Microstructural characterisation techniques

Shearing, P. R., Brett, D. J. L. Brandon, N. P. Towards intelligent engineering of SOFC electrodes a review of advanced microstructural characterisation techniques. International Materials Reviews 55, 347-363, doi 10.1179/095066010xl2777205875679 (2010). 

Microstructural characterisation techniques for the study of reactor pressure vessel... 

Most of microstructural characterisation techniques for cementitious materials belong to the discipline of materials science and are not well studied by civil engineers, who make up the majority of researchers on cementitious materials. At the same time most machine operators in materials science departments are not familiar with the foibles of cementitious materials. All too often this leads to poor-quality results. In this book we aim to provide practical information not usually discussed in scientific articles to help researchers obtain the best results from microstructural characterisation methods. We aim to highlight common pitfalls and give guidance on the best use of the different techniques and interpretation of the results. 

Chemical characterisation of F uptake in archaeological bone has already been developed in the 19th century [1,2] and is now well established [60], However, relatively few studies use a combined multianalytical approach using trace elemental and microstructure analytical techniques (PIXE/PIGE, TEM-EDX) for evidencing modifications on different microscopic and nanoscopic levels (Fourier transform-infrared spectroscopy (FT-IR), X-ray diffraction (XRD), SEM, TEM) and enabling an objective evaluation of the F uptake mechanisms [32-34,51],... 

It is possible to carry out particle shape analysis and topological characterisation of granular textures in microstructures. The technique was used to study unreacted cement (Holzer et al. 2006) impregnated with Wood s metal (Bi 50%, Pb 25%, Sn 12.5%, Cd 12.5% melting point 70°C) in order to prevent charge effects. Polishing was as standard for preparing... 

Table 2.7 lists techniques used to characterise carbon-blacks. Analysis of CB in rubber vulcanisates requires recovery of CB by digestion of the matrix followed by filtration, or by nonoxidative pyrolysis. Dispersion of CB within rubber products is usually assessed by the Cabot dispersion test, or by means of TEM. Kruse [46] has reviewed rubber microscopy, including the determination of the microstructure of CB in rubber compounds and vulcanisates and their qualitative and quantitative determination. Analysis of free CB features measurements of (i) particulate and aggregate size (SEM, TEM, XRD, AFM, STM) (ii) total surface area according to the BET method (ISO 4652), iodine adsorption (ISO 1304) or cetyltrimethylammonium bromide (CTAB) adsorption (ASTM D 3765) and (iii) external surface area, according to the dibutylphthalate (DBP) test (ASTM D 2414). TGA is an excellent technique for the quantification of CB in rubbers. However, it is very limited in being able to distinguish the different types of... 

Micro structures in heterogeneous catalysts are closely related to the catalytic properties. TEM and related microanalytic techniques are powerful tools in characterising catalysts at atomic level. The obtained structural information is essential to the understanding of correlations between microstructures and catalytic properties. In this lecture note, the general principle of characterization of catalysts by TEM is introduced and the applications on Pt/Si02 model system and on VPO catalysts are intensively described. 

Rowe RC, McMahon J. The characterisation of the microstructure of gels and emulsions containing cetostearyl alcohol and cetrimide using electron microscopy—a comparison of techniques. Colloid Surf 1987 27 367-373. 

Scattering techniques are non intrusive, non-destructive and have particular advantages in the characterisation of the surface and porous properties of materials containing either closed or molecular sized pores and where outgass-ing pre-treatment may result in irreversible changes in microstructure. Measurements may be carried out, indeed, in the presence of a gas or with hydrated materials and there is no need to evacuate the sample. 

Throughout the book numerous references are made to the available range of general purpose NMR spectroscopy texts. The reader should turn to these for a full introduction to solution and solid-state techniques and their application to chemical science. Alternatively, texts are available which treat NMR as one of the range of spectroscopies of relevance to polymer characterisation. The reader will also be made aware of some excellent works on specific aspects of polymer NMR, including microstructural determination and high-resolution solid-state methods. In a number of cases these would form a... 

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