Silver coated bioactive glass particles for wound healing applications

Bioactive glass particles (0.42SiO₂–0.15CaO–0.23Na₂O–0.20ZnO) of varying size (<90 μm and 425–850 μm) were synthesized and coated with silver (Ag) to produce Ag coated particles (PAg). These were compared against the uncoated analogous particles (Pcon.). Surface area analysis determined that Ag coating of the glass particles resulted in increased the surface area from 2.90 to 9.12 m²/g (90 μm) and 1.09–7.71 m²/g (425–850 μm). Scanning electron microscopy determined that the Ag coating remained at the surface and there was little diffusion through the bulk. Antibacterial (Escherichia coli—13 mm and Staphylococcus epidermidis—12 mm) and antifungal testing (Candida albicans—7.7 mm) determined that small Ag-coated glass particles exhibited the largest inhibition zones compared to uncoated particles. pH analysis determined an overall higher pH consider in the smaller particles, where after 24 h the large uncoated and Ag coated particles were 8.27 and 8.74 respectively, while the smaller uncoated and Ag coated particles attained pH values of 9.63 and 9.35 respectively.     

A sol–gel-derived α-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> crystal interlayer modified 316L porous stainless steel to support TiO<Subscript>2</Subscript>, SiO<Subscript>2</Subscript>, and TiO<Subscript>2</Subscript>–SiO<Subscript>2</Subscript> hybrid membranes

A homogeneous α-Al₂O₃ crystal membrane was fabricated by the sol–gel technique on 316L porous stainless steel (PSS) substrate with an average pore size of 1.0 μm. The preparation process was optimized by carefully choosing the binder, the concentrations of the casting solutions and the sintering temperatures of the membranes. Compared to methylcellulose and polyethylene glycol 20000, polyvinyl alcohol 1750 was found to be the most effective binder to fabricate a homogeneously structured Al₂O₃ membrane without defects. The concentration to prepare an uniform coverage membrane with a thickness of ~10 μm was 0.032 mol/L. When sintered at 1000 °C, γ-Al₂O₃ membrane with ~3 μm grains was obtained. When sintered at 1200 °C, γ-Al₂O₃ completely transformed into α-Al₂O₃ and the grains grew to ~5 μm. Accordingly, the process was applied to a bigger pore-sized PSS with an average pore size of 1.5 μm to fabricate an α-Al₂O₃ intermediate layer to initially modify its surface. A single α-Al₂O₃ crystal layer with a thickness of ~5 μm and an average pore size of 0.7 μm was achieved. Subsequently, TiO₂, SiO₂, and TiO₂–SiO₂ hybrid membranes were tried on the modified PSS. Defect-free microfiltration membranes with average pore sizes of ~0.3 μm were readily fabricated. The results indicate that the sol–gel method is promising to initially modify the PSS substrates and the sol–gel-derived α-Al₂O₃ crystal layer is an appropriate intermediate layer to modify the PSS and to support smaller grain-sized top membranes.     

Cathodoluminescence properties of SiO<Subscript>2</Subscript>:Pr<Superscript>3+</Superscript>and ZnO·SiO<Subscript>2</Subscript>:Pr<Superscript>3+</Superscript> phosphor nanopowders

The successful incorporation of ZnO nanoparticles in Pr³⁺-doped SiO₂ using a sol–gel process is reported. SiO₂:Pr³⁺ gels, with or without ZnO nanoparticles, were dried at room temperature and annealed at 600 °C. On the basis of the X-ray Diffraction (XRD) results, the SiO₂ was amorphous regardless of the incorporation of Pr³⁺ and nanocrystalline ZnO or annealing at 600 °C. The particles were mostly spherical and agglomerated as confirmed by Field Emission Scanning Electron Microscopy. Thermogravimetric analysis of dried gels performed in an N₂ atmosphere indicated that stable phases were formed at ≥900 °C. Absorption bands ascribed to ³H₄-³P_{(J = 0,1,2)}, ¹I₆ and ¹D₂ in the UV–VIS region were observed from SiO₂:Pr³⁺ colloids. The red cathodoluminescent (CL) emission corresponding to the ³P₀ → ³H₆ transition of Pr³⁺ was observed at 614 nm from dried and annealed SiO₂:Pr³⁺ powder samples. This emission was increased considerably when ZnO nanoparticles were incorporated. The CL intensity was measured at an accelerating voltage of 1-5 keV and a fixed beam current of 8.5 μA. The effects of accelerating voltage on the CL intensity and the CL degradation of SiO₂:Pr³⁺ and ZnO·SiO₂:Pr³⁺ were also investigated using Auger electron spectroscopy coupled with an Ocean Optics S2000 spectrometer.     

