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J. Semicond. > 2013, Volume 34 > Issue 12 > 123001

SEMICONDUCTOR MATERIALS

GaN nanopillars with a nickel nano-island mask

Zengqin Lin, Xiangqian Xiu, Shiying Zhang, Xuemei Hua, Zili Xie, Rong Zhang, Peng Chen, Ping Han and Youdou Zheng

+ Author Affiliations

 Corresponding author: Xiu Xiangqian, Email: xqxiu@nju.edu.cn

DOI: 10.1088/1674-4926/34/12/123001

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Abstract: Uniform GaN nanopillar arrays have been successfully fabricated by inductively coupled plasma etching using self-organized nickel nano-islands as the masks on GaN/sapphire. GaN nanopillars with diameters of 350 nm and densities of 2.6×108 cm-2 were demonstrated and controlled by the thickness of Ni film and the NH3 annealing time. These GaN nanopillars show improved optical properties and strain change compared to that of GaN film before ICP etching. Such structures with large-area uniformity and high density could provide additional advantages for light emission of light-emitting diodes, quality improvement of ELO regrowth, etc.

Key words: GaN nanopillarsnickel nano-islandthermal ammonia etchingmaskICPSEM

Gallium nitride (GaN) has attracted much attention due to its excellent optoelectronic property with a direct band gap of 3.4 eV, high mobility and excellent thermal stability[1]. It is widely accepted that GaN nanostructures are highly promising materials for producing devices with excellent performance, such as LDs[2], LEDs[3], solar cells[4], sensors[5], and piezo-electric nanogenerators[6]. GaN nanostructures have many superior properties due to the possibility of quantum confinement, coaxial heterostructures, correlated photon emission, and photonic crystal effects, which make it a potential contender for nanolasers and nanoLEDs[7, 8]. In particular, these GaN nanostructures could provide additional advantages for light emission, quality improvement of regrowth, etc[9, 10]. GaN nanostructures such as nanorods (NRs) with high aspect-ratio and large surface-to-volume ratio can dramatically reduce the dislocation density in the upper part of the NRs[11]. Besides, the nanopillars with small footprints help to relieve the strain induced by thermal expansion mismatch and avoid crack generation. The light-extraction efficiency is expected to increase owing to the non-planar geometry of nanowires. Compared to thin films, heterostructures on GaN nanostructure arrays with low defect density are much easier to fabricate and lead to high-performance devices[12]. Also, GaN nanostructures can provide a unique opportunity for understanding the electronic, optical, and mechanical properties of the material.

Nano-GaN has been successfully synthesized via different methods, such as molecular beam epitaxy[13], selective growth on patterned substrates by metalorganic chemical vapor deposition (MOCVD)[14], and hydride vapor-phase epitaxy (HVPE)[15]. These above-mentioned methods are so-called "bottom-up" techniques, where nanostructures are grown from atoms or molecules to clusters. However, they often show a broad distribution of size, length, and orientation.

Contrary to bottom-up synthesis, a top-down etching process is an alternate way to achieve nanostructures[16, 17]. Top-down methods, such as inductively coupled plasma (ICP) etching, is more economic and extensively controlled and could be applied in the fabrication of a large-area nano-GaN in the future. In this work, we fabricate uniform GaN nanopillar arrays by inductively coupled plasma etching using Ni nano-islands as the masks. A high density of c-axis oriented nanopillars (108 cm2) with a tip diameter of about 350 nm and a height of 2 μm has been reported.

Figure 1 shows a schematic diagram of the formation of GaN nanopillars on sapphire. A 2 μm GaN layer on (0001) sapphire by MOCVD was used as the original substrate[18]. A Ni metal film was first deposited on GaN/sapphire by electron-beam evaporation. Then, Ni film/GaN/sapphire is annealed under the ammonia for the Ni nano-islands mask on GaN/sapphire. Finally, GaN not covered with Ni nano-islands was removed by ICP etching. During the ICP etching, the flow rates of chlorine and BCl3 were maintained at 48 and 6 sccm, respectively. For the whole process, the chamber pressure, ICP power, and RF power were 7.50 × 109 Pa, 300 W, and 100 W, respectively. Photoluminescence (PL) spectra were recorded by using a continuous wave He-Cd laser source at room temperature (RT). Scanning electron microcopy (SEM), energy dispersive X-ray (EDS), and Raman scattering measurements have been used to characterize the morphologies and structural properties.

