A simple method to ameliorate hierarchical porous structures of SiO2 xerogels through adjusting water contents

In this contribution, hierarchical micro-/meso-porous SiO₂ xerogels were successfully prepared through a Stöber methodology coupled with following drying process. The SiO₂ xerogels were consisted of nanoparticles of 20–40 nm in size with different contents of water. Fourier transform infrared spectroscopy proved that SiOC₂H₅ and SiOH groups could be formed in SiO₂ xerogels. Further analyses declared that the amount of the SiOC₂H₅ groups decreased while the concentration of SiOH was firstly increased and then suffered a decline with improving contents of water. Besides, the SiO₂ xerogels was endowed with controllable micro-/meso-porous structure. Furthermore, the formation mechanism of the micro-/meso-porous SiO₂ xerogels was tentatively put forward. As a consequence, SiO₂ xerogels with controllable hierarchical micro-/meso-porous structure could act as the smart material for huge development in catalytic fields.     

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.     

Luminescence at 1.53 μm for a new Er3+-doped transparent oxyfluoride glass ceramic

Transparent 45SiO₂25Al₂O₃5CaO10NaF15CaF₂ glass ceramics doped with different levels of Er³⁺ were prepared. The spherical CaF₂ nanocrystals with 10–20 nm in size were verified to be homogeneously embedded among the glassy matrix. Room temperature absorption and emission spectra corresponding to ⁴I_13/2 ↔ ⁴I_15/2 transitions of Er³⁺ ions in precursor glasses and glass ceramics, respectively had been measured. For glass ceramics, with increasing of Er³⁺ content from 0.1 to 2.0 mol%, the FWHM values of the emission bands increased from 42 to 71 nm; meanwhile, the lifetime of ⁴I_13/2 level slightly reduced. However, both the values of FWHM and lifetime were larger than those of precursor glasses due to the change of ligand field of Er³⁺ ions.     

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.     

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.     

Optical properties of TiO2 and disperse red-19 composite

Characteristic absorption and photoluminescence (PL) of TiO₂ and disperse red-19 (DR-19) composite have been investigated. Two step synthetic processes were employed to incorporate the DR-19 to the TiO₂ sol–gel. Firstly, urethane bonds between the DR-19 (OH) and 3-isocyanatopropyl triethoxysilane (ICPTES, NCO) were fabricated (ICPDR) prior incorporation to the TiO₂ sol–gel. Secondary, hydrolysis of the ethoxy group from the ICPDR and condensation reaction between silanol groups from ICPDR and TiO₂ sol–gel were performed by adding ICPDR to the TiO₂ sol–gel and aged for several days at room temperature (ICPDRTiO₂). There was no absorption peak shift with increasing the DR-19 concentration in methanol. However, UV–visible absorption band was shifted toward red approximately 0.09 eV for the ICPDRTiO₂ film, which indicated the formation of dimmer or more aggregates. The PL peaks of ICPDRTiO₂ were red-shifted compared with DR-19 in methanol (0.12 eV) and ICPDR film (0.09 eV). The relatively large emission peak shift toward red could be due to the fluorescence resonance energy transfer (FRET) between DR-19 and TiO₂ in ICPDRTiO₂ matrix.     

Synthesis,crystal structure,luminescent properties and photo degradation of mer-tris(8-Hydroxy-quinolinato-N,O)-indium(iii) hydrate 0.5 methanol solvate

