Electro and Magneto-Electropolished Surface Micro-Patterning on Binary and Ternary Nitinol

In this study, an Atomic Force Microscopy (AFM) roughness analysis was performed on non-commercial Nitinol alloys with Electropolished (EP) and Magneto-Electropolished (MEP) surface treatments and commercially available stents by measuring Root-Mean-Square (RMS) , Average Roughness (Ra), and Surface Area (SA) values at various dimensional areas on the alloy surfaces, ranging from (800 x 800 nm) to (115 x 115µm), and (800 x 800 nm) to (40 x 40 µm) on the commercial stents. Results showed that NiTi-Ta 10 wt% with an EP surface treatment yielded the highest overall roughness, while the NiTi-Cu 10 wt% alloy had the lowest roughness when analyzed over (115 x 115 µm). Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopy (EDS) analysis revealed unique surface morphologies for surface treated alloys, as well as an aggregation of ternary elements Cr and Cu at grain boundaries in MEP and EP surface treated alloys, and non-surface treated alloys. Such surface micro-patterning on ternary Nitinol alloys could increase cellular adhesion and accelerate surface endothelialization of endovascular stents, thus reducing the likelihood of in-stent restenosis and provide insight into hemodynamic flow regimes and the corrosion behavior of an implantable device influenced from such surface micro-patterns.

Conjugated Quantum Dots Inhibit the Amyloid β (1–42) Fibrillation Process

Nanoparticles have enormous potential in diagnostic and therapeutic studies. We have demonstrated that the amyloid beta mixed with and conjugated to dihydrolipoic acid- (DHLA) capped CdSe/ZnS quantum dots (QDs) of size approximately 2.5 nm can be used to reduce the fibrillation process. Transmission electron microscopy (TEM) and atomic force microscopy (AFM) were used as tools for analysis of fibrillation. There is a significant change in morphology of fibrils when amyloid β (1–42) (Aβ (1–42)) is mixed or conjugated to the QDs. The length and the width of the fibrils vary under modified conditions. Thioflavin T (ThT) fluorescence supports the decrease in fibril formation in presence of DHLA-capped QDs.

Enhanced Biocompatibility of NiTi (Nitinol) Via Surface Treatment and Alloying

It is projected that by 2020, there will be 138 million Americans over 45, the age at which the increased incidence of heart diseases is documented. Many will require stents. This multi-billion dollar industry, with over 2 million patients worldwide, 15% of whom use Nitinol stents have experienced a decline in sales recently, due in part to thrombosis. It is a sudden blood clot that forms inside stents. As a result, the Food and Drug Administration and American Heart Association are calling for a new generation of stents, new designs and different alloys that are more adaptable to the arteries. The future of Nitinol therefore depends on a better understanding of the mechanisms by which Nitinol surfaces can be rendered stable and inert. In this investigation, binary and ternary Nitinol alloys were prepared and subjected to various surface treatments such as electropolishing (EP), magnetoelectropolishing (MEP) and water boiling & passivation (W&P). In vitro corrosion tests were conducted on Nitinol alloys in accordance with ASTM F 2129-08. The metal ions released into the electrolyte during corrosion tests were measured by Inductively Coupled Plasma Mass Spectroscopy (ICP-MS). Biocompatibility was assessed by observing the growth of human umbilical vein endothelial cells (HUVEC) on the surface of Nitinol alloys. Static and dynamic immersion tests were performed by immersing the Nitinol alloys in cell culture media and measuring the amount of metal ions released in solution. Sulforhodamine B (SRB) assays were performed to elucidate the effect of metal ions on the growth of HUVEC cells. The surfaces of the alloys were studied using Scanning Electron Microscopy (SEM) and X-ray Photoelectron Spectroscopy (XPS) respectively. Finally, wettability and surface energy were measured by Contact Angle Meter, whereas surface roughness was measured by Atomic Force Microscopy (AFM). All the surface treated alloys exhibited high resistance to corrosion when compared with untreated alloys. SRB assays revealed that Ni and Cu ions exhibited greater toxicity than Cr, Ta and Ti ions on HUVEC cells. EP and MEP alloys possessed relatively smooth surfaces and some were composed of nickel oxides instead of elemental nickel as determined by XPS. MEP exhibited lowest surface energy and lowest surface roughness.

