The effect of testing procedure on DSC measurements of Gd-Ti-Zr alloy using ZrO2 container

Differential Scanning Calorimetry (DSC) was applied to determine the critical temperatures of phase transformations in the Gd40Ti30Zr30 alloy (wt%). The comparative measurements were carried out using three types of measuring devices at a temperature RT- 1650°C in the same flowing gas (Ar, 99.9992%) but applying different testing procedures, which allowed obtaining dissimilar oxygen contents in the surrounding atmosphere. The high temperature interaction and reactivity taking place between molten alloy samples and ZrO2 container during DSC tests were evaluated by structural analysis of the resulting interfaces using alloy samples solidified inside the ZrO2 containers. The conducted research has demonstrated methodological difficulties accompanying measurements of the thermophysical properties of Gd-rich alloys by the container-assisted DSC method, particularly when the tests are performed in flowing argon atmosphere with significantly reduced oxygen content. Under non-oxidizing conditions, the degradation of ZrO2 container can take place during DSC testing because the selected Gd40Ti30Zr30 alloy reacts with the ZrO2 to form a continuous interfacial reaction product layer. Under slightly oxidizing conditions, the gadolinium oxide formed in situ on the alloy surface, plays the role of a barrier for direct contact between molten alloy and container and thus may suppress or even prevent the degradation of the container and its subsequent strong bonding with the holder

Omega phase formation in ti–3wt

It is well known that severe plastic deformation not only leads to strong grain refinement and material strengthening but also can drive phase transformations. A study of the fundamentals of α → ω phase transformations induced by high-pressure torsion (HPT) in Ti–Nb-based alloys is presented in the current work. Before HPT, a Ti–3wt.%Nb alloy was annealed at two different temperatures in order to obtain the α-phase state with different amounts of niobium. X-ray diffraction analysis, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were applied for the characterisation of phase transitions and evolution of the microstructure. A small amount of the β-phase was found in the initial states, which completely transformed into the ω-phase during the HPT process. During HPT, strong grain refinement in the α-phase took place, as did partial transformation of the α- into the ω-phase. Therefore, two kinds of ω-phase, each with different chemical composition, were obtained after HPT. The first one was formed from the β-phase, enriched in Nb, and the second one from the α-phase. It was also found that the transformation of the α-phase into the ω-phase depended on the Nb concentration in the α-Ti phase. The less Nb there was in the α-phase, the more of the α-phase was transformed into the ω-phase

Kinetics of Corrosion Process in H2SO4 and HNO3 Aqueous Solutions of Lead Free Sn-Ag-Cu Solder Alloys

This paper presents the results of the corrosion resistance of Sn-Ag-Cu alloys in air-saturated aqueous solutions containing NO3-, SO42- ions, whose concentration was equivalent to their contents in acid rains and in concentrations 10 - 100 times higher. The Ag, Cu and Sn concentrations in the corrosive media were determined using the Atomic Absorption Spectrometry. The specific dissolution rate and corrosion current were derived using the a rotating disc technique. The corrosion rate of Sn- Ag-Cu alloys depends on pH of the examined solutions and on the concentration of oxygen near the phase boundary. In the whole range of concentrations of the applied H2SO4 + HNO3 mixtures of acids, the pure Sn was more corrosion resistant than eutectic alloy as well as the near eutectic one, following the sequence: Sn>Sn3.66Ag0.91Cu>3.8Ag0.7Cu

Kinetics of Corrosion Process in H2SO4 and HNO3 Aqueous Solutions of Lead Free Sn-Ag-Cu Solder Alloys

This paper presents the results of the corrosion resistance of Sn-Ag-Cu alloys in air-saturated aqueous solutions containing NO3-, SO42- ions, whose concentration was equivalent to their contents in acid rains and in concentrations 10 - 100 times higher. The Ag, Cu and Sn concentrations in the corrosive media were determined using the Atomic Absorption Spectrometry. The specific dissolution rate and corrosion current were derived using the a rotating disc technique. The corrosion rate of Sn- Ag-Cu alloys depends on pH of the examined solutions and on the concentration of oxygen near the phase boundary. In the whole range of concentrations of the applied H2SO4 + HNO3 mixtures of acids, the pure Sn was more corrosion resistant than eutectic alloy as well as the near eutectic one, following the sequence: Sn>Sn3.66Ag0.91Cu>3.8Ag0.7Cu