Tris-(8-hydroxyquinioline) aluminium (Alq₃) is widely used in organic light emitting diodes as an emission and electron transport layer. In this study the effect of solvent molecules, in the solid state crystal lattice, on the photoluminescence properties of synthesized mer-tris(8-Hydroxy-quinolinato-N, O)-indium(iii) hydrate 0.5 methanol solvate (mer-[In(qn)₃]⋅H₂O⋅0.5 CH₃OH) was studied. Single crystals were obtained through a recrystallization process and single crystal X-ray diffraction was performed to obtain the unit cell structure. The main absorption peaks were assigned to ligand centered electronic transitions, while the solid state photoluminescence excitation peak at 440 nm was assigned to the 0–0 vibronic state of In(qn)₃. Broad emission at 510 nm was observed and was ascribed to the relaxation of an excited electron from the S₁–S₀ level. A powder sample was annealed at 130 °C for 2 h. A decrease in intensity was observed and could possibly be assigned to a loss of solvent species. To study the photon degradation, the sample was irradiated with an UV lamp for ∼15 h. The emission data was collected and the change in photoluminescence intensity with time was monitored. High resolution X-ray photoelectron spectroscopy (XPS) scans of the O-1s peak revealed that after annealing the binding energy shifted to lower energies indicating a possible loss of the H₂O and CH₃OH present in the crystal. The O-1s peak of the degraded sample indicated the possible formation of CO (∼532.5 eV), COH and OCOH (∼530.5 eV) on the phenoxide ring.     

Low-pressure-plasma-deposited coatings formed from mechanically alloyed powders

A limiting feature of the low-pressure-plasma-coating process at the present state of the art is the need for ?400 mesh (?37 μm) feed powder for the gun. In this study we demonstrated that mechanically alloyed MCrAltype (where M is cobalt, nickel or iron) powders suitable for low pressure plasma spraying can be prepared using the attritor process.A two-step attriting process was developed which yields a large fraction of ?400 mesh powders. A study of the effects of attritor processing parameters was made on Co29Cr6Al1Y powder that was mechanically alloyed from a blend of cobalt, chromium, CoAl and CoY powders. Coatings deposited onto IN-738 pin specimens by low pressure plasma spraying were hot corrosion tested; these compare favorably with Co29Cr6Al1Y coatings deposited using atomized powders.A three-step attriting process also was developed which is particularly useful in forming MCrAl-type powders using elemental aluminum as a starting ingredient.     

Effect of water content in sol on optical properties of hybrid sol–gel derived TiO2/SiO2/ormosil film

Sol–gel derived TiO₂/SiO₂/ormosil hybrid planar waveguides have been deposited on soda-lime glass slides and silicon substrates, films were heat treated at 150 °C for 2 h or dried at room temperature. Different amounts of water were added to sols to study their impacts on microstructures and optical properties of films. The samples were characterized by m-line spectroscopy, Fourier transform infrared spectroscopy (FT-IR), UV/VIS/NIR spectrophotometer (UV–vis), atomic force microscopy (AFM), thermal analysis instrument and scattering-detection method. The refractive index was found to have the largest value at the molar ratio H₂O/OR = 1 in sol (OR means OCH₃, OC₂H₅ and OC₄H₉ in the sol), whereas the thickest film appears at H₂O/OR = 1/2. The rms surface roughness of all the films is lower than 1.1 nm, and increases with the increase of water content in sol. Higher water content leads to higher attenuation of film.     

Nanoparticles of the giant dielectric material,calcium copper titanate from a sol–gel technique

The precursor of CaCu₃Ti₄O₁₂ (CCTO) nano particles have been successfully synthesized by sol–gel method at 90 °C. The dried precursor powder was milled and then calcined at 450 °C, 550 °C, 650 °C, 800 °C, 850 °C and 950 °C for 3 h. The phase formation of CCTO was analyzed by step by step using FTIR and XRD. Particle size and shape were evaluated by AFM. The XRD results of the powder calcined at 800 °C indicated the formation of CCTO phase. AFM studies showed that average particle size of the CCTO powder range 90–120 nm. The absorption bands corresponding to vibrations of CaO, CuO and TiOTi were observed at 606, 525 and 463 cm^? 1 using FTIR. The samples sintered at 1040 °C showed the densities as high as 96% of theoretical density. The grain sizes of sintered pellets were determined by FE-SEM. The dielectric properties of prepared samples were studied by LCR meter.     

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.     

