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.

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.

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.

Phase identification in SiC whisker reinforced Al2O3-R2O3-based composites

1992 ◽  
Vol 50 (1) ◽  
pp. 152-153
Author(s):  
C.M. Sung ◽  
K.J. Ostreicher ◽  
M.L. Huckabee ◽  
S.T. Buljan
Keyword(s):  
Analytical Electron Microscopy ◽  
Phase Identification ◽  
Reinforced Composites ◽  
Ion Milling ◽  
X Ray ◽  
Binary Oxides ◽  
Analytical Electron ◽  
The Matrix ◽  
Second Phases ◽  
Convergent Beam

A series of binary oxides and SiC whisker reinforced composites both having a matrix composed of an α-(Al, R)2O3 solid solution (R: rare earth) have been studied by analytical electron microscopy (AEM). The mechanical properties of the composites as well as crystal structure, composition, and defects of both second phases and the matrix were investigated. The formation of various second phases, e.g. garnet, β-Alumina, or perovskite structures in the binary Al2O3-R2O3 and the ternary Al2O3-R2O3-SiC(w) systems are discussed.Sections of the materials having thicknesses of 100 μm - 300 μm were first diamond core drilled. The discs were then polished and dimpled. The final step was ion milling with Ar+ until breakthrough occurred. Samples prepared in this manner were then analyzed using the Philips EM400T AEM. The low-Z energy dispersive X-ray spectroscopy (EDXS) data were obtained and correlated with convergent beam electron diffraction (CBED) patterns to identify phase compositions and structures. The following EDXS parameters were maintained in the analyzed areas: accelerating voltage of 120 keV, sample tilt of 12° and 20% dead time.

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.

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.

Extended Core Edge Fine Structure in the E.M.

1980 ◽  
Vol 38 ◽  
pp. 120-121
Author(s):  
R.D. Leapman
Keyword(s):  
Fine Structure ◽  
Electron Scattering ◽  
Inelastic Electron ◽  
High Resolution Imaging ◽  
X Ray ◽  
Analytical Electron ◽  
Analytical Electron Microscope ◽  
Core Electrons ◽  
Resolution Imaging ◽  
X Ray Absorption

Extended X-ray Absorption Fine Structure (EXAFS) analysis makes use of synchrotron radiaion to measure modulations in the absorption coefficient above core edges and hence to obtain information about local atomic environments. EXAFS arises when ejected core electrons are backscattered by surrounding atoms and interfere with the outgoing waves. Recently, interest has also been shown in using inelastic electron scattering1-4. Some advantages of Extended X-ray-edge Energy Loss Fine Structure (EXELFS) are: a) small probes formed by the analytical electron microscope give spectra from μm to nm sized areas, compared with mm diameter areas for the X-ray technique, b) EXELFS can be combined with other techniques such as electron diffraction or high resolution imaging, and c) EXELFS is sensitive to low Z elements with K edges from ˜200 eV to ˜ 3000 eV (B to Cl).

The Impact of EDS In Materials Science Microanalysis

1998 ◽  
Vol 4 (S2) ◽  
pp. 168-169
Author(s):  
D. B. Williams
Keyword(s):  
Materials Science ◽  
X Ray ◽  
Electron Probe Microanalyzer ◽  
Thin Foils ◽  
Analytical Electron ◽  
Analytical Electron Microscope ◽  
Small Collection ◽  
Excellent Energy Resolution ◽  
The Impact

Since its invention in 1968, the EDS has played an essential role in X-ray analysis of materials, at the micrometer level, in the electron probe microanalyzer (EPMA). In the EPMA, the characteristic X-ray intensity from bulk specimens is sufficient that, despite its very small collection angle, the wavelength dispersive spectrometer (WDS) can also be used. Given the excellent energy resolution of the WDS it has often been the spectrometer of choice for bulk quantitative X-ray microanalysis. Therefore, the most important role of the EDS has been in X-ray microanalysis of thin specimens in the analytical electron microscope (AEM) because, in an AEM, the limited confines of the stage mean that EDS is the only viable spectrometer. Since the pioneering work of Cliff and Lorimer in the 1970s, EDS has been the method by which all high spatial resolution X-ray microanalysis of thin foils has been performed.

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