Bioactivity of CaSiO<Subscript>3</Subscript>/poly-lactic acid (PLA) composites prepared by various surface loading methods of CaSiO<Subscript>3</Subscript> powder

Mixing bioactive ceramic powders with polymers is an effective method for generating bioactivity to the polymer-matrix composites but it is necessary to incorporate up to 40 vol% of bioactive ceramic powder. However, such a high mixing ratio offsets the advantages of the flexibility and formability of polymer matrix and it would be highly advantageous to lower the mixing ratio. Since surface loading of ceramic powders in the polymer is thought to be an effective way of reducing the mixing ratio of the ceramic powder while maintaining bioactive activity, CaSiO₃/poly-lactic acid (PLA) composites were prepared by three methods; (1) casting, (2) spin coating and (3) hot pressing. In methods (1) and (2), a suspension was prepared by dissolving PLA in chloroform and dispersing CaSiO₃ powder in it. The suspension was cast and dried to form a film in the case of method (1) while it was spin-coated on a PLA substrate in method (2). In method (3), CaSiO₃ powder was surface loaded on to a PLA substrate by hot pressing. The bioactivity of these samples was investigated in vitro using simulated body fluid (SBF). Apatite formation was not observed in the samples prepared by method (1) but some apatite formation was achieved by mixing polyethylene glycol (PEG) with the PLA, producing a porous polymer matrix. In method (2), apatite was clearly observed after soaking for 7 days. Enhanced apatite formation was observed in method (3), the thickness of the resulting apatite layers becoming about 20 μm after soaking for 14 days. Since the amount of CaSiO₃ powder used in these samples was only ≤0.4 vol%, it is concluded that this preparation method is very effective in generating bioactivity in polymer-matrix composites by loading with only very small amounts of ceramic powder.     

Ti<Subscript>3</Subscript>SiC<Subscript>2</Subscript>/TiC composites prepared by PDS

Synthesis of composite materials with improved mechanical properties is considered. Pulse discharge sintering (PDS) technique was utilized for consolidation and synthesis of double phase Ti₃SiC₂/TiC composites from the initial powders TiH₂/SiC/TiC. Scanning electron microscopy with energy-dispersive spectrometry (SEM with EDS) and X-ray diffractometry (XRD) were exploited for the analysis of the microstructure and composition of the sintered specimens. Mechanical tests showed high bending and compression strength and low Vickers hardness of Ti₃SiC₂-rich specimens. The reasons of this behaviour are in the features of the textured microstructure of Ti₃SiC₂ phase.     

Crack propagation in layered Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/ZrO<Subscript>2</Subscript> composites prepared by electrophoretic deposition

Crack propagation through layered Al₂O₃/ZrO₂ composites was studied. The specimens were prepared via electrophoretic deposition of alumina and zirconia powders from suspensions with monochloroacetic acid and isopropanol. The kinetics of electrophoretic deposition could be described fully if the electrophoretic mobility and conductivity of suspensions were known. The conductivity of suspensions increased in the course of deposition. Adjusting to properly controlled kinetics of deposition and sintering, deposits were prepared with strongly bonded layers of different pre-defined thicknesses and, consequently, with different magnitudes of residual stress. Cracks, produced by an indentation technique, propagated askew towards layer interfaces deflected towards the interface in the Al₂O₃ layers and away from the interface in the ZrO₂ layers. Changes in the direction of crack propagation were described for the whole range of angles of incidence (0°–90°). The biggest change in the crack propagation was observed for the angle of incidence 45° and was ca. 15°, irrespective of the magnitude of residual stress in the layers.     