Characterization of SiO2/Ag composite particles synthesized by in situ reduction and its application in electrically conductive adhesives

In the study, SiO₂/Ag composite particles with silver coating onto the surface of silica have been successfully prepared via a novel and facile approach (Oxidation–Reduction Method). In this approach, the SiO₂ particles were first modified with 3-ammoniatriethoxysilane (APTES) and glyoxalic acid (GA) through two-step reaction, the aldehyde group (CHO) were anchored onto the surfaces of silica spheres via electrostatic attraction, these [Ag(TEA)₂]⁺ ions in the solution were then reduced by the CHO and coated onto the surface of silica to obtain SiO₂/Ag composite particles. The effects of the reaction conditions on silver content and synthetic mechanism had also been discussed. The structure, morphology and optical properties of the SiO₂/Ag composite particles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and UV–vis spectroscopy. The results showed the surface of SiO₂ was surrounded by pure silver nanoparticles, and the silver nanoparticles had face-centered-cubic structure, the SiO₂/Ag composite particles with core–shell morphology and special optical properties. And the small content SiO₂/Ag composite particles applied in electrically conductive adhesives (ECAs) improved the electrical bulk resistivity and tensile shear strength.     

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.     

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.     

Investigation on the film-coating mechanism of alumina-coated rutile TiO2 and its dispersion stability

The alumina and alumina-coated rutile TiO₂ samples were synthesized by the chemical liquid deposition method under various pH values and aging temperature. The prepared samples were characterized by X-ray diffraction (XRD), Transmission electron microscopy (TEM), ζ-potential as well as X-ray photoelectron spectroscopy (XPS). The relationship between pH values, the dispersion stability, crystalline types and microstructure of alumina-coated rutile TiO₂ samples were studied. It is indicated that the coating film exhibited amorphous hydrous alumina (at pH 3–7), boehmite (at pH 7–9) and bayerite (pH > 11), respectively. And the higher aging temperature was in favor of the elevation of boehmite content of coating film. As the boehmite content increased, the dispersion stability was gradually enhanced and the prepared sample exhibited optimum dispersion stability at pH 9 and aging temperature 200 °C, respectively. The increase of steric hindrance and electrostatic repulsion led to the promotion of dispersion stability via coating hydrous alumina film on the surface of rutile TiO₂. The detection of AlO and the significantly enhancement of AlOTi intensity confirmed that the film coating process should be main attributed to both chemical bonding and physical adsorption.     

Plasma- and vacuum-plasma-sprayed Cr3C2 composite coatings

Plasma- and detonation-sprayed chromium carbide-Nichrome coatings have long been used for applications requiring superior wear resistance at temperatures up to 820°C. The coatings are typically sprayed from mechanical blends of powder containing from 17 to 35 wt.% Nichrome. These coatings are susceptible to non-uniformity of microstructure because of segregation of the blended powders. Oxide formation occurs in both ambient atmosphere plasma and detonation-applied coatings.A new Cr₃C₂Nichrome composite powder was developed for application by the plasma and vacuum plasma processes. The developed material consists of 50 wt.% Cr₃C₂ clad with 50 wt.% 80-20 Nichrome. Unlike powder blends, each Cr₃C₂ powder particle is clad with an essentially continuous layer of Nichrome. The developed material is sized ?270 mesh + 5 μm.Coatings of the composite Cr₃C₂ material were sprayed using the conventional non-transferred arc plasma and the low pressure low oxygen vacuum plasma processes. These coatings were compared with coatings sprayed from a commercially available blend of 75 wt.% Cr₃C₂25wt.% Nichrome. Unlike the blend, the microstructure of both composite coatings showed Cr₃C₂ to be present as discrete second-phase particles embedded in the Nichrome matrix. The vacuum-plasma-sprayed composite coating showed no visible oxide. Macrohardness (Rockwell C hardness) and microhardness (diamond pyramid hardness for a load of 300 gf) readings of the conventionally sprayed coatings were 50 HRC and 600 HDP 300 respectively. The hardness values for the vacuum-plasma-sprayed composite were 60 HRC and 860 HDP 300. The abrasive slurry wear resistance of the conventionally sprayed composite was three times that of the blend, while the wear resistance of the vacuum-plasma-sprayed composite was four times that of the standard blend coatings.The air-plasma-sprayed composite Cr₃C₂Nichrome coatings are expected to exhibit performance characteristics comparable with similar detonation-applied coatings. The vacuum-plasma-sprayed composite coatings combine superior wear resistance with low oxide and are recommended for severe high temperature wear environments.     

