The effects of the SiOSi segment presence in BAPP/BPDA polyimide system on morphology and hardness properties for opto-electronic application

Recent technological advances demanded incorporation of SiOSi segment into polyimides (PI)s to improve versatility in terms of processing, morphology and optoelectronic properties. In order to study the role of SiOSi segment in the morphology and hardness properties of PI, the SiOSi segment have been introduced into the PI backbone through the conventional copolymerization and in PI matrix through sol gel method. The PI series were characterized by Fourier transform infra-red (FT-IR), nuclear magnetic resonance (NMR) spectroscopy, elemental analysis, solution viscosity and gel permeation chromatography (GPC). Scanning electron microscope (SEM) analysis suggested a microphase separation between the two components. FT-IR spectra confirmed the presence of silicone segment, as well as a complete imidization of PI series. Micrograph suggested a homogeneous phase between the PI and silicone segment for copolymerization series while sol gel technique revealed the inorganic particles were distributed homogenously in PI matrix. It was also found that the presence SiOSi segment in PI backbone and PI matrix influenced the opto-electronic properties.     

Phase constitutions of MoSiN anti-oxidation multi-layer coatings on CC composites by fused slurry

To improve the oxidation resistance of MoSi fused slurry coating fabricated in vacuum, MoSiN multi-layer coatings were synthesized on C/C composites in nitrogen atmosphere by fused slurry using same Mo and Si element powders. The phase compositions and microstructures were characterized by X-ray diffractometry (XRD), optical microscopy (OM), scanning electron microscopy (SEM) with energy-dispersive spectroscopy (EDS). The results indicate that the MoSiN coating contains SiC inner layer and MoSi₂/Si main layer, which was similar with MoSi coating. Additionally, a thin outer layer with nano-filiform morphology has been found on the coating surface, which consists of SiC, Si₃N₄, AlN, Al₂O₃ and sialon phase. Oxidation experiments show that the MoSiN multi-layer coating exhibits excellent oxidation resistance at 1400 °C and anti-oxidizing potential ability at 1450 °C.     

Effect of annealing temperature on the microstructure and photoluminescence of low resistivity Si/SiN/TaN thin films using magnetron sputtering

A lot of studies have been devoted to the porous Si, erbium-doped Si and Si-embedded in dielectric matrix of SiO or SiN together with long-time conventional furnace annealing. Besides, it is noted that these Si nanostructured films were highly resistive and non-conducting. In this paper, we have investigated the effect of annealing temperature on the microstructure and photoluminescence of low-resistivity Si/SiN/TaN nanocomposite thin films which are deposited by magnetron sputtering and followed by rapid thermal annealing (RTA). All samples are of luminescence and staying low resistivity at about 1462–2162 μΩ cm which increases with increasing annealing temperatures. The asymmetric broad photoluminescence (PL) peak covered the wavelengths of 400–700 nm. The wide visible PL spectra can be deconvoluted into three bands of blue (~ 455 nm), green-yellow (~ 525 nm), and orange emissions (~ 665 nm), which correspond to the emission origins from unsatisfied states in imperfections of interface between the Si:O and SiN:O, located states related to the mixed SiO or SiN bonds in SiN:O layer and nc-Si embedded in SiN:O matrix. The detailed mechanism of broad visible PL was investigated in terms of microstructure and bonding configuration evolution. The relationship between the annealing temperature, microstructure and PL behavior of Si/SiN/TaN multilayer films is discussed and established.     

Metakaolin-based inorganic polymer composite: Effects of fine aggregate composition and structure on porosity evolution,microstructure and mechanical properties

This paper examines the phase transformation, pore evolution, microstructural and mechanical changes that occur in inorganic polymer cement (IPC) in the presence of three different grade of fine aggregates (ф < 100 μm) of ladle slag, nepheline syenite and quartz sand. Experimental results indicate that polycondensation was enhanced in nepheline syenite based specimens, compared to quartz sand, due to the increase in HMAS phases in relation to the dissolution and interaction of amorphous/disordered fraction of aggregates. HCS and HCAS with HMAS phases were identified in the ladle slag based specimens. The formation of these new phases reduced both the cumulative pore volume and pores size. The apparent increase in volume of capillary pores in ladle slag based specimens was explained by the residual bubbles from the carbonates included in raw slag. The flexural strength of the inorganic polymer cement increases from 4 MPa to 4.2, 4.8 and 6.8 MPa with the addition of 20 wt% of quartz sand, nepheline syenite and ladle slag respectively. These values increase significantly between 28 and 180 days of curing (9.1 MPa for ladle slag and 10.0 MPa for nepheline syenite). It was concluded that fines can be used to remove the HM and poorly bounded alumina oligomers in metakaolin based inorganic polymer matrices and improve the interfacial zone for the design of an optimum grade and high-performance composites.     