Figure  1.  Schematic diagram of the formation of GaN nanopillars on sapphire. (a) Ni film deposition on the GaN/sapphire. (b) Ammonia annealing on Ni/GaN/sapphire. (c) ICP etching. (d) Ni removal.

Figure 2 shows the SEM images of 35 nm thick Ni film annealed using ammonia at 850 ℃ for different times. Ni film was transformed to nano-islands after the NH3 annealing, which was attributed to the heating effect and partially etched off by NH3 plasma at the same time[19]. The average size of nano-islands decreases from 600 to 400 nm as the annealing time increased from 4 to 12 min (Figs. 2(a)-2(c)) and then the bigger Ni nano-islands begin to absorb any smaller islands nearby and the average size of the Ni nano-islands increase until all the Ni islands are fully discrete (Figs. 2(d) and 3). Figure 3 shows the change of the average size of the Ni nano-islands from Ni film with different thicknesses at the same NH3 conditions. They have the similar trend for the size of Ni islands as the annealing time changes.

Figure  2.  SEM micrographs of Ni film of 35 nm with NH3 annealing time. (a) 4 min. (b) 8 min. (c) 12 min. (d) 16 min.
Figure  3.  The average diameter of Ni nano-islands with different annealing times for Ni film of 35 nm and 45 nm.

Figure 4 shows the SEM images of Ni film with different initial thickness annealed using ammonia at 850 ℃ for 12 min. It can be seen that the size of the Ni islands increased with increasing the Ni film thickness, but the uniformity became worse. As can be seen above, we think that uniformly distributed Ni nano-islands can be obtained by controlling the NH3 annealing time and initial thickness of Ni films. In our research, the optimal parameters for the NH3 annealing are as follows: 12 min, 850 ℃ and 35 nm Ni film.

Figure  4.  SEM images of Ni films annealed using ammonia at 850 ℃ for 12 min with different initial thicknesses. (a) 35 nm. (b) 45 nm. (c) 60 nm. (d) 80 nm.

Figure 5 shows the SEM image of GaN with 35 nm Ni film by NH3 annealing at 850 ℃ for 12 min after the ICP process, where the uniform array of GaN nanopillars is observed on the surface. GaN nano-pillars are quite homogeneous in their shape and size and almost of the same height, which indicates that GaN film under the Ni nano-island mask is not affected by the ICP process while the exposed GaN is etched away. From the top-view SEM images, the average tip diameter and the density of the pillars at different parts of the sample are calculated to be about 350 nm and 2.6 × 108 cm2, respectively. Comparing the final diameter of the pillars (350 nm) with that of Ni islands (400 nm), it is evident that there is a lateral etching in Cl2 plasma, which produces tapered structures. Two possible sources of lateral etching are wider ion angular distribution function (IADF) and the mask erosion due to the formation of Ni chlorides under highly reactive Cl ions[16, 20].

Figure  5.  SEM image of GaN nanopillars after ICP.

Because GaN nano-pillars have a homogeneous vertical shape, we think that some Ni particles remain on the top of the GaN nanopillars. SEM with energy dispersive X-ray (EDX) spectrometry has been carried out for the presence of Ni and the residual Ni can be seen only on the top part of the pillars (Fig. 6).

Figure  6.  SEM images and typical EDX spectrum of GaN nanopillars (taken before Ni removal).

The results of the Raman scattering measurements are shown in Fig. 7, where the E2 (high) and A1 (LO) modes can be seen. The strain within the GaN samples was estimated from the frequency shifts of the E2 (high) phonon line in the Raman spectra[21]. The E2 (high) peak position for GaN film on sapphire was 568.11 cm1, and that for the GaN nanopillars was 565.73 cm1. Compared with GaN bulk materials, the strain was transformed from the press stress in GaN film to the tensile stress in GaN nanopillars due to the ICP etching.

Figure  7.  Raman spectra of the GaN sample before and after ICP.
Figure  8.  PL spectra of GaN nanopillars and GaN films at room temperature.