Surface modification on polyethylene terephthalate films with 2-methacryloyloxyethyl phosphorylcholine

In this study, the surface of polyethylene terephthalate (PET) was modified to improve the protein and cell adhesion behavior with low temperature ammonia plasma treatment followed by 2-methacryloyloxyethyl phosphorylcholine (MPC) grafting. The x-ray photoelectron spectroscopy (XPS) results showed that the COO^?, NCO and POH groups were successfully incorporated onto the sample surface after MPC grafting. Furthermore, formation of new bonds, N and NH on the sample surface grafted with MPC was recorded by Fourier transform infrared spectroscopy (FTIR). A large number of spherical particles at submicron to nanometer scale were also observed on the surface by atomic force microscopy (AFM). The cell adhesion experiments on PET film surfaces were evaluated and the highly hydrophilic surfaces could not promote cell adhesion and spreading. All results achieved in this study have clearly indicated that the method combining low temperature ammonia plasma treatment and MPC grafting is an effective way of producing a suitably hydrophilic PET surface with the capability of weakening the protein adsorption greatly.     

High efficiency visible-light-driven Fe2O3-xSx/S-doped g-C3N4 heterojunction photocatalysts: Direct Z-scheme mechanism

Several nanoporous Fe_2 O_3-xSx/S-doped g-C_3 N_4(CNS) Z-scheme hybrid heterojuctions have been successfully synthesized by one-pot in situ growth of the Fe_2O_3-xSx particles on the surface of CNS. The characterization results show that S-doping in the g-C3 N4 backbone can greatly enhance the charge mobility and visible light harvesting capability. In addition, porous morphology of hybrid composite provides available open pores for guest molecules and also improves light absorbing property due to existence of multiple scattering effects. More importantly, the Fe_2 O_3-xSx nanoparticles formed intimate heterojunction with CNS and developed the efficient charge transfer by extending interfacial interactions occurred at the interfaces of both components. It has been found that the Fe_2 O_3-xSx/CNS composites have an enhanced photocatalytic activity under visible light irradiation compared with isolated Fe_2 O_3 and CNS components toward the photocatalytic degradation of methylene blue(MB). The optimal loaded Fe_2 O_3-xSx value obtained is equal to 6.6 wt% that provided 82% MB photodegradation after 150 min with a reaction rate constant of 0.0092 min~(-1) which was faster than those of the pure Fe_2 O_3(0.0016 min~(-1))and CNS(0.0044 min~(-1)) under the optimized operating variables acquired by the response surface methodology. The specific surface area and the pore volume of Fe_2 O_3(6.6)/CNS hybrid are 33.5 m~2/g and0.195 cm~3/g, which are nearly 3.8 and 7.5 times greater compared with those of the CNS, respectively. The TEM image of Fe_2 O_3(6.6)/CNS nanocomposite exhibits a nanoporous morphology with abundant uniform pore sizes of around 25 nm. Using the Mott-Schottky plot, the conduction and valence bands of the CNS are measured(at pH = 7) equal to-1.07 and 1.48 V versus normal hydrogen electrode(NHE), respectively.Trapping tests prove that ·OH-and ·O_2-radicals are major active species in the photocatalytic reaction.It has been established that formation of the Z-scheme Fe_2 O_3(6.6)/CNS heterojunction between CNS and Fe_2 O_3 directly produces ·OH as well as ·O_2-radicals which is consistent with the results obtained from trapping experiments.