Kinetics of transient liquid phase diffusion bonding process for joining aluminium metal matrix composite

Abstract

The mechanism and kinetics of the transient liquid phase diffusion bonding process in a 6061–15 wt-%SiCp composite at 570°C, 0·2 MPa, with 200 μm thick copper foil interlayer, has been investigated by microstructural characterisation of the bond region using optical microscopy, scanning electron microscopy and electron probe microanalysis. The kinetics of isothermal solidification, representing the displacement of the solid/liquid interface y (in micrometres) as a function of time t (in seconds), followed a power law relationship y?=?157t^0·07. According to this kinetic equation, the effective diffusivity of copper in the composite system was found to be ～10⁶ times higher than the lattice diffusivity, indicating the dominance of short circuit diffusion through the defect rich particle/matrix interface.     

Influence of bonding variables on transient liquid phase bonding behavior of nickel based superalloy IN-738LC

The effect of process variables on the microstructure and properties of transient liquid phase (TLP) bonded IN-738LC superalloy was investigated using AMS 4776 filler metal. Continuous centerline eutectic phases, characterized as nickel-rich and chromium-rich borides, were observed at the joints with incomplete isothermal solidification. The eutectic width decreased with the increase of holding time and the increase in initial gap size resulted in thicker eutectic width in the samples bonded at the same temperature and for equivalent holding times. In contrast to the conventional expectation of the increase in the rate of isothermal solidification with the increase of temperature, rate decrease was observed with the increase of temperature to 1150 °C. The investigations demonstrated that low isothermal solidification rate was not only due to the enrichment of liquid phase with the base alloying elements such as Ti but also because of the reduction of solid solubility limit of B in the base metal contributed to the reduction of isothermal solidification rate. Microhardness and shear strength tests were carried out in order to investigate mechanical properties of the bonded samples. In the bonding condition in which isothermal solidification did not completely occur, eutectic constituent with the highest hardness in the bond region was the preferential failure source. The results showed that homogenized joints had the highest shear strength.     

Characterisation of dislocations, nanopipes and inversion domains in GaN by transmission electron microscopy

Transmission electron microscopy is used to analyse a range of defects observed in hexagonal GaN films grown on sapphire and GaN substrates by metalorganic chemical vapour deposition. Large angle convergent beam electron diffraction is used to analyse the Burgers vectors of dislocations and to show that hollow tubes, or nanopipes, are associated with screw dislocations having Burgers vectors±c. Weak-beam electron microscopy shows that dislocations are dissociated into partials in the (0001) basal plane, but that threading segments are generally undissociated. The presence of high densities of inversion domains in GaN/sapphire films is confirmed using convergent beam electron diffraction and the atomic structure of the {

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} inversion domain boundary is determined by an analysis of displacement fringes seen in inclined domains.     

Quantitative characterization of clay dispersion in polypropylene-clay nanocomposites by combined transmission electron microscopy and optical microscopy

This paper presents a novel method to describe the microstructure of polymer/clay nanocomposites quantitatively. Based on the image analyses of transmission electron microscopy (TEM) and optical microscopy micrographs, two parameters, degree of dispersion (χ) and mean interparticle distance per unit volume of clay (λ_V) are proposed to describe the level of clay dispersion. The degree of dispersion gives the percentage of exfoliation, and λ_V is a measure of spatial separation between particles relative to clay loading. A polypropylene/clay system was chosen as an example to show the effects of processing conditions and biaxial stretching on clay dispersion using the proposed quantifiers. It provides insights into the ‘real’ clay dispersion using a combination of both microscopical and macroscopical aspects.     

Comparison of glass hydration layer thickness measured by transmission electron microscopy and nanoindentation

The thicknesses of the hydration layers on the surfaces of 2 silicate glasses have been assessed using a) a combination of focused ion beam milling and transmission electron microscopy and b) nanoindentation; the two approaches give consistent layer thicknesses. Lighter contrast of the hydrated layers in TEM suggests that the layers have reduced density when compared to the bulk glasses; this is consistent with the reduced near surface modulus and hardness of hydrated glasses observed in nanoindentation.     

Ellipsometry and transmission electron microscopy study of MoSi2 coatings after oxidation at high temperature in air

MoSi₂ coatings were deposited on Si (100) substrates by means of magnetron sputtering. The structural and optical properties of the coatings were then investigated through transmission electron microscopy (TEM) and UV-visible-near IR ellipsometry after heat treatments in air at two temperatures (1100 K and 1600 K). After annealing at 1100 K, no silica layer could be observed by TEM at the surface of the MoSi₂ coating, whereas annealing at 1600 K gave rise to a protective silica layer. As observed by TEM, this silica layer contained nanometric molybdenum silicide crystals. Increasing the annealing time at 1600 K from 20 min to 2 h resulted in both a higher concentration and growth of these molybdenum silicide crystals in the silica layer. An optical model, taking into account the observed microstructure and allowing a good fit of the ellipsometry data, was developed. It is also shown that the dielectric constants of the non-oxidized part of the MoSi₂ layer became modified when the annealing temperature (1100 K versus 1600 K) and the annealing time at 1600 K (20 min versus 2 h) were increased.     