Degradation performance of biodegradable FeMnC(Pd) alloys

Biodegradable metals offer great potential in circumventing the long-term risks and side effects of medical implants. Austenitic FeMnCPd alloys feature a well-balanced combination of high strength and considerable ductility which make them attractive for use as degradable implant material. The focus of this study is the evaluation of the degradation performance of these alloys by means of immersion testing and electrochemical impedance spectroscopy in simulated body fluid. The FeMnCPd alloys are characterized by an increased degradation rate compared to pure Fe, as revealed by both techniques. Electrochemical measurements turned out to be a sensitive tool for investigating the degradation behavior. They not only show that the polarization resistance is a measure of corrosion tendency, but also provide information on the evolution of the degradation product layers. The mass loss data from immersion tests indicate a decreasing degradation rate for longer times due to the formation of degradation products on the sample surfaces. The results are discussed in detail in terms of the degradation mechanism of Fe-based alloys in physiological media.     

High contrast glasses for all-solid fibers fabrication

We present composition development of borosilicate glasses for fabrication of high refractive index contrast, all-solid photonic crystal fibers. An oxide system composed of SiO₂B₂O₃Al₂O₃Li₂ONa₂OK₂O was adjusted to match thermal properties of selected highly nonlinear, lead bismuth gallium silicate glass. A high difference of refractive index of 0.376 is achieved at a wavelength of 1550 nm. We proved experimentally that the developed pair of glasses enables to draw optical fibers, and we propose a design of a photonic crystal fiber structure for broadband supercontinuum generation.     

Poly (hydroxyethyl methacrylate-glycidyl methacrylate) films modified with different functional groups: In vitro interactions with platelets and rat stem cells

Copolymerization of 2-hydroxyethylmethacrylate (HEMA) with glycidylmethacrylate (GMA) in the presence of α-α′-azoisobisbutyronitrile (AIBN) resulted in the formation of hydrogel films carrying reactive epoxy groups. Thirteen kinds of different molecules with pendant NH₂ group were used for modifications of the p(HEMA-GMA) films. The NH₂ group served as anchor binding site for immobilization of functional groups on the hydrogel film via direct epoxy ring opening reaction. The modified hydrogel films were characterized by FTIR, and contact angle studies. In addition, mechanical properties of the hydrogel films were studied, and modified hydrogel films showed improved mechanical properties compared with the non-modified film, but they are less elastic than the non-modified film. The biological activities of these films such as platelet adhesion, red blood cells hemolysis, and swelling behavior were studied. The effect of modified hydrogel films, including NH₂, (using different aliphatic CH₂ chain lengths) CH₃, SO₃H, aromatic groups with substituted OH and COOH groups, and amino acids were also investigated on the adhesion, morphology and survival of rat mesenchymal stem cells (MSCs). The MTT colorimetric assay reveals that the p(HEMA-GMA)-GA-AB, p(HEMA-GMA)-GA-Phe, p(HEMA-GMA)-GA-Trp, p(HEMA-GMA)-GA-Glu formulations have an excellent biocompatibility to promote the cell adhesion and growth. We anticipate that the fabricated p(HEMA-GMA) based hydrogel films with controllable surface chemistry and good stable swelling ratio may find extensive applications in future development of tissue engineering scaffold materials, and in various biotechnological areas.     