Structure and photoluminescence of SiC/ZnO nanocomposites prepared by radio frequency alternate sputtering

SiC/ZnO nanocomposites were prepared by radio frequency alternate sputtering followed by annealing in N₂ ambient. Well-crystallized ZnO matrix was obtained after annealed at 750 °C according to X-ray diffractometer patterns. Transmission electron microscopy analyses indicated that the SiC thin layer aggregated to form SiC nanoclusters with the average size of 7.2 nm when the annealing temperature was 600 °C. When the annealing temperatures increased above 900 °C, some of the SiC nanoclusters changed into SiC nanocrystals and surfacial atoms of the SiC nanoparticles were surrounded by a layer of SiO _x (x ≤ 2) according to the Fourier transform infrared spectrums. The SiC/ZnO nanocomposites annealed at 750 °C exhibit strong photoluminescence bands ranging from 250 to 600 nm. UV light originates from the near band edge emission of ZnO and the blue emission peaked at around 465 nm (2.7 eV) may be due to the formation of emission centers caused by the defects in Si–O network, while the green-emission peak at around 550 nm (2.3 eV) may be attributed to the deep level recombination luminescence caused by the vacancies of oxygen and zinc.     

Fabrication of spherical CaO–SrO–ZnO–SiO2 particles by sol–gel processing

This study was concerned with the fabrication of ceramic CaO–SrO–ZnO–SiO₂ spherical particles, which are novel candidates for the glass phase in glass polyalkenoate cements (GPCs). GPCs made from these glasses have potential as bone cements because, unlike conventional GPCs, they do not contain aluminum ions, which inhibit the calcification of hydroxyapatite in the body. The glass phase of GPCs require a controllable glass morphology and particle size distribution. Sol–gel processing can potentially be used to fabricate homogenous ceramic particles with controlled morphology. However, a thorough study on preparation conditions of spherical CaO–SrO–ZnO–SiO₂ particles by sol–gel processing has, to date, not been reported. In this study, gels were prepared by hydrolysis and polycondensation of tetraethoxysilane (TEOS) in an aqueous solution containing polyethylene glycol and nitrates of calcium, strontium and zinc. It was possible to control the morphology and size of the gels by varying the H₂O/TEOS molar ratio and the metal ion content in the starting compositions. An aliquot of 3–5 μm homogenous spherical particles were obtained at a H₂O/TEOS molar ratio of 42.6 when the starting composition molar ratios were Sr(NO₃):Ca(NO₃)₂:Zn(NO₃)₂:Si(OC₂H₅)₄ = x:0.12:(0.40 − x):0.48 (0 ≤ x ≤ 0.8). Starting composition limitations are caused by the low solubility of strontium ions in the minimal amount of water used and the acceleration of hydrolysis as well as polycondensation at higher water content.     

Structured ZnO-based contacts deposited by non-reactive rf magnetron sputtering on ultra-thin SiO2/Si through a stencil mask

In this paper, we study the localized deposition of ZnO micro and nanostructures deposited by non-reactive rf-magnetron sputtering through a stencil mask on ultra-thin (10 nm) SiO₂ layers containing a single plane of silicon nanocrystals (NCs), synthetized by ultra-low energy ion implantation followed by thermal annealing. The localized ZnO-deposited areas are reproducing the exact stencil mask patterns. A resistivity of around 5 × 10^− 3 Ω cm is measured on ZnO layer. The as-deposited ZnO material is 97% transparent above the wavelength at 400 nm. ZnO nanostructures can thus be used as transparent electrodes for Si NCs embedded in the gate-oxide of MOS devices.     

Synthesis of β-SiC nanostructures via the carbothermal reduction of resorcinol–formaldehyde/SiO2 hybrid aerogels

The novel resorcinol–formaldehyde/SiO₂ (RF/SiO₂) hybrid aerogels were chosen to synthesize the cubic silicon carbide (β-SiC) nanostructures via a carbothermal reduction route. In this process, the in situ polymerized RF/SiO₂ aerogels were used as both the silicon and carbon sources. The morphologies and structures of SiC nanostructures were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), and high-resolution transmission electron microscope (HRTEM) equipped with EDS. The effects of C/Si atomic ratios in RF/SiO₂ aerogels and heat treatment temperatures on the formation of SiC nanomaterials were investigated in detail. It was shown that β-SiC nanowhiskers with diameters of 50–150 nm and high crystallinity were obtained at the temperatures from 1400 to 1500 °C. The role of the interpenetrating network of RF/SiO₂ hybrid aerogels in the carbothermal reduction was discussed and a possible mechanism was proposed.     

