scholarly journals Formation mechanisms and atomic configurations of nitride phases at the interface of aluminum nitride and titanium

2008 ◽  
Vol 23 (8) ◽  
pp. 2221-2228 ◽  
Author(s):  
Chia-Hsiang Chiu ◽  
Chien-Cheng Lin

Aluminum nitride was bonded with a titanium foil at 1400 °C for up to 1 h in Ar. The AlN/Ti interfacial reactions were investigated using analytical electron microscopy. Reaction layers, consisting of δ-TiN, τ2-Ti2AlN, γ-TiAl, α2-Ti3Al, a two-phase region (α2-Ti3Al + α-Ti), and α-Ti (Al, N) solid solution, were observed after annealing at 1400 °C for 0.1 h. Among these phases, the α2-Ti3Al and (α2-Ti3Al + α-Ti) were formed during cooling. Further diffusion of N atoms into the reaction zone precipitates a chopped fiber-like α2-Ti2AlN in the matrix of γ-TiAl, with [110]γ−TiAl//[11¯20]τ2−Ti2AlN and (1¯1¯1)γ−TiAl//(1¯10¯3)τ2−Ti2AlN, by substituting N atoms for one-half Al atoms after annealing at 1400 °C for 1 h. The released Al atoms, due to the precipitation of τ2-Ti2AlN, resulted in an ordered Al-rich γ-TiAl or Ti3Al5. Furthermore, the α-Ti (Al, N) was nitridized into a lamellar layer (δ-TiN + α-Ti) with [110]δ−TiN//[11¯20]α−Ti and (111)δ−TiN//(0001)α−Ti.

2013 ◽  
Vol 58 (2) ◽  
pp. 473-476 ◽  
Author(s):  
G. Cempura ◽  
A. Kruk ◽  
C. Thomser ◽  
M. Wirtz ◽  
A. Czyrska-Filemonowicz

The microstructure of two tungsten based alloys (W-1.1%TiC and W-1.7% TiC) was characterized using light microscopy, analytical electron microscopy and electron tomography. These alloys represent a class of W based dispersion strengthened alloys with TiC used as strengthening particles. Addition of TiC leads to improved creep resistance and tensile strength of the W based alloys. The results show that the W-1.7%TiC alloy exhibits large scatter in grain size, much higher porosity and contains also Ti-O particles. The W-1.1%TiC alloy has fine grained microstructure with uniformly distributed fine TiC particles within the matrix and low porosity. As a result of the different microstructure, the W-1.1%TiC alloy exhibits better mechanical properties, when compared to the W-1.7%TiC alloy.


Author(s):  
M. Isaacson ◽  
M.L. Collins ◽  
M. Listvan

Over the past five years it has become evident that radiation damage provides the fundamental limit to the study of blomolecular structure by electron microscopy. In some special cases structural determinations at very low doses can be achieved through superposition techniques to study periodic (Unwin & Henderson, 1975) and nonperiodic (Saxton & Frank, 1977) specimens. In addition, protection methods such as glucose embedding (Unwin & Henderson, 1975) and maintenance of specimen hydration at low temperatures (Taylor & Glaeser, 1976) have also shown promise. Despite these successes, the basic nature of radiation damage in the electron microscope is far from clear. In general we cannot predict exactly how different structures will behave during electron Irradiation at high dose rates. Moreover, with the rapid rise of analytical electron microscopy over the last few years, nvicroscopists are becoming concerned with questions of compositional as well as structural integrity. It is important to measure changes in elemental composition arising from atom migration in or loss from the specimen as a result of electron bombardment.


Author(s):  
R.G. Frederickson ◽  
R.G. Ulrich ◽  
J.L. Culberson

Metallic cobalt acts as an epileptogenic agent when placed on the brain surface of some experimental animals. The mechanism by which this substance produces abnormal neuronal discharge is unknown. One potentially useful approach to this problem is to study the cellular and extracellular distribution of elemental cobalt in the meninges and adjacent cerebral cortex. Since it is possible to demonstrate the morphological localization and distribution of heavy metals, such as cobalt, by correlative x-ray analysis and electron microscopy (i.e., by AEM), we are using AEM to locate and identify elemental cobalt in phagocytic meningeal cells of young 80-day postnatal opossums following a subdural injection of cobalt particles.


