scholarly journals Contribution of Local Analysis Techniques for the Characterization of Iron and Alloying Elements in Nitrides: Consequences on the Precipitation Process in Fe–Si and Fe–Cr Nitrided Alloys

Materials ◽  
2018 ◽  
Vol 11 (8) ◽  
pp. 1409
Author(s):  
Hugo Van Landeghem ◽  
Raphaële Danoix ◽  
Mohamed Gouné ◽  
Sylvie Bordère ◽  
Andrius Martinavičius ◽  
...  

Atom Probe Tomography (APT), Transmission Electron Microscopy (TEM), and 3D mechanical calculations in complex geometry and anisotropic strain fields were employed to study the role of minor elements in the precipitation process of silicon and chromium nitrides in nitrided Fe–Si and Fe–Cr alloys, respectively. In nitrided Fe–Si alloys, an original sequence of Si3N4 precipitation was highlighted. Al–N clusters form first and act as nucleation sites for amorphous Si3N4 nitrides. This novel example of particle-simulated nucleation opens a new way to control Si3N4 precipitation in Fe–Si alloys. In nitrided Fe–Cr alloys, both the presence of iron in chromium nitrides and excess nitrogen in the ferritic matrix are unquestionably proved. Only a certain part of the so-called excess nitrogen is shown to be explained by the elastic accommodation of the misfit between nitride and the ferritic matrix. The presence of immobile excess nitrogen trapped at interfaces can be highly suspected.

1999 ◽  
Vol 577 ◽  
Author(s):  
K. Hono ◽  
D. H. Ping ◽  
S. Hirosawa

ABSTRACTThe nanocrystallization processes in Fe-Si-B-Nb-Cu and Fe-Nd-B(-Cu-Nb) amorphous alloys have been studied by transmission electron microscopy (TEM) and a three dimensional atom probe (3DAP). Cu additions are effective in refining the nanocrystalline microstructures of both alloys, because Cu atom clusters formed prior to the crystallization reaction serve as heterogeneous nucleation sites for the primary crystals. However, the clustering behaviors of Cu atoms in these two alloy systems are different, i.e., Cu completely dissolves in the Nd2Fe1 4B phase in the final microstructure of the Nd4.5Fe75.8B18.5Cu0.2Nb1 alloy, whereas CL' clusters grow to fcc-Cu particles in the Fe73.5Si13.5B9Nb3Cu1 alloy. The nanocrystallization processes in these two alloys clarified by the 3DAP results are compared.


Metals ◽  
2019 ◽  
Vol 9 (10) ◽  
pp. 1118
Author(s):  
Mattias Thuvander ◽  
Marcus Andersson ◽  
Krystyna Stiller

Molybdenum has been found to influence the complex precipitation process in a martensitic precipitation hardening stainless steel during aging at 475 °C in several different ways. Three steels with different Mo content (0, 1.2 and 2.3 at.%) were investigated. Studies of the microstructure were performed with atom probe tomography and energy filtered transmission electron microscopy. It is shown that, at the initial stage of aging, a faster nucleation of Cu-rich clusters takes place with increasing Mo content. The Cu-clusters act as precipitation sites for other solute elements and promote the nucleation of Ni-rich phases. During further aging, a higher Mo content in the material instead slows down the growth and coarsening of the Ni-rich phases, because Mo segregates to the interface between precipitate and matrix. Additionally, Mo promotes decomposition of the matrix into α and α′ regions. After longer aging times (>40 h) quasicrystalline Mo-rich R′ phase forms (to a greater extent in the material having the highest Mo content). The observations serve to understand the hardness evolution during aging.


