Porous titanium (Ti) scaffolds by freezing TiH2/camphene slurries

Porous titanium (Ti) scaffolds with interconnected pores were fabricated by freezing titanium hydride (TiH₂)/camphene slurries at 33 °C for 24 h, followed by freeze-drying and subsequent heat-treatment at 1300 °C for 2 h in vacuum. All of the fabricated samples revealed highly porous structures having large pores up to 100 μm in size surrounded by Ti metal walls without any secondary phases. When the initial TiH₂ content was increased from 15 to 25 vol.%, the porosity was decreased from 63 to 49%, while the compressive strength was significantly improved from 81 to 253 MPa.     

Compressive strength and processing of camphene-based freeze cast calcium phosphate scaffolds with aligned pores

Porous calcium phosphate (CaP) scaffolds with aligned pores were fabricated by unidirectionally freezing a CaP/camphene slurry at 32 °C for various times (1, 2, 3 days). During this process, camphene dendrites grew preferentially from the bottom to the top of the cast body. The frozen samples were then freeze-dried to remove the solid camphene and sintered at 1200 °C for 3 h to densify the CaP walls. All of the fabricated samples showed a highly aligned pore structure with a porosity of 62-65 vol.%, regardless of the freezing time. As the freezing time was increased from 1 to 3 days, the pore size increased from 122 to 166 μm due to the continual overgrowth of camphene dendrites, while the compressive strength decreased from 9.3 ± 1.6 to 6.2 ± 1.3 MPa due to the increase in pore size. However, it should be noted that the compressive strength of the sample tested parallel to the freezing direction was much higher than that of the sample tested normal to the direction of freezing, indicating the utility of the aligned pores.     

Highly porous hydroxyapatite bioceramics with interconnected pore channels using camphene-based freeze casting

We fabricated highly porous hydroxyapatite (HA) bioceramics using the camphene-based freeze casting method. In this method, HA/camphene slurries with various HA contents (10, 15, and 20 vol.%) were prepared by ball-milling at 60 °C and then cast into a mold at room-temperature. This method allowed the fabricated sample to have completely interconnected pore channels by removing the frozen camphene network via sublimation and dense HA walls by sintering the highly packed HA powder networks at 1250 °C for 3 h. As the initial HA content was increased from 10 to 20 vol.%, the porosity decreased from 75 to 56%, while the compressive strength remarkably increased from 0.94 to 17 MPa.     

Fabrication of polycrystalline lanthanum manganite (LaMnO3) nanofibers by electrospinning

Lanthanum manganite (LaMnO₃) nanofibers were successfully fabricated by electrospinning utilizing sol-gel precursors. Polycrystalline cubic-perovskite structure LaMnO₃ fibers of 50-100 nm were obtained by calcination of the inorganic/organic hybrid fibers at 600 °C for 1 h. The XRD results showed that the grain size of the fibers increased significantly with the increase of calcinations temperature. The average diameter of crystal grains was 17 nm after calcined at 400 °C for 2 h, then grew to 20 nm after heated up to 600 °C for 1 h. The morphology, microstructure, crystal structure and thermal analysis were investigated by SEM, TEM, XRD and TG-DSC, respectively.     

Microstructural control of Ni-YSZ cermet anode for planer thin-film solid oxide fuel cells

Ni-Y₂O₃-stabilized ZrO₂ (Ni-YSZ) cermet anode was fabricated for solid oxide fuel cells (SOFCs) by conventional ceramic processing using NiO-YSZ composite particles. Microstructures of the anode were carefully characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The Ni-YSZ cermet anode was consisting of fine YSZ connections, as the conducting pass of oxygen ions, on the surface of Ni network, as that of electrons, with continuous pore structure and as that of gaseous species. No amorphous phases were present at the interface between Ni and YSZ, and there was an orientation relationship between Ni and YSZ grains, (111)_Ni//(111)_YSZ. The cermet anode showed a high electrical performance at 800 °C. These results indicated that the electrochemical activity of the Ni-YSZ cermet anode was enhanced with the present microstructure.     

