Porosity and thickness effect of porous silicon layer on photoluminescence spectra

F. S. Husairi, K. A. Eswar, Muliyadi Guliling, Z. Khusaimi, M. Rusop, and S. Abdullah

Citation: AIP Conference Proceedings 1963, 020060 (2018); doi: 10.1063/1.5036906

View online: https://doi.org/10.1063/1.5036906
View Table of Contents: http://aip.scitation.org/toc/apc/1963/1
Published by the American Institute of Physics
 Porosity and Thickness Effect of Porous Silicon Layer on
Photoluminescence Spectra

F.S. Husairi1,2,*, K.A. Eswar1,2, Muliyadi Guliling1,2,4, Z. Khusaimi1,2, M. Rusop1,3,

S. Abdullah1,2

NANO-SciTech Centre (NST), Institute of Science;

1
2
Faculty of Applied Sciences;
3
NANO-ElecTronic Centre (NET), Faculty of Electrical Engineering;
Universiti Teknologi MARA (UiTM),
40450 Shah Alam, Selangor, Malaysia
4
Faculty of Applied Sciences, Universiti Teknologi MARA (UiTM), Cawangan Kota Kinabalu, Sabah, Malaysia

a)
Corresponding author: mhusairifadzilah@yahoo.com

Keywords: Porous silicon; current density; porosity, thickness; photoluminescence

Abstract. The porous silicon nanostructures was prepared by electrochemical etching of p-type silicon wafer. Porous silicon
prepared by using different current density and fix etching time with assistance of halogen lamp. The physical structure of porous
silicon measured by the parameters used which know as experimental factor. In this work, we select one of those factors to
correlate which optical properties of porous silicon. We investigated the surface morphology by using Surface Profiler (SP) and
photoluminescence using Photoluminescence (PL) spectrometer. Different physical characteristics of porous silicon produced
when current density varied. Surface profiler used to measure the thickness of porous and the porosity calculated using mass
different of silicon.
Photoluminescence characteristics of porous silicon depend on their morphology because the size and distribution of pore its
self will effect to their exciton energy level. At J=30 mA/cm2 the shorter wavelength produced and it followed the trend of
porosity with current density applied.

INTRODUCTION
Porous silicon nanostructure (PSiN) is a interesting material because their large ratio of surface area to volume
[1], high chemical reactivity at room temperature [2] and potential compatibility with silicon integration
technologies [3]. PSiN is a material that produced on silicon wafer. It can prepared by using electrochemical
anodization etching technique [4], stain etching processes in hydrofluoric acid-based solution [5] and a hydrothermal
etching technique in a hydrofluoric acid free solution [6].
Porous silicon is an interesting material in sensor field because it had a high sensitivity because of its very large
specific surface area and possesses the capability in term of device integration [7, 8]. The surface of PSiN influences
the optical [9, 10] and electrical [11-13] behavior. Based on that, morphological properties of PSiN can be goes

8th International Conference on Nanoscience and Nanotechnology 2017 (NANO-SciTech 2017)

AIP Conf. Proc. 1963, 020060-1–020060-5; https://doi.org/10.1063/1.5036906
Published by AIP Publishing. 978-0-7354-1668-0/$30.00

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under surface modification that are useful for any application explored. The physical properties of PSiN can be
varied by control the etching parameters, such as, current, etching time, HF concentration, doping level and type. In
this work, we prepared PSiNs by using photo-electrochemical etching method with hydrofluoric acid (HF) and
ethanol as a based electrolyte. We have used its tunable morphology to understand the electrical activity of porous
silicon. Before this we already report the surface morphology effect to the electrical properties of PSiNs [16]. In this
paper, we test characterized samples using Photoluminescence (PL) spectrometer.

METHODOLOGY

PSiN is prepared by using electrochemical etching method and [100] of p-type Si wafer with 0.4-2 Ω cm
resistivity and 330±40 µm thickness used as a sample. A square dimension approximately 2 cm on an edge is
cleaved and placed in cell using a piece of aluminum foil as a back contact and a small O-ring to seal the wafer to
the cell. The etching process is set up at various current densities (20 - 40 mA/cm2) with a constant anodization time,
20 minutes. Then the sample is prepared by anodization ethanoic hydrofluoric acid (HF) 48% electrolyte and
absolute ethanol (C2H5OH) at ratio 1:1 with illumination by halogen lamp. The halogen lamp used to accelerate
etching process during the preparation of sample. After the preparation of PSiN done, the sample was clean with
distilled water and it dried by using nitrogen gas.

Tungsten rod
(cathode)

Teflon cell

O-ring

Silicon wafer

Aluminum base
(anode)
FIGURE 1. Experimental set-up of electrochemical etching.

