Complex microstructural changes in as-cast eutectoid Zn-Al alloy

Phase transformations and microstructural changes of an as-cast eutectoid Zn-Al alloy (ZnAl₂₂Cu₂) were investigated during isothermal holding. The typical dendritic structures consisted of _s phase as a core with the edge of decomposed _s phase and decomposed _s in the interdendritic regions. A series of complex phase transformations was observed. Both decompositions of _s and _s were determined at an early stage of ageing and a four-phase transformation, _f+T+, was observed at the boundaries of _f phase and the phase, instead of clearly observed at the boundaries of phase, in a solution-treated Zn-Al alloy during prolonged ageing.     

Ageing characteristics of cast Zn-Al based alloy (ZnAl7Cu3)

Microstructure and ageing characteristics of a cast Zn-Al based alloy (ZnAl7Cu3) were studied using X-ray diffraction, electron scanning microscopy and back-scattered diffraction techniques. Two stages of phase transformation, i.e., decomposition of zinc rich phase and four phase transformation, + T + , were detected during ageing at 150°C. Electron back-scattered diffraction technique was applied in distinguishing both zinc rich and phases.     

Phase decomposition in extruded Zn-Al based alloy

Ageing characteristics of an extruded eutectoid Zn-Al based alloy were investigated using X-ray diffraction and scanning electron microscopy techniques. The extruded alloy consisted of Al rich phase and Zn rich _E and phases. The original cast eutectoid Zn-Al alloy was extruded at 250 °C. Both supersaturated _s and _s phase decomposed during extrusion and appeared as fine and coarse lamellar structures. The _E and phases particles formed in the original interdendritic region. It was found that two Zn rich phases _E and decomposed sequentially during ageing at 170, 140 °C. The decomposition of the _E phase occurred as a discontinuous precipitation in the early stage of ageing and the decomposition of the phase took place in a four phase transformation: + T + in the prolonged ageing. Two typical morphologies of the decomposition of the Zn rich phases _E and were distinctive in back-scattered scanning electron microscopy.     

TEM study of metastable β-phase decomposition in rapidly solidified Ti-6Al-4V alloy

A new rationale is presented for various decomposition products obtained from the metastable -phase found in Ti-6A1-4V alloy produced by hot isostatic pressing comminuted melt-spun fibres and cooled to room temperature by furnace cooling. This alloy has an -matrix with about 8 vol% retained -phase, which is supersaturated with -stabilizers to such an extent that the martensitic transformation has been suppressed. The metastable -phase decomposes by different modes during continuous cooling, depending on the actual composition of individual -grains. Less enrichment of vanadium and iron favours the direct formation of the equilibrium -phase from the -matrix, while greater enrichment of vanadium and iron leads to a spinodal decomposition of the metastable -phase, resulting in a + two-phase structure. During further continuous cooling, the -phase which is lean in -stabilizers will transform into isothermal -phase. In addition, an unknown phase has also been observed in the -phase, which is typified by the appearance of 1/2{112} reflections in the SAD patterns.     

Ageing characteristics of furnace cooled eutectoid Zn-Al based alloy

Phase transformations and microstructural changes of a furnace cooled eutectoid Zn-Al based alloy were studied during ageing at 100 and 170°C using X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) techniques. Three phase transformations occurred in the furnace cooled eutectoid Zn-Al alloy. The metastable _FC phase decomposed during isothermal ageing. The four-phase transformation, + T + followed the discontinuous decomposition of the _FC phase. Typical morphologies of the decomposition of the _FC and phases were observed in scanning electron microscopy. Decomposition of Al-rich phase was observed during the prolonged ageing by transmission electron microscopy. The different types of decomposition of the different metastable phases dominated at different stages of ageing.     

The crystallization of the amorphous alloy Fe40Ni40P14B6

The isothermal transformation behaviour of the metallic glass Fe₄₀Ni₄₀P₁₄B₆ between 320 and 400° C is described. Crystallization occurs by a eutectic mechanism to form Fe-Ni austenite and a body-centred tetragonal phase which is isomorphous with Fe₃P and Ni₃P. The eutectic crystals have a barrel shape such that the c-axis of the tetragonal phase is parallel to the barrel axis. The orientation relationship between the two phases is 1 1 0T 1 1 0 and 0 0 1T 1 1 2. The austenite phase contains (1 1 1) twins.     

