In vitro biological performance of nano-particles on the surface of hydroxyapatite coatings

The biocompatibility of a kind of heat-treated bilayer hydroxyapatite (HA) coatings with nano-particles was investigated, mainly in terms of the immersion in simulated body fluid (SBF) and osteoblast adhesion. Scanning electron microscopy (SEM) was used to observe the morphology of coatings and cellular adhesion. The phases present in the coatings were determined by X-ray diffraction (XRD). Calcium ion (Ca²⁺) concentration in SBF was measured by Atomic absorption spectrophotometer. The results show nano-HA heat-treated at 650 °C for 0.5 h (BBCs) is comparatively stable during immersion in SBF and favor of the adhesion of osteoblasts. Cellular filopodia adhere firmly to the nano-particles and stretch in various direction.     

On the influence of the surface roughness onto the ultrathin SiO2/Si structure properties

The surface roughness of the semiconductor substrate substantially influences properties of the whole semiconductor/oxide structure. SiO₂/Si structures were prepared by using low temperature nitric acid oxidation of silicon (NAOS) method and then the whole structure was passivated by the cyanidization procedure. The influence of the surface morphology of the silicon substrate onto the electrical properties of ultrathin NAOS SiO₂ layer was investigated. Surface height function properties were studied by the AFM method and electrical properties were studied by the STM method. The complexity of analyzed surface structure was sensitive to the oxidation and passivation steps. For describing changes in the oxide layer structure, several fractal measures in an analysis of the STM images were used. This fractal geometry approach enables quantifying the fine spatial changes in the tunneling current spectra.     

Surface characteristics and in vitro biocompatibility of a manganese-containing titanium oxide surface

This study investigated the surface characteristics and in vitro biocompatibility of a titanium (Ti) oxide layer incorporating the manganese ions (Mn) obtained by hydrothermal treatment with the expectation of utilizing potent integrin-ligand binding enhancement effect of Mn for future applications as an endosseous implant surface. The surface characteristics were evaluated by scanning electron microscopy, thin-film X-ray diffractometry, X-ray photoelectron spectroscopy, optical profilometry and inductively coupled plasma-atomic emission spectroscopy (ICP-AES). The in vitro biocompatibility of the Mn-containing Ti oxide surface was evaluated in comparison with untreated bare Ti using a mouse calvaria-derived osteoblastic cell line (MC3T3-E1). The hydrothermal treatment produced a nanostructured Mn-incorporated Ti oxide layer approximately 0.6 μm thick. ICP-AES analysis demonstrated that the Mn ions were released from the hydrothermally treated surface into the solution. Mn incorporation notably decreased cellular attachment, spreading, proliferation, alkaline phosphatase activity, and osteoblast phenotype gene expression compared with the bare Ti surface (p < 0.05). The results indicate that the Mn-incorporation into the surface Ti oxide layer has no evident beneficial effects on osteoblastic cell function, but instead, actually impaired cell behavior.     

Study on the surface bioactivity of novel magnetic A-W glass ceramic in vitro

Novel magnetic A-W glass ceramic (M GC) in the system MgO-CaO-SiO₂-P₂O₅-CaF₂-MnO-ZnO-Fe₂O₃ was synthesized by doping Mn-Zn ferrite to apatite-wollastonite glass ceramic. The phase composition was investigated by XRD. The magnetic property was measured by VSM. The in vitro bioactivity was tested by immersion in simulated body fluid. The result shows apatite, wollastonite, fluorapatite and Zn_0.75Mn_0.75Fe_1.5O₄ are the main phases of M GC. Under a magnetic field of 10,000 Oe, the saturation magnetization and coercive force of the material are 6 emu g⁻ and 180 Oe, respectively. After soaking in SBF for 14 days, the surface of M GC is coated by a hydroxycarbonate apatite layer.     

Superhydrophobic properties of silver-coated films on copper surface by galvanic exchange reaction

Hydrophobic properties of thin nanostructured silver films produced by galvanic exchange reaction on a copper surface were studied after passivation with stearic acid. The morphology of the silver films was controlled by varying the concentration of silver nitrate in the solution. Water contact angle as high as 156° and contact angle hysteresis as low as 5° were achieved for samples obtained with initial silver ion concentration of 24.75 mM in the solution. However, a strong dependence of contact angle and contact angle hysteresis on the fractal-like morphology of the silver films was observed with the variation of silver ion concentration.     

