Characterization of HIP'ed, High Purity Si3N4 Grain Boundaries

1992 ◽  
Vol 287 ◽  
Author(s):  
Ping Lu ◽  
S.C. Danforth ◽  
W.T. Symons

ABSTRACTLaser synthesized, ultra-fine, amorphous, Si3N4 powders were densified via HIP'ing without any oxide sintering aids. Exposed samples were made from powder that had been exposed to the atmosphere, thereby picking up an oxide surface layer, and unexposed samples were made from powders processed entirely under glove box conditions, i.e. without oxygen contamination. TEM (and sintering) studies indicate that the exposed samples HIP'ed at temperatures in excess of the melting point of Si02, densified via a solution-reprecipitation mechanism, with a resultant intergranular glassy phase of high purity Si02. In contrast, unexposed samples had to be HIP'ed to 2050°C to achieve a density of ∼70 %p Th. These samples consisted of equiaxed β-Si3N4 grains, with localized high density regions where no inter-granular phase (crystalline or glassy) was detected to within 0.66 nm.

1988 ◽  
Vol 120 ◽  
Author(s):  
S. C. Farmer ◽  
P. Pirouz ◽  
A. H. Heuer

AbstractA SiC whisker reinforced HIPped RBSN material fabricated with a Y2O3 sintering aid was characterized using TEM. The matrix is > 90% β-Si3 N4 with a Y-Si-O-N glassy phase at the Si3 N4 grain boundaries and about the SiC whiskers. The SiC whisiers are heavily faulted and have a well defined core. Si3 N4 precipitates are observed in the core region after composite fabrication. A preliminary mechanism for the growth of the SiC whisker, based on the VLS mechanism is proposed.


Author(s):  
D.W. Susnitzky ◽  
S. McKeman ◽  
C.B. Carter

Potassium-rich aluminates have been observed along the grain boundaries of many commercial aluminas. The presence of alkali aluminates can seriously limit the operation lifetime of sodium vapor lamp tubing by increasing the rate of sodium leakage out of the tube. As part of an investigation into phase and interface structure within the K2O-Al2O3 system, high-purity α-Al2O3, seeded with small granules of potassium carbonate, was studied. In samples which were vacuum hot-pressed within a graphite die at 1400°C for 30min, the potassium (K) doping resulted in the precipitation of a spatially inhomogeneous array of K-rich aluminates. It has since been determined that the precipitation phenomenon was due to insufficient mixing of the starting powders. The potassium carbonate was therefore not originally distributed uniformly within the compacts and locally high K concentrations thus resulted.


1993 ◽  
Vol 115 (3) ◽  
pp. 292-299 ◽  
Author(s):  
G. Raiser ◽  
R. J. Clifton

The objective of this investigation is to use a plate impact recovery experiment to identify the dominant failure mechanisms in conventional α-Al2O3 ceramics and thereby gain insight into the most promising, failure-resistant microstructures. A “soft-recovery” configuration is used wherein a star-shaped flyer impacts a square specimen. The impedances, shapes, thicknesses and orientation of all plates are designed to ensure a known history of longitudinal, planar stress waves throughout a central octagonal region of the specimen. The plane waves generated from this experiment are monitored by a laser interferometer system that allows data to be collected at four separate locations. The validity of the approach is demonstrated by a shot in which all plates were stressed within their elastic range. Subsequently, several experiments were conducted at nearly the same stress level with commercially sintered aluminas having different grain size and different glass content. These experiments, taken as a whole, demonstrate that improvement in alumina’s dynamic compressive properties is obtained by reducing the grain size. In compression, a reduction in grain size lowers average residual stresses at triple junctions and grain boundaries and makes the material less susceptible to inelastic deformation and sliding at triple junctions and grain boundaries. A reduction in the weight percent of pre-processing impurities (and therefore the amount of intergranular glassy phase) yields strong improvements in the dynamic tensile strength of the ceramic. A decrease in the amount of glassy phase tends to make tensile damage less likely by improving grain boundary strength. These trends were tested by conducting recovery experiments on a high-purity, small-grain alumina, processed in-house through hot pressing. Both the compressive resistance and, especially, the tensile resistance were superior to those found for all other tested specimens. The overall results suggest that the best failure resistance will be obtained for new, high-purity, ultrafine-grain ceramics that are prepared by hot pressing of nanometer scale powders.


