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The study involved measurements of surface tension of liquid binary copper-titanium alloys with respect to their chemical composition and temperature as well as investigations of the liquid alloy–refractory material-gaseous phase system wettability using usual refractory materials, i.e., graphite, aluminum oxide and magnesium oxide. The experiments were performed with the use of the sessile drop method and a high-temperature microscope coupled with a camera and a computer. The aim of this study was to determine the influence of titanium content in the Cu-Ti alloy on the surface tension and contact angle at the interface between the liquid alloy and the refractory material. The influence of temperature on these parameters was also examined. The tests were carried out for copper-titanium alloys with a maximum content of 1.5% wt. Ti, in the temperature range of 1373 to 1573 K. The test results indicate that as the titanium content in the alloy increases, its surface tension increases slightly. However, an increase in temperature causes a decrease in the surface tension of the alloys. In the case of an alloy containing 1.5% wt. Ti, surface tension at a temperature of 1373 K reaches 1351 mN∙m−1, and at a temperature of 1573 K, it decreases to 1315 mN∙m−1. As the temperature and titanium content in the alloy increase, a decrease in the contact angle is observed. The highest values of contact angles were recorded in the case of contact of the liquid alloy with graphite. For an alloy containing 0.1% wt. Ti at a temperature of 1373 K, the contact angle reaches 132°, while at a temperature of 1573 K, it decreases to 128°. For an alloy containing 1.5% wt. Ti, the values of contact angles are 100° and 96°, respectively. However, the contact angles have the lowest values for magnesium oxide. In the case of a temperature of 1573 K and an alloy containing 1.5% wt. Ti, the contact angle reaches 49°. Such a significant impact of titanium content on the contact angles may be due to its high affinity for oxygen (contact with a substrate made of Al2O3 and MgO and its reactivity with carbon (contact with graphite). [ABSTRACT FROM AUTHOR]

The high-temperature interaction between molten gray cast iron and Ti + C substrates that are composed of titanium and graphite powders was investigated by the sessile drop method combined with the non-contact heating of an alloy/substrate couple to a test temperature of 1330 °C in an inert gas atmosphere (argon). During the high-temperature testing, the images of the couple were recorded by a high-speed high-resolution CCD camera and used for estimating the values of the contact angles over time. An analysis of the wettability kinetics of the different Ti + C substrates by molten cast iron as well as a detailed structural characterization of the solidified couples with the help of light microscopy, electron microscopy (SEM, TEM), X-ray diffraction, and energy-dispersive X-ray spectroscopy have allowed us to explain the mechanism of high-temperature interaction in the selected couples. It was evidenced that the good wetting and fast infiltration of all of the examined substrates with the selected alloy had a reactive nature due to the dissolution of the Ti and graphite in the molten alloy (dissolutive wetting) and the reactively formed wettable TiC phase. These high-temperature phenomena contributed to the formation of three metal-infiltrated zones with different amounts and distributions of TiC particles in the Fe-based matrix. [ABSTRACT FROM AUTHOR]

The study involved measurements of surface tension of liquid binary copper-titanium alloys with respect to their chemical composition and temperature as well as investigations of the liquid alloy–refractory material-gaseous phase system wettability using usual refractory materials, i.e., graphite, aluminum oxide and magnesium oxide. The experiments were performed with the use of the sessile drop method and a high-temperature microscope coupled with a camera and a computer. The aim of this study was to determine the influence of titanium content in the Cu-Ti alloy on the surface tension and contact angle at the interface between the liquid alloy and the refractory material. The influence of temperature on these parameters was also examined. The tests were carried out for copper-titanium alloys with a maximum content of 1.5% wt. Ti, in the temperature range of 1373 to 1573 K. The test results indicate that as the titanium content in the alloy increases, its surface tension increases slightly. However, an increase in temperature causes a decrease in the surface tension of the alloys. In the case of an alloy containing 1.5% wt. Ti, surface tension at a temperature of 1373 K reaches 1351 mN∙m−1, and at a temperature of 1573 K, it decreases to 1315 mN∙m−1. As the temperature and titanium content in the alloy increase, a decrease in the contact angle is observed. The highest values of contact angles were recorded in the case of contact of the liquid alloy with graphite. For an alloy containing 0.1% wt. Ti at a temperature of 1373 K, the contact angle reaches 132°, while at a temperature of 1573 K, it decreases to 128°. For an alloy containing 1.5% wt. Ti, the values of contact angles are 100° and 96°, respectively. However, the contact angles have the lowest values for magnesium oxide. In the case of a temperature of 1573 K and an alloy containing 1.5% wt. Ti, the contact angle reaches 49°. Such a significant impact of titanium content on the contact angles may be due to its high affinity for oxygen (contact with a substrate made of Al2O3 and MgO and its reactivity with carbon (contact with graphite).

