Structure of a new orthorhombic phase in NiTi: Mn shape memory alloys

Author(s):  
Jenö Beyer ◽  
Lajos Tóth

The structural changes during reversible martensitic transformation of near-equiatomic NiTi alloys can best be studied in TEM at around room temperature. Ternary additions like Mn offer this possibility by suppressing the Ms temperature below RT. Besides the stable intermetallic phases (Ti2Ni, TiNi, TiNi3) several metastable phases with various crystallographic structures (rhombohedral, hexagonal, monoclinic, cubic) have also been reported to precipitate due to suitable annealing procedures.TiNi:Mn samples with 0.9 and 1.3 at% Mn were arc melted in argon atmosphere and homogenized at 948 °C for 72 hours in high vacuum in an infrared furnace. After spark cutting slices of 0.2 mm, TEM specimens were prepared by electrochemical polishing with the twin-jet technique in methanol - perchloric acid electrolyte. The TEM study was carried out in a JEOL 200 CX analytical electron microscope.In this paper a new intermetallic phase is reported which has been observed in both samples by TEM during the martensitic transformation process.

Author(s):  
L. S. Lin ◽  
J. M. Walsh

The combined chemical and structural analysis capabilities of the analytical electron microscope (AEM) make it an important tool for understanding the nature of protective coatings on nickel-base superalloys. One of the important coating systems for protecting turbine blades from oxidation and hot corrosion is a MCrAlY alloy applied by electron beam physical vapor deposition (where M = Ni, Co, or Fe). In the as deposited condition this coating consists of a fairly open, generally columnar structure. A post-coating heat treatment on the order of 2 to 4 hours at approximately 1100°C is normally given to the coating. The major coating constituents are a β[(Ni,Co)Al] intermetallic phase and a γ[Co,Cr,Ni] solid solution phase. This heat treatment results in the formation of a ∼ 10 μm interdiffusion zone of phase transformation products at the coating/substrate interface and a thin protective layer (< 1 μm) of Al2O3 at the coating surface (Fig. l). While the coating contains just a few tenths of a percent yttrium, this yttrium plays an important role in improving the adherence of the protective Al2O3 layer. It has previously been proposed that the yttrium causes oxide pegs to develop at the Al2O3/coating alloy interface and that these pegs improve oxide adherence by mechanically keying the Al2O3 to the coating alloy.


Author(s):  
E. F. Koch ◽  
E. L. Hall ◽  
S. W. Yang

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.


Author(s):  
E. L. Hall

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.


Author(s):  
C. W. Mehard ◽  
W. L. Epstein

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.


Author(s):  
N. Ridley ◽  
S.A. Al-Salman ◽  
G.W. Lorimer

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.


Author(s):  
Daniel UGARTE

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.


Author(s):  
Zenji Horita ◽  
Ryuzo Nishimachi ◽  
Takeshi Sano ◽  
Minoru Nemoto

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.


Author(s):  
S. M. Zemyan ◽  
D. B. Williams

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.


Author(s):  
Vinayak P. Dravid ◽  
H. Zhang ◽  
L.D. Marks ◽  
J.P. Zhang

A 200 kV cold field emission gun atomic resolution analytical electron microscope (ARAEM, Hitachi HF-2000) has been recently installed at Northwestern. The ARAEM offers an unprecedented combination of atomic structure imaging of better than 0.20 nm nominal point-to-point resolution and about 0.10 nm line resolution, alongwith nanoscale analytical capabilities and electron holography in one single instrument. The ARAEM has been fully functional/operational and this paper presents some illustrative examples of application of ARAEM techniques to oxide superconductors. Additional results will be presented at the meeting.


Author(s):  
T. Kaneyama ◽  
M. Naruse ◽  
Y. Ishida ◽  
M. Kersker

In the field of materials science, the importance of the ultrahigh resolution analytical electron microscope (UHRAEM) is increasing. A new UHRAEM which provides a resolution of better than 0.2 nm and allows analysis of a few nm areas has been developed. [Fig. 1 shows the external view] The followings are some characteristic features of the UHRAEM.Objective lens (OL)Two types of OL polepieces (URP for ±10' specimen tilt and ARP for ±30' tilt) have been developed. The optical constants shown in the table on the next page are figures calculated by the finite element method. However, Cs was experimentally confirmed by two methods (namely, Beam Tilt method and Krivanek method) as 0.45 ∼ 0.50 mm for URP and as 0.9 ∼ 1.0 mm for ARP, respectively. Fig. 2 shows an optical diffractogram obtained from a micrograph of amorphous carbon with URP under the Scherzer defocus condition. It demonstrates a resolution of 0.19 nm and a Cs smaller than 0.5 mm.


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