Influence of surface topography and pore architecture of alkali-treated titanium on in vitro apatite deposition

Alkali-treated titanium surfaces have earlier shown to induce bone-like apatite deposition. In the present study, the effect of surface topography of two-dimensional and pore architecture of three-dimensional alkali-treated titanium substrates on the in vitro bioactivity was investigated. Titanium plates with a surface roughness of R_a = 0.13 μm, 0.56 μm, 0.83 μm, and 3.63 μm were prepared by Al₂O₃ grit-blasting. Simple tetragonal and face-centered Ti6Al4V scaffolds with spatial gaps of 450-1100 μm and 200-700 μm, respectively, were fabricated by a three-dimensional fiber deposition (3DFD) technique. After alkali treatment, the titanium plates with a surface roughness of R_a = 0.56 μm were completely covered with hydroxyapatite globules after 7 days in simulated body fluid (SBF), while the coverage of the samples with other surface roughness values remained incomplete. Similarly, face-centered Ti₆Al₄ scaffolds with spatial gaps of 200-700 μm exhibited a full surface coverage after 21 days in SBF, while simple tetragonal scaffolds with spatial gaps of 450-1100 μm were only covered for 45-65%. This indicates the importance of surface topography and pore architecture for in vitro bioactivity.     

Investigation into defects occurring on the polymer surface during the photolithography process

With a view to improving the realisation of polymer optical waveguide some features relevant to the photolithography process are analysed. This paper focuses on defects that occur on the surface of polymer layers involved in the process. For example, depending on the heat treatment or the deposited material, some worm-like defects appear on the polymer surface. When they occur, the waveguide surface roughness becomes too high (about one hundred nm and more). This means that the optical performance of the waveguides is too poor. In this document, we show the changes in temperature on polymer film surfaces which are coated with a thin inorganic layer and the occurrence of these defects is observed. This work confirms that the defect occurrence is clearly linked to the glass transition temperature. The paper reports that, in some cases, the adjustment of thermal properties by annealing can advantageously shift the glass transition, without changing the target optical properties.     

Influence of surface roughness and contact load on friction coefficient and scratch behavior of thermoplastic olefins

To study the effects of surface roughness and contact load on the friction behavior and scratch resistance of polymers, a set of model thermoplastic olefins (TPO) systems with various surface roughness (R_a) levels were prepared and evaluated. It is found that a higher R_a corresponds to a lower surface friction coefficient (μ_s). At each level of R_a, μ_s gets larger as contact load increases, with a greater increase in μ_s as R_a level increases. It is also observed that with increasing contact load and increasing R_a, the μ_s tend to level off. In evaluating TPO scratch resistance, a lower μ_s would delay the onset of ductile drawing-induced fish-scale surface deformation feature, thereby raising the load required to cause scratch visibility. However, as the contact load is further increased, the μ_s evolves to become scratch coefficient of friction (SCOF) as significant sub-surface deformation and tip penetration occur and material displacement begins, i.e., ploughing. No dependence of R_a and μ_s on the critical load for the onset of ploughing is observed. In this work, the distinction between μ_s and SCOF will be illustrated. Approaches for improving scratch resistance of polymers via control of R_a are also discussed.     

Comparison of fractal analyses methods and fractal dimension for pre-treated stainless steel surfaces and the correlation to adhesive joint strength

The fractal dimensions of six differently mechanically pre-treated stainless steel samples were investigated using five fractal algorithms. The surfaces were analyzed using a profiler, atomic force microscopy (AFM), scanning electron microscopy (SEM) and light microscopy (LM), and thereafter adhesively bonded and tested in single-overlap joints to test their tensile strength. All samples showed different fractal behavior, depending on the microscopic methods and fractal algorithms. However, the overall relation between fractal dimension and tensile strength is qualitatively the same, except for the SEM images. This verifies that tensile strength is correlated to fractal dimension, although only within the length-scale of the profiler and the light microscope (≈0.5–100 μm). The AFM method was excluded in this comparison, since the limitation in the z-direction for the AFM scanner made it difficult to scan the rougher parts of the blasted samples. The magnitude of the surfaces is a parameter not often considered in fractal analysis. It is shown that the magnitude, for the Fourier method, is correlated to the arithmetic average difference, R_a, but only weakly to the fractal dimension. Hence, traditional parameters, such as R_a, tell us very little about the spatial distribution of the elevation data. Received: 22 December 1999 / Accepted: 9 October 2000 / Published online: 9 February 2001     

AFM lateral force imagining of modified polychloroprene: A study based on roughness analysis

Films of a binary polymer blends comprising polychloroprene (PCP) and piperylene-styrene copolymer (PSC) have been prepared by solution casting. The dependence of the surface morphology of the free blend films on PSC content was studied with both roughness and correlation analysis of lateral force microscopy (LFM) images. Significant changes in roughness and lateral parameter values of different blend film sides have been observed depending on the blend composition. It was shown that up to 15 wt.% PSC is distributed continuously in PCP bulk. The increase of roughness and lateral parameter values at the air/film surface shows the enrichment of PCP in the blends containing 25 wt.% or more PSC. The enrichment of PCP on the air/film surface favours the increase of PSC concentration at the backing/film surface. The films underside morphology becomes similar to that of PSC, when its content reaches 40 wt.%.     