[Display omitted] Contact angle can be a key parameter in chemical engineering. However, the development and the optimization of numerous processes using supercritical CO 2 , considered as environmentally friendly, require new measurements under dense CO 2 atmosphere. Besides, the influence of the roughness or the wetting regime on the contact angle is known at ambient conditions but remains to be discussed for systems under high pressure. Contact angle measurements of ethanol, water, and their mixtures, with ethanol mass fractions ranging from 0.25 to 0.75, on two stainless steels in saturated CO 2 at pressures ranging from 0.1 MPa to 15.1 MPa, and at 313 K and 333 K were carried out in a set-up improving mass transfer between the studied liquid and the continuous fluid phase. Stainless steel surfaces have been characterized by atomic force and scanning electron microscopies allowing the application of the Wenzel equation. Ethanol wetted totally both stainless steels while contact angles of all other liquids were increased by the rise of pressure, with contact angles up to 128° for water at 15.1 MPa. Trapped bubbles were observed at the solid/liquid interface and the bubble formation is discussed. Furthermore, the potential influence of bubble presence on the wetting regime is prospected through the question: could the pressure rise modify the wetting regime? [ABSTRACT FROM AUTHOR]

This work focuses on wetting two types of substrates (a platinum substrate and a polished graphite substrate) by molten polycomponent oxide system CaO–MgO–SiO2–Al2O3–B2O3 to test the level of interaction at high temperatures. The tested systems were subjected to high-temperature wetting tests in the temperature range from liquidus temperature to 1550 °C using the sessile drop method. A total of four oxide systems were tested with graded boron oxide contents ranging from 0 to 30 wt%. The experiments were conducted in a CLASIC high-temperature resistance observation furnace and an inert atmosphere of high-purity argon. Droplet silhouettes were obtained with a CANON EOS 550D high-resolution camera during heat treatment, with reactive and non-reactive wetting occurring depending on the substrate type. The dependence of the average wetting angles on temperature and time was evaluated, and it was found that boron oxide decreased the average wetting angles of molten oxide droplets. The analyses were accompanied by the SEM/EDX analysis of the substrate and FTIR analysis of the droplets after high-temperature experiments. The phase composition of the oxide systems was evaluated by XRD analysis. [ABSTRACT FROM AUTHOR]

For the first time, experimental data on the high-temperature interaction of liquid Mg with pure Ag are presented. The study was performed by the sessile drop method and capillary purification procedure. The test was carried out under isothermal conditions at 720 °C in a protective atmosphere of Ar + 5 wt.% H2. The solidified couple was subjected to detailed microstructural observations by scanning electron microscopy (SEM) coupled with energy-dispersive x-ray spectroscopy (EDS). Under the used conditions, immediately after contact with the Ag substrate, liquid Mg drop showed a good wetting (θ0 ~ 65°) followed by fast spreading over the substrate in subsecond time to form the final contact angle of θf ~ 31°.SEM/EDS analysis showed that θf is apparent because of a deep crater (200 μm) formed in the substrate under the drop by the dissolution of Ag in liquid Mg. SEM/EDS observations of complex structural transformations in the Mg/Ag couple due to high-temperature contact and subsequent cooling are in good agreement with the Ag-Mg phase diagram. Besides substrate dissolution, the interaction between liquid Mg and solid Ag at 720 °C is accompanied with the alloying of the Mg drop with Ag and the formation of a continuous layer of the β-AgMg phase at the Mg/Ag interface. During cooling, the chemical composition of the Mg(Ag) drop continuously changes, and this process is followed by the formation of the β-AgMg phase by secondary precipitation from Ag-saturated liquid, a partial transformation of the β-AgMg to ε′-Ag17Mg54 phase by peritectic reaction, followed by the solid-state transformation of the ε′-phase to the ε-AgMg3 phase, and finally, the solidification of residual liquid in the form of the two-phase eutectic mixture of AgMg4 + (Mg). The results obtained suggest that a very good wetting and fast spreading observed experimentally for the Mg/Ag couple is caused by high reactivity between liquid Mg and Ag substrate leading to the combined effect of two reactive wetting mechanisms, i.e. through dissolutive wetting and wetting through the formation of the interfacial reaction product (β-phase). [ABSTRACT FROM AUTHOR]

