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Title: Optical properties of nanocrystal-silicon thin films on silicon nanopillar arrays after thermal
annealing

Article Type: Research Paper

Keywords: nanocrystal-silicon, nanopillar array, reflectivity, photoluminescence, solar cell

Corresponding Author: Dr. Bo Qian,

Corresponding Author's Institution: Suzhou Institute of Nano-Tech and Nano-Bionics(SINANO),

Chinese Academy of Sciences

First Author: YongLei Li

Order of Authors: YongLei Li; Bo Qian; Cong Li; Jun Xu; Chunping Jiang

Manuscript Region of Origin: CHINA

Suggested Reviewers: Liangcai Wu

Shanghai Institute of Microsystem And Information Technology
wuliangcai@mail.sim.ac.cn
Expert in silicon nanocrystal-based devices

Aleksei Anopchenko
University of Trento
anopchenko@science.unitn.it
Expert in silicon nanocrystals photonic devices including solar cell, light emitting diode.

Rui Huang
Department of Physics and Electronic Engineering, Hanshan Normal University
rhuangnju@126.com
Expert in silicon-based thin films and semiconductor nanowires
Cover Letter

Editor
Applied Surface Science
Sep.28, 2012

Dear editor:
We would like submit an original paper titled as “Optical properties of
nanocrystal-silicon thin films on silicon nanopillar arrays after thermal annealing
(Authors: Yonglei Li, Bo Qian*, Cong Li, Jun Xu, Chunping Jiang)” to Applied Surface
Science.

In this paper, the optical properties of nanocrystal-silicon thin films on silicon nanopillar
arrays after thermal annealing have been carefully studied. The results show the structure
have great potential to the design of solar cell devices.

The corresponding author is:

Bo Qian

Suzhou Institute of Nano Tech and Nano Bionics

Chinese Academy of Science
398 Ruo Shui Road,Suzhou Industrial Park
Suzhou,Jiangsu,215125
P.R.China
Phone: +86-512-6287-2727 (o)
+86-139-2198-7988 (m)
E-mail:bqian2010@sinano.ac.cn

Thank you very much for your help. It is greatly appreciated if you can give us
the suggestions and comments as soon as possible.

Best wishes!
Sincerely yours,

Bo Qian

Nano-devices and materials division

Suzhou Institute of Nano Tech and Nano Bionics

Chinese Academy of Science
398 Ruo Shui Road,Suzhou Industrial Park

Suzhou,Jiangsu,215125
*Highlights (for review)

Highlights:

 A combined structure fabricated by conformally assembling nc-Si film on a

periodic arranged silicon nanopillar array has been demonstrated.

 The reflectivity spectra of this combined structure have revealed a remarkable

reduction and the minimum reflectivity has been demonstrated to be 0.7%.

 By tuning thermal annealing temperature, this structure shows a wide-range

tunability of light emission efficiency of nc-Si, from big suppression to large

enhancement, compared with the referential flat sample. The maximum emission

suppression factor is 12.5 while the maximum enhancement factor is 8.8.

*Manuscript
Click here to view linked References

Optical properties of nanocrystal-silicon thin films on silicon

nanopillar arrays after thermal annealing

Yonglei Li1,2, Bo Qian1,3*, Cong Li3, Jun Xu3, Chunping Jiang1

1
Key Laboratory of Nanodevices and Applications, Suzhou Institute of Nano-tech and

Nano-bionics, Chinese Academy of Sciences, Suzhou 215125, P. R. China

2
University of Chinese Academy of Sciences, Beijing 100049, P. R. China

3
Nanjing National Laboratory of Microstructures and Key Laboratory of Advanced Photonic and

Electronic Materials, Department of Physics, Nanjing University, Nanjing 210093, P. R. China

* E-mail: bqian2010@sinano.ac.cn

Abstract:
The optical properties of nanocrystal-silicon (nc-Si) thin films on silicon

nanopillar arrays after thermal annealing treatments have been investigated in this

paper. The structure was prepared by SiO2 nanosphere lithography, reactive-ion

etching, conformal deposition method and thermal annealing treatment, successively.

The thickness of nc-Si thin film is about 100 nm, while the diameter, period and

height of silicon nanopillar arrays are about 250 nm, 500 nm and 1 µm, respectively.

By reflectivity and photoluminescence (PL) spectroscopy measurements in visible to

near-infrared wavelength range, the minimum reflectivity of about 0.7% has been

demonstrated in such kind of structure, meanwhile, a large variation (from 12.5 times

of suppression to 8.8 times of enhancement compared to the flat referential thin films)

of the light emission efficiencies of the samples depending on the thermal annealing

temperatures has been observed, which is due to the temperature dependent

modification of optical constants of nc-Si thin films. By combining the nc-Si with
silicon nanopillar arrays, the structure will be very promising for the design of radial

p-i-n junction solar cell devices.

