Composites surface analytical techniques

X-ray photoelectron spectroscopy (XPS) is currently the most widely used surface-analytical technique, and is therefore described here in more detail than any of the other techniques. At its inception hy Sieghahn and coworkers [2.1] it was called ESCA (electron spectroscopy for chemical analysis), hut the name ESCA is now considered too general, because many surface-electron spectroscopies exist, and the name given to each one must be precise. The name ESCA is, nevertheless, still used in many places, particularly in industrial laboratories and their publications. Briefly, the reasons for the popularity of XPS are the exceptional combination of compositional and chemical information that it provides, its ease of operation, and the ready availability of commercial equipment. 

Its ability to distinguish among different elements and different chemical bonding configurations has made XPS the most popular surface analytical technique for providing structural, chemical bonding, and composition data... 

Analysis by the Detection of Scattered Ions. Ions generally penetrate the specimen much less deeply than electrons of equivalent energy, so they are more surface-sensitive. Ion-based surface analytical techniques are popular because of their sensitivity and their ability, in some cases, to reveal the depth composition profile. 

The surface analytical techniques mentioned above provide wealth information on the composition and structure of polymer surfaee and changes resulting from modification by plasma discharge. It should be however stressed that, despite of broad spectrum of analytical techniques available, the information is not sufficient to understand all imderlying proeesses in their eomplexity. Espeeially, it is the case of plasma treatment when the interaetions of many plasma eonstituents with polymer surface may play a role. Existing theoretical models are restricted to some specific cases and they usually deseribe only some part of the proeess. 

Castle, J.E. and Watts, J.F. (1988). The study of interfaces in composite materials by surface analytical techniques. In Interfaces in Polymer, Ceramic and Metal Matrix Composites (Proc. ICCI-II) (H. Ishida ed ), Elsevier Seienee, New York, pp. 57-71. 

In addition to the electrochemical techniques, many surface analytical techniques are constantly in use, such as ellipsome-try for the surface thin oxide thickness, multiple reflection infrared spectroscopy (MIR), and X-ray photoelectron spectroscopy (XPS) for surface layer composition, total reflection X-ray fluorescence spectroscopy (TXRFS) for the metal surface contaminants, and naturally atomic force microscopy (AFM) for the surface roughness profile. 

SIMS and SNMS are versatile analytical techniques for the compositional characterization of solid surfaces and interfaces in materials research.92-94 As one of the most important applications, both surface analytical techniques allow depth profile analysis (concentration profile as a function of the depth analyzed) to be performed in materials science and the semiconductor industry with excellent depth resolution in the low nm range. For depth profiling in materials science, dynamic SIMS and SNMS using high primary ion beam doses are applied. Both techniques permit the analysis of light elements such as H, , C and N, which are difficult to measure with other analytical techniques. 

The next chapter is a review of current practice in lubrication of internal combustion engines and lubricant design. The role of individual lubricant components and their use in mineral and synthetic formulations is covered. This is followed by a discussion of the tribochemical effects of additive interactions. The heart of the manuscript is chapters, "Tribochemical nature of antiwear film , "Surface tribochemistry and activated processes", and "Analytical techniques in lubricating practices". Topics covered include tribofilm formation, organomolybdenum compounds in surface protection, catalytic activity of rubbing surfaces, introduction of some techniques for evaluation of tribofilms composition and analytical techniques for evaluation of lubricant degradation. Examples of the application of basic concepts are introduced, eg., acidity and basicity in the process of lubricant deterioration. 

The failure analysis can be done using a judicious combination of several methods such as visual examination, metallography, microscopy, electron microprobe, energy dispersive X-ray analysis, X-ray diffraction methods for determining residual stress in the sample, surface analytical techniques to determine the nature and composition of surface deposits and finite element analysis modeling. 