Author(s):  
M. José-Yacamán

Electron microscopy is a fundamental tool in materials characterization. In the case of nanostructured materials we are looking for features with a size in the nanometer range. Therefore often the conventional TEM techniques are not enough for characterization of nanophases. High Resolution Electron Microscopy (HREM), is a key technique in order to characterize those materials with a resolution of ~ 1.7A. High resolution studies of metallic nanostructured materials has been also reported in the literature. It is concluded that boundaries in nanophase materials are similar in structure to the regular grain boundaries. That work therefore did not confirm the early hipothesis on the field that grain boundaries in nanostructured materials have a special behavior. We will show in this paper that by a combination of HREM image processing, and image calculations, it is possible to prove that small particles and coalesced grains have a significant surface roughness, as well as large internal strain.


Author(s):  
V. C. Kannan ◽  
S. M. Merchant ◽  
R. B. Irwin ◽  
A. K. Nanda ◽  
M. Sundahl ◽  
...  

Metal silicides such as WSi2, MoSi2, TiSi2, TaSi2 and CoSi2 have received wide attention in recent years for semiconductor applications in integrated circuits. In this study, we describe the microstructures of WSix films deposited on SiO2 (oxide) and polysilicon (poly) surfaces on Si wafers afterdeposition and rapid thermal anneal (RTA) at several temperatures. The stoichiometry of WSix films was confirmed by Rutherford Backscattering Spectroscopy (RBS). A correlation between the observed microstructure and measured sheet resistance of the films was also obtained.WSix films were deposited by physical vapor deposition (PVD) using magnetron sputteringin a Varian 3180. A high purity tungsten silicide target with a Si:W ratio of 2.85 was used. Films deposited on oxide or poly substrates gave rise to a Si:W ratio of 2.65 as observed by RBS. To simulatethe thermal treatments of subsequent processing procedures, wafers with tungsten silicide films were subjected to RTA (AG Associates Heatpulse 4108) in a N2 ambient for 60 seconds at temperatures ranging from 700° to 1000°C.


2014 ◽  
Vol 52 (9) ◽  
pp. 695-704
Author(s):  
Yun Soo Lim ◽  
Dong Jim Kim ◽  
Seong Sik Hwang
Keyword(s):  

2010 ◽  
Vol 72 ◽  
pp. 46-52 ◽  
Author(s):  
Laurent Royer ◽  
Stéphane Mathieu ◽  
Christophe Liebaut ◽  
Pierre Steinmetz

For energy production and also for the glass industry, finding new refractory alloys which could permit to increase the process temperatures to 1200°C or more is a permanent challenge. Chromium base alloys can be good candidates, considering the melting point of Cr itself, and also its low corrosion rate in molten glass. Two families of alloys have been studied for this purpose, Cr-Mo-W and Cr-Ta-X alloys (X= Mo, Si..). A finer selection of compositions has been done, to optimize their chemical and mechanical properties. Kinetics of HT oxidation by air, of corrosion by molten glass and also creep properties of several alloys have been measured up to 1250°C. The results obtained with the best alloys (Cr-Ta base) give positive indications as regards the possibility of their industrial use.


2021 ◽  
pp. 0887302X2110094
Author(s):  
V. Mamtha ◽  
H. N. Narasimha Murthy ◽  
V. Pujith Raj ◽  
Prashantha Tejas ◽  
C. S. Puneet ◽  
...  

Antibacterial activity and fire retardation are equally desired for protective clothing. For achieving this, AgNP and MgO are independently researched as nanofillers in Polyurethane based electrospun nanofibers and their synergistic effect is scarcely addressed. This article reports synthesis and characterization of MgO of 70.01 nm and AgNP of 51 to 76 nm by solution combustion and hydrothermal routes respectively and their incorporation in electrospinning of Polyurethane. Flow rate 1 ml/hr, applied voltage 13 kV, tip to collector distance 15 cm were adopted for the electrospinning. Nanofibers of 65 nm were obtained for PU/MgO (3 wt. %) and 106 nm for PU/MgO (3 wt. %)/Ag (1 wt. %). Addition of MgO increased the melting point, after flame time and afterglow time. Incorporation of AgNP improved antibacterial activity. PU/MgO/Ag (2 wt. %) exhibited zone of inhibition of 2.1 cm and 3 cm against E. Coli and S. Aureus, respectively.


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