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7/28/2019 PL Spectra and Structure of Porous Si
1/6
Semicond. Sci. Technol. 11 (1996) 18151820. Printed in the UK
Correlation of photoluminescence
spectra and structure of porous
silicon
B Bessas, H Ezzaouia, H Elhouichet, M Oueslati andR Bennaceur
Institut National de Recherche Scientifique et Technique, USI, Laboratoire dePhotovoltaque et des Materiaux Semiconducteurs, BP 95, 2050 Hammam-Lif,Tunisia Laboratoire de Spectroscopie Raman, Departement de Physique, Faculte desSciences de Tunis, 1006 Le Belvedere, Tunis, Tunisia Laboratoire de Physique de la Matiere Condensee, Department de Physique,Faculte des Sciences de Tunis, 1006 Le Belvedere, Tunis, Tunisia
Received 23 April 1996, accepted for publication 5 August 1996
Abstract. Porous silicon (PS) layers emitting red photoluminescence (PL) have
been prepared by anodization of p-type (100) monocrystalline silicon substrate inaqueous HF solutions. PS layers oxidized in free air exhibit under UVphotoirradiation an intense yellow-orange PL, whilst as-prepared samples emit redPL. Our aim is to explain the PL behaviour and its origin in both unetched and HFetched as-prepared and oxidized PS layers according to calculated PL based onquantum confinement formalism and to infrared spectroscopy (IRS). It was foundthat the PL behaviour is associated with a quantum size effect and concentrationchange in quantum dots and wires. It was observed that HF etching of oxidized PSmay induce a preponderance of dots or wires in the PS structure, depending on theoxidation degree, and produce a PL blueshift or redshift respectively. By correlatingPL spectra of unetched and HF-etched oxidized PS, we found that highly oxidizedPS transforms into an SiO2 matrix in which photoluminescent nanocrystalline Siquantum dots are embedded.
1. Introduction
Recently, significant attention has been focused on porous
silicon (PS) owing to its visible photoluminescence (PL)
at room temperature [1]. The first visible PL in porous
silicon was obtained by Pickering et al [2], but it was not
until 1990 that Canham pointed out the importance of this
surprising phenomenon [1].
The mechanism of PL in PS remains unclear, and as
yet there has been no universal agreement on its origin.
PS is formed by electrochemical etching of single-crystal
silicon in hydrofluoric acid (HF), and it was found to
be composed of silicon nanocrystallites [3] covered by
hydrides or polysilanes [4, 5], amorphous silicon and silicondioxide [6]. Thus, the disagreement about the origin of the
PL may be due to the structure and the composition of
PS, which are difficult to control and thus difficult to know
with certainty. However, the quantum size effect in silicon
nanocrystallites [1, 7] is the hypothesis most often used to
explain such PL from an indirect-bandgap semiconductor.
HF chemical etching has been widely used [1, 4, 8] to
determine the effect of the different structures existing in
PS on its emission properties. Indeed, concentrated HF
attacks bulk 111 n-type Si at a rate of 18 A h1 [9]
and easily removes amorphous hydrogenated silicon at a
relatively high rate ( 100 A h1 for unannealed films and40 A h1 for partially annealed films [10]). Furthermore,silicon oxides are easily removed by HF etching.
Several experiments using different oxidation meth-
ods [8, 11] have been used to passivate the highly reactive
PS surface and to determine the origin of the PL. Both HF
etching and oxidation produce a structural change in PS,
inducing a PL blueshift [11] or redshift [4], and this raised
many controversies regarding the PL origins. In this paper
we try to clear up these controversies. We report results
concerning the effect of HF etching and natural oxidation
assisted by UV photoirradiation on the PL behaviour and
structure of PS. The PL behaviour is correlated with the
PS structure, based on calculation of PL spectra and on
infrared spectroscopy (IRS).
2. Experiment
The PS layers are obtained by anodization in aqueous
HF solution of (100)-oriented, boron-doped p-type silicon
substrates of resistivity 11.5 cm. The samples have
a polished mirror-like surface. Screen-printed Al/Ag thick
0268-1242/96/121815+06$19.50 c 1996 IOP Publishing Ltd 1815
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B Bessas et al
film or eutectic GaIn were used as the contact on the back
side of the Si wafers to ensure uniform current distribution.
