Micro-abrasion wear behaviour of TiAlCrSiN nanostructured coatings

The injection process of glass fibres reinforced plastics promotes the moulds surface degradation by erosion. In order to improve its wear resistance, several kinds of PVD thin hard coatings were used. It is well-known that nanostructures present a better compromise between hardness and toughness. Indeed, when the coating is constituted by a large number of ultra-thin different layers, cracks and interface troubles tend to decrease. However, it is not clear that these nanostructures present a better wear behaviour in erosion processes. In order to study its wear behaviour, a sputtered PVD nanostructured TiAlCrSiN coating was used. The substrate and film surfaces topography were analyzed by profilometry and atomic force microscopy techniques. Film adhesion to the substrate was evaluated by scratch tests. The surface hardness was measured with a Vickers micro-hardness tester. The wear resistance was evaluated by micro-abrasion with a rotating ball tribometer tests. Slurry of SiC particles in distilled water was used in order to provoke the surface abrasion. Different duration tests were performed in order to analyze the wear evolution. After these tests, the wear mechanisms developed were analyzed by scanning electron microscopy. Wear craters were measured and the wear rate was calculated and discussed. With the same purpose, coated inserts were mounted in an injection mould working with a 30% glass fibres reinforced polypropylene. After 45 000 cycles no relevant wear was registered.

Forward osmosis membranes tailored by hydrogel coatings

Dissertação para obtenção do Grau de Mestre em Engenharia Química e Bioquímica

Electrochemical vs antibacterial characterization of ZrCN-Ag coatings

Nowadays, antibacterial properties are becoming a viable feature to be introduced in biomaterials due to the possibility of modifying the materials' surface used in medical devices in a micro/nano metric scale. As a result, it is mandatory to understand the mechanisms of the antimicrobial agents currently used and their possible failures. In this work, the antibacterial activity of ZrCNAg films is studied, taking into consideration the ability of silver nanoparticles to be dissolved when embedded into a ceramic matrix. The study focuses on the silver release evaluated by glow discharge optical emission spectroscopy and the effect of the fluid composition on this release. The results revealed a very low silver release of the films, leading to non-antibacterial activity of such materials. The silver release was found to be dependent on the electrolyte composition. NaCl (8.9 g L? 1) showed the lowest spontaneously silver ionization, while introducing the sulfates in Hanks' balanced salt solution (HBSS) such ionization is increased; finally, the proteins incorporated to the (HBSS) showed a reduction of the silver release, which also explains the low ionization in the culture medium (tryptic soy broth) that contains high quantities of proteins.

Caracterização química e física de conformal coatings envolvidos na produção de PCBA's

Dissertação de mestrado integrado em Engenharia de Materiais

Production and characterization of ZrCN-Ag coatings deposited by mganetron sputtering

Tese de Doutoramento (Programa doutoral em Engenharia de Materiais)

Development of multifunctional coatings deposited on polymers based sensors for biomedical applications

Tese de Doutoramento (Programa Doutoral em Engenharia de Materiais)

Antibacterial Ag/a-C nanocomposite coatings: The influence of nano-galvanic a-C and Ag couples on Ag ionization rates

Biofilm formation has been pointed as a major concern in different industrial applications, namely on biomedical implants and surgical instruments, which has prompted the development of new strategies for production of efficient antimicrobial surfaces. In this work, nano âgalvanic couples were created to enhance the antibacterial properties of silver, by embedding it into amorphous carbon (a-C) matrix. The developed Ag/a-C nanocomposite coatings, deposited by magnetron sputtering, revealed an outstanding antibacterial activity against S.epidermidis, promoting a total reduction in biofilm formation with no bacteria counts in all dilution. The open circuit potential (OCP) tests in 0.9% NaCl confirmed that a-C shows a positive \OCP\ value, in contrast to Ag coating, thus enhancing the ionization of biocidal Ag+ due to the nano-galvanic couple activation. This result was confirmed by the inductively coupled plasma-optical emission spectroscopy (ICP-OES), which revealed a higher Ag ionization rate in the nanocomposite coating in comparison with the Ag coating. The surface of Ag/a-C and Ag coatings immersed in 0.9% NaCl were monitored by scanning electron microscopy (SEM) over a period of 24 hours, being found that the Ag ionization determined by ICP-OES was accompanied by an Ag nanoparticles coalescence and agglomeration in Ag/a-C coating.

