Maurice N. Collins

Hyaluronic acid based scaffolds for tissue engineering--a review.

This review focuses on hyaluronic acid (HA) tissue scaffolding materials. Scaffolds are defined in terms of formation mechanisms and mode of action. Solution properties are discussed as an understanding of the hydrodynamics of HA is fundamental in optimising the subsequent modification and the chemistries behind important tissue engineering applications that are emerging from recent research on this increasingly valuable carbohydrate polymer are described. Key scaffold characteristics such as mechanical, biological function and degradation are discussed. The latest technologies behind scaffold processing are assessed and the applications of HA based scaffolds are discussed.

Physical properties of crosslinked hyaluronic acid hydrogels

In order to improve the mechanical properties and control the degradation rate of hyaluronic acid (HA) an investigation of the structural and mechanical properties of the hydrogels crosslinked using divinyl sulfone (DVS), glutaraldehyde (GTA) and freeze-thawing, or autocrosslinking has been carried out. The thermal and mechanical properties of the gels were characterised by differential scanning calorimetry (DSC), dynamic mechanical thermal analysis (DMTA) and compression tests. The solution degradation products of each system have been analysed using size exclusion chromatography (SEC) and the Zimm–Stockmayer theory applied. Autocrosslinked gels swell the most quickly, whereas the GTA crosslinked gels swell most slowly. The stability of the autocrosslinked gels improves with a reduction in solution pH, but is still poor. GTA and DVS crosslinked gels are robust and elastic when water swollen, with glass transition values around 20°C. SEC results show that the water soluble degradation products of the gels show a reduction in the radius of gyration at any particular molecular weight and this is interpreted as indicating increased hydrophobicity arising from chemical modification.

Effect of Ag content on the microstructure of Sn‐Ag‐Cu based solder alloys

Purpose – The purpose of this paper is to examine the microstructure and evaluate the intermetallic compounds in the following lead‐free solder alloys: Sn98.5Ag1.0Cu0.5 (SAC105) Sn97.5Ag2.0Cu0.5 (SAC205) Sn96.5Ag3.0Cu0.5 (SAC305) and Sn95.5Ag4.0Cu0.5 (SAC405).Design/methodology/approach – X‐ray diffraction (XRD) and scanning electron microscopy (SEM) were employed to identify the main intermetallics formed during solidification. Differential scanning calorimetry (DSC) was used to investigate the undercooling properties of each of the alloys.Findings – By using XRD analysis in addition to energy dispersive spectroscopy (EDS) it was found that the main intermetallics were Cu6Sn5 and Ag3Sn in a Sn matrix. Plate‐like e‐Ag3Sn intermetallics were observed for all four alloys. Solder alloys SAC105, SAC205 and SAC305 showed a similar microstructure, while SAC405 displayed a fine microstructure with intermetallic phases dense within the Sn matrix.Originality/value – Currently, low‐silver content SAC alloys are bei...

The influence of the Pb-free solder alloy composition and processing parameters on thermal fatigue performance of a ceramic chip resistor

This paper presents the results of a thermal fatigue study of a 2512 ceramic chip resistor assembled with various Pb free solders including SnCu, SAC105, SAC205, SAC305, and SAC405. The test matrix also includes some limited evaluations with other variables such as cooling rate (solidification rate), thermal preconditioning and nitrogen (inert) reflow atmosphere. The matrix also includes a SnPb eutectic control cells. The resistor test vehicle provides an expedient and self-consistent method for evaluating the relative fatigue performance of the various alloys. A study of the as-assembled solder joints was conducted to characterize the microstructure of the solder joints with varying silver content. Thermal fatigue was evaluated using an accelerated temperature cycle of 0/100 °C with dwell times of 10 and 60 minutes. The test results show a direct relationship between characteristic fatigue life and Ag content, with the higher Ag content alloys outperforming those with the lowest Ag content. As might be anticipated, there also was a consistent inverse relationship between fatigue life and dwell time for the Pb free solders. The failure analysis and microstructural evolution is characterized with optical metallography and scanning electron microscopy and the fatigue reliability of the Pb free solders is discussed in terms of the microstructures.

