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At least 145 records · Page 8

On the densification of cubic ZrO{sub 2} nanocondensates by capillarity force and turbostratic C–Si–H multiple shell

A turbostratic C–Si–H lamellar phase with 0.35–0.39 nm interspacing and ZrO{sub 2} condensates having cubic (c), tetragonal and monoclinic structures stabilized by increasing particle size were synthesized by pulsed laser ablation on Zr plate in TEOS and characterized by X-ray/electron diffraction and optical spectroscopy. The c-ZrO{sub 2} phase ca. 10% denser than the ambient lattice was stabilized as 3–10 nm sized cubo-octahedral nanoparticles but as abnormal large-sized (up to 30 nm) ones when encapsulated by the C{sub 1−x}Si{sub x}:H multiple shell with defective graphite-like structure units to exert an effective compressive stress. The potential application of such core–shell nanostructure with enhanced binding of Zr and O ions and implication for natural dynamic occurrence of the C{sub 1−x}Si{sub x}:H phase are addressed. - Graphical abstract: Lattice image of a typical cubic-ZrO{sub 2} particle densified by the turbostratic Si{sub x}C{sub 1−x}:H shell. Highlights: ► Turbostratic C–Si–H lamellar phase and ZrO{sub 2} condensates were synthesized by PLA. ► The c-ZrO{sub 2} phase ca. 10% denser than the ambient lattice was stabilized as 3–10 nm. ► The c-ZrO{sub 2} particles up to 30 nm were densified when encapsulated by the C{sub 1−x}Si{sub x}:H multiple shell. ► Tight ion binding of the c-ZrO{sub 2} due to capillarity force and turbostratic shell.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Microstructural study and densification analysis of hot work tool steel matrix composites reinforced with TiB{sub 2} particles

Hot work tool steels are characterized by good toughness and high hot hardness but are less wear resistant than other tooling materials, such as high speed steel. Metal matrix composites show improved tribological behavior, but not much work has been done in the field of hot work tool steels. In this paper TiB{sub 2}-reinforced hot work tool steel matrix composites were produced by spark plasma sintering (SPS). Mechanical alloying (MA) was proposed as a suited process to improve the composite microstructure. Density measurements and microstructure confirmed that MA promotes sintering and produces a fine and homogeneous dispersion of reinforcing particles. X-ray diffraction patterns of the sintered composites highlighted the formation of equilibrium Fe{sub 2}B and TiC, as predicted by thermodynamic calculations using Thermo-Calc® software. Scanning electron microscopy as well as scanning Kelvin probe force microscopy highlighted the reaction of the steel matrix with TiB{sub 2} particles, showing the formation of a reaction layer at the TiB{sub 2}-steel interface. Phase investigations pointed out that TiB{sub 2} is not chemically stable in steel matrix because of the presence of carbon even during short time SPS. - Highlights: • TiB{sub 2} reinforced steel matrix composites were produced by spark plasma sintering. • TiB{sub 2} was successfully dispersed in the steel matrix by mechanical alloying. • Steel and TiB{sub 2} react during sintering forming equilibrium Fe{sub 2}B and TiC. • The new phases were investigated by means of AFM, Volta potential and XRD analyses.

36 MATERIALS SCIENCE↗

Studies on densification, mechanical, micro-structural and structure–properties relationship of magnesium aluminate spinel refractory aggregates prepared from Indian magnesite

The present work intends to study the development of magnesium aluminate spinel aggregates from Indian magnesite in a single firing stage. The raw magnesite has been evaluated in terms of chemical analysis, differential thermal analysis, thermogravimetric analysis, infrared spectroscopy, and X-ray diffraction. The experimental batch containing Indian magnesite and calcined alumina has been sintered in the temperature range of 1550 °C–1700 °C. The sintered material has been characterized in terms of physico-chemical properties like bulk density, apparent porosity, true density, relative density and thermo-mechanical/mechanical properties like hot modulus of rupture, thermal shock resistance, cold modulus of rupture and structural properties by X-ray diffraction in terms of phase identification and evaluation of crystal structure parameters of corresponding phases by Rietveld analysis. The microstructures developed at different temperatures have been analyzed by field emission scanning electron microscope study and compositional analysis of the developed phase has been carried out by energy dispersive X-ray study. - Highlights: • The studies have been done to characterize the developed magnesium aluminate spinel. • The studies reveal correlation between refractory behavior of spinel and developed microstructures. • The studies show the values of lattice parameters of developed phases.