In order to control the experimental conditions, and hence
the porosity of the PS layers, we used the diagram given by
Zhang et al [12] which depicts the critical current densities
as a function of HF concentration. The PS samples were
anodized in the dark in 3% HF solution (prepared from
49% HF and deionized water) at a constant current density
of 5 mA cm2 for a period of 20 min; the resultant porosity
(the ratio of pore volume to the total volume in the anodizedSi region) of the PS layer, determined by the gravimetric
method [13], is about 80%. As-prepared PS layers of 80%
porosity present a yellow-gold colour. After anodization,
the PS layers were rinsed with deionized water, dried
under nitrogen flux and stored in a dry, quite dark box,
in order to preserve their characteristics and to avoid PL
degradation [14]. Oxidized PS layers were obtained by
performing an experimental cycle consisting of exposing
PS to UV irradiation (light from a 30 W deuterium lamp
focused on 1 cm2) for 5 min a day and to normal aging in
free air and ambient light.
The PL spectra were monitored using a set-up
consisting of the 514.5 nm line of the Ar ion laser,a series of lenses, a triple-grating spectrometer and a
photomultiplier. As-prepared PS samples to be studied
must be stored in an inert ambient (such as N2) prior to
exposure to light, in order to avoid PL evolution in the
presence of O2 [15]. In order to study the evolution of the
terminal chemical bonds in the PS layer and their effects
on the PL, IRS measurements were performed on a Perkin-
Elmer spectrophotometer.
3. Theoretical approach
To calculate the PL lineshape, we assume that PS is formed
by Si crystallites in the form of quantum dots and wires.Also, we assume that both dots and wires have a Gaussian
distribution of diameter d centred around a mean d0. The
Gaussian distribution is given as
Gd =1
2exp
(d d0)
2
22
(1)
where is the root mean square value.
We use the same calculations and assumptions as those
made by John and Singh [16], but vary both dot and wire
diameter and take a dependence of d1.39 for the energygap versus the crystallite diameter d [17] (deduced from the
LCAO method) rather than a d2 dependence [16] (deduced
from effective mass theory). The total PL emitted fromxw wires and xd dots (xw and xd being the concentration
of wires and dots respectively in the PS layer) is It =Iw + Id, where Iw and Id represent the PL spectra ofwires and dots respectively. The PL energy is given by
h = Eg Eb + E, where Eg is the bulk silicon gap,Eb the exciton binding energy and E the confinement
energy of electrons in quantum dots or wires. Since Egranges from 1.14 to 1.17 eV, depending on the temperature
and the exciton binding energy Eb 0.15 eV [16], one maytake EgEb = 1 eV. Thus the PL energy is h = E+1.
By introducing a d1.39 dependence of the confinementenergy, E = cd/w/d1.39 where cw and cd are appropriatelydimensioned constants. The contributions of wires and dots
to the PL lineshape are
Iw = kwxwE3.16
exp1
2
d0w
w
2 c0.72w
d0wE0.72 1
2(2)
Id=
kdxdE3.88
exp1
2
d0d
d
2 c0.72dd0d
E0.72 12
(3)
kw and kd being suitable normalization constants.
4. Results and discussion
4.1. Effect of HF etching on the PL and structure of
as-prepared PS
Figure 1 shows experimental and calculated PL spectra
of unetched and HF-etched as-prepared PS at room
temperature. The effect of HF etching on as-prepared
PS is well illustrated: when an as-prepared PS layerundergoes etching in a 30% HF solution, for 60 min, its PL
peak increases in intensity and blueshifts from 1.78 eV to
1.94 eV. Calculated PL spectra were obtained by computing
equations (2) and (3) with the optimized parameters shown
in table 1. One can notice that there is a good agreement
between theoretical and experimental curves. It seems
that we have obtained better agreement than John and
Singh [16], who used a d2 dependence of the energygap versus the crystallite diameter. On the other hand,
for as-prepared PS, our calculation has given dot and wire
concentrations of 70% and 30% respectively and a dot mean
diameter slightly larger than that for wires (cf table 1).
For as-prepared PS made by Cullis and Canham [3] theconcentration of dots and wires (calculation made by John
and Singh [16]) is about 10% and 90% respectively. These
Figure 1. Room-temperature photoluminescence spectraof as-prepared PS of 80% porosity: (a) unetched PS,(b) etched in a 30% HF solution. Broken curves aretheoretically calculated PL spectra.
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Correlation of photoluminescence and structure of PS
Table 1. Optimized fitting parameters giving the theoreticalcurves shown in figure 1.
xd xw d0d d0w d w(%) (%) (nm) (nm) (nm) (nm)
As-prepared 70 30 3.3 2.83 0.35 0.3As-prepared 85 15 2.96 2.5 0.305 0.26
+60 min HF
contradictory results are probably due to the difference in
the substrate resistivity and the preparation conditions.
