About 1.5-μm-thick single-layer TiN, CrN, TiAlN coatings and nanolayered TiN/CrN, TiAlN/CrN multilayer coatings were deposited on silicon (111) substrates using a reactive direct current magnetron sputtering process. Structural characterization of the coatings was done using x-ray diffraction (XRD) and micro-Raman spectroscopy. All the coatings exhibited NaCl B1 structure in the XRD data. Raman spectroscopy data of as-deposited coatings exhibited two broad bands centered at 230–250 and 540–630 cm-1. These bands have been assigned to acoustical and optical phonon modes, respectively. Thermal stability of the coatings was studied by heating the coatings in air in a resistive furnace for 30 min in the temperature range 400–900 °C. Structural changes as a result of heating were characterized using Raman spectroscopy and XRD. Raman data showed that TiN, CrN, TiN/CrN, TiAlN, and TiAlN/CrN coatings started to oxidize at 500, 600, 750, 800, and 900 °C, respectively. To isolate the oxidation-induced spectral changes as a result of heating of the coatings in air, samples were also annealed in vacuum at 800 °C under similar conditions. The Raman data of vacuum-annealed coatings showed no phase transformation, and intensity of the optical phonon mode increased and shifted to lower frequencies. The origin of these spectral changes is discussed in terms of defect structure of the coatings. Our results indicate that the thermal stability of nanolayered multilayer coatings is superior to the single-layer coatings.
An inexpensive and facile one-step method to develop a superhydrophobic coating on the copper surface is reported. Superhydrophobic CuO/Cu(OH) 2 surfaces were prepared by a simple solution-immersion process at room temperature, without using a low surface energy material. The structure and composition of as-prepared CuO/Cu(OH) 2 hierarchical structure were confirmed by X-ray diffraction, micro-Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS). The growth stage was carefully examined by field emission scanning electron microscopy (FESEM), and it was observed that initially Cu(OH) 2 nanoneedle arrays were formed on the copper surface and subsequently the CuO microflowers formed on the nanoneedle arrays. The contact angle as a function of immersion time was studied using a contact angle goniometer. The correlation between the microstructure of the immersed copper surface and the contact angle was examined carefully using FESEM and atomic force microscopy (AFM). Our results based on FESEM and AFM studies show that the CuO/Cu(OH) 2 coatings demonstrate superhydrophobicity only for an optimal combination of the solid region (i.e., microflowers and nanoneedles) and air pockets (i.e., voids). The maximum static water contact angle on the prepared surface was 159°. The wettability transition of the CuO/Cu(OH) 2 surface from superhydrophobicity to superhydrophilicity was studied by the alteration of oxygen plasma treatment and dark storage. The FESEM, AFM, and XPS studies showed that this transformation was mainly due to the morphological changes that occur in addition to the chemical changes taking place on the CuO/Cu(OH) 2 surface under the influence of oxygen plasma. XPS analysis demonstrated that the incorporation of oxygen species by oxygen plasma activation accounted for the highly hydrophilic character of the surface.
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