Lignin-based carbon fibers for composite fiber applications

Carbon fibers have been produced for the first time from a commercially available kraft lignin, without any chemical modification, by thermal spinning followed by carbonization. A fusible lignin with excellent spinnability to form a fine filament was produced with a thermal pretreatment under vacuum. Blending the lignin with poly(ethylene oxide) (PEO) further facilitated fiber spinning, but at PEO levels greater than 5%, the blends could not be stabilized without the individual fibers fusing together. Carbon fibers produced had an over-all yield of 45%. The tensile strength and modulus increased with decreasing fiber diameter, and are comparable to those of much smaller diameter carbon fibers produced from phenolated exploded lignins. In view of the mechanical properties, tensile 400–550 MPa and modulus 30–60 GPa, kraft lignin should be further investigated as a precursor for general grade carbon fibers.     

Physical aging deep in the glassy state of a fully cured polyimide

Physical aging of a fully cured polyimide/glass fiber specimen has been investigated deep in the glassy state using a freely oscillating torsion pendulum (TBA). A single specimen, the physical aging effects of which could be erased by heating to above T_g = 304°C (0.8 Hz), could be used for all experiments. Data were obtained during isothermal aging at different aging temperatures, T_α, (from 10°C to T_g) and during subsequent temperature scans (T_α to 5 to 315°C). The aging rate depended upon the value of T_α relative to both T_g and the β-relaxation temperature, T_β = 139°C (1.3 Hz). Changes in thermomechanical behavior due to aging were localized about T_α. This suggests that only an intermediate portion of the relaxation spectrum participates in, and is affected by, isothermal physical aging. It follows, and is observed, that the intensity of the β-relaxation mechanical loss peak is perturbed most significantly by aging at T_α near T_β. The effect of isothermal aging deep in the glassy state could be essentially eliminated by heating to below T_g. © 1992 John Wiley & Sons, Inc.     

Removing paraffin‐based wax coatings from old corrugated containers using supercritical carbon dioxide

Supercritical carbon dioxide (SC‐CO₂) extractions of paraffin‐based wax coatings from saturated and curtain‐coated old corrugated containers (OCC) are reported. Extractions were performed in a 500‐mL reactor (300 bar, 100°C, 50 g CO₂/min and 1 h). Wax removal efficiencies of 98 and 70% for saturated and curtain‐coated OCC, respectively, were obtained. Under similar conditions, extractions in the presence of water resulted in an extraction efficiency of 99% for saturated OCC. Decreasing the operating pressure to 200 bar decreased the extraction efficiency to approximately 50%. Gas chromatography (GC) of the wax coatings on OCC, before and after extraction with SC‐CO₂, showed a slight shift in the molecular weight distribution of the paraffin wax (after SC‐CO₂ extraction) toward higher molecular weights for both saturating wax and curtain‐coating wax. There was no evidence of chemical degradation or modification of the paraffin wax coatings by SC‐CO₂. The packing density, packing arrangement, and dimensions of the curtain‐coated OCC in the extraction apparatus affected the extraction efficiency. Loose packing compared to tight packing, 1 × 1 cm squares versus 1 × 20 cm strips, had higher extraction efficiencies; a random packing arrangement was better than packing with the fluting material in the direction of SC‐CO₂ flow. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 83: 2699–2704, 2002     

Free volume after cure vs. fractional conversion for a high-Tg epoxy/amine thermosetting system

Isothermal glassy-state properties of cured thermosetting materials pass through maximum and minimum values with increasing fractional chemical conversion. In this work, a diglycidyl ether of bisphenol A (a diepoxide) and trimethylene glycol di-p-aminobenzoate (a tetrafunctional aromatic diamine) system was investigated for the purpose of analyzing the complex behavior after cure of the isothermal properties of the glassy state with increasing conversion. The glass transition temperature (T_g) is used as a direct measure of conversion. Dilatometric, differential scanning calorimetry, torsional braid analysis, and positron annihilation spectroscopy techniques were used to monitor the density, T_g, modulus, and free volume of the material after cure with increasing conversion. The specific volume at 25°C after cure passes through a minimum and the modulus passes through a maximum with increasing conversion. The fractional free volume and the average radius of free volume at 25°C after cure pass through minimum values with respect to conversion. The specific volume, modulus, and fractional free volume at 25°C vs. conversion data qualitatively correlate. The anomaly of the increasing specific volume in the glassy state with increasing conversion is thus considered to arise from changes in free volume on a length scale corresponding to angstroms. The increasing free volume with increasing conversion is related to the phenomenon of antiplasticization. © 1995 John Wiley & Sons, Inc.     