PL spectra of the GaN film and GaN nanopillars array are measured at room temperature (RT). The PL spectrum of GaN nanopillars has a sharper and stronger near-band-edge emission as compared with GaN film, where a 61 meV redshift can be observed. ICP damage, a Stokes shift, or defect impurity states[22, 23] may induce the redshift of the PL band. A biaxial stress relaxation of about 2.8 GPa is estimated by using the proportionality factor K= 21.1 meV/GPa for the stress-induced PL peak shift[24]. In addition, an enhancement of the near-band-edge PL intensity value indicates good optical quality of the GaN nanopillars. We attributed the enhancement of PL intensity to the reduction of the internal reflection[25].

High-density GaN nanopillar arrays have been successfully fabricated using Ni nano-islands as the inert masks. The thickness and the NH3 annealing time of Ni film have an important effect on the size and distribution of GaN nanopillars. The PL peak redshift indicates that the significant stress relaxation and the enhancement of PL intensity imply an improvement of optical properties. Further work will focus on the growth of GaN LEDs on the GaN nanopillar arrays for the achieving high luminescence efficiency.



[1]
Pearton S J, Zolper J C, Shui R J, et al. GaN:processing, defects, and devices. J Appl Phys, 1999, 86:1 doi: 10.1063/1.371145
[2]
Qian F, Li Y, Gradecak S, et al. Multi-quantum-well nanowire heterostructures for wavelength-controlled lasers. Nat Mater, 2008, 7:701 doi: 10.1038/nmat2253
[3]
Zhong Z, Qian F, Wang D, et al. Synthesis of p-type gallium nitride nanowires for electronic and photonic nanodevices. Nano Lett, 2003, 3:343 doi: 10.1021/nl034003w
[4]
Tang Y B, Chen Z H, Song H S, et al. Vertically aligned p-type single-crystalline GaN nanorod arrays on n-type Si for heterojunction photovoltaic cells. Nano Lett, 2008, 8:4191 doi: 10.1021/nl801728d
[5]
Dobrokhotov V, McIlroy D N, Norton M G, et al. Principles and mechanisms of gas sensing by GaN nanowires functionalized with gold nanoparticles. J Appl Phys, 2006, 99:104302 doi: 10.1063/1.2195420
[6]
Wang X B, Song J H, Zhang F, et al. Electricity generation based on one-dimensional group-Ⅲ nitride nanomaterials. Adv Mater, 2010, 22:2155 doi: 10.1002/adma.v22:19
[7]
Duan X, Huang Y, Agarwal R, et al. Single-nanowire electrically driven lasers. Nature, 2003, 421:241 doi: 10.1038/nature01353
[8]
Huang Y, Duan X, Lieber C M. Nanowires for integrated multicolor nanophotonics. Small, 2005, 1:142 doi: 10.1002/smll.200400030/abstract
[9]
Lee C H, Kim Y J, Hong Y J, et al. Flexible inorganic nanostructure light-emitting diodes fabricated on grapheme films. Adv Mater, 2011, 10:1002 doi: 10.1002/adma.201102407/full?isReportingDone=true
[10]
Lai C M, Liu W Y, Tsay J D, et al. Self-separated freestanding GaN grown on patterned substrate by hydride vapor phase epitaxy. Phys Status Solidi, 2007, 7:2231 doi: 10.1002/pssc.200674733/abstract
[11]
