Effect of furnace atmosphere and silica content on the consolidation behaviour of magnesia partially stabilised zirconia

1990 ◽  
Vol 48 (4) ◽  
pp. 1056-1057
Author(s):  
J. Drennan ◽  
R.H.J. Hannink ◽  
D.R. Clarke ◽  
T.M. Shaw
Keyword(s):  
Liquid Phase ◽  
Silica Content ◽  
Liquid Phase Sintering ◽  
Furnace Atmosphere ◽  
Boundary Phase ◽  
Analytical Electron ◽  
Analytical Electron Microscope ◽  
Series Of Experiments ◽  
Compositional Gradients ◽  
Mobile Liquid

Magnesia partially stabilised zirconia (Mg-PSZ) ceramics are renowned for their excellent nechanical properties. These are effected by processing conditions and purity of starting materials. It has been previously shown that small additions of strontia (SrO) have the effect of removing the major contaminant, silica (SiO2).The mechanism by which this occurs is not fully understood but the strontia appears to form a very mobile liquid phase at the grain boundaries. As the sintering reaches the final stages the liquid phase is expelled to the surface of the ceramic. A series of experiments, to examine the behaviour of the liquid grain boundary phase, were designed to produce compositional gradients across the ceramic bodies. To achieve this, changes in both silica content and furnace atmosphere were implemented. Analytical electron microscope techniques were used to monitor the form and composition of the phases developed. This paper describes the results of our investigation and the presentation will discuss the work with reference to liquid phase sintering of ceramics in general.

The Effect of Specimen Thickness and Probe Size on Aem Analysis of Cr-Depletion Profiles in Sensitized Stainless Steel

1982 ◽  
Vol 40 ◽  
pp. 518-519
Author(s):  
E. L. Hall
Keyword(s):  
Grain Boundaries ◽  
Boundary Region ◽  
Chromium Concentration ◽  
Foil Thickness ◽  
Specimen Thickness ◽  
Probe Size ◽  
Analytical Electron ◽  
Analytical Electron Microscope ◽  
Sensitization Process ◽  
Compositional Gradients

Sensitization in stainless steels is caused by the formation of chromium-rich M23C6 carbides at grain boundaries, which depletes the adjacent matrix and boundary region of chromium, and hence leads to rapid intergranular attack. To fully understand the sensitization process, and to test the accuracy of theories proposed to model this process, it is necessary to obtain very accurate measurements of the chromium concentration at grain boundaries in sensitized specimens. Quantitative X-ray spectroscopy in the analytical electron microscope (AEM) enables the chromium concentration profile across these boundaries to be studied directly; however, it has been shown that a strong effect of foil thickness and electron probe size may be present in the analysis of rapidly-changing compositional gradients. The goal of this work is to examine these effects.

Energy-filtered imaging of interfacial composition in complex Ni-base superalloys

1995 ◽  
Vol 53 ◽  
pp. 260-261
Author(s):  
E. L. Hall ◽  
J. Bentley
Keyword(s):  
X Ray ◽  
Collector Plate ◽  
Quantitative Measurements ◽  
Solute Depletion ◽  
Diffusion Controlled ◽  
Interfacial Composition ◽  
Analytical Electron ◽  
Analytical Electron Microscope ◽  
Second Phases ◽  
Compositional Gradients

In a wide variety of important engineering materials, including structural Ni, Fe, and Al-base alloys, the study of compositional gradients that occur at grain boundaries and other interfaces due to the precipitation of solute-rich second phases is of critical importance. X-ray spectrometry in the analytical electron microscope (AEM) has been used for many years to study solute depletion at interfaces in these alloys. It has been particularly effective at providing accurate, quantitative measurements in cases where the interface precipitates are spaced far apart and where relatively wide compositional gradients result from diffusion-controlled “collector-plate” mechanisms. However, in complex alloys, with heavy grain boundary coverage, multiple precipitate types, and/or multiphase matrices, x-ray microanalysis is more limited due to beam spreading and die associated 5-20nm spatial resolution achieved in these alloys with AEMs equipped with thermionic sources.Elemental mapping in an AEM equipped with an imaging energy-filter is an alternative method for the study of interface compositional gradients. It has been shown to be effective for this purpose in relatively simple situations in steels.

