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This article focuses on the experimental determination of the transformation temperature of Si-30B alloy in the temperature range of 25-1820 °C in a flowing gas atmosphere (He, 99.9992%) carried out by simultaneous differential thermal analysis and thermogravimetric analysis (DTA–TG) using a graphite container. The DTA curve during heating showed the presence of two critical temperatures, i.e., T = 1380.7 °C and T = 1532.0 °C. The first one corresponds to the melting point of a eutectic system (Si + SiB6). The high-temperature interaction and reactivity between the alloy and the container during DTA–TG test were evaluated by scanning electron microscopy coupled with energy-dispersive x-ray analysis. The results have demonstrated that the graphite container reacts with both liquid silicon and boron dissolved in liquid constituent of the alloy to form SiC and B4C, respectively.

High-temperature interaction between molten conventional gray cast iron (wt.%: 4.1 C; 1 Si; 0.20 Mn; 0.03 S; 0.04 P, the rest—Fe) and multiphase Al2O3-ZrO2-SiO2 ceramic substrate (wt.%: 51.5 Al2O3, 33.8 ZrO2, 13.3 SiO2, ~ 1 NaO2, 0.15 Fe2O3 + TiO2 + CaO) was examined at a temperature of 1450 °C for 15 min under inert flowing gas atmosphere (Ar, 850-900 hPa) using a sessile drop method coupled with contact heating procedure. Melting, wetting behavior and solidification of gray cast iron sample were continuously recorded with a high-speed high-resolution CCD camera. Under conditions of this study, selected gray cast iron alloy does not wet the Al2O3-ZrO2-SiO2 ceramic forming the final contact angle with average value of θf ~ 135°. The wetting kinetic curve was not smooth and its shape suggests the effect of substrate chemical heterogeneity due to multiphase composition of the substrate material. After the sessile drop test, the solidified drop was easily detached from the ceramic substrate along the drop-side interface showing a lack of bonding between the drop and the substrate. Structural characterization of the drop/substrate couple evidenced the nucleation and growth of graphite at the drop surface and at the drop/substrate interface taken place during solidification and resulting into the formation of discontinuous interfacial graphite layer.

Background: Umbilical vessels present after birth allow a unique central access for both venous and arterial catheterization, yet the catheterization complications can be misdiagnosed as the complications of prematurity per se. Methods: A prospective observational study of 41 used polyurethane umbilical catheters, both venous and arterial was conducted in a tertiary neonatal intensive care unit. The study consisted of bedside ultrasound imaging and post-removal microbiological and microstructural analysis to assess the in vivo catheters’ changes and their clinical significance. Results: The study has shown that catheters’ surface thrombosis and bacterial colonization happen more often within umbilical venous than within arterial catheters (31% vs 8% in both cases) and are inversely proportional to the patient’s gestational age (thrombosis: Me: 28 weeks vs no thrombosis: 32 weeks; p = 0.05, bacterial colonization: 27 weeks vs no colonization: 30 weeks; p = 0.013), respectively. The clots formed near the catheter’s tip are correlated with catheter’s bacterial colonization. Chemical analysis with energy dispersive spectroscopy showed a higher calcium composition in used catheters (19.89% vs 0%, p = 0.016) and structure analysis in the scanning electron microscopy proved that within hours catheters become covered with an external coating of a constant thickness, not affected by the catheterization time. Conclusion: The following observations give a better insight to the complex in vivo interactions and call for a more intense bedside-monitoring of the indwelling devices.

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.

Differential scanning calorimetry (DSC) technique has been applied for the experimental determination of temperature and heat of phase transition of pure silicon (7 N) during heating and cooling cycles at the rate of 10 K min−1. The measurements were carried out in the temperature range of 25–1450 °C in a flow gas atmosphere (Ar, 99.9992%) using three types of crucibles made of alumina, h-BN and alumina covered with h-BN coating. The following characteristics were estimated from DSC curves: melting point of silicon—1414 °C, the heat of fusion—1826 J g−1 and the heat of solidification—1654 J g−1. It was found that the silicon evaporation phenomenon accompanying the tests had no effect on the measurements of temperature during solid-to-liquid and liquid-to-solid transformations and on the measurement of the latent heat of fusion. The effect of crucible type on the DSC measurements is discussed.

