Abstract

We report results from our extensive studies on the fabrication of ultra-thin, flexible, and cost-effective Ag nanoparticle (NP) coated free-standing porous silicon (FS-pSi) for superior molecular sensing. The FS-pSi has been prepared by adopting a simple wet-etching method. The deposition time of AgNO3 has been increased to improve the number of hot-spot regions, thereby the sensing abilities are improved efficiently. FESEM images illustrated the morphology of uniformly distributed AgNPs on the pSi surface. Initially, a dye molecule [methylene blue (MB)] was used as a probe to evaluate the sensing capabilities of the substrate using the surface-enhanced Raman scattering (SERS) technique. The detection was later extended towards the sensing of two important explosive molecules [ammonium nitrate (AN), picric acid (PA)], and a pesticide molecule (thiram) clearly demonstrating the versatility of the investigated substrates. The sensitivity was confirmed by estimating the analytical enhancement factor (AEF), which was ∼107 for MB and ∼104 for explosives and pesticides. We have also evaluated the limit of detection (LOD) values in each case, which were found to be 50 nM, 1 µM, 2 µM, and 1 µM, respectively, for MB, PA, AN, and thiram. Undeniably, our detailed SERS results established excellent reproducibility with a low RSD (relative standard deviation). Furthermore, we also demonstrate the reasonable stability of AgNPs decorated pSi by inspecting and studying their SERS performance over a period of 90 days. The overall cost of these substrates is attractive for practical applications on account of the above-mentioned superior qualities.

© 2021 Optical Society of America under the terms of the OSA Open Access Publishing Agreement

1. Introduction

An ultra-thin material with free-standing capability and flexibility would offer extensive opportunities in the fabrication of optoelectronics and, specifically, in the field of sensing devices for real-world and on-site applications [16]. The cornerstone of conventional rigid surface-enhanced Raman scattering (SERS) substrates faces major complications in (a) sample collection (b) inefficient hot spot detection, and (c) is relatively expensive, which could not fulfil the device miniaturization and emerging scientific demands. Likewise, an ideal SERS substrate should be versatile in flexibility, efficient on-site detection, and possess mass production scalability in addition to proficient hot-spot centers, sensitivity, selectivity, and reproducibility. Therefore, the development of ultra-thin, porous, and flexible substrates is one of the challenging tasks in SERS-based sensing [711]. Among the other semiconductor materials, Si nanostructures (NSs) are anticipated to be one of the effective materials in the SERS community due to their tunable morphology, bio-compatibility, nature of the effective molecular binding, and compatibility with conventional silicon processing technology [1216]. In this strategical approach, there is an increasing demand for the fabrication of free-standing single-crystal porous silicon (pSi) for building an opportunity to integrate SERS-active substrates with other functional devices on a single silicon wafer.

Porous silicon (pSi) is one of the diverse porous nanostructures and was accidentally observed by Uhlir et al. at Bell labs while performing the electro-polishing of Si and Ge [17]. Typically, the nanocrystalline pSi is prepared by an easy and convenient electrochemical or anodic etching of crystalline Si using an aqueous HF-based electrolyte [18]. This process produces homogenous pSi with significant control over the pore size and porosity. In the process of pSi formation, the complete dissolution mechanism of Si in electrolytes, composed of HF and alcohol, and their properties were demonstrated in our earlier reports [1922]. Interestingly, pSi comprises micro, meso, and macro meter pores with cylindrical columns with large surface area, unique optical properties, the ability of metal ion reduction, and chemical stability, which are adequate for effective incorporation of analyte molecules to make it perform robust SERS-activity [19,2327]. Essentially, the proposal for utilization of pSi in the area of the SERS community has been initiated in the early years of the 2000s, and ever since it has attracted a reasonable majority of active participation in the fabrication of SERS-based substrates [28,29]. As a consequence, we have made an attempt to develop a free-standing single-crystal porous silicon (FS-pSi) as a flexible substrate for molecular sensing, because of its flexibility, porous structure, ease in handling capability, large surface to volume ratio, and high integrity on metal NSs formation. The promising free-standing pSi can be achieved by detaching the pSi layer from the parent Si substrate [30,31]. The detachment process involved the dissolution of Si in alkaline solutions. The dissolution approach depends on the transport properties at the interface of silicon–electrolyte in anodic etching or polishing based on Fick’s law [17,32,33]. Indeed, to the best of our knowledge, there are no reports on the pSi as a flexible substrate in the application of SERS sensing. SERS is one of the most promising analytical techniques among the different methodologies investigated recently that relies on optical, electrical, and/or magnetic properties with a single molecular detection capability [34]. The SERS technique recently opened various application avenues for its efficacy in medicine, detection of environmental pollutants, food safety, and military applications due to its high precision, sensitivity, and selectivity [35,36]. The mechanism of plasmonic SERS has been explained broadly based on two mechanisms, i.e., an electromagnetic mechanism (EM) and a chemical mechanism (CM) [3739]. The charge transfer (CT) effect is predominant in the chemical enhancement mechanism. The CT is closely related to the coupling between composite surface and the bridging analyte molecules. CT is induced when the incident light matches the potential barrier between the energy of metal Fermi level and electron affinity of the probe molecule [40,41]. The contribution of enhancement in the Raman signal is a synergetic effect of EM and CM and it is very difficult to extract the exact contributions of each of them. However, it is well known that the electromagnetic contribution shows a higher degree of spectral enhancement in the SERS phenomenon. The electromagnetic field enhancement strongly depends on the plasmonic nanostructures for effective molecular detection generally by inducing localized surface plasmon resonance [42]. By considering the highlights of plasmonic nanostructures in SERS phenomena, much attention was paid to the preparation of plasmonic SERS-active substrates with high sensitivity, reliable reproducibility, and distinct selectivity, etc. [13,43,44]. Therefore, our objective was the synthesis of flexible SERS substrates comprising silver nanoparticles (NPs) decorated FS-pSi layer for trace-level molecular detection with a high degree of stability and reproducibility for on-site applications.

2. Experimental procedures

Materials and chemicals. Single crystalline p-type, boron-doped Si wafers with a resistivity of 1-10 Ω-cm were purchased from commercial vendors and cleaned thoroughly before first use. The silver salt (AgNO3), ethanol (reagent grade), and highly concentrated Hydrofluoric acid (48%HF) were purchased from standard chemical suppliers. The dye molecule MB (C16H18CIN3S·H2O) and Thiram (C6H12N2S4) were obtained from Sigma-Aldrich. The explosives used for SERS detection, AN (NH4NO3), and PA (C6H3N3O7) were procured from High Energy Materials Research Laboratory (HEMRL), Pune, India.

Synthesis of FS-pSi layer. Low dimensional, nanocrystalline pSi has been prepared by opting for a convenient solution-based anodic etching process. Boron-doped commercially available Si wafers (typically 1×1 cm2) were cleaned with acetone and ethanol to remove any surface contaminations. This procedure was followed by dipping them in diluted HF for native oxide etching. The detailed necessary procedures were reported in our earlier works [19,45]. The pre-cleaned Si wafer was directly mounted into an in-house etch-cell setup for anodic etching, which acts as an anode and a platinum coil served as a cathode. An etch-cell filled with an electrolyte of composition 1:1:2::H2O:HF: ethanol was used to initiate the etching process. The FS-pSi layer was prepared by applying pulsed current densities of J=30 mA/cm2 for 60 minutes and Jc=170 mA/cm2 for 1 minute by a Keithley-2400 DC current source (voltage: 5 V to 200 V; DC current: 10 pA to 1 A) for anodization and electro-polishing, respectively, despite resistivity discrepancies. Figure 1 shows the successive synthesis steps of FS-pSi layers. The detached pSi layer was retained on the scotch tape for better flexibility. Figure 2 shows the photographic representations of the free-standing pSi layer after its detachment from the etched silicon substrate. The FS-pSi layers were quite stable even after folding the substrate for several attempts.

 figure: Fig. 1.

Fig. 1. Processing steps for the fabrication of AgNPs@FS-pSi layer by anodic-etching followed by electro-polishing.

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 figure: Fig. 2.

Fig. 2. Photographs of FS-pSi (a) floating on water (b) freely held by a tweezer, and (c) mounted on a flexible scotch tape.

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Decoration of AgNPs. FS-pSi layers were subsequently decorated with Ag nanoparticles (NPs) through a two-step electroless deposition process (i.e., galvanic immersion process). In the first step, 0.002 M AgNO3 was deposited on the FS-pSi layer, and in the second step, the deposited samples were immersed in a 5 M HF solution for 15 s. The density of AgNPs was modulated by varying the deposition time, i.e., 30 min, 60 min, and 4 hours. These samples are labeled as AgNPs@FSpSi-30min, AgNPs@FSpSi-60min, and AgNPs@FSpSi-4h, respectively. Ultimately, the optimized AgNPs@FSpSi-60 min sample has been used for further investigations. In the present study, a 3” Si wafer (with a cost of ∼25 US ${\$}$) was sliced into pieces of 1.5×1.5 cm2 for subsequent sample processing. The sliced piece (2.25 cm2) of Si, costing typically <5 US ${\$}$, has been used for the fabrication of free-standing porous Si. It is pertinent to note here that the parental Si used for etching can further be recycled (and used for the fabrication of FS-pSi) after subsequent sample cleaning/dusting. According to the measurement demand, the resulting AgNPs decorated FS-pSi with ∼10 mm diameter was further diced into 2 pieces and utilized for characterization studies. Through several measurements and analyses, we demonstrate here that the single piece of SERS-active substrate is quite economical (costing typically <1 US ${\$}$) with an effective capability of rapid detection of hazardous materials.

Measurements. The morphological changes and evolutions of AgNPs decorated FS-pSi layers were investigated by Field Emission Scanning Electron Microscopy (FESEM- Carl ZEISS, FEG, Ultra 55–5 eV energy for imaging and 20 eV for Energy-dispersive X-ray spectroscopy (EDS) measurement). Furthermore, these samples were utilized as SERS substrates for molecular detection using a Raman spectrometer (Horiba-Scientific) and 532 nm laser excitation with an input laser power of ∼25 mW. The measurement parameters such as spot size was ∼800 nm while 10 s acquisition time has been maintained through the measurements. The considered probe molecules [methylene blue (MB) and explosive molecules such as picric acid (PA), ammonium nitrate (AN), and pesticide such as Thiram] are dispersed in ethanol, which were drop-casted on SERS-active substrates for further Raman investigations. The Raman spectra presented in the manuscript were as measured with a simple baseline correction only. The comprehensive data analysis and discussions are presented in the subsequent sections.

3. Results and discussion

The FESEM image shown in Fig. 3(a) illustrates the morphology of the anodized FS-pSi layer confirming its porous nature. We propose and demonstrate that when this surface is functionalized with plasmonic nanoparticles it will act as an efficient, flexible substrate for sensing a wide range of analyte molecules. The surface roughness of as prepared FS-pSi layer was estimated using optical ellipsometry and was found to be 550 ± 25 nm. As a result of etching, we attained mesoporous Si with a pore size of about 52 ± 0.9 nm by evaluating the sample surface, data of which is depicted in Fig. 3(b).

 figure: Fig. 3.

Fig. 3. (a) The morphology of as-anodized FS-pSi layer and (b) the histogram of the pore size distribution (solid line indicates the Gaussian fit).

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The pSi with mesoporous nature opens great opportunities for the fabrication of SERS-active substrate because of its high mechanical strength, tunable nanoscale pores, and surface reproducibility. The other physical properties such as porosity and the thickness of pSi layers have been extracted by dissolution mechanism followed by weight measurements. The weight measurements were performed on pre-anodized Si [referred to as m1], immediately after anodization [referred to as m2], and finally after rapid stripping of pSi in KOH solution [marked as m3]. The porosity of pSi was estimated using Eq. (1) [46].

$$P = \frac{{({{m_1} - {m_2}} )}}{{({{m_1} - {m_3}} )}}$$

The thickness of the pSi layer was estimated using Eq. (2)

$$W = \frac{{({{m_1} - {m_3}} )}}{{S \times d}}$$
where d and S are the density of Si and area of the Si exposed to electrolyte during anodization respectively. The estimated values are summarized in Table 1.