Nucleation and growth mechanism of apatite on a bioactive and degradable ceramic/polymer composite with a thick polymer layer

Nucleation and growth mechanism of apatite on a bioactive and degradable PLLA/SiO₂–CaO composite with a thick PLLA surface layer were investigated compared to that on a bioactive but non-degradable polyurethane (PU)/SiO₂–CaO composite with a thick PU surface layer. The bioactive SiO₂–CaO particles were made by a sol–gel method from tetraethyl orthosilicate and calcium nitrate tetrahydrate under acidic condition followed by heat treatment at 600 °C for 2 h. The PLLA/SiO₂–CaO and PU/SiO₂–CaO composites were then prepared by a solvent casting method which resulted in thick PLLA and PU surface layers, respectively, due to precipitation of SiO₂–CaO particles during the casting process. Two composites were exposed to SBF for 1 week and this exposure led to form uniform and complete apatite coating layer on the PLLA/SiO₂–CaO composite but not on the PU/SiO₂-CaO composite. These results were interpreted in terms of the degradability of the polymers. A practical implication of the results is that a post-surface grinding or cutting processes to expose bioactive ceramics to the surface of a composite with a thick biodegradable polymer layer is not required for providing apatite forming ability, which has been considered as one of the pragmatic obstacles for the application as a bone grafting material.     

Photoresponse of n -ZnO/ p -Si heterojunction towards ultraviolet/visible lights: thickness dependent behavior

A series of n-ZnO/p-Si thin film heterojunctions have been fabricated by a low cost sol–gel technique for different ZnO film thicknesses and the dark as well as photo current–voltage (I–V) characteristics have been investigated in details. The heterojunction with ZnO thickness of 0.46 μm shows the best diode characteristics in terms of rectification ratio, I _F/I _R = 5.7 × 10³ at 5 V and reverse leakage current density, J _R = 7.6 × 10⁻⁵ A cm⁻² at −5 V. From the photo I–V curves and wavelength dependent photocurrent of the heterojunctions, it is found that the junction with 0.46 μm ZnO thickness shows the highest sensitivity towards both UV and visible lights.     

RF sputtered piezoelectric zinc oxide thin film for transducer applications

This paper demonstrates the substrate dependency of the c-axis zinc oxide growth in radio-frequency sputtering system. Different deposition conditions were designed to study the influences of Si, SiO₂/Si, Au/Ti/Si, and Au/Ti/SiO₂/Si substrates on the piezoelectric and crystalline qualities of the ZnO thin films. Experimental results showed that the multilayer of Au/Ti/SiO₂/Si-coated silicon substrate provided a surface that facilitated the growth of ZnO thin film with the most preferred crystalline orientation. The 1.5 μm-thick thermally grown amorphous silicon dioxide layer effectively masked the crystalline surface of the silicon substrate, thus allowing the depositions of high-quality 20 nm-thick titanium adhesion layer followed by 150 nm-thick of gold thin film. The gold-coated surface allowed deposition of highly columnar ZnO polycrystalline structures. It was also demonstrated that by lowering the deposition rate at the start of sputtering by lowering RF power to less than one-third of the targeted RF power, a fine ZnO seed layer could be created for subsequent higher-rate deposition. This two-step deposition method resulted in substantially enhanced ZnO film quality compared to single-step approach. The influence of stress relaxation by annealing was also investigated and was found to be effective in releasing most of the residual stress in this layered structure.     

Effect of ZnO on the microstructure and electrical properties of (K<Subscript>0.5</Subscript>Na<Subscript>0.5</Subscript>)NbO<Subscript>3</Subscript> lead-free piezoelectric ceramics

K_0.5Na_0.5NbO₃–x ZnO (KNN–xZn) lead-free ceramics have been prepared using the conventional sintering technique and the effects of ZnO addition on the phase structure and piezoelectric properties of the ceramics have been studied. Our results reveal that a small amount of ZnO can improve the density of the ceramics effectively. Because of the high density and ZnO doping effects, the piezoelectric and dielectric properties of the ceramics are improved considerably. The good piezoelectric and dielectric properties of d ₃₃ = 114 pC/N, k _p = 0.36, ε _r = 395, and Q _m = 68 were obtained for the KNN ceramics doped with 1 mol% ZnO. Therefore, the KNN-1.0 mol%Zn ceramics is a good candidate for lead-free piezoelectric application.     