Sol–gel synthesis of tantalum oxide and phosphonic acid-modified carbon nanotubes composite coatings on titanium surfaces

Carbon nanotubes used as fillers in composite materials are more and more appreciated for the outstanding range of accessible properties and functionalities they generate in numerous domains of nanotechnologies. In the framework of biological and medical sciences, and particularly for orthopedic applications and devices (prostheses, implants, surgical instruments, …), titanium substrates covered by tantalum oxide/carbon nanotube composite coatings have proved to constitute interesting and successful platforms for the conception of solid and biocompatible biomaterials inducing the osseous regeneration processes (hydroxyapatite growth, osteoblasts attachment). This paper describes an original strategy for the conception of resistant and homogeneous tantalum oxide/carbon nanotubes layers on titanium through the introduction of carbon nanotubes functionalized by phosphonic acid moieties (P(O)(OH)₂). Strong covalent CP bonds are specifically inserted on their external sidewalls with a ratio of two phosphonic groups per anchoring point. Experimental results highlight the stronger “tantalum capture agent” effect of phosphonic-modified nanotubes during the sol–gel formation process of the deposits compared to nanotubes bearing oxidized functions (OH, CO, C(O)OH). Particular attention is also paid to the relative impact of the rate of functionalization and the dispersion degree of the carbon nanotubes in the coatings, as well as their wrapping level by the tantalum oxide matrix material. The resulting effect on the in vitro growth of hydroxyapatite is also evaluated to confirm the primary osseous bioactivity of those materials. Chemical, structural and morphological features of the different composite deposits described herein are assessed by X-ray photoelectron spectroscopy (XPS), scanning (SEM) and transmission (TEM) electronic microscopies, energy dispersive X-rays analysis (EDX) and peeling tests.     

Acid properties of NaH-mordenites: Infrared spectroscopic studies of ammonia sorption

Ammonia was used as a probe molecule to study the acid properties of NaH-mordenites. Ammonia reaches all acid sites in both large and narrow channels. The concentration of Bronsted sites (SiOHAl groups) and of Lewis acid sites was followed as a function of the Na/H exchange degree and the calcination temperature (extent of dehydroxylation). In NaH-mordenites of exchange degrees lower than 80%, the concentration of Bronsted sites was found to be practically the same as the theoretical value (the amount of Al minus the amount of Na). In H-mordenites of exchange degrees of 100%, the experimental value was 20% lower than the theoretical one. This difference was explained by a dehydroxylation that occurs during activation at 820 K. Studies of dehydroxylation have shown that bulk dehydroxylation starts at about 900 K. At 1050 K, most hydroxyls are lost, and the concentration of Lewis acid sites attains the maximal value, 4.5 sites/u.c. This value is comparable to the theoretical one, half of the Al content in H-mordenite (3.6 sites/u.c.). Variation of the OH stretching frequency with the Na/H exchange degree and with the extent of dehydroxylation suggests variation of the acid strength. This is discussed in the terms of the heterogeneity of SiOHAl groups in NaH-mordenites.     

NiB deposits on p-silicon using borohydride as a reducing agent

A solution, with various deposition parameters optimized to deposit electroless NiB films on p-silicon, has been developed, using sodium borohydride as the reducing agent. This has been done with a view to replace the existing silver–aluminum back contact for crystalline silicon solar cells with NiB films. The deposition has been studied by varying the temperature, time of deposition and the concentration of the reducing agent used, keeping the pH of the solution unchanged. Sheet resistance of the deposited films were measured to confirm the growth. Preliminary studies on contact resistance between NiB film and p-Si have been carried out.     

Whether do nano-particles act as nucleation sites for C-S-H gel growth during cement hydration?

In this study, three modelling experiments were designed to investigate whether nano-particles incorporated in the cement paste act as nucleation sites for CSH gel growth during cement hydration. The nano-particles with (nano-SiO₂) and without (nano-TiO₂) pozzolanic reactivity were used. In the first experiment, both the cement and nano-particles were dispersed in water to prepare dilute cement paste, in which the cement and nano-particles can contact each other. In the second one, the cement particles were laid inside a filter paper funnel and immersed in tap and ultrapure water with nano-particles dispersed, in order to separate the cement particles with nano-particles by using the filter paper. In the third one, large clinker particle was embedded in resin, surface-polished and then exposed upside down in ultrapure water with and without nano-particles dispersed. After hydration for 7 days, the hydration products in the paste or the nano-particle dispersion were observed by using TEM and the hydrated surface of the embedded clinkers were detected by using SEM. Based on the experimental results and the detailed discussions by using the classic nucleation theory, it was found that there may have no nucleus function of the nano-particles for the CSH gel precipitation during cement hydration, at least in the hydrating system with nano-silica and nano-TiO₂ addition. It was proposed to more reasonably explain the observations in the three modelling experiments by using the topochemical reaction instead of the through-solution mechanism for the CSH gel formation.     