Tables Icon

Table 1. The estimated physical parameters of FS-pSi fabricated by anodic etching.

The FS-pSi layer comprised a high density of open bonds due to its large surface area and dense surface states, which are favorable for metal atom reduction through a solution-based metal deposition [44]. Therefore, a simple and inexpensive galvanic immersion process [47] has been implemented for the fabrication of a cost-effective, robust plasmonic SERS substrate.

Figures 4(a)-(c) illustrate the FS-pSi layer decorated at various densities of the AgNPs and the corresponding EDS data, shown in Fig. 4(d), represents the elements present in the sample. It is evident from Fig. 4 that with an increase in the density of AgNPs on FS-pSi, a higher density of hotspots was attained, which certainly helps in obtaining superior SERS signals. It is a noteworthy observation that the distribution of NPs [see an image in Fig. 4(a)] was dispersed well but with a lower density due to the minimal 30 min deposition. Next, 60 min deposition time led to an evenly distributed AgNPs on the sample surface, and the data is shown in Fig. 4(b). With an increase in the deposition time to about 4 hours [Fig. 4(c)], the density of NPs was much higher with an inhomogeneous aggregation. The aggregation of AgNPs at a longer deposition time might be due to the coalescence of NPs with the formed initial NPs according to the Volmer-Weber mechanism [48]. The size of AgNPs was estimated to be 30 ± 0.4 nm in the case of 60 min. deposition time by adopting an analysis using the ImageJ software. Furthermore, to accomplish our prospective objectives, the AgNPs decorated FS-pSi (AgNPs@FSpSi) prepared at optimum conditions were utilized for molecular sensing based on the SERS method. As a result, the dynamics and versatility of SERS-active substrates were tested with diverse molecules such as a dye molecule [Methylene blue (MB)], a couple of explosives [Picric Acid, Ammonium Nitrate (PA, AN)], and a pesticide molecule (Thiram). Primarily, the sensitivities of the substrate were examined by experiencing the MB molecules with concertation ranging from 100 µM to 100 nM, data of which is shown in Fig. 5(a). The prominent modes of MB were identified at 1284 cm-1, 1435 cm-1, 1626 cm-1, which correspond to the C-H in-plane bending, C-C asymmetric, C-N ring stretching, modes respectively [49]. The intensity of the prominent peak at 1626 cm-1 decreases with decreasing concentration. The sensing capabilities of 10 µM MB were significantly correlated with the density of AgNPs on the FS-pSi, which is illustrated in Fig. 5(b). The intensity of 1626 cm-1 peak was observed to duly increase with increasing density of AgNPs. This observation is possibly owing to dense hot spots and effective local field spots, which are accountable for achieving lower detection limits.

 figure: Fig. 4.

Fig. 4. AgNPs decoration of FS-pSi at various deposition times (a) 30 min, (b) 60 min, (c) 4 hours, and (d) EDS spectrum of AgNPs@FSpSi-60min sample. [Inset of the figure (d) illustrates the distribution of AgNPs over the sample surface of FSpSi-60min [shown in (b)] and the solid line is a Gaussian fit].

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 figure: Fig. 5.

Fig. 5. The SERS spectra of MB molecules on AgNPs@FS-60min substrate at a concentration of (a)-(i) 100 µM (ii) 50 µM (iii) 10 µM (iv) 5 µM (v) 1 µM and (vi) 100 nM concentration (b) SERS spectra of MB (5 µM) at various AgNPs deposition time on FS-pSi. Spectra in (a) and (b) are stacked in Y-axis to avoid ambiguity in the data.

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The corresponding linear dependence of the Raman mode at 1626 cm-1 following analyte concentration with an R2 value of 0.83 is presented in Fig. 6(a). Apart from the linearity, the activity of sensing was also assessed by evaluating the analytical enhancement factor (AEF) by considering the adsorption factor η in the standard procedure using Eq. (3) [50,51]. The extracted AEF values are depicted in Table 2,

$$AEF = \frac{{{I_{SERS}}}}{{{I_{RS}}}} \times \frac{{{N_{RS}}}}{{\eta {\ast }{N_{SERS}}}}$$
where ISERS is the SERS intensity of analyte from the AgNPs@FSpSi, IRS is the intensity of the same mode from pSi substrate, NSERS and NRaman are the number of molecules contributing towards the SERS and Raman signals respectively. The calculated AEF (for a concentration of 100 nM MB) is ∼7.4×105, which is presented in Table 2. It is important to note here that the as-prepared FS-pSi did not show any significant molecular fingerprints in the Raman spectrum. Despite possessing strong enhancement factors, the commercial sensing abilities of a SERS substrate should satisfy the essential considerations including (a) stability (over a long period of time) (b) reproducibility (over the entire SERS substrate), and (c) recyclability (to reduce the overall costs of substrates). The stability factor is the ultimate parameter for long-term utilization in real-world applications. The stability of AgNPs-FSpSi-60 min was investigated over a period of ∼90 days with intervals of 10 days against exposure to ambient conditions. Typically, there were no substantial variations in the intensity for a continuous period of about three weeks. With aging time the Raman signal progressively decreased up to 60% and, finally, the Raman modes were diminished by >90% at the end of 12 weeks. Figure 6(b) illustrates the stability data of the SERS substrate accomplished with a 50 µM concentration of MB over a period of 90 days.

 figure: Fig. 6.

Fig. 6. (a) Linear dependence of log (SERS intensity) versus log (analyte concentration) for the principal modes of MB molecules, (b) The stability estimation of AgNPs@FSpSi-60min substrate with 50 µM concentration of MB over a period of 90 days.

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Tables Icon

Table 2. Detailed comparison and assessment of the estimated AEF for various analyte molecules and concentrations considered in the present study.

Additionally, to evaluate the signal consistency over the entire SERS substrate, the Raman signal of MB (10 µM) was recorded from 10 random positions of the sample surface, and the data obtained is displayed in Fig. 7(a) with corresponding statistical analysis shown in Fig. 7(b). The examination of the intensity variations of Raman mode at 1626 cm-1 shows sensible reproducibility with a relative standard deviation (RSD) value of 5%, which meets the important criterion of rapid and reliable detection in practical applications. After the primary investigations on the MB molecule, the sensitivity of these substrates was substantiated by extending the detection of high-energy molecules (explosives) such as picric acid (PA) and ammonium nitrate (AN), because these probe molecules are effectively exploited in the field of defense. Therefore, devoted attention is essential to identify these molecules, especially at trace level concentrations. Picric acid is a well-recognized explosive due to its ease of synthesis from generous chemicals and has toxic properties [52]. The detection of PA was accomplished with concentration levels ranging from 100 µM to 5 µM and the SERS data obtained is presented in Fig. 8(a). It is observed that the characteristic peaks were indexed at 832 cm-1, 1177 cm-1, and 1346 cm-1 [53]. The corresponding bond assessments are C-H bending, C-O stretching, and NO2 symmetric stretching, respectively [53]. Especially, the intensity of the Raman mode of PA (50 µM) at 1346 cm-1 was found to predominantly increase as a function of PA concentration. This is due to the modulated density of hot spots responsible for molecular detection of PA and the detailed spectra are presented in Fig. 8(b). Figure 8(c) clearly shows the linear dependence of the log(intensity) versus log(concentration) in the case of PA. The data is shown for three different Raman peaks in the spectra. The role of porosity (in pSi) in the measurements can only be ascertained by performing SERS measurements with similar sized nanoparticles on pSi and plain Si, which we could not achieve in this case. We plan to perform these experiments in the future by drop-casting the laser prepared nanoparticles on plain Si and pSi and identifying the porosity role in the Raman enhancements.

 figure: Fig. 7.

Fig. 7. (a) Reproducibility of the SERS spectra of 10 µM MB molecules detected at 10 different spots on AgNPs@FSpSi-60min, and (b) the corresponding standard analysis with RSD values.

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 figure: Fig. 8.

Fig. 8. The SERS spectra of PA, an explosive molecule, on AgNPs@FSpSi-60min substrate at concentration of (a)-(i) 100 µM, (ii) 50 µM, (iii) 30 µM, (iv) 10 µM, and (v) 5 µM concentrations, (b) SERS spectra of PA (30 µM) at various AgNPs deposition time on FS-pSi, and (c) corresponding linear calibration [log (SERS intensity) versus log (concentration)] of the different Raman modes observed at 832 cm-1, 1177 cm-1, and 1346 cm-1.

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The reproducibility of this substrate was examined by recording the SERS spectra of PA (at 30 µM) at various positions (randomly picked) of the sample surface and the analysed data with most prominent peaks at 832 cm-1, 1177 cm-1, and 1346 cm-1 are presented in Fig. 9(a). The estimated intensity of the Raman spectra is reasonably constant over the wide range of sample surfaces with a deviation (RSD) of <10%. The corresponding histograms in Fig. 9(b) depict typically obtained low RSD values of about 23%, 9%, and 7%, respectively, for the 832 cm-1, 1177 cm-1, and 1346 cm-1 peaks. The estimated AEF was found to be ∼1.3×104 for a 5 µM concentration of PA. The AEFs for other concentrations are summarized in Table 2.

 figure: Fig. 9.

Fig. 9. (a) Reproducibility of the SERS spectra of 50 µM PA molecules detected at 10 different spots on AgNDs@FSpSi-60min, and (b) the corresponding histogram with RSD values.

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In addition, another explosive ammonium nitrate (AN), which is a common fertilizer, has several bottlenecks in detection due to its lower sensing abilities and matrix effects. The various concentrations of AN molecules (ranging from 100 µM to 1 µM) were subjected to SERS measurements for examining the quality of AgNPs@FS-pSi substrate. The intensity distinctions were keenly observed by stacking the Raman spectra of AN molecules at various concentrations and are illustrated in Fig. 10(a). The characteristic Raman peaks were observed at 711 cm-1, and 1042 cm-1, with the corresponding assessments being bending of NO3-, and symmetric NO3- stretching, respectively [53]. The foremost signature of AN at 1040 cm-1 demonstrated intensity variation as a function of analyte concentrations. The Raman spectra of SERS-active substrates illustrating the hot-spots dependence (recorded with 50 µM concentration of AN) are presented in Fig. 10(b). The linear dependence on the intensity and concentration was obtained by plotting the log of intensity versus concentration shown in Fig. 10(c). The reproducibility spectra of AN for 50 µM concentration are presented in Fig. 10(d) with a corresponding RSD extracted from the data to be 4%. The calculated AEF was found to be 105 for 1 µM concentration. All the values are listed in Table 2.

 figure: Fig. 10.

Fig. 10. The SERS spectra of AN molecule on AgNPs@FSpSi-60min substrate at (a)-(i) 100 µM, (ii) 50 µM, (iii) 10 µM, (iv) 5 µM, and (v) 1 µM concentrations, (b) The SERS spectra of AN (50 µM) at various AgNPs deposition time on FS-pSi, and (c) corresponding linear calibration [log (SERS intensity) versus log (concentration)] of the Raman modes at 711 cm-1, and 1042 cm-1 (d) Reproducibility of AN (50 µM) on AgNDs@FSpSi-60min substrate and inset shows the corresponding standard deviation.