The interface between plastic and wood fibres strongly influences the mechanical properties of a plastic/wood fibre composite. A means for evaluating the effectiveness of surface treatment on the wood fibres in the PVC/wood fibre composites is presented that investigated the adhesion between PVC and laminated wood veneers. Wood veneers were first treated with gamma-aminopropyltriethoxysilane, dichlorodiethylsilane, phthalic anhydride, and maleated PP for surface modification. The chemical modification made on the wood surfaces was then characterised by different complementary surface analytical techniques X-ray photoelectron spectroscopy and surface tension measurements. 63 refs. 

As a preparation to the following sections, we briefly discuss some aspects of measuring adsorption from fluid phases, including dilute solutions. For the sake of systematics, we divide the treatment into two parts (1) adsorption on disperse systems, sometimes poorly defined, and (ii) the same on well-defined, mostly smooth model surfaces. In case (1) adsorption is almost exclusively determined from solution analysis, i.e. by depletion, so that problems arise with the separation of liquid from solid and the accurate bulk composition determinations. In case (ii), adsorbed amounts can often be determined directly using typical surface analytical techniques. 

In addition to the electrochemical techniques, many insitu and exsitu surface analytical techniques are used in studies of silicon electrodes, such as ellipsometry for determining thin surface film thickness, ° infrared spectroscopy for surface adsorption, 260,424 surface composition, and for... 

Surface analyses of unreacted and chemically modified cottons can be used to advantage in textile problem solving, provided there is an understanding of the principles and limits of surface analytical techniques. Surface analyses in combination with other techniques can be used to characterize surfaces, detect changes in composition with depth from surfaces, and even to determine differences in surface and bulk compositions of textile samples. 

The following major chapter is devoted to a short description of surface analytical techniques for the investigation of adsorption. Modem experimental methods will be preferred over older less reliable ones which have been applied at high pressme or poor vacuum to samples with ill-defined stracture and composition. This chapter will complement the description of techniques given in the Landolt-Bomstein volume III/24. 

The composition of a specimen is often determined by X-ray fluorescence (XRF) spectrometry, which performs rapid, qualitative, and semiquantitative determination of major and minor surface elements. Although both wavelength- and energy-dispersive (ED) analyzers can be used to detect the secondary X-rays, ED-XRE instruments are more common for the compositional determination of archaeological and conservation samples. Detection limits of 0.1% are expected therefore, the analysis is difficult for trace elements. A laboratory XRE system, commonly used to quantify elements in metal and ceramic samples (noninsulating materials need to be coated), is considered to be an indispensable tool. As with all these surface analytical techniques, care has to be taken that weathering products (thick patinas or corrosion crusts) do not obscure bulk analysis results. Thus, samples are normally prepared to provide a flat polished surface to produce quantitative results. 

Scanning electron microscopy (SEM) is one of the most versatile and widely used of the surface analytical techniques as it allows both the morphology and composition of various materials in modern science to be studied. It is considered a relatively rapid. 

ABSTRACT. The paper details the use of scanning electron microscopy, surface reflectance infrared spectroscopy, Auger electron spectroscopy, ion scattering spectroscopy, secondary ion mass spectroscopy, and x-ray photoelectron spectroscopy in the analysis of polymeric adhesives and composites. A brief review of the principle of each surface analytical technique will be followed by application of the technique to interfacial adhesion with an emphasis on polymer/metal, fiber/matrix, and composite/composite adhesion. 

The objective of this paper is to present a review of the results of some of the microscopic/spectroscopic techniques which have been used in the study of adhesion. The spectroscopic techniques to be discussed are listed in Table I adapted from Baun (4). A brief review of each technique will be followed by a discussion of results illustrating the application of the technique to polymer/metal, fiber/matrix, and composite/composite adhesion. A recent, more detailed review of the use of surface analytical techniques applied to polymer/metal adhesion has been published (6). 

ToF-secondary ion mass spectrometry (ToF-SIMS) is a versatile surface analytical technique that provides detailed information about molecular composition and imaging of surface monolayers with high sensitivity and resolution. In a typical SIMS sample, surfaces are exposed to a beam of energetic primary ions or atoms (5—25 keV), which results in the emission of secondary ions including quasimolecular ions, atoms, and molecules (Benninghoven, 1994). The secondary ions formed as a result of this... 

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