Microstructure fabrication with a CO2 laser system: characterization and fabrication of cavities produced by raster scanning of the laser beam

In this paper we describe the use of a CO(2) laser for production of cavities and microstructures in poly(methyl methacrylate) (PMMA) by moving the laser beam over the PMMA surface in a raster pattern. The topography of the cavities thus produced is studied using stylus and optical profilometry and scanning electron microscopy (SEM). The microstructures display artifacts from the laser ablation process and we describe how the laser ablation parameters can be optimized in order to minimize these artifacts. Using this technique it is possible to generate structures with a depth from 50 microm and a minimum width of approximately 200 microm up to depth and widths of several mm, governed by the beam size and the laser settings.     

Control of surface topography in biomimetic calcium phosphate coatings

The behavior of cells responsible for bone formation, osseointegration, and bone bonding in vivo are governed by both the surface chemistry and topography of scaffold matrices. Bone-like apatite coatings represent a promising method to improve the osteoconductivity and bonding of synthetic scaffold materials to mineralized tissues for regenerative procedures in orthopedics and dentistry. Polycaprolactone (PCL) films were coated with calcium phosphates (CaP) by incubation in simulated body fluid (SBF). We investigated the effect of SBF ion concentration and soaking time on the surface properties of the resulting apatite coatings. CaP coatings were examined by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectrometry (FTIR), and energy dispersive X-ray spectrometry (EDX). Young's modulus (E(s)) was determined by nanoindentation, and surface roughness was assessed by atomic force microscopy (AFM) and mechanical stylus profilometry. CaP such as carbonate-substituted apatite were deposited onto PCL films. SEM and AFM images of the apatite coatings revealed an increase in topographical complexity and surface roughness with increasing ion concentration of SBF solutions. Young's moduli (E(s)) of various CaP coatings were not significantly different, regardless of the CaP phase or surface roughness. Thus, SBF with high ion concentrations may be used to coat synthetic polymers with CaP layers of different surface topography and roughness to improve the osteoconductivity and bone-bonding ability of the scaffold.     

Observation of ground surface roughness values obtained by stylus profilometer and white light interferometer for common metal materials

To find some practical understandings and to derive some rules for roughness calibration for common metal materials, this paper counts surface roughness on 50 ground workpieces of five different materials obtained by a stylus profilometer (here-in-after, ‘SP’) and a white light interferometer (here-in-after, ‘WLI’). The materials include iron, stainless steel, 45 steel, copper and aluminium on which hardness values are widely ranged. The results show that SP measurement result is generally smaller than WLI measurement result for its stylus tip size and scratches on surface. The SP method has obvious scratches on soft materials (Al and Cu), which leads to the reduction of low spatial frequency information on the measured profile. WLI measurement result is more accurate when measured surface is smooth while SP is more suitable for rough and hard surface roughness measurement.     

Scanning white-light interferometry as a novel technique to quantify the surface roughness of micron-sized particles for inhalation

A novel approach of measuring the surface roughness of spherical and flat micron-sized drug particles using scanning white-light interferometry was applied to investigate the surface morphology of micron-sized active pharmaceutical ingredients (APIs) and excipient particles used for inhalation aerosols. Bovine serum albumin (BSA) and alpha-lactose monohydrate particles were chosen as model API and excipient particles, respectively. Both BSA and lactose particles were prepared with different degrees of surface corrugation using either controlled spray drying (four samples of BSA) or decantation (two samples of lactose). Particle size distributions were characterized by laser diffraction, and particles were imaged by scanning electron microscopy (SEM). Surface roughness of the BSA and lactose particles was quantified by white-light optical profilometry using vertical scanning interferometry (VSI) at full resolution using a 50x objective lens with 2.0x and 0.5x fields of view for BSA and lactose, respectively. Data were analyzed using Vision software (version 32, WYKO), and surface roughness values are expressed as root-mean-square roughness ( Rrms). Furthermore, data were compared to topographical measurements made using conventional atomic force microscopy. Analysis of the optical profilometry data showed significant variation in BSA roughness ranging from 18.58 +/- 3.80 nm to 110.90 +/- 13.16 nm for the smoothest and roughest BSA particles, respectively, and from 81.20 +/- 15.90 nm to 229.20 +/- 68.20 nm for decanted and normal lactose, respectively. The Rrms values were in good agreement with the AFM-derived values. The particle morphology was similar to SEM and AFM images. In conclusion, scanning white-light interferometry provides a useful complementary tool for rapid evaluation of surface morphology and roughness in particles used for dry powder inhalation formulation.     

