Evolution of the fractal structure during sintering of SnO2 compacted sol-gel powder

The structural evolution during sintering of compacted SnO2 sol-gel powder was investigated using nitrogen adsorption isotherm analysis. Results show that for sintering temperatures up to 400°C the samples have a fractal pore size distribution. As the sintering temperature increases, a structural rearragement occurs, allowing an increase of the efficiency of particle packing and the reduction of fractality. Above 400°C, the pore size growth associated with grain coalescence is the main structural change observed as the sintering temperature increases. © 1995.

Synthesis and sintering of ultra fine NaNbO3 powder by use of polymeric precursors

Ultra-fine NaNbO3 powder was prepared by the use of polymeric precursors. X-ray diffraction (XRD) results showed that this niobate nucleates from the amorphous precursor, with no intermediate phases, at low temperature (500°C). Studies by XRD and nitrogen adsorption/desorption showed that powders with high crystallinity ( ≈ 100%) and high surface areas (>20 m2/g) are obtained after calcination at 700°C for 5 h. Compacts of calcined powders showed high sinterability reaching 98% of theoretical density when sintered at 1190°C for 3 h.

On Ti-18Si-6B and Ti-7.5Si-22.5B powder alloys prepared by high-energy ball milling and sintering

Recently, a new ternary phase was discovered in the Ti-Si-B system, located near the Ti6Si2B composition. The present study concerns the preparation of titanium alloys that contain such phase mixed with α-titanium and other intermetallic phases. High-purity powders were initially processed in a planetary ball-mill under argon atmosphere with Ti-18Si-6B and Ti-7.5Si-22.5B at. (%) initial compositions. Variation of parameters such as rotary speed, time, and ball diameters were adopted. The as-milled powders were pressureless sintered and hot pressed. Both the as-milled and sintered materials were characterized by X-ray diffraction, scanning electron microscopy and energy-dispersive spectrometry. Sintered samples have presented equilibrium structures formed mainly by the α-Ti+Ti6Si2B+Ti5Si3+TiB phases. Silicon and boron peaks disappear throughout the milling processes, as observed in the powder diffraction data. Furthermore, an iron contamination of up to 10 at. (%) is measured by X-ray spectroscopy analysis on some regions of the sintered samples. Density, hardness and tribological results for these two compositions are also presented here.

Production of nanoTiC–graphite composites using Ti-doped self-sintering carbon mesophase powder

This work reports the synthesis of nanoTiC–graphite composites using mesophase pitch containing titanium as TiC or TiO2 nanoparticles. NanoTiC–graphite composites have been prepared using Ti-doped self-sintering mesophase powders as starting materials without using any binders or a metal carbide-carbon mixing stage. The effect of manufacture variables on the graphite compacts properties was studied. Graphites were characterised using XRD and Raman spectroscopy, SEM and TEM, as well as by their mechanical, electrical and thermal properties. The presence of TiC promotes graphitisation producing materials with larger crystal sizes. The kind of titanium source and mesophase content of the starting pitch affects to the final properties. Mesophase pitch with higher amount of mesophase content produces graphites with higher degree of graphitisation. The incorporation of TiC nanoparticles to the graphites composites improved thermal conductivity more than four times, and mechanical properties are not significantly modified by the presence of TiC.

The investigation of the activated sintering of tungsten powder. Prepared under U. S. Navy, Bureau of Naval Weapons contract no. w 61-0326-d, final report covering the period Nov. 1, 1961 to Jan. 31, 1963,

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On the sintering of uncompacted, pre-alloyed Al powder alloys

The effect of the addition of elemental Mg, Sri and Pb on the sintering of impressed prealloyed 2124 and 6061 powder has been investigated. Despite being sintered at a temperature that resulted in similar to20 vol.% liquid phase, high density was possible only upon the addition of similar to1% elemental Mg as well as trace amounts of Sri or Pb. Additions of Mg facilitated oxide disruption, while Sri and Pb segregated to the liquid phase, where they reduced the liquid's surface tension, thus improving sintering. (C) 2002 Elsevier Science B.V. All rights reserved.