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The AgNPs@FSpSi-60min substrates were further investigated by performing the SERS measurements on a pesticide (Thiram) with different concentrations, ranging from 10 µM to 100 nM, and the data is shown in Fig. 11(a). The Raman peaks were observed at 1140 cm-1, 1385 cm-1, and 1428 cm-1 with the corresponding vibrations designated to CN stretching mode, symmetric CH3 deformation mode, asymmetric CH3 deformation mode, respectively [54]. The most distinct peak observed at 1385 cm-1 was noticed to be enriched with an increase in the density of AgNPs for 10 µM concentration and the data is presented in Fig. 11(b). A linear relation has been obtained via a log plot of intensity versus concentration and the data is presented in Fig. 11(c). The sensitivity of substrate with different concentrations was estimated by calculating the AEF, which is depicted in Table 2. For a specific (100 nM) concentration of thiram, the AEF was calculated to be 2.9×104.

 figure: Fig. 11.

Fig. 11. The SERS spectra of thiram (pesticide) on AgNPs@FSpSi-60min at (a) (i) 10 µM (ii) 5 µM (iii) 1 µM and (iv) 100 nM concentrations (b) SERS spectra of thiram (10 µM) at various AgNPs deposition time on FSpSi and (c) corresponding linear relationship of log (SERS intensity) versus log (concentration).

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Table 3 shows the comparison data of the detection capabilities of different pSi-based and flexible SERS substrates along with the values obtained from the present work. It is apparent that the SERS substrates investigated in this work are found to be on par (or better in few cases) with many of the recently reported flexible substrates. Further, the Raman enhancements achieved for the ammonium nitrate molecules (104) here seem to be comparable with those of silver dendrites (104) achieved by a simple electroless etching process that was recently reported by our group [13]. Interestingly, the preparation of both the substrates involved simple chemistry. A LOD of 36 nM (at least two orders of magnitude higher) was achieved in the case of PA SERS measurements [15] reported again by our group wherein we utilized Si micro-squared array substrate loaded/decorated with Ag-Au alloy NPs (obtained by femtosecond ablation). However, the procedure adopted there was slightly complex and involved more than one step. Further, the costs involved in that work will be higher than those involved here. It is extremely important to understand the (niche) application in mind before deciding on a particular SERS substrate. Our group has been working extensively on a variety of SERS substrates using different methodologies such as femtosecond/picosecond ablation and chemical methods wherein we have successfully demonstrated that solid [50,53,61] and hybrid SERS substrates [15,62,63] provide higher enhancement factors whereas the costs involved are also higher. Further, there is a need for the analyte molecule to be collected and taken to the SERS substrate for measurements. If we use flexible SERS substrates (for example paper substrates reported in [57]), we accomplish the collection of samples/analytes from different surfaces onto the SERS substrate directly thereby extending the provision of doing the measurements/detection in the field. However, enhancements, in this case, are moderate whereas the costs involved are much lower compared to solid/hybrid substrates. Similarly, in the present case though the enhancements are moderate (i) there is scope for improving them through further detailed optimization studies and, more significantly, (ii) the costs involved are much lower (commercial substrates cost 10-30 times more than that reported here). For example, each of the Stellarnet SERS substrates (cellulose with AuNPs) costs ∼10 USD (www.stellarnet.us) while each SERSitive substrates (electrodeposited Ag/Au on ITO glass) costs 25-30 USD (sensitive.eu). It is also pertinent to note here that these are tried and tested/optimized commercial substrates following years of research studies. We have performed a detailed study (results communicated elsewhere [64]) wherein a thorough comparison has been made on various flexible SERS substrate's performance, ease of preparation, and cost. We firmly believe that further optimization of the investigated substrates presented here is possible, resulting in further improved enhancement factors.

Tables Icon

Table 3. Summary of detection capability of various SERS substrates (typically metal nanoparticles comprising flexible and/or pSi substrate).

Furthermore, the important information of the limit of detection (LOD) [65,66] was extracted by examining the intensive Raman peaks of MB, PA, AN, and thiram at 1626 cm-1, 1346 cm-1, 1042 cm-1, and 1385 cm-1, respectively. The spectra presented in Figs. 12(a)-(d) depict the SERS intensity as a function of analyte concentration while the corresponding linear fits are presented in Figs. 12(e)-(h). The data and fits were found to be linear at lower concentrations while we see a slight saturation behavior at higher concentrations of the analyte molecules probably due to the complete adsorption leading to an occupation of all the available sites for enhancement on the nanostructure. The typical definition of LOD is ${\raise0.7ex\hbox{${3\sigma }$} \!\mathord{\left/ {\vphantom {{3\sigma } b}}\right. }\!\lower0.7ex\hbox{$b$}}$, where $\sigma $ is the standard deviation of FS-pSi substrate and ‘b’ is the slope of the resultant linear plot at lower analyte concentrations [Figs. 12 (e)-(h))]. The extracted LODs for MB, PA, AN, and thiram were 50 nM, 1 µM, 2 µM, and 1 µM, respectively.

 figure: Fig. 12.

Fig. 12. The SERS intensity versus analyte concentration for (a) MB - 1626 cm-1 (b) PA - 1346 cm-1 (c) AN - 1042 cm-1 (d) thiram-1385 cm-1, and (e)-(h) Linear dependence of the log SERS intensities verses lower molecular concentrations.

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The present investigations will be extended towards the detection of other hazardous molecules with the dependence of size and shape of AgNPs on the FS-pSi substrates. There is a huge scope in the modification of the AgNP sizes. In addition, the effect of pore size on the distribution and dimension of AgNPs will be evaluated by modulating the etching parameters such as etching current density (J) and the resistivity of Si. Moreover, additional attempts will be accomplished to improve the molecular AEF by decorating bi-metallic nanoparticles (for example, AgNPs and AuNPs obtained using femtosecond ablation [53]) on these FS-pSi substrates.

4. Conclusions

We reported here the synthesis of a new ultra-thin material with free-standing capability and flexibility for trace-level molecular detection. The FS-pSi has been prepared by adopting a simple anodic etching. The density of AgNPs could be controlled by altering the AgNO3 deposition time. The optimized AgNPs@FSpSi samples were subjected to testing of various analytes to assess the sensing capabilities. The SERS-active substrate was initially exposed to dye molecules (MB) and subsequently, the studies were extended towards the detection of AN, PA, and thiram. The estimated AEFs were in the range of 107-104 for MB and explosives. There is a possibility of increasing these numbers, essential for practical applications. Indeed, after evaluating all the possible parameters (versatility, stability, reproducibility, cost), we firmly believe that these AgNPs@FSpSi substrates are possible robust candidates for superior molecular detection with several attractive and important features. A very recent review article [67], which appeared after the preparation of this manuscript, on the diverse SERS applications of porous silicon vindicates the potential and the detailed studies performed in this work.

Funding

Institute of Eminence (UOH/IOE/RC1/RC1‐20‐016); DS Kothari Postdoctoral Fellowship (sanction order no. F.4-2/2006 (BSR)/PH/19-20/0008); Defence Research and Development Organisation (#ERIP/ER/1501138/M/01/319/D (R&D)).

Acknowledgments

VSV thanks UGC, New Delhi, for fellowship in the form of DS Kothari postdoctoral fellowship [sanction order no. F.4-2/2006 (BSR)/PH/19-20/0008]. APP thanks National Academy of Sciences India (NASI) for award of NASI Senior Scientist Platinum Jubilee Fellowship. V.R. Soma thanks DRDO, India for financial support [Project # ERIP/ER/1501138/M/01/319/D(R&D)]. V.R. Soma and S.V.S.N. Rao thank the University of Hyderabad (UoH) for financial support through the Institute of Eminence (IoE) project [No. UOH/IOE/RC1/RC1-20-016]. The IoE scheme was granted to the UoH by the Ministry of Education, Government of India, vide MHRD notification F11/9/2019-U3(A). V.R. Soma thanks the Director, ACRHEM, University of Hyderabad, India and Late Dr. A.K. Razdan, LASTEC, India for their support and encouragement.

Disclosures

The authors declare no conflicts of interest.

Data availability

Data underlying the results presented in this paper are not publicly available at this time but may be obtained from the authors upon reasonable request.

References

1. T. Böcking, K.A. Kilian, P.J. Reece, K. Gaus, M. Gal, and J.J. Gooding, “Biofunctionalization of free-standing porous silicon films for self-assembly of photonic devices,” Soft Matter 8(2), 360–366 (2012). [CrossRef]  

2. M. Sharma, P.R. Pudasaini, F. Ruiz-Zepeda, D. Elam, and A.A. Ayon, “Ultrathin, flexible organic-inorganic hybrid solar cells based on silicon nanowires and PEDOT:PSS,” ACS Appl. Mater. & Interf. 6(6), 4356–4363 (2014). [CrossRef]  

3. C. Pang, H. Cui, G. Yang, and C. Wang, “Flexible transparent and free-standing silicon nanowires paper,” Nano Lett. 13(10), 4708–4714 (2013). [CrossRef]  

4. S. Emamian, A. Eshkeiti, B.B. Narakathu, S.G.R. Avuthu, and M.Z. Atashbar, “Gravure printed flexible surface enhanced Raman spectroscopy (SERS) substrate for detection of 2,4-dinitrotoluene (DNT) vapor,” Sens. Actuators B Chem. 217, 129–135 (2015). [CrossRef]  

5. D. Cheng, M. He, J. Ran, G. Cai, J. Wu, and X. Wang, “Depositing a flexible substrate of triangular silver nanoplates onto cotton fabrics for sensitive SERS detection,” Sens. Actuators B Chem. 270, 508–517 (2018). [CrossRef]  

6. R.M. Cardoso, S.V.F. Castro, M.N.T. Silva, A.P. Lima, M.H.P. Santana, E. Nossol, R.A.B. Silva, E.M. Richter, T.R.L.C. Paixao, and R.A.A. Munoz, “3D-printed flexible device combining sampling and detection of explosives,” Sens. Actuators B Chem. 292, 308–313 (2019). [CrossRef]  

7. Y. He and T. Leïchlé, “Fabrication of lateral porous silicon membranes for planar microfluidics by means of ion implantation,” Sens. Actuators B Chem. 239, 628–634 (2017). [CrossRef]  

8. Q. He, Y. Han, Y. Huang, J. Gao, Y. Gao, L. Han, and Y. Zhang, “Reusable dual-enhancement SERS sensor based on graphene and hybrid nanostructures for ultrasensitive lead (II) detection,” Sens. Actuators B Chem. 341, 130031 (2021). [CrossRef]  

9. X. Tu, Z. Li, J. Lu, Y. Zhang, G. Yin, W. Wang, and D. He, “In situ preparation of Ag nanoparticles on silicon wafer as highly sensitive SERS substrate,” RSC Adv. 8(6), 2887–2891 (2018). [CrossRef]  

10. N.N. Durmanov, R.R. Guliev, A.V. Eremenko, I.A. Boginskaya, I.A. Ryzhikov, E.A. Trifonova, E.V. Putlyaev, A.N. Mukhin, S.L. Kalnov, M.V. Balandina, A.P. Tkachuk, V.A. Gushchin, A.K. Sarychev, A.N. Lagarkov, I.A. Rodionov, A.R. Gabidullin, and I.N. Kurochkin, “Non-labeled selective virus detection with novel SERS-active porous silver nanofilms fabricated by Electron Beam Physical Vapor Deposition,” Sens. Actuators B Chem. 257, 37–47 (2018). [CrossRef]  

11. S. Niyomdecha, W. Limbut, A. Numnuam, P. Asawatreratanakul, P. Kanatharana, and P. Thavarungkul, “A novel BOD biosensor based on entrapped activated sludge in a porous chitosan-albumin cryogel incorporated with graphene and methylene blue,” Sens. Actuators B Chem. 241, 473–481 (2017). [CrossRef]  

12. V.S. Vendamani, S.V.S. Nageswara Rao, S. Venugopal Rao, D. Kanjilal, and A.P. Pathak, “Three-dimensional hybrid silicon nanostructures for surface enhanced Raman spectroscopy based molecular detection,” J. Appl. Phys. 123(1), 014301 (2018). [CrossRef]  