Efficient eco-friendly approach towards bimetallic nanoparticles synthesis and characterization using Exiguobacterium aestuarii by statistical optimization

ABSTRACT

Biogenic synthesis of bimetallic nanoparticles (gold – AuNp and selenium – SeNp) using inexpensive Tryptophan Enriched Banana Peel Media for the growth of marine isolate (Exiguobacterium aestuarii SBG4 MH185868). The response surface methodology is employed for optimizing production conditions. The surface plasmon resonance band showed λ_max at 540?nm (AuNp) and 284?nm (SeNp). FTIR and zeta potential analysis confirmed the stability, whereas XRD spectra revealed the nature of nanoparticles obtained at optimum conditions. SEM micrographs showed nanospheres of the following size: AuN, 30?±?5 nm and SeNp, 50?±?5 nm. Biocompatibility of Np evaluated by the hemolytic activity showed <20% hemolysis even at highest concentrations (100?µg/ml). AuNp showed the least cytotoxicity, whereas SeNp showed considerable cytotoxicity against the breast cancer cell lines MCF – 7 and MDA-MB-231. Hence, we utilized the environment-friendly growth media for the controlled synthesis of dual Np using single bacterial strain involving feasible steps in downstream processing.     

溶胶处理对硅灰石表面性质的影响

本工作用锡和锌两种溶胶对硅灰石进行表面处理。用酸碱测定、X-射线光电子能谱(XPS)、傅里叶变换红外光谱(FT-IR)、粒度分析、比表面测定和扫描电子显微分析(SEM)等方法研究了溶胶处理对硅灰石表面化学性质和物理性质的影响情况。结果表明经过溶胶处理,锡或锌是以氧化物的形式包覆在硅灰石的表面,使得硅灰石的表面组成、形貌和酸碱性都发生了变化。     

Summary of ISO/TC 201 Standard: X ISO 17560:2002—Surface chemical analysis—Secondary ion mass spectrometry—Method for depth profiling of boron in silicon

This International Standard specifies a secondary ion mass spectrometric method using magnetic‐sector or quadrupole mass spectrometers for depth profiling of boron in silicon, and using stylus profilometry or optical interferometry for depth calibration. This method is applicable to single‐crystal, polycrystal or amorphous silicon specimens with boron atomic concentrations between 1 × 10¹⁶ and 1 × 10²⁰ atoms cm^?3, and to the crater depth of 50 nm or deeper. Optical interferometry is generally applicable to crater depths in the range 0.5–5 µm. Copyright © 2004 John Wiley & Sons, Ltd.     

A novel dual surface modification on titanium in dental use: Characterization and topography

This laboratory study aimed to compare, contrast, and evaluate the effect of a novel dual surface modification method on the adhesion strength of resin composite cement to titanium. C.p.-2 grade titanium samples were silica-coated, etched with HNO₃(69vol %) or a blend of HCl (35vol %) and H₃PO₄ (85vol %), for 1 h at 80°C. Surface roughness was measured by surface roughness profilometry, topographic analysis by scanning electron microscopy (SEM), atomic force microscopy (AFM), and surface analyses by energy dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS). Silanization of all specimens was carried out after SEM, EDX, and AFM analysis, before enclosed mold microshear bond strength testing (EM-μSBS). Adhesion strengths were measured after artificial ageing: 1 day, 1 week, 4 weeks, and 8 weeks by EM-μSBS testing and failure mode analysis by optical microscopy. Polished titanium was used as a control. The highest surface roughness was observed in titanium samples treated with silica-coating + HCl-H₃PO₄ etching. The elemental composition confirmed the presence of Ti, O, C, with Si and Al in samples treated with silica-coating. A gradual decrease in EM-μSBS values was observed in all titanium samples with adhesive and cohesive failure modes. The novel dual surface modification method applied in this study suggests that silica-coating + HCl-H₃PO₄etching strongly affects titanium surface topography and roughness. The presence of Si on silica-coated surface modified titanium before silanization with an experimental silane has a positive effect on the EM-μSBS of titanium samples treated with silica-coating only or silica-coating + HNO₃ etching.     