Tribological and mechanical behaviour of dual-particle (nanoclay and CaSiO<Subscript>3</Subscript>)-reinforced E-glass-reinforced epoxy nanocomposites

An E-glass-reinforced epoxy-based nanocomposite containing organomodified nanoclay (15–20 nm) and calcium silicate particles (75–149 μm) was developed through mechanical shearing mixing and hand layup techniques. Three weight fractions (2, 3 and 4%) of nanoclay were selected to study the effects of nanoclay on mechanical and wear behaviour of nanocomposites. Tensile and flexural properties of nanocomposites were evaluated and compared. The wear properties were evaluated for three speed (3.14, 4.19 and 5.24 m s^?1) and load (20, 50, and 80 N) conditions based on a design of experiment (L16 matrix) concept. The wear loss results were statistically analysed to study the significance of load, speed and nanoclay content. The morphologies of wear surface and fracture surface were examined with the aid of a scanning electron microscope (SEM) to identify the wear and fracture mechanisms. It was found that the wear loss increases with increasing nanoclay amount due to the particle agglomeration effects. Statistical analysis determines that the load is the most significant parameter affecting the wear resistance of nanocomposites. The mean and S/N ratio analyses rank the parameters significance in affecting wear resistance as follows: load > nanoclay content > speed. The wear mechanisms of nanocomposites are complex due to the observation of multiple features such as fibre thinning, matrix wear and fibre/matrix debonding as against abrasive wear in the pure epoxy. Tensile and flexural test results show that a good dispersion of nanoclay is achieved with 2 wt% amount in epoxy-based nanocomposites. The mechanical properties degrade above 2 wt% due to the excessive reinforcement, uneven distribution and the particle agglomeration effects. Fractography studies of tension-failed samples show that pure epoxy resin fails by multimode gauge explosive mode, whereas nanocomposites fail mainly by the matrix/fibre interface failure and fibre breakages.     

Preparation and characterization of Eu<Superscript>3+</Superscript> activated CaSiO<Subscript>3</Subscript>, (CaA)SiO<Subscript>3</Subscript> [A = Ba or Sr] phosphors

Eu³⁺ activated CaSiO₃, (Ca, Ba) SiO₃ and (Ca, Sr) SiO₃ have been prepared by sol-gel technique. Residual solvent and organic contents in the gel were removed by firing at 100°C for 3–4 h at 300 and 600°C for 2 h. Small exothermic shoulder around 850 to 875°C, as observed in DTA curve, corresponds to crystallization temperature of the doped calcium silicate. Influence of firing temperature on the luminescence of Eu³⁺ shows the maximum emission intensity in gel fired at 850°C. Photoluminescence emission peak is observed at 614 nm due to⁵D₀ →⁷F₂ transition of Eu³⁺ ion in (Ca, Ba) SiO₃ and (Ca, Sr) SiO₃ phosphors, when excited by 254 nm. The (Ca, Ba) SiO₃ material is proposed as an efficient red phosphor.     

Synthesis and structure of (NH<Subscript>4</Subscript>)<Subscript>3</Subscript>[UO<Subscript>2</Subscript>(CH<Subscript>3</Subscript>COO)<Subscript>3</Subscript>]<Subscript>2</Subscript>(NCS)

The compound (NH₄)₃[UO₂(CH₃COO)₃]₂(NCS) (I) was synthesized and examined by single crystal X-ray diffraction analysis. The compound crystallizes in the rhombic system with the unit cell parameters a = 11.5546(4), b = 18.5548(7), c = 6.7222(3) Å, V = 1441.19(10) ų, space group P2₁2₁2, Z = 2, R = 0.0345. The uranium-containing structural units of crystals of I are isolated mononuclear groups [UO₂(CH₃COO)₃]^? belonging to crystal-chemical group AB ₃ ⁰¹ (A = UO ₂ ²⁺ , B⁰¹ = CH₃COO^?) of uranyl complexes. The specific features of packing of the uranium-containing complexes in the crystal structure are considered.     