Resin-based binders are one of the main materials used in foundry molding and core sands. This work adds to the research on self-curing sands with furfuryl resin, which dominates in the production of large-size castings. The work concerns the possibility of using biodegradable polymers as a component of resin-based binders. Biodegradable or partially biodegradable polymers are a group of materials which have an increasing level of importance in many areas of life and technology. This is mainly due to the increase in waste deposited in landfills, water and soil. This problem also concerns waste from the casting production process with the use of disposable molds with resin-based binders, which are mainly residues from their mechanical regeneration process. The aim of the research presented in this paper was to determine the effect of polycaprolactone (PCL) on the structure of post-regeneration dust from molding sands before and after the biodegradation process carried out in a water environment. Structure studies were carried out by Fourier transform infrared spectroscopy (FTIR) and the changes in the mass by TG/DTA-QMS analysis. The article also presents the results of the research of the morphology carried out by scanning electron microscopy (SEM) and the chemical oxygen demand index (COD) in water extracts of dust samples.

The aim of the study was to obtain a preliminary data focused on the steam oxidation performance of multilayered coatings deposited on 310 stainless steel and 800H Incoloy. The coatings were obtained through the aluminizing thermal diffusion technology with the formation of aluminides; some coating options had an additional top layer of selected composition. In this study, five different coating systems, as well as uncoated metals, were exposed at 1000 °C using thermogravimetric analysis instrumentation simulating an initial stage of steam oxidation corrosion. In this work, along with determination of the mass change of the samples, microanalyses using light optical microscopy, scanning electron microscopy (SEM) equipped with energy x-ray dispersive spectrometry (EDS), as well as surface micro-hardness determination, have been carried out. The designed coating systems demonstrated promising high-temperature steam oxidation performance with no breakaway degradation issues.

The wettability of graphene-coated SiC single crystal (CGn/SiCsc) by liquid Cu (99.99%) was investigated by a sessile drop method in vacuum conditions at temperature of 1100 °C. The graphene layer was produced via a chemical vapor deposition routine using 4H-SiC single crystal cut out from 6″ wafer. A dispensed drop technique combined with a non-contact heating of a couple of materials was applied. The Cu drop was squeezed from a graphite capillary and deposited on the substrate directly in a vacuum chamber. The first Cu drop did not wet the CGn/SiCsc substrate and showed a lack of adhesion to the substrate: the falling Cu drop only touched the substrate forming a contact angle of θ0 = 121° and then immediately rolled like a ball along the substrate surface. After settling near the edge of the substrate in about 0.15 s, the Cu drop formed an asymmetric shape with the right and left contact angles of different values (θR = 86° and θL = 70°, respectively), while in the next 30 min, θR and θL achieved the same final value of ~ 52°. The second Cu drop was put down on the displacement path of the first drop, and immediately after the deposition, it also did not wet the substrate (θ = 123°). This drop kept symmetry and the primary position, but its wetting behavior was unusual: both θR and θL decreased in 17 min to the value of 23° and next, they increased to a final value of 65°. Visual observations revealed a presence of ~ 2.5-mm-thick interfacial phase layer reactively formed under the second drop. Scanning electron microscopy (SEM) investigations revealed the presence of carbon-enriched precipitates on the top surface of the first Cu drop. These precipitates were identified by the Raman spectroscopy as double-layer graphene. The Raman spectrum taken from the substrate far from the drop revealed the presence of graphene, while that obtained from the first drop displacement path exhibited a decreased intensity of 2D peak. The results of SEM investigations and Raman spectroscopy studies suggest that the presence of graphene layer on the SiC substrate suppresses but does not completely prevent chemical interaction between liquid Cu drop and SiC. Both chemical degradation (etching) and mechanical degradation of the graphene layer during drop rolling due to high adhesion of the Cu drop to the SiC substrate are responsible for mass transfer through the 2nd drop/substrate interface that in turn results in significant changes of structure and chemistry of the drop and the interface.

Light, stiff and strong materials capable of bearing load have become increasingly valuable for the design, construction and assembling of lightweight transportation systems such as aircraft, high-speed trains or even for the construction of satellites. In spite of the need, there are few promising new materials in current development that are suited for advanced applications. It is not surprising that R&D is highly focused on advanced ceramics and composites, i.e. MMC-type where the metal phase is an Al, Si or Ti-based alloy. To produce SiC-based composites with desirable properties, the reactive infiltration process has well known advantages over other conventional processing techniques. These processing routes have particular advantages over classical sintering and hot pressing techniques, i.e. lower processing temperatures, shorter times and near-net shape fabrication capabilities. However, many aspects are still not fully understood mainly related to the interfacial phenomena occuring during infiltration process. Currently, three are the greatest open challenges for scientists: theoretical description of the process by computational models, decrease or replacement of the unreacted Si, and finally, the possibility to “control” the “pore closure” phenomenon. A key contribution could be coming from know-how on wetting characteristics, reactivity, surface properties and thermodynamics concerning reacting phases [1]. Systematic investigations of wetting characteristics, reactivity, surface properties and thermodynamics concerning Si-Ti/C-based substrate couple have been carried out. In addition, infiltration experiments have been performed between Si-Ti/C-preform with different porosity. All the collected findings will be detailed in a next paper. In this work, the more relevant results obtained by wetting tests will be reported and briefly discussed., The NCN-National Science Center, Poland is greatly acknowledged for the financial support through the POLONEZ project number UMO-2016/23/P/ST8/01916. This project was carried out under POLONEZ-3 program which has received funding from European Union's Horizon 2020 research and innovation program under Marie Skłodowska-Curie grant agreement. No 665778.

