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

To improve the photoresponsivity of hematite-based photoanode via better charge transfer rate and short paths for the electron transport, carbon quantum dots (CQDs) were used as conductive nano-scaffolds for the growth of photoactive material on Ti substrate. CQDs@α-Fe2O3 nanoparticulates with the average diameter of 3–5 nm were uniformly grown on the substrate under the finely optimized experimental conditions to prepare Ti/CQDs@α-Fe2O3 photoanode. The photocurrent response of the resulted photoanode with a photocurrent density of 2.1 mA cm−2 at applied Ebias of +0.5 V vs. Ag/AgCl was increased by a factor of 10 compared to Ti/α-Fe2O3, mainly due to the improvement in charge-transfer rate and suppression of electron-hole recombination derived from the increased hole-diffusion length in conducting nano-scaffold structure. The surface morphology of samples was investigated with FE-SEM and HRTEM. Charge transfer resistance (Rct) of Ti/α-Fe2O3 and Ti/CQDs@α-Fe2O3 photoanodes were estimated to be about 90.9 and 3.7 KΩ, respectively. After the continuous 4 h illumination of Ti/CQDs@α-Fe2O3 photoanode under the visible light irradiation, the efficiency of water splitting process (i.e. the photocurrent) did not changed significantly (±5%), indicating the high stability of photoanode and tightly deposited CQDs@α-Fe2O3 on Ti substrate, which was confirmed by FE-SEM image of the sample after the experiment. The formation of carbon-oxygen chemical bonds between CQDs and hematite molecules was confirmed by X-ray photoelectron spectroscopy (XPS). Finally, based on XRD pattern and photoresponses of various photoanodes annealed at different temperatures, the results showed that the structure design is as significant as crystallinity in hematite-based photoelectrodes.

Carbon quantum dots as nano-scaffolds for α-Fe2O3 growth: Preparation of Ti/CQD@α-Fe2O3 photoanode for water splitting under visible light irradiation

In situ x-ray spectroscopies offer a powerful way to understand the electronic structure of the electrode–electrolyte interface under operating conditions. However, most x-ray techniques require vacuum, making it necessary to design spectro-electrochemical cells with a delicate interface to the wet electrochemical environment. The design of the cell often dictates what measurements can be done and which electrochemical processes can be studied. Hence, it is important to pick the right spectro-electrochemical cell for the process of interest. To facilitate this choice, and to highlight the challenges in cell design, we critically review four recent, successful cell designs. Using several case studies, we investigate the opportunities and limitations that arise in practical experiments.

A comparative study of electrochemical cells for in situ X-ray spectroscopies in the soft and tender X-ray range

Ferrofluids investigated along for about five decades are ultrastable colloidal suspensions of magnetic nanoparticles, which manifest simultaneously fluid and magnetic properties. Their magnetically controllable and tunable feature proved to be from the beginning an extremely fertile ground for a wide range of engineering applications. More recently, biocompatible ferrofluids attracted huge interest and produced a considerable increase of the applicative potential in nanomedicine, biotechnology and environmental protection. This paper offers a brief overview of the most relevant early results and a comprehensive description of recent achievements in ferrofluid synthesis, advanced characterization, as well as the governing equations of ferrohydrodynamics, the most important interfacial phenomena and the flow properties. Finally, it provides an overview of recent advances in tunable and adaptive multifunctional materials derived from ferrofluids and a detailed presentation of the recent progress of applications in the field of sensors and actuators, ferrofluid-driven assembly and manipulation, droplet technology, including droplet generation and control, mechanical actuation, liquid computing and robotics.

Ferrofluids and bio-ferrofluids: looking back and stepping forward.

Effects of low temperature annealing on the photo-electrochemical performance of tin-doped hematite photo-anodes

The reaction of iron chlorides with an alkaline reagent is one of the most prominent methods for the synthesis of iron oxide nanoparticles. We studied the particle formation mechanism using triethanolamine as reactant and stabilizing agent. In situ fast-X-ray absorption near edge spectroscopy and small-angle X-ray scattering provide information on the oxidation state and the structural information at the same time. In situ data were complemented by ex situ transmission electron microscopy, wide-angle X-ray scattering and Raman analysis of the formed nanoparticles. The formation of maghemite nanoparticles (γ-Fe2O3) from ferric and ferrous chloride was investigated. Prior to the formation of these nanoparticles, the formation and conversion of intermediate phases (akaganeite, iron(II, III) hydroxides) was observed which undergoes a morphological and structural collapse. The thus formed small magnetite nanoparticles (Fe3O4) grow further and convert to maghemite with increasing reaction time.

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Time-resolved in situ studies on the formation mechanism of iron oxide nanoparticles using combined fast-XANES and SAXS

Iron can form numerous oxides, hydroxides, and oxide−hydroxides. Despite their relevance, many of the transformation processes between these phases are still poorly understood. In particular the crystallization of quasi-amorphous hydroxides and oxide−hydroxides is difficult to assess, since typical diffraction and scattering methods provide only sample-averaged information about the crystallized phases. We report a new approach for the investigation of the crystallization of oxide−hydroxides. The approach relies on model-type films that comprise a defined homogeneous nanostructure. The nanostructure allows quantitative linking of information obtained by bulk-averaging diffraction techniques (XRD, SAXS) with locally resolved information, i.e., domain sizes (SEM, TEM, LEEM) and phase composition (SAED). Using time-resolved imaging and diffraction we deduce mechanism and kinetics for the crystallization of ferrihydrite into hematite. Hematite forms via nucleation of hematite domains and subsequent domain gro...

Katrin Schulz

Papers

Time-resolved in situ studies on the formation mechanism of iron oxide nanoparticles using combined fast-XANES and SAXS

Mechanism and Kinetics of Hematite Crystallization in Air: Linking Bulk and Surface Models via Mesoporous Films with Defined Nanostructure