Si<Subscript>3</Subscript>N<Subscript>4</Subscript>/TiN composites produced from TiO<Subscript>2</Subscript>-Modified Si<Subscript>3</Subscript>N<Subscript>4</Subscript> powders

Si₃N₄/TiN composites have been produced by hot pressing at temperatures from 1600 to 1800°C in a nitrogen atmosphere, using silicon nitride powders prepared by self-propagating high-temperature synthesis and surface-modified with titanium dioxide nanoparticles. We examined the effect of TiO₂ content on the microstructure, phase composition, and mechanical strength of the ceramics. It is shown that titanium nitride can be formed by the reaction Si₃N₄ + TiO₂ → TiN + NO + N₂O + 3Si. The Si₃N₄/TiN composites containing 5–20% TiN have a low density, high porosity, and a bending strength of 60 MPa or lower. In Si₃N₄/TiN ceramics produced using calcium aluminates as sintering aids, the silicon nitride grains are densely packed, which ensures an increase in strength to 650 MPa.     

Preparation of magnetic composites through SrO-Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-B<Subscript>2</Subscript>O<Subscript>3</Subscript> glass crystallization

Glasses with nominal compositions 11SrO · 5.5Fe₂O₃ · 4.5Al₂O₃ · 4B₂O₃ (1) and 15SrO · 5.5Fe₂O₃ · 4.5Al₂O₃ · 4B₂O₃ (2) were prepared by rapidly quenching oxide melts between counterrotating steel rollers. The glasses were then heat-treated in the range 650–950°C to produce glass-ceramic samples. The samples were characterized by X-ray diffraction, electron microscopy, and magnetic measurements. The phase composition of the glass-ceramics was determined, and their microstructure and magnetic properties were studied. The annealing temperature was shown to have a strong effect on the coercivity of the materials, which reaches 650 and 570 kA/m for compositions 1 and 2, respectively.     

Preparation and characterization of porous Si<Subscript>3</Subscript>N<Subscript>4</Subscript> ceramics prepared by compression molding and slip casting methods

Porous silicon nitride (Si₃N₄) ceramics were fabricated by compression molding and slip casting methods using petroleum coke as pore forming agent, and Y₂O₃-Al₂O₃ as sintering additives. Microstructure, mechanical properties and gas permeability of porous Si₃N₄ ceramics were investigated. The mechanical properties and microstructure of porous Si₃N₄ ceramics prepared by compression molding were better than those which were prepared by slip casting method, whereas slip casting method is suitable for the preparation of porous Si₃N₄ ceramics with higher porosity and excellent gas permeability.     

Y<Subscript>2</Subscript>O<Subscript>3</Subscript> and Nd<Subscript>2</Subscript>O<Subscript>3</Subscript> co-stabilized ZrO<Subscript>2</Subscript>-WC composites

Y₂O₃ + Nd₂O₃ co-stabilized ZrO₂-based composites with 40 vol% WC were fully densified by pulsed electric current sintering (PECS) at 1350 °C and 1450 °C. The influence of the PECS temperature and Nd₂O₃ co-stabilizer content on the densification, hardness, fracture toughness and bending strength of the composites was investigated. The best combination of properties was obtained for a 1 mol% Y₂O₃ and 0.75 mol% Nd₂O₃ co-stabilized composite densified for 2 min at 1450 °C under a pressure of 62 MPa, resulting in a hardness of 15.5 ± 0.2 GPa, an excellent toughness of 9.6 ± 0.4 MPa.m^0.5 and an impressive 3-point bending strength of 2.04 ± 0.08 GPa. The hydrothermal stability of the 1 mol% Y₂O₃ + 1 mol% Nd₂O₃ co-stabilized ZrO₂-WC (60/40) composites was compared with that of the equivalent 2 mol% Y₂O₃ stabilized ceramic. The double stabilized composite did not degrade in 1.5 MPa steam at 200 °C after 4000 min, whereas the yttria stabilized composite degraded after less than 2000 min. Moreover, the (1Y,1Nd) ZrO₂-WC composites have a substantially higher toughness (~9 MPa.m^0.5) than their 2Y stabilized equivalents (~7 MPa.m^0.5).     