Brownian dynamics simulations of polyelectrolyte adsorption onto topographically patterned surfaces

The effect of patterned surface topography on the adsorption of single polyelectrolyte molecules is explored using Brownian dynamics simulations. The polyelectrolyte is modeled as a free-draining, freely jointed bead-rod chain, and electrostatic interactions are incorporated using a screened Coulombic potential with excluded volume interactions accounted for by the repulsive part of a Lennard-Jones potential. Topography consisting of periodically spaced valleys of square cross section separated by flat hills is considered. Chain conformations are characterized for a wide range of valley widths, depths, and spacings as well as for several different types of surface charge distributions. Depending on the parameter values describing the topography, the chains are found to adopt conformations ranging from flat and extended to those associated with bridge-, brush-, or semi-bridge-like structures. The formation of these structures is rationalized on the basis of a free-energy model that takes into account the increase in free energy due to entropic confinement, excluded volume interactions, and chain stretching as well as the decrease in free energy due to bead-surface electrostatic attraction. The results of this work are expected to be useful in designing patterned surface topography to control the conformations of adsorbed polyelectrolyte molecules.     

Effect of the corona treatment and of the 1,4-cyclohexanedimethanol on the surface characteristics of the poly(ethylene terephthalate) film

Several techniques have been applied for the characterization of three PET films surfaces: homopolymer PET film, corona treated PET film and a poly(ethylene terephthalate-co-1,4-cyclohexanedimethanol) film. The objective of this work is to investigate and to apply precise and mutually complementary techniques which give detailled information about theses surfaces, as there are few papers with global and conclusive results. The film surfaces were investigated to support the development of new products and envisage new apllications to the existent films. Scanning electron micrographs, attenuated total reflection Fourier transform infrared spectroscopy (FTIR-ATR) and multiple internal reflection Fourier transform infrared spectroscopy (FTIR-MIR) spectra show that the chemical composition, topography and surface roughness of the films are different. The corona-treated PET film shows high surface tension value due to the major contribution on the polar groups and oxidation level acquired. The copolyester film is much less crystalline than the other films analyzed, as demonstrated by refractive index measurements and X-ray photoelectron spectroscopy (XPS). The amorphous structures obtained and the high tension level of the corona-treated films provide a better understanding of the adhesion phenomena. In view of results obtained, one can assume that corona treated films owing to its higher surface tension and films with CHDM owing to its surface amorphization should provide manufacturing industries better processing conditions than films without surface treatment and also higher levels of adhesion to paints and coatings.     

Preparation and characterization of novel polyimide‐silica hybrids

Polyimide‐silica (PI‐SiO₂) hybrids were prepared from a novel polyimide (PI), derived from pyromellitic dianhydride (PMDA), 1,6‐bis(4‐aminophenoxy)hexane (synthesized) and 4,4′‐oxydianiline. SiO₂ networks (5–30 wt%) were generated through sol–gel process using either tetraethylorthosilicate (TEOS) or a mixture of 3‐aminopropyltriethoxysilane‐PMDA‐based coupling oligomers (APA) and TEOS. Thin, free standing hybrid films were obtained from the respective mixtures by casting and curing processes. The hybrid films were characterized using Fourier transform infrared, ²⁹Si nuclear magnetic resonance (NMR), field emission scanning electron microscopy (FE‐SEM), energy dispersive X‐ray spectrometry and atomic force microscopy (AFM) techniques. ²⁹Si NMR results provide information about formation of organically modified silicate structures that were further substantiated by FE‐SEM and AFM micrographs. Contact angle measurements and thermogravimetric thermograms reveal that the addition of APA profoundly influences surface energy, interfacial tension, thermal stability and the residual char yield of modified hybrids in comparison to those obtained by mixing only TEOS. It was found that reduced particle size, efficient dispersion and improved interphase interactions were responsible for the eventual property enhancement. Copyright © 2012 John Wiley & Sons, Ltd.     