36 MATERIALS SCIENCE↗

Synthesis, densification and characterization of ultra-fine W-Al2O3 composite powder

Highlights: • W-Al{sub 2}O{sub 3} ultrafine powder was prepared by hydrothermal synthesis. • Al{sub 2}(WO{sub 4}){sub 3} was a key process for forming nano-Al{sub 2}O{sub 3} coated W structure. • This coated structure inhibited the further growth of W particles. • Dispersed Al{sub 2}O{sub 3} particles improved obviously mechanical properties of W alloy. • Fracture mode changed into intergranular from transcrystalline with Al{sub 2}O{sub 3} addition. - Abstract: W-Al{sub 2}O{sub 3} composite powder was prepared via hydrothermal synthesis containing doping, annealing and reduction. The precursors WO{sub 3} and AlOOH were synthesized by the two sets of the hydrothermal reactions, respectively. The formation of Al{sub 2}(WO{sub 4}){sub 3} from these two precursors in an aqueous solution is a key process, which is beneficial to improve the mixing uniformity of final powder to a molecular level. During subsequent reduction, nano-Al{sub 2}O{sub 3} coated W particles were obtained, and inhibited the further deposition of reduced W atoms on the adjacent W particles, obtaining ultra-fine Al{sub 2}O{sub 3}/W composite powder. After sintering, the dense and fine-grained W-Al{sub 2}O{sub 3} alloy was obtained due to the high sintering activity of ultra-fine powder. Compared with the pure tungsten, the W-Al{sub 2}O{sub 3} alloy displays obvious higher values of both strength and plasticity especially when the Al{sub 2}O{sub 3} content is 2 wt%.

36 MATERIALS SCIENCE↗

Crystallization, densification and dielectric properties of CaO–MgO–Al{sub 2}O{sub 3}–SiO{sub 2} glass with ZrO{sub 2} as nucleating agent

SEM micrographs for the pure CaO–MgO–Al{sub 2}O{sub 3}–SiO{sub 2} glass sintered at 850–1000 °C (a) 850 °C, (b) 900 °C, (c) 950 °C, (d) 1000 °C. - Highlights: • ZrO{sub 2} effects on the crystallization of LTCC glass system were investigated. • ZrO{sub 2} effects on the dielectric properties of LTCC glass system were investigated. • LTCC with a dielectric constant of 6.65 and a low dielectric loss can be obtained. - Abstract: The zirconium oxide effects on the crystallization and dielectric properties of CaO–MgO–Al{sub 2}O{sub 3}–SiO{sub 2} (CMAS) glass were investigated. The results showed that phyllosiloxide and anorthite crystallites were observed in sequence during sintering. For glass added with 8 wt% ZrO{sub 2}, homogeneously dispersed tetragonal ZrO{sub 2} crystallites were observed at 850 °C. The as-prepared CMAS glass–ceramics exhibited a dielectric constant of about 6–7 and a dielectric loss below 0.005 at 100 MHz. The dielectric properties of CMAS glass with 8 wt% ZrO{sub 2} sintered at 850 °C show a low dielectric constant of 6.65 and a dielectric loss tangent of about 2.5 × 10{sup −3}, which provides a promising candidate for LTCC applications.

36 MATERIALS SCIENCE↗

A visco-plastic constitutive model for accurate densification and shape predictions in powder metallurgy hot isostatic pressing

Powder metallurgy hot isostatic pressing (PM-HIP) is an advanced manufacturing process that produces near net shape parts with high material utilization and uniform microstructures. Despite being used frequently to produce small-scale components, the application of PM-HIP to large-scale components is limited due to inadequate understanding of its complex mechanisms that cause unpredictable post-HIP shape distortions. A computational model can provide necessary information about the intermediate and final stages of the HIP process that can help understand it better and make accurate predictions. Generally, two types of computational models are employed for PM-HIP of metal powders, namely, plastic and visco-plastic models. Between these, the plastic model is preferred due to its cheaper calibration approach requiring less experimental data. However, the plastic model sometimes produces incorrect predictions when slight variations of the HIP conditions are encountered in practical situations. Therefore, this work presents a visco-plastic model that addresses these limitations of the plastic model. A novel modified calibration approach is employed for the visco-plastic model that utilizes less experimental data than existing approaches. With the new approach, the data requirement is same for both plastic and visco-plastic models. This also enables a quantitative comparison of plastic and visco-plastic models, which have been only qualitatively compared in the past. When calibrated with the same experimental data, both the models are found to produce similar results. In conclusion, the calibrated visco-plastic model is applied to several complex geometries, and the predictions are found to be in good agreement with experimental observations.

