This review examines characterization challenges inherently associated with understanding nanomaterials and the roles surface and interface characterization methods can play in meeting some of the challenges. In parts of the research community, there is growing recognition that studies and published reports on the properties and behaviors of nanomaterials often have reported inadequate or incomplete characterization. As a consequence, the true value of the data in these reports is, at best, uncertain. With the increasing importance of nanomaterials in fundamental research and technological applications, it is desirable that researchers from the wide variety of disciplines involved recognize the nature of these often unexpected challenges associated with reproducible synthesis and characterization of nanomaterials, including the difficulties of maintaining desired materials properties during handling and processing due to their dynamic nature. It is equally valuable for researchers to understand how characterization approaches (surface and otherwise) can help to minimize synthesis surprises and to determine how (and how quickly) materials and properties change in different environments. Appropriate application of traditional surface sensitive analysis methods (including x-ray photoelectron and Auger electron spectroscopies, scanning probe microscopy, and secondary ion mass spectroscopy) can provide information that helps address several of the analysis needs. In many circumstances, extensions of traditional data analysis can provide considerably more information than normally obtained from the data collected. Less common or evolving methods with surface selectivity (e.g., some variations of nuclear magnetic resonance, sum frequency generation, and low and medium energy ion scattering) can provide information about surfaces or interfaces in working environments ( or ) or information not provided by more traditional methods. Although these methods may require instrumentation or expertise not generally available, they can be particularly useful in addressing specific questions, and examples of their use in nanomaterial research are presented.
Increasingly, it is recognized that understanding and predicting nanoparticle behavior is often limited by the degree to which the particles can be reliably produced and adequately characterized. Two examples that demonstrate how sample preparation methods and processing history may significantly impact particle behavior are: 1) an examination of cerium oxide (ceria) particles reported in the literature in relation to the biological responses observed and 2) observations related that influence synthesis and aging of ceria nanoparticles. Examining data from the literature for ceria nanoparticles suggests that thermal history is one factor that has a strong influence on biological impact. Thermal processing may alter many physicochemical properties of the particles, including density, crystal structure, and the presence of surface contamination. However, these properties may not be sufficiently recorded or reported to determine the ultimate source of an observed impact. A second example shows the types of difficulties that can be encountered in efforts to apply a well-studied synthesis route to producing well-defined particles for biological studies. These examples and others further highlight the importance of characterizing particles thoroughly and recording details of particle processing and history that too often are underreported.
Cerium oxide nanoparticles (nanoceria) have gained considerable attention in biological research due to their anti-oxidant like behaviour and regenerative nature.
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