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SERS: an Update of Progress Made Electronically reprinted from November 2015 ® Molecular Spectroscopy Workbench SERS: An Update of Progress Made This column is a mini survey of progress that has been made in the area of surface enhancement over the last few years since my previous column on surface-enhanced Raman scattering (SERS) in 2008. The potential of SERS to provide signals of analytes at very low concentrations continues to beckon the analytical chemist. What the last few years has produced is a body of work describing the role of the plasmonic properties of metals, based on their geometrical and electronic properties, in enhancing the signals. As this field matures, we foresee production of surface-enhancing films and particles, engineered to provide large enhancements at selected wavelengths that will provide repro- ducible Raman signals for applications in areas such as environmental and biomedical studies. Fran Adar y earlier article on surface-enhanced Raman scat- ously compare the sensitivity and reproducibility of various tering (SERS) (1) did not include much discus- SERS substrates.” But it is necessary to recognize that SERS Msion of particular applications except to mention measurement detects a two-dimensional (2D) area while a improved sensitivity for bioclinical studies. Here, I provide comparable bulk measurement detects molecules in a three- a conceptual introduction to plasmonics to support the con- dimensional volume. Furthermore, it is difficult to calculate tention that, in the not-too-distant future, SERS will enable the number of adsorbed molecules on the SERS surface and measurements at low concentrations. in the detected volume of a normal Raman measurement; therefore, the assessment proposed in this article (2) is an Background Motivation empirical protocol. The SERS enhancement value (SEV) was Aside from its potential to enhance analytical sensing defined as the ratio of the concentrations that produced, on measurements in manufacturing, biomedicine, and envi- a particular instrument, the same instrument responses for ronmental testing, the United States military has shown normal Raman scattering versus SERS scattering. In this a keen interest in surface enhancement for detection and case, the metric selected was the ratio of the area of a peak identification of biological and chemical warfare agents. in the spectrum of BPE (trans-1,2-bis(4-pyridyl)-ethylene) to Because of reproducibility issues, workers at two of the US the ethanol in which the BPE was dissolved. This protocol Army’s laboratories have published a paper titled “Surface- provides a means to determine, for a particular type of SERS Enhanced Raman Scattering (SERS) Evaluation Protocol substrate, on a given instrument using standardized acquisi- for Nanometallic Surfaces” (2) to provide to the community tion conditions, the minimum detectable concentration of “analytical and spectroscopic figures of merit to unambigu- an analyte and to determine SERS reproducibility, from spot to spot on a given substrate, from sub- frequency of the metal structure.” If a molecule resides in the gap, it will strate to substrate, and over time. And In 1997, Emory and Nie (8) reported experience a very large electric field. it also provides a qualitative means of super-enhancement from single silver This large field in turn induces an comparing different substrate types. colloidal nanoparticles in a heteroge- enhanced polarizability and then an Because the military is interested not neous population, with enhancement enhanced Raman signal. Moskovits only in the detection of warfare agents, factors of the order of 1014 to 1015. summarizes that the electromagnetic but also the identification of false Certainly this publication went far in theory accounts for all SERS observa- positives and false negatives, it uses the explaining the large discrepancies that tions—the nanostructure requirement, receiver operating characteristic (ROC) had been noticed from laboratory to the behavior of the various metals curves for analysis of when, and how laboratory. The group of Louis Brus (in terms of their enhancement capa- (warning versus evacuation) to react continued this type of work—associat- bilities), the increased enhancement (3). ing SERS “hot spots” with particles of from interacting metal nanoparticles, Clearly, if the Defense Advanced particular size, shape, and aggregation and the polarization sensitivity. He Research Projects Agency (DARPA) (9). By measuring Rayleigh and Mie also mentions other electromagnetic is investing so much effort into this scattering in addition to absorption mechanisms, in particular the light- technology, it is believed that the pay- and SERS they proposed modified ening rod effect for ellipsoids and off in terms of military capabilities enhancing mechanisms including the nanorods with sharp curvature. And and homeland security will be high. chemical mechanism of Otto (10) and he discusses single-molecule SERS. Because of this, DARPA put out a re- a mechanism involving the interaction Single-molecule Raman scattering was quest for proposals to fund research of ballistic electrons with chemisorbed more thoroughly reviewed in 2006 in that would determine, in a rigorous molecules. Note that single-molecule Applied Spectroscopy (13). An interest- fashion, what is the origin of SERS so SERS had been predicted a year earlier ing methodology was described in this that it could be relied on as an analyti- by Kneipp, and colleagues (11). 