Measuring surface topography with scanning electron microscopy. I. EZEImage: a program to obtain 3D surface data.

Scanning electron microscopy (SEM) is widely used in the science of materials and different parameters were developed to characterize the surface roughness. In a previous work, we studied the surface topography with fractal dimension at low scale and two parameters at high scale by using the variogram, that is, variance vs. step log-log graph, of a SEM image. Those studies were carried out with the FERImage program, previously developed by us. To verify the previously accepted hypothesis by working with only an image, it is indispensable to have reliable three-dimensional (3D) surface data. In this work, a new program (EZEImage) to characterize 3D surface topography in SEM has been developed. It uses fast cross correlation and dynamic programming to obtain reliable dense height maps in a few seconds which can be displayed as an image where each gray level represents a height value. This image can be used for the FERImage program or any other software to obtain surface topography characteristics. EZEImage also generates anaglyph images as well as characterizes 3D surface topography by means of a parameter set to describe amplitude properties and three functional indices for characterizing bearing and fluid properties.     

Surface characterization of laser-treated poly(ethylene terephthalate) by optical profilometry and scanning tunneling microscopy

Characteristic changes in the surface topography due to UV laser treatment are of high significance for the determination of material destruction thresholds and surface structure development. E.g. irradiation of poly(ethylene terephthalate) (PET) film with pulsed UV laser light of 248 nm modifies the smoth surface of the polymer into a well oriented structured surface. The development of these structures were studied with scanning tunneling microscopy (STM) and high resolution optical profilometry. Three dimensional data of the surface were taken from the samples after each laser pulse. A change of topographic data was found in relation to fluence and number of pulses applied. © 1993 John Wilcy & Sons, Inc.     

Electron reflectivity from clean and oxidized steel surface

This paper aims to elucidate the effect of an air-formed native oxide covering mild steel surface on the contrast in the scanning electron microscopy (SEM) images obtained with the landing energy from 5 keV down to 0 eV. Part of the mild steel surface was in-situ cleaned by Ar⁺ ion sputtering process in order to remove native oxide from the surface. It enabled us to observe the oxide-free and the naturally oxidized area on the mild steel surface simultaneously in the SEM micrographs. Presence of the native oxide starts to play a role in the SEM images acquired at landing energy below roughly 3 keV. Contrast between differently oriented grains situated inside the area covered by the native oxide starts to be negligible with landing energy decreasing below 3 keV, up to some ultra-low values where the contrast increases again. Total reflectivity contrast between the clean and the oxidized area increases exponentially with landing energy decreasing below 3 keV. The reflectivity-versus-energy curves of the cleaned and the naturally oxidized mild steel surface are markedly different. The reflectivity of the electrons is correlated with the density of states (DOS), as is demonstrated at very low landing energies. Sensitivity of the very low-energy electrons to the electronic structure was verified by comparison of the experimental data with the simulations of reflectivities, band structure, and DOS. The theoretical predictions are based on the density-functional theory calculations and they have been performed in energy range corresponding to specular reflectivities of the Fe-BCC (001) orientation. We have also observed that close to the mirror condition, that is, near-zero landing energies, the primary electrons become sensitive to the surface potential differences caused by the work function differences of clean and native oxide-covered steel surfaces.     

Measuring surface topography by scanning electron microscopy. II. Analysis of three estimators of surface roughness in second dimension and third dimension.

Scanning electron microscopy (SEM) is widely used in surface studies and continuous efforts are carried out in the search of estimators of different surface characteristics. By using the variogram, we developed two of these estimators that were used to characterize the surface roughness from the SEM image texture. One of the estimators is related to the crossover between fractal region at low scale and the periodic region at high scale, whereas the other estimator characterizes the periodic region. In this work, a full study of these estimators and the fractal dimension in two dimensions (2D) and three dimensions (3D) was carried out for emery papers. We show that the obtained fractal dimension with only one image is good enough to characterize the roughness surface because its behavior is similar to those obtained with 3D height data. We show also that the estimator that indicates the crossover is related to the minimum cell size in 2D and to the average particle size in 3D. The other estimator has different values for the three studied emery papers in 2D but it does not have a clear meaning, and these values are similar for those studied samples in 3D. Nevertheless, it indicates the formation tendency of compound cells. The fractal dimension values from the variogram and from an area versus step log-log graph were studied with 3D data. Both methods yield different values corresponding to different information from the samples.     

