@article {1282, title = {Pre-treatments applied to oxidized aluminum surfaces to modify the interfacial bonding with bis-1,2-(triethoxysilyl)ethane (BTSE) - Part I. High-purity Al with native oxide}, journal = {Applied Surface Science}, volume = {252}, number = {5}, year = {2005}, note = {ISI Document Delivery No.: 993WHTimes Cited: 5Cited Reference Count: 39}, month = {Dec}, pages = {1293-1304}, type = {Article}, abstract = {A remote microwave-generated H-2 plasma and heating to 250 degrees C were separately used to modify high-purity oxidized aluminum surfaces and to assess whether these treatments can help enhance adhesion with bis-1,2-(triethoxysilyl)ethane (BTSE) coatings. Different initial oxide surfaces were considered, corresponding to the native oxide and to surfaces formed by the Forest Products Laboratory (FPL) treatment applied for either 15 or 60 min. BTSE is applied from solution at pH 4, and competing processes of etching, protonation (to form OH groups) and coupling (to form Al-O-Si interfacial bonds) occur at the solid-liquid interface. Scanning electron microscopy (SEM) was used to determine how the topographies of the modified Al surfaces changed with the different pre-treatments and with exposure to a buffer solution of pH 4. Secondary-ion mass spectrometry (SIMS) was used to determine the direct amount of Al-O-Si interfacial bonds by measuring the ratio of peak intensities 71-70 amu, while X-ray photoelectron spectroscopy (XPS) was used to determine the overall strength of the silane coating adhesion by measuring the Si 2p signals before and after application of an ultrasonic rinse to the coated sample. Measured Al 2p and O 1s spectra helped assess how the different pre-treatments modified the various Al oxidized surfaces prior to BTSE coating. Pre-treated samples that showed increased Al-O-Si bonding after BTSE coating corresponded to surfaces, which did not show evidence of significant etching after exposure to a pH 4 environment. This suggests that such surfaces are more receptive to the coupling reaction during exposure to the BTSE coating solution. These surfaces include all H-2 plasma-treated samples, the heated native oxide and the sample that only received the 15 min FPL treatment. In contrast, other surfaces that show evidence of etching in pH 4 environments are samples that received lower amounts of Al-O-Si interfacial bonding. Overall, heating improved the BTSE adhesive bonding for the native Al oxide, while H-2 plasma treatment improved the BTSE bonding for surfaces that had initially been FPL-treated for 15 and 60 min. (c) 2005 Elsevier B.V All rights reserved.}, keywords = {aluminum, ESCA, OXIDATION, PARALLEL FACTOR-ANALYSIS, silane adsorption, SILANE COUPLING AGENTS, SIMS, SPECTROSCOPY, surface pre-treatment, THIN-FILMS, TOF-SIMS, X-ray photoelectron, XPS, XPS INVESTIGATIONS, ZIRCONIUM-OXIDE}, isbn = {0169-4332}, url = {://000233985900014}, author = {Teo, M. and Kim, J. and Wong, P. C. and Wong, K. C. and Mitchell, K. A. R.} } @article {1153, title = {Pre-treatments applied to oxidized aluminum surfaces to modify the interfacial bonding with bis-1,2-(triethoxysilyl)ethane (BTSE) - Part II. Anodized 7075-T6 Al alloy}, journal = {Applied Surface Science}, volume = {252}, number = {5}, year = {2005}, note = {ISI Document Delivery No.: 993WHTimes Cited: 6Cited Reference Count: 46}, month = {Dec}, pages = {1305-1312}, type = {Article}, abstract = {The methods of X-ray pbotoelectron spectroscopy (XPS), secondary-ion mass spectrometry (SIMS), and scanning electron microscopy (SEM) have been used to investigate aspects of the bonding of bis-1,2-(triethoxysilyl)ethane (BTSE) onto anodized samples of 7075-T6 aluminum alloy that have been subjected to the various pre-treatments considered in Part I. The oxide layer thins when this sample is subjected to a Forest Products Laboratory (FPL) treatment; topographical changes are detected by SEM after only 5 min, and the "scallop structures" increase in size for longer times of the FPL treatment. These 7075-Al surfaces adsorb more BTSE than the high-purity Al samples considered in Part I, although the interfacial bonding indicated by the [AlOSi](+)/[Al2O](+) SIMS ratios measured for the former samples are constant for different times of FPL treatment, unlike the situation for high-purity Al. Heating anodized 7075-Al samples, either before or after FPL treatment, has no significant effect on the subsequent BTSE adsorption, but a H-2 plasma treatment can enhance the interfacial Al-O-Si bonding with a decrease in the total BTSE polymerization. (c) 2005 Elsevier B.V. All rights reserved.}, keywords = {2024-T3, AGENTS, aluminum, corrosion, COUPLING, ESCA, HYDROXIDES, silane adsorption, SIMS, SPECTROSCOPY, surface pre-treatment, THIN-FILMS, X-ray photoelectron, XPS, XPS INVESTIGATIONS, ZIRCONIUM-OXIDE}, isbn = {0169-4332}, url = {://000233985900015}, author = {Kim, J. and Teo, M. and Wong, P. C. and Wong, K. C. and Mitchell, K. A. R.} } @article {4403, title = {SIMS studies of the effect of H at interfaces formed by oxidized zirconium}, journal = {Canadian Journal of Chemistry-Revue Canadienne De Chimie}, volume = {76}, number = {12}, year = {1998}, note = {ISI Document Delivery No.: 180RKTimes Cited: 2Cited Reference Count: 13}, month = {Dec}, pages = {1796-1799}, type = {Article}, abstract = {Secondary ion mass spectrometry (SIMS) has been used to guide the search for an oxidation procedure that can produce a thin and relatively sharp oxide layer on macroscopic zirconium. A new preparation based on dip coating in H2O2 solution is indicated to be suitable for this purpose. SIMS further indicates that the oxide interface, for such a prepared sample, shows substantial degradation when it is heated in H-2 gas at 300 degrees C. The presence of H appears to facilitate O migration into the metallic region, an observation that supplements those made previously on oxidized thin-film samples of zirconium prepared by deposition under ultrahigh-vacuum conditions.}, keywords = {electron, GROWTH, HYDROGEN, interfacial reactivity, OXIDATION, OXIDE, oxidized, OXYGEN, secondary ion mass spectrometry, SURFACES, THIN-FILMS, XPS INVESTIGATIONS, ZIRCONIUM, ZR(0001)}, isbn = {0008-4042}, url = {://000079398800002}, author = {Shimizu, K. and Flinn, B. J. and Wong, P. C. and Mitchell, K. A. R.} }