Characterisation of nano-structured titanium and aluminium nitride coatings by indentation, transmission electron microscopy and electron energy loss spectroscopy

Titanium and aluminium nitride Ti_1 − xAl_xN films deposited by radiofrequency magnetron reactive sputtering onto steel substrate are examined by transmission electron microscopy over all the range of composition (x = 0, 0.5, 0.68, 0.86, 1). The deposition parameters are optimised in order to grow nitride films with low stress over all the composition range. Transmission electron microscopy cross-section images of Vickers indentation prints performed on that set of coatings show the evolution of their damage behaviour as increasing x Al content. Cubic Ti-rich nitrides consist of small grains clustered in rather large columns sliding along each other during indentation. Hexagonal Al-rich films grow in thinner columns which can be bent under the Vickers tip. Indentation tests carried out on TiN and AlN films are simulated using finite element modelling. Particular aspects of shear stresses and displacements in the coating/substrate are investigated. The growth mode and the nanostructure of two typical films, TiN and Ti_0.14Al_0.86N, are studied in detail by combining transmission electron microscopy cross-sections and plan views. Electron energy loss spectrum taken across Ti_0.14Al_0.86N film suggests that a part of nitrogen atoms is in cubic-like local environment though the lattice symmetry of Al-rich coatings is hexagonal. The poorly crystallised domains containing Ti and N atoms in cubic-like environment are obviously located in grain boundaries and afford protection of the coating against cracking.     

Direct nanofabrication and transmission electron microscopy on a suite of easy-to-prepare ultrathin film substrates

A high-yield, easy to master method for preparing electron transparent metal, oxide, and carbon ultrathin film substrates suitable for direct nano/micro-fabrication and transmission electron microscopy (TEM) is presented. To demonstrate the versatility of these substrates for fabrication processes, we use e-beam lithography, self-assembled colloidal and protein templates, and microcontact printing to create patterned masks for subsequent electrodeposition of two dimensional and three dimensional structures. The electrodeposited structures range in scale from a few nanometers to a few micrometers in characteristic dimensions. Because fabrication occurs directly on ultrathin films, TEM analysis of the resulting materials and buried interfaces is straightforward without any destructive sample preparation. We show that all the normal TEM analytical methods (imaging, diffraction, electron and X-ray spectroscopies) are compatible with the fabricated structures and the thin film substrates. These electron transparent substrates have largely rendered the need for TEM sample preparation on fabricated structures obsolete in our lab.     

Microstructural analysis of germanium modified tin‐copper brazing filler metals for transient liquid phase bonding of aluminium

The present contribution summarises first results that have been achieved with the new brazing material Sn75Cu20Ge5 (wt‐%) for transient liquid phase (TLP) bonding of aluminium cast alloy AlSi7Mg0.3 (wt‐%). The microstructure of the braze ribbons and the obtained joints have been thoroughly investigated on different length‐scales using scanning and transmission electron microscopy as well. Whereas the braze ribbon material is only composed of beta‐tin, η‐phase (Cu₆Sn₅) and some germanium rich precipitates, the transient liquid phase joint displays a much more complex microstructure that consist mainly of beta‐tin and different aluminium‐copper and aluminium‐germanium phases. In addition small silicon oxide rods and a hitherto unreported hexagonal aluminium‐copper‐magnesium‐germanium phase with approximated lattice parameters a = 0.7123 nm, c = 2.40 nm have been found in the seam of the joint.     

Transmission electron microscopy application for the analysis of carbon black and metal-carbon nanostructures

Abstract

The article presents the analytical possibilities of the combined use of transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS) methods to study of carbon black and metal-carbon nanostructures. Platinum nanoparticles were shown to be formed on the carbon polyhedral structures and nanocapsules as a result of laser exposure to the carbon black suspensions in H₂PtCl₆ aqueous solution. Phase composition of nickel-carbon and cobalt-carbon core-shell structures was identified.     