Effects of SrO–B2O3–SiO2 glass additive on the microstructure and dielectric properties of CaCu3Ti4O12

The effect of SrO–B₂O₃–SiO₂ glass additive (SBS) on the microstructure and dielectric properties of CaCu₃Ti₄O₁₂ (CCTO) ceramics was investigated. This SBS–added CCTO ceramics were prepared by the solid state reaction. The undesirable impurity phases Ca₃SiO₅ started appearing in the XRD patterns, suggesting a possible chemical reaction between CaTiO₃ and SiO₂ (the devitrification production of SBS glass). The SBS glass additive promoted the grain growth and densification of CCTO ceramics. Cole–Cole plots of conductance suggested that the resistivity grain boundary decreased with increasing amount of SBS glass (when x = 0–2 wt%), then increased (when x = 2–3 wt%). The addition of SBS glass was desirable to increase the dielectric constants (up to 10⁴) and lowered the dielectric losses of CCTO over the frequency range of 450–40 kHz at the relatively lower sintering temperature for relatively shorter sintering time (1,050 °C, 12 h).     

Structure and ferroelectric properties of stoichiometric and Sr-deficient–SrBi<Subscript>4</Subscript>Ti<Subscript>4</Subscript>O<Subscript>15</Subscript> thin films

SrBi₄Ti₄O₁₅ (SBTi) and Bi-excess and Sr-deficient SBTi (Sr-deficient SBTi, Sr_0.8Bi_4.13Ti₄O₁₅) thin films were deposited on Pt/Ti/SiO₂/Si (100) substrates using a sol–gel method. Structure and electric properties were investigated systematically. These films were random oriented. The remnant polarization (2P _r) of SBTi film was about 25.3 μC/cm², which was larger than the reported value of SBTi thin film. The film with Sr-deficient and Bi-excess composition showed a very large remnant polarization of 36.6 μC/cm². The capacitance–voltage (C–V) characteristics of both the films showed normal ferroelectric behavior. The Curie temperatures of the same Sr-deficient and Bi-excess component ceramics sample increased slightly in comparison with that of SBTi. More importantly, the Sr-deficient and Bi-excess SBTi thin film showed high fatigue resistance against continuous switching up to 4.4 × 10¹⁰ cycles.     

The ferroelectric properties and residual stress analysis of Bi<Subscript>3.15</Subscript>Nd<Subscript>0.85</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> thin films with a LaNiO<Subscript>3</Subscript> buffer layer

Bi_3.15Nd_0.85Ti₃O₁₂ (BNT) thin film with a thin LaNiO₃ film as buffer layer was fabricated by sol–gel method on Pt/TiO₂/SiO₂/Si substrate. The BNT thin films have a perovskite phase with a dense microstructure. The P _r and V _c value are 25.5 μc/cm² and 3.7 V, respectively under the applied voltage of 15 V. After the switching of 2 × 10⁹ cycles, the P _r value decreases to 86% of its pre-fatigue value. The leakage current density of the BNT thin films with LaNiO₃ buffer layer were generally in the order of 10⁻⁸ to 10⁻⁶ A/cm². The fatigue and leakage current properties were improved dramatically compared with the BNT film without a LaNiO₃ buffer layer that we prepared before. The measured residual stress was tensile stress and its value was 176 MPa.     

Influence of seed layers on the vertical growth of ZnO nanowires

We synthesized vertically aligned ZnO nanowires on SiO₂ wafer <100> using the Au, ZnO and Au/ZnO seed layers through the physical vapor deposition process. The growth direction of ZnO nanowire was controlled by using the three different seed layers. From the XRD results, we observed the highest intensity of the (002) peak on the Au/ZnO seed layer among the three seed layers. The SEM images show that all of the ZnO nanowires have an average diameter of about 100 ~ 200 nm and a length of about 5 μm, and the nanowires grown on the Au/ZnO seed layer are oriented the most perpendicularly to the substrate surface. From the PL analysis, we observed that the intensity of broad emissions at 400-600 nm relating the green emission for the ZnO nanowires on the Au/ZnO seed layer was much weaker than that for the ZnO nanowires on the ZnO seed layer. The experiment results indicate that the selection of seed layers is important to grow nanowires vertically for the application of nanoscale devices.     

Facile preparation of Ag/ZnO nanoparticles via photoreduction

Ag/ZnO nanoparticles can be obtained via photocatalytic reduction of silver nitrate at ZnO nanorods when a solution of AgNO₃ and nanorods ZnO suspended in ethyleneglycol is exposed to daylight. The mean size of the deposited sphere like Ag particles is about 5 nm. However, some of the particles can be as large as 20 nm. The ZnO nanorods were pre-prepared by basic precipitation from zinc acetate di-hydrate in the ionic liquid 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)amide. They are about 50–300 nm in length and 10–50 nm in width. Transmission electron microscopy (TEM), energy-dispersive X-ray analysis (EDS), X-ray powder diffraction (XRD), UV–Vis spectroscopy, X-ray photoelectron spectroscopy (XPS), and photoluminescence (PL) were used to characterize the resulting Ag/ZnO nanocomposites.     