The results of microstructural examinations of reaction products formed at liquid copper/graphene-coated monocrystalline SiC interface are presented. Samples were prepared during a wettability test performed under a vacuum at T = 1100 °C kept constant for 30 min by capillary purification-sessile drop method. Careful analyses of the microstructure and chemical composition were carried out at the interfaces by high resolution scanning electron microscopy combined with local analysis of chemical composition, Raman spectroscopy and computed tomography. The detailed structural investigations showed that in both systems, at the drop/substrate interface, the substrate (SiC) was dissolved and the zone of reaction products was composed of alternately arranged dark and bright layers.

The wetting behavior and reactivity between molten pure Gd and polycrystalline 3YSZ substrate (ZrO2 stabilized with 3 wt% of Y2O3)were experimentally determined by a sessile drop method using a classical contact heating coupled with drop pushing procedure. The test was performed under an inert flowing gas atmosphere (Ar) at two temperatures of 1362?C and 1412?C. Immediately after melting (Tm=1341?C), liquid Gd did not wet the substrate forming a contact angle of ?=141?. The non-wetting to wetting transition (? < 90?) took place after about 110 seconds of interaction and was accompanied by a sudden decrease in the contact angle value to 67?. Further heating of the couple to 1412 ?C did not affect wetting (?=67??1?). The solidified Gd/3YSZ couple was studied by means of optical microscopy and scanning electron microscopy coupled with X-ray energy dispersive spectroscopy. Structural investigations revealed that the wettability in the Gd/3YSZ system is of a reactive nature associated with the formation of a continuous layer of a wettable reaction product Gd2Zr2O7.

To develop an optimised manufacturing method of fly ash-reinforced metal matrix composites, the preliminary tests were performed on the cenospheres selected from fly ash (FACS) with halloysite nanotubes (HNTs) addition. The preform made out of FACS with and without the addition of HNT (with 5 and 10 wt.%) has been infiltrated by the pure aluminium (Al) via adapted gas pressure infiltration process. This paper reveals the influence of HNT addition on the microstructure (analysis was done by computed tomography and scanning electron microscopy combined with energy-dispersive x-ray spectroscopy), thermal properties (thermal expansion coefficient, thermal conductivity and specific heat) and the mechanical properties (hardness and compression test) of manufactured composites. The analysis of structure-property relationships for Al/FACS-HNT composites produced shows that the addition of 5 wt.% of HNT to FACS preform contributes to receiving of the best mechanical and structural properties of investigated composites.

Compact Cu matrix composites reinforced with graphene were prepared by thermochemical processes and cold isostatic pressing. Thermophysical properties were investigated using laser flash analysis, differential scanning calorimetry, and dilatometry. From the results of the measurements, it follows that within the entire investigated temperature range, both the thermal diffusivity and the calculated values therefrom of the thermal conductivity of copper-graphene composites change according to the temperature changes. Above 500 °C, abnormal decrease of the thermal diffusivity was registered for sample prepared from pure copper powder. In this case, the elevated temperature of test could cause sintering of copper particles, which were not coated by graphene. The as-received composites had higher thermal diffusivity and the thermal conductivity at the room temperature in comparison to the material obtained by standard pressing of pure copper powder. However, the production methods of some samples could cause their partial sintering. Based on the study, it could not be concluded that graphene only has impacts on the thermophysical properties.