The interaction between molten iron and refractory is of great significance to understand the damage of refractory in steelmaking processes. In this work, the interactions between the molten iron and three kinds of magnesia aggregates: No. 1 containing CaZrO3-ZrO2 intergranular phase (mainly CaZrO3), No. 2 containing ZrO2-MgAl2O4 intergranular phase (mainly ZrO2) and No. 3 fused magnesia, were studied by the sessile drop method at 1823 K under two kinds of oxygen partial pressures of PO2 ≈ 1.87 × 10−1 Pa and PO2 ≈ 1.87 × 10−3 Pa. It was found that the interaction mechanism between molten iron and substrate was almost the same under the two oxygen partial pressures. No. 2 substrate had a larger interacted area with molten iron due to its physical properties and chemical composition and more amount of slag was formed between them. The oxygen was easy to be released from the closed pores in No. 2 substrate so that the molten iron on No. 2 substrate had higher oxygen content, resulting in the decreases of the contact angle and the surface tension of molten iron. Accordingly, No. 2 substrate was penetrated most seriously. The intergranular phase of No. 1 substrate was more resistant to FeO corrosion than that of No. 2 substrate. The FeO penetration into No. 3 substrate was mainly along the grain boundary. The larger bulk density and grain size of No. 3 substrate could reduce the FeO penetration.

In this paper examinations of high-temperature wetting tests of 3 systems of liquid alloy – cast iron in contact with ceramic materials: magnesia ceramics in combination with natural graphite were presented. After wettability testing, the microscopic observations of the morphology of the sample surface and the cross-section microstructure with the chemical composition in micro-areas were examined. One of the objective of this work was also to verify whether the graphite content would affect the wettability of the magnesia ceramics. The study of high-temperature wetting kinetics of the liquid alloy in contact with the ceramic material, by the "sessile drop" method with capillary purification (CP) procedure was conducted. Under the test conditions, at a temperature of 1450°C and time 15 minutes, all 3 experimental systems showed a non-wetting behaviour. The average contact angle for the system with cast iron drop on magnesia ceramics was 140°, on magnesia ceramics with 10 parts per weight of graphite was 137° and on magnesia ceramics with 30 parts per weight of graphite - 139°. Microscopic observations revealed that in the case of the sample consisting of the cast iron drop on the substrate with magnesia ceramics, the formation of fine separations was not observed, unlike the systems with the substrate with magnesia ceramics and the addition of natural graphite. Numerous, fine droplets accumulate on the graphite flakes and consist mainly of Si as well as Fe and O. On the other hand, the rough MgO grains have a gray, matt surface, without fine separations. The conducted observations indicate the mechanical nature of the bonding - liquid metal penetrates into the pores of the rough ceramics of the substrate. However, in the case of systems of cast iron drop with magnesia ceramics and addition of graphite, probably the adhesive connection and the physical attraction of elements derived from cast iron drop with the flake graphite appeared as well.