Mechanically activated crystallization of phase pure nanocrystalline forsterite powders

Pure nanocrystalline forsterite was successfully synthesized via a mechanical activation route assisted with heat treatment. X-ray diffraction (XRD), scanning electron microscopy (SEM) and simultaneous thermal analysis (STA) techniques were utilized to characterize the prepared powders. Results showed that pure nanocrystalline forsterite could be fabricated completely by 10 h of mechanical activation and post-heat treatment at 1000-1200 °C for 1 h. By 10 h mechanical activation, the initial temperature of forsterite crystallization was reduced to about 820 °C. The obtained nanocrystalline forsterite powder had crystallite size about 57 nm according to Williamson-hall approach and particle sizes smaller than 1000 nm. XRD patterns showed that pure forsterite could not be obtained by mechanical activation process alone and that enstatite could be fabricated by increasing the time of milling. Liberation of CO₂ gas increased the rate of forsterite formation by increasing contact surface between grains.     

Fabrication and characterization of self-organized mixed oxide nanotube arrays by electrochemical anodization of Ti-6Al-4V alloy

Self-organized mixed oxide nanotube arrays were fabricated by anodization of Ti-6Al-4V alloy in H₃PO₄/NH₄F aqueous solution. The nanotubes of 90-180 nm in diameter and 10-20 nm in wall thicknesses could be tuned by changing anodization voltages. Whereas, the as-prepared nanotube arrays were amorphous; to induce crystallinity, the products were annealed at 400 °C, 500 °C and 600 °C, respectively. The UV-Vis spectra of samples annealed at 600 °C gives the maximum absorption in the visible spectra range. Various characterization techniques (viz., FESEM, XPS, XRD, and UV-Vis) were used to study the morphology, composition, phase and band gap of the films.     

Processing microstructure property correlation of porous Ni-YSZ cermets anode for SOFC application

The present paper investigates microstructural properties and electrical conductivity of cermets prepared by a solid-state technique, a liquid-dispersion technique and a novel electroless coating technique. The Ni-YSZ processed through different techniques shows varying temperature-conductivity behaviour. The cermets synthesised by electroless coating were found to be electronically conducting with 20 vol% nickel, which is substantially lower than that normally reported. The conductivity of Ni-YSZ cermets was found highest for the samples prepared by an electroless coating technique and lowest for the samples prepared by a solid-state technique, the samples prepared from liquid-dispersion show an intermediate value for a constant nickel content. The variation in electrical conductivity has been well explained from the microstructure of the samples.     

Novel synthesis of lace-like nanoribbons of boehmite and γ-alumina by dry gel conversion method

Pure lace-like nanoribbons of AlOOH boehmite have been fabricated by an innovative dry gel conversion without the presence of catalysts and templates. Through steam-assisted crystallization at 200 °C for 48 h, the dried powder of amorphous aluminium hydroxide gel was transformed to lace-like nanoribbons in length of 1-2 μm and width about 100 nm as well as thickness of 5-6 nm. After calcination at 600 °C for 5 h, γ-Al₂O₃ was obtained and the morphology of lacelike was preserved.     

Highly porous hydroxyapatite scaffolds with elongated pores using stretched polymeric sponges as novel template

This study reports a simple way of improving the compressive strength of highly porous hydroxyapatite (HA) scaffolds by adopting elongated polymeric sponges as a novel template. In this method, as-received polymeric sponges with isotropic pores were stretched uniaxially to 50% elongation at 200 °C for 2 h, and then coated with a HA slurry. The HA-coated sponges were heat-treated at 800 °C for 3 h to remove the polymeric sponges and at 1250 °C for 3 h to sinter the HA walls. The fabricated samples showed a highly anisotropic pore structure with elongated pores parallel to the direction of the elongation of the polymeric sponge. This simple method allowed a highly porous scaffold to have a high compressive strength of 3.8 ± 0.1 MPa at a porosity of 76% when tested parallel to the direction of pore elongation.     

Effects of aging treatment on microstructure and tribological properties of nickel-based high-temperature self-lubrication wear resistant composite coatings by laser cladding

The NiCr/Cr₃C₂–WS₂ high-temperature self-lubrication wear resistant composite coatings were fabricated on substrate of a hot-rolled AISI304 austenitic stainless steel by laser cladding. The high-temperature phase stability of the composite coatings was evaluated by aging at 600 °C for 10 h, 30 h, 50 h, and the microstructures of the as-laser clad and aged coatings were examined by means of XRD, SEM, EDS, respectively. The sliding wear resistance of the as-laser clad and aged coatings was evaluated at 600 °C. The results show that NiCr/Cr₃C₂–WS₂ composite coating has excellent high-temperature phase stability, the γ-(Fe,Ni)/Cr₇C₃ eutectic phases, Cr₇C₃ and (Cr,W)C hard phases, CrS/WS₂ mixed solid lubricant phases all existed in the as-laser clad and aged coatings. The volume fraction of eutectic phases decreased gradually with the increasing of aged time due to their dissolution. The microhardness of the aged coating decreased slightly after aging the coating 50 h at 600 °C due to the dissolution of the eutectic phases and notable breaking or granulation of the Cr₇C₃ hard phase, but the tribological properties were not significantly affected by aging treatment.     

