Nanostructures have attracted huge interest as a rapidly growing class of materials for many applications. Several techniques have been used to characterize the size, crystal structure, elemental composition and a variety of other physical properties of nanoparticles. In several cases, there are physical properties that can be evaluated by more than one technique. Different strengths and limitations of each technique complicate the choice of the most suitable method, while often a combinatorial characterization approach is needed. In addition, given that the significance of nanoparticles in basic research and applications is constantly increasing, it is necessary that researchers from separate fields overcome the challenges in the reproducible and reliable characterization of nanomaterials, after their synthesis and further process (e.g. annealing) stages. The principal objective of this review is to summarize the present knowledge on the use, advances, advantages and weaknesses of a large number of experimental techniques that are available for the characterization of nanoparticles. Different characterization techniques are classified according to the concept/group of the technique used, the information they can provide, or the materials that they are destined for. We describe the main characteristics of the techniques and their operation principles and we give various examples of their use, presenting them in a comparative mode, when possible, in relation to the property studied in each case.

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Characterization techniques for nanoparticles: comparison and complementarity upon studying nanoparticle properties

The important role that surface chemical analysis methods can and should play in the characterization of nanoparticles is described. The types of information that can be obtained from analysis of nanoparticles using Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary-ion mass spectrometry (TOF-SIMS), low-energy ion scattering (LEIS), and scanning-probe microscopy (SPM), including scanning tunneling microscopy (STM) and atomic force microscopy (AFM), are briefly summarized. Examples describing the characterization of engineered nanoparticles are provided. Specific analysis considerations and issues associated with using surface-analysis methods for the characterization of nanoparticles are discussed and summarized, with the impact that shape instability, environmentally induced changes, deliberate and accidental coating, etc., have on nanoparticle properties.

Application of Surface Chemical Analysis Tools for Characterization of Nanoparticles

XPS analysis of nanostructured materials and biological surfaces

In the past, palladium as a member of the platinum group metals was mainly known as an expensive noble metal. Probably, only fast hydrogen absorption into bulk palladium reminded of its unique catalytic activity. At the beginning of the twenty-first century, detailed studies of the electron structure of palladium atom/nanocluster/nanoparticles launched a new understanding of the selective catalytic activity of this noble metal. This review presents the simplest and most useful methods of synthesizing palladium in a nano scale. In addition, the most famous and required applications of nano-palladium are described in the second half of the review. With the rapid development of nanotechnologies, palladium nanoparticles are becoming prospective selective catalysts for complex chemical reactions.

Chemical synthesis and application of palladium nanoparticles

An extensive comparative study of the effects of microwave versus conventional heating on the nucleation and growth of near-monodisperse Rh, Pd, and Pt nanoparticles has revealed distinct and preferential effects of the microwave heating method. A one-pot synthetic method has been investigated, which combines nucleation and growth in a single reaction via precise control over the precursor addition rate. Using this method, microwave-assisted heating enables the convenient preparation of polymer-capped nanoparticles with improved monodispersity, morphological control, and higher crystallinity, compared with samples heated conventionally under otherwise identical conditions. Extensive studies of Rh nanoparticle formation reveal fundamental differences during the nucleation phase that is directly dependent on the heating method; microwave irradiation was found to provide more uniform seeds for the subsequent growth of larger nanostructures of desired size and surface structure. Nanoparticle growth kinetics a...

Beneficial effects of microwave-assisted heating versus conventional heating in noble metal nanoparticle synthesis.

Synthesis and characterization of Rh(PVP) nanoparticles studied by XPS and NEXAFS

Characterization of Pd(PVP) nanoparticles studied by AFM, Pd L3-edge and Cl K-edge NEXAFS (Proceedings of PSA-07 (International Symposium on Practical Surface Analysis) November 25-28, 2007, Kanazawa, Japan)

We have investigated the reaction of L-cysteine in Rh(PVP) nanoparticle colloidal solution using S-K and Cl-K edges near edge X-ray absorption fine structure and circular dichroism measurements In our previous study, it was shown using S-K edge NEXAFS technique that cystine molecules were synthesized by dissolving L-cysteine into the Rh(PVP) nanocolloidal solution In this study, we have revealed the details of cystine synthesis reaction There are four reactions, which are the adsorption of L-cysteine on Rh nanoparticle surface, the L-cysteine decomposition to cysteine thiolate, the formation of the complex structure similar to (NH4)3[RhCl6] and the synthesis of cystine molecule on Rh nanoparticle surface These reactions start immediately after dissolving L-cysteine into the nanocolloidal solution [DOI: 101380/ejssnt2009314]

Spectroscopic Study on the Reaction of L-Cysteine in Rh(PVP) Nanoparticle Colloidal Solution

Reaction of L-cysteine on Rh(PVP) nanoparticle surface in the aqueous environment studied by NEXAFS (Proceedings of PSA-07 (International Symposium on Practical Surface Analysis) November 25-28, 2007, Kanazawa, Japan)

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Synthesis and characterization of Rh(PVP) nanoparticles studied by XPS and NEXAFS

Characterization of Pd(PVP) nanoparticles studied by AFM, Pd L3-edge and Cl K-edge NEXAFS (Proceedings of PSA-07 (International Symposium on Practical Surface Analysis) November 25-28, 2007, Kanazawa, Japan)

Spectroscopic Study on the Reaction of L-Cysteine in Rh(PVP) Nanoparticle Colloidal Solution

Reaction of L-cysteine on Rh(PVP) nanoparticle surface in the aqueous environment studied by NEXAFS (Proceedings of PSA-07 (International Symposium on Practical Surface Analysis) November 25-28, 2007, Kanazawa, Japan)