Antibacterial properties of multifunctional coatings Ag-ZrCN for biomedical devices: a novel approach

PhD in Sciences Specialty in Physics

Structural characterization of laser-treated Cr3C2-NiCr coatings

The interconnected porosity of the Cr3C2-NiCr coatings obtained by high-velocity oxy fuel spraying is detrimental in corrosion and wear resistance applications. Laser treatments allow sealing of their surfaces through melting and resolidification of a thin superficial layer. A Nd:YAG laser beam was used to irradiate Cr3C2-NiCr coatings either in the continuous wave mode or at different repetition rates in the pulsed one. Results indicated that high peak and low mean laser irradiances are not good, since samples presented deep grooves and an extensive crack network. At low peak and higher mean laser irradiances the surface was molten, and only a few shallow cracks were observed. The interconnected porosity was completely eliminated in a layer up to 80 m thick, formed by large Cr7C3 grains imbedded in a NiCr matrix.

Hydroxyapatite coatings grown by pulsed laser deposition with a beam of 355 nm wavelength

Calcium phosphate coatings, obtained at different deposition rates by pulsed laser deposition with a Nd:YAG laser beam of 355-nm wavelength, were studied. The deposition rate was changed from 0.043 to 1.16 /shot by modification of only the ablated area, maintaining the local fluence constant to perform the ablation process in similar local conditions. Characterization of the coatings was performed by scanning electron microscopy, x-ray diffractometry, and infrared, micro-Raman, and x-ray photoelectron spectroscopy. The coatings showed a compact surface morphology formed by glassy gains with some droplets on them. Only hydroxyapatite (HA) and alpha-tricalcium phosphate (alpha-TCP) peaks were found in the x-ray diffractograms. The relative content of alpha TCP diminished with decreasing deposition rates, and only HA peaks were found for the lowest rate. The origin of alpha TCP is discussed.

Structural characterization of laser-treated Cr3C2-NiCr coatings

The interconnected porosity of the Cr3C2-NiCr coatings obtained by high-velocity oxy fuel spraying is detrimental in corrosion and wear resistance applications. Laser treatments allow sealing of their surfaces through melting and resolidification of a thin superficial layer. A Nd:YAG laser beam was used to irradiate Cr3C2-NiCr coatings either in the continuous wave mode or at different repetition rates in the pulsed one. Results indicated that high peak and low mean laser irradiances are not good, since samples presented deep grooves and an extensive crack network. At low peak and higher mean laser irradiances the surface was molten, and only a few shallow cracks were observed. The interconnected porosity was completely eliminated in a layer up to 80 m thick, formed by large Cr7C3 grains imbedded in a NiCr matrix.

Ultraviolet optical and microstructural properties of MgF2 and LaF3 coatings deposited by ion-beam sputtering and boat and electron-beam evaporation

Single layers of MgF2 and LaF3 were deposited upon superpolished fused-silica and CaF2 substrates by ion-beam sputtering (IBS) as well as by boat and electron beam (e-beam) evaporation and were characterized by a variety of complementary analytical techniques. Besides undergoing photometric and ellipsometric inspection, the samples were investigated at 193 and 633 nm by an optical scatter measurement facility. The structural properties were assessed with atomic-force microscopy, x-ray diffraction, TEM techniques that involved conventional thinning methods for the layers. For measurement of mechanical stress in the coatings, special silicon substrates were coated and analyzed. The dispersion behavior of both deposition materials, which was determined on the basis of various independent photometric measurements and data reduction techniques, is in good agreement with that published in the literature and with the bulk properties of the materials. The refractive indices of the MgF2 coatings ranged from 1.415 to 1.440 for the wavelength of the ArF excimer laser (193 nm) and from 1.435 to 1.465 for the wavelength of the F2 excimer laser (157 nm). For single layers of LaF3 the refractive indices extended from 1.67 to 1.70 at 193 nm to ~1.80 at 157 nm. The IBS process achieves the best homogeneity and the lowest surface roughness values (close to 1 nmrms) of the processes compared in the joint experiment. In contrast to MgF2 boat and e-beam evaporated coatings, which exhibit tensile mechanical stress ranging from 300 to 400 MPa, IBS coatings exhibit high compressive stress of as much as 910 MPa. A similar tendency was found for coating stress in LaF3 single layers. Experimental results are discussed with respect to the microstructural and compositional properties as well as to the surface topography of the coatings.

