SPR in Au nanocubes is usually dominated by a single dipole resonance, a thin layer of Ag shell with cubic shape could cause the multiple plasmon resonances.

The variation of absorption features also implies the conversion efficiency of cation exchange reaction between Ag+ and Cd2+. On the absorption spectrum of Au-Ag2S core-shell NPs, the existence of a valley at 320 nm (caused by the interband transition of Ag below 320 nm) and a weak band around 400 nm indicates the residual Ag domains in the shell. In Fig. 3(c), these features disappear in Au-AgCdS(II), which means the residual Ag has been reacted out. However, in Fig. 3(d), the retaining of these features in Au-AgCdS(I) implies the existence of residual Ag. Meanwhile, the band position blue-shifts only 17 nm and the band FWHM narrows only 25%, which indicates the extent of exchange between Ag+ and Cd2+ is small without adding TBP.

The Au-AgCdS core-shell NPs show interesting FL behaviors in Fig. 4
Fig. 4 FL spectra of Au-Ag2S (0 hr), (a) Au-AgCdS(II) NPs and (b) Au-AgCdS(I) NPs synthesized at different reaction time T (T = 1, 2, 4 and 6 hrs) at 400 nm excitation wavelength.
. The Au-AgCdS(II) exhibit an emission peak at 700 nm, which is probably the defect emission of CdS nanocrystal. As the reaction time increases, the emission intensity increases gradually. Beside the emission peak at 700 nm, an emission band arises at 570 nm and reaches the maximum at 2 hrs. We attribute this emission to the Ag-Cd-S ternary complex located in some regions [37

37. J. M. Huang and C. J. Murphy, “Luminescence of CdS nanoparticles doped and activated with foreign ions,” Proc. MRS 560, 33–38 (1999). [CrossRef]

39

39. R. Sethi, L. Kumar, P. K. Sharma, and A. C. Pandey, “Tunable visible emission of Ag-doped CdZnS alloy quantum dots,” Nanoscale Res. Lett. 5(1), 96–102 (2010). [CrossRef] [PubMed]

]. This emission decreases and disappears when the reaction proceeds forward, which means the emission is very sensitive to the ratio of Ag2S and CdS. By contrast, in Fig. 4(b), the Au-AgCdS(I) have no emission at 700 nm because the CdS component is small in Au-AgCdS(I) shell, while the emission behavior at 570 nm is similar to that of the Au-AgCdS(II). This result accords with the conclusion deduced from the absorption evolution in Figs. 3(c) and 3(d) that the cation exchange reaction without TBP is inefficient.

4. Conclusions

Acknowledgments

This work was supported by the National Program on Key Science Research of China (2011CB922201), and the NSFC (61008043, 11174229 and 11204221).

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J. M. Huang and C. J. Murphy, “Luminescence of CdS nanoparticles doped and activated with foreign ions,” Proc. MRS 560, 33–38 (1999). [CrossRef]

38.

N. P. Smirnova, A. I. Kryukov, A. M. Eremenko, Yu. A. Galagan, and S. Ya. Kuchmii, “Preparation and optical properties of a new nanostructural material: silver-ion-doped CdS nanoparticles in silicate matrices,” Theor. Exp. Chem. 34(5), 272–276 (1998). [CrossRef]

39.

R. Sethi, L. Kumar, P. K. Sharma, and A. C. Pandey, “Tunable visible emission of Ag-doped CdZnS alloy quantum dots,” Nanoscale Res. Lett. 5(1), 96–102 (2010). [CrossRef] [PubMed]

OCIS Codes
(160.3900) Materials : Metals
(160.6000) Materials : Semiconductor materials
(240.6680) Optics at surfaces : Surface plasmons
(260.2510) Physical optics : Fluorescence

ToC Category:
Materials

History
Original Manuscript: July 22, 2013
Revised Manuscript: September 29, 2013
Manuscript Accepted: September 30, 2013
Published: October 9, 2013

Citation
Xiao-Li Liu, Shan Liang, Fan Nan, Yue-Yue Pan, Jun-Jun Shi, Li Zhou, Shuang-Feng Jia, Jian-Bo Wang, Xue-Feng Yu, and Qu-Quan Wang, "Stepwise synthesis of cubic Au-AgCdS core-shell nanostructures with tunable plasmon resonances and fluorescence," Opt. Express 21, 24793-24798 (2013)
http://www.opticsinfobase.org/oe/abstract.cfm?URI=oe-21-21-24793


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