Bernard Haochih Liu

Focused-ion-beam-fabricated Au nanorods coupled with Ag nanoparticles used as surface-enhanced Raman scattering-active substrate for analyzing trace melamine constituents in solution

A well-ordered Au-nanorod array with a controlled tip ring diameter (Au_NRsd) was fabricated using the focused ion beam method. Au_NRsd was then coupled with Ag nanoparticles (Ag NPs) to bridge the gaps among Au nanorods. The effect of surface-enhanced Raman scattering (SERS) on Au_NRsd and Ag NPs/Au_NRsd was particularly verified using crystal violet (CV) as the molecular probe. Raman intensity obtained from a characteristic peak of CV on Au_NRsd was estimated by an enhancement factor of ≈10(7) in magnitude, which increased ≈10(12) in magnitude for that on Ag NPs/Au_NRsd. A highly SERS-active Ag NPs/Au_NRsd was furthermore applied for the detection of melamine (MEL) at very low concentrations. Raman-active peaks of MEL (10(-3) to 10(-12)M) in water or milk solution upon Au_NRsd or Ag NPs/Au_NRsd were well distinguished. The peaks at 680 and 702 cm(-1) for MEL molecules were found suitable to be used as the index for sensing low-concentration MEL in a varied solution, while that at 1051 cm(-1) was practical to interpret MEL molecules in water or milk solution bonded with Au (i.e., Au_NRsd) or Ag (i.e., Ag NPs/Au_NRsd) surface. At the interface of Ag NPs/Au_NRsd and MEL molecules in milk solution, a laser-induced electromagnetic field or hotspot effect was produced and competent to sense low-concentration MEL molecules interacting with Ag and Au surfaces. Accordingly, Ag NPs/Au_NRsd is very promising to be used as a fast and sensitive tool for screening MEL in complex matrices such as adulteration in e.g., food and pharmaceutical products.

In situ biosensing of the nanomechanical property and electrochemical spectroscopy of Streptococcus mutans-containing biofilms

This work presents in situ biosensing approaches to study the nanomechanical and electrochemical behaviour of Streptococcus mutans biofilms under different cultivation conditions and microenvironments. The surface characteristics and sub-surface electrochemistry of the cell wall of S. mutans were measured by atomic force microscopy (AFM) based techniques to monitor the in situ biophysical status of biofilms under common anti-pathogenic procedures such as ultraviolet (UV) radiation and alcohol treatment. The AFM nanoindentation suggested a positive correlation between nanomechanical strength and the level of UV radiation of S. mutans; scanning impedance spectroscopy of dehydrated biofilms revealed reduced electrical resistance that is distinctive from that of living biofilms, which can be explained by the discharge of cytoplasm after alcohol treatment. Furthermore, the localized elastic moduli of four regions of the biofilm were studied: septum (Z-ring), cell wall, the interconnecting area between two cells and extracellular polymeric substance (EPS) area. The results indicated that cell walls exhibit the highest elastic modulus, followed by Z-ring, interconnect and EPS. Our approach provides an effective alternative for the characterization of the viability of living cells without the use of biochemical labelling tools such as fluorescence dyeing, and does not rely on surface binding or immobilization for detection. These AFM-based techniques can be very promising approaches when the conventional methods fall short.

Intense Raman scattering on hybrid Au/Ag nanoplatforms for the distinction of MMP-9-digested collagen type-I fiber detection