Luminescence and scintillation properties of BaF2Ce transparent ceramic

Cerium doped Barium Fluoride (BaF₂Ce) transparent ceramic was fabricated and its luminescence and scintillation properties were studied. The photoluminescence shows the emission peaks at 310 nm and 323 nm and is related to the 5d-4f transitions in Ce³⁺ ion. Photo peak at 511 keV and 1274 keV were obtained with BaF₂Ce transparent ceramic for Na-22 radioisotopes. Energy resolution of 13.5% at 662 keV is calculated for the BaF₂Ce transparent ceramic. Light yield of 5100 photons/MeV was recorded for BaF₂Ce(0.2%) ceramic and is comparable to its single crystal counterpart. Scintillation decay time measurements shows fast component of 58 ns and a relatively slow component of 434 ns under 662 keV gamma excitation. The slower component in BaF₂Ce(0.2%) ceramic is about 200 ns faster than the STE emission in BaF₂ host and is associated with the dipole-dipole energy transfer from the host matrix to Ce³⁺ luminescence center.     

CO2 reduction to CH4 with H2 on photoirradiated TS-1

CO₂ reduction on reduced titanium silicalite (TS-1) with photoirradiation in the presence of H₂ was investigated in a closed circulation system. CO₂ was reduced to give CH₄ under u.v. irradiation, which TS-1 absorbs. The amount of the carbon species on TS-1 after photoirradiation indicated that all Ti atoms in the framework may act as a photocatalytic site. Infrared spectrum of TS-1 after the reaction showed that CH₂ and CH₃ were left on TS-1.     

Fibroblast functionality on novel Ti30Ta nanotube array

In this study, the mechanical substrate and topographical surface properties of anodized Ti30Ta alloy were investigated using scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS) and contact angle measurement. The anodization process was performed in an electrolyte solution containing HF (48%) and H₂SO₄ (98%) in the volumetric ratios 1:9 with the addition of 5% dimethyl sulfoxide (DMSO) at 15 V, 25 V and 35 V for 20 and 40 min, producing a nanotube architecture when anodized at 35 V for 40 min. Human dermal fibroblasts (HDF, neonatal) were utilized to evaluate the biocompatibility of Ti30Ta nanotubes and Ti30Ta alloy after 1 and 3 days of culture. Cellular adhesion, proliferation, viability, cytoskeletal organization and morphology were investigated using fluorescence microscope imaging, biochemical assay and SEM imaging respectively. The results presented identify altered material properties and improved cellular interaction on Ti30Ta nanotubes as compared to Ti30 Ta alloy.     

Room temperature solid–solid reaction preparation of ironboron alloy nanoparticles and Mössbauer spectra

The amorphous ironboron alloy can be prepared very easily by a room temperature solid–solid reaction of the FeCl₃·6H₂O, CrCl₃·6H₂O and KBH₄ powders. The characterizations show that the product is mainly composed of amorphous ironboron alloy nanoparticles. ⁵⁷Fe Mossbauer spectra at 84 and 295 K show that there are three kinds of Fe-containing components in the sample. There are the superparamagnetic relaxation in Mössbauer spectra and the continuous distribution of internal magnetic field in the ironboron alloy.     

Characteristics evaluation of calcium carbonate particles modified by surface functionalization

Calcium carbonate (CaCO₃) particles were modified by a direct blending method using different coupling agents. The changes in the CaCO₃ particles were determined using different techniques. Compared with pristine particles, the modified CaCO₃ particles show good dispersion, particularly those modified by γ-methacryloxypropyl trimethoxy silane. Results of the thermogravimetric analysis indicated that the coupling agents were adsorbed or anchored on the surface of the CaCO₃ particles, thereby hindering aggregation. The formation of covalent bonds [CaOSi] or [CaOTi] was verified using Fourier transform infrared spectroscopy and X-ray diffraction. The modified CaCO₃ particles showed more stable colloidal dispersion in ethyl acetate than that of pristine CaCO₃ particles. Some silane or titanate coupling agents can be combined with CaCO₃ by covalent bonds, thereby changing the surface properties of CaCO₃ and enhancing dispersion in many organic media. The hydroxyl groups on the surface of CaCO₃ particles can interact with silanol groups or titanate coupling agents forming an organic coating layer.     