Sintering and densification mechanisms of Y2BaCuO5 pellets

The sintering and densification of Y2BaCuO5 (Y-211) pellets made from powders with different characteristics have been investigated in the temperature range 1000-1140°C. A pellet made from powder containing Ba-rich secondary phases shows very early liquid-assisted sintering and densification and clear evidence of exaggerated grain growth. The melting of BaCuO2 and YBa2Cu3O7-δ (Y-123) secondary phases increases the rate of densification of Y-211 pellets made from other powders at temperatures above 1025-1030°C. All the liquid produced by the melting of the latter phases recrystallizes as intergranular layers of Y-123. These intergranular layers account for the darker appearance and for measurable electrical conductivities at room temperature of the pellets sintered at the higher temperatures. The development of exaggerated grain growth within a uniform fine-grained matrix opens the possibility of using controlled secondary recrystallization to obtain large single domains of Y-211, provided that the trapping of porosity can be avoided or minimized. © 1999 Elsevier Science S.A.

Low-temperature synthesis and sintering of γ-Y2Si2O7

In this article, a novel pressureless solid-liquid reaction method is presented for preparation of yttrium disilicate (γ-Y2Si2O7). Single-phase γ-Y2Si2O7 powder was synthesized by calcination of SiO2 and Y2O3 powders with the addition of LiYO2 at 1400 °C for 4 h. The addition of LiYO2 significantly decreased the synthesis temperature, shortened the calcination time, and enhanced the stability of γ-Y2Si2O7. The sintering of these powders in air and O2 was studied by means of thermal mechanical analyzer. It is shown that the γ-Y2Si2O7 sintered in oxygen had a faster densification rate and a higher density than that sintered in air. Furthermore, single-phase γ-Y2Si2O7 with a density of 4.0 g/cm3 (99% of the theoretical density) was obtained by pressureless sintering at 1400 °C for 2 h in oxygen. Microstructures of the sintered samples are studied by scanning electron microscope.

An aqueous-solution based low-temperature pathway to synthesize giant dielectric CaCu3Ti4O12-Highly porous ceramic matrix and submicron sized powder

A simple, cost-effective and environment-friendly pathway for preparing highly porous matrix of giant dielectric material CaCu3Ti4O12 (CCTO) through combustion of a completely aqueous precursor solution is presented. The pathway yields phase-pure and impurity-less CCTO ceramic at an ultra-low temperature (700 degrees C) and is better than traditional solid-state reaction schemes which fail to produce pure phase at as high temperature as 1000 degrees C (Li, Schwartz, Phys. Rev. B 75, 012104). The porous ceramic matrix on grinding produced CCTO powder having particle size in submicron order with an average size 300 nm. On sintering at 1050 degrees C for 5 h the powder shows high dielectric constants (>10(4) at all frequencies from 100 Hz to 100 kHz) and low loss (with 0.05 as the lowest value) which is suitable for device applications. The reaction pathway is expected to be extended to prepare other multifunctional complex perovskite materials. (C) 2010 Elsevier B.V. All rights reserved.

Sintering of beta titanium: Role of dislocation pipe diffusion

Sintering of titanium in its high temperature beta phase was studied by isothermal dilatometry. The sintering shrinkage y did not follow the normal time exponent type of behaviour, instead being described by the equation y = Kt(m)/[1-(A+Bt)(2)], where m = 1.93 +/- 0.07, with an activation energy of 62-90 kJ mol(-1). A detailed analysis of these results, based on the 'anomalous' diffusion behaviour reported for beta titanium, is carried out. It is shown that the generation of a high density of dislocations during the alpha --> beta phase transformation, coupled with sluggish recovery at the sintering necks, enables sintering mass transport by pipe diffusion through dislocation cores from sources of matter within the particles to become dominant.

The effect of powder processing on densification, microstructure and mechanical properties of hydroxyapatite

The influence of powder processing and sintering temperature on densification, microstructure and mechanical properties of hydroxyapatite (HAp) ceramics was studied. The as-dried, calcined and processed HAp powders were uniaxially compacted and sintered at various temperatures (1000-1400 degreesC) for 3 h. The as-dried and processed powders, attained 97% of theoretical density (TD) at 1100 degreesC) at higher sintering temperatures, the density of the as-dried powder compact was found to decrease. A uniform microstructure with fine grain size (2.3 pm) was observed for material obtained from processed powder, whereas exaggerated grain growth with closed pores were observed in as-dried and unprocessed powder compacts. The Vickers' hardness, fracture toughness and flexural strength of HAp were determined and a maximum value of 6.3 GPa and 0.88 MPam(1/2) and 60.3 MPa, respectively were obtained for processed compact. The processing of HAp has improved its densification, microstructure homogeneity and mechanical properties. (C) 2002 Elsevier Science Ltd and Techna S.r.l. All rights reserved.