The wetting behavior of liquid magnesium drop on pure tungsten substrates was investigated, for the first time, with the sessile drop method combined with non-contact heating and capillary purification of a Mg drop from a native oxide film. A specially designed apparatus dedicated to the investigation of the high-temperature interaction of dissimilar materials was used. The comparative experiments were performed under isothermal conditions at temperatures of 700 °C and 740 °C using two atmospheres: Ar + 5 wt.% H2 and pure Ar, respectively. During high-temperature tests for 180 s, the images of the Mg/W couples were recorded with CCD cameras (57 fps) from two directions of observation. The solidified drop/substrate couples were subjected to structural characterization using scanning electron microscopy (SEM) coupled with energy-dispersive X-ray spectroscopy (EDS). Under the applied measurement conditions, liquid Mg revealed non-wetting behavior on W substrates (a contact angle θ > 90°). The average value of the contact angle under the flowing Ar atmosphere at 740 °C was θav = 115°, whereas it was higher under the flowing Ar + 5 wt.%. H2 atmosphere at a lower temperature of 700 °C, showing θav = 122°. Independently on employed atmosphere and temperature, SEM + EDS analysis of solidified sessile drop couples did not display any new phases and mass transfer between the Mg drop and the W substrate, whereas the presence of discontinuities at the Mg/W interface of cross-sectioned couples were well-distinguished. Non-wetting and a lack of permanent bonding between the Mg drop and W substrates have a good agreement with the Mg–W phase diagram calculated with the help of FactSage software and FTlite database, i.e., the non-reactive nature of the Mg/W couple because W does not dissolve in liquid Mg and it does not form any compounds with Mg. These findings allow for the recommendation of tungsten as a suitable refractory material for long-time contact with liquid Mg in different container-assisted methods of materials characterization as well as in liquid-assisted processing of Mg components. [ABSTRACT FROM AUTHOR]

• Wetting experiment using capillary purification procedure in sessile drop method ensured the in-situ cleaning of Al drop from native oxide. • Al drop showed good wetting at 720 °C on the deformed steel substrate - contact angle decreased from 35° to 7° after 100 s. • The interface zone was of dual-morphology: grains of Al5Fe2 phase penetrating steel substrate and θ-Al13Fe4 phase growing towards Al drop. • The Al5Fe2 phase formed the long colonies of similarly oriented grains, while the θ-Al13Fe4 phase was of needle shape morphology. • Dissolution of steel substrate and formation of the thick product layer beneath the drop were responsible for good wetting behaviour. The high-temperature liquid Al - solid S355J2N steel interaction was studied using a modified wettability test. A sessile drop method with a capillary purification procedure was employed for the first time, involving non-contact aluminium isothermal heating followed by the dropping of a pure liquid Al drop onto the severely deformed steel substrate and isothermal contact heating of Al with steel. The calculated contact angles and wetting kinetics curves demonstrated a good spreading and wetting of the investigated system. Scanning electron microscopy investigations played an important role in interpretation of the microstructural characteristics of the specimen, especially those located at the drop/substrate interface. The electron backscattered diffraction measurements allowed to characterize the microstructure of the interface zone to obtain more detailed information about the grain size, type of the intermetallic phases: θ-Al 13 Fe 4 , Fe 2 Al 5 , FCC Al and ferrite and their distribution in the neighborhood of the interface zone. These intermetallics were also confirmed via transmission electron microscopy studies coupled with energy-dispersive X-ray spectroscopy analysis of the drop/substrate interface. Research findings provide valuable insights into the liquid Al and steel interaction during the explosive welding process, where the local melting of metal takes place at the interface of colliding plates, strongly deformed due to the collision. [ABSTRACT FROM AUTHOR]

This work focuses on wetting two types of substrates (a platinum substrate and a polished graphite substrate) by molten polycomponent oxide system CaO–MgO–SiO2–Al2O3–B2O3 to test the level of interaction at high temperatures. The tested systems were subjected to high-temperature wetting tests in the temperature range from liquidus temperature to 1550 °C using the sessile drop method. A total of four oxide systems were tested with graded boron oxide contents ranging from 0 to 30 wt%. The experiments were conducted in a CLASIC high-temperature resistance observation furnace and an inert atmosphere of high-purity argon. Droplet silhouettes were obtained with a CANON EOS 550D high-resolution camera during heat treatment, with reactive and non-reactive wetting occurring depending on the substrate type. The dependence of the average wetting angles on temperature and time was evaluated, and it was found that boron oxide decreased the average wetting angles of molten oxide droplets. The analyses were accompanied by the SEM/EDX analysis of the substrate and FTIR analysis of the droplets after high-temperature experiments. The phase composition of the oxide systems was evaluated by XRD analysis.