Nanostructured phase formation in CeO<Subscript>2</Subscript>/LaAlO<Subscript>3</Subscript> and CeO<Subscript>2</Subscript>/(Ni-W) prepared by deposition from metalorganic solutions

We have studied nanoscale structural evolution processes and phase formation in barrier cerium oxide layers grown from methacrylate solutions on lanthanum aluminate and a nickel-tungsten tape by dip coating. The layers were characterized by atomic force microscopy, scanning electron microscopy, precision electron diffraction, X-ray microanalysis, and X-ray diffraction (including texture analysis). We have investigated nanostructured morphological forms of buffer cerium oxide layers in all synthesis steps: liquid-phase, pyrolytic, and crystalline. We have established a granular character of the nanostructure and determined the type of orientation of the films: 〈111〉 texture with a 〈200〉 additional orientation. Optimal conditions for the synthesis of a barrier layer several tens of nanometers in thickness are proposed.     

Microwave absorption characteristics of CH<Subscript>3</Subscript>NH<Subscript>3</Subscript>PbI<Subscript>3</Subscript> perovskite/carbon nanotube composites

The CH₃NH₃PbI₃ (MAPbI₃) and CH₃NH₃PbI₃/carbon nanotube (MC) composite have been successfully synthesized by a facile in situ solution method, which are investigated as the microwave absorption materials. For the MAPbI₃ particles, the minimum reflection loss is only ?4.9 dB around 16.4 GHz due to the poor relative complex permittivity. Then, the relative complex permittivity of MC composites could be adjusted by changing the mass fraction of CNTs in composite, which is a vital role for the dielectric loss. The reflection loss of MC-5 composite (MAPbI₃/CNT, 5:1 wt%) can be improved to ?35.7 dB with thickness of 1.3 mm at 13.1 GHz. When the thickness is <3.0 mm, the microwave absorption bandwidth of MC-5 is 11.8 GHz (5.0–16.8 GHz) under the reflection loss lower than ?20 dB. The quarter-wavelength (λ/4) matching model is used to discuss the microwave absorption mechanism of MC composites. These results indicate that MC-5 composite could be used as the microwave absorption materials with strong reflection loss, lightweight and broad bandwidth.     

Emission analysis of Pr<Superscript>3+</Superscript> &; Ho<Superscript>3+</Superscript>: Ca<Subscript>4</Subscript>GdO(BO<Subscript>3</Subscript>)<Subscript>3</Subscript> powder phosphors

Emission spectral results of Pr³⁺ & Ho³⁺ ions doped Ca₄GdO(BO₃)₃ powder phosphors are reported here. XRD, SEM and FTIR measurements have been carried out for them. The emission spectrum of Pr³⁺: Ca₄GdO(BO₃)₃ has shown an emission transition ¹D₂ → ³H₄ at 606 nm with λ_exci = 480 nm (³H₄ → ³P₀) and Ho³⁺: Ca₄GdO(BO₃)₃ phosphor has shown an emission transition ⁵S₂ → ⁵I₈ at 549 nm with λ_exci = 447 nm (⁵I₈ → ⁵F₁). Emission performances of these two phosphors have been explained in terms of energy level diagrams.     

Electromagnetic properties of low-temperature-sintered (Ba<Subscript>0.6</Subscript>Sr<Subscript>0.4</Subscript>)TiO<Subscript>3</Subscript>/NiCuZn composites

Dense (Ba_0.6Sr_0.4)TiO₃/Ni_0.37Cu_0.20Zn_0.43Fe_1.92O_3.88 (BST/NiCuZn) composites were prepared by the conventional solid-state reaction method and sintered at 1,050°C. The phase composition and surface morphology of the composites were investigated using XRD and SEM, respectively. The dielectric and magnetic properties of the composites were also reported. In low frequency range the dielectric properties of the BST/NiCuZn composites show Maxwell–Wagner relaxation. In high frequency range the BST/NiCuZn composites possess high dielectric constants and permeabilities, which can be used in high-frequency communications for capacitor-inductor integrating devices such as electromagnetic interference filters and antennas.     