1994 ◽  
Vol 338 ◽  
Author(s):  
Radhika Srinivasan ◽  
Tue Nguyen ◽  
Herbert L. Ho ◽  
Tai D. Nguyen

ABSTRACTDiffusion-induced precipitation in arsenosilicate glass (AsSG) under high temperature anneal is studied by high resolution Transmission Electron Microscopy (TEM), and other techniques. Polycrystalline precipitates of a few hundred angstroms in size have been observed near the interface of AsSG and the silicon substrate, covering the entire interface area after high temperature anneal. It is proposed that high concentrations of arsenic (above the solid solubility limit) precipitate initially at nucleation sites near the AsSG/silicon interface. Further anneal-induced diffusion of arsenic to the interface promotes growth of the precipitates. As a result, the precipitates cover the entire interface area, and impede further As diffusion into the Si substrate. Techniques to avoid the precipitation process without compromising the thermal budget or reduced arsenic diffusion have been explored and will be discussed.


2006 ◽  
Vol 519-521 ◽  
pp. 215-220 ◽  
Author(s):  
Shoichi Hirosawa ◽  
Tomoya Omura ◽  
Yoshikazu Suzuki ◽  
Tatsuo Sato

In this work, the bake-hardening (BH) response of an Al-3.0Mg-1.0Cu (in mass%) alloy has been improved by the small addition of Ag as a good example of our proposed Nanocluster Assist Processing (NCAP) technique. From the detailed observation through high resolution transmission electron microscopy (HRTEM), it is found that the origin of the increased hardness in the Ag-added alloy is attributed to the densely and uniformly formed Z phase at the expense of Guinier-Preston- Bagaryatsky (GPB) zones and the S’ phase. It is new findings that the Z phase is formed even in the ternary alloy although the chemical composition lies in the (α+S+T) phase field. Based on the threedimensional atom probe (3DAP) results, furthermore, it is suggested that nanoclusters of Mg, Ag and/or Cu provide effective nucleation sites for the Z phase, whereas nanoclusters of Mg and Cu do less. Such unique characteristics of Ag are clearly seen in the newly constructed interaction energy map (IE map).


Author(s):  
J. R. Michael ◽  
K. A. Taylor

Although copper is considered an incidental or trace element in many commercial steels, some grades contain up to 1-2 wt.% Cu for precipitation strengthening. Previous electron microscopy and atom-probe/field-ion microscopy (AP/FIM) studies indicate that the precipitation of copper from ferrite proceeds with the formation of Cu-rich bcc zones and the subsequent transformation of these zones to fcc copper particles. However, the similarity between the atomic scattering amplitudes for iron and copper and the small misfit between between Cu-rich particles and the ferrite matrix preclude the detection of small (<5 nm) Cu-rich particles by conventional transmission electron microscopy; such particles have been imaged directly only by FIM. Here results are presented whereby the Cu Kα x-ray signal was used in a dedicated scanning transmission electron microscope (STEM) to image small Cu-rich particles in a steel. The capability to detect these small particles is expected to be helpful in understanding the behavior of copper in steels during thermomechanical processing and heat treatment.


Author(s):  
T. Marieb ◽  
J. C. Bravman ◽  
P. Flinn ◽  
D. Gardner ◽  
M. Madden

Electromigration and stress voiding have been active areas of research in the microelectronics industry for many years. While accelerated testing of these phenomena has been performed for the last 25 years[1-2], only recently has the introduction of high voltage scanning electron microscopy (HVSEM) made possible in situ testing of realistic, passivated, full thickness samples at high resolution.With a combination of in situ HVSEM and post-testing transmission electron microscopy (TEM) , electromigration void nucleation sites in both normal polycrystalline and near-bamboo pure Al were investigated. The effect of the microstructure of the lines on the void motion was also studied.The HVSEM used was a slightly modified JEOL 1200 EX II scanning TEM with a backscatter electron detector placed above the sample[3]. To observe electromigration in situ the sample was heated and the line had current supplied to it to accelerate the voiding process. After testing lines were prepared for TEM by employing the plan-view wedge technique [6].


