ISSN 0306-8919, Volume 41, Number 3

This article was published in the above mentioned Springer issue. The material, including all portions thereof, is protected by copyright; all rights are held exclusively by Springer Science + Business Media. The material is for personal use only; commercial use is not permitted. Unauthorized reproduction, transfer and/or use may be a violation of criminal as well as civil law.

Opt Quant Electron (2009) 41:189201 DOI 10.1007/s11082-009-9341-y

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Fabrication and characterization of porous silicon layers for applications in optoelectronics

R. S. Dubey D. K. Gautam

Received: 2 June 2009 / Accepted: 14 October 2009 / Published online: 6 November 2009 Springer Science+Business Media, LLC. 2009

Abstract In the present paper, several samples of porous silicon monolayers and multilayers were prepared at different anodization conditions with xed HF concentration. The room temperature photoluminescence wavelength observed to be increased with increased etching time and current density respectively. By Raman measurement it has been observed that as the size of silicon crystallites decreased with increased etching time, the silicon optical phonon line shifted somewhat to lower frequency from 520.5 cm1 and became broader asymmetrically. The surface roughness and pyramid like hillocks surface was conrmed by AFM measurement. In SEM images, the porous silicon layers were clearly observed by white and black strips. It was also observed that the reectivity increased as the number of porous silicon layers was increased. Keywords crystals Porous silicon Photoluminescence Raman peak Reectivity Photonic

1 Introduction Porous silicon (PS) offers major potential for integrated optoelectronics technology and has accepted the new challenges to fabricate silicon based photonic devices using existing established silicon technology. Due to shifting of fundamental absorption edge into the short wavelength and observed photoluminescence in the visible region of the spectrum, porous silicon has opened the door to a multitude of applications in advanced optoelectronics technology (Canham 1990; Lang et al. 1993; Hou et al. 1996; Kalem and Yavuzcein 1999; Barillaro

R. S. Dubey (B ) IACQER, Advanced Research Laboratory for Nanomaterials and Devices, Swarnandhra College of Engineering and Technology, Seetharampuram, Narsapur, Andhra Pradesh, India e-mail: rag_pcw@yahoo.co.in D. K. Gautam Department of Electronics, North Maharashtra University, Post Box 80, Umavinagar, Jalgaon, Maharashtra, India

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et al. 2001). Porous silicon is dened as a matrix or a network of nanoscale sized silicon wires and voids which are formed when crystalline silicon wafers are etched electrochemically in hydrouoric acid based electrolyte solution under constant anodization conditions. Several models have been proposed to explain the observed photoluminescence from porous silicon, these are hydrogenated amorphous silicon model, surface hydrides model, defect model, siloxene model, surface states model and quantum connement model (Pavesi and Guardini 1996; Vasquez-A et al. 2007; Voos et al. 1992; Weng et al. 1993; Bisi et al. 2000). A multilayer structure of porous silicon exhibits a strong modulation of light hence, can be replaced other dielectric layers in interference lters or mirrors. Such periodic dielectric media is known as one-dimensional (1D) photonic crystals (PCs) and have attracted intense research after the pioneer works of Yablonovitch (1987) and John (1987). The forbidden frequencies or wavelengths form a band gap for light waves, which is the core of photonic crystal operation (Dubey and Gautam 2008). Using porous silicon layers 1D photonic crystal can be easily prepared by the periodic variation of the electrochemical formation parameters which leads to periodic variations of the refractive index of each layers (Agrawal and del Rio 2003; Lugo et al. 2002; Setzu et al. 2000). Due to wide use of solar energy, there is need of creation of new technologies and materials which can be reduced the cost of solar cells therefore, porous silicon is expected to be promising one (Boeringer and Tsu 1994; Lipiski et al. 2003; Dobrza nski et al. 2006; Smestad et al. 1992; Lin et al. 2008). For solar cells, porous silicon layer acts as an ultra efcient anti-reection coating, while a graded layer with varying expanded band gap offers increased absorption in visible spectrum regions. Porous silicon is also used as smart transducer material for sensing applications for the detection of vapors, liquids and biochemical molecules (Singh et al. 2008; Moretti et al. 2007; Descrovi et al. 2007; Ouyang et al. 2006). In this paper, the synthesis and characterization of monolayers and multilayers of porous silicon is presented. In Sect. 2, the experimental details for the preparation of porous silicon layers have been presented. The optical and structural properties of porous silicon monolayers and multilayers are discussed in Sect. 3. Finally, Sect. 4 concludes the paper.