The contact angle is a numerical index of differentiation between hydrophilic and hydrophobic soils. The objectives of this research are: 1) assessing different methods such as capillary rise, the molarity of ethanol droplet, repellency index, and sessile drop, and 2) Determining the most efficient method in a typical soil with sandy loam texture. In this study, hydrophobic soil was hydrophobized artificially using stearic acid and according to the water drop penetration time classification method. Calculated contact angles of hydrophilic soil with capillary rise method, the molarity of ethanol droplet method, repellency index (two methods of calculation), and sessile drop method were 89.9, 75.41, (57.81), 56.28, and 58.91, respectively. Using the contact angle measuring device, the contact angle of five hydrophobic levels were 58.91, 104.92, 120.48, 129.96, and 173.07, respectively. According to the precession of the device where the operator is capable to control data and processes and there is no limitation in usage, therefore, the sessile drop method is the most suitable method to measure contact angle. The contact angle of the late method and water drop penetration data are positively correlated (R2 = 0.975).

In this paper examinations of high-temperature wetting tests of 3 systems of liquid alloy – cast iron in contact with ceramic materials: magnesia ceramics in combination with natural graphite were presented. After wettability testing, the microscopic observations of the morphology of the sample surface and the cross-section microstructure with the chemical composition in micro-areas were examined. One of the objective of this work was also to verify whether the graphite content would affect the wettability of the magnesia ceramics. The study of high-temperature wetting kinetics of the liquid alloy in contact with the ceramic material, by the "sessile drop" method with capillary purification (CP) procedure was conducted. Under the test conditions, at a temperature of 1450°C and time 15 minutes, all 3 experimental systems showed a non-wetting behaviour. The average contact angle for the system with cast iron drop on magnesia ceramics was 140°, on magnesia ceramics with 10 parts per weight of graphite was 137° and on magnesia ceramics with 30 parts per weight of graphite - 139°. Microscopic observations revealed that in the case of the sample consisting of the cast iron drop on the substrate with magnesia ceramics, the formation of fine separations was not observed, unlike the systems with the substrate with magnesia ceramics and the addition of natural graphite. Numerous, fine droplets accumulate on the graphite flakes and consist mainly of Si as well as Fe and O. On the other hand, the rough MgO grains have a gray, matt surface, without fine separations. The conducted observations indicate the mechanical nature of the bonding - liquid metal penetrates into the pores of the rough ceramics of the substrate. However, in the case of systems of cast iron drop with magnesia ceramics and addition of graphite, probably the adhesive connection and the physical attraction of elements derived from cast iron drop with the flake graphite appeared as well. [ABSTRACT FROM AUTHOR]

Surface characteristics of printing substrates are of the utmost importance to all types of paper that interact with ink. During all types of printing processes, the behaviour of the liquid phase (ink or dye) on the paper is directly defined by the paper cellulose-based surface. The printed ink spreads and penetrates more into paper fibres when the paper surface is rougher and more permeable. Contact angle measurements by sessile drop method are considered the most appropriate for determining the paper sheet surface energy. Paper as hydrophilic material has a high absorption rate resulting in a low contact angle. The objective of this study was to evaluate the surface free energy of laboratory-made papers containing straw pulp obtained from residues after the harvest of the most cultivated cereals in Croatia (wheat, barley and triticale). The obtained surface free energy results are promising for straw pulp usage in the manufacture of printing paper.

The corrosion of refractory is generally related to the wetting between slag and refractory. Investigating the wetting and corrosion characteristics of refractory by molten slag has a positive significance to elucidating the corrosion mechanism and understanding the slag resistance. In this work, the apparent contact angles of the CaO–Al 2 O 3 –SiO 2 –(MgO) molten slags on microporous magnesia aggregate (MM) and fused magnesia (FM) substrates were respectively measured by sessile drop method under Ar atmosphere at 1550 °C. The dissolution of the MM substrate and the slag penetration behavior were investigated by combining the theoretical calculation of the FactSage thermodynamic software with the examination of SEM-EDS. The results show that MM substrate had a better slag resistance than FM substrate. The final apparent contact angles (θ f) of slags with the CaO/SiO 2 values of 3, 5 and 11 on MM substrate were 15.8°, 21.4°, and 9.2°, respectively, and that with the MgO content of 3, 6 and 9 mass% were 11.1°, 14.2°, and 52.5°, respectively. The larger the CaO/SiO 2 value of the slag, the more beneficial it was to slowing down the dissolution of MM and FM substrates; the original slag with MgO was also beneficial to lessening the dissolution of the MM substrate, which was better than that with a high CaO/SiO 2 value. The formation of MA could inhibit the slag from penetrating. In addition, for slags with different CaO/SiO 2 values, the effects of surface tension and viscosity on slag penetration were more significant than that of contact angle; for slags with different MgO contents, the effect of contact angle on slag penetration was more significant than those of surface tension and viscosity. [ABSTRACT FROM AUTHOR]