Phenomenological Study of the Effect of Microstructural Evolution on the Thermal Fatigue Resistance of Pb-Free Solder Joints

Unlike SnPb solders, the thermal fatigue reliability of the Sn-Ag-Cu (SAC) solders is believed to be influenced significantly by both the initial and evolving microstructures. This paper presents a phenomenological study of the relationship between the initial SAC solder joint microstructure, the evolving microstructure, and the thermal fatigue performance measured by accelerated temperature cycling (ATC). To reflect the board assemblies that are in field use, commercial surface mount components with multiple geometries and materials and from different package assemblers were joined to the board with different lead free SAC alloys. The initial microstructures of the board level solder joints were altered in a variety of ways including: 1) varying the solder joint cooling rate; 2) varying the number of solder reflow exposures; and 3) exposure to different isothermal temperature exposures. In all cases the solder joint microstructure was exposed to one or more of these treatments prior to exposure to temperature cycling. In addition, some of the test boards were exposed to different cycling dwell times to determine if the microstructural evolution that occurred during ATC testing effected the respective characteristic lifetimes of the joints. The microstructural evolution was tracked and characterized with optical metallography and scanning electron microscopy. These results could have practical implications in terms of limiting the ability to develop acceleration factors and effective strain-based models for predicting Pb-free solder joint life.

Antibacterial and antioxidative activity of O-amine functionalized chitosan

Cinnamaldehyde was immobilized to O-amine functionalized chitosan via a coupling reaction. Fourier transform infrared spectroscopy confirmed N-cinnamyl substitution. Wetting analyses demonstrate more hydrophobicity in the N-cinnamyl substituted O-amine functionalized chitosan compared to chitosan or unsubstituted O-amine functionalized chitosan. Thermal gravimetric analysis and differential scanning calorimetry demonstrates that the prepared N-cinnamyl substituted O-amine functionalized chitosan exhibits higher thermostability than unmodified chitosan at temperatures in which polysaccharides are commonly stored and utilised. The N-cinnamyl substituted O-amine functionalized chitosan, against four different bacteria strains [two gram-positive (Staphylococcus aureus and Bacillus cereus) and two gram-negative (Escherichia coli and Pseudomonas aeruginosa)], displays promotion of inhibition activity against these bacterial strains. Finally, the antioxidative activity of the N-cinnamyl substituted O-amine functionalized chitosan was compared with those activities of chitosan and O-amine functionalized chitosan. This was evaluated by uninhibited and inhibited hyaluronan degradation and ABTS assay. The N-cinnamyl substituted O-amine functionalized chitosan shows a lower activity towards donating a hydrogen radical compared to chitosan or O-amine functionalized chitosan. On the other hand, the N-cinnamyl substituted O-amine functionalized chitosan exhibited a higher ability to scavenge the ABTS+ cation radical compared to chitosan and O-amine functionalized chitosan.

Influence of tiopronin, captopril and levamisole therapeutics on the oxidative degradation of hyaluronan

The ability to protect hyaluronic acid (HA) from oxidative degradation by cupric ions and ascorbate (production of (•)OH and peroxy-type radicals) during acute phase joint inflammation has been investigated using the following drugs: tiopronin, captopril, and levamisole. Radical scavenging activity, i.e. the propensity for donation of electrons was assessed for the drugs by ABTS and DPPH assays. The kinetics of HA degradation have been measured in the presence of each drug using rotational viscometry. The results of ABTS and DPPH assays show the highest radical scavenging activity for captopril, followed by tiopronin. For levamisole, no effect was observed. Captopril and tiopronin prevented HA degradation induced by (•)OH radicals in a similar manner, while tiopronin was more effective in scavenging peroxy-type radicals. On the other hand, levamisole was shown to be a pro-oxidant. Recovered HA fragments were characterized using FT-IR analysis, the incorporation of a sulphur atom from captopril and tiopronin but not from levamisole into the HA molecule was demonstrated.

