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Oxygen isotope exchange experiments, H218O/H216O ('wet' anneals) and 18O2/16O2 ('dry' anneals), were performed on single crystal samples of yttria-stabilized zirconia (YSZ) at a temperature of T = 1073 K with subsequent determination of the oxygen isotope profiles in the solid by time-of-flight secondary ion mass spectrometry (ToF-SIMS). Such experiments yielded oxygen tracer diffusion coefficients ( D*) and oxygen tracer surface exchange coefficients ( k*), from both the polished (smooth) and unpolished (rough) sides of single crystal samples, as a function of water partial pressure pH2O and oxygen partial pressure pO2. Isothermal values of D* were found to depend on neither pO2 nor pH2O (nor surface roughness). Isothermal values of k*, in contrast, displayed a strong dependence on pO2 or pH2O; k*wet was, in addition, 2-3 orders of magnitude higher than k*dry. Surprisingly, surface roughness had little effect on k*wet, whereas rough surfaces exhibited much higher k*dry values than smooth surfaces. Data for k*wet obtained as a function of temperature at pH2O = 18 mbar show a change in activation enthalpy at T ≈ 973 K. The behavior of k* is discussed in terms of surface composition, surface area and surface reaction mechanisms. [ABSTRACT FROM AUTHOR]

Low-energy ion scattering (LEIS) is known for its extreme surface sensitivity, as it yields a quantitative analysis of the outermost surface as well as highly resolved in-depth information for ultrathin surface layers. Hence, it could have been generally considered to be a suitable technique for the analysis of graphene samples. However, due to the low scattering cross section for light elements such as carbon, LEIS has not become a common technique for the characterization of graphene. In the present study we use a high-sensitivity LEIS instrument with parallel energy analysis for the characterization of CVD graphene transferred to thermal silica/silicon substrates. Thanks to its high sensitivity and the exceptional depth resolution typical of LEIS, the graphene layer closure was verified, and different kinds of contaminants were detected, quantified, and localized within the graphene structure. Utilizing the extraordinarily strong neutralization of helium by carbon atoms in graphene, LEIS experiments performed at several primary ion energies permit us to distinguish carbon in graphene from that in nongraphitic forms (e.g., the remains of a resist). Furthermore, metal impurities such as Fe, Sn, and Na located at the graphene-silica interface (intercalated) are detected, and the coverages of Fe and Sn are determined. Hence, high-resolution LEIS is capable of both checking the purity of graphene surfaces and detecting impurities incorporated into graphene layers or their interfaces. Thus, it is a suitable method for monitoring the quality of the whole fabrication process of graphene, including its transfer on various substrates.

With the widespread use of engineered nanoparticles for biomedical applications, detailed surface characterization is essential for ensuring reproducibility and the quality/suitability of the surface chemistry to the task at hand. One important surface property to be quantified is the overlayer thickness of self-assembled monolayer (SAM) functionalized nanoparticles, as this information provides insight into SAM ordering and assembly. We demonstrate the application of high sensitivity low energy ion scattering (HS-LEIS) as a new analytical method for the fast thickness characterization of SAM functionalized gold nanoparticles (AuNPs). HS-LEIS demonstrates that a complete SAM is formed on 16-mercaptohexadecanoic acid (C16COOH) functionalized 14 nm AuNPs. HS-LEIS also experimentally provides SAM thickness values that are in good agreement with previously reported results from simulated electron spectra for surface analysis (SESSA) analysis of X-ray photoelectron spectroscopy (XPS) data. These results indicate HS-LEIS is a valuable surface analytical method for the characterization of SAM functionalized nanomaterials.

Electrical field-flow fractionation (ElFFF) and sedimentation field-flow fractionation (SdFFF) were used in combination to study the adsorption of the triblock polymeric surfactant, Pluronic F108 [(EO)129-(PO)56-(EO)129] to 200 nm polystyrene (PS) latex spheres. The SdFFF technique allowed an accurate determination of the mass of surfactant adsorbed on each particle from a solution of given concentration. To complement this isotherm study, we show that ElFFF can be used to measure fractional coverages of the formed electrically neutral surfactant layers on the charged PS particles. Through a combination of the two techniques it is possible to gain information about the structure of the adsorbate layer. Thus, when Pluronic F108 is taken up by the PS surface from solutions of low concentration, all three blocks appear to adhere to the surface as long as there is free space available. As the solution concentration increases and the fractional coverage reaches approximately 20%, the surface turns crowded enough to let the strongly adsorbing PPO blocks competitively displace the weakly adherent PEO blocks, which gradually rise to extend into the aqueous phase until the surface is fully saturated.