In vitro remineralization of human dental enamel by bioactive glasses

Different compositions of silicate-based bioactive glasses of the system SiO₂–CaO–P₂O₅ (45S, 58S, and 77S) were evaluated for teeth remineralization effect on the etched human dental enamel in simulate human oral environment. Enamel samples were subjected to demineralization in citric acid solution, then treated with different bioactive glass pastes, and finally soaked in simulated oral fluid (SOF) for 7 days before evaluation. The results indicated that enamel surface formed a homogenous and dense mineralized layer with the treatment of 45S and 58S samples. The average thickness was 4 and 2.5 μm, respectively. But 77S treatment showed a loose and uneven remineralized layer. Although the surface roughness decreased with the increase of silicon content, mechanical strength of enamel samples became less gradually. Taken together, 45S paste had the best remineralization ability, best mechanical strength, and satisfactory surface roughness. These results also indicated that the level of silicon content of bioactive glasses played a key role in dental enamel remineralization.     

Structure and dielectric/piezoelectric properties of LiNbO3-doped BiScO3–PbTiO3 ceramics with morphotropic phase boundary composition

0.02LiNbO₃–0.98{(1 − x)BiScO₃–xPbTiO₃} (2LN–BS–xPT) ceramics near the morphotropic phase boundary (MPB) were investigated. MPB region of 2LN–BS–xPT ceramics was identified to be in the composition of 0.62 < x ≤ 0.64. The coexistence of the tetragonal domain structure and a polar microdomain structure was observed by transmission electron microscope for x = 0.64. It is found that 2LN–BS–xPT ceramics (x = 0.64) showed good piezoelectric and ferroelectric properties with piezoelectric constant d ₃₃ about 505 pC/N, planar electromechanical coupling factors k _p about 0.47, and remnant polarization P _r about 40 μC/cm², respectively, while T _max is about ~350–400 °C. The high-temperature relaxation behavior was also studied in 2LN–BS–xPT ceramics. Effects of thermal depoling on the piezoelectric properties of 2LN–BS–xPT ceramics indicated good thermal stability before 300 °C for x = 0.62 and 0.64.     

Effect of oxygen pressure of SiOx buffer layer on the electrical properties of GZO film deposited on PET substrate

The present work was made to investigate the effect of oxygen pressure of SiO_x layer on the electrical properties of Ga-doped ZnO (GZO) films deposited on poly-ethylene telephthalate (PET) substrate by utilizing the pulsed-laser deposition at ambient temperature. For this purpose, the SiO_x buffer layers were deposited at various oxygen pressures ranging from 13.3 to 46.7 Pa. With increasing oxygen pressure during the deposition of SiO_x layer as a buffer, the electrical resistivity of GZO/SiO_x/PET films gradually decreased from 7.6 × 10^− 3 to 6.8 × 10^− 4 Ω·cm, due to the enhanced mobility of GZO films. It was mainly due to the grain size of GZO films related to the roughened surface of the SiO_x buffer layers. In addition, the average optical transmittance of GZO/SiO_x/PET films in a visible regime was estimated to be ~ 90% comparable to that of GZO deposited onto a glass substrate.     

Rapid Thermal Annealing of ZnO Nanocrystalline Films for Dye-Sensitized Solar Cells

Nanocrystalline ZnO thin films were prepared by the sol–gel method and annealed at 600 °C by conventional (CTA) and rapid thermal annealing (RTA) processes on fluorine-doped tin oxide (FTO)-coated glass substrates for application as the work electrode for a dye-sensitized solar cell (DSSC). ZnO films were crystallized using a conventional furnace and the proposed RTA process at annealing rates of 5 °C/min and 600 °C/min, respectively. The ZnO thin films were characterized by X-ray diffraction (XRD) and atomic force microscopy (AFM) analyses. Based on the results, the ZnO thin films crystallized by the RTA process presented better crystallization than films crystallized in a conventional furnace. The ZnO films crystallized by RTA showed higher porosity and surface area than those prepared by CTA. The results show that the short-circuit photocurrent (J _sc) and open-circuit voltage (V _oc) values increased from 4.38 mA/cm² and 0.55 V for the DSSC with the CTA-derived ZnO films to 5.88 mA/cm² and 0.61 V, respectively, for the DSSC containing the RTA-derived ZnO films.