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Sulfide assisted growth of silicon nano wires by thermal evaporation of sulfur powders

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Đây là một bài báo khoa học về dây nano silic trong lĩnh vực nghiên cứu công nghệ nano dành cho những người nghiên cứu sâu về vật lý và khoa học vật liệu.Tài liệu có thể dùng tham khảo cho sinh viên các nghành vật lý và công nghệ có đam mê về khoa học

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Physica E 24 (2004) 278–281

Sulfide-assisted growth of silicon nano-wires by

thermal evaporation of sulfur powders Junjie Niua, Jian Shaa,b, Deren Yanga,*

a

State Key Lab of Silicon Materials, Zhejiang University, Hangzhou 310027, People’s Republic of China

b Department of Physics, Zhejiang University, Hangzhou 310027, People’s Republic of China

Received 23 March 2004; accepted 11 May 2004 Available online 10 July 2004

Abstract

Silicon nanowires (SiNWs) with a diameter of B20 nm were synthesized by the thermal evaporation of sulfur powders on silicon wafers The source of the SiNWs came from the silicon substrates It is considered that the generated SiS compound assisted the formation of SiNWs Finally, the Raman shift of SiNWs was discussed

r2004 Elsevier B.V All rights reserved

PACS: 71.55.Cn; 81.05.Ys

Keywords: Silicon; Nanowires; Sulfide assisted

1 Introduction

Recently the one-dimensional nano-materials,

especially silicon nanowires (SiNWs), have

stimu-lated much interest because of their different

properties in comparison with the corresponding

bulk materials [1–6] Several synthesized methods

for SiNWs have been reported, including laser

ablation[7], chemical-vapor-deposition (CVD) via

vapor–liquid–solid (VLS) mechanism[8–13],

ther-mal evaporation via oxygen-assisted [14–17] and

solid–liquid–solid (SLS) mechanisms [18–20], and

electronic-chemical method[21]

In this paper, the thermal evaporation of sulfur powders on silicon wafers used to grow SiNWs is reported Compared with the other approach, this process was simple and the source of SiNWs was from the silicon wafer substrates but not from the silane gas [11]

and silicon oxide [14,17] It is also found that sulfide played an important role in the formation

of SiNWs, therefore, a sulfide-assisted growth mechanism was suggested In the experiments, the samples were checked by filed emission scanning electron microscopy (FESEM), transmis-sion electron microscopy (TEM), and X-ray diffraction (XRD), respectively Finally, the Ra-man spectroscopy was also used to investigate the SiNWs

*Corresponding author Tel./fax: +86-571-879-523-22.

E-mail address: mseyang@zju.edu.cn (D Yang).

1386-9477/$ - see front matter r 2004 Elsevier B.V All rights reserved.

doi:10.1016/j.physe.2004.05.002

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2 Experimental

SiNWs were produced on p-type (1 1 1) silicon

wafers with a resistivity of about 0.001 O cm by

means of a low-vacuum CVD system First,

several pieces of silicon wafers and plenty of sulfur

powders were placed in a semi-sealed alumina boat

which was put at the center of a horizontal quartz

tube furnace Then the furnace was evacuated to

reach 30 Pa by a mechanical pump The

tempera-ture of the system was then raised to 900C at a

heating rate of 25C min1and continually up to

1250C at a heating rate of 10C min1, and held

at 1250C for 30 min at a constant pressure of

30 Pa After reaction, the weak black and yellow

substrates with the as-grown materials were

removed from the furnace and characterized by

FESEM (FEI, Sirion), TEM (JEOL, JEM200CX),

XRD (Rigaku, D/MAX-rA), and Raman

scatter-ing spectroscopy (Nicolet Almega), respectively

The possible chemical composition of the

as-grown materials on the wafers was investigated

by using energy-dispersive X-ray spectroscopy

(EDX) attached to the FESEM

3 Results and discussion

The FESEM morphology of the SiNWs with a

diameter ofB20 nm (that of a very few SiNWs is

over 50 nm) is shown inFig 1 The EDX (the inset

ofFig 1) taken from the corresponding nanowires

indicates that the nanowires were silicon

How-ever, oxygen could also be detected The oxygen is

considered to have come mainly from the surface

oxidation of nanowires This suggests that the

nanowires were composed of silicon and silicon

oxide as sheath Actually, some SiNWs could be

oxidized to be silicon oxide nanowires because of

the low-vacuum system and high temperature, as

found in our previous work[6] The TEM image of

a number of curved SiNWs is shown in Fig 2 It

can be seen that the average diameter of the

SiNWs wasB20 nm, while the minimum one was

less than 10 nm The structure of the SiNWs is

indicated by the selected area electric diffraction

(SAED) image in the top right ofFig 2 The weak

electric diffraction spots proved that the SiNWs

did not crystallize well This might be due to the fast growth rate of the SiNWs The thorough analysis of crystal nature is indicated by the XRD data as shown in Fig 3 The sharp peaks of Si (1 1 1), Si (3 1 1), Si (4 0 0), and Si (3 3 1) indicates that the SiNWs were crystalline Some crystal Al peaks and low-intensity peaks of SiS2 (3 0 1) and SiS (2 1 3) are simultaneously observed Al peaks