13. V.S. Vendamani, S.V.S.N. Rao, A.P. Pathak, and V.R. Soma, “Robust and cost-effective silver dendritic nanostructures for SERS-based trace detection of RDX and ammonium nitrate,” RSC Adv. 10(73), 44747–44755 (2020). [CrossRef]  

14. S. Hamad, S.S. Bharati Moram, B. Yendeti, G.K. Podagatlapalli, S.V.S. Nageswara Rao, A.P. Pathak, M. A. Mohiddon, and V. R. Soma, “Femtosecond Laser-Induced, Nanoparticle-Embedded Periodic Surface Structures on Crystalline Silicon for Reproducible and Multi-utility SERS Platforms,” ACS Omega 3(12), 18420–18432 (2018). [CrossRef]  

15. S.S.B. Moram, A.K. Shaik, C. Byram, S. Hamad, and V.R. Soma, “Instantaneous trace detection of nitro-explosives and mixtures with nanotextured silicon decorated with Ag-Au alloy nanoparticles using the SERS technique,” Anal. Chim. Acta 1101, 157–168 (2020). [CrossRef]  

16. P. Serre, C. Ternon, V. Stambouli, P. Periwal, and T. Baron, “Fabrication of silicon nanowire networks for biological sensing,” Sens. Actuators B Chem. 182, 390–395 (2013). [CrossRef]  

17. J. A. Uhlir, “Electrolytic Shaping of Germanium and Silicon,” The Bell Sys. Tech. J. 35(2), 333–347 (1956). [CrossRef]  

18. T. Unagami, “Formation Mechanism of Porous Silicon Layer by Anodization in HF Solution,” J. Electrochem. Soc. 127(2), 476–483 (1980). [CrossRef]  

19. V.S. Vendamani, S.V.S. Nageswara Rao, and A.P. Pathak, “Structural and optical properties of porous silicon prepared by anodic etching of irradiated silicon,” Nucl. Instrum. Meth. Phys. Res. Section B: Beam Inter. Mater. and Atoms 315, 188–191 (2013). [CrossRef]  

20. S.V.S.N. Rao, V.S. Vendamani, S.K. Satrasala, S.K. Padhe, K.S. Rao, S. Dhamodaran, and A.P. Pathak, “Ion beam studies of semiconductor nanoparticles for the integration of optoelectronic devices,” AIP Conf. Proc.1336, 332–336 (2011).

21. L.T. Canham, “Silicon quantum wire array fabrication by electrochemical and chemical dissolution of wafers,” Appl. Phys. Lett. 57(10), 1046–1048 (1990). [CrossRef]  

22. A.G. Cullis, L.T. Canham, and P.D.J. Calcott, “The structural and luminescence properties of porous silicon,” J. Appl. Phys. 82(3), 909–965 (1997). [CrossRef]  

23. F.A. Harraz, “Porous silicon chemical sensors and biosensors: A review,” Sens. Actuators B Chem. 202, 897–912 (2014). [CrossRef]  

24. A.M. Alwan, L.A. Wali, and A.A. Yousif, “Optimization of AgNPs/mesoPS active substrates for ultra–low molecule detection process,” Silicon 10(5), 2241–2251 (2018). [CrossRef]  

25. S.K. Ramakrishan, M. Martin Fernandez, T. Cloitre, V. Agarwal, F.J.G. Cuisinier, and C. Gergely, “Porous silicon microcavities redefine colorimetric ELISA sensitivity for ultrasensitive detection of autoimmune antibodies,” Sens. Actuators B Chem. 272, 211–218 (2018). [CrossRef]  

26. S. Mourya, A. Kumar, J. Jaiswal, G. Malik, B. Kumar, and R. Chandra, “Development of Pd-Pt functionalized high performance H2 gas sensor based on silicon carbide coated porous silicon for extreme environment applications,” Sens. Actuators B Chem. 283, 373–383 (2019). [CrossRef]  

27. H.V. Bandarenka, K.V. Girel, S.A. Zavatski, A. Panarin, and S.N. Terekhov, “Progress in the development of SERS-active substrates based on metal-coated porous silicon,” Materials 11(5), 852 (2018). [CrossRef]  

28. T. Cao, Y. Zhao, C.A. Nattoo, R. Layouni, and S.M. Weiss, “A smartphone biosensor based on analysing structural colour of porous silicon,” Analyst 144(13), 3942–3948 (2019). [CrossRef]  

29. F. Giorgis, E. Descrovi, A. Chiodoni, E. Froner, M. Scarpa, A. Venturello, and F. Geobaldo, “Porous silicon as efficient surface enhanced Raman scattering (SERS) substrate,” Appl. Surf. Sci. 254(22), 7494–7497 (2008). [CrossRef]  

30. O. Garel, C. Breluzeau, E. Dufour-Gergam, A. Bosseboeuf, B. Belier, V. Mathet, and F Verjus, “Fabrication of free-standing porous silicon microstructures,” J. Micromech. Microeng. 17(7), S164–S167 (2007). [CrossRef]  

31. P.R. G. Lammel, “Free-standing, mobile 3D porous silicon microstructures,” Sensors and Actuators A: Phys. 85(1-3), 356–360 (2000). [CrossRef]  

32. X.G. Zhang, S.D. Collins, and R.L. Smith, “Porous silicon formation and electropolishing of silicon by anodic polarization in HF solution,” J. Electrochem. Soc. 136, 1561–1565 (1989). [CrossRef]  

33. M.T. S. Billat, R. Arens-Fischer, M.G. Berger, M. Kruger, and H. Luth, “Influence of etch stops on the microstructure of porous silicon layers,” Thin Solid Films 297(1-2), 22–25 (1997). [CrossRef]  

34. X.M. Qian and S.M. Nie, “Single-molecule and single-nanoparticle SERS: from fundamental mechanisms to biomedical applications,” Chem. Soc. Rev. 37(5), 912–920 (2008). [CrossRef]  

35. M. Sree Satya Bharati, C. Byram, and V. R. Soma, “Femtosecond laser fabricated Ag@Au and Cu@Au alloy nanoparticles for surface enhanced Raman spectroscopy based trace explosives detection,” Front. Phys. 6, 28 (2018). [CrossRef]  

36. S. Yang, X. Dai, B.B. Stogin, and T.S. Wong, “Ultrasensitive surface-enhanced Raman scattering detection in common fluids,” Proc. Nat. Acad. Sci. 113(2), 268–273 (2016). [CrossRef]  

37. D.-Y. Xu, X.-M. Liu, S. Duan, X. Xu, B. Ren, S.-H. Lin, and Z.-Q. Tian, “Chemical enhancement effects in SERS Spectra: A quantum chemical study of pyridine interacting with Copper, Silver, Gold and Platinum metals,” J. Phys. Chem. C 112(11), 4195–4204 (2008). [CrossRef]  

38. Y. Tang, Z. Zhao, H. Hu, Y. Liu, X. Wang, S. Zhou, and J. Qiu, “Highly stretchable and ultrasensitive strain sensor based on reduced graphene oxide microtubes-elastomer composite,” ACS Appl. Mater. & Interf. 7(49), 27432–27439 (2015). [CrossRef]  

39. C. Cheng, J. Li, H. Lei, and B. Li, “Surface enhanced Raman scattering of gold nanoparticles aggregated by a gold-nanofilm-coated nanofiber,” Photonics Res. 6, 357 (2018). [CrossRef]  

40. S.I. Kudryashov, P.A. Danilov, A.P. Porfirev, I.N. Saraeva, T.H.T. Nguyen, A.A. Rudenko, R.A. Khmelnitskii, D.A. Zayarny, A.A. Ionin, A.A. Kuchmizhak, S.N. Khonina, and O.B. Vitrik, “High-throughput micropatterning of plasmonic surfaces by multiplexed femtosecond laser pulses for advanced IR-sensing applications,” Appl. Surf. Sci. 484, 948–956 (2019). [CrossRef]  

41. Sara Fateixa, Helena I. S. Nogueira, and Tito Trindade, “Hybrid nanostructures for SERS: materials development and chemical detection,” Phys. Chem. Chem. Phys. 17(33), 21046–21071 (2015). [CrossRef]  

42. M. Fan, G.F. Andrade, and A.G. Brolo, “A review on the fabrication of substrates for surface enhanced Raman spectroscopy and their applications in analytical chemistry,” Anal. Chim. Acta 693(1-2), 7–25 (2011). [CrossRef]  

43. C. Novara, S. Dalla Marta, A. Virga, A. Lamberti, A. Angelini, A. Chiadò, P. Rivolo, F. Geobaldo, V. Sergo, A. Bonifacio, and F. Giorgis, “SERS-Active Ag nanoparticles on porous silicon and PDMS Substrates: A comparative study of uniformity and Raman efficiency,” J. Phys. Chem. C 120(30), 16946–16953 (2016). [CrossRef]  

44. F. Zhong, Z. Wu, J. Guo, and D. Jia, “Porous silicon photonic crystals coated with Ag nanoparticles as efficient substrates for detecting trace explosives using SERS,” Nanomaterials 8(11), 872 (2018). [CrossRef]  

45. V.S. Vendamani, S. Hamad, V. Saikiran, A.P. Pathak, S. Venugopal Rao, V.V. Ravi Kanth Kumar, and S.V.S.N. Rao, “Synthesis of ultra-small silicon nanoparticles by femtosecond laser ablation of porous silicon,” J. Mater. Sci. 50(4), 1666–1672 (2015). [CrossRef]  

46. L. T. Canham, “Properties of Porous Silicon,” INSPEC, The Institution of Electrical Engineers, London, United Kingdom, (1997) 12–22.

47. D. Wang, F. Wang, and H. Yang, “Robust, flexible, sticky and high sensitive SERS membrane for rapid detection applications,” Sens. Actuators B Chem. 274, 676–681 (2018). [CrossRef]  

48. G. Oskam, J.G. Long, A. Natarajan, and P. C. Searson, “Electrochemical deposition of metals onto silicon,” J Phys. D: Appl. Phys. 31(16), 1927–1949 (1998). [CrossRef]  

49. W. Zhang, Z. Chen, Y. Guan, C. Liu, K. Zheng, and X. Zou, “Aptamer-functionalized screen-printed electrode coupled with graphene oxide and methylene blue nanocomposite as enhanced signal label for total arsenic determination in shellfish,” Sens. Actuators B Chem. 335, 129383 (2021). [CrossRef]  

50. S. Hamad, G.K. Podagatlapalli, M.A. Mohiddon, and V.R. Soma, “Cost effective nanostructured copper substrates prepared with ultrafast laser pulses for explosives detection using surface enhanced Raman scattering,” Appl. Phys. Lett. 104(26), 263104 (2014). [CrossRef]  

51. U.P. Shaik, S. Hamad, M. Ahamad Mohiddon, V.R. Soma, and M. Ghanashyam Krishna, “Morphologically manipulated Ag/ZnO nanostructures as surface enhanced Raman scattering probes for explosives detection,” J. Appl. Phys. 119(9), 093103 (2016). [CrossRef]  

52. Y. Fan, Y. Zhang, N. Li, S.G. Liu, T. Liu, N. Li, and H. Luo, “A facile synthesis of water-soluble carbon dots as a label-free fluorescent probe for rapid, selective and sensitive detection of picric acid,” Sens. Actuators B Chem. 240, 949–955 (2017). [CrossRef]  

53. M.S. Satya Bharati, B. Chandu, and S.V. Rao, “Explosives sensing using Ag–Cu alloy nanoparticles synthesized by femtosecond laser ablation and irradiation,” RSC Adv. 9(3), 1517–1525 (2019). [CrossRef]  

54. S. Kumar, P. Goel, and J.P. Singh, “Flexible and robust SERS active substrates for conformal rapid detection of pesticide residues from fruits,” Sens. Actuators B Chem. 241, 577–583 (2017). [CrossRef]  

55. C. Wang, B. Liu, and X. Dou, “Silver nanotriangles-loaded filter paper for ultrasensitive SERS detection application benefited by interspacing of sharp edges,” Sens. Actuators B Chem. 231, 357–364 (2016). [CrossRef]  