Growth and vacuum post-annealing effect on the properties of the new absorber CuSbS2 thin films

Post-growth treatments in vacuum atmosphere were performed on CuSbS₂ films prepared by the single-source thermal evaporation method on glass substrates. The films were annealed in vacuum atmosphere for 2 h in temperature range 130-200 °C. The effect of this thermal treatment on the structural, optical and electrical properties of the films was studied. X-ray diffraction (XRD) patterns indicated that the films exhibited an amorphous structure for annealing temperature below 200 °C and a polycrystalline structure with CuSbS₂ principal phase. For the films annealed at temperatures below 200 °C one direct optical transition in range 1.8-2 eV was found. For the films annealed at 200 °C, two optical direct transitions emerged at 1.3 and 1.79 eV corresponding to the CuSbS₂ and Sb₂S₃ values respectively. The electrical measurements showed a conversion from low resistivities (3.10^− 2-9.10^− 2) Ω cm for the samples annealed at temperatures below 200 °C to relatively high resistivities (2 Ω cm) for the samples annealed at 200 °C. In all cases the samples exhibited p-Ztype conductivity.     

Nanoporous TiO2 thin film based conductometric H2 sensor

Nanoporous titanium dioxide (TiO₂) based conductometric sensors have been fabricated and their sensitivity to hydrogen (H₂) gas has been investigated. A filtered cathodic vacuum arc (FCVA) system was used to deposit ultra-smooth Ti thin films on a transducer having patterned inter-digital gold electrodes (IDTs). Nanoporous TiO₂ films were obtained by anodization of the titanium (Ti) thin films using a neutral 0.5% (wt) NH₄F in ethylene glycol solution at 5 V for 1 h. After anodization, the films were annealed at 600 °C for 8 h to convert the remaining Ti into TiO₂. The scanning electron microscopy (SEM) images revealed that the average diameters of the nanopores are in the range of 20 to 25 nm. The sensor was exposed to different concentrations of H₂ in synthetic air at operating temperatures between 100 °C and 300 °C. The sensor responded with a highest sensitivity of 1.24 to 1% of H₂ gas at 225 °C.     

Fabrication of titanium scaffolds with porosity and pore size gradients by sequential freeze casting

This paper reports a novel method for producing porous Ti scaffolds with a gradient in porosity and pore size using the freeze casting method, in which TiH₂/camphene slurries with various TiH₂ contents (40, 25, and 10 vol.%) were cast sequentially into a mold, followed by freeze drying and heat-treatment in a vacuum at 1300 °C for 3 h. This simple sequential freeze casting method produced good bonding between the layers with different porosities of 35, 53, and 75 vol.% obtained using the TiH₂ contents of 40, 25 and 10 vol.%, respectively. In addition, the pore size could be increased significantly by increasing the freezing time. The pore sizes obtained in the regions produced using 40, 25, and 10 vol.% TiH₂ after freezing for 7 days were 96, 166, and 270 μm, respectively.     

The study on electrical behavior of Gd2O3-WO3 complex ceramics at high temperature

Gd₂O₃-WO₃ complex ceramics are fabricated by the conventional solid-state reaction process. The electrical characteristics and dielectric properties of the samples were measured at various ambient temperatures in a low electric field (E < 150 V/mm). As the temperature increases, the dielectric constant and the loss tangent show an obvious change at about 50 °C and 330 °C. When the temperature is above 200 °C, the samples display stable nonlinear electrical properties characterized by semiconductivity, and the nonlinearity increases along with increasing temperature. XRD analysis reveals that Gd₂W₂O₉ is the main phase and Gd₂O₃ is the secondary phase. Based on the phase transition of tungsten trioxide, these electrical properties of Gd₂O₃-WO₃ complex ceramics can be simply explained.     