2 Experimental details Various samples of porous silicon monolayers and multilayers were prepared by using <100> oriented boron-doped p-type substrates of 10 ohm. cm as starting material. The electrochemical cell used has two electrode congurations with a platinum electrode and a silicon wafer as anode. Before synthesis, the silicon wafer was rinsed in de-ionized water after heating separately in trichloroethylene, methanol and acetone for 5 min. Then the cleaned silicon wafers were dried in presence of nitrogen. The electrolyte used was HF (48%): H2 O:C2 H5 OH in a volume ratio of 1:1:2. The mixing of ethanol in electrolyte solution is helpful to improve the lateral homogeneity and the uniformity of the porous silicon layer by promoting the hydrogen bubble removal. For the formation of monolayer of porous silicon, a xed current density J was applied for a xed etching time t. In order to prepare a multilayer structure of porous silicon, we have rst prepared a stack of two layers of different refractive index by applying current density J1 & J2 for the etching time t1 & t2 respectively. Further, this process is repeated for desired stacks. The prepared samples were characterized for reectance by UVvisible spectrophotometer (Shimadzu UV-1601). The photoluminescence was measured by using a monochromator (Jobin Yvon) with an attached charge coupled device. A beam of 488 nm line from argon laser at 10 mW output power was used for excitation. To link crystallographic perfection of

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Fabrication and characterization of porous silicon layers Table 1 Photoluminescence peaks at various etching time J = 50 mA/cm2 Etching time ( min) 2 3 4

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J = 30 mA/cm2 PL peak (eV) 1.93 1.85 1.79 Etching PL peak time ( min) (nm) 2 3 4 629 630 650 PL peak (nm) 640 670 690

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PL peak (eV) 1.97 1.96 1.90

the starting material with resulting porous morphology the Raman measurements using Lympus EX41 Raman Division (HR800) were done. The surface morphology and roughness of prepared samples were obtained by atomic force microscopy Nanoscope E (NSE) in contact mode. The scanning electron microscopy using Leica Cambridge 440 Microscope (UK) was done to see the porous zone clearly distinguished from the substrate.

3 Results and discussion Several samples of porous silicon monolayers and multilayers were prepared at different anodization conditions with xed HF concentration. The prepared samples show distinct color distribution over the entire surface of porous silicon. The prepared porous structure in bulk silicon is strongly responsible for the photoluminescence on its surface which can be conrmed by shifting in the band gap energy of bulk silicon. The room temperature photoluminescence measurements of various samples prepared at different anodization conditions are depicted in Figs. 1, 2, 3. The photoluminescence peak corresponding to the red band emission at wavelength 640, 670 and 690 nm can be observed in Fig. 1ac respectively. It is obvious that as the current density increases the silicon crystallite size will decrease which causes the variation in the PL intensity. In fact, the porosity of porous silicon layer is a direct function of applied current density and as the pore size varies accordingly the size of silicon crystallites will change. Therefore, the PL wavelength shifts to higher wavelength or lower energy as the etching time is increased. In case of Fig. 1b, a broad range of PL at wavelength 670 nm is observed which is probably due to a wide distribution of the energy band gap caused by different pore sizes. It is noted that the wavelength of red emission peak varies between a minimum of 640 nm and maximum of 690 nm. This shows that the band gap can be tuned from 1.931.79 eV by adjusting the anodization time from 25 min at applied 50 mA/cm2 current density. Similarly, Fig. 2ac shows the red emission PL of porous silicon prepared at 30 mA/cm2 under 2, 3 and 4 min anodization time, respectively. In this case, if the current density is kept lower (30 mA/cm2 ) than previous one, so pores of reduced size is expected. On the basis of this, if we compare the Figs. 1 and 2 we will nd that the PL wavelength is decreased. However, in Fig. 2b a broad peak of red emission is observable at 650 nm. In this case, the wavelength of red emission peak varies between a minimum of 629 nm and maximum of 650 nm. It indicates that the band gap can be tuned from 1.971.90 eV by adjusting the anodization time 24 min at applied 30 mA/cm2 current density. Red emission band has attracted the most attention because it is the only band to be efciently electrically excited (Bisi et al. 2000). Table 1 shows the PL peak and band gap energy observed at various anodization time and current densities. We have also prepared multilayers of porous silicon to observe the variation in the PL wavelength. Figure 3 shows the PL samples prepared by the tuning of 50 and 30 mA/cm2 current density under 2 min etching time. Figure 3a, b are corresponding to the two and three

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192 Fig. 1 Photoluminescence of porous silicon monolayer prepared at J = 50 mA/cm2 under etching time a 2 min, b 3 min, c 5 min