56. S.S.B. Moram, C. Byram, and V.R. Soma, “Gold-nanoparticle- and nanostar-loaded paper-based SERS substrates for sensing nanogram-level Picric acid with a portable Raman spectrometer,” Bull. Mater. Sci. 43, 8190–8201 (2020). [CrossRef]  

57. S.S.B. Moram, C. Byram, S.N. Shibu, B.M. Chilukamarri, and V.R. Soma, “Ag/Au nanoparticle-loaded paper-based versatile surface-enhanced Raman spectroscopy substrates for multiple explosives detection,” ACS Omega 3(7), 8190–8201 (2018). [CrossRef]  

58. V.-T. Vo, Y. Gwon, V.-D. Phung, Y.-D. Son, J.-H. Kim, and S.-W. Lee, “Ag-Deposited Porous Silicon as a SERS-Active Substrate for the Sensitive Detection of Catecholamine Neurotransmitters,” Electron. Mater. Lett. 17(3), 292–298 (2021). [CrossRef]  

59. R. Gao, X. Song, C. Zhan, C. Weng, S. Cheng, K. Guo, N. Ma, H. Chang, Z. Guo, L. B. Luo, and L. Yu, “Light trapping induced flexible wrinkled nanocone SERS substrate for highly sensitive explosive detection,” Sensors and Actuators B: Chemical 314, 128081 (2020). [CrossRef]  

60. C. Li, J. Yu, S. Xu, S. Jiang, X. Xiu, C. Chen, A. Liu, T. Wu, B. Man, and C. Zhang, “Constructing 3D and flexible plasmonic structure for high-performance SERS application,” Adv. Mater. Technol. 3, 1800174 (2018). [CrossRef]  

61. C. Byram, S. S. B. Moram, and V. R. Soma, “SERS based multiple analyte detection from explosive mixtures using picosecond laser fabricated gold nanoparticles, nanostructures,” Analyst 144(7), 2327–2336 (2019). [CrossRef]  

62. Tania K. Naqvi, Abhilash Bajpai, Sree Satya Bharati Moram, Manish M. Kulkarni, Azher M. Siddiqui, S. Venugopal Rao, and Prabhat K. Dwivedi, “Ultra-sensitive reusable SERS sensor for multiple hazardous materials detections on single platform,” J. Hazard. Mater. 407, 124353 (2021). [CrossRef]  

63. Tania K. Naqvi, Moram Sree Satya Bharati, Alok K. Srivastava, Manish M. Kulkarni, Azher M. Siddiqui, S. Venugopal Rao, and Prabhat K. Dwivedi, “Femtosecond laser textured silver/graphene oxide hybrid SERS substrate for detection of an explosive precursor 2,4-DNT,” ACS Omega 4(18), 17691–17701 (2019). [CrossRef]  

64. Moram Sree Satya Bharati and Venugopal Rao Soma, “Flexible SERS Substrates for Hazardous Materials Detection: Recent Advances,” Optoelectronic Advances 4, 210048 (2021).

65. Govind Kumar and R.K. Soni, “Silver Nanocube- and Nanowire-Based SERS Substrates for Ultra-low Detection of PATP and Thiram Molecules,” Plasmonics 15(6), 1577–1589 (2020). [CrossRef]  

66. A. Shrivastava and V.B. Gupta, “Methods for the determination of limit of detection and limit of quantitation of the analytical methods,” Chron Young Sci 2, 21–25 (2011). [CrossRef]  

67. N. Khinevich, H. Bandarenka, S. Zavatski, K. Girel, A. Tamulevičienė, and T.S. Tamulevičius, “Porous silicon - A versatile platform for mass-production of ultrasensitive SERS-active substrates,” Microporous and Mesoporous Mater. 323, 111204 (2021). [CrossRef]  

References

  • View by:

  1. T. Böcking, K.A. Kilian, P.J. Reece, K. Gaus, M. Gal, and J.J. Gooding, “Biofunctionalization of free-standing porous silicon films for self-assembly of photonic devices,” Soft Matter 8(2), 360–366 (2012).
    [Crossref]
  2. M. Sharma, P.R. Pudasaini, F. Ruiz-Zepeda, D. Elam, and A.A. Ayon, “Ultrathin, flexible organic-inorganic hybrid solar cells based on silicon nanowires and PEDOT:PSS,” ACS Appl. Mater. & Interf. 6(6), 4356–4363 (2014).
    [Crossref]
  3. C. Pang, H. Cui, G. Yang, and C. Wang, “Flexible transparent and free-standing silicon nanowires paper,” Nano Lett. 13(10), 4708–4714 (2013).
    [Crossref]
  4. S. Emamian, A. Eshkeiti, B.B. Narakathu, S.G.R. Avuthu, and M.Z. Atashbar, “Gravure printed flexible surface enhanced Raman spectroscopy (SERS) substrate for detection of 2,4-dinitrotoluene (DNT) vapor,” Sens. Actuators B Chem. 217, 129–135 (2015).
    [Crossref]
  5. D. Cheng, M. He, J. Ran, G. Cai, J. Wu, and X. Wang, “Depositing a flexible substrate of triangular silver nanoplates onto cotton fabrics for sensitive SERS detection,” Sens. Actuators B Chem. 270, 508–517 (2018).
    [Crossref]
  6. R.M. Cardoso, S.V.F. Castro, M.N.T. Silva, A.P. Lima, M.H.P. Santana, E. Nossol, R.A.B. Silva, E.M. Richter, T.R.L.C. Paixao, and R.A.A. Munoz, “3D-printed flexible device combining sampling and detection of explosives,” Sens. Actuators B Chem. 292, 308–313 (2019).
    [Crossref]
  7. Y. He and T. Leïchlé, “Fabrication of lateral porous silicon membranes for planar microfluidics by means of ion implantation,” Sens. Actuators B Chem. 239, 628–634 (2017).
    [Crossref]
  8. Q. He, Y. Han, Y. Huang, J. Gao, Y. Gao, L. Han, and Y. Zhang, “Reusable dual-enhancement SERS sensor based on graphene and hybrid nanostructures for ultrasensitive lead (II) detection,” Sens. Actuators B Chem. 341, 130031 (2021).
    [Crossref]
  9. X. Tu, Z. Li, J. Lu, Y. Zhang, G. Yin, W. Wang, and D. He, “In situ preparation of Ag nanoparticles on silicon wafer as highly sensitive SERS substrate,” RSC Adv. 8(6), 2887–2891 (2018).
    [Crossref]
  10. N.N. Durmanov, R.R. Guliev, A.V. Eremenko, I.A. Boginskaya, I.A. Ryzhikov, E.A. Trifonova, E.V. Putlyaev, A.N. Mukhin, S.L. Kalnov, M.V. Balandina, A.P. Tkachuk, V.A. Gushchin, A.K. Sarychev, A.N. Lagarkov, I.A. Rodionov, A.R. Gabidullin, and I.N. Kurochkin, “Non-labeled selective virus detection with novel SERS-active porous silver nanofilms fabricated by Electron Beam Physical Vapor Deposition,” Sens. Actuators B Chem. 257, 37–47 (2018).
    [Crossref]
  11. S. Niyomdecha, W. Limbut, A. Numnuam, P. Asawatreratanakul, P. Kanatharana, and P. Thavarungkul, “A novel BOD biosensor based on entrapped activated sludge in a porous chitosan-albumin cryogel incorporated with graphene and methylene blue,” Sens. Actuators B Chem. 241, 473–481 (2017).
    [Crossref]
  12. V.S. Vendamani, S.V.S. Nageswara Rao, S. Venugopal Rao, D. Kanjilal, and A.P. Pathak, “Three-dimensional hybrid silicon nanostructures for surface enhanced Raman spectroscopy based molecular detection,” J. Appl. Phys. 123(1), 014301 (2018).
    [Crossref]
  13. V.S. Vendamani, S.V.S.N. Rao, A.P. Pathak, and V.R. Soma, “Robust and cost-effective silver dendritic nanostructures for SERS-based trace detection of RDX and ammonium nitrate,” RSC Adv. 10(73), 44747–44755 (2020).
    [Crossref]
  14. S. Hamad, S.S. Bharati Moram, B. Yendeti, G.K. Podagatlapalli, S.V.S. Nageswara Rao, A.P. Pathak, M. A. Mohiddon, and V. R. Soma, “Femtosecond Laser-Induced, Nanoparticle-Embedded Periodic Surface Structures on Crystalline Silicon for Reproducible and Multi-utility SERS Platforms,” ACS Omega 3(12), 18420–18432 (2018).
    [Crossref]
  15. S.S.B. Moram, A.K. Shaik, C. Byram, S. Hamad, and V.R. Soma, “Instantaneous trace detection of nitro-explosives and mixtures with nanotextured silicon decorated with Ag-Au alloy nanoparticles using the SERS technique,” Anal. Chim. Acta 1101, 157–168 (2020).
    [Crossref]
  16. P. Serre, C. Ternon, V. Stambouli, P. Periwal, and T. Baron, “Fabrication of silicon nanowire networks for biological sensing,” Sens. Actuators B Chem. 182, 390–395 (2013).
    [Crossref]
  17. J. A. Uhlir, “Electrolytic Shaping of Germanium and Silicon,” The Bell Sys. Tech. J. 35(2), 333–347 (1956).
    [Crossref]
  18. T. Unagami, “Formation Mechanism of Porous Silicon Layer by Anodization in HF Solution,” J. Electrochem. Soc. 127(2), 476–483 (1980).
    [Crossref]
  19. V.S. Vendamani, S.V.S. Nageswara Rao, and A.P. Pathak, “Structural and optical properties of porous silicon prepared by anodic etching of irradiated silicon,” Nucl. Instrum. Meth. Phys. Res. Section B: Beam Inter. Mater. and Atoms 315, 188–191 (2013).
    [Crossref]
  20. S.V.S.N. Rao, V.S. Vendamani, S.K. Satrasala, S.K. Padhe, K.S. Rao, S. Dhamodaran, and A.P. Pathak, “Ion beam studies of semiconductor nanoparticles for the integration of optoelectronic devices,” AIP Conf. Proc.1336, 332–336 (2011).
  21. L.T. Canham, “Silicon quantum wire array fabrication by electrochemical and chemical dissolution of wafers,” Appl. Phys. Lett. 57(10), 1046–1048 (1990).
    [Crossref]
  22. A.G. Cullis, L.T. Canham, and P.D.J. Calcott, “The structural and luminescence properties of porous silicon,” J. Appl. Phys. 82(3), 909–965 (1997).
    [Crossref]
  23. F.A. Harraz, “Porous silicon chemical sensors and biosensors: A review,” Sens. Actuators B Chem. 202, 897–912 (2014).
    [Crossref]
  24. A.M. Alwan, L.A. Wali, and A.A. Yousif, “Optimization of AgNPs/mesoPS active substrates for ultra–low molecule detection process,” Silicon 10(5), 2241–2251 (2018).
    [Crossref]
  25. S.K. Ramakrishan, M. Martin Fernandez, T. Cloitre, V. Agarwal, F.J.G. Cuisinier, and C. Gergely, “Porous silicon microcavities redefine colorimetric ELISA sensitivity for ultrasensitive detection of autoimmune antibodies,” Sens. Actuators B Chem. 272, 211–218 (2018).
    [Crossref]
  26. S. Mourya, A. Kumar, J. Jaiswal, G. Malik, B. Kumar, and R. Chandra, “Development of Pd-Pt functionalized high performance H2 gas sensor based on silicon carbide coated porous silicon for extreme environment applications,” Sens. Actuators B Chem. 283, 373–383 (2019).
    [Crossref]
  27. H.V. Bandarenka, K.V. Girel, S.A. Zavatski, A. Panarin, and S.N. Terekhov, “Progress in the development of SERS-active substrates based on metal-coated porous silicon,” Materials 11(5), 852 (2018).
    [Crossref]
  28. T. Cao, Y. Zhao, C.A. Nattoo, R. Layouni, and S.M. Weiss, “A smartphone biosensor based on analysing structural colour of porous silicon,” Analyst 144(13), 3942–3948 (2019).
    [Crossref]
  29. F. Giorgis, E. Descrovi, A. Chiodoni, E. Froner, M. Scarpa, A. Venturello, and F. Geobaldo, “Porous silicon as efficient surface enhanced Raman scattering (SERS) substrate,” Appl. Surf. Sci. 254(22), 7494–7497 (2008).
    [Crossref]
  30. O. Garel, C. Breluzeau, E. Dufour-Gergam, A. Bosseboeuf, B. Belier, V. Mathet, and F Verjus, “Fabrication of free-standing porous silicon microstructures,” J. Micromech. Microeng. 17(7), S164–S167 (2007).
    [Crossref]
  31. P.R. G. Lammel, “Free-standing, mobile 3D porous silicon microstructures,” Sensors and Actuators A: Phys. 85(1-3), 356–360 (2000).
    [Crossref]
  32. X.G. Zhang, S.D. Collins, and R.L. Smith, “Porous silicon formation and electropolishing of silicon by anodic polarization in HF solution,” J. Electrochem. Soc. 136, 1561–1565 (1989).
    [Crossref]
  33. M.T. S. Billat, R. Arens-Fischer, M.G. Berger, M. Kruger, and H. Luth, “Influence of etch stops on the microstructure of porous silicon layers,” Thin Solid Films 297(1-2), 22–25 (1997).
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  34. X.M. Qian and S.M. Nie, “Single-molecule and single-nanoparticle SERS: from fundamental mechanisms to biomedical applications,” Chem. Soc. Rev. 37(5), 912–920 (2008).
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  35. M. Sree Satya Bharati, C. Byram, and V. R. Soma, “Femtosecond laser fabricated Ag@Au and Cu@Au alloy nanoparticles for surface enhanced Raman spectroscopy based trace explosives detection,” Front. Phys. 6, 28 (2018).
    [Crossref]
  36. S. Yang, X. Dai, B.B. Stogin, and T.S. Wong, “Ultrasensitive surface-enhanced Raman scattering detection in common fluids,” Proc. Nat. Acad. Sci. 113(2), 268–273 (2016).
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  37. D.-Y. Xu, X.-M. Liu, S. Duan, X. Xu, B. Ren, S.-H. Lin, and Z.-Q. Tian, “Chemical enhancement effects in SERS Spectra: A quantum chemical study of pyridine interacting with Copper, Silver, Gold and Platinum metals,” J. Phys. Chem. C 112(11), 4195–4204 (2008).
    [Crossref]
  38. Y. Tang, Z. Zhao, H. Hu, Y. Liu, X. Wang, S. Zhou, and J. Qiu, “Highly stretchable and ultrasensitive strain sensor based on reduced graphene oxide microtubes-elastomer composite,” ACS Appl. Mater. & Interf. 7(49), 27432–27439 (2015).
    [Crossref]
  39. C. Cheng, J. Li, H. Lei, and B. Li, “Surface enhanced Raman scattering of gold nanoparticles aggregated by a gold-nanofilm-coated nanofiber,” Photonics Res. 6, 357 (2018).
    [Crossref]
  40. S.I. Kudryashov, P.A. Danilov, A.P. Porfirev, I.N. Saraeva, T.H.T. Nguyen, A.A. Rudenko, R.A. Khmelnitskii, D.A. Zayarny, A.A. Ionin, A.A. Kuchmizhak, S.N. Khonina, and O.B. Vitrik, “High-throughput micropatterning of plasmonic surfaces by multiplexed femtosecond laser pulses for advanced IR-sensing applications,” Appl. Surf. Sci. 484, 948–956 (2019).
    [Crossref]
  41. Sara Fateixa, Helena I. S. Nogueira, and Tito Trindade, “Hybrid nanostructures for SERS: materials development and chemical detection,” Phys. Chem. Chem. Phys. 17(33), 21046–21071 (2015).
    [Crossref]
  42. M. Fan, G.F. Andrade, and A.G. Brolo, “A review on the fabrication of substrates for surface enhanced Raman spectroscopy and their applications in analytical chemistry,” Anal. Chim. Acta 693(1-2), 7–25 (2011).
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  43. C. Novara, S. Dalla Marta, A. Virga, A. Lamberti, A. Angelini, A. Chiadò, P. Rivolo, F. Geobaldo, V. Sergo, A. Bonifacio, and F. Giorgis, “SERS-Active Ag nanoparticles on porous silicon and PDMS Substrates: A comparative study of uniformity and Raman efficiency,” J. Phys. Chem. C 120(30), 16946–16953 (2016).
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  44. F. Zhong, Z. Wu, J. Guo, and D. Jia, “Porous silicon photonic crystals coated with Ag nanoparticles as efficient substrates for detecting trace explosives using SERS,” Nanomaterials 8(11), 872 (2018).
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  45. V.S. Vendamani, S. Hamad, V. Saikiran, A.P. Pathak, S. Venugopal Rao, V.V. Ravi Kanth Kumar, and S.V.S.N. Rao, “Synthesis of ultra-small silicon nanoparticles by femtosecond laser ablation of porous silicon,” J. Mater. Sci. 50(4), 1666–1672 (2015).
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  47. D. Wang, F. Wang, and H. Yang, “Robust, flexible, sticky and high sensitive SERS membrane for rapid detection applications,” Sens. Actuators B Chem. 274, 676–681 (2018).
    [Crossref]
  48. G. Oskam, J.G. Long, A. Natarajan, and P. C. Searson, “Electrochemical deposition of metals onto silicon,” J Phys. D: Appl. Phys. 31(16), 1927–1949 (1998).
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  49. W. Zhang, Z. Chen, Y. Guan, C. Liu, K. Zheng, and X. Zou, “Aptamer-functionalized screen-printed electrode coupled with graphene oxide and methylene blue nanocomposite as enhanced signal label for total arsenic determination in shellfish,” Sens. Actuators B Chem. 335, 129383 (2021).
    [Crossref]
  50. S. Hamad, G.K. Podagatlapalli, M.A. Mohiddon, and V.R. Soma, “Cost effective nanostructured copper substrates prepared with ultrafast laser pulses for explosives detection using surface enhanced Raman scattering,” Appl. Phys. Lett. 104(26), 263104 (2014).
    [Crossref]
  51. U.P. Shaik, S. Hamad, M. Ahamad Mohiddon, V.R. Soma, and M. Ghanashyam Krishna, “Morphologically manipulated Ag/ZnO nanostructures as surface enhanced Raman scattering probes for explosives detection,” J. Appl. Phys. 119(9), 093103 (2016).
    [Crossref]
  52. Y. Fan, Y. Zhang, N. Li, S.G. Liu, T. Liu, N. Li, and H. Luo, “A facile synthesis of water-soluble carbon dots as a label-free fluorescent probe for rapid, selective and sensitive detection of picric acid,” Sens. Actuators B Chem. 240, 949–955 (2017).
    [Crossref]
  53. M.S. Satya Bharati, B. Chandu, and S.V. Rao, “Explosives sensing using Ag–Cu alloy nanoparticles synthesized by femtosecond laser ablation and irradiation,” RSC Adv. 9(3), 1517–1525 (2019).
    [Crossref]
  54. S. Kumar, P. Goel, and J.P. Singh, “Flexible and robust SERS active substrates for conformal rapid detection of pesticide residues from fruits,” Sens. Actuators B Chem. 241, 577–583 (2017).
    [Crossref]
  55. C. Wang, B. Liu, and X. Dou, “Silver nanotriangles-loaded filter paper for ultrasensitive SERS detection application benefited by interspacing of sharp edges,” Sens. Actuators B Chem. 231, 357–364 (2016).
    [Crossref]
  56. S.S.B. Moram, C. Byram, and V.R. Soma, “Gold-nanoparticle- and nanostar-loaded paper-based SERS substrates for sensing nanogram-level Picric acid with a portable Raman spectrometer,” Bull. Mater. Sci. 43, 8190–8201 (2020).
    [Crossref]
  57. S.S.B. Moram, C. Byram, S.N. Shibu, B.M. Chilukamarri, and V.R. Soma, “Ag/Au nanoparticle-loaded paper-based versatile surface-enhanced Raman spectroscopy substrates for multiple explosives detection,” ACS Omega 3(7), 8190–8201 (2018).
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  58. V.-T. Vo, Y. Gwon, V.-D. Phung, Y.-D. Son, J.-H. Kim, and S.-W. Lee, “Ag-Deposited Porous Silicon as a SERS-Active Substrate for the Sensitive Detection of Catecholamine Neurotransmitters,” Electron. Mater. Lett. 17(3), 292–298 (2021).
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  59. R. Gao, X. Song, C. Zhan, C. Weng, S. Cheng, K. Guo, N. Ma, H. Chang, Z. Guo, L. B. Luo, and L. Yu, “Light trapping induced flexible wrinkled nanocone SERS substrate for highly sensitive explosive detection,” Sensors and Actuators B: Chemical 314, 128081 (2020).
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  60. C. Li, J. Yu, S. Xu, S. Jiang, X. Xiu, C. Chen, A. Liu, T. Wu, B. Man, and C. Zhang, “Constructing 3D and flexible plasmonic structure for high-performance SERS application,” Adv. Mater. Technol. 3, 1800174 (2018).
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  61. C. Byram, S. S. B. Moram, and V. R. Soma, “SERS based multiple analyte detection from explosive mixtures using picosecond laser fabricated gold nanoparticles, nanostructures,” Analyst 144(7), 2327–2336 (2019).
    [Crossref]
  62. Tania K. Naqvi, Abhilash Bajpai, Sree Satya Bharati Moram, Manish M. Kulkarni, Azher M. Siddiqui, S. Venugopal Rao, and Prabhat K. Dwivedi, “Ultra-sensitive reusable SERS sensor for multiple hazardous materials detections on single platform,” J. Hazard. Mater. 407, 124353 (2021).
    [Crossref]
  63. Tania K. Naqvi, Moram Sree Satya Bharati, Alok K. Srivastava, Manish M. Kulkarni, Azher M. Siddiqui, S. Venugopal Rao, and Prabhat K. Dwivedi, “Femtosecond laser textured silver/graphene oxide hybrid SERS substrate for detection of an explosive precursor 2,4-DNT,” ACS Omega 4(18), 17691–17701 (2019).
    [Crossref]
  64. Moram Sree Satya Bharati and Venugopal Rao Soma, “Flexible SERS Substrates for Hazardous Materials Detection: Recent Advances,” Optoelectronic Advances 4, 210048 (2021).
  65. Govind Kumar and R.K. Soni, “Silver Nanocube- and Nanowire-Based SERS Substrates for Ultra-low Detection of PATP and Thiram Molecules,” Plasmonics 15(6), 1577–1589 (2020).
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  66. A. Shrivastava and V.B. Gupta, “Methods for the determination of limit of detection and limit of quantitation of the analytical methods,” Chron Young Sci 2, 21–25 (2011).
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  67. N. Khinevich, H. Bandarenka, S. Zavatski, K. Girel, A. Tamulevičienė, and T.S. Tamulevičius, “Porous silicon - A versatile platform for mass-production of ultrasensitive SERS-active substrates,” Microporous and Mesoporous Mater. 323, 111204 (2021).
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2021 (6)

Q. He, Y. Han, Y. Huang, J. Gao, Y. Gao, L. Han, and Y. Zhang, “Reusable dual-enhancement SERS sensor based on graphene and hybrid nanostructures for ultrasensitive lead (II) detection,” Sens. Actuators B Chem. 341, 130031 (2021).
[Crossref]

W. Zhang, Z. Chen, Y. Guan, C. Liu, K. Zheng, and X. Zou, “Aptamer-functionalized screen-printed electrode coupled with graphene oxide and methylene blue nanocomposite as enhanced signal label for total arsenic determination in shellfish,” Sens. Actuators B Chem. 335, 129383 (2021).
[Crossref]

V.-T. Vo, Y. Gwon, V.-D. Phung, Y.-D. Son, J.-H. Kim, and S.-W. Lee, “Ag-Deposited Porous Silicon as a SERS-Active Substrate for the Sensitive Detection of Catecholamine Neurotransmitters,” Electron. Mater. Lett. 17(3), 292–298 (2021).
[Crossref]

Tania K. Naqvi, Abhilash Bajpai, Sree Satya Bharati Moram, Manish M. Kulkarni, Azher M. Siddiqui, S. Venugopal Rao, and Prabhat K. Dwivedi, “Ultra-sensitive reusable SERS sensor for multiple hazardous materials detections on single platform,” J. Hazard. Mater. 407, 124353 (2021).
[Crossref]

Moram Sree Satya Bharati and Venugopal Rao Soma, “Flexible SERS Substrates for Hazardous Materials Detection: Recent Advances,” Optoelectronic Advances 4, 210048 (2021).