Keywords: nanocrystal-silicon, nanopillar array, reflectivity, photoluminescence,

solar cell.
1. Introduction

Silicon nanostructures, including silicon nanocrystals (nc-Si) [1-5] and

nanowires (SiNWs) or nanopillars [6], are promising candidates for next generation

solar cells with higher energy conversion efficiencies and lower cost. In nc-Si, it has

been observed that there is carrier multiplication by generation of two or more

electron-hole pairs following the absorption of a single photon [1]. This may lead to

improved photovoltaic (PV) efficiencies, which is close to the energy conservation

limit [2]. Meanwhile, SiNWs or nanopillar arrays are also very attractive for energy

conversion for the new generation photovoltaic technology, since the structure’s

extraordinary light-trapping path length enhancement factor is above the randomized

scattering (Lambertian) limit [7-10] and is superior to other light trapping methods.

Furthermore, the design of radial p-n junction structures on silicon nanopillars by

conformal deposition method provide short travel distances of photo-excited minority

carriers to the collection electrodes, leading to enhanced carrier-collection efficiency

and minimum bulk recombination [11-13]. Another advantage of the radial geometry

is the high tolerance of PVs for material defects, permitting the use of lower-quality

Si with shorter minority-carrier diffusion lengths [6].

Therefore, it will be interesting to combining nc-Si and silicon nanopillar arrays

to realize solar cell devices to achieve higher PV efficiencies [14], and the radial p-i-n

junction geometry will be a suitable design [11]. Different from the previous work [11]

on single SiNW, in this paper, a hybrid structure of nc-Si thin films and Si nanopillar

arrays were prepared by conformal deposition method. The optical properties

including reflectivity spectra and photoluminescence spectra of such structures with

different thermal annealing temperatures have been investigated. This work will be a

promising step to the design of nc-Si based photonics devices.

2. Experimental Details

The samples were fabricated by five steps as following: (I) Self-assembling of a

close-packed 500 nm SiO2 nanosphere monolayer was performed on a clean Si wafer

by dip-coating method [7, 9]. The volume percent (V%) of SiO2 nanospheres in ethyl

alcohol is 3～5%. (II) Si nanopillar array was formed by nanosphere lithography

technology [15] and an inductively coupled-plasma deep reactive-ion-etching

(ICP-DRIE) process. The selective and anisotropic etching process was based on

fluorine chemistry using a mixture gas of C4F8, SF6 and O2, with the flux ratio of

80sccm:70sccm:5sccm. (III) The remained nanospheres were selectively wiped off

from the tips of the pillars by a buffered HF solution. (IV) 100 nm-thick Si-rich SiOx

(x<2 ) film was deposited conformably upon the nanopillar array to construct the final

combined structure by plasma enhanced chemical vapor deposition (PECVD) [16]

with the reaction gas flux ratio here is SiH4/N2O/Ar=35sccm/710sccm/180sccm. Note

that the same film was also deposited on flat Si wafer for reference. (V) To form nc-Si,

all the samples were annealed at temperatures of 1100 ℃, 1150℃, 1200℃, 1250 ℃,

respectively, for 30 min in N2 protection, which is a usual way to prepare Si

nanocrystals [17, 18].

The samples’ surface morphologies and sizes were characterized by Hitachi

S4800 scanning electron microscope (SEM) in the whole process. High-resolution

transmission electron microscopy (HRTEM) was also performed to confirm the

existence of nc-Si. To study the optical properties, room-temperature

photoluminescence (PL) spectra of our samples, excited by a He-Cd 325nm laser and

received by a CCD detector, were performed and analyzed with a grating

monochromator. The reflectivity spectra of nc-Si films on flat Si wafers and on

nanopillar arrays were also measured. The refractive index of nc-Si films on flat

referential substrates was measured by J.A.Woollam M-2000 ellipsometer.

3. Results and Discussion

Figure 1 gives the structure details in SEM images for each fabrication step. It

can be confirmed in Fig. 1(a) that the large area, close-packed, hexagonal SiO2

nanosphere monolayer has be produced by dip-coating. Although minority line and

point defects exist, they are negligible compared to the whole area. After 4 minute

ICP-DRIE process, the pattern of SiO2 nanosphere monolayer was transform into

silicon nanopillar arrays as shown in Fig. 1(b). The size of SiO2 nanospheres on

nanopillars is reduced after etching. Following the nanosphere mask, the period of

nanopillar arrays is about 500 nm. The pillar arrays after wiping off the SiO 2

nanospheres are presented in Fig. 1(c). The diameter and height of each nanopillar is

about 250 nm and 1 µm respectively. From the inset of Fig. 1(c), the bottom of pillar

array is observed relatively larger than the other part, just like a collar around it. This

is probably due to the etching gas distribution between nanopillars. Fig. 1(d) shows

the final structure after depositing 100 nm SiOx film on pillar array. The height of

each pillar remains 1 µm while the diameter increases to about 330 nm, from which

thickness of nc-Si film along the radial direction can be calculated to be about 40 nm,

which means the lateral growth rate of the film is largely reduced. Note that the

roughness of pillars is increased because of the conformal growth effect. However,

such roughness has been proved to increase the electrical injection efficiency [6].