The thickness of the porous silicon was investigated using Surface Profiler (SP) and photoluminescences using
Photoluminescences (PL) spectrometer brand Modu – Laser PL which used He-Cd Laser 325 as a laser source.

RESULTS AND DISCUSSION

Pores formation in silicon during anodization process had grab a lot attention and give rise to many theories
proposed [4, 17, 18]. Generally, the porous silicon formation is a result of inhomogeneous dissolution porous silicon
surface by HF solution. During the electrochemical etching, the effect of chemical dissolution is increase porosity
and pore radii. The porosity of porous silicon comes out by using different mass percentage calculation.
𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚1 − 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚2
𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃 (%) = × 100%
𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚1 − 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚3

Mass1 is a mass of silicon before etch, mass2 is a mass of silicon after etch and mass3 is a mass of silicon after
porous removed. The variation porosity and thickness of samples prepared with different current density applied is
presented in Table 1.

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 TABLE 1. Current density effect to porosity and thickness of porous silicon formed.
Current density, Porosity (%) Thickness (µm)
J (mA/cm2)
20 71.43 5.86
25 77.91 5.51
30 82.35 5.56
35 80.65 5.29
40 78.10 5.47

We can see that porosity of PSiNs depends on current density applied, increasing current density reaching
roughly saturation, which seem at J= 30 mA/cm2 (Fig. 1). The increasing PSiNs porosity refers to smaller the size of
silicon pillar. Thereafter, porous silicon develops cracks and some small pores start to form again. There appears to
be a relationship behavior of the etching process. The thickness of the PSiNs samples is consistent because constant
time applied during the etching process (in Table 1). Actually the thickness more effect by anodization time.

FIGURE 2. Porosity and thickness dependence of p-type PSiNs samples to current density applied.

Photoluminescence spectra of the PSiNs samples are presented in Fig 3 below. We see that the PL shift to
shorter wavelength with increased current density applied. The minimum wavelength produced is at J=25 and 30
mA/cm2 at 664.2159 nm. This behavior confirms the porosity calculated, and it consistent to quantum confinement
mechanism which tell that when PSiNs porosity increases the mean size of silicon nanopillar (diameter of pillar)
decrease and the PL maximum shift toward to the blue. It back to red shift when the porosity turn to lower value. It
cause by the distribution of smalls pillar reform on surface.

FIGURE 3. PL emission of porous silicon on different current density used: (a) 20, (b) 25, (c) 30, (d) 35 and (e) 40 mA/cm2.

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 The relationship photoluminescence spectra and current density presented by graph plotted in Fig 4 below.
At the same anodization time, similar morphology for a broad range of current densities produced; that increasing in
porosity produced the small blue shift of the PL maximum. This same with reported by Milani group [19]. The
luminescence show increasing patent by current density applied. Actually, a few theories reported to explain the
mechanism of photo emission such as quantum confinement, charge accumulation, surface distribution etc. By that
graph, we can see that the intensity increase by current density applied. During the anodization process, electrons
from bulk silicon will accumulate at interface between silicon surface and electrolyte (HF solution). So, we believe
that, the intensity of luminescence affected by charge accumulation at the silicon pillar after etching process.

FIGURE 4. Graph effect of current density to wavelengths and intensity of photoluminescence spectra.

From the PL result, we can calculate its band gap energy. The peak position will determined the value of band gap.
Cause sample prepared at J=25 and 30 mA/cm2 had shorter wavelength, automatically it’s have highest bandgap
energy, 1.8704 eV.

TABLE 2. The bandgap energy of PSiNs samples calculated by PL spectra at various current densities applied.
Current density, J (mA/cm2) Band Energy, E (eV)
20 1.8695
25 1.8704
30 1.8704
35 1.8687
40 1.8531

CONCLUSION
Porous silicon successful fabricated by using anodization etching method at different current density
applied. We have found that the porosity of porous silicon can be calculated by using percentage mass different
method. The porosity linearly relation with current density applied with porosity highest at J=30 mA/cm2 (82.35%).
The thickness of PSiNs samples almost consistent which at around 5.5 – 5.7 µm. Samples with current density 25
and 30 mA/cm2 posses’ highest energy compare to other.

ACKNOWLEDGEMENT
The authors would like to thank UniversitiTeknologi MARA and also Malaysia Ministry of Higher Education for
their support and funding from I-Rags Grant, file no: 600-RMI/IRAGS 5/3 (20/2015). Thanks to NANO-Scitech
Centre and NANO-Electronic Centre colleagues for their helpful support and encouragements

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