Zubia D, Hersee S D. Nanoheteroepitaxy:the application of nanostructuring and substrate compliance to the heteroepitaxy of mismatched semiconductor materials. J Appl Phys, 1999, 85:6492 doi: 10.1063/1.370153
[12]
Deb P, Kim H, Qin Y, et al. GaN nanorod Schottky and p-n junction diodes. Nano Lett, 2006, 6:2893 doi: 10.1021/nl062152j
[13]
Kim H M, Kang T W, Chung K S. Nanoscale ultraviolet-light-emitting diodes using wide-bandgap gallium nitride nanorods. Adv Mater, 2003, 15:567 doi: 10.1002/adma.200304554
[14]
Hersee S D, Sun X Y, Wang X. The controlled growth of GaN nanowires. Nano Lett, 2006, 6:1808 doi: 10.1021/nl060553t
[15]
Kim H M, Kim D S, Park Y S, et al. Growth of GaN nanorods by a hydride vapor phase epitaxy method. Adv Mater, 2002, 14:991 doi: 10.1002/(ISSN)1521-4095
[16]
Paramanik D, Motayed A, Aluri G S, et al. Formation of large-area GaN nanostructures with controlled geometry and morphology using top-down fabrication scheme. J Vac Sci Technol B, 2012, 30:052202 doi: 10.1116/1.4739424
[17]
Choi W K, Liew T H, Dawood M K. Synthesis of silicon nanowires and nanofin arrays using interference lithography and catalytic etching. Nano Lett, 2008, 11:3799 doi: 10.1021/nl802129f
[18]
Xie Zili, Zhou Yuanjun, Song Lihong, et al. Structural properties of GaN (0001) epitaxial layers revealed by high resolution X-ray diffraction. Physics, Mechanics & Astronomy, Science China, 2010, 53:68 doi: 10.1007/s11433-010-0102-5?slug=full%20text
[19]
Choi J H, Lee T Y, Choi S H, et al. Density control of carbon nanotubes using NH3 plasma treatment of Ni catalyst layer. Thin Solid Films, 2003, 435:318 doi: 10.1016/S0040-6090(03)00341-9
[20]
Jansen H V, de Boer M J, Unnikrishnan S. Black silicon method X:a review on high speed and selective plasma etching of silicon with profile control:an in-depth comparison between Bosch and cryostat DRIE processes as a roadmap to next generation equipment. J Micromech Microeng, 2009, 19:033001 doi: 10.1088/0960-1317/19/3/033001
[21]
Perlin P, Jauberthie-Carillon C, Itie J P, et al. Raman scattering and X-ray-absorption spectroscopy in gallium nitride under high pressure. Phys Rev B, 1992, 45:83 doi: 10.1103/PhysRevB.45.83
[22]
George S, Ilan S, Warren M, et al. Catalytic hydride vapour phase epitaxy growth of GaN nanowires. Nanotechnology, 2005, 16:2342 doi: 10.1088/0957-4484/16/10/058
[23]
Seo H W, Bae S Y, Park J H, et al. Strained gallium nitride nanowires. Chem Phys, 2002, 116:9492 doi: 10.1063/1.1475748
[24]
Zhao D G, Xu S J, Xie M H, et al. Stress and its effect on optical properties of GaN epilayers grown on Si (111), 6H-SiC (0001), and c-plane sapphire. Appl Phys Lett, 2003, 83:677 doi: 10.1063/1.1592306
[25]
Schnitzer I, Yablonovitch E, Caneau C, et al. 30% external quantum efficiency from surface textured, thin-film light-emitting diodes. Appl Phys Lett, 1993, 63:2174 doi: 10.1063/1.110575
Fig. 1.  Schematic diagram of the formation of GaN nanopillars on sapphire. (a) Ni film deposition on the GaN/sapphire. (b) Ammonia annealing on Ni/GaN/sapphire. (c) ICP etching. (d) Ni removal.