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Fabrication and characterization of porous silicon layers Fig. 2 Photoluminescence of porous silicon monolayer prepared at J = 30 mA/cm2 under etching time a 2 min, b 3 min, c 4 min

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Fig. 3 Photoluminescence a two, b three bilayers of porous silicon anodized at J1 = 50 & J2 = 30 mA/cm2 under 2 min etching time Fig. 4 Raman spectra of porous silicon monolayers formed under various etching time at J = 30 mA/cm2

Intensity (a.u.)

t=4min. t=3min. t=2min. C-Silicon

500

520

540

Raman Shift (cm-1)

bilayers (stacks) of high and low refractive index layer of porous silicon. By comparing these gures, we have concluded that as the number of bilayers increases the PL peak shifts to the lower wavelength while remaining in the red band. It is actually expected phenomena since, as the number of pores is increased in silicon wafer it ultimately reduces the size of silicon crystallite as a consequence there will be a shift in Raman as well as PL peak. Figures 4 and 5 shows the Raman shift of porous silicon monolayers formed at various etching time for J = 30 and 50 mA/cm2 , respectively. The solid curves in Figs. 4 and 5 shows the Raman peak from pure single crystalline silicon observed at 520.5 cm1 with its shape is nearly Lorentzian. In crystalline silicon, the optical phonon is observed in the center of the Brillouin zone with its energy of 520.5 cm1 and this is due to the conservation of quasimomentum in crystals. It is known that phonons in small crystallites are localized hence; their quasimomentum is no longer well dened according to the uncertainty principle. Thus, the conservation law of the quasimomenturn is no longer valid. As a result, all the phonons of dispersion relation estimated with a weight function which contributes to the measured Raman signal. As the size of nanocrystal decreases, the silicon optical phonon line shifts to lower frequency and becomes broader asymmetrically (Yeo et al. 2005; Sui et al. 1992; Cho et al. 1998; Kozlowski and Lang 1992). This shifting of peak attributes the reduction in the phonon energy as a result of disturbances in the silicon lattice due to porous structure. This attributes the theory of the light emission in porous silicon as due to transition of the carriers

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Fabrication and characterization of porous silicon layers Fig. 5 Raman spectra of porous silicon monolayers formed under various etching time at J = 50 mA/cm2

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Intensity (a.u.)

t=5min. t=4min. t=3min. C-Silicon

500

520

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Raman Shift (cm-1)

for L 1 and L 2 valleys of band structure as reported by Gautam et al. (1988) and Khokle (1987). In fact, the band structure of silicon gets modied by making the silicon porous and the valleys shift towards K = 0. In simple words, the maximum part of applied energy is converted into emission therefore the band structure of silicon is modied. This suggests that the Raman contribution is exclusively from the porous silicon layer not from bulk silicon. As depicted in Figs. 4 and 5, as the etching time increases the Raman peaks gradually shifts from 520.5 cm1 with the increment in full width at half maximum. According to the variation in the anodization parameters, the shifting of red emission can be observed. Photoluminescence of red band originates from centers located at the surface of the silicon branches is logical when one consider that the large surface area of porous silicon would provide numerous recombination centers. The recombination centres are formed by silicon atoms at the surface of the crystallite adjusting their bond lengths and angles to accommodate changes in local conditions. Among different hypothesis presented so far on the photoluminescence from porous silicon surface, quantum connement effect is popular one which is due to the charge carriers in narrow crystalline silicon wall separating the pore walls. As we have shown in Figs. 4 and 5 the shifting of Raman peak is minor (in the range of 0.8) at various anodization conditions. Usually, as the size of nanocrystals decreases, the silicon optical phonon line shifts to lower frequency and becomes broader asymmetrically (Yeo et al. 2005; Sui et al. 1992; Cho et al. 1998; Kozlowski and Lang 1992). However, our results are consistent with another hypothesis according to which the porous silicon luminescence is due to the presence of surface conned molecular emitters i.e., siloxene (Pavesi and Guardini 1996; Vasquez-A et al. 2007; Voos et al. 1992; Weng et al. 1993; Bisi et al. 2000). The same conclusion is also reported by Zhao et al. (2006), Yeo et al. (2005). Hence, the Raman peak observed in Figs. 4 and 5 indicates the less possibility of quantum connement effect. Figures 6 and 7 shows the AFM images of monolayers of porous silicon anodized at distinct anodization parameters. Figure 6a shows the AFM image of porous silicon monolayer prepared at J = 50 A/cm2 under 2 min anodization time. The prepared porous silicon layer shows the surface roughness and pyramid like hillocks surface. The observed average diameter of pores and its roughness are 39.06 and 6.83 nm respectively. The surface morphology conrms the pore formation with its depth is about 8.926 nm. Figure 6b shows the AFM images of sample prepared at same current density but increased etching time i.e., 3 min. This image also conrms the formation of pores. It is observed that as the anodization time increases the column length also increases. The average diameter and depth of the pores is 42.05 and 13 nm respectively. In this case, the pore depth is increased due to change of anodization time 23 min, however, the average roughness of porous silicon is 6.33 nm.