Combination of extreme service conditions and complex thermomechanical loadings, e.g., in electronics or power industry, requires using advanced materials with unique properties. Dissipation of heat generated during the operation of high-power electronic elements is crucial from the point of view of their efficiency. Good cooling conditions can be guaranteed, for instance, with materials of very high thermal conductivity and low thermal expansion coefficient, and by designing the heat dissipation system in an accurate manner. Conventional materials such as silver, copper, or their alloys, often fail to meet such severe requirements. This paper discusses the results of investigations connected with Cu-C (multiwall carbon nanotubes (MWNTs), graphene nanopowder (GNP), or thermally reduced graphene oxide (RGO)) composites, produced using the spark plasma sintering technique. The obtained composites are characterized by uniform distribution of a carbon phase and high relative density. Compared with pure copper, developed materials are characterized by similar thermal conductivity and much lower values of thermal expansion coefficient. The most promising materials to use as heat dissipation elements seems to be copper-based composites reinforced by carbon nanotubes (CNTs) and GNP.

Wetting characteristics of the Al/ZrB2 system were experimentally determined by the sessile drop method with application of separate heating of the ZrB2 and Al samples and combined with in situ cleaning of Al drop from native oxide film directly in vacuum chamber. The tests were performed in ultrahigh vacuum of 10−6 mbar at temperatures 710, 800, and 900 °C as well as in flowing inert gas (Ar) atmosphere at 1400 °C. The results evidenced that liquid Al does not wet ZrB2 substrate at 710 and 800 °C, forming high contact angles (θ) of 128° and 120°, respectively. At 900 °C, wetting phenomenon (θ < 90°) occurs in 29th minute and the contact angle decreases monotonically to the final value of 80°. At 1400 °C, wetting takes place immediately after drop deposition with a fast decrease in the contact angle to 76°. The solidified Al/ZrB2 couples were studied by scanning and transmission electron microscopy coupled with x-ray energy diffraction spectroscopy. Structural characterization revealed that only in the Al/ZrB2 couple produced at the highest temperature of 1400 °C new phases (Al3Zr, AlB2 and α-Al2O3) were formed.

Wettability between liquid Ag and graphene-coated SiC single crystal has been investigated by dispensed drop method at T = 970 C under vacuum accompanied with subsecond recording of the drop/substrate images (100 frames per second) by high-speed high-resolution CCD camera. Non-contact heating method coupled with capillary purification of the Ag drop procedure has been applied. Scanning electron microscopy combined with EDS analysis and scanning probe microscopy combined with Raman spectroscopy techniques has been utilized for microstructure and surface characterization of samples before and after high-temperature wetting tests. Immediately after its detachment from the capillary, the Ag drop showed non-wetting behavior (h > 90) forming a high contact angle of h = 114. Surface characterization of the drop surface after wettability tests evidenced the presence of graphene and Si transferred from the substrate to the top of Ag drop. These findings suggest chemical interaction phenomena occurring at the interface. Locally, an intimate contact between liquid Ag and SiC substrate was allowed by the appearance of discontinuities in the graphene layer basically produced by thermomechanical stress. Local dissolution of carbon into liquid Ag and its reorganization (by segregation, nucleation and growth) as secondary graphene layer at the Ag surface was also observed.

For a successful implementation of newly proposed silicon-based latent heat thermal energy storage systems, proper ceramic materials that could withstand a contact heating with molten silicon at temperatures much higher than its melting point need to be developed. In this regard, a non-wetting behavior and low reactivity are the main criteria determining the applicability of ceramic as a potential crucible material for long-term ultrahigh temperature contact with molten silicon. In this work, the wetting of hexagonal boron nitride (h-BN) by molten silicon was examined for the first time at temperatures up to 1750 °C. For this purpose, the sessile drop technique combined with contact heating procedure under static argon was used. The reactivity in Si/h-BN system under proposed conditions was evaluated by SEM/EDS examinations of the solidified couple. It was demonstrated that increase in temperature improves wetting, and consequently, non-wetting-to-wetting transition takes place at around 1650 °C. The contact angle of 90° ± 5° is maintained at temperatures up to 1750 °C. The results of structural characterization supported by a thermodynamic modeling indicate that the wetting behavior of the Si/h-BN couple during heating to and cooling from ultrahigh temperature of 1750 °C is mainly controlled by the substrate dissolution/reprecipitation mechanism. © The Author(s) 2017 Open Access This article is distributed under the terms of the Creative Commons Attribution 4.0 International License (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution, and reproduction in any medium, provided you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons license, and indicate if changes were made.