Fig. 2.  SEM micrographs of Ni film of 35 nm with NH3 annealing time. (a) 4 min. (b) 8 min. (c) 12 min. (d) 16 min.

Fig. 3.  The average diameter of Ni nano-islands with different annealing times for Ni film of 35 nm and 45 nm.

Fig. 4.  SEM images of Ni films annealed using ammonia at 850 ℃ for 12 min with different initial thicknesses. (a) 35 nm. (b) 45 nm. (c) 60 nm. (d) 80 nm.

Fig. 5.  SEM image of GaN nanopillars after ICP.

Fig. 6.  SEM images and typical EDX spectrum of GaN nanopillars (taken before Ni removal).

Fig. 7.  Raman spectra of the GaN sample before and after ICP.

Fig. 8.  PL spectra of GaN nanopillars and GaN films at room temperature.

[1]
Pearton S J, Zolper J C, Shui R J, et al. GaN:processing, defects, and devices. J Appl Phys, 1999, 86:1 doi: 10.1063/1.371145
[2]
Qian F, Li Y, Gradecak S, et al. Multi-quantum-well nanowire heterostructures for wavelength-controlled lasers. Nat Mater, 2008, 7:701 doi: 10.1038/nmat2253
[3]
Zhong Z, Qian F, Wang D, et al. Synthesis of p-type gallium nitride nanowires for electronic and photonic nanodevices. Nano Lett, 2003, 3:343 doi: 10.1021/nl034003w
[4]
Tang Y B, Chen Z H, Song H S, et al. Vertically aligned p-type single-crystalline GaN nanorod arrays on n-type Si for heterojunction photovoltaic cells. Nano Lett, 2008, 8:4191 doi: 10.1021/nl801728d
[5]
Dobrokhotov V, McIlroy D N, Norton M G, et al. Principles and mechanisms of gas sensing by GaN nanowires functionalized with gold nanoparticles. J Appl Phys, 2006, 99:104302 doi: 10.1063/1.2195420
[6]
Wang X B, Song J H, Zhang F, et al. Electricity generation based on one-dimensional group-Ⅲ nitride nanomaterials. Adv Mater, 2010, 22:2155 doi: 10.1002/adma.v22:19
[7]
Duan X, Huang Y, Agarwal R, et al. Single-nanowire electrically driven lasers. Nature, 2003, 421:241 doi: 10.1038/nature01353
[8]
Huang Y, Duan X, Lieber C M. Nanowires for integrated multicolor nanophotonics. Small, 2005, 1:142 doi: 10.1002/smll.200400030/abstract
[9]
Lee C H, Kim Y J, Hong Y J, et al. Flexible inorganic nanostructure light-emitting diodes fabricated on grapheme films. Adv Mater, 2011, 10:1002 doi: 10.1002/adma.201102407/full?isReportingDone=true
[10]
Lai C M, Liu W Y, Tsay J D, et al. Self-separated freestanding GaN grown on patterned substrate by hydride vapor phase epitaxy. Phys Status Solidi, 2007, 7:2231 doi: 10.1002/pssc.200674733/abstract
[11]
Zubia D, Hersee S D. Nanoheteroepitaxy:the application of nanostructuring and substrate compliance to the heteroepitaxy of mismatched semiconductor materials. J Appl Phys, 1999, 85:6492 doi: 10.1063/1.370153
[12]
Deb P, Kim H, Qin Y, et al. GaN nanorod Schottky and p-n junction diodes. Nano Lett, 2006, 6:2893 doi: 10.1021/nl062152j
[13]
Kim H M, Kang T W, Chung K S. Nanoscale ultraviolet-light-emitting diodes using wide-bandgap gallium nitride nanorods. Adv Mater, 2003, 15:567 doi: 10.1002/adma.200304554
[14]
Hersee S D, Sun X Y, Wang X. The controlled growth of GaN nanowires. Nano Lett, 2006, 6:1808 doi: 10.1021/nl060553t
[15]
Kim H M, Kim D S, Park Y S, et al. Growth of GaN nanorods by a hydride vapor phase epitaxy method. Adv Mater, 2002, 14:991 doi: 10.1002/(ISSN)1521-4095
[16]
Paramanik D, Motayed A, Aluri G S, et al. Formation of large-area GaN nanostructures with controlled geometry and morphology using top-down fabrication scheme. J Vac Sci Technol B, 2012, 30:052202 doi: 10.1116/1.4739424
[17]
Choi W K, Liew T H, Dawood M K. Synthesis of silicon nanowires and nanofin arrays using interference lithography and catalytic etching. Nano Lett, 2008, 11:3799 doi: 10.1021/nl802129f
[18]
Xie Zili, Zhou Yuanjun, Song Lihong, et al. Structural properties of GaN (0001) epitaxial layers revealed by high resolution X-ray diffraction. Physics, Mechanics & Astronomy, Science China, 2010, 53:68 doi: 10.1007/s11433-010-0102-5?slug=full%20text
[19]
Choi J H, Lee T Y, Choi S H, et al. Density control of carbon nanotubes using NH3 plasma treatment of Ni catalyst layer. Thin Solid Films, 2003, 435:318 doi: 10.1016/S0040-6090(03)00341-9
[20]