Development of cross‐linked starch microcellular foam by solvent exchange and reactive supercritical fluid extrusion

Starch microcellular foams (SMCFs) are prepared by pore preserving drying or formation processes and contain pores in the micron size range. SMCFs have high specific surface area and are useful for applications such as opacifying pigments or as adsorbent materials. The objective of this research was to determine how the processing conditions and use of a crosslinking agent would affect the foam structure and properties. SMCFs (crosslinked and uncrosslinked) were prepared from molded aquagels and carbon dioxide extrusion processes separately and then solvent exchanged. Extruded samples showed macroscopic pores whereas samples from aquagels showed a much finer micropore structure. Aquagel‐based SMCF samples had lower density and higher brightness than did extruded samples. The starch foams with micropore structure had low density and high brightness. The solvent exchange process was the most important variable in generating a microcellular structure. Micropores and not macropores contributed to increased brightness of these materials. The brightness and density of the foams were found to be linearly related. Crosslinking with epichlorohydrin imparted significant water resistance to the extruded samples as evidenced in lower water swelling and higher contact angles. Equilibrium moisture content was correlated with the microporous structure. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Survival of probiotic lactobacilli in the upper gastrointestinal tract using an in vitro gastric model of digestion

The aim of this study was to investigate survival of three commercial probiotic strains (Lactobacillus casei subsp. shirota, L. casei subsp. immunitas, Lactobacillus acidophilus subsp. johnsonii) in the human upper gastrointestinal (GI) tract using a dynamic gastric model (DGM) of digestion followed by incubation under duodenal conditions. Water and milk were used as food matrices and survival was evaluated in both logarithmic and stationary phase. The % of recovery in logarithmic phase ranged from 1.0% to 43.8% in water for all tested strains, and from 80.5% to 197% in milk. Higher survival was observed in stationary phase for all strains. L. acidophilus subsp. johnsonii showed the highest survival rate in both water (93.9%) and milk (202.4%). Lactic acid production was higher in stationary phase, L. casei subsp. shirota producing the highest concentration (98.2 mM) after in vitro gastric plus duodenal digestion.     

Diversity of bacterial population of table olives assessed by PCR-DGGE analysis

Nocellara Etnea and Geracese table olives are produced according to traditional process, in which lactic acid bacteria (LAB) and yeasts are the dominant microorganisms. With the aim to evaluate the effect of selected starter cultures on dynamics of bacterial population during fermentation and on growth/survival of Listeria spp. artificially inoculated into the olive brine, a polyphasic approach based on the combination of culturing and PCR-DGGE analysis was applied. Plating results showed a different concentration of the major bacterial groups considered among cultivars and the beneficial effect of LAB starters, which clearly inhibited Enterobacteriaceae. Moreover, results indicated that the brine conditions applied did not support the growth/survival of Listeria monocytogenes strain, artificially inoculated, highlighting the importance of selecting right fermentation parameters for assuring microbiological safety of the final products. Comparison of DGGE profile of Nocellara Etnea and Geracese table olives, displayed a great difference among cultivars, revealing a wide biodiversity within Lactobacillus population during Geracese olives fermentation. Based on cloning and sequencing of the most dominant amplicons, the presence, among others, of Lactobacillus paracollinoides and Lactobacillus coryniformis in Geracese table olives was revealed in table olives for the first time.     

256-channel bidirectional optical interconnect using VCSELs andphotodiodes on CMOS

Two-dimensional parallel optical interconnects (2-D-POIs) are capable of providing large connectivity between elements in computing and switching systems. Using this technology we have demonstrated a bidirectional optical interconnect between two printed circuit boards containing optoelectronic (OE) very large scale integration (VLSI) circuits. The OE-VLSI circuits were constructed using vertical cavity surface emitting lasers (VCSELs) and photodiodes (PDs) flip-chip bump-bonded to a 0.35-μm complementary metal-oxide-semiconductor (CMOS) chip. The CMOS was comprised of 256 laser driver circuits, 256 receiver circuits, and the corresponding buffering and control circuits required to operate the large transceiver array. This is the first system, to our knowledge, to send bidirectional data optically between OE-VLSI chips that have both VCSELs and photodiodes cointegrated on the same substrate     

Melt spinning of thermotropic cellulose derivatives

The melt spinning of two thermotropic cellulose derivatives—trimethyl silyl cellulose and phenyl acetoxy cellulose—is described in this article. Removal of the substituents was facile, rapid, and essentially complete. Both the melt‐spun and regenerated fibers had banded textures typical of fibers spun from a liquid crystalline phase. The regenerated cellulose fibers had high strengths and moduli compared to viscose rayon and Lyocel cellulose fibers. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 77: 418–423, 2000