Structure and properties of Ba(Zr<Subscript>0.2</Subscript>Ti<Subscript>0.8</Subscript>)O<Subscript>3</Subscript> ceramics prepared by spark plasma sintering

Ba(Zr_0.2Ti_0.8)O₃ (BZT) ceramics are prepared from spray-dried powder by spark plasma sintering (SPS) and by normal sintering. By the application of SPS, ceramics with >96% relative densities could be obtained by sintering at 1,100 °C for 5 min in air atmosphere. The pellet as sintered by SPS at 1,100 °C was black and conductive. Although SPS was carried out in air atmosphere, the samples were deoxidized by heating the carbon die. By post-annealing at 1,000 °C for 12 h in air, the pellet was oxidized and became white and insulating. Grain growth was suppressed in the ceramics prepared by SPS, and the average grain size was 0.52 μm. The starting powder contained 1.90% carbon, mainly as binder, and the SPS-prepared ceramics and ordinary prepared ceramics contained 0.15 and 0.024% carbon, respectively. The BZT ceramics obtained by SPS and the subsequent annealing at 1,000 °C for 12 h exhibited a mild temperature dependence of their dielectric constant. The field-induced displacement of the BZT ceramics was less hysteretic and smaller than that of the ceramics sintered by the conventional method.     

Phase composition and microstructure of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-Cr<Subscript>2</Subscript>O<Subscript>3</Subscript> solid solutions prepared by self-propagating high-temperature synthesis

The combustion synthesis, microstructure, chemical composition, and phase composition of cast Al₂O₃-Cr₂O₃ materials are described. The synthesized solid solutions are based on corundum or chromia, depending on the Al₂O₃ and Cr₂O₃ contents. Using self-propagating high-temperature synthesis, a cast aluminum oxynitride is obtained for the first time.     

Magnetic and ferroelectric properties of SmBi<Subscript>4</Subscript>Fe<Subscript>0.5</Subscript>Co<Subscript>0.5</Subscript>Ti<Subscript>3</Subscript>O<Subscript>15</Subscript> compounds prepared with different synthesis methods

The SmBi₄Fe_0.5Co_0.5Ti₃O₁₅ compounds were prepared by the insertion of the SmFe_0.5Co_0.5O₃ into the Bi₄Ti₃O₁₂ host and the conventional solid state reaction method, respectively. X-ray diffraction analysis indicates that the conventional solid state reaction method favors the formation of a single phase four-layer Aurivillius phase of SmBi₄Fe_0.5Co_0.5Ti₃O₁₅ more easily than that prepared by the insertion method. Magnetic and ferroelectric measurements demonstrate that the samples prepared by both methods exhibit coexistence of strong ferromagnetic and weak ferroelectric behaviors at room temperature. Compared with the Bi₅FeTi₃O₁₅, the ferromagnetism of the SmBi₄Fe_0.5Co_0.5Ti₃O₁₅ was dramatically enhanced by the partial substitution of Co for Fe and Sm for Bi. The SmBi₄Fe_0.5Co_0.5Ti₃O₁₅ samples exhibit large magnetic responses (2M _r ?~?643 memu/g and coercive fields 2H _c ?~?344 Oe) at room temperature.     

Effect of Al<Subscript>2</Subscript>O<Subscript>3</Subscript> on the properties of nanocrystalline ZrO<Subscript>2</Subscript> + 3 mol % Y<Subscript>2</Subscript>O<Subscript>3</Subscript> powder

We have studied the properties of nanocrystalline ZrO₂〈3 mol % Y₂O₃〉 and 90 wt % ZrO₂〈3 mol % Y₂O₃〉-10 wt % Al₂O₃ powders prepared via hydrothermal treatment of coprecipitated hydroxides at 210°C. The results demonstrate that Al₂O₃ doping raises the phase transition temperatures of the metastable low-temperature ZrO₂ polymorphs and that the structural transformations of the ZrO₂ and Al₂O₃ in the doped material inhibit each other.