N. Khinevich, H. Bandarenka, S. Zavatski, K. Girel, A. Tamulevičienė, and T.S. Tamulevičius, “Porous silicon - A versatile platform for mass-production of ultrasensitive SERS-active substrates,” Microporous and Mesoporous Mater. 323, 111204 (2021).
[Crossref]

2020 (5)

Govind Kumar and R.K. Soni, “Silver Nanocube- and Nanowire-Based SERS Substrates for Ultra-low Detection of PATP and Thiram Molecules,” Plasmonics 15(6), 1577–1589 (2020).
[Crossref]

R. Gao, X. Song, C. Zhan, C. Weng, S. Cheng, K. Guo, N. Ma, H. Chang, Z. Guo, L. B. Luo, and L. Yu, “Light trapping induced flexible wrinkled nanocone SERS substrate for highly sensitive explosive detection,” Sensors and Actuators B: Chemical 314, 128081 (2020).
[Crossref]

S.S.B. Moram, C. Byram, and V.R. Soma, “Gold-nanoparticle- and nanostar-loaded paper-based SERS substrates for sensing nanogram-level Picric acid with a portable Raman spectrometer,” Bull. Mater. Sci. 43, 8190–8201 (2020).
[Crossref]

V.S. Vendamani, S.V.S.N. Rao, A.P. Pathak, and V.R. Soma, “Robust and cost-effective silver dendritic nanostructures for SERS-based trace detection of RDX and ammonium nitrate,” RSC Adv. 10(73), 44747–44755 (2020).
[Crossref]

S.S.B. Moram, A.K. Shaik, C. Byram, S. Hamad, and V.R. Soma, “Instantaneous trace detection of nitro-explosives and mixtures with nanotextured silicon decorated with Ag-Au alloy nanoparticles using the SERS technique,” Anal. Chim. Acta 1101, 157–168 (2020).
[Crossref]

2019 (7)

R.M. Cardoso, S.V.F. Castro, M.N.T. Silva, A.P. Lima, M.H.P. Santana, E. Nossol, R.A.B. Silva, E.M. Richter, T.R.L.C. Paixao, and R.A.A. Munoz, “3D-printed flexible device combining sampling and detection of explosives,” Sens. Actuators B Chem. 292, 308–313 (2019).
[Crossref]

S. Mourya, A. Kumar, J. Jaiswal, G. Malik, B. Kumar, and R. Chandra, “Development of Pd-Pt functionalized high performance H2 gas sensor based on silicon carbide coated porous silicon for extreme environment applications,” Sens. Actuators B Chem. 283, 373–383 (2019).
[Crossref]

T. Cao, Y. Zhao, C.A. Nattoo, R. Layouni, and S.M. Weiss, “A smartphone biosensor based on analysing structural colour of porous silicon,” Analyst 144(13), 3942–3948 (2019).
[Crossref]

Tania K. Naqvi, Moram Sree Satya Bharati, Alok K. Srivastava, Manish M. Kulkarni, Azher M. Siddiqui, S. Venugopal Rao, and Prabhat K. Dwivedi, “Femtosecond laser textured silver/graphene oxide hybrid SERS substrate for detection of an explosive precursor 2,4-DNT,” ACS Omega 4(18), 17691–17701 (2019).
[Crossref]

C. Byram, S. S. B. Moram, and V. R. Soma, “SERS based multiple analyte detection from explosive mixtures using picosecond laser fabricated gold nanoparticles, nanostructures,” Analyst 144(7), 2327–2336 (2019).
[Crossref]

M.S. Satya Bharati, B. Chandu, and S.V. Rao, “Explosives sensing using Ag–Cu alloy nanoparticles synthesized by femtosecond laser ablation and irradiation,” RSC Adv. 9(3), 1517–1525 (2019).
[Crossref]

S.I. Kudryashov, P.A. Danilov, A.P. Porfirev, I.N. Saraeva, T.H.T. Nguyen, A.A. Rudenko, R.A. Khmelnitskii, D.A. Zayarny, A.A. Ionin, A.A. Kuchmizhak, S.N. Khonina, and O.B. Vitrik, “High-throughput micropatterning of plasmonic surfaces by multiplexed femtosecond laser pulses for advanced IR-sensing applications,” Appl. Surf. Sci. 484, 948–956 (2019).
[Crossref]

2018 (14)

C. Cheng, J. Li, H. Lei, and B. Li, “Surface enhanced Raman scattering of gold nanoparticles aggregated by a gold-nanofilm-coated nanofiber,” Photonics Res. 6, 357 (2018).
[Crossref]

F. Zhong, Z. Wu, J. Guo, and D. Jia, “Porous silicon photonic crystals coated with Ag nanoparticles as efficient substrates for detecting trace explosives using SERS,” Nanomaterials 8(11), 872 (2018).
[Crossref]

D. Wang, F. Wang, and H. Yang, “Robust, flexible, sticky and high sensitive SERS membrane for rapid detection applications,” Sens. Actuators B Chem. 274, 676–681 (2018).
[Crossref]

S.S.B. Moram, C. Byram, S.N. Shibu, B.M. Chilukamarri, and V.R. Soma, “Ag/Au nanoparticle-loaded paper-based versatile surface-enhanced Raman spectroscopy substrates for multiple explosives detection,” ACS Omega 3(7), 8190–8201 (2018).
[Crossref]

C. Li, J. Yu, S. Xu, S. Jiang, X. Xiu, C. Chen, A. Liu, T. Wu, B. Man, and C. Zhang, “Constructing 3D and flexible plasmonic structure for high-performance SERS application,” Adv. Mater. Technol. 3, 1800174 (2018).
[Crossref]

M. Sree Satya Bharati, C. Byram, and V. R. Soma, “Femtosecond laser fabricated Ag@Au and Cu@Au alloy nanoparticles for surface enhanced Raman spectroscopy based trace explosives detection,” Front. Phys. 6, 28 (2018).
[Crossref]

H.V. Bandarenka, K.V. Girel, S.A. Zavatski, A. Panarin, and S.N. Terekhov, “Progress in the development of SERS-active substrates based on metal-coated porous silicon,” Materials 11(5), 852 (2018).
[Crossref]

A.M. Alwan, L.A. Wali, and A.A. Yousif, “Optimization of AgNPs/mesoPS active substrates for ultra–low molecule detection process,” Silicon 10(5), 2241–2251 (2018).
[Crossref]

S.K. Ramakrishan, M. Martin Fernandez, T. Cloitre, V. Agarwal, F.J.G. Cuisinier, and C. Gergely, “Porous silicon microcavities redefine colorimetric ELISA sensitivity for ultrasensitive detection of autoimmune antibodies,” Sens. Actuators B Chem. 272, 211–218 (2018).
[Crossref]

D. Cheng, M. He, J. Ran, G. Cai, J. Wu, and X. Wang, “Depositing a flexible substrate of triangular silver nanoplates onto cotton fabrics for sensitive SERS detection,” Sens. Actuators B Chem. 270, 508–517 (2018).
[Crossref]

V.S. Vendamani, S.V.S. Nageswara Rao, S. Venugopal Rao, D. Kanjilal, and A.P. Pathak, “Three-dimensional hybrid silicon nanostructures for surface enhanced Raman spectroscopy based molecular detection,” J. Appl. Phys. 123(1), 014301 (2018).
[Crossref]

S. Hamad, S.S. Bharati Moram, B. Yendeti, G.K. Podagatlapalli, S.V.S. Nageswara Rao, A.P. Pathak, M. A. Mohiddon, and V. R. Soma, “Femtosecond Laser-Induced, Nanoparticle-Embedded Periodic Surface Structures on Crystalline Silicon for Reproducible and Multi-utility SERS Platforms,” ACS Omega 3(12), 18420–18432 (2018).
[Crossref]

X. Tu, Z. Li, J. Lu, Y. Zhang, G. Yin, W. Wang, and D. He, “In situ preparation of Ag nanoparticles on silicon wafer as highly sensitive SERS substrate,” RSC Adv. 8(6), 2887–2891 (2018).
[Crossref]

N.N. Durmanov, R.R. Guliev, A.V. Eremenko, I.A. Boginskaya, I.A. Ryzhikov, E.A. Trifonova, E.V. Putlyaev, A.N. Mukhin, S.L. Kalnov, M.V. Balandina, A.P. Tkachuk, V.A. Gushchin, A.K. Sarychev, A.N. Lagarkov, I.A. Rodionov, A.R. Gabidullin, and I.N. Kurochkin, “Non-labeled selective virus detection with novel SERS-active porous silver nanofilms fabricated by Electron Beam Physical Vapor Deposition,” Sens. Actuators B Chem. 257, 37–47 (2018).
[Crossref]

2017 (4)

S. Niyomdecha, W. Limbut, A. Numnuam, P. Asawatreratanakul, P. Kanatharana, and P. Thavarungkul, “A novel BOD biosensor based on entrapped activated sludge in a porous chitosan-albumin cryogel incorporated with graphene and methylene blue,” Sens. Actuators B Chem. 241, 473–481 (2017).
[Crossref]

Y. He and T. Leïchlé, “Fabrication of lateral porous silicon membranes for planar microfluidics by means of ion implantation,” Sens. Actuators B Chem. 239, 628–634 (2017).
[Crossref]

S. Kumar, P. Goel, and J.P. Singh, “Flexible and robust SERS active substrates for conformal rapid detection of pesticide residues from fruits,” Sens. Actuators B Chem. 241, 577–583 (2017).
[Crossref]

Y. Fan, Y. Zhang, N. Li, S.G. Liu, T. Liu, N. Li, and H. Luo, “A facile synthesis of water-soluble carbon dots as a label-free fluorescent probe for rapid, selective and sensitive detection of picric acid,” Sens. Actuators B Chem. 240, 949–955 (2017).
[Crossref]

2016 (4)

U.P. Shaik, S. Hamad, M. Ahamad Mohiddon, V.R. Soma, and M. Ghanashyam Krishna, “Morphologically manipulated Ag/ZnO nanostructures as surface enhanced Raman scattering probes for explosives detection,” J. Appl. Phys. 119(9), 093103 (2016).
[Crossref]

C. Wang, B. Liu, and X. Dou, “Silver nanotriangles-loaded filter paper for ultrasensitive SERS detection application benefited by interspacing of sharp edges,” Sens. Actuators B Chem. 231, 357–364 (2016).
[Crossref]

C. Novara, S. Dalla Marta, A. Virga, A. Lamberti, A. Angelini, A. Chiadò, P. Rivolo, F. Geobaldo, V. Sergo, A. Bonifacio, and F. Giorgis, “SERS-Active Ag nanoparticles on porous silicon and PDMS Substrates: A comparative study of uniformity and Raman efficiency,” J. Phys. Chem. C 120(30), 16946–16953 (2016).
[Crossref]