Obtenção e caracterização de complexos polieletrolíticos de quitosana e poli (metacrilato de sódio)

Polyelectrolyte complexes (PECs) nanoparticles were prepared using chitosan and sodium polymethacrylate. The complex formation was investigated using turbidimetry, conductometry, viscometry, and dynamic light scattering. The presence of excess positive charges was evidenced by zeta potential measurements. The particle diameter was characterized by dynamic light scattering and the morphology by atomic force microscopy. In all experiments an abrupt change in behavior was observed at a carboxyl:amino molar ratio around 0.7−0.8. Those changes in behavior were related to a proposed mechanism of complex formation based on the decrease of macromolecular dimensions of soluble polyelectrolyte complex clusters, followed by phase segregation

Comparação entre técnicas de nitretação em cátodo oco e gaiola catódica na deposição de TiN

The plasma nitriding has been used in industrial and technological applications for large-scale show an improvement in the mechanical, tribological, among others. In order to solve problems arising in the conventional nitriding, for example, rings constraint (edge effect) techniques have been developed with different cathodes. In this work, we studied surfaces of commercially pure titanium (Grade II), modified by plasma nitriding treatment through different settings cathodes (hollow cathode, cathodic cage with a cage and cathodic cage with two cages) varying the temperature 350, 400 and 430oC, with the goal of obtaining a surface optimization for technological applications, evaluating which treatment generally showed better results under the substrate. The samples were characterized by the techniques of testing for Atomic Force Microscopy (AFM), Raman spectroscopy, microhardness, X-ray diffraction (XRD), and a macroscopic analysis. Thus, we were able to evaluate the processing properties, such as roughness, topography, the presence of interstitial elements, hardness, homogeneity, uniformity and thickness of the nitrided layer. It was observed that all samples were exposed to nitriding modified relative to the control sample (no treatment) thus having increased surface hardness, the presence of TiN observed by XRD as per both Raman and a significant change in the roughness of the treated samples . It was found that treatment in hollow cathode, despite having the lowest value of microhardness between treated samples, was presented the lowest surface roughness, although this configuration samples suffer greater physical aggressiveness of treatment

Influência da superfície do titânio nitretado a plasma em diferentes atmosferas na ativação de plaquetas sanguíneas

This study aimed to analyze the biological response of titanium surfaces modified by plasma Ar + N2 + H2. Titanium disks grade II received different surface treatments Ar + N2 + H2 plasma, constituting seven groups including only polished samples used as standard. Before and after treatment the samples were evaluated in terms of topography, crystal structure and wettability, using atomic force microscopy, X-ray diffraction, Raman spectroscopy and testing of the sessile drop, respectively. Rich plasma (PRP) was applied to the surfaces modified in culture plates. Images obtained by scanning electron microscopy of the adhered platelets were analyzed to verify the behavior of platelets in the different experimental conditions. We verified that the adition of H2 on plasma atmosphere resulted in more rough surfaces, with round tops. These surfaces, in contrast to that surfaces treated with high concentration of N2, are less propense to platelet aggregation and, consequently, to the formation of thrombus when applied in biomedical devices.

Estudo da deposição de filmes finos de BaTi(1-X)Zr(X)O3 por meio de planejamento Box-Behnken

Ferroelectric ceramics with perovskite structure (ABO3) are widely used in solid state memories (FeRAM’s and DRAM's) as well as multilayered capacitors, especially as a thin films. When doped with zirconium ions, BaTiO3-based materials form a solid solution known as barium zirconate titanate (BaTi1-xZrxO3). Also called BZT, this material can undergo significant changes in their electrical properties for a small variation of zirconium content in the crystal lattice. The present work is the study of the effects of deposition parameters of BaTi0,75Zr0,25O3 thin films by spin-coating method on their morphology and physical properties, through an experimental design of the Box-Behnken type. The resin used in the process has been synthesized by the polymeric precursor method (Pechini) and subsequently split into three portions each of which has its viscosity adjusted to 10, 20 and 30 mPa∙s by means of a rotary viscometer. The resins were then deposited on Pt/Ti/SiO2/Si substrates by spin-coating method on 15 different combinations of viscosity, spin speed (3000, 5500 and 8000 rpm) and the number of deposited layers (5, 8 and 11 layers) and then calcined at 800 ° C for 1 h. The phase composition of the films was analyzed by X-ray diffraction (XRD) and indexed with the JCPDS 36-0019. Surface morphology and grain size were observed by atomic force microscopy (AFM) indicating uniform films and average grain size around 40 nm. Images of the cross section of the films were obtained by scanning electron microscopy field emission (SEM-FEG), indicating very uniform thicknesses ranging from 140-700 nm between samples. Capacitance measurements were performed at room temperature using an impedance analyzer. The films presented dielectric constant values of 55-305 at 100kHz and low dielectric loss. The design indicated no significant interaction effects between the deposition parameters on the thickness of the films. The response surface methodology enabled better observes the simultaneous effect of variables.

