Unambiguous identification of the measurement methodologies is fundamental to reduce the uncertainty and support traceability of particle shape and size at the nanoscale. In this work, the critical aspects in atomic force microscopy measurements, that is, drawbacks on sample preparation, instrumental parameters, image pre-processing, size reconstruction, and tip enlargement, are discussed in reference to quantitative dimensional measurements on different kinds of nanoparticles (inorganic and biological) with different shapes (spherical, cylindrical, complex geometry). Once the cross-section profile is extracted, top-height measurements on isolated nanoparticles of any shape can be achieved with sub-nanometer accuracy. Lateral resolution is affected by the pixel size and shape of the probe, causing dilation in the atomic force microscopy image. For the reconstruction of critical sizes of inorganic non-spherical nanoparticles, a geometric approach that considers the nominal shape because of the synthesis conditions is presented and discussed.
Accurate measurements of line-width standards, sidewalls and non-spherical nanoparticles performed at the nanoscale by means of atomic force microscopy (AFM) suffer from errors due to the tip shape and size. To reduce the uncertainty, the study here presented aims to investigate a bio-plant nanostructure, namely the tobacco mosaic virus (TMV), as a candidate reference tip characterizer. The TMV has a rod-shaped structure with a diameter of about 18 nm, reported earlier from x-ray fibre diffraction, thus representing a reference at the nanoscale. When imaged by AFM, the diameter of the TMV is determined as the top height of the rod from the reconstructed cross-section profile of isolated virions, deposited on a flat substrate like mica. A mean diameter of 16.5 nm, smaller than the nominal value by fibre diffraction measurements, is determined with our metrological AFM. Meanwhile, tip–sample–substrate interactions are discussed with reference to experimental data and models in the literature, in order to determine deformations and the associated uncertainty of corrections, with which the difference between the AFM-reconstructed top-height diameter and the nominal value reduces to about 0.3 nm. Once the virus is fully characterized, a tip profile is estimated by the AFM-reconstructed cross-section profiles of the TMV. The approach is used to evaluate the tip-related enlargement from the nominal circle size, assumed undeformed, of the TMV cross-section profile. A good repeatability of the reconstructed tip shape is achieved from subsequent imaging of virions, while tip degradations are somewhat visible over the working time.
Cu-based nanomaterials have received considerable attention as promising and cost-effective substrates for surface-enhanced Raman spectroscopy (SERS) applications despite their relatively low enhancement factor (EF) compared to noble metals like gold and silver. In this study, a fast and affordable synthesis route is proposed to obtain a three-dimensional porous copper film (NPC) via an electrodeposition technique based on the dynamic hydrogen bubbling template (DHBT). Two sets of NPC film were synthesized, one without additives and the other with cetyltrimethylammonium bromide (CTAB). The impacts of deposition time on the NPCs’ porous morphology, thickness, and SERS performance were systematically investigated. With the optimal deposition time, the nanopore sizes could be tailored from 26.8 to 73 μm without additives and from 12.8 to 24 µm in the presence of CTAB. The optimal additive-free NPC film demonstrated excellent SERS performance at 180 s of deposition, while the CTAB-modified film showed strong enhancement at 120 s towards methylene blue (MB), a highly toxic dye, achieving a detection limit of 10−6 M. Additionally, the samples with CTAB showed better efficiency than those without CTAB. The calculated EF of NPC was found to be 5.9 × 103 without CTAB and 2.5 × 103 with the CTAB, indicating the potential of NPC as a cost-effective candidate for high-performance SERS substrates. This comprehensive study provides insights into optimizing the structural morphology of the NPCs to maximize their SERS enhancement factor and improve their detection sensitivity toward MB, thus overcoming the limitations associated with conventional copper-based SERS substrates.
The improvement of the mucosal sealing around the implant represents a challenge, one that prompted research into novel materials. To this purpose, a printable poly(ε-caprolactone) (PCL)-based composite loaded with alumina-toughened zirconia (ATZ) at increasing rates of 10, 20, and 40 wt.% was prepared, using a solvent casting method with chloroform. Disks were produced by 3D printing; surface roughness, free energy and optical contact angle were measured. Oral fibroblasts (PF) and epithelial cell (SG) tests were utilized to determine the biocompatibility of the materials through cell viability assay and adhesion and spreading evaluations. The highest level of ATZ resulted in an increase in the average roughness (Sa), while the maximum height (Sz) was higher for all composites than that of the unmixed PCL, regardless of their ATZ content. Surface free energy was significantly lower on PCL/ATZ 80/20 and PCL/ATZ 60/40, compared to PCL and PCL/ATZ 90/10. The contact angle was inversely related to the quantity of ATZ in the material. PF grew without variations among the different specimens at 1 and 3 days. After 7 days, PF grew significantly less on PCL/ATZ 60/40 and PCL/ATZ 80/20 compared to unmixed PCL and PCL 90/10. Conversely, ATZ affected and improved the growth of SG. By increasing the filler amount, PF cell adhesion and spreading augmented, while PCL/ATZ 80/20 was the best for SG adhesion. Overall, PCL/ATZ 80/20 emerged as the best composite for both cell types; hence, it is a promising candidate for the manufacture of custom made transmucosal dental implant components.
16 May 2018 in Surface Topography: Metrology and Properties
Nowadays the development in photovoltaic (PV) cells manufacturing requires increasingly sophisticated technologies, and in order to avoid efficiency losses in PV cell, printing techniques of the front contacts have to be well controlled. To this purpose, printed linear conductors (PLCs) on a PV standard cell are characterized by morphology- and resistance-based measurements, creating a well-calibrated test structure towards the development of an application-oriented material measure. It can be noticed that morphology and texture parameters determined by stylus and optical profilers are well in agreement, and the resistance calculated from the reconstructed cross-section area matches quite well the measured resistance of fingers. Uncertainties of about 14% to 17% are estimated for local measurements of morphology-based and measured resistance of finger segments up to 5 mm length. Fingers characterized by somewhat larger roughness/waviness values ( , , ) show some local irregularities, which may degrade the electrical contact of the PV front surface.