Antibacterial burst-release from minimal Ag-containing plasma polymer coatings.

Biomaterials releasing silver (Ag) are of interest because of their ability to inhibit pathogenic bacteria including antibiotic-resistant strains. In order to investigate the potential of nanometre-thick Ag polymer (Ag/amino-hydrocarbon) nanocomposite plasma coatings, we studied a comprehensive range of factors such as the plasma deposition process and Ag cation release as well as the antibacterial and cytocompatible properties. The nanocomposite coatings released most bound Ag within the first day of immersion in water yielding an antibacterial burst. The release kinetics correlated with the inhibitory effects on the pathogens Pseudomonas aeruginosa or Staphylococcus aureus and on animal cells that were in contact with these coatings. We identified a unique range of Ag content that provided an effective antibacterial peak release, followed by cytocompatible conditions soon thereafter. The control of the in situ growth conditions for Ag nanoparticles in the polymer matrix offers the possibility to produce customized coatings that initially release sufficient quantities of Ag ions to produce a strong adjacent antibacterial effect, and at the same time exhibit a rapidly decaying Ag content to provide surface cytocompatibility within hours/days. This approach seems to be favourable with respect to implant surfaces and possible Ag-resistance/tolerance built-up.

Surface assembly of poly(I:C) on PEGylated microspheres to shield from adverse interactions with fibroblasts.

By expressing an array of pattern recognition receptors (PRRs), fibroblasts play an important role in stimulating and modulating the response of the innate immune system. The TLR3 ligand polyriboinosinic acid-polyribocytidylic acid, poly(I:C), a mimic of viral dsRNA, is a vaccine adjuvant candidate to activate professional antigen presenting cells (APCs). However, owing to its ligation with extracellular TLR3 on fibroblasts, subcutaneously administered poly(I:C) bears danger towards autoimmunity. It is thus in the interest of its clinical safety to deliver poly(I:C) in such a way that its activation of professional APCs is as efficacious as possible, whereas its interference with non-immune cells such as fibroblasts is controlled or even avoided. Complementary to our previous work with monocyte-derived dendritic cells (MoDCs), here we sought to control the delivery of poly(I:C) surface-assembled on microspheres to human foreskin fibroblasts (HFFs). Negatively charged polystyrene (PS) microspheres were equipped with a poly(ethylene glycol) (PEG) corona through electrostatically driven coatings with a series of polycationic poly(L-lysine)-graft-poly(ethylene glycol) copolymers, PLL-g-PEG, of varying grafting ratios g from 2.2 up to 22.7. Stable surface assembly of poly(I:C) was achieved by incubation of polymer-coated microspheres with aqueous poly(I:C) solutions. Notably, recognition of both surface-assembled and free poly(I:C) by extracellular TLR3 on HFFs halted their phagocytic activity. Ligation of surface-assembled poly(I:C) with extracellular TLR3 on HFFs could be controlled by tuning the grafting ratio g and thus the chain density of the PEG corona. When assembled on PLL-5.7-PEG-coated microspheres, poly(I:C) was blocked from triggering class I MHC molecule expression on HFFs. Secretion of interleukin (IL)-6 by HFFs after exposure to surface-assembled poly(I:C) was distinctly lower as compared to free poly(I:C). Overall, surface assembly of poly(I:C) may have potential to contribute to the clinical safety of this vaccine adjuvant candidate.

Hydro-Surface Preparation and Coating for Painted Structural Steel, TR-407, 1999

Cities and counties in Iowa have more than 8,890 steel bridges, most of which are painted with red lead paint. The Iowa Department of Transportation (Iowa DOT) maintains less than 35 bridges coated with red lead paint, including seven of the large border bridges over the Mississippi and Missouri Rivers. Because of the federal and state regulations for bridge painting, many governmental agencies have opted not to repaint, or otherwise maintain, lead paint coatings. Consequently, the paint condition on many of these bridges is poor, and some bridges are experiencing severe rusting of structural members. This research project was developed with two objectives: 1) to evaluate the effectiveness of preparing the structural steel surface of a bridge with high pressure water jetting instead of abrasive blasting and 2) to coat the structural steel surface with a moisture-cured polyurethane paint under different surface preparation conditions.