Nanopartículas catiônicas de poli (ácido lático) para liberação modificada de peptídios da peçonha do escorpião Tityus serrulatus

Reported accidents involving the poisoning scorpions are still frequent in Brazil, mainly caused by Tityus serrulatus, known as yellow scorpion. Although antivenom sera are produced routinely by various government laboratories, the effectiveness of its use depends on how quickly treatment is initiated and efficiency in the production of antibodies by the immunized animals. In this study, the development of cationic polymeric nanoparticles of poly(lactic acid) aimed to create a modified delivery system for peptides and proteins of T. serrulatus venom, able to enhance the production of serum antibodies against the scorpion toxins. The cationic nanoparticles were obtained by a low energy nanoprecipitation, after study of the parameters’ variations effects over the physicochemical properties of the particles. The surface functionalization of the nanoparticles with the hyperbranched polyethyleneimine was proved by zeta potential analysis and enabled the adsorption by electrostatic interaction of different types of proteins. The protein loading efficiency of 40-80 % to bovine serum albumin (BSA) and 100 % to scorpion venom peptides evaluated by spectrophotometry and polyacrylamide gel electrophoresis confirmed the success of the selected parameters established for obtainment of nanoparticles, produced with size between 100 to 250 nm. The atomic force microscopy analysis and in vitro release showed that the spherical nanoparticles provided a sustained release profile of proteins by diffusion mechanism, demonstrating the potential for application of the nanoparticles in vivo.

Nanopartículas catiônicas de poli (ácido lático) para liberação modificada de peptídios da peçonha do escorpião Tityus serrulatus

Reported accidents involving the poisoning scorpions are still frequent in Brazil, mainly caused by Tityus serrulatus, known as yellow scorpion. Although antivenom sera are produced routinely by various government laboratories, the effectiveness of its use depends on how quickly treatment is initiated and efficiency in the production of antibodies by the immunized animals. In this study, the development of cationic polymeric nanoparticles of poly(lactic acid) aimed to create a modified delivery system for peptides and proteins of T. serrulatus venom, able to enhance the production of serum antibodies against the scorpion toxins. The cationic nanoparticles were obtained by a low energy nanoprecipitation, after study of the parameters’ variations effects over the physicochemical properties of the particles. The surface functionalization of the nanoparticles with the hyperbranched polyethyleneimine was proved by zeta potential analysis and enabled the adsorption by electrostatic interaction of different types of proteins. The protein loading efficiency of 40-80 % to bovine serum albumin (BSA) and 100 % to scorpion venom peptides evaluated by spectrophotometry and polyacrylamide gel electrophoresis confirmed the success of the selected parameters established for obtainment of nanoparticles, produced with size between 100 to 250 nm. The atomic force microscopy analysis and in vitro release showed that the spherical nanoparticles provided a sustained release profile of proteins by diffusion mechanism, demonstrating the potential for application of the nanoparticles in vivo.

Micromachined silicon lenses for terahertz applications

Silicon microlenses are a very important tool for coupling terahertz (THz) radiation into antennas and detectors in integrated circuits. They can be used in a large array structures at this frequency range reducing considerably the crosstalk between the pixels. Drops of photoresist have been deposited and their shape transferred into the silicon by means of a Reactive Ion Etching (RIE) process. Large silicon lenses with a few mm diameter (between 1.5 and 4.5 mm) and hundreds of μm height (between 50 and 350 μm) have been fabricated. The surface of such lenses has been characterized using Scanning Electron Microscopy (SEM) and Atomic Force Microscopy (AFM), resulting in a surface roughness of about ∼3 μm, good enough for any THz application. The beam profile at the focal plane of such lenses has been measured at a wavelength of 10.6 μm using a tomographic knife-edge technique and a CO2 laser.

Microparticle surface layering through dry coating:impact of moisture content and process parameters on the properties of orally disintegrating tablets

OBJECTIVES: The aim of this study was to investigate the influence of process parameters during dry coating on particle and dosage form properties upon varying the surface adsorbed moisture of microcrystalline cellulose (MCC), a model filler/binder for orally disintegrating tablets (ODTs). METHODS: The moisture content of MCC was optimised using the spray water method and analysed using thermogravimetric analysis. Microproperty/macroproperty assessment was investigated using atomic force microscopy, nano-indentation, scanning electron microscopy, tablet hardness and disintegration testing. KEY FINDINGS: The results showed that MCC demonstrated its best flowability at a moisture content of 11.2% w/w when compared to control, comprising of 3.9% w/w moisture. The use of the composite powder coating process (without air) resulted in up to 80% increase in tablet hardness, when compared to the control. The study also demonstrated that surface adsorbed moisture can be displaced upon addition of excipients during dry processing circumventing the need for particle drying before tabletting. CONCLUSIONS: It was concluded that MCC with a moisture content of 11% w/w provides a good balance between powder flowability and favourable ODT characteristics.