Fig 1 FESEM image of the SiNWs on a silicon wafer The lower left inset is the EDX taken from the corresponding sample.

Fig 2 TEM image of the SiNWs The top right inset is the SAED taken from one of the SiNWs On top left is the magnified TEM image of a SiNW with tip.

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come from the sample preparation process for

the XRD analysis, while SiS2comes mainly from

the decomposition of SiS The discussion of the

growth mechanism is displayed below

As the function of silicon oxide in the

oxygen-assisted mechanism [15,16], in our experiments,

the silicon sulfide (SiS) also played a key role

in assisting the growth of SiNWs Therefore, a

sulfide-assisted model for SiNW growth is

sug-gested here

The reaction procedure mainly took two steps

One was that the sulfur reacted with the silicon

substrate and generated SiS compound at the

lower temperature (B900C) The next step was

that the SiS decomposed to be Si and SiS2 at

higher temperature (B1000C) During the

de-composition, SiNWs grew up from the generated

Si as source The reaction equations are shown

below

S þ O2 ¼ SO2m ð1Þ

S þ Si ¼ SiS ðB900CÞ ð2Þ

2SiSm ¼ Si þ SiS2 ðB1000

and

SiS2þ 2H2O ¼ SiO2þ2H2Sm: ð4Þ

When the temperature reached B900C, Eq (2)

happened and the SiS film was produced

Con-tinually, the SiS is decomposed into Si and SiS at

higher temperature (B1000C), which could be confirmed by the XRD spectrum in Fig 3 Therefore, it is believed that the SiNWs generated from the SiS acted as nucleation centers which were located at the tip of the SiNWs, as shown in the top left ofFig 2 Thus, the tip should contain SiS2 But there was no S signal in the EDX spectrum (the inset ofFig 1) and only weak SiS2

peaks are displayed in XRD data (Fig 3) This is because the SiS2 could sublimate and disappear when the temperature was higher than 1090C Furthermore, SiS2 was also easy to react with

H2O, which exists in air, as illustrated in Eq (4) Surely, not only SiS but also other sulfides such

as zinc sulfide, ferric sulfide, etc, which form silicon sulfides by the reaction with silicon, can also be used to assist the growth of SiNWs In principle, all of silicon compounds, such as silicon sulfide shown in this paper and silicon oxide [17], can assist the formation of SiNWs It is called the silicon compound-assisted mechanism for SiNWs growth

The SiNWs and bulk silicon in comparison were also checked using Raman spectroscopy (Fig 4)

It is clear that the 510.5 cm1 peak of the SiNWs (Fig 4(a)) shows a B10 cm1 downshift compared with the 520.3 cm1peak of bulk silicon (Fig 4(b)) Usually, the peak of 510.5 cm1 was regarded to be the first-order transverse optical phonon mode (TO) The downshift might be

0

500

1000

1500

2000

Al(111) Al(200) SiS2(213) SiS2(301)

Al(220)

Al(311) Si(331) Si(400)

Si(311) Si(111)

2 θ (degrees)

Fig 3 XRD spectrum of the as-grown SiNWs.

0 1000 2000 3000 4000

b

a 510.5cm -1

520.3cm -1

Raman Shift (cm-1) Fig 4 Raman spectra of SiNWs (a) and bulk silicon (b).

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associated with the quantum confinement effect

and laser heating effect [22,23]

4 Conclusion

In summary, silicon nanowires (SiNWs) with a

diameter ofB20 nm were successfully synthesized

on silicon wafers by thermal evaporation of sulfur

powders It is considered that the decomposition

of SiS resulted in the formation of SiNWs

Furthermore, a sulfide-assisted growth model of

SiNWs was suggested At last, the Raman shift of

SiNWs was also discussed

Acknowledgements

This work was supported by the National

Natural Science Foundation of China (Nos

50272057 and 60225010) and the Key Project

of Chinese Ministry of Education The authors

would like to thank Prof Youwen Wang and

Mr Z.C Chen for their great help in the

measurements of TEM and Raman spectroscopy

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