Author(s):  
J. R. Porter ◽  
J. I. Goldstein ◽  
D. B. Williams

Alloy scrap metal is increasingly being used in electric arc furnace (EAF) steelmaking and the alloying elements are also found in the resulting dust. A comprehensive characterization program of EAF dust has been undertaken in collaboration with the steel industry and AISI. Samples have been collected from the furnaces of 28 steel companies representing the broad spectrum of industry practice. The program aims to develop an understanding of the mechanisms of formation so that procedures to recover residual elements or recycle the dust can be established. The multi-phase, multi-component dust particles are amenable to individual particle analysis using modern analytical electron microscopy (AEM) methods.Particles are ultrasonically dispersed and subsequently supported on carbon coated formvar films on berylium grids for microscopy. The specimens require careful treatment to prevent agglomeration during preparation which occurs as a result of the combined effects of the fine particle size and particle magnetism. A number of approaches to inhibit agglomeration are currently being evaluated including dispersal in easily sublimable organic solids and size fractioning by centrifugation.


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):  
J. R. Michael ◽  
A. D. Romig ◽  
D. R. Frear

Al with additions of Cu is commonly used as the conductor metallizations for integrated circuits, the Cu being added since it improves resistance to electromigration failure. As linewidths decrease to submicrometer dimensions, the current density carried by the interconnect increases dramatically and the probability of electromigration failure increases. To increase the robustness of the interconnect lines to this failure mode, an understanding of the mechanism by which Cu improves resistance to electromigration is needed. A number of theories have been proposed to account for role of Cu on electromigration behavior and many of the theories are dependent of the elemental Cu distribution in the interconnect line. However, there is an incomplete understanding of the distribution of Cu within the Al interconnect as a function of thermal history. In order to understand the role of Cu in reducing electromigration failures better, it is important to characterize the Cu distribution within the microstructure of the Al-Cu metallization.


Author(s):  
Edward A Kenik

Segregation of solute atoms to grain boundaries, dislocations, and other extended defects can occur under thermal equilibrium or non-equilibrium conditions, such as quenching, irradiation, or precipitation. Generally, equilibrium segregation is narrow (near monolayer coverage at planar defects), whereas non-equilibrium segregation exhibits profiles of larger spatial extent, associated with diffusion of point defects or solute atoms. Analytical electron microscopy provides tools both to measure the segregation and to characterize the defect at which the segregation occurs. This is especially true of instruments that can achieve fine (<2 nm width), high current probes and as such, provide high spatial resolution analysis and characterization capability. Analysis was performed in a Philips EM400T/FEG operated in the scanning transmission mode with a probe diameter of <2 nm (FWTM). The instrument is equipped with EDAX 9100/70 energy dispersive X-ray spectrometry (EDXS) and Gatan 666 parallel detection electron energy loss spectrometry (PEELS) systems. A double-tilt, liquid-nitrogen-cooled specimen holder was employed for microanalysis in order to minimize contamination under the focussed spot.


Author(s):  
C.M. Sung ◽  
K.J. Ostreicher ◽  
M.L. Huckabee ◽  
S.T. Buljan

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.


Author(s):  
M. Tamizifar ◽  
G. Cliff ◽  
R.W. Devenish ◽  
G.W. Lorimer

Small additions of copper, <1 wt%, have a pronounced effect on the ageing response of Al-Mg-Si alloys. The object of the present investigation was to study the effect of additions of copper up to 0.5 wt% on the ageing response of a series of Al-Mg-Si alloys and to use high resolution analytical electron microscopy to determine the composition of the age hardening precipitates.The composition of the alloys investigated is given in Table 1. The alloys were heat treated in an argon atmosphere for 30m, water quenched and immediately aged either at 180°C for 15 h or given a duplex treatment of 180°C for 15 h followed by 350°C for 2 h2. The double-ageing treatment was similar to that carried out by Dumolt et al. Analyses of the precipitation were carried out with a HB 501 Scanning Transmission Electron Microscope. X-ray peak integrals were converted into weight fractions using the ratio technique of Cliff and Lorimer.


Author(s):  
A. T. Fisher ◽  
P. Angelini

Analytical electron microscopy (AEM) of the near surface microstructure of ion implanted ceramics can provide much information about these materials. Backthinning of specimens results in relatively large thin areas for analysis of precipitates, voids, dislocations, depth profiles of implanted species and other features. One of the most critical stages in the backthinning process is the ion milling procedure. Material sputtered during ion milling can redeposit on the back surface thereby contaminating the specimen with impurities such as Fe, Cr, Ni, Mo, Si, etc. These impurities may originate from the specimen, specimen platform and clamping plates, vacuum system, and other components. The contamination may take the form of discrete particles or continuous films [Fig. 1] and compromises many of the compositional and microstructural analyses. A method is being developed to protect the implanted surface by coating it with NaCl prior to backthinning. Impurities which deposit on the continuous NaCl film during ion milling are removed by immersing the specimen in water and floating the contaminants from the specimen as the salt dissolves.


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