In-situ examination of the selective etching of an alkanethiol monolayer covered Au{111} surface

An examination of the selective etching mechanism of a 1-alkanethiol self-assembled monolayer (SAM) covered Au{111} surface using in-situ atomic force microscopy (AFM) and molecular resolution scanning tunnelling microscopy (STM) is presented. The monolayer self-assembles on a smooth Au{111} surface and typically contains nanoscale non-uniformities such as pinholes, domain boundaries and monatomic depressions. During etching in a ferri/ferrocyanide water-based etchant, selective and preferential etching occurs at SAM covered Au(111) terrace and step edges where a lower SAM packing density is observed, resulting in triangular islands being relieved. The triangular islands are commensurate with the Au(111) lattice with their long edges parallel to its [11-0] direction. Thus, SAM etching is selective and preferential attack is localized to defects and step edges at sites of high molecular density contrast.

An investigation by AFM and TEM of the mechanism of anodic formation of nanoporosity in n-InP in KOH

The early stages of nanoporous layer formation, under anodic conditions in the absence of light, were investigated for n-type InP with a carrier concentration of ∼3× 1018 cm-3 in 5 mol dm-3 KOH and a mechanism for the process is proposed. At potentials less than ∼0.35 V, spectroscopic ellipsometry and transmission electron microscopy (TEM) showed a thin oxide film on the surface. Atomic force microscopy (AFM) of electrode surfaces showed no pitting below ∼0.35 V but clearly showed etch pit formation in the range 0.4-0.53 V. The density of surface pits increased with time in both linear potential sweep and constant potential reaching a constant value at a time corresponding approximately to the current peak in linear sweep voltammograms and current-time curves at constant potential. TEM clearly showed individual nanoporous domains separated from the surface by a dense ∼40 nm InP layer. It is concluded that each domain develops as a result of directionally preferential pore propagation from an individual surface pit which forms a channel through this near-surface layer. As they grow larger, domains meet, and the merging of multiple domains eventually leads to a continuous nanoporous sub-surface region.

Nanoporous InP: anodic formation and growth mechanism in aqueous electrolytes

Porous layers can be formed electrochemically on (100) oriented n-InP substrates in aqueous KOH. A nanoporous layer is obtained underneath a dense near-surface layer and the pores appear to propagate from holes through the near-surface layer. In the early stages of the anodization transmission electron microscopy (TEM) clearly shows individual porous domains that appear to have a square-based pyramidal shape. Each domain appears to develop from an individual surface pit which forms a channel through this near-surface layer. We suggest that the pyramidal structure arises as a result of preferential pore propagation along the <100> directions. AFM measurements show that the density of surface pits increases with time. Each of these pits acts as a source for a pyramidal porous domain. When the domains grow, the current density increases correspondingly. Eventually the domains meet, forming a continuous porous layer, the interface between the porous and bulk InP becomes relatively flat and its total effective surface area decreases resulting in a decrease in the current density. Current-time curves at constant potential exhibit a peak and porous layers are observed to form beneath the electrode surface. The density of pits formed on the surface increases with time and approaches a plateau value. Porous layers are also observed in highly doped InP but are not observed in wafers with doping densities below ~5 × 1017 cm-3. Numerical models of this process have been developed invoking a mechanism of directional selectivity of pore growth preferentially along the <100> lattice directions. Manipulation of the parameters controlling these curves shows that the fall-off in current is controlled by the rate of diffusion of electrolyte through the pore structure with the final decline in current being caused by the termination of growth at the pore tips through the formation of passivating films or some other irreversible modification of the pore tips.

The nature of alkanethiol self-assembled monolayer adsorption on sputtered gold substrates

A detailed study of the self-assembly and coverage by 1-nonanethiol of sputtered Au surfaces using molecular resolution atomic force microscopy (AFM) and scanning tunneling microscopy (STM) is presented. The monolayer self-assembles on a smooth Au surface composed predominantly of {111} oriented grains. The domains of the alkanethiol monolayer are observed with sizes typically of 5-25 nm, and multiple molecular domains can exist within one Au grain. STM imaging shows that the (4 × 2) superlattice structure is observed as a (3 × 2√3) structure when imaged under noncontact AFM conditions. The 1-nonanethiol molecules reside in the threefold hollow sites of the Au{111} lattice and aligned along its lattice vectors. The self-assembled monolayer (SAM) contains many nonuniformities such as pinholes, domain boundaries, and monatomic depressions which are present in the Au surface prior to SAM adsorption. The detailed observations demonstrate limitations to the application of 1-nonanethiol as a resist in atomic nanolithography experiments to feature sizes of ∼20 nm.