Characteristics of intermetallic phases in Cu/(Sn,Ni) diffusion couples annealed at 220 °C

The influence of Ni addition (5 at.%) on the morphology and chemical composition of the phases formedduring solid state reaction in Cu/(Sn,Ni) diffusion couples, annealed at 220 C for different periods oftime, was investigated. Chemical analysis of the reaction zone performed using scanning electron microscopy(SEM/EDS) identified several intermetallic phases. Near to the copper substrate, a thin andcontinuous layer of the Cu$_3$Sn phase was observed. Moving towards the (Sn,Ni) end of the diffusioncouple, the (Cu$_{1x}$Ni$_x$)$_6$Sn$_5$ phase was identified. This phase was represented by two types of structures: adiscontinuous layer located close to the Cu$_3$Sn phase, and precipitates (needles or faced) within the(Sn,Ni) end. These structures of (Cu$_{1x}$Ni$_x$)$_6$Sn$_5$ also varied in chemical composition. The experiment withsynchrotron radiation demonstrated two crystallographic variants of the Cu$_6$Sn$_5$ phase: hightemperaturehexagonal $\eta$ and low-temperature monoclinic $\eta'$; however, only the hexagonal variantwas confirmed by TEM. Differences in the morphology and chemical composition of the (Cu$_{1x}$Ni$_x$)$_6$Sn$_5$ phase were attributed to various mechanisms of their formation. The precipitates with a higher contentof Ni were most probably transformed from the Ni$_3$Sn$_4$ phase present in the initial (Ni,Sn) end-member,while the formation of the Ni-poor layer took place as a result of diffusion at the initial interface. Afterthe annealing experiment, the (Ni$_{1x}$Cu$_x$)$_3$Sn$_4$ phase was observed beyond the interface area as small, irregularly distributed precipitates in the (Sn,Ni) end-member. TEM examination allowed for the precisephase characterisation of the mentioned intermetallics. Moreover, except for the strong reflectionsvisible in SADP fitted to the hexagonal $\eta$-Cu$_6$Sn$_5$ phase, additional reflections were observed andassigned to the cubic Cu$_9$NiSn$_3$ phase

Charakterystyka szybko chłodzonych taśm stopu Al-Mn-Fe w stanie wyjściowym oraz po wygrzewaniu