γ ? α2 Phase transformation in fractured high temperature stress rupture Ti-48Al-2Nb(at.%)

The ₂ phase transformation in fractured high temperature stress rupture Ti-48Al-2Nb(at.%) alloy has been studied by analytical electron microscopy. ₂ and phases were found at grain boundaries. ₂ layers that suspended in layers and interfacial ledge higher than 2d ₍₁₁₁₎ at /₂ interfaces were observed in the lamellar grains. These facts indicated that ₂ phase transformation and dynamic recrystallization have occurred during high temperature stress rupture deformation. It can be concluded that deformation induced ₂ phase transformation and dynamic recrystallization resulted in the presence of particles at grain boundaries. A structural and compositional transition area between deformation-induced ₂(or ) and its adjacently original (or ₂) phases was found by HREM and EDS and is suggested as a way to transform between and ₂ phase during high temperature stress rupture deformation. The transition area was formed by slide of partial dislocations on close-packed planes and diffusion of atoms.     

The athermal α → ω transformation in Zr-2 at% Nb alloy

The athermal transformation in Zr-2 at.% Nb alloy has been investigated by transmission electron microscopy. Analysis of the selected-area diffraction pattern has shown that the orientation relationships between the omega and the parent-phase in quenched Zr-2 at.% Nb alloy are the same as have been previously observed for the reaction in pure zirconium. Thus it was deduced that the direct transition has taken place in the alloy during cooling. The-originated -particles were visualized using the dark-field technique. The formation of the athermal omega in the-region of-stabilized Zr-Nb alloy is discussed in terms of the relative positions of the free energy equilibrium curvesT ₀ ,T ₀ ,T ₀ and the correspondingM _s ,M _s andT _s start curves. It is concluded that the omega phase can occur over a much wider range of alloy compositions than is usually recognized on the basis of transformation data.     

A transmission-electron-microscopy study of a face-centred-cubic phase in an Al-Li-Cu-Mg-Zr alloy

Icosahedral T₂ phases can form either by solid-state precipitation or during solidification in Al-Li-Cu-Mg alloys. The T₂ phase forming during solidification can transform to an R phase at high annealing temperatures. The T₂ phase forming by solid-state precipitation coexists with the Y phase, which has a face-centred cubic (f.c.c.) structure with lattice parameter a2.0 nm and can form microtwins with the twin plane of (111). The orientation relationships between the C phase and the T₂ phase are: i¯5Y0 1 1, Y1 1 3; i¯3Y1 1 1, Y1 2 3, Y1 1 5; Y2 3 5; i2Y0 1 1, Y1 1 1, Y1 1 2, Y1 1 3, Y1 1 5.     

Influence of the α/β-SiC phase transformation on microstructural development and mechanical properties of liquid phase sintered silicon carbide

The transformation kinetics and microstructural development of liquid phase sintered silicon carbide ceramics (LPS-SiC) are investigated. Complete densification is achieved by pressureless and gas pressure sintering in argon and nitrogen atmospheres with Y2O3 and AlN as sintering additives. Studies of the phase transformation from to -SiC reveals a dependency on the initial -content and the sintering atmosphere. The transformation rate decreases with an increasing -content in the starting powder and in presence of nitrogen. The transformation is completely supressed for pure -SiC starting powders when the additive system consists of 10.34 wt% Y2O3 and 2.95 wt% AlN. Materials without phase transformation showed a homogeneous microstructure with equiaxed grains, whereas microstructures with elongated grains were developed from SiC powders with a high initial /-ratio (>1:9) when phase transformation occurs. Since liquid phase sintered silicon carbide reveals predominantly an intergranular fracture mode, the grain size and shape has a significant influence on the mechanical properties. The toughness of materials with platelet-like grains is about twice as high as for materials with equiaxed grains. Materials exhibiting elongated microstructures show also a higher bending strength after post-HIPing.     

The Ni3Al-Ni3Cr-Ni3Mo section of the Ni-Cr-Al-Mo system

An investigation is reported of the constitution of the 75 at % nickel section of the Ni-Cr-Al-Mo system in the temperature range 1523 to 1073 K. Alloys in the region 10 to 20 at % Al were annealed at 1523, 1273, and 1073 K, respectively, and subjected to electron microprobe analysis, X-ray diffraction, and microscopical and hardness examination. Constitutional data are presented as partial isothermal sections and as vertical sections. At 1523 K the section consists only of fields containing ,+ and , the last mentioned phase being predominant. With decreasing temperature the and + fields increase in extent. Also, the NiMo and Ni₃Mo phases were encountered in the ternary Ni-Al-Mo alloy studied. The quaternary + alloys showed small lattice mismatch values, i.e. up to 0.25%. Raft like morphologies of were found in the quaternary alloys, resulting from directional coarsening. Observations of as-cast structures are also reported.     