Transmission electron microscopy (TEM) analysis
[18, 19] shows that as-prepared PS of 80% porosity(obtained from p-type silicon) has a microporous structure
with a pore size almost identical to crystallite size; the latter
is about 3 nm and is in good agreement with our results(table 1). On the other hand, due to agressive anodization
(i.e. high porosity), TEM analysis [18, 19] revealed many
wire sections undulating in width [18] or detached [19],
leading to the formation of interconnected dots or free dots
respectively embedded in an amorphous phase. Thus, from
a simple undulating wire may originate many dots having aslightly larger mean diameter than that of the original wire.
Indeed, the dot mean diameter corresponds approximately
to the maximum diameter of the original undulating wire,
which is greater than the wire mean diameter. According
to root mean square values (table 1), it is evident that some
of the wires may have a larger diameter than some of the
dots. Therefore, according to TEM analysis [18,19], the
assumption that dots originate from many undulating wire
sections could explain the preponderance of quantum dots
in PS of 80% porosity (obtained from anodization of p-type
silicon of 11.5 cm resistivity).
HF etching has changed the concentration of dots and
wires from 70% to 85% and from 30% to 15% respectively
(cf table 1), probably by amplifying undulation in partiallyundulating wire sections. This may explain, in part, the
observed PL blueshift, but the size reduction in both dots
and wires may make a large contribution to this behaviour.
Hence, by taking just the PL calculation into account, the
PL blueshift depicted in figure 1 is due to an enlargement
of pores by chemical dissolution, hence to quantum sized
crystallites as described by Canham [1], and to a non-
negligible change in the population of crystallites that
luminesce (cf table 1). Although HF attacks bulk Si and
removes all amorphous phases, as previously described,
in PS it leaves a hydrogen-passivated Si skeleton. It is
therefore important to quantitatively evaluate the variation
of hydrogen content produced by HF etching in thePS layer, and to see whether it influences the emission
properties of PS. Figure 2, curves (2-a) and (2-b), shows
IR spectra of as-prepared and HF-etched PS, corresponding
to the PL spectra of figure 1. It was found that in both
cases the surface of the Si crystallites is surrounded by
SiHx bonds, exhibiting different vibrational modes [20].
It is important to note the existence of SiO bonds, even
after 60 min of HF etching, proof that PS instantaneously
becomes oxidized when it comes into contact with air. It
should be noted that all SiO bonds originate from the PS
structure, since IRS of the underlying Si substrate does not
exhibit any SiO peak (figure 2 curve (2-c)).
One can notice that SiHx bonds slightly decrease after
HF etching, except for SiH bonds corresponding to the
wagging mode at 661 cm1, and HF-etched PS has nogreater hydrogen content than as-prepared PS. This result
is contrary to what has been reported elsewhere [4, 21].
By correlating PL and IR spectra (figures 1 and 2), we
can deduce that the SiHx bonds and their content have
no influence on the observed PL blueshift. This is indisagreement with some authors [4, 21] who have argued
that SiHx bonds may play a more important role than
mere passivation. Just the variation in the intensity of
the wagging mode is not sufficient to explain such a PL
blueshift from 1.78 eV to 1.94 eV. The slight variation
of hydrogen content in HF-etched PS may be explained
by a new distribution of the SiHx bonds on smaller
crystallites. According to PL calculation, HF etching
has simply modified the size and the population of the
crystallites that luminesce, leading to a PL blueshift.
4.2. Effect of aging assisted by UV photoirradiation on
the PL and structure of PS
UV photoirradiation was performed to accelerate the
oxidation mechanism and to replace unstable SiHx bonds
by stable SiO bonds [22]. The UV photoirradiation
treatment begins 10 min after PS preparation, the IR
spectrum for which is shown in figure 2 curve (2-a).
From the first moments of UV irradiation, in ambient
air, we observe (qualitatively with the naked eye) a
relatively important reduction in the PL intensity. The
photodegradation can occur even on a time-scale of
milliseconds [23]. This could be related to photoinduced
structural changes such as hydrogen photodesorption from
the Si crystallites. However, after rapid photodegradation in
the initial stage of the photoirradiation, a photoenhancementeffect was observed. Thus, the photocreated Si dangling
bonds are being made passive by photo-oxidation [24].