Hot isostatic pressing↗

Densification Pressure Optimization of MOF-808-Based Membranes for Lithium Metal Batteries

The use of metal–organic frameworks (MOFs) in hybrid electrolytes for lithium (Li) metal batteries has grown in prominence in recent years, primarily due to the chemical tunability of the MOF’s pore structures, which can directly influence Li–ion transport properties. The most attractive form factor for a MOF electrolyte is a thin, flexible membrane, which requires the application of pressure to increase the contact between the MOF particles. Herein, a systematic study of the influence of pressure on the properties of MOF-808-based membranes is presented. It is shown that when a dry, roll-pressed membrane is subjected to pressure ≥120 MPa, a total loss of crystallinity and a significant loss of porosity is observed. Alternatively, a slurry-cast membrane, compressed under controlled pressures, can maintain crystallinity and porosity while decreasing the interparticle void space. Interesting, the conductivity of the membranes infiltrated with liquid electrolyte is not greatly affected by the pressure applied, though ultimately it is shown that for cycling with Li metal, compressed membranes with compact particles are preferred. In conclusion, this study highlights the critical importance of controlling the pressure applied to MOF-based membranes during fabrication and during cell assembly and lays out the foundation for further investigation of how to optimize membrane fabrication for hybrid electrolytes that use MOFs as the dominate component.

25 ENERGY STORAGE↗

Densification of the interlayer spacing governs the nanomechanical properties of calcium-silicate-hydrate

Calciuam-silicate-hydrate (C-S-H) is the principal binding phase in modern concrete. Molecular simulations imply that its nanoscale stiffness is 'defect-driven', i.e., dominated by crystallographic defects such as bridging site vacancies in its silicate chains. However, experimental validation of this result is difficult due to the hierarchically porous nature of C-S-H down to nanometers. Here in this paper, we integrate high pressure X-ray diffraction and atomistic simulations to correlate the anisotropic deformation of nanocrystalline C-S-H to its atomic-scale structure, which is changed by varying the Ca-To-Si molar ratio. Contrary to the 'defect-driven' hypothesis, we clearly observe stiffening of C-S-H with increasing Ca/Si in the range 0.8 ≤ Ca/Si ≤ 1.3, despite increasing numbers of vacancies in its silicate chains. The deformation of these chains along the b-Axis occurs mainly through tilting of the Si-O-Si dihedral angle rather than shortening of the Si-O bond, and consequently there is no correlation between the incompressibilities of the a-and b-Axes and the Ca/Si. On the contrary, the intrinsic stiffness of C-S-H solid is inversely correlated with the thickness of its interlayer space. This work provides direct experimental evidence to conduct more realistic modelling of C-S-H-based cementitious material.

36 MATERIALS SCIENCE↗

Densification of chemical vapor deposition silicon dioxide film using oxygen radical oxidation

Silicon dioxide (SiO{sub 2}) films formed by chemical vapor deposition (CVD) were treated with oxygen radical oxidation using Ar/O{sub 2} plasma excited by microwave. The mass density depth profiles, carrier trap densities, and current-voltage characteristics of the radical-oxidized CVD-SiO{sub 2} films were investigated. The mass density depth profiles were estimated with x ray reflectivity measurement using synchrotron radiation of SPring-8. The carrier trap densities were estimated with x ray photoelectron spectroscopy time-dependent measurement. The mass densities of the radical-oxidized CVD-SiO{sub 2} films were increased near the SiO{sub 2} surface. The densities of the carrier trap centers in these films were decreased. The leakage currents of the metal-oxide-semiconductor capacitors fabricated by using these films were reduced. It is probable that the insulation properties of the CVD-SiO{sub 2} film are improved by the increase in the mass density and the decrease in the carrier trap density caused by the restoration of the Si-O network with the radical oxidation.

36 MATERIALS SCIENCE↗