Effects of tensile strain on the nanostructure of irradiated and thermally stabilised ultra high molecular weight polyethylenes for orthopaedic devices

Ultra high molecular weight polyethylene (UHMWPE), of the types used in orthopaedic implants, has been irradiated in air and in nitrogen to give received doses between zero and ten Mrad and has been subject to tensile testing whilst simultaneously recording the wide angle and small angle X-ray scattering (WAXS and SAXS) diffraction patterns, using the synchrotron facilities at Diamond. Commercial implant grade polymer, which has been subject to irradiation and two different thermal annealing or stabilising processes, to prevent age related embrittlement, has also been examined. With all materials, as the sample elongates lamellae reorganisation processes occur at a strain of around 0.1, as the unit cell converts from orthorhombic to monoclinic, and yield commences. Yield in the irradiated polymers is associated with a pronounced peak in the stress–strain curve, whereas yield in unirradiated, and in thermally annealed polymers, does not involve a peak in the stress curve. SAX plots show that lamellae reorganisation, during yield, occurs much faster in irradiated materials. This lamellae reorganisation is thought to involve a slip and glide initiated unravelling of the folds, accompanied by refolding and reorientation of parts of existing lamellae. It is proposed that in irradiated materials this is facilitated by nucleation sites on the surface of the lamellae, resulting from radiation damage. The total crystallinity increases slightly during the yielding process and it is thought that this crystal growth involves an interfacial all-trans amorphous phase previously identified with these materials. The greatest effects arise when the samples are irradiated in air. This suggests that the stabilising processes, involving annealing of irradiated polymers, probably work through restoring crystal perfection, as well as increasing the network density in the amorphous phase. Taken in conjunction with existing knowledge on free radical quenching, the information generated allows a much greater understanding of the steps necessary to produce a stable implant grade UHMWPE. It is well known that premature failure of hard metal on polyethylene joint systems causes much discomfort and difficult revision surgery. In recent years irradiated and annealed polymers have taken over much of the market, but the mechanism of action of the annealing processes is only partially understood. Free radical quenching is clearly part of the story, but is not in itself sufficient to explain why irradiated and heat treated polymers perform much better than those simply irradiated under nitrogen. This paper proposes that the heat treatment processes are important in restoring crystal perfection after radiation damage. Irradiation inserts nucleation sites for crystal slip and glide, which occurs when the polymer is strained, but annealing at temperatures close to Tm, restores perfection. This is shown through simultaneous SAXS and WAXS analysis whilst the sample is being strained in the X-ray beam.

Surface finish effect on reliability of SAC 305 soldered chip resistors

Purpose – The purpose of this paper is to assess the long‐term reliability of lead‐free Sn96.5Ag3.0Cu0.5 (SAC305) under accelerated temperature cycling (ATC) conditions. Test vehicles consisted of commercial 2512 ceramic chip resistors soldered to printed circuit boards (PCBs) using three different Pb‐free surface finishes: organic solderability preservative (OSP), immersion silver (IAg) and electroless nickel immersion gold (ENIG).Design/methodology/approach – Two populations of solder joints were monitored continuously during a thermal cycle of 0°C to 100°C with a ramp rate of 10°C/min and a 30 min dwell at the temperature extremes. One population was cycled to 2,500 cycles, the other population was cycled to 8,250 cycles. Failures were defined in accordance with the IPC‐9701A industry test guidelines and failure data are reported as characteristic life, η. Microstructural evolution was characterised using metallographic techniques and back‐scattered scanning electron microscopy (SEM). Fractography was ...

Hydrogen peroxide generation by the Weissberger biogenic oxidative system during hyaluronan degradation.

By applying the enzyme catalase, our study on hyaluronan degradation confirms the generation of hydrogen peroxide using the Weissberger biogenic oxidative system (WBOS), which is composed of ascorbate and cupric ions. Dynamic viscosities of hyaluronan (HA) solutions influenced by WBOS in the absence and presence of catalase were analysed by rotational viscometry. Molar masses of HAs were determined by size-exclusion chromatography with multi-angle laser-light scattering. Our results show that catalase dose-dependently inhibited the degradation of HA macromolecules, which presumably confirms the generation of H2O2 in the reaction system. This has implications in range of biomedical applications such as arthritic joint treatment, tissue engineering, ocular and cosmetic surgery.