Surface and Interface Analysis Methods

Analysis methods, used for the investigation of modified surfaces and interfaces, are briefiy reviewed. Emphasis is on the combination of chemical, structural/ morphological, electronic, and optical characterization. Many techniques such as transmission electron microscopy (TEM), standard X-ray photoelectron spectroscopy (XPS) using A1 or Mg K radiation, high-resolution scanning electron microscopy (HRSEM), and standard scanning probe microscopies (AEM in contact 

Accordingly, methods are presented below that are either less well known or that are of specific use for the characterization of electrochemically and photo-electrochemicahy condihoned surfaces and interfaces. 

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J. F. Watts, in Handbook of Surface and Interface Analysis Methods for Problem Solving (Eds J.C. Riviere, S. Myhra), Marcel Dekker Inc., 1998, pp. 781-833. 

I J.F. Watts, M.-L. Abel, in State-of-the-Art Application of Surface and Interface Analysis Methods to Environmental Materials Interactions (Eds. D. R. Baer, C.R. Clayton, G.D. Davis, G.P. Halada), The Electro-... 

Riviere JC, Myhra S eds.. Handbook of Surface and Interface Analysis Methods of Problem Solving, Marcel Dekker, New York, 1998. 

Watts JF (1988) Surf Interf Anal 12 497 Watts JF (2009) Adhesion science and technology. In Riviere JC, Myhra S (eds) Handbook of surface and interface analysis methods for problem solving. CRC Press, Boca Raton, pp 5651-5656 Watts JF (2010) Role of corrosion in the failure of adhesive joints. In Richardson JA et al (eds) Shreir s corrosion, vol 3. Elsevier, Amsterdam, pp 2463-2481 Watts JF, Wolstenholme J (2003) An introduction to surface analysis by electron spectroscopy. Wiley, Chichester... 

An introduction to several of the more common methods of surface and interface analysis has been presented in this article. This treatment is certainly not comprehensive. An ever-expanding number of methods for the interrogation of surfaces and interfaces are available to the analyst. The ones chosen for discussion here were meant to be representative of methods that can answer the more general questions posed at the beginning of this article. The reader is encouraged to pursue further reading on other techniques for specific appHcations in the many excellent monographs on the subject of surface and interface analysis. 

Radiographic. Radiography is an exceUent nondestmctive test (NDT) method for evaluating the bond of Al—steel electrical and Al—Al—steel stmctural transition joints. It provides the capabiHty of precisely and accurately defining all nonbond and flat-bond areas of the Al—steel interface, regardless of size or location (see Surface and interface analysis). 

Ref [i] Holze R (2008) Surface and interface analysis an electrochemists toolbox. Springer, Berlin [ii] Neudeck A, Marken F, Compton RG (2005) UV/Vis/NIR spectroelectrochemistry. In Electroanalytical Methods. Scholz F (ed), Springer, Berlin, pp 167... 

F.A. Debruijn, G.B. Marin, J.W. Niemantsverdriet, W. Visscher, J.A.R. Vanveen, Characterization of graphite-supported platinum catalysts by electrochemical methods and XPS. Surface and Interface Analysis 1992, 19(1-12), 537-542. 

Forthcoming books in the Techniques in Analytical Chemistry Series will cover a variety of techniques including chemometric methods, biosensors, surface and interface analysis, measurements in biological systems, inductively coupled plasma-mass spectrometry, gas chromatography-mass spectrometry, Fourier transform infrared spectroscopy, and other significant topics. The editors welcome your comments and suggestions regarding current and future titles, and hope you find the series useful. 

Van der Veen JF (1985) Surface Science Reports 5 199 Verelas and Biersack JP (1970) Nucl. Instrum. Methods 79 213 Weidhaas J and Lang W (2004) Surface and Interface Analysis 17(6) 357 Ziegler JF, Biersack JP and Littmark (1985) The Stopping and range of ions in matter (Pergaman Press NY) Vol.I (new edition 2003)... 

Tyler, B.J., Castner. D.G. and Ratner, B.D. (1989) Regularisation — a stable and accurate method for generating depth profiles from angle dependent XPS ckita. Surface and Interface Analysis, 14, 44,3-450. 

Mellott, N. P., Brantley, S. L., Hamilton J. P. Pantano, C. G. (2001) Evaluation of surface preparation methods for glass. Surface and Interface Analysis, 31, 362-68. Mellott, N. P. Pantano, C. G. (2009). Multicomponent almninosilicate glass mechanisms of acid corrosion and surface layer formation. Journal of Non-Crystalline Solids, Submitted Manuscript. 

The chemical, stmctural, and electronic characteristics of surfaces and interfaces are usually different from those of the bulkphase(s). Thus, methods to be used for the analysis of surfaces must be selective in response to the surface or interfacial region relative to the bulk. Surfaces and interfaces are most commonly explored using techniques based on the interaction of photons, electrons, or ions with the surface or using a force such as electric field or van der Waals attraction. These excitations generate a response involving the production of photons, electrons, ions or the alteration of a force that is then sensed in the analysis. 

Analysis of Surface Elemental Composition. A very important class of surface analysis methods derives from the desire to understand what elements reside at the surface or in the near-surface region of a material. The most common techniques used for deterrnination of elemental composition are the electron spectroscopies in which electrons or x-rays are used to stimulate either electron or x-ray emission from the atoms in the surface (or near-surface region) of the sample. These electrons or x-rays are emitted with energies characteristic of the energy levels of the atoms from which they came, and therefore, contain elemental information about the surface. Only the most important electron spectroscopies will be discussed here, although an array of techniques based on either the excitation of surfaces with or the collection of electrons from the surface have been developed for the elucidation of specific information about surfaces and interfaces. 

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