Author(s):  
E.A. Kenik ◽  
T.A. Zagula ◽  
M.K. Miller ◽  
J. Bentley

The state of long-range order (LRO) and short-range order (SRO) in Ni4Mo has been a topic of interest for a considerable time (see Brooks et al.). The SRO is often referred to as 1½0 order from the apparent position of the diffuse maxima in diffraction patterns, which differs from the positions of the LRO (D1a) structure. Various studies have shown that a fully disordered state cannot be retained by quenching, as the atomic arrangements responsible for the 1½0 maxima are present at temperatures above the critical ordering temperature for LRO. Over 20 studies have attempted to identify the atomic arrangements associated with this state of order. A variety of models have been proposed, but no consensus has been reached. It has also been shown that 1 MeV electron irradiation at low temperatures (∼100 K) can produce the disordered phase in Ni4Mo. Transmission electron microscopy (TEM), atom probe field ion microscopy (APFIM), and electron irradiation disordering have been applied in the current study to further the understanding of the ordering processes in Ni4Mo.


Minerals ◽  
2021 ◽  
Vol 11 (7) ◽  
pp. 727
Author(s):  
Shiyun Jin ◽  
Huifang Xu ◽  
Seungyeol Lee

The enigmatic Bøggild intergrowth in iridescent labradorite crystals was revisited in light of recent work on the incommensurately modulated structures in the intermediated plagioclase. Five igneous samples and one metamorphic labradorite sample with various compositions and lamellar thicknesses were studied in this paper. The lamellar textures were characterized with conventional transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM). The compositions of individual lamellae were analyzed with high-resolution energy-dispersive X-ray spectroscopy (EDS) mapping and atom probe tomography (APT). The average structure states of the studied samples were also compared with single-crystal X-ray diffraction data (SC-XRD). The Na-rich lamellae have a composition of An44–48, and the Ca-rich lamellae range from An56 to An63. Significant differences between the lamellar compositions of different samples were observed. The compositions of the Bøggild intergrowth do not only depend on the bulk compositions, but also on the thermal history of the host rock. The implications on the subsolidus phase relationships of the plagioclase feldspar solid solution are discussed. The results cannot be explained by a regular symmetrical solvus such as the Bøggild gap, but they support an inclined two-phase region that closes at low temperature.


2006 ◽  
Vol 519-521 ◽  
pp. 555-560 ◽  
Author(s):  
Peter V. Liddicoat ◽  
Tomoyuki Honma ◽  
L.T. Stephenson ◽  
Simon P. Ringer

During age-hardening of certain Al-Zn-Mg-Cu alloys, a 90% hardness increase can occur with 75 seconds. The clustering and precipitation of solute element species during this early rapid hardening (RH) period has been investigated through atom probe tomography, transmission electron microscopy, and Vickers hardness measurements. This study has focussed on the effect of copper by analysing three alloys; Al-2.0Zn-1.8Mg-0.7Cu, Al-2.0Zn-1.7Mg-0.2Cu and Al-1.9Zn-1.7Mg (at.%). The early RH reaction in these alloys accounts for up to 70% of the total hardening (peak hardness minus as-quenched hardness) and takes place during the first 60 seconds of ageing. We report preferred solute-solute interactions in the as-quenched materials. This quenched-in nanostructure acts as a template for subsequent solute clustering, the nature of which we have correlated with ageing.


1984 ◽  
Vol 41 ◽  
Author(s):  
S. D. Walck ◽  
J. J. Hren

AbstractAccurate depth profiling of implanted hydrogen and its isotopes in metals is extremely important. Field ion microscopy and atom-probe techniques provide the most accurate depth profiling analytical method of any available. In addition, they are extremely sensitive to hydrogen. This paper reports our early work on hydrogen trapping at defects in metals using the Field Ion Microscope/Imaging Atom Probe (FIM/IAP). Our results deal primarily with the control experiments required to overcome instrumental difficulties associated with in situ implantation and the influence of a high electric field. Transmission Electron Microscopy (TEM) has been used extensively to independently examine the influence of high electric fields on emitters.


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