Mechanism of β1 formation in conventional dental amalgams

This study reexamined the mechanism of ₁ formation in conventional dental amalgams in the light of a previously unrecognized intergranular structure, the SnHg-₂ phase. Two amalgams, A (45. 5% Hg) and B (65. 0% Hg), were made from a Zn-free alloy of the following composition (wt%): Ag-70, Sn-26, Cu-4. After storage at 37°C for 1 day, both amalgams were heat treated at 70°C for up to 16 days. The structural changes in the two amalgams as a function of their heat treatment were characterized by differential scanning calorimetry and X-ray diffraction techniques. On the basis of the experimental data, we have proposed a new mechanism on ₁ formation. This mechanism involves a series of interrelated reactions. The primary one is a reaction between AgSn- and ₂ that leads to the nucleation of ₁ at boundaries. Simultaneous operation of several secondary and tertiary reactions result in (1) further growth of ₁ and its continuing change in composition, (2) loss of Sn from the ₁ matrix, (3) conversion of CuHg into , and (4) a possible transformation of ₂ into Sn-rich ₁ or ₁.     

Precipitation sequence of various kinds of metastable phases in Al-1.0mass% Mg2Si-0.4mass% Si alloy

The precipitation of three new types of metastable phases, i.e., TYPE-A, TYPE-B and TYPE-C, with different crystal structures from the phase is proposed from our research on the change in crystal structures and formation sequence of metastable phases during the aging of the Al-1.0mass% Mg₂Si-0.4mass% Si alloy by a combination of analytical high resolution electron microscopy and energy dispersive X-ray spectroscopy. The sequence of their formation is explained as follows. First, precipitation of the phase and TYPE-B precipitate, then dissolution into the matrix and degradation of the TYPE-B precipitate. Finally, predominant precipitation of the metastable TYPE-A precipitate. The TYPE-C precipitate appeared heterogeneously in the over-aged condition.     

An electron microscopic study of nickel sulfide inclusions in toughened glass

It has been known since the early sixties that nickel sulfide inclusions cause spontaneous fracture of toughened (thermally tempered) glass, but despite the considerable amount of work done on this problem in the last four decades, failures still occur in the field with regularity. In this study we have classified (by viewing through a 60× optical microscope) inclusions into two groups, which are classic and atypical nickel sulfides. The classics look like the nickel sulfide inclusions found at the initiation-of-fracture of windows that have broken spontaneously. We have compared the structure and composition of the atypical inclusions with the structure and composition of the classics. All of the classic and atypical nickel sulfide inclusions studied in this work were found to have a composition in the range of Ni₅₂S₄₈to Ni₄₈S₅₂. Inclusions on the nickel rich side of stoichiometric NiS were found to be two-phase assemblies, and inclusions on the sulphur rich side of NiS were single phase. It had been proposed that the atypicals were passive, and of a different composition to the classics. However, we found that the difference between passive and dangerous nickel sulfide inclusions was not a difference in composition but rather a difference in the type of material in the internal pore space. The passive's had carbon char in their internal pore space, whereas the pore space of dangerous inclusions contained Na₂O. The presence of Na₂O and carbon char with the inclusions indicates that the formation of the inclusions results from a reaction of a nickel-rich phase with sodium sulphate and carbon.     

Precipitation in Ni-Co-Al alloys

Discontinuous precipitation of the phase in Ni-Co-Al alloys has been studied in the temperature range 673 to 973 K using optical microscopy and transmission electron microscopy. Discontinuous precipitation was observed to occur in all the alloys to some degree, the extent of the precipitation decreasing with decreasing cobalt content of the alloy. Only in high cobalt alloys (greater than 38 at%) did the discontinuous transformation go to completion. The discontinuous transformation product consisted of fine straight coherent lamellae with a specific cube-cube orientation relationship to the matrix at low ageing temperatures and short times. At higher temperatures and longer times, continuous and discontinuous coarsening processes produced a coarse, less regular structure with a plate spacing ten times that of the regular structure. The overall kinetics of the discontinuous transformation were affected by the prior continuous precipitation of particles ahead of the discontinuous reaction fronts. The coarsening of these continuous particles as a function of time stopped the transformation in low cobalt alloys and continuously slowed the rate of transformation in high cobalt alloys resulting in Avrami exponents,n, less than 1. Reversion experiments and experiments on prestrained specimens yielded Avrami exponents ofn=1 lending support to the above suggestion. The major effect of cobalt in these alloys was to increase their propensity to transform discontinuously. This effect was largely due to the decrease in the rate of continuous precipitation and coarsening as a result of the increased partitioning of cobalt between and in high cobalt alloys.     