To study the basic structure and optical properties of nc-Si thin films, the TEM

and ellipsometry measurement were performed with the referential nc-Si thin films on

flat Si wafers. Fig. 2(a) presents a typical TEM picture of a nc-Si thin film sample, in
which nc-Si was obtained after 1200 ℃ thermal annealing. The average size of the

nc-Si is about 3.5nm. Fig. 2(b) illustrates the evolution of refractive index for SiOx

film on flat substrate annealed at different temperature. In the spectrum ranging from

350 nm to 1000 nm, it can be clearly observed that there is a monotonic decreasing of

the refractive index when increasing the annealing temperature, which indicates

increasingly widen of the optical band gap of the SiOx film [19-21]. This can be due

to continuously decrease of the degree of disorder of the thin film, caused by the

formation of nc-Si in it [22].

To demonstrate the extraordinary light trapping ability of Si nanopillar arrays

[7-10], the reflectivity spectra of samples with the same nc-Si films on flat Si wafer

and on nanopillar arrays at different annealing temperature were measured for

comparison. Fig. 3(a) illustrated the results of the sample annealed at 1250℃. It can be

observed that the main band in the reflectivity spectra of the nc-Si film on flat wafers

is ranging from 300nm to 650nm, the maximum value is about 20.5% at around

375nm; for the wavelength longer than 650nm, the reflectivity is lower than 8%. For

the samples on nanopillar arrays, the reflectivity band of flat samples vanishes and the

reflectivity at 375nm is reduced to 1.4%, about 15 times reduction. The minimum

reflectivity of the nanopillar samples is about 0.7% at about 550 nm, while the whole

reflection spectra is lower than 3%. Fig. 3(b) shows the maximum and minimum

reflectivity in all the reflectivity spectra for samples annealed at different

temperatures. It can be observed that, for flat samples, the maximum of the

reflectivity is increasing from 12.8% to 21.9% with improving annealing temperature,

while the minimum of reflectivity is increasing from 2.4% to 4.3%. For nanopillar

array samples, the maximum value of reflectivity is decreasing from 2.4% to 1.5%,
while the minimum reflectivity is, almost stay the same, lower than 1.0%. The results

demonstrate such kind of structure on nanopillar arrays is very suitable for solar cell

applications.

Fig. 4(a) shows the schematics of the optical setup for PL measurements. The

position of CCD detector is carefully adjusted to avoid the collection of input laser

light, though at this condition it only can get part of the emission information.

Following parts of Fig. 4 present the PL spectra of the nc-Si films on nanopillar arrays

annealed at different temperatures meanwhile those of the same nc-Si films on flat Si

substrates are also presented for references. From Fig. 4(b-e), two main emission

bands centered around 430 nm and 790 nm can be observed in almost all of the

samples, except the flat sample annealed at 1100℃ in Fig. 4(b). The peak at around

430nm is commonly attributed to the recombination at an oxygen-related defect state

(O-Si-O) [23, 24] related to nc-Si in SiO2 matrices [18, 25-27]. The peak at around

790 nm in the near-infrared is generally assigned to the excitonic emission [28, 29]

from Si=O state [30, 31] on the surface of nc-Si [18]. It should be noted that the peak

shift in Fig. 4(b) from flat sample to the related nanopillar structure is probably due to

the change of nc-Si size on the related combined structure at the lowest annealing

temperature of 1100 ℃.

Interestingly, it can be observed in Fig. 4(b-e) that the combined nanopillar array

structure shows a rather large tunability to the emission efficiency of nc-Si by

controlling the annealing temperature. When annealed at 1100 ℃, as described in Fig.

4(b), the PL intensity of the combined structure shows a big suppression compared

with the related flat sample, with the maximum suppression factor of 12.5 at 670 nm.

It acts as a role of inhibiting or trapping light emission, just like the anti-reflection
surface for solar cells. At 1150 ℃ in Fig. 4(c), the structure increases a little bit of the

emission intensity at around 430 nm, while oppositely decreases that at around 800

nm. When annealing temperature increases to 1200 ℃ in Fig. 4(d), the structure

slightly reduces the intensity for both of the main emission bands above. At the

highest annealing temperature of 1250 ℃, comparison between the PL lineshapes of

the both reveals that the structure possesses a tremendously large enhancement ability.