Improvement of surface porosity and properties of alumina films by incorporation of Fe micrograins in micro-arc oxidation

Micro-arc oxidation (MAO) is an effective approach to improve the properties of aluminum and its alloy by forming ceramic films on the surface. However, the oxide layers often have a porous surface structure, which exhibits relatively high friction coefficients. In this work, in order to enhance the surface and mechanical properties of the films produced by micro-arc oxidation, Al₂O₃ coatings embedded with Fe micrograins of different thicknesses were produced on aluminum alloys by adding Fe micrograins into the electrolyte during MAO. Compared to the Al₂O₃ coatings without Fe micrograins, the MAO Al₂O₃ coatings with Fe micrograins are much denser and harder, and the wear resistance is also improved significantly. The enhancement can be attributed to the enhancement of the surface structure and morphology of the MAO Al₂O₃ coatings with embedded Fe micrograins.     

A Model for the Contact Angle of Liquid Droplets on Rough Surfaces

Up to now, measured results of the contact angle on rough surfaces have been explained usually based on the Wenzel equation （1936） and the Cassie-Baxter equation （1944）. However, these equations do not take into account considerations of liquid wetting behaviors on rough surfaces, and this leads to poor understanding of the mechanisms of contact between liquid droplets and rough surfaces （e.g. contact angle hysteresis）. We propose a new model for the contact angle of liquid droplets. By means of the present model, we can well understand the evperimental data which could not be well explained by the Wenzel equation and the Cassie-Baxter equation.     

Direct experimental confirmation of the critical behaviour of antiphase domain boundaries at the second order phase transition of Al-Fe binary alloys

The present work reports, for the first time, a direct experimental observation of the critical phenomenon associated with the B2-A2 order-disorder transition of Al-Fe binary alloys. Transmission electron microscopy and energy dispersion spectroscopy are employed to span the morphological changes through the transition line from the ordered B2 phase to the disordered A2 phase. Dark field images of the microstructure around the transition line for samples aged at 973 and 1073 K for various times show an interface roughening for the {100} antiphase domain boundaries in body-centered cubic binary alloys having the B2 structure. This observation confirms theory about the instability of the second-order transition in such alloys. This behaviour occurs for compositions with Al-content slightly higher (by ∼4 at.% Al) than that of the critical point of the equilibrium order-disorder transition. In addition, roughness-induced wetting transition is also observed for alloys having compositions ranging from 1.3 to 1.5 at.% Al above the transition line. The interface roughening transition is thought to be unstable second-order while the wetting transition is suggested to be a stable first-order one.     

Structure and morphology of Cu/Ni film grown by electrodeposition method: A study of neutron reflectivity and AFM

We present detailed study of structure and interface morphology of an electrodeposited Cu/Ni film using X-ray diffraction, X-ray reflectivity, neutron reflectivity and atomic force microscopy (AFM) techniques. The crystalline structure of the film has been determined by X-ray diffraction, which suggest polycrystalline growth of the film. The depth profile of density in the sample has been obtained from specular X-ray and neutron reflectivity measurements. AFM image of the air-film interface shows that the surface is covered by globular islands of different sizes. The AFM height distribution of the surface clearly shows two peaks and the relief structure (islands) on the surface in the film, which can be treated as a quasi-two-level random rough surface structure. We have demonstrated that the detailed morphology of air-film interfaces, the quasi-two-level surface structure as well as morphology of the buried interfaces can be obtained from off-specular neutron reflectivity data. AFM and off-specular neutron reflectivity measurements also show that the morphologies of electrodeposited surface is distinctively different as compared to that of sputter-deposited surfaces in the sample.     

Bottom and top AF/FM interfaces of NiFe/FeMn/NiFe trilayers

X-ray reflectivity analyses were performed in the Si/WTi (7 nm)/NiFe (30 nm)/FeMn (13 nm)/NiFe (10 nm)/WTi (7 nm) exchange-biased system prepared by magnetron sputtering under three different argon working pressures. Layer-by-layer analyses were realized in order to obtain the interfacial roughness parameters quantitatively. For a fixed argon pressure, the root-mean-square roughness (including the atomic grading) of the upper (FeMn/NiFe) interface are greater than that for the lower one in all studied samples. Argon working pressure also has severe influence over the NiFe/FeMn interfaces, being more pronounced at the upper interfaces.     