Interfacial microstructure and defect analysis in Cu(In,Ga)Se([sub]2)-based multilayered film by analytical transmission electron microscopy and focused ion beam

Interfacial microstructures of Cu(In,Ga)Se₂(CIGS)-based multilayered film are closely characterized by TEM (transmission electron microscopy), SEM (scanning electron microscopy) and FIB (focused ion beam). A cross-sectional TEM, energy dispersive X-ray spectroscopy and energy-filtered TEM reveal that a pronounced Cu diffusion occurs across the interface of the CdS/CIGS, which leads to a large amount of Cu rich in the CdS layer and a Cu-deficient sub-surface in the CIGS layer as well as a rough interfacial structure. TEM studies further reveal that the interface microstructures in the multilayered film are dissimilar, both ZnO/CdS and CdS/CIGS interfaces are strongly bonded whereas the CIGS/Mo interface is weakly bonded and interface separation occasionally occurs. Mo back contact layer shows a well adhesion to glass substrate.Detailed observation on defects in the CIGS-based multilayered film is carried out by 3D (3-dimensional) FIB and SEM techniques. Sequential 2D (2-demensional) cross-sectioning shows that dominant growth-defects in the CIGS and top SiO₂ layers are micro-scale crack, appearing as diversified morphologies. The micro-scale crack in the CIGS layer is possibly released by propagating into the adjacent layer while the crack in the SiO₂ layer is relieved usually by forming a small particle behind. It is noted that in the multilayered film the interface frequently acts as crack initiation sites due to distinct thermal expansion coefficients.     

Transmission electron and optical microscopy of the domain structure of Ni3B7O13Br ferroic boracite

The study investigated the domain structure of nickel bromine boracite single crystals, by means of polarised-light in conjunction with transmission electron microscopy. Single crystals of Ni₃B₇O₁₃Br were grown by chemical transport reactions in closed quartz ampoules, in the temperature range of 1130 K and were examined by polarising optical microscopy (PLM), and transmission electron microscopy (TEM). PLM was also used in order to study the behaviour of birefringence as a function of temperature. For TEM the single crystals were crushed and mounted on holey carbon films. Comparative electron microscope images were useful for revealing the domain structure of this fully ferroelectric/fully ferroelastic material previously observed between the crossed polars of an optical microscope. X-ray diffraction analysis of the crystal under study was performed at room temperature.     

An analysis of the capillary force and optimum liquid volume in a transient liquid phase sintering process

A transient liquid phase sintering process, called the ISM (in situ microfusion) process, has been developed for Al---Fe alloys, where an exothermic reaction in the system is utilized to produce a small volume of liquid and densify the powder compact. The model of an interparticle force, due to the capillary action of a liquid in contact with two solid spheres, and the optimum liquid volume, in the rearrangement process for full densification in conventional liquid phase sintering, are no longer thought to be suitable for this particular process. A model has been established for the ISM process, in which two partly melted spheres are attracted by the molten liquid between them and the liquid volume is equal to that melted from the two spheres. Based on this system, the interparticle force two partly melted spheres was calculated and the optimum liquid volume estimated for the ISM process, both of which are in good agreement with previous experimental work.     

Effect of carbon content on solidification behaviors and morphological characteristics of the constituent phases in Cr-Fe-C alloys

A combination of transmission electron microscopy, electron backscatter diffraction and wavelength dispersive spectrum has been used to identify crystal structure, grain boundary characteristic and chemical composition of the constituent phases in Cr-Fe-C alloys with three different carbon concentrations. Depending on the three different carbon concentrations, the solidification structures are found to consist of primary α-phase and [α + (Cr,Fe)₂₃ C₆] eutectic in Cr-18.4Fe-2.3 C alloy; primary (Cr,Fe)₂₃ C₆ and [α + (Cr,Fe)₂₃ C₆] eutectic in Cr-24.5Fe-3.8 C alloy and primary (Cr,Fe)₇ C₃ and [α + (Cr,Fe)₇ C₃] eutectic in Cr-21.1Fe-5.9 C alloy, respectively. The grain boundary analysis is useful to understand growth mechanism of the primary phase. The morphologies of primary (Cr,Fe)₂₃ C₆ and (Cr,Fe)₇ C₃ carbides are faceted structures with polygonal shapes, different from primary α-phase with dendritic shape. The primary (Cr,Fe)₂₃ C₆ and (Cr,Fe)₇ C₃ carbides with strong texture exist a single crystal structure and contain a slight low angle boundary, resulting in the polygonal growth mechanism. Nevertheless, the primary α-phase with relative random orientation exhibits a polycrystalline structure and comprises a massive high-angle boundary, caused by the dendritic growth mechanism.     

Comparative determination of the α/β phase fraction in α+β-titanium alloys using X-ray diffraction and electron microscopy

A comparison is made between the measured α/β phase fractions in Ti-6246 using X-ray diffraction (XRD) and electron microscopy. Image analysis of SEM and TEM images was compared to the phase fraction estimate obtained using electron backscattered diffraction, lab and high-energy synchrotron XRD. There was a good agreement between the electron microscopic and diffraction techniques, provided that the microstructural parameters of grain size and texture are estimated correctly when using quantitative Rietveld refinement.