Determination of the textural characteristics of carbon samples using scanning electronic microscopy images: comparison with mercury porosimetry data

In this paper, scanning electron microscopy (SEM) images of carbon samples were analysed, and some textural characteristics were obtained and compared with those determined using mercury porosimetry data. Fractal dimensions were calculated from both mercury porosimetry and SEM images as methods for characterising the porous distribution (heterogeneity) of the samples. Lacunarity is easily determined from SEM images as a measure of the degree of heterogeneity of a porous surface. A relationship between the lacunarity and the fractal dimensions calculated using both methods is shown. Pore-size distributions were also determined from the analysis of SEM images. We show that the analysis of SEM images is a valuable complement to mercury porosimetry measurements and a useful tool for the characterisation of porous surfaces. This method offers the possibility of evaluating the features of porous materials and comparing the results to those obtained using mercury intrusion analysis.     

A study of the surface analysis of some water‐soluble polymers by inverse gas chromatography

The surface characterization of 2‐(dimethylamino)ethylmethacrylate (DMA) and 2‐(N‐morpholino)ethylmethacrylate (MEMA) homopolymers and DMA–MEMA diblock copolymer was studied using inverse‐gas chromatography (IGC). The analyzed surface properties of (co)polymers were the dispersive component of the surface energy ( ) and the acid–base characters of (co)polymer surfaces. The specific free energy (ΔG^sp), enthalpy (ΔH^sp), and entropy (ΔS^sp) of adsorption of polar probes on (co)polymers were calculated. The values of ΔH^sp were correlated with both the donor and the modified acceptor numbers (AN) of the probes to quantify the acidic K_A and the basic K_D parameters of (co)polymer surfaces. The values obtained for the K_A and K_D parameters indicated basic characters for the surface of (co)polymers. The dispersive component values of the surface energy and the acid–base surface parameters of the DMA–MEMA diblock copolymer surface were found to be between those homopolymers as expected. Copyright © 2008 John Wiley & Sons, Ltd.     

Topographical properties of polymer films deposited in capillaries for electrophoretic separations of large organic molecules

Topography and thickness of hydrophilic polymer coatings of fused-silica capillaries for capillary electrophoresis (CE) were investigated using atomic force microscopy (AFM), scanning electron microscopy (SEM), and profilometry. Three hydrogels, poly(2-hydroxyethyl methacrylate) [poly(HEMA)], poly(diethylene glycol monomethacrylate) [poly(DEGMA)], and poly(triethylene glycol monomethacrylate) [poly(TEGMA)], were deposited using two procedures, either by simple physical sorption of the polymers, or by derivatization of the capillary wall surface with glycidyl methacrylate (EPMA) followed by polymerization of the appropriate monomers. The performance of the modified capillaries was tested under CE conditions (decrease in the electroosmotic flow, EOF dependence on pH, separation of milk and standard proteins). It has been found that the most important property of the polymer coating is its thickness, whereas its topography and the degree of its hydrophobicity are less significant. Film deposition by physical adsorption is preferable to polymerization on the derivatized surface.     

Study of prehispanic wall paintings from Xochicalco, Mexico, using PIXE, XRD, SEM and FTIR

The characterization of samples of painted plasters obtained from the archaeological site of Xochicalco, in Central Mexico, is presented. Elemental concentrations of the painted layers were obtained by using proton induced X-ray emission (PIXE). The main crystalline structures of the samples are identified with the help of X-ray diffraction (XRD), while the microstructure is studied by scanning electron microscopy (SEM). The information resulting from the application of these three techniques is used to achieve more accurate values for the elemental concentrations. Additional data regarding organic components of the paintings was obtained through Fourier transform infrared spectrometry (FTIR). Although the latter results only provided reliable data on inorganic components, they help to clarify the results from XRD and confirm those of SEM.