The wetting and corrosion behavior of the corundum substrate anode by CaO–SiO 2 –MgO molten slag was investigated via the joint application of the sessile drop method with applied voltage and SEM-EDS technique. The slag drop exhibited a good wettability on the corundum substrate. The apparent contact angle at zero voltage slightly exceeded that at a 1 V applied voltage but was lower than those at 1.5 V and 2 V ones. Low applied voltage of 1 V had little effect on the corundum substrate's direct dissolution corrosion processes; high ones of not less than 1.5 V caused the electrode reaction to occur. The stirring effect of O 2 bubbles from the anode reaction aggravated the substrate's direct dissolution and physical stripping. It was found that the applied voltage could inhibit the slag penetration, and the apparent contact angle had no obvious relation with the direct dissolution thickness and penetration depth. A thin but almost continuous MgO⋅Al 2 O 3 (MA) layer could form at the slag/substrate interface at the applied voltage of 1.5 V. These results indicate the positive effect of applied voltage on the distribution of interfacial products and the molten slag penetration in reducing the corrosion of corundum anode under certain conditions. However, when the applied voltage was too high, the vigorous electrode reaction could aggravate the direct dissolution and physical stripping of the corundum anode, and damage the continuation of the formed interface product layer with a high melting point. [ABSTRACT FROM AUTHOR]

High temperature behavior of three compacted graphite iron (CGI) alloys on polycrystalline alumina substrates (99.7%, poro­sity

In this paper, temperature and concentration dependencies on density and surface tension of liquid Fe-C-O-Cr alloys (1.93 - 4.80 wt.% Cr) were investigated in high-temperature resistance observation furnace by a sessile drop method during heating from liquidus temperature to 1600°C. The interfacial characteristics (interfacial tension, wetting angle, work of adhesion, and spreading coefficient) of liquid alloy/alumina system were also determined depending on temperature. The effect of temperature and chromium content on surface and interfacial properties was proven in case of all examined alloys. Based on the fact that the content of surface-active elements such as oxygen (up to 195 ppm) and sulfur (up to 545 ppm) was higher, the influence of activities of both mentioned elements on surface tension of alloy samples was assessed. Particular attention was paid to the dependence of the surface tension temperature coefficient on oxygen and sulfur activity.

The wetting behavior of liquid magnesium drop on pure tungsten substrates was investigated, for the first time, with the sessile drop method combined with non-contact heating and capillary purification of a Mg drop from a native oxide film. A specially designed apparatus dedicated to the investigation of the high-temperature interaction of dissimilar materials was used. The comparative experiments were performed under isothermal conditions at temperatures of 700 °C and 740 °C using two atmospheres: Ar + 5 wt.% H2 and pure Ar, respectively. During high-temperature tests for 180 s, the images of the Mg/W couples were recorded with CCD cameras (57 fps) from two directions of observation. The solidified drop/substrate couples were subjected to structural characterization using scanning electron microscopy (SEM) coupled with energy-dispersive X-ray spectroscopy (EDS). Under the applied measurement conditions, liquid Mg revealed non-wetting behavior on W substrates (a contact angle θ > 90°). The average value of the contact angle under the flowing Ar atmosphere at 740 °C was θav = 115°, whereas it was higher under the flowing Ar + 5 wt.%. H2 atmosphere at a lower temperature of 700 °C, showing θav = 122°. Independently on employed atmosphere and temperature, SEM + EDS analysis of solidified sessile drop couples did not display any new phases and mass transfer between the Mg drop and the W substrate, whereas the presence of discontinuities at the Mg/W interface of cross-sectioned couples were well-distinguished. Non-wetting and a lack of permanent bonding between the Mg drop and W substrates have a good agreement with the Mg–W phase diagram calculated with the help of FactSage software and FTlite database, i.e., the non-reactive nature of the Mg/W couple because W does not dissolve in liquid Mg and it does not form any compounds with Mg. These findings allow for the recommendation of tungsten as a suitable refractory material for long-time contact with liquid Mg in different container-assisted methods of materials characterization as well as in liquid-assisted processing of Mg components.