Hardness Limits of SiC and Si3N4 Ceramic Materials

2005 ◽  
Vol 287 ◽  
pp. 311-316 ◽  
Author(s):  
Miroslav Balog ◽  
Pavol Šajgalík ◽  
Zoltán Lenčéš ◽  
Miroslav Hnatko ◽  
Jozef Kečkéš
Keyword(s):  
Liquid Phase ◽  
Grain Boundary ◽  
Solid Solutions ◽  
Ceramic Materials ◽  
Liquid Phase Sintering ◽  
Boundary Phase ◽  
Polymer Precursor ◽  
Micro Hardness ◽  
Boundary Composition

Nano- and macro-hardness of SiC and Si3N4 based ceramic materials prepared by liquid phase sintering were evaluated. The applied loads were 3.5 mN and 9.81 N, respectively. The measurements showed that the nano-hardness of both ceramics is substantially higher compared to the macro-hardness. The influence of solid solutions and grain boundary composition on the hardness of SiC-based ceramics was studied. The macro-hardness is strongly dependent on the grain boundary composition while the nano-hardness was nearly the same for all tested samples with different Re2O3-AlN additives. In the case of Si3N4 based ceramics the SiC nano-inclusions content was varied. As a source of SiC nanoinclusions and grain boundary phase modifierSiNC polymer precursor has been used. Nano- as well as micro-hardness increased with increasing SiC content. Present paper deals with the explanation of both results.

Chemical partitioning of elements in Ni-base MC-carbide reinforced eutetic superalloys

1983 ◽  
Vol 41 ◽  
pp. 250-251
Author(s):  
E. F. Koch ◽  
E. L. Hall ◽  
S. W. Yang
Keyword(s):  
Alloy Composition ◽  
Volume Fraction ◽  
Lattice Mismatch ◽  
Turbine Blades ◽  
Eutectic Alloys ◽  
Alloy Matrix ◽  
X Ray ◽  
Gas Turbine Blades ◽  
Analytical Electron ◽  
Analytical Electron Microscope

The plane-front solidified eutectic alloys consisting of aligned tantalum monocarbide fibers in a nickel alloy matrix are currently under consideration for future aircraft and gas turbine blades. The MC fibers provide exceptional strength at high temperatures. In these alloys, the Ni matrix is strengthened by the precipitation of the coherent γ' phase (ordered L12 structure, nominally Ni3Al). The mechanical strength of these materials can be sensitively affected by overall alloy composition, and these strength variations can be due to several factors, including changes in solid solution strength of the γ matrix, changes in they γ' size or morphology, changes in the γ-γ' lattice mismatch or interfacial energy, or changes in the MC morphology, volume fraction, thermal stability, and stoichiometry. In order to differentiate between these various mechanisms, it is necessary to determine the partitioning of elemental additions between the γ,γ', and MC phases. This paper describes the results of such a study using energy dispersive X-ray spectroscopy in the analytical electron microscope.

Diagnosis of Silica Induced Granulomatous Hypersensitivity

1982 ◽  
Vol 40 ◽  
pp. 336-337
Author(s):  
C. W. Mehard ◽  
W. L. Epstein
Keyword(s):  
Electron Microscope ◽  
White Female ◽  
X Rays ◽  
Blood Tests ◽  
Analytical Electron ◽  
Analytical Electron Microscope

The underlying cause of a disease may not he readily apparent but may have a long history in development. We report one such case which was diagnosed with the aid of the analytical electron microscope.The patient, a 48 yr. old white female, developed a tender nodule on the sole of her foot in December, 1981. Subsequently additional lesions developed on the same foot resulting in deep pain and tenderness. Superficial lesions also extended up to the knee on both legs. No abnormalities were revealed in blood tests or chest X-rays.

Application of analytical electron microscopy to the study of partitioning of silicon in a 2 wt% Si eutectoid steel

1978 ◽  
Vol 36 (1) ◽  
pp. 616-617
Author(s):  
N. Ridley ◽  
S.A. Al-Salman ◽  
G.W. Lorimer
Keyword(s):  
Electron Microscopy ◽  
Electron Microscope ◽  
Analytical Electron Microscopy ◽  
Eutectoid Steel ◽  
Minimum Diameter ◽  
Thin Foils ◽  
Analytical Electron ◽  
Analytical Electron Microscope ◽  
Transformation Front

The application of the technique of analytical electron microscopy to the study of partitioning of Mn (1) and Cr (2) during the austenite-pearlite transformation in eutectoid steels has been described in previous papers. In both of these investigations, ‘in-situ’ analyses of individual cementite and ferrite plates in thin foils showed that the alloying elements partitioned preferentially to cementite at the transformation front at higher reaction temperatures. At lower temperatures partitioning did not occur and it was possible to identify a ‘no-partition’ temperature for each of the steels examined.In the present work partitioning during the pearlite transformation has been studied in a eutectoid steel containing 1.95 wt% Si. Measurements of pearlite interlamellar spacings showed, however, that except at the highest reaction temperatures the spacing would be too small to make the in-situ analysis of individual cementite plates possible, without interference from adjacent ferrite lamellae. The minimum diameter of the analysis probe on the instrument used, an EMMA-4 analytical electron microscope, was approximately 100 nm.