Curve b in figure 3 shows that after 5 min of UV
photoirradiation, the PL peak of as-prepared PS has
blueshifted and increased in intensity. Curves c, d, e
in figure 3 depict the variation of the PL spectrum of
PS for different oxidation times. Under such oxidation
conditions, the PL peak blueshifts day after day (figure 3),
but its intensity seems to be dependent on the degree of
oxidation. Indeed, one can notice that the PL intensity
of PS oxidized over 15 days is lower than that oxidized
over 5 days. It should be noted that this result is not
specific to the oxidation conditions applied, since it hasbeen observed under other oxidation conditions [25]. In
fact, degradation appears when PS becomes oxidized (the
spectra are measured when the intensity stabilizes). The
origin of this degradation is detailed elsewhere [26].
Calculated PL spectra show that during oxidation the
concentration of dots increases and that of wires decreases
(cf table 2). This is accompanied by a reduction in the mean
diameter of both dot and wire crystallites. It is well known
that oxidation produces a thinning of the Si crystallites;
this thinning occurs day after day and should be the main
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B Bessas et al
Figure 2. Infrared absorbance spectra of: (2-a) freshly prepared PS layer of 80% porosity, (2-b) as-prepared PS of 80%porosity etched during 60 min in a 30% HF solution, (2-c) silicon substrate.
Figure 3. Evolution of room-temperaturephotoluminescence of PS versus post-anodizationtreatment: (a) as-prepared PS, (b) as-prepared + 5 min UV,(c) oxidized over 3 days at room temperature + 5 minUV/day, (d) oxidized over 5 days at roomtemperature + 5 min UV/day, (e) oxidized over 15 days atroom temperature + 5 min UV/day. Broken curves aretheoretically calculated PL spectra.
factor responsible for the PL blueshift. On the other hand,
apart from the fact that thinning affects both dot and wire
diameter, it would also transform, via oxide growth, manyundulating wire sections into oxide-covered interconnected
dots and/or free dots embedded in the oxide. In assuming
that the thinning rate, throughout oxide growth, is the same
for dots and wires, the dot mean diameter should remain
slightly greater than that of wire, in oxidized PS (cf table 2).
The PS samples oxidized for 5 and 15 days have been
submitted to 1 min of HF etching. A PL blueshift was
observed for the 5-day oxidized PS and a redshift for the
15-day oxidized PS (figure 4). The decrease of the PL
intensity in HF-etched oxidized PS (figure 5) is due to SiO2
Figure 4. Room-temperature photoluminescence spectraof oxidized PS, before (a and b) and after (c and d) 1 minetching in a 30% HF solution: (a) oxidized over 5 days atroom temperature + 5 min UV/day, (b) oxidized over 15days at room temperature + 5 min UV/day, (c) = (a) + 1 minof HF etching, (d) = (b) + 1 min of HF etching. Brokencurves are theoretically calculated PL spectra.
dissolution and consequently to the removal of many of the
Si crystallites embedded in the oxide. Also, an important
degradation phenomenon has been observed in oxidized
PS [26], before stabilization and measurement of the PLspectra. In both cases, the concentration of dots decreased
and that of wires increased (see table 2).
The decrease in the concentration of dots, obtained after
HF etching of 5-day oxidized PS, is probably due to the
fact that many dots have been trapped in the growing oxide
and then removed. This may also contribute to the large
downshift of the PL intensity (figure 4). Thus, the PL
blueshift produced in 5-day oxidized PS, after such HF
treatment, is due to the large reduction in diameter of both
dots and wires (see table 2).
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Correlation of photoluminescence and structure of PS
Table 2. Optimized fitting parameters giving the theoretical curves shown in figures 3, 4 and 6.
Oxidation time xd xw d0d d0w d wand treatment (%) (%) (nm) (nm) (nm) (nm)
3 days 76.5 23.5 3.15 2.7 0.36 0.285 days 83 17 3.10 2.62 0.35 0.3115 days 91 9 2.75 2.39 0.3 0.1565 days + 1 min HF 69 31 2.74 2.26 0.25 0.2715 days + 1 min HF 0 100 2.2 0.4
Figure 5. Infrared absorbance spectra of 15-day oxidized PS: (a) unetched, (b) etched for 1 min in a 30% HF solution.
PL calculation (see table 2) shows that for 15-day
oxidized PS, HF etching has removed all Si quantum
dots leaving only 100% wires, evidently linked to the
underlying Si substrate. At first sight this means that
at this oxidation stage all dots are trapped in the oxide.Indeed, IRS shows that in 15-day oxidized PS (figure 5,
curve (5-a)) all Si crystallites are surrounded by SiO
bonds. Nevertheless, SiH bonds in Si3SiH having a
bending mode at 624 cm1 [20] persist. The persistence ofthese bonds is not surprising, since it has been reported that
considerable numbers of H atoms still remain in oxidized
PS, even after thermal oxidation at high temperature [27].