Well-ordered Au-nanorod arrays were fabricated using the focused ion beam method (denoted as fibAu_NR). Au or Ag nanoclusters (NCs) of various sizes and dimensions were then deposited on the fibAu_NR arrays using electron beam deposition to improve the surface-enhanced Raman scattering (SERS) effect, which was verified using a low concentration of crystal violet (10(-)(5)M) as the probe molecule. An enhancement factor of 6.92 × 10(8) was obtained for NCsfibAu_NR, which is attributed to the combination of intra-NC and NR localized surface plasmon resonance. When 4-aminobenzenethiol (4-ABT)-coated Au or Ag nanoparticles (NPs) were attached to NCsfibAu_NR, the small gaps between 4-ABT-coated NPs and intra-NCs allowed detection at the single-molecule level. Hotspots formed at the interfaces of NCs/NRs and NPs/NCs at a high density, producing a strong local electromagnetic effect. Raman spectra from as-prepared type I collagen (Col-I) and Ag-NP-coated Col-I fibers on NCsfibAu_NR were compared to determine the quantity of amino acids in their triple helix structure. Various concentrations of matrix-metalloproteinase-9-digested Col-I fibers on NCsfibAu_NR were qualitatively examined at a Raman laser wavelength of 785nm to determine the changes of amino acids in the Col-I fiber structure. The results can be used to monitor the growth of healing Col-I fibers in a micro-environment.

Effects of Annealing on Magnetic Properties of Electrical Steel and Performances of SRM After Punching

This paper compares the microstructure and magnetic properties of punched electrical steel before and after annealing. The effects of this manufacturing process on performance of a switched reluctance motor (SRM) are also investigated. The punching of laminations distorts the grains near the cut edges, and therefore an anneal process is used to recover the damage caused by punching. In this paper, samples are annealed at 750°C for an hour under a N2 atmosphere. The damaged regions and corresponding recovery after annealing are observed under microscope as the measured core losses are improved up to 37%. The SRM performance is measured and it is found that the torque density can be enhanced when using the annealed electrical steel.

Direct deformation study of AFM probe tips modified by hydrophobic alkylsilane self-assembled monolayers

The in-use wear of atomic force microscopy (AFM) probe tips is crucial for the reliability of AFM measurements. Increase of tip size for several nanometers is difficult to monitor but it can already taint subsequent AFM data. We have developed a method to study the shape evolution of AFM probe tips in nanometer scale. This approach provides direct comparison of probe shape profiles, and thus can help in evaluation of the level of tip damage and quality of acquired AFM data. Consequently, the shape degradation of probes modified by hydrophobic alkylsilane self-assembled monolayers (SAMs) was studied. The tip wear length and wear volume were adopted to quantitatively verify the effectiveness of hydrophobic coatings. When compared with their silicon counterparts, probes modified by SAM materials exhibit superior wear-resistant behavior in tapping mode scans.

Simulation-aided design and fabrication of nanoprobes for scanning probe microscopy

We proposed and demonstrated a flexible and effective method to design and fabricate scanning probes for atomic force microscopy applications. Computer simulations were adopted to evaluate design specifications and desired performance of atomic force microscope (AFM) probes; the fabrication processes were guided by feedback from simulation results. Through design-simulation-fabrication iterations, tipless cantilevers and tapping mode probes were successfully made with errors as low as 2% in designed resonant frequencies. For tapping mode probes, the probe tip apex achieved a 10nm radius of curvature without additional sharpening steps; tilt-compensated probes were also fabricated for better scanning performance. This method provides AFM users improved probe quality and practical guidelines for customized probes, which can support the development of novel scanning probe microscopy (SPM) applications.

3D printing of low melting temperature alloys by fused deposition modeling

Fused deposition modeling (FDM) is the most commonly used 3D printing technique that directly extrudes molten materials layer by layer and overcomes the constraints of fabricating complicate geometries. This technique is fast, relatively easy to perform, thus more economical compared to other 3D printing methods. However, the materials that can be extruded by FDM are limited to polymers at the present time. This study aimed to develop a fused deposition modeling for metals (FDMm) system that can deposit metallic structures directly on a platform. An extruding nozzle designed by the researchers was connected to a commercial fused deposition machine to extend the materials selection from polymers to low melting temperature metals. Continuous Sn99.3Cu0.7 lead free solder and Sn60Pb40 lead free solder were successfully extruded in a linear shape and showed that the fabrication parameters for metals are significantly different from those for polymers. Controlling the fabrication parameters also allowed the deposition of metal at a uniform geometry. Optical microscopy and scanning electron microscopy were used to analyze the FDMm-fabricated samples. Good layer to layer bonding and overall material strength can be achieved by fine-tuning of process parameters.