S. Yang, X. Dai, B.B. Stogin, and T.S. Wong, “Ultrasensitive surface-enhanced Raman scattering detection in common fluids,” Proc. Nat. Acad. Sci. 113(2), 268–273 (2016).
[Crossref]

2015 (4)

S. Emamian, A. Eshkeiti, B.B. Narakathu, S.G.R. Avuthu, and M.Z. Atashbar, “Gravure printed flexible surface enhanced Raman spectroscopy (SERS) substrate for detection of 2,4-dinitrotoluene (DNT) vapor,” Sens. Actuators B Chem. 217, 129–135 (2015).
[Crossref]

V.S. Vendamani, S. Hamad, V. Saikiran, A.P. Pathak, S. Venugopal Rao, V.V. Ravi Kanth Kumar, and S.V.S.N. Rao, “Synthesis of ultra-small silicon nanoparticles by femtosecond laser ablation of porous silicon,” J. Mater. Sci. 50(4), 1666–1672 (2015).
[Crossref]

Sara Fateixa, Helena I. S. Nogueira, and Tito Trindade, “Hybrid nanostructures for SERS: materials development and chemical detection,” Phys. Chem. Chem. Phys. 17(33), 21046–21071 (2015).
[Crossref]

Y. Tang, Z. Zhao, H. Hu, Y. Liu, X. Wang, S. Zhou, and J. Qiu, “Highly stretchable and ultrasensitive strain sensor based on reduced graphene oxide microtubes-elastomer composite,” ACS Appl. Mater. & Interf. 7(49), 27432–27439 (2015).
[Crossref]

2014 (3)

S. Hamad, G.K. Podagatlapalli, M.A. Mohiddon, and V.R. Soma, “Cost effective nanostructured copper substrates prepared with ultrafast laser pulses for explosives detection using surface enhanced Raman scattering,” Appl. Phys. Lett. 104(26), 263104 (2014).
[Crossref]

M. Sharma, P.R. Pudasaini, F. Ruiz-Zepeda, D. Elam, and A.A. Ayon, “Ultrathin, flexible organic-inorganic hybrid solar cells based on silicon nanowires and PEDOT:PSS,” ACS Appl. Mater. & Interf. 6(6), 4356–4363 (2014).
[Crossref]

F.A. Harraz, “Porous silicon chemical sensors and biosensors: A review,” Sens. Actuators B Chem. 202, 897–912 (2014).
[Crossref]

2013 (3)

V.S. Vendamani, S.V.S. Nageswara Rao, and A.P. Pathak, “Structural and optical properties of porous silicon prepared by anodic etching of irradiated silicon,” Nucl. Instrum. Meth. Phys. Res. Section B: Beam Inter. Mater. and Atoms 315, 188–191 (2013).
[Crossref]

C. Pang, H. Cui, G. Yang, and C. Wang, “Flexible transparent and free-standing silicon nanowires paper,” Nano Lett. 13(10), 4708–4714 (2013).
[Crossref]

P. Serre, C. Ternon, V. Stambouli, P. Periwal, and T. Baron, “Fabrication of silicon nanowire networks for biological sensing,” Sens. Actuators B Chem. 182, 390–395 (2013).
[Crossref]

2012 (1)

T. Böcking, K.A. Kilian, P.J. Reece, K. Gaus, M. Gal, and J.J. Gooding, “Biofunctionalization of free-standing porous silicon films for self-assembly of photonic devices,” Soft Matter 8(2), 360–366 (2012).
[Crossref]

2011 (2)

M. Fan, G.F. Andrade, and A.G. Brolo, “A review on the fabrication of substrates for surface enhanced Raman spectroscopy and their applications in analytical chemistry,” Anal. Chim. Acta 693(1-2), 7–25 (2011).
[Crossref]

A. Shrivastava and V.B. Gupta, “Methods for the determination of limit of detection and limit of quantitation of the analytical methods,” Chron Young Sci 2, 21–25 (2011).
[Crossref]

2008 (3)

X.M. Qian and S.M. Nie, “Single-molecule and single-nanoparticle SERS: from fundamental mechanisms to biomedical applications,” Chem. Soc. Rev. 37(5), 912–920 (2008).
[Crossref]

D.-Y. Xu, X.-M. Liu, S. Duan, X. Xu, B. Ren, S.-H. Lin, and Z.-Q. Tian, “Chemical enhancement effects in SERS Spectra: A quantum chemical study of pyridine interacting with Copper, Silver, Gold and Platinum metals,” J. Phys. Chem. C 112(11), 4195–4204 (2008).
[Crossref]

F. Giorgis, E. Descrovi, A. Chiodoni, E. Froner, M. Scarpa, A. Venturello, and F. Geobaldo, “Porous silicon as efficient surface enhanced Raman scattering (SERS) substrate,” Appl. Surf. Sci. 254(22), 7494–7497 (2008).
[Crossref]

2007 (1)

O. Garel, C. Breluzeau, E. Dufour-Gergam, A. Bosseboeuf, B. Belier, V. Mathet, and F Verjus, “Fabrication of free-standing porous silicon microstructures,” J. Micromech. Microeng. 17(7), S164–S167 (2007).
[Crossref]

2000 (1)

P.R. G. Lammel, “Free-standing, mobile 3D porous silicon microstructures,” Sensors and Actuators A: Phys. 85(1-3), 356–360 (2000).
[Crossref]

1998 (1)

G. Oskam, J.G. Long, A. Natarajan, and P. C. Searson, “Electrochemical deposition of metals onto silicon,” J Phys. D: Appl. Phys. 31(16), 1927–1949 (1998).
[Crossref]

1997 (2)

M.T. S. Billat, R. Arens-Fischer, M.G. Berger, M. Kruger, and H. Luth, “Influence of etch stops on the microstructure of porous silicon layers,” Thin Solid Films 297(1-2), 22–25 (1997).
[Crossref]

A.G. Cullis, L.T. Canham, and P.D.J. Calcott, “The structural and luminescence properties of porous silicon,” J. Appl. Phys. 82(3), 909–965 (1997).
[Crossref]

1990 (1)

L.T. Canham, “Silicon quantum wire array fabrication by electrochemical and chemical dissolution of wafers,” Appl. Phys. Lett. 57(10), 1046–1048 (1990).
[Crossref]

1989 (1)

X.G. Zhang, S.D. Collins, and R.L. Smith, “Porous silicon formation and electropolishing of silicon by anodic polarization in HF solution,” J. Electrochem. Soc. 136, 1561–1565 (1989).
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1980 (1)

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M.S. Satya Bharati, B. Chandu, and S.V. Rao, “Explosives sensing using Ag–Cu alloy nanoparticles synthesized by femtosecond laser ablation and irradiation,” RSC Adv. 9(3), 1517–1525 (2019).
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V.S. Vendamani, S.V.S.N. Rao, A.P. Pathak, and V.R. Soma, “Robust and cost-effective silver dendritic nanostructures for SERS-based trace detection of RDX and ammonium nitrate,” RSC Adv. 10(73), 44747–44755 (2020).
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M.S. Satya Bharati, B. Chandu, and S.V. Rao, “Explosives sensing using Ag–Cu alloy nanoparticles synthesized by femtosecond laser ablation and irradiation,” RSC Adv. 9(3), 1517–1525 (2019).
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Data availability

Data underlying the results presented in this paper are not publicly available at this time but may be obtained from the authors upon reasonable request.

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Figures (12)

Fig. 1.
Fig. 1. Processing steps for the fabrication of AgNPs@FS-pSi layer by anodic-etching followed by electro-polishing.
Fig. 2.
Fig. 2. Photographs of FS-pSi (a) floating on water (b) freely held by a tweezer, and (c) mounted on a flexible scotch tape.
Fig. 3.
Fig. 3. (a) The morphology of as-anodized FS-pSi layer and (b) the histogram of the pore size distribution (solid line indicates the Gaussian fit).
Fig. 4.
Fig. 4. AgNPs decoration of FS-pSi at various deposition times (a) 30 min, (b) 60 min, (c) 4 hours, and (d) EDS spectrum of AgNPs@FSpSi-60min sample. [Inset of the figure (d) illustrates the distribution of AgNPs over the sample surface of FSpSi-60min [shown in (b)] and the solid line is a Gaussian fit].
Fig. 5.
Fig. 5. The SERS spectra of MB molecules on AgNPs@FS-60min substrate at a concentration of (a)-(i) 100 µM (ii) 50 µM (iii) 10 µM (iv) 5 µM (v) 1 µM and (vi) 100 nM concentration (b) SERS spectra of MB (5 µM) at various AgNPs deposition time on FS-pSi. Spectra in (a) and (b) are stacked in Y-axis to avoid ambiguity in the data.
Fig. 6.
Fig. 6. (a) Linear dependence of log (SERS intensity) versus log (analyte concentration) for the principal modes of MB molecules, (b) The stability estimation of AgNPs@FSpSi-60min substrate with 50 µM concentration of MB over a period of 90 days.
Fig. 7.
Fig. 7. (a) Reproducibility of the SERS spectra of 10 µM MB molecules detected at 10 different spots on AgNPs@FSpSi-60min, and (b) the corresponding standard analysis with RSD values.
Fig. 8.
Fig. 8. The SERS spectra of PA, an explosive molecule, on AgNPs@FSpSi-60min substrate at concentration of (a)-(i) 100 µM, (ii) 50 µM, (iii) 30 µM, (iv) 10 µM, and (v) 5 µM concentrations, (b) SERS spectra of PA (30 µM) at various AgNPs deposition time on FS-pSi, and (c) corresponding linear calibration [log (SERS intensity) versus log (concentration)] of the different Raman modes observed at 832 cm-1, 1177 cm-1, and 1346 cm-1.
Fig. 9.
Fig. 9. (a) Reproducibility of the SERS spectra of 50 µM PA molecules detected at 10 different spots on AgNDs@FSpSi-60min, and (b) the corresponding histogram with RSD values.
Fig. 10.
Fig. 10. The SERS spectra of AN molecule on AgNPs@FSpSi-60min substrate at (a)-(i) 100 µM, (ii) 50 µM, (iii) 10 µM, (iv) 5 µM, and (v) 1 µM concentrations, (b) The SERS spectra of AN (50 µM) at various AgNPs deposition time on FS-pSi, and (c) corresponding linear calibration [log (SERS intensity) versus log (concentration)] of the Raman modes at 711 cm-1, and 1042 cm-1 (d) Reproducibility of AN (50 µM) on AgNDs@FSpSi-60min substrate and inset shows the corresponding standard deviation.
Fig. 11.
Fig. 11. The SERS spectra of thiram (pesticide) on AgNPs@FSpSi-60min at (a) (i) 10 µM (ii) 5 µM (iii) 1 µM and (iv) 100 nM concentrations (b) SERS spectra of thiram (10 µM) at various AgNPs deposition time on FSpSi and (c) corresponding linear relationship of log (SERS intensity) versus log (concentration).
Fig. 12.
Fig. 12. The SERS intensity versus analyte concentration for (a) MB - 1626 cm-1 (b) PA - 1346 cm-1 (c) AN - 1042 cm-1 (d) thiram-1385 cm-1, and (e)-(h) Linear dependence of the log SERS intensities verses lower molecular concentrations.

Tables (3)

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Table 1. The estimated physical parameters of FS-pSi fabricated by anodic etching.

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Table 2. Detailed comparison and assessment of the estimated AEF for various analyte molecules and concentrations considered in the present study.

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Table 3. Summary of detection capability of various SERS substrates (typically metal nanoparticles comprising flexible and/or pSi substrate).

Equations (3)

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P = ( m 1 m 2 ) ( m 1 m 3 )
W = ( m 1 m 3 ) S × d
A E F = I S E R S I R S × N R S η N S E R S

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