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Fig. 6 3D AFM image of porous silicon monolayers prepared at J = 50 mA/cm2 under a t = 2 min, b t = 3 min, c t = 5 min

Fig. 7 3D AFM image of porous silicon monolayers prepared at J = 30 mA/cm2 under a t = 2 min, b t = 3 min, c t = 5 min

In photoluminescence study, we have found the enhanced PL intensity which is due to the increased size and height of the pitches which is observable in the AFM images of porous silicon prepared at increased anodization time. Figure 6c shows the surface morphology of the sample prepared at increased anodization time of 5 min. At this etching time, the average diameter and depth of the pore are 54.69 and 14.4 nm, respectively. However, the surface roughness is 7.918 nm. From Fig. 6ac, we have found that as the anodization time increases the depth of the pores are increased in the manner of 8.926, 13 and 14.4 nm anodized at 2, 3 and 5 min etching time, respectively. Similarly, Fig. 7ac shows the AFM images of porous silicon surfaces anodized at 30 mA/cm2 constant current density with varying etching time 2, 3 and 4 min respectively. Figure 7a shows the AFM image of the prepared sample at J = 30 mA/cm2 under 2 min etching time. The average diameter, depth and roughness of the pores are 26.43, 8.2 and 3.6 nm, respectively. Figure 7b shows the surface morphology of the porous silicon sample anodized under 3 min at 30 mA/cm2 current density. The average diameter, depth and roughness of the pores are 35.1, 11 and 4.7 nm, respectively. The surface morphology of the porous silicon sample shown in Fig. 7c is anodized under 4 min at 30 mA/cm2 current density. The diameter, depth of pores and the surface roughness are 42.07, 12 and 5.133 nm, respectively. AFM images in Figs. 6 and 7 shows different size of pores formed at different anodization parameters during synthesis. The formation of these pores is responsible for the shift of Raman peak due to change in crystallite size of silicon. Accordingly, these changes are highly responsible for its photoluminescence in the visible wavelength range.

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Fig. 8 Plane view SEM image of sample S1 gure (a) and S2 gure (b) anodized under J = 30 and 50 mA/cm2 , respectively

Fig. 9 Plane view SEM image sample S3 gure (a) and S4 gure (b) anodized by tuning of current J1 & J2 for three periods

Figures 810 shows the surface morphology of as-grown porous silicon monolayers and multilayers. Figure 8a,b shows the scanning electron microscopy (SEM) plane view images of porous silicon monolayer (sample S1 and S2) etched under current density J = 30 and 50 mA/cm2 . The etching time of sample S1 and S2 are 2 min respectively. The morphology of the porous silicon layer shows that the electrochemical etching of silicon occurred uniformly and made the granular structure in a columnar shape which can be observed in the image of sample S1 and S2. It is also observable that as the current density increases from J = 3050 mA/cm2 , the etching depth is also increased. The array of void spaces (dark) in silicon matrix (bright) can be seen clearly in another top view SEM of porous silicon multilayer (sample S3 and S4) which is shown in Fig. 9a,b. These samples composed of three periods of high and low refractive index layers prepared by tuning of current density J1 = 50 & J2 = 30 mA/cm2 for 2 and 3 min etching time, respectively. A large number of small pores that are aligned in random direction are observable in SEM images. The average pore diameter obtained from sample S3 and S4 are to be 4.5 and 12 m, respectively. Figure 10a,b shows the SEM images of multilayered structure of porous silicon (sample S5 and S6) in which different formed layers can be seen clearly. For S5, we have found the rst and second layer thicknesses are 1.36 and 0.56 m for current density of 50 and 30 mA/cm2