Sintering behavior of Ni/Y2O3-ZrO2cermet electrodes of solid oxide fuel cells

The sintering behavior of Ni/Y₂O₃-ZrO₂(YSZ) cermet electrode coating on 3 mol% Y₂O₃-ZrO₂electrolyte was studied under moist and dry hydrogen atmosphere at 1000°C for up to 2000 h. The sintering behavior of Ni/YSZ cermet electrodes was dominated by the agglomeration and grain growth of Ni particles in the cermets, which was critically related to the content of Ni and YSZ phases in the cermet. For pure Ni electrode coating, the sintering was substantial and cross plane cracks and isolated Ni island were formed after sintering at 1000°C for only 250 h. However with the addition of YSZ phase, the sintering of Ni/YSZ cermet anode coatings was significantly reduced. For the cermet composition of Ni (50 vol%)/YSZ (50 vol%), the change in the surface porosity and pore size distribution after sintering at 1000°C for 2000 h was very small. The microstructural stability of the Ni (50 vol%)/YSZ (50 vol%) cermet electrodes was also demonstrated by the performance stability tested under current load of 250 mAcm^–2at 1000°C for over 2500 h.     

Fabrication of porous titanium scaffolds with high compressive strength using camphene-based freeze casting

We herein report the fabrication of highly porous titanium (Ti) scaffolds with unusually high compressive strength by freezing a titanium hydride (TiH₂)/camphene slurries at 42 °C. As the freezing time was increased from 1 to 7 days, the pore size obtained was increased significantly from 143 to 271 μm due to the continual overgrowth of camphene dendrites. However, interestingly, the formation of the micro-pores inside the Ti walls was suppressed at longer freezing time. This resulted in a significant increase in compressive strength up to 110 ± 17 MPa with a porosity of 64%. It is believed that this unusually high compressive strength with large interconnected pores makes this material suitable for applications as load-bearing parts.     

Study of silicon-on-insulator substrates incorporated with buried MoSi2 layer

Silicon-on-Insulator (SOI) substrates incorporated with buried MoSi₂ were fabricated using room temperature plasma bonding technology and smart cut technology. The molybdenum disilicide phase formation and morphology were studied by means of four-point probe measurements, X-ray diffraction analysis, atomic force microscopy and transmission electron microscopy examination. It is found that the transition of high-resistance phase Mo₃Si to low-resistance phase h-MoSi₂ occurs at approximately 750 °C. The t-MoSi₂ phase emerges at approximately 900 °C. SOI substrate incorporated with buried silicide layer of complete t-MoSi₂ phase can be achieved by 900 °C annealing for 20 min.     

Microstructure and spectral selectivity of Mo-Al2O3 solar selective absorbing coatings after annealing

Mo, Al₂O₃ single layer, Mo-Al₂O₃ granular cermet layer, Mo/Al₂O₃ tandem and an optimized Mo-Al₂O₃ multilayer coating with a double cermet layer configuration were deposited on stainless steel substrates by magnetron sputtering technique. The samples were annealed in vacuum at different temperatures ranging from 350 °C to 1000 °C for 2-5 h to evaluate their thermal stability. The spectral absorbance and thermal emissivity for the multi-layer selective coatings in the region of 1.3-25 μm were 0.91-0.93 and 0.19-0.27, respectively, depending on heat treatment temperature. Increasing annealing temperature has more obvious influence on the rise of emissivity than the drop of spectral absorbance. The microstructure, surface morphology, composition distribution and diffusion for various films before and after high temperature aging were investigated employing scanning electronic microscopy, X-ray diffraction and X-ray photoelectron spectroscopy. Fe₂O₃, as a diffusion barrier between Mo layer and SS substrate, effectively holds back the presence of Mo₂C and Fe₂MoC complex phases. Al₂O₃ is a stable phase even at 1000 °C for 3 h. However, defects such as widened boundaries, cracks and holes, which could appear in Al₂O₃ layer when heated at higher temperature than 650 °C, will provide the paths of Mo diffusion. Two diffusion modes of Mo, including inner self-congregation of Mo inside the cermet layer and Mo infiltration through the Al₂O₃ layer in Mo/Al₂O₃ tandem at 800 °C for 5 h, were observed after annealing.     

The influence of annealing temperatures on the properties of Bi2VO5.5/LaNiO3/Si thin films

Bi₂VO_5.5 ferroelectric thin films were fabricated on LaNiO₃/Si(100) substrate via chemical solution deposition. Ferroelectric and dielectric properties of the thin films annealed at 500-700 °C were studied. The thin film annealed at 700 °C exhibited more favorable ferroelectric and dielectric properties than those annealed at lower temperatures. The values of remnant polarization 2P_r and coercive field E_c for the film annealed at 700 °C are 10.62 µC/cm² and 106.3 kV/cm, respectively. The leakage current of the film is about 1.92 × 10^− 8 A/cm² at 6 V. The possible mechanism of the dependence of electrical properties of the films on the annealing temperature was discussed.