Ageing, Shocks and Wear Mechanisms in ZTA and the Long-Term Performance of Hip Joint Materials

The surface morphologies and microstructures of Zirconia Toughened Alumina (ZTA) femoral heads were analyzed following in vitro tests aiming to simulate in vivo degradation. Three phenomena potentially leading to degradation were investigated: shocks, friction and hydrothermal ageing. Shocks due to micro-separation created the main damage with the formation of wear stripes on the femoral head surfaces. Atomic Force Microscopy (AFM) images suggested the release of wear debris of various shapes and sizes through inter- and intra-granular cracks; some debris may have a size lower than 100 nm. A decrease in hardness and Young’s modulus was measured within the wear stripes by nanoindentation technique and was attributed to the presence of surface and sub-surface micro-cracks. Such micro-cracks mechanically triggered the zirconia phase transformation in those worn areas, which in return presumably reduced further crack propagation. In comparison with shocks, friction caused little wear degradation as observed from AFM images by scarce pullout of grains. The long-term resistance of the ZTA composite material against hydrothermal ageing is confirmed by the present observations.

In-situ, time-lapse study of extracellular polymeric substance discharge in Streptococcus mutans biofilm

Streptococcus mutans is one of the main pathogens that cause tooth decay. By metabolizing carbohydrates, S. mutans emits extracellular polymeric substance (EPS) that adheres to the tooth surface and forms layers of biofilm. Periodontal disease occurs due to the low pH environment created by S. mutans biofilm, and such an acidic environment gradually erodes tooth enamel. Since the existence of EPS is essential in the formation of biofilm, the in-situ investigation of its generation and distribution in real time is the key to the control and suppression of S. mutans biofilm. Prior studies of the biofilm formation process by fluorescence microscope, scanning electron microscope, or spectroscope have roughly divided the mechanism into three stages: (1) initial attachment; (2) microcolonies; and (3) maturation. However, these analytical methods are incapable to observe real-time changes in different locations of the extracellular matrix, and to analyze mechanical properties for single bacteria in micro and nanoscale. Since atomic force microscopy (AFM) operates by precise control of tip-sample interaction forces in liquid and in air, living microorganisms can be analyzed under near-physiological conditions. Thus, analytical techniques based on AFM constitute powerful tools for the study of biological samples, both qualitatively and quantitatively. In this study, we used AFM to quantitatively track the changes of multiple nanomechanical properties of S. mutans, including dissipation energy, adhesion force, deformation, and elastic modulus at different metabolic stages. The data revealed that the bacterial extracellular matrix has a gradient distribution in stickiness, in which different stickiness indicates the variation of EPS compositions, freshness, and metabolic stages. In-situ, time-lapse AFM images showed the local generation and distribution of EPS at different times, in which the highest adhesion distributed along sides of the S. mutans cells. Through time-lapse analysis, we concluded that each contour layer is associated with a dynamic process of cell growth and nutrient consumption, and S. mutans is capable of controlling the priority of EPS secretion at specific locations. The live bacteria exhibited cyclic metabolic activities in the period of 23-34min at the maturation stage of biofilm formation. In addition, the discharge of EPS is responsive to the shear stress caused by the topographical change of biofilm to provide stronger mechanical support in the formation of 3D networked biofilm.

Nanomechanical probing of the septum and surrounding substances on Streptococcus mutans cells and biofilms

We report a unique bio-nanomechanical behavior at the septum (Z-ring) of Streptococcus mutans-containing biofilm through in situ measurements obtained by atomic force microscopy. A distinct serrated pattern on the releasing force-displacement curves can only be observed with the use of a sharp nanosized probe tip, and this was found at the septum of S. mutans. Further investigations suggested the serrated patterns could be due to the unfolding of some sub-surface divisome proteins. Seismometer measurements were conducted at the septum by placing an ultra-sensitive atomic force microscope probe on the surface. Unique periodic vibrations were observed at the septum under various biofilm conditions. This finding suggests the possibility of remodeling of the cell wall nanostructure at the septum of S. mutans.