2006 article where solution concentra- cal technique. The article cited above Moskovits published a second tions of metallic clusters and target (2) describes the methods developed to review (12) 20 years after the first analyte were chosen to approximate 0 evaluate and compare SERS substrates in which he states “. that all of the to several molecule–metal clusters in a prepared by different laboratories, and major features of SERS . are es- focal volume of the order of picoliters to compare the heterogeneity of the sentially incomprehensible without to femtoliters when using a Raman substrates of a given type. invoking the electromagnetic theory,” microscope as the sampling tool. The but the controversy regarding the integrated signal for a particular ana- Evolution of SERS Research possibility of a strong chemical effect lyte line was plotted as a function of The initial report on strongly enhanc- persists “because of the simplicity of time, and represented the amount of ing Raman signals was published in its (SERS) experimental actualization, detected analyte in the focal volume, 1974 (4). However, if one tried to fol- (which) is primarily a chemical (and which fluctuated because of Brown- low the field during the first 20 years lately a biochemical) tool whereas its ian motion. (A far red excitation, 830 or so, you would see that the signals origin requires a rather deep knowl- nm, was used to couple the laser to the were highly variable from laboratory edge of condensed matter physics aggregated plasmon absorption, but to laboratory, and a vigorous debate and especially the optical response of its intensity was kept to a minimum arose as to whether the origin of the materials, which includes a number of to avoid “laser trapping.”) A histo- enhancement was chemical or physical. physical subtleties.” gram plot of the signal (frequency of Fleischman and colleagues (4) believed In his 1985 review, Moskovits de- events detected at given signal levels) that the large enhancement arose from scribed more than seven different indicated “quantized” detected levels; increased surface area produced by preparation techniques from which he the histogram was fitted to Poisson the substrate preparation, but by 1977 already inferred that the best enhance- statistics that indicated the presence Jeanmaire and van Duyne (5) and Al- ments occurred in the presence of of 0, 1, 2, and 3 molecules per detected brecht and Creighton (6) showed that coupled, microscopic metal domains event, with the total probability drop- the increased surface area could not ac- (7). His 2005 article includes a clear ex- ping with the number of molecules per count for all the enhancement. Already planation of why particle dimers pro- event. At the end of this article, Kneipp in a review published in 1985, Mos- duce such strong enhancement (12); his and colleagues indicated the potential kovits (7) reported that “the majority Figure 1 (which is derived from simple importance of the single-molecule view is that the largest contributor to principles of electromagnetism that are SERS capability in detecting and dif- the intensity amplification results from shown here in my Figure 1) illustrates ferentiating chemicals such as DNA the electric field enhancement that oc- how an electric field (for example, fragments or even single bases. Then curs in the vicinity of small, interacting from the photon) polarized along the in 2011, Volker Deckert’s group dem- metal particles that are illuminated interparticle axis induces a polariza- onstrated that a tip-enhanced Raman with light resonant or near resonant tion along that direction that scales to spectroscopy (TERS) system has the with the localized surface-plasmon the -8th power of the gap dimension. capabilities to detect and differentiate mersed in the field, will be based on the review article by Halas and colleagues that appeared in 2011 (16) and includes more than 500 references to the field up until that time. My goal here is to provide a sparse introduction to a complex field that now Ephoton really does show promise for producing reliable, reproducible, inexpensive SERS substrates. The interested reader is urged to access the literature. As stated above, in his 1985 review Moskovits argued that electromagnetic theory can account for the SERS phenom- enon. In his 2005 review he added that the SERS enhancement is increased dramatically when two SERS active particles are close together, the molecule of interest is in the space between the two particles, and the electric field is parallel to the two- particle axis. The plasmonics that have been developed over the last 10 or more years are based on this elemental SERS d system. Figure 1 is a description of the SERS dimer from which plasmonics have evolved.
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