Jansen H V, de Boer M J, Unnikrishnan S. Black silicon method X:a review on high speed and selective plasma etching of silicon with profile control:an in-depth comparison between Bosch and cryostat DRIE processes as a roadmap to next generation equipment. J Micromech Microeng, 2009, 19:033001 doi: 10.1088/0960-1317/19/3/033001
[21]
Perlin P, Jauberthie-Carillon C, Itie J P, et al. Raman scattering and X-ray-absorption spectroscopy in gallium nitride under high pressure. Phys Rev B, 1992, 45:83 doi: 10.1103/PhysRevB.45.83
[22]
George S, Ilan S, Warren M, et al. Catalytic hydride vapour phase epitaxy growth of GaN nanowires. Nanotechnology, 2005, 16:2342 doi: 10.1088/0957-4484/16/10/058
[23]
Seo H W, Bae S Y, Park J H, et al. Strained gallium nitride nanowires. Chem Phys, 2002, 116:9492 doi: 10.1063/1.1475748
[24]
Zhao D G, Xu S J, Xie M H, et al. Stress and its effect on optical properties of GaN epilayers grown on Si (111), 6H-SiC (0001), and c-plane sapphire. Appl Phys Lett, 2003, 83:677 doi: 10.1063/1.1592306
[25]
Schnitzer I, Yablonovitch E, Caneau C, et al. 30% external quantum efficiency from surface textured, thin-film light-emitting diodes. Appl Phys Lett, 1993, 63:2174 doi: 10.1063/1.110575
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    Zengqin Lin, Xiangqian Xiu, Shiying Zhang, Xuemei Hua, Zili Xie, Rong Zhang, Peng Chen, Ping Han, Youdou Zheng. GaN nanopillars with a nickel nano-island mask[J]. Journal of Semiconductors, 2013, 34(12): 123001. doi: 10.1088/1674-4926/34/12/123001
    Z Q Lin, X Q Xiu, S Y Zhang, X M Hua, Z L Xie, R Zhang, P Chen, P Han, Y D Zheng. GaN nanopillars with a nickel nano-island mask[J]. J. Semicond., 2013, 34(12): 123001. doi: 10.1088/1674-4926/34/12/123001.
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      Zengqin Lin, Xiangqian Xiu, Shiying Zhang, Xuemei Hua, Zili Xie, Rong Zhang, Peng Chen, Ping Han, Youdou Zheng. GaN nanopillars with a nickel nano-island mask[J]. Journal of Semiconductors, 2013, 34(12): 123001. doi: 10.1088/1674-4926/34/12/123001 ****Z Q Lin, X Q Xiu, S Y Zhang, X M Hua, Z L Xie, R Zhang, P Chen, P Han, Y D Zheng. GaN nanopillars with a nickel nano-island mask[J]. J. Semicond., 2013, 34(12): 123001. doi: 10.1088/1674-4926/34/12/123001.
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      Zengqin Lin, Xiangqian Xiu, Shiying Zhang, Xuemei Hua, Zili Xie, Rong Zhang, Peng Chen, Ping Han, Youdou Zheng. GaN nanopillars with a nickel nano-island mask[J]. Journal of Semiconductors, 2013, 34(12): 123001. doi: 10.1088/1674-4926/34/12/123001 ****
      Z Q Lin, X Q Xiu, S Y Zhang, X M Hua, Z L Xie, R Zhang, P Chen, P Han, Y D Zheng. GaN nanopillars with a nickel nano-island mask[J]. J. Semicond., 2013, 34(12): 123001. doi: 10.1088/1674-4926/34/12/123001.

      GaN nanopillars with a nickel nano-island mask

      DOI: 10.1088/1674-4926/34/12/123001
      Funds:

      the National Natural Science Foundation of China 60936004

      the National Natural Science Foundation of China 61176063

      the Hi-Tech Research Project 2011AA03A103

      the Special Funds for Major State Basic Research Project 2011CB301900

      the National Natural Science Foundation of China 60990311

      the Natural Science Foundation of Jiangsu Province BK2011010

      the Special Funds for Major State Basic Research Project 2010CB327504

      the Special Funds for Major State Basic Research Project 2012CB619304

      Project supported by the Special Funds for Major State Basic Research Project (Nos. 2011CB301900, 2012CB619304, 2010CB327504), the Hi-Tech Research Project (No. 2011AA03A103), the National Natural Science Foundation of China (Nos. 60990311, 61274003, 60936004, 61176063), and the Natural Science Foundation of Jiangsu Province (No. BK2011010)

      the National Natural Science Foundation of China 61274003

      More Information
      • Corresponding author: Xiu Xiangqian, Email: xqxiu@nju.edu.cn
      • Received Date: 2013-04-25
      • Revised Date: 2013-06-24
      • Published Date: 2013-12-01

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