The ionic contamination on printed circuit boards (PCB) having different surface finishes was examined using ionograph. The study was performed at the RT on three types of PCBs covered with: (i) hot air solder leveling (HASL LF), (ii) electroless nickel immersion gold (ENIG), and (iii) organic surface protectant (OSP), all on Cu substrates, as well as two types of fluxes, namely EF2202 and RF800. In the group of boards without soldered components, the lowest average value of contamination was for the ENIG 18 µm surface (0.01 μg NaCl/cm2). Boards with soldered components were more contaminated (from 0.29 μg NaCl/cm2 for the HASL LF 18 µm surface). After spraying boards with fluxing agents, the values of contaminants were the highest. The influence of phosphorus content in Ni-P layer of ENIG finish on ionic contamination was examined. In the group of PCBs with Au coating, the smallest amount of surface contaminants (0.32 μg NaCl/cm2) was for Ni-2-5%P layer. PCBs with Ni-11%P layer were higher contaminated (0.47 μg NaCl/cm2), and another with Ni-8%P layer had 0.81 μg NaCl/cm2. PCBs without Au coating, had the lowest contamination (0.48 μg NaCl/cm2) at phosphorous content equal 11%P. Higher contamination (0.67 μg NaCl/cm2) was at 2-5%P, up to 1.98 μg NaCl/cm2 for 8% of P. Boards with Au finish have lower value of contamination than identical boards without Au layer thus contributing to better reliability of electronic assemblies, since its failures due to current leakage and corrosion can be caused by contaminants.

The solderability of the SAC305 alloy in contact with printed circuit boards (PCB) having different surface finishes was examined using the wetting balance method. The study was performed at a temperature of 260 °C on three types of PCBs covered with (1) hot air solder leveling (HASL LF), (2) electroless nickel immersion gold (ENIG), and (3) organic surface protectant (OSP), organic finish, all on Cu substrates and two types of fluxes (EF2202 and RF800). The results showed that the PCB substrate surface finish has a strong effect on the value of both the wetting time t 0 and the contact angle θ. The shortest wetting time was noted for the OSP finish (t 0 = 0.6 s with EF2202 flux and t 0 = 0.98 s with RF800 flux), while the ENIG finish showed the longest wetting time (t 0 = 1.36 s with EF2202 flux and t 0 = 1.55 s with RF800 flux). The θ values calculated from the wetting balance tests were as follows: the lowest θ of 45° was formed on HASL LF (EF2202 flux), the highest θ of 63° was noted on the OSP finish, while on the ENIG finish, it was 58° (EF2202 flux). After the solderability tests, the interface characterization of cross-sectional samples was performed by means of scanning electron microscopy coupled with energy dispersive spectroscopy.

This work presents the results of a morphology analysis of the scale formed on Crofer 22APU steel at high temperature in atmospheres containing SO2. The studies of steel oxidation were conducted on pre-oxidised and non-pre-oxidised steel within the temperature range of 700–900 °C in a mixture of air of a varying SO2 content and in pure air. In the case of oxidation in pure air it was established that on the surface of the Crofer 22APU a two-layer scale is formed. The outer layer of the scale contains MnCr2O4, whereas the inner layer contains Cr2O3. The scale formed in the atmosphere containing SO2 is also comprised of two layers (outer MnCr2O4 and inner Cr2O3). The analyses were carried out with the use of the 35S isotope. The analyses of the phase composition and morphology of the formed scale were conducted with the use of SEM/EDX and TEM.

Usually, ‘as-received’ thin foils and/or sheets of FeCrAl+RE (RE: mostly Y and Hf) alloys are subjected to oxidation exposures directed towards testing their high-temperature oxidation behaviour at...

The results of corrosion studies of composite materials obtained by two state-of-the –art methods of powder metallurgy are presented in the article. The main goal of the studies was determination of high-temperature corrosion resistance of steel-matrix composites reinforced with 8 vol.% TiB 2 . Thermogravimetric analyses were conducted at 1100oC in air in 24 h cycle. Microstructure of the composited after thermogravimetric studies was observed at scanning electron microscope.

This work presents results observed after the first 5 h of oxidation of Haynes® 282® alloy. The steam oxidation tests have been carried out in pure water at 760 °C for 1, 2 and 5 h, respectively, using an accurate thermogravimetric balance technique. The alloy used for comparison in this work was fabricated using three different methods. The initial steam oxidation performance of the commercially wrought alloy Haynes® 282® was compared with a fabricated cast alloy and a HIP/PM alloy. The results show that in terms of corrosion resistance, fabrication techniques appear to have little impact on steam oxidation performance and behavior. The exposed Ni-based alloys all developed the oxide scales consisting mainly of Cr2O3 phase mixed with some TiO2, while internal Al and Ti precipitations along the grain boundaries were observed both in Haynes® 282® wrought and HIP/PM alloy.