Liquid phase sintering of RE2O3: YSZ ceramics Part I Grain growth and expelling of the grain boundary glass phase

Experiments on silicate liquid phase sintering of YSZ ceramics with addition of 0.5 mol% of rare earth ions have been done in order to study the effect of these ions on the kinetics of grain growth and the expulsion of glass through the grain boundaries. Kinetics follow a third power law in the following order YPr>YPrEr>YY>YEr. The expelled glass does not spread over the ceramic grains and its mass is inversely related to grain size. Glass phase separation inside the grain boundaries is found to be a necessary condition for glass expulsion.     

Investigation of the excitonic insulator phase in bismuth-antimony alloys

Pressure-induced metal-semiconductor transitions in bismuth-antimony alloys in a strong magnetic field (up to 70 kOe) at helium temperatures have been investigated. It is found that for values of the overlap-gap |G|1 meV the alloy forms an excitonic insulator (EI) in magnetic fields above a certain threshold (30–40 kOe). It is inferred that the EI energy gap increases with the magnetic field. The maximum gap observed in fields of 70 kOe turns out to be ₀₀7.5 K. An analysis of the results shows that transitions to the EI phase are observed from both the semimetal and the semiconducting states. The critical transition temperatureT _c is related to the EI gap by the expressionT _c0.7. Arguments are advanced in support of the fact that the formation of the EI phase involves the pairing of electrons at theL point with holes at theT point.     

Stress-induced phase transformations in a hot-deformed two-phase (α2+γ) TiAl alloy

Stress-induced 2, 2 and 9R phase transformations in a hot-deformed Ti–45 at% Al–10 at% Nb alloy have been investigated using high-resolution transmission electron microscopy. The 2 phase transformation is an interface-related process. The interfacial superdislocations emitted from the misoriented semicoherent 2– interface react with each other or with the moving dislocations in the phase, resulting in the formation of the 2 phase. The nucleation of the 2 phase transformation takes place either at the 2– interfaces or at the stacking faults on the basal plane of 2 phase, and the growth of plate is accomplished by the moving of a/61 0 1 0 Shockley partials on alternate basal plane (0 0 0 1)2. The 9R structure was usually found to form at incoherent twin or pseudotwin boundaries. During deformation the interfacial Shockley partial dislocations of these incoherent twin and pseudotwin boundaries may glide on (1 1 1) planes into the matrix, resulting in the formation of 9R structure. The interfaces (including 2– and – interfaces) as well as the crystallographic orientation relationship between the as-received or stress-induced 2, and 9R phase have been analysed. The mechanisms for the stress-induced 2, 2 and 9R phase transformations were also discussed. © 1998 Chapman & Hall     

Morphology and phase transition of high melt temperature crystallized poly(vinylidene fluoride)

When PVDF is crystallized at temperatures above 155°C it presents a multiform morphology composed of ringed, non ringed and mixed spherulites. Infrared spectroscopy showed that the ringed spherulites are formed exclusively by the phase when crystallization takes place at temperatures below 155°C. Higher temperatures induce a solid-state phase transformation in these structures, increasing the amount of phase with crystallization time. The rate at which this transformation takes place increases with crystallization temperature. The non ringed spherulites, only formed at crystallization temperatures above 155°C, consist predominantly of the phase, crystallized from the melt, with small phase inclusions. The melt process of the different spherulites, observed by optical microscopy and calorimetric measurements (DSC) showed that the melt temperature of the phase, originated from the phase transition, is 8°C higher than that crystallized directly from the melt. Optical micrographs of samples heated up to 186°C and quickly cooled allowed visualization of the ringed spherulite regions which underwent the phase transformation at different crystallization times and temperatures.     

Precipitation hardening in Cu 1.81 wt % Be 0.28 wt % Co

The structure of the precipitation hardening alloy Cu 1.81 wt % Be 0.28 wt % Co has been studied as a function of ageing temperature and time, by transmission electron microscopy. The continuous precipitation sequence found is: supersaturated solid solution G.P. zones .The G.P. zone is an ordered platelet precipitate, which is coherent on {100} matrix planes and is nucleated in very high densities (>10²⁴ m^–3). The coherency stress fields, due to the misfit of the G.P. zone and matrix, overlap to produce a net matrix contrast along {110} 10, and give the characteristic tweed structure, which can be described by the kinematical theory of diffraction. The semi-coherent intermediate precipitate is nucleated by the G.P. zones and the transformation is characterized from the changes in the arrowhead structure produced in the electron diffraction patterns. No transformation of to the equilibrium precipitate is found for the ageing times investigated.