Preparation and in vitro characterization of aerosol-deposited hydroxyapatite coatings with different surface roughnesses

Hydroxyapatite (HA) coatings with different surface roughnesses were deposited on a Ti substrate via aerosol deposition (AD). The effect of the surface roughness on the cellular response to the coating was investigated. The surface roughness was controlled by manipulating the particle size distribution of the raw powder used for deposition and by varying the coating thickness. The coatings obtained from the 1100 °C-heated powder exhibited relatively smooth surfaces, whereas those fabricated using the 1050 °C-heated powder had network-structured rough surfaces with large surface areas and were superior in terms of their adhesion strengths and in vitro cell responses. The surface roughness (R_a) values of the coatings fabricated using the 1050 °C-heated powder increased from approximately 0.65 to 1.03 μm as the coating thickness increased to 10 μm. The coatings with a rough surface had good adhesion to the Ti substrate, exhibiting high adhesion strengths ranging from 37.6 to 29.5 MPa, depending on the coating thickness. The optimum biological performance was observed for the 5 μm-thick HA coating with an intermediate surface roughness value of 0.82 μm.     

Ni thin films vacuum-evaporated on polyethylene naphthalate substrates with and without the application of magnetic field

We study the structural properties of the surface roughness, the surface mound size and the interfacial structure in Ni thin films vacuum-deposited on polyethylene naphthalate (PEN) organic substrates with and without the application of magnetic field and discuss its feasibility of fabricating quantum cross (QC) devices. For Ni/PEN evaporated without the magnetic field, the surface roughness decreases from 1.3 nm to 0.69 nm and the surface mound size increases from 32 nm to 80 nm with the thickness increased to 41 nm. In contrast, for Ni/PEN evaporated in the magnetic field of 360 Oe, the surface roughness tends to slightly decrease from 1.3 nm to 1.1 nm and the surface mound size shows the almost constant value of 28-30 nm with the thickness increased to 35 nm. It can be also confirmed for each sample that there is no diffusion of Ni into the PEN layer, resulting in clear Ni/PEN interface and smooth Ni surface. Therefore, these experimental results indicate that Ni/PEN films can be expected as metal/insulator hybrid materials in QC devices, leading to novel high-density memory devices.     

Combinatorial investigation of nanostructures formed in a titanium dioxide based nanocomposite film on top of fluor‐doped tin oxide layers

Nanostructures formed in a titanium dioxide (TiO₂)–poly(styrene)‐block‐poly(ethyleneoxide) nanocomposite film on top of fluor‐doped tin oxide (FTO) layers are investigated. The combinatorial approach is based on probing a wedge‐shaped FTO‐gradient with grazing incidence small angle X‐ray scattering (GISAXS) in combination with a moderate micro‐focus X‐ray beam. The characteristic lateral length is given by adjacent nanowire‐shaped TiO₂ regions. It decreases from 200 nm on the thick FTO layer to 90 nm on the bare glass surface.

     

Swift ion irradiations of Fe/Fe/Si trilayers

We report here on changes in magnetism and microstructure when implanting, at 92 or 300 K, up to 5 × 10¹⁵ Au²⁶⁺-ions cm⁻² of 350 MeV into ^natFe(45 nm)/⁵⁷Fe(20 nm)/Si trilayers. This choice of ions and energy allowed to test the irradiation effects in the regime of pure electronic stopping. The samples were analysed before and after irradiation by Rutherford back-scattering spectroscopy, X-ray diffraction, conversion electron Mössbauer spectroscopy, and magneto-optical Kerr effect. Up to 1 × 10¹⁵ ions cm⁻², there was interface broadening at a mixing rate of Δσ²/Φ = 55(5) nm⁴, followed by full Fe-Si inter-diffusion. The Mössbauer spectra revealed fractions of α-Fe and amorphous ferromagnetic and paramagnetic iron silicides, but no crystalline Fe-Si phase. The magnetic remanence in the as-deposited Fe-layer showed small components of uniaxial and four-fold magnetization. For increasing ion fluence, the component with four-fold symmetry grew at the expense of the uniaxial component. For the highest fluences, an isotropic magnetization was found.     

Investigation of the running-in process and friction coefficient under the lubrication of ionic liquid/water mixture

The tribological properties of three different films commonly used in microelectromechanical systems (MEMS) under the lubrication of ionic liquid (IL)/water mixtures with various concentrations in the running-in process have been investigated. Results show that coefficients of friction (COFs) and wear rates for low temperature silicon oxide (LTO)/Si₃N₄ vary in a similar way to the ones for poly-Si/Si₃N₄ under the lubrications of different IL/water mixtures. In contrast, the differences in COFs and wear rates are more significant in that the COFs and wear rates increase dramatically with the decrease in IL/water concentration in the case of self-mated Si₃N₄, while the differences in COFs and wear rates for the two other tribopairs are relatively small when the concentration is changed. The period of the running-in process reduces with the increase in IL/water concentration for all the tribopairs. Effective hydrodynamic lubrication can be found in the case of Si₃N₄/Si₃N₄ tribopair at higher IL/water concentrations without an evident running-in process, however, such a phenomenon cannot be observed for the other two tribopairs. Different wear mechanisms will also be analyzed in this paper.