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Fig. 10 Cross-sectional SEM image of sample S5 (a) and S6 (b)

under 1 min etching time. However, for S6 we have found that for current density of 50 and 30 mA/cm2 the obtained thicknesses are 1.84 and 0.72 m corresponding to the rst and second layer etched under 2 min etching time. By changing the ratio of silicon and air, a wide range of refractive indices can be obtained. The sample S5 and S6 are composed of six periods of high and low refractive index layers respectively. Figure 10a,b, shows the layered structures of porous silicon by white and black strips of refractive index n 1 = 2.14 and n 2 = 1.88 of sample S5 and n 1 = 1.42 and n 2 = 2.65 of sample S6. The SEM micrograph of S5 show the non-uniform layers under 2 min. etching time but, as the etching time reduces to the 1 min the structure of S6 becomes more uniform with good homogeneity as depicted in SEM micrograph. The refractive index contrast of S6 is large as compared to the S5 hence; a large photonic band gap can be obtained by tuning the etching time. The reectivity of porous silicon layer varies with respect to the anodization parameters hence, so it is essential to check the reectivity of prepared porous silicon layers. Figure 11, shows the reection spectra of porous silicon monolayers (sample S1 and S2) prepared at current density J = 30 & 50 mA/cm2 respectively. The prepared porous silicon layers are very thin which can be regarded as thin lms. Hence, the bumps shown in the reection spectra are obviously caused by constructive and destructive interference of the beams reected from upper and lower interfaces of porous silicon layer. The number of bumps increases as the anodization time is increased. It is observed that the reection varies sinusoidally on wavelength scale. The doted and solid curves are corresponding to the porous silicon samples S1 and S2 prepared at 2 min anodization time. It is remarkable that the increase in current density from 30 to 50 mA/cm2 causes to increase the reection through the surface of porous silicon layer. Figure 12 shows the typical reection spectra of the samples S3 and S4 which are composed of three periods of low and high refractive index layers. The dotted and solid curves are corresponding to the sample S3 and S4 prepared by optimizing the current density J1 = 50 & J2 = 30 mA/cm2 for 2 and 3 min etching time, respectively. In this gure, the spectral bandwidth of maximum reectivity is observed as the number of bilayers is increased. The progressive decrease of the fringes maxima at lower wavelength is due to the increasing absorption of the porous silicon layers. As the current density is changed the refractive index is also changed which change the porosity of the layer as a result of it, the reectance is varied. Similarly, Fig. 13 shows the reectivity of multilayered structure of porous silicon (i.e., sample S5 and S6) which are composed of six periods of low and high refractive index layers. The structure is anodized by the tuning of 30 and 50 mA/cm2 current

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Fabrication and characterization of porous silicon layers Fig. 11 Reection spectra of sample S1 and S2 at current densities J = 30 & 50 mA/cm2 for 2 min etching time

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Fig. 12 Reection spectra of sample S3 and S4 prepared by tuning of current density J1 = 50 & J2 = 30 mA/cm2 for 2 and 3 min etching time, respectively

Fig. 13 Reection spectra of sample S5 and S6 prepared by the tuning of current densities J1 = 30 & J2 = 50 mA/cm2 for 1 & 2 min etching time, respectively

density for 1 and 2 min etching time. The progressive decrease of the fringes maxima outside the stop band indicates the absorption of incidence light on the surface of the porous silicon layers.

4 Conclusions Various samples of porous silicon prepared under different anodization conditions were characterized and studied. It was observed that as the current density increases, the porosity of the porous silicon layer is increased and consequently refractive index is reduced. As the anodization time increases, the size of silicon crystallites reduced which causes the corresponding shifting in the Raman peak as well as band gap of porous silicon. From Raman study it was revealed that as the size of silicon crystallites decreased with increased current

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density and etching time the silicon optical phonon line shifted somewhat to lower frequency from 520.5 cm1 and became broader asymmetrically. This shifting of peak attributed the reduction in the phonon energy as a result of disturbances in the silicon lattice due to porous structure. As the maximum part of applied energy is converted into emission hence, the band structure of silicon is modied. This suggests that the Raman contribution is exclusively from the porous silicon layer not from bulk silicon. AFM characterization shows the rough silicon surface which can be regarded as a condensation point for small skeleton clusters to form. In SEM analysis, the structures of porous silicon layers are clearly observed by white and black strips. It is also observed that the reectivity increases as the number of porous silicon layers is increased which is useful in order to tune the maximum reection band for 1D photonic crystals. It is important to note that the small shifting of Raman peaks at different etching and current density attributes the less possibility of quantum connement in prepared samples. Hence, the red band emission observed in visible spectrum attributed to the hydrides presence on the surface of porous silicon. This study explores the applicability of electrochemically prepared porous silicon layer for its various applications in advanced optoelectronics eld.
Acknowledgments The authors wish to express their gratitude to Dr. V. Ganesan, and Dr. V. Sathe for characterizing the porous silicon samples at UCG-DAE Consortium for Scientic Research Laboratory, Indore (MP), INDIA.

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