Strength reliability and in vitro degradation of three-dimensional powder printed strontium-substituted magnesium phosphate scaffolds

Strontium ions (Sr2+) are known to prevent osteoporosis and also encourage bone formation. Such twin requirements have motivated researchers to develop Sr-substituted biomaterials for orthopaedic applications. The present study demonstrates a new concept of developing Sr-substituted Mg-3(PO4)(2) - based biodegradable scaffolds. In particular, this work reports the fabrication, mechanical properties with an emphasis on strength reliability as well as in vitro degradation of highly biodegradable strontium-incorporated magnesium phosphate cements. These implantable scaffolds were fabricated using three-dimensional powder printing, followed by high temperature sintering and/or chemical conversion, a technique adaptable to develop patient-specific implants. A moderate combination of strength properties of 36.7 MPa (compression), 242 MPa (bending) and 10.7 MPa (tension) were measured. A reasonably modest Weibull modulus of up to 8.8 was recorded after uniaxial compression or diametral tensile tests on 3D printed scaffolds. A comparison among scaffolds with varying compositions or among sintered or chemically hardened scaffolds reveals that the strength reliability is not compromised in Sr-substituted scaffolds compared to baseline Mg-3(PO4)(2). The micro-computed tomography analysis reveals the presence of highly interconnected porous architecture in three-dimension with lognormal pore size distribution having median in the range of 17.74-26.29 mu m for the investigated scaffolds. The results of extensive in vitro ion release study revealed passive degradation with a reduced Mg2+ release and slow but sustained release of Sr2+ from strontium-substituted magnesium phosphate scaffolds. Taken together, the present study unequivocally illustrates that the newly designed Sr-substituted magnesium phosphate scaffolds with good strength reliability could be used for biomedical applications requiring consistent Sr2+-release, while the scaffold degrades in physiological medium. Statement of significance The study investigates the additive manufacturing of scaffolds based on different strontium-substituted magnesium phosphate bone cements by means of three-dimensional powder printing technique (3DPP). Magnesium phosphates were chosen due to their higher biodegradability compared to calcium phosphates, which is due to both a higher solubility as well as the absence of phase changes (to low soluble hydroxyapatite) in vivo. Since strontium ions are known to promote bone formation by stimulating osteoblast growth, we aimed to establish such a highly degradable magnesium phosphate ceramic with an enhanced bioactivity for new bone ingrowth. After post-processing, mechanical strengths of up to 36.7 MPa (compression), 24.2 MPa (bending) and 10.7 MPa (tension) could be achieved. Simultaneously, the failure reliability of those bioceramic implant materials, measured by Weibull modulus calculations, were in the range of 4.3-8.8. Passive dissolution studies in vitro proved an ion release of Mg2+ and PO43- as well as Sr2+, which is fundamental for in vivo degradation and a bone growth promoting effect. In our opinion, this work broadens the range of bioceramic bone replacement materials suitable for additive manufacturing processing. The high biodegradability of MPC ceramics together with the anticipated promoting effect on osseointegration opens up the way for a patient-specific treatment with the prospect of a fast and complete healing of bone fractures. (C) 2015 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Spark plasma sintering of TiNi nano-powders for biological application

Nano-sized TiNi powder with an average size of 50nm was consolidated using spark plasma sintering (SPS) at 800 °C for 5min. A layer of anatase TiO 2 coating was formed on the sintered TiNi by chemical reaction with a hydrogen peroxide (H2O2) solution at 60 °C followed by heat treatment at 400 °C to enhance the bioactivity of the metal surface. Cell culture using osteoblast cells and a biomimetic test in simulated body fluid proved the biocompatibility of the chemically treated SPS TiNi. © IOP Publishing Ltd.

Bulk ultrafine binderless (W0.4Al0.6)C prepared by high pressure sintering

Pure (W0.4Al0.6)C powder of about 1 mu m in diameter was sintered by the high pressure sintering (HPS) process without the addition of any binder phase. The microstructure, Vickers micro hardness and density versus the sintering time and temperature are well described. The most suitable sintering condition under pressure of 4.5 GPa is 1873 K for 8 min. Under this sintering condition, the hardness can reach 2295 kg mm(-2) and the relative density can reach 98.6%.