Surface aspects of discolouration in Bisphenol A Polycarbonate (BPA-PC), used as lens in LED-based products

The surface-related reactions during discolouration of Bisphenol A Polycarbonate (BPA-PC), used as LED lens plates, under thermal stress are studied. X-ray photoelectron spectroscopy (XPS) has been used to monitor the changes in the surface chemistry of BPA-PC plates over a temperature range of 100–140 °C for a period up to 3000 h. Increasing time under thermal stress is associated with the discolouration, and increase in the yellowing index (YI) of PC plastic lens. The XPS results show that discolouration is associated with oxidation at the surface, finding a significant increase in the signal ratio O_1s/C_1s in the XPS spectra of degraded specimens. During thermal ageing, the CH concentration decreases and new oxide features CO and OCO form, with the latter being a support for oxidation at the surface being a major reaction during discolouration. Results also show that irradiation with blue light during thermal ageing accelerates the kinetics of discolouration and the increased O_1s/C_1s ratio in XPS spectra.     

Studies on optimization of silica nanoparticles dosage in cementitious system

Optimization of silica nanoparticles (SNPs) dosage in cementitious system was carried out analytically as well as experimentally by understanding the early stage hydration reaction of tricalcium silicate (C₃S). XRD and TGA results show the maximum nucleation effect of SNPs at 8 h, when the rate of product formation was higher than the control (∼66% additional CSH and ∼61% more CH with 10% SNPs addition). While at 24 h of hydration, ∼25% additional CSH was formed and CH content reduced by ∼32% with 10% addition showing the pozzolanic effect of SNPs. Further, FTIR results reveal that SNPs accelerate the polymerization in silicate chain and with 10% SNPs addition more crystalline (probably tobermorite like) structure is formed. This is responsible for the formation of highly compact and dense microstructure at 24 h as observed in electron micrographs, which may be responsible for the slow hydration rate at later age. XRD, FTIR and TGA studies on C₃S revealed that up to 5% addition of SNPs is beneficial, whereas higher dosages do not contribute significantly. Based on these investigations, studies were performed on cement paste, mortar and concrete samples, which revealed that 2–3% addition of SNPs is the optimum quantity for significant contribution in strength properties.     

Effects of He (90%)/H2 (10%) plasma treatment on electric properties of low dielectric constant SiCOH films

In microelectronics industry, integration of the low dielectric constant (low-k) material films is a continuing issue due to the decreasing device feature size. To improve electric properties, various post-deposition treatments of the low-k material films can be used. In this work, we used room temperature treatment of He/H₂ plasma and investigated the effects of plasma treatment on the electrical properties of low-k SiOCH films. Plasma treatment time changed from 300 to 1800 s. After treatment, the dielectric constant was decreased from 2.9 to 2.48, and the thickness of the low-k SiCOH films changed by only ～5%. The leakage current densities of the low-k SiCOH films were decreased to ～10^?11 A/cm², with treatment time ≥600 s. The breakdown occurred only around 2 V for films plasma-treated for 600 and 900 s. However, for 1800 s treatment time, the breakdown voltage was enhanced dramatically and breakdown occurred at applied voltage higher than 40 V. The surface composition change of the films after treatment was investigated by X-ray photoelectron spectroscopy (XPS). As the plasma treatment time was increased, the intensities of CC/CH and CSi peaks were decreased while the intensities of SiO and CO peaks were increased. It is thought that increase of oxygen content of the SiCOH film, after plasma treatment, contributed to leakage current reduction and breakdown voltage increase.     

Strength and fracture toughness of Ti5Al2.5Sn ELI alloy at cryogenic temperatures

The mechanical properties of a Ti5Al2.5Sn ELI alloy and its weldment were determined at 293, 77 and 4 K The alloy had a yield strength of 1400MPa and fracture toughness of 90 MPa m^½ at 4 K The tungsten-inert gas (TIG) welding resulted in a decrease in ductility and fracture toughness due to oxygen contamination. There was no brittle failure but a peculiar fracture facet was observed at cryogenic temperatures. This is called a ‘groove’ facet where discussed in the text The groove is a ductile fractured surface and its formation is closely related to mechanical twinning.