Optimization of carbon nanotube synthesis from porous anodic Al-Fe-Al templates

A parametric study of carbon nanotube (CNT) synthesis from catalytically active porous anodic Al-Fe-Al multilayer templates was conducted with respect to pore aspect ratio, Fe layer thickness, CNT synthesis temperature, and pre-anodization thermal annealing. Performance metrics included CNT catalytic activity and the pore wall integrity at the Al-Fe-Al interface. The observed CNT density was a strong function of pore diameter, synthesis temperature and pre-anodization annealing of the catalyst film. Vertical pore wall integrity at the Al-Fe-Al interface was optimized by selection of pre-anodization annealing conditions, with interfacial void formation observed in the absence of this technique. Based on CNT growth rates, an activation energy of 0.52 eV was observed for CNT synthesis for all film structures, regardless of pore aspect ratio. The optimization of templated CNT synthesis is expected to assist in the development of high-density vertically oriented CNT-based devices.     

Fluorescence correlation spectroscopy at 100 nM concentrations using near-field scanning optical microscopic (NSOM) geometries and highly diffracting force sensing fiber probes

A tapered cantilevered optical fiber probe is introduced for fluorescence correlation spectroscopy (FCS). The probe has an aperture that is coated with metal and its dimension can be very well defined. Its design is based on cantilevered near-field optical fiber probes that allow for on-line atomic force feedback. This permits unprecedented stability in FCS measurements. Even such probes that have large diameters are below the cutoff wavelength of light propagation in optical fibers. Such large diameter probes produce bright spots of light that are highly diffracting. Therefore, only the fluence of light very close to the surface of the glass probe aperture is sufficient to exhibit a high probability of fluorescence excitation. From the results presented in this paper the z extent of such probes seems comparable to what can be obtained from prism-based evanescent wave methods, but with much more flexibility and including force sensing capability. In agreement with theoretical results on prism evanescent field-based excitation, it is shown that even with large xy dimensions for the fiber probes in this paper, fluorescence correlation spectra from 100 nM fluorophore concentrations can be recorded. This is 10 times larger than the concentrations generally required for conventional confocal FCS. The results suggest that such an approach has considerable potential for applications of FCS in membrane, near-membrane, solution, and even within-cell environments. The latter is achieved through atomic force feedback controlled penetration of tapered cantilevered metal-coated glass fibers into cells, and this is also reported in this paper.     

The Synthesis and Biological Evaluation of Multifunctionalised Derivatives of Noscapine as Cytotoxic Agents

Noscapine, a phthalideisoquinoline alkaloid derived from Papaver somniferum, is a well‐known antitussive drug that has a relatively safe in vitro toxicity profile. Noscapine is also known to possess weak anticancer efficacy, and since its discovery, efforts have been made to design derivatives with improved potency. Herein, the synthesis of a series of noscapine analogues, which have been modified in the 6′, 9′, 1 and 7‐positions, is described. In a previous study, replacement of the naturally occurring N‐methyl group in the 6′‐position with an N‐ethylaminocarbonyl was shown to promote cell‐cycle arrest and cytotoxicity against three cancer cell lines. Here, this modification has been combined with other structural changes that have previously been shown to improve anticancer activity, namely halo substitution in the 9′‐position, regioselective O‐demethylation to reveal a free phenol in the 7‐position, and reduction of the lactone to the corresponding cyclic ether in the 1‐position. The incorporation of new aryl substituents in the 9′‐position was also investigated. The study identified interesting new compounds able to induce G2/M cell‐cycle arrest and that possess cytotoxic activity against the human prostate carcinoma cell line PC3, the human breast adenocarcinoma cell line MCF‐7, and the human pancreatic epithelioid carcinoma cell line PANC‐1. In particular, the ethyl urea cyclic ether noscapinoids and a compound containing a 6′‐ethylaminocarbonyl along with 9′‐chloro, 7‐hydroxy and lactone moieties exhibited the most promising biological activities, with EC₅₀ values in the low micromolar range against all three cancer cell lines, and these derivatives warrant further investigation.     

Comparing Different Synthesis Procedures for Carbide‐Derived Carbon‐Based Structured Catalyst Supports

Different approaches were analyzed to combine the tuneable micropore structure of carbide‐derived carbons with a foam‐like secondary porosity. The resulting structured catalyst supports were characterized in detail and applied in the model reaction of ethene hydrogenation. Preparation methods studied were dip‐coating using polytetrafluoroethylene as binder on cellular metal structures, a chemical vapor deposition coating of the metal structures with thin carbide layers and subsequent conversion to carbide‐derived carbon, and the partial or full conversion of carbide foams to carbon/carbide composites. For the binder method, optimal parameters for stable slurry preparation as well as for calcination of the slurry were obtained. It could further be demonstrated that the conversion of carbide foams into carbon/carbide composites leads to an appreciation between decreasing mechanical strength and increasing specific surface area.     