STEM Study of Surface Plasmon Excitation in Small Spherical Particles

1990 ◽  
Vol 48 (2) ◽  
pp. 42-43
Author(s):  
Daniel UGARTE
Keyword(s):  
Energy Loss ◽  
Spherical Particles ◽  
Small Particles ◽  
Bulk Materials ◽  
Low Loss ◽  
Plasmon Excitation ◽  
Surface Modes ◽  
Surface Plasmon Excitation ◽  
Analytical Electron ◽  
Analytical Electron Microscope

Small particles exhibit chemical and physical behaviors substantially different from bulk materials. This is due to the fact that boundary conditions can induce specific constraints on the observed properties. As an example, energy loss experiments carried out in an analytical electron microscope, constitute a powerful technique to investigate the excitation of collective surface modes (plasmons), which are modified in a limited size medium. In this work a STEM VG HB501 has been used to study the low energy loss spectrum (1-40 eV) of silicon spherical particles [1], and the spatial localization of the different modes has been analyzed through digitally acquired energy filtered images. This material and its oxides have been extensively studied and are very well characterized, because of their applications in microelectronics. These particles are thus ideal objects to test the validity of theories developed up to now.Typical EELS spectra in the low loss region are shown in fig. 2 and energy filtered images for the main spectral features in fig. 3.

point-Analysis Using the Extrapolation Method in the Analytical Electron microscope

1990 ◽  
Vol 48 (2) ◽  
pp. 430-431
Author(s):  
Zenji Horita ◽  
Ryuzo Nishimachi ◽  
Takeshi Sano ◽  
Minoru Nemoto
Keyword(s):  
Electron Microscope ◽  
Extrapolation Method ◽  
X Ray ◽  
Absorption Correction ◽  
Point Analysis ◽  
Analytical Electron ◽  
Analytical Electron Microscope ◽  
Data Points ◽  
Identical Composition ◽  
X Ray Absorption

Absorption correction is often required in quantitative x-ray microanalysis of thin specimens using the analytical electron microscope. For such correction, it is convenient to use the extrapolation method[l] because the thickness, density and mass absorption coefficient are not necessary in the method. The characteristic x-ray intensities measured for the analysis are only requirement for the absorption correction. However, to achieve extrapolation, it is imperative to obtain data points more than two at different thicknesses in the identical composition. Thus, the method encounters difficulty in analyzing a region equivalent to beam size or the specimen with uniform thickness. The purpose of this study is to modify the method so that extrapolation becomes feasible in such limited conditions. Applicability of the new form is examined by using a standard sample and then it is applied to quantification of phases in a Ni-Al-W ternary alloy.The earlier equation for the extrapolation method was formulated based on the facts that the magnitude of x-ray absorption increases with increasing thickness and that the intensity of a characteristic x-ray exhibiting negligible absorption in the specimen is used as a measure of thickness.

Peak-to-background measurements on a 300-kV TEM/STEM

1992 ◽  
Vol 50 (2) ◽  
pp. 1236-1237 ◽  
Author(s):  
S. M. Zemyan ◽  
D. B. Williams
Keyword(s):  
Electron Microscope ◽  
X Ray ◽  
Background Ratio ◽  
Window Method ◽  
Analytical Electron ◽  
Analytical Electron Microscope ◽  
Cr Film

As has been reported elsewhere, a thin evaporated Cr film can be used to monitor the x-ray peak to background ratio (P/B) in an analytical electron microscope. Presented here are the results of P/B measurements for the Cr Ka line on a Philips EM430 TEM/STEM, with Link Si(Li) and intrinsic Ge (IG) x-ray detectors. The goal of the study was to determine the best conditions for x-ray microanalysis.We used the Fiori P/B definition, in which P/B is the ratio of the total peak integral to the average background in a 10 eV channel beneath the peak. Peak and background integrals were determined by the window method, using a peak window from 5.0 to 5.7 keV about Cr Kα, and background windows from 4.1 to 4.8 keV and 6.3 to 7.0 keV.

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