Figure 5, curve (5-b), shows IRS of 15-day oxidized PS
after 1 min of HF etching. The presence of the bending
mode at 624 cm1, before and after HF treatment, suggeststhat the corresponding SiH bonds could be related to the
surface of the underlying Si substrate. The non-existence
of any SiO peak or SiHx peak proves that all dots areremoved and that the existing luminescing wires linked
to the underlying Si substrate are scarce. This confirms
our calculation result, where only 9% of wire crystallites
exist in 15-day oxidized PS (table 2). The number of wire
crystallites is best conserved after HF etching. Regarding
the PL behaviour of 15-day oxidized PS, after HF etching
(figure 4), we are in the presence of two competing
phenomena, a thinning effect (table 2) and a quasicomplete
presence of quantum wires which would induce a blueshift
and a redshift respectively. Indeed, the PL contributions of
Figure 6. Theoretically calculated PL contributions of dots(dotted curves) and wires (broken lines) to the total (fullcurves) in 5-day (a) and 15-day (b) oxidized PS.
dots and wires in the total PL spectrum, depicted in figure
6, show that the disappearance of quantum dots induces a
redshift, since the PL contribution of quantum dots is more
energetic than that of wires (figure 6).
The oxide dissolution mostly results in a large PL
redshift [11], suggesting that the observed PL blueshift
during oxidation does not result from a thinning effect of
the Si crystallites. In fact, the result of oxide dissolution
depends on the conditions of preparation of PS and on the
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oxidation methods. For oxidized PS, John and Singh [16]
have estimated the concentration of dots and wires to
be 15% and 85% respectively (experimental data taken
from Vial et al [28]); these values are reversed in our
5-day oxidized PS (table 2). When quantum wires are
preponderant, oxide dissolution may easily remove many
of the trapped minority dots, inducing a redshift; this is the
case in the experiments of Muller et al [11] and Vial et al
[28].
One may remark that 30% HF solution attacks oxidizedPS at a relatively high rate of about 3.5 A min1 (seetable 2). This rate is excessively high compared with that
reported for monocrystalline silicon [9]. In fact, when Si
quantum dots and wires are oxidized, an amorphous silicon
phase is found at the interface between the Si crystallite core
and the oxide [5, 29]. The dissolution rate of amorphous
silicon is rather high [10], so it should make a large
contribution to the rate of HF attack on oxidized PS, and
hence on the important reduction in the diameter of dots
and wires. As we have no data concerning the HF attack
rate in PS, it appears that the amorphous phase existing
at the SiO2/Si interface would be responsible for a such
reduction in the diameter of dots and wires.Since the SiO2 growing layer is accompanied by an
expansion of about 56% [30], and referring to table 2 and
figure 5, we can affirm that highly oxidized PS transforms
into an SiO2 matrix in which photoluminesent Si quantum
dots are embedded.
Techniques other than PS preparation [31] have been
used to obtain a luminescing SiO2 matrix in which Si
crystallites are implanted. A similarity in the emission
properties has been pointed out: it has been shown that
the PL energy depends on crystallite size, which in our
case depends on SiO2 growth.
Passivation and thinning of the Si crystallites are
the main responsibilities of SiO2
, although in other
works [28, 32] the existence of possible luminescing centres
at the SiO2/Si interface has been reported.
5. Conclusion
The effect of HF etching on the PL behaviour of as-
prepared and oxidized PS has been studied. The change
in the emission properties has been explained based on
confinement in Si quantum dots and wires and on infrared
spectroscopy. In as-prepared PS, HF etching produces a PL
blueshift, due to a change in concentration and reduction
in size of dot and wire Si crystallites. It was found
that in as-prepared PS, HF etching does not produce anyincrease in hydrogen content, as has always been reported,
but it simply modifies the size and the population of the
crystallites that luminesce. In oxidized PS, it has been
shown that oxidation induces a PL blueshift which becomes
all the more important as SiO2 grows; HF etching may
produce a PL blueshift or redshift depending on the degree
of oxidation and consequently on the evolution of dot and
wire concentration. Highly oxidized PS transforms into
an SiO2 matrix in which luminescing Si quantum dots of
reduced size are confined.
Acknowledgment
This work is supported by the Secretariat dEtat a la
Recherche Scientifique et a la Technologie (PNM 92).
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