Density of additively-manufactured, 316L SS parts using laser powder-bed fusion at powers up to 400 W

Selective laser melting is a powder-based, additive-manufacturing process where a three-dimensional part is produced, layer by layer, by using a high-energy laser beam to fuse the metallic powder particles. A particular challenge in this process is the selection of appropriate process parameters that result in parts with desired properties. In this study, we describe an approach to selecting parameters for high-density (>99 %) parts using 316L stainless steel. Though there has been significant success in achieving near-full density for 316L parts, this work has been limited to laser powers <225 W. We discuss how we can exploit prior knowledge, design of computational experiments using a simple model of laser melting, and single-track experiments to determine the process parameters for use at laser powers up to 400 W. Our results show that, at higher power values, there is a large range of scan speeds over which the relative density remains >99 %, with the density reducing rapidly at high speeds due to insufficient melting, and less rapidly at low speeds due to the effect of voids created as the process enters keyhole mode.     

Absolute photoluminescence quantum efficiency measurement of light-emitting thin films

We developed an integrated monochromatic excitation light source integrating sphere based detection system to accurately characterize the absolute photoluminescence quantum efficiency of commonly used polymer light emitting films without using a reference sample. Our methodology is similar to the method reported by de Mello et al. [Adv. Mater. 9, 230 (1997)] In this Note, we show that the absolute photoluminescence quantum efficiency might only be measured when an appropriate calibration of the spectral variation of the measurement system is done. This calibration is especially important when employing a short excitation wavelength (<400 nm) for common silicon-based detector.     

Rapid consolidation of powdered materials by induction hot pressing

A rapid hot press system in which the heat is supplied by RF induction to rapidly consolidate thermoelectric materials is described. Use of RF induction heating enables rapid heating and consolidation of powdered materials over a wide temperature range. Such rapid consolidation in nanomaterials is typically performed by spark plasma sintering (SPS) which can be much more expensive. Details of the system design, instrumentation, and performance using a thermoelectric material as an example are reported. The Seebeck coefficient, electrical resistivity, and thermal diffusivity of thermoelectric PbTe material pressed at an optimized temperature and time in this system are shown to agree with material consolidated under typical consolidation parameters.     

Multi-laboratory simulator studies on effects of serum proteins on PTFE cup wear

A multi-laboratory, simulator study investigated the wear of polytetrafluorethylene (PTFE) cups run in bovine serum. Each laboratory used its own test protocol with a variety of simulator types. Our wear model incorporated 32 mm dia CoCr heads matched to PTFE cups run with serum protein-concentrations in the range 17–69 mg/ml. The multi-lab data demonstrated that protein-concentration had the most significant effect on wear performance. Both inverted and anatomical cups followed the same trend with first a rapid increase in wear-rates apparent for the initially low-protein levels and then a wear-rate reduction effect becoming apparent beyond 17 mg/ml of proteins. The results showed that as the protein concentration increased from 17 to 69 mg/ml, the magnitude of the wear-rates increased 200% but the protein wear-rate gradient decreased 24–60% with “inverted” and “anatomical” cups, respectively. This effect was more pronounced with ‘anatomical” than “inverted” cups. Thus, the wear-trends with “inverted” cups were generally the more consistent, particularly at the low-protein levels. Increasing the serum volume by two-fold in one study increased the PTFE wear-magnitudes approximately 40% and the protein-wear gradient by 30%. These PTFE wear phenomena were consistent with the concept that low-concentrations of proteins promoted polymer wear but high-protein concentrations resulted in a protein-degradation phenomenon which progressively masked the actual polymer wear. In the selected protein range 17–69 mg/l, the multi-laboratory simulator data consistently overestimated the average clinical wear-rate by at least 50–100% depending on protein range. It would, therefore, appear clinically relevant to study PTFE wear with an inverted-cup model using a large volume of serum but only in low-protein concentrations. The protein-related wear phenomena observed with PTFE cups in this multi-laboratory project may also have relevance for wear-simulation of UHMWPE cups.     

Automation for High-throughput Identification and Picking of GFP Expressing Colonies

Green fluorescent protein (GFP) has many applications as a marker in living cells, and has become widely used as a reporter gene in microbial, plant and animal cells. Screening microbial colonies for GFP expression enables various types of assays (e.g. for secretory mutations). However, this is laborious, non-quantitative and potentially hazardous to the operator (due to UV illumination) when performed manually. In order to address this the GloPix robot was developed. The imaging system discriminates between colonies based on the level of fluorescence activity and the picking function automatically transfers cells to microplate wells. Measuring fluorescent activity allows quantitation of fluorescent tag concentration/expression.