Microstructure of conventionally cast and melt spun Al91Mn7Fe2 alloy was examined by X-ray diffraction, SEM and TEM techniques. Three different phases were found in a mould cast ingot: Al6(Mn, Fe), Al4(Mn, Fe) and aluminium solid solution. Rapidly quenched ribbons cast using melt spinning technique with different speed values of rotating wheel: 25, 30 and 36 m/s had average width in a range of 30-50 µ. It was found that ribbons contain quasicrystalline particles with different sizes and shapes including large dendrites in a range of micrometers and smaller spherical particles below 1 µ embedded in an aluminium matrix. Composition of these particles was similar to the Al4(Mn, Fe) phase. Also quasicrystals in the form of eutectic were observed with slightly different composition close to the Al6(Mn, Fe) phase. All observed particles revealed 2, 3 and 5- fold symmetry, typical for icosahedral quasicrystals. Increase in microhardness up to 274 HV for melt spun ribbon comparing to 141 HV for the as-cast ingot was observed due to a change in phase composition and refinement of the phases. Thermal stability of quasicrystalline phase in the ribbon was examined by annealing in different temperatures. Temperatures for thermal treatment were chosen based on DSC curve which contains the exothermic peak in the temperature range 300-500degrees Celsius. Analysis of ribbons annealed for 30 minutes at 400degrees Celsius showed that transformation of quasicrystals to stable crystalline phase starts at quasicrystal/Al-matrix interfaces. After annealing for 4 hours at 500degrees Celsius only the Al6(Mn, Fe) phase and aluminium solid solution were observed in the ribbon microstructure.Mikrostrukturę stopu Al91Mn7Fe2 odlanego do kokili oraz przygotowanego metoda odlewania na wirujący walec (melt spinning) scharakteryzowano za pomocą dyfrakcji rentgenowskiej oraz transmisyjnej i skaningowej mikroskopii elektronowej. W strukturze wlewka zaobserwowano trzy fazy: Al6(Mn, Fe), Al4 (Mn, Fe) oraz roztwór stały aluminium. Szybko chłodzone taśmy odlano przy trzech różnych prędkościach obracającego się walca: 25, 30 i 36 m/s. Grubość wszystkich otrzymanych taśm wynosiła około 30-50 µm. Mikrostruktura taśm składała sie z cząstek kwazikrystalicznych o zróżnicowanych kształtach i rozmiarach (w tym dużych dendrytów rzędu kilku mikrometrów, oraz mniejszych kulistych cząstek poniżej 1µm). Skład chemiczny tych cząstek był zbliżony do składu fazy Al4(Mn, Fe). Zaobserwowano również kwazikryształy w postaci eutektyki o składzie zbliżonym do składu fazy Al6(Mn, Fe). Uzyskane dyfrakcje elektronowe z obserwowanych cząstek wykazywały symetrie 2, 3 i 5-krotna, typowa dla kwazikryształów ikozaedrycznych. Zmiany składu fazowego oraz rozdrobnienia faz spowodowały wzrost mikrotwardości z 140 HV dla stopu wyjściowego do wartości 270 HV dla taśm. Stabilność termiczna fazy kwazikrystalicznej badano poprzez wygrzewanie taśm w różnych temperaturach, które wybrano w oparciu o krzywa DSC zawierająca pik egzotermiczny w przedziale temperatur 300-500 stopni Celsjusza. Analiza mikrostruktury taśmy wygrzewanej przez 30 min w 400 stopniach Celsjusza wykazała, że przemiana fazy kwazikrystalicznej w stabilna fazę krystaliczna rozpoczyna sie na granicy kwazikryształ/osnowa. Po wygrzewaniu przez 4 godz. w 500 stopniach Celsjusza w strukturze taśmy występowała jedynie faza Al6(Mn, Fe) oraz roztwór stały aluminium

Growth kinetics of the intermetallic phase in diffusion-soldered (Cu-5 at.%Ni)/Sn/(Cu-5 at.%Ni) interconnections

A stereological analysis was carried out in order to obtain the kinetics parameters of the (Cu1-xNix)6Sn5 growth in the diffusion soldered (Cu–5 at.%Ni)/Sn/(Cu–5 at.%Ni) interconnections where previously anomalous fast growth of this phase was described. The n-parameter in the equation x = ktn was found to be 0.27–0.15 in the temperature range 240–260 °C, respectively. This is far away from the volume control process (n = 1 if total surface of forming phase is the reference). The TEM/EDX microanalysis made across the (Cu1-xNix)6Sn5/Sn – solder showed sudden change of Sn and Cu content typical for the grain boundary diffusion as the rate controlling mechanism

Morphology and chemical composition of Cu/Sn/Cu and Cu(5 at-%Ni)/Sn/Cu(5 at-%Ni) interconnections

In the present paper, scanning and transmission electron microscopies as well as energy dispersive X-ray spectroscopy investigations were performed to describe the morphology and chemical composition of the intermetallic phases growing in Cu/Sn/Cu and Cu(Ni)/Sn/Cu(Ni) interconnections during the diffusion soldering process. The obtained results revealed that even a small amount of Ni addition (5 at-%) to the Cu substrate totally changes the morphology and the rate of formation of the intermetallic phase layers in the solder/substrate reaction zone of the interconnections prepared at the same time and joining temperature conditions. The presented studies are promising in terms of the shortening of the soldering time in the elecronic industry