For the emission band centered around 430 nm, emission intensity of this combined

structure is about 8.8 times as tall as that of the flat sample, while for the band at

around 800 nm, the enhancement factor is about 5.5.

As the monotonic decrease of refractive index of nc-Si films when increasing

annealing temperature shown in Fig. 2(b), Tunable PL efficiency on this combined

nanopillar structure in Fig. 4(b-e) is probably related to the dynamic optical periodic

modification of our nanopillar array with nc-Si conformal film on it when annealed at

different temperatures. The results are very important and helpful for the design of

nc-Si based photonic devices [32].

4. Conclusion

We have demonstrated a combined structure fabricated by conformally

assembling nc-Si film on a periodic arranged silicon nanopillar array. By tuning the

thermal annealing temperature, photoluminescence behavior of such kind of structure

shows a wide-range tunability of light emission efficiency of nc-Si, from big

suppression to large enhancement, comparing with the referential flat sample. The

maximum emission suppression factor is about 12.5 meanwhile the maximum

enhancement factor is 8.8. The reflectivity spectra of this combined structure have

revealed a remarkable reduction and the minimum reflectivity has been demonstrated
to be 0.7%, which shows a great potential application for the design of solar cell

devices.

Acknowledgment

The author is grateful to Nanofabrication Facility of Suzhou Institute of

Nano-tech and Nano-bionics (SINANO) for the device fabrication. This work is

supported by “973” project (No. 2010CB934100) and NSFC (No. 61107091).

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Figure(s)
Click here to download Figure(s): Figures_Yonglei Li.doc

Captions:

Figure 1: Real-time monitoring of our combined structure by SEM images during the

whole fabrication process. (a) Closely self-assembled nanosphere monolayer via

dip-coating. (b) Nanopillar array with spheres on the tips after ICP-DRIE. (c)

Nanopillar array after removal of the residual mask. (d) Final combined structure after

depositing a layer of nc-Si film upon pillar array. The inset of each picture is the

sectional view. Scale bar of the inset is 1 µm.

Figure 2: (a) High resolution TEM image of the nc-Si film annealed at 1200℃. The

visible Silicon nanocrystals are highlighted by circles for clarity with average size

about 3.5nm. (b) Curves of refractive index of nc-Si thin films deposited on flat Si

wafers with different annealing temperatures.

Figure 3: (a) Reflectivity spectra of the nc-Si thin films on flat Si wafer (represented

by squares) and on nanopillar array (represented by circles). Both the samples were

annealed at 1250℃. (b) The maximum and minimum reflectivity of all the reflectivity

spectra for samples annealed at different temperatures.

Figure 4: Schematic diagram of PL testing (Fig. (a)) & Comparison of PL lineshapes

between the same nc-Si film deposited on flat Si wafer and our nanopillar array. Films

were annealed at (b) 1100℃, (c) 1150℃, (d) 1200℃ and (e) 1250℃, respectively.
Figure 1

Yonglei Li et al
Figure 2

1.58
o o
Annealed at 1100 C Annealed at 1150 C
o o
1.56 Annealed at 1200 C Annealed at 1250 C
Refractive index

1.54

1.52

1.50

1.48

1.46

300 400 500 600 700 800 900 1000

Wavelength (nm)

Yonglei Li et al
Figure 3

22
20 nc-Si film on flat Si wafer
nc-Si film on nanopillar array
18
16 375nm
20.5%
Reflectivity(%)

14
12
10
8
6 375nm, 1.4%
4 550nm, 0.7%
2
0
300 400 500 600 700 800 900 1000
Wavelength(nm)

20

16
Reflectivity(%)

nc-Si film on flat wafer, min value

12
nc-Si film on flat wafer, max value
nc-Si film on nanopillar array, min value
8 nc-Si film on nanopillar array, max value

0
1100 1150 1200 1250
O
Annealing temperature ( C)

Yonglei Li et al
Figure 4

o
Annealed at 1100 C nc-Si on flat wafer
nc-Si on nanopillar array
4000
Intensity (a.u.)

2000

0
400 600 800 1000
Wavelength (nm)

Yonglei Li et al
Figure 4

o
Annealed at 1150 C nc-Si on flat wafer
800 nc-Si on nanopillar array
Intensity (a.u.)

600

400

200

400 600 800 1000

Wavelength (nm)

o
Annealed at 1200 C nc-Si on flat wafer
nc-Si on nanopillar array
1000
Intensity (a.u.)

500

0
400 600 800 1000
Wavelength (nm)

Yonglei Li et al
Figure 4

4000 o
Annealed at 1250 C nc-Si on flat wafer
nc-Si on nanopillar array
3500

3000
Intensity (a.u.)

2500

2000

1500

1000

500

400 600 800 1000

Wavelength (nm)

Yonglei Li et al