Moisture damage occurs due to loss of cohesion and/or adhesion, which results in loss of stiffness and strength. Currently, the surface free energy (SFE) approach is used to calculate mixture performance in terms of various SFE parameters to assess moisture susceptibility of various newly developed binders. In the present study, the concept of SFE is used to evaluate the moisture-induced damage potential of newly modified bitumen using high-density polyethylene (HDPE) pyro-oil. For this purpose, parameters of SFE considered are work of adhesion, work of cohesion, wettability, and energy ratio (ER). HDPE pyro-oil was obtained from pyrolysis process at 750°C. For determination of surface tension properties of base and modified bitumen, this study used glycerol, formamide, and distilled water as probe liquid, and a sessile drop method was adopted to measure the static contact angle. The aggregates considered in this study were basalt, gravel, and limestone. Dispersive and polar components of aggregates were directly taken from the literature. In contrast, for base bitumen (VG30) and pyro-oil–modified bitumen (POMB), these components were determined using van Oss–Chaudhury–Good theory. Along with this, the variation in contact angle, SFE components and surface tension parameter of base and modified bitumen were studied for different time of ageing (0, 45, 85, and 150 min) using rolling thin film oven (RTFO) as per guidelines of Superpave. The investigation concludes that, for the parameters under study, the analysis of data does not show any regular pattern. Work of adhesion decreases whereas work of cohesion increases with ageing resulting in increased moisture susceptibility for pyro-oil–modified bitumen. Further, the results showed that pyro-oil was effective in enhancing the surface tension parameter as compared to the base binder for different ageing conditions. Based on the results of energy ratio, it is concluded that a combination of the binder with basalt gives higher resistance to moisture damage than limestone and gravel. [ABSTRACT FROM AUTHOR]

The contact angle is a numerical index of differentiation between hydrophilic and hydrophobic soils. The objectives of this research are: 1) assessing different methods such as capillary rise, the molarity of ethanol droplet, repellency index, and sessile drop, and 2) Determining the most efficient method in a typical soil with sandy loam texture. In this study, hydrophobic soil was hydrophobized artificially using stearic acid and according to the water drop penetration time classification method. Calculated contact angles of hydrophilic soil with capillary rise method, the molarity of ethanol droplet method, repellency index (two methods of calculation), and sessile drop method were 89.9, 75.41, (57.81), 56.28, and 58.91, respectively. Using the contact angle measuring device, the contact angle of five hydrophobic levels were 58.91, 104.92, 120.48, 129.96, and 173.07, respectively. According to the precession of the device where the operator is capable to control data and processes and there is no limitation in usage, therefore, the sessile drop method is the most suitable method to measure contact angle. The contact angle of the late method and water drop penetration data are positively correlated (R² = 0.975). [ABSTRACT FROM AUTHOR]

The contact angle between a membrane surface and a waterdrop lying on its surface provides important information about the hydrophilicity/hydrophobicity of the membrane. This method is well-developed for solid non-swelling materials. However, ion-exchange membranes (IEMs) are gel-like solids that swell in liquids. When an IEM is exposed to air, its degree of swelling changes rapidly, making it difficult to measure the contact angle. In this paper, we examine the known experience of measuring contact angles and suggest a simple equipment that allows the membrane to remain swollen during measurements. An optimized protocol makes it possible to obtain reliable and reproducible results. Measuring parameters such as drop size, water dosing speed and others are optimized. Contact angle measurements are shown for a large number of commercial membranes. These data are supplemented with values from other surface characteristics from optical and profilometric measurements.

High temperature behavior of three compacted graphite iron (CGi) alloys on polycrystalline alumina substrates (99.7%, porosity <3%) were examined by the sessile drop method combined with classical contact heating procedure in flowing Ar. High-speed high-resolution CCd camera was used for continuous recording of the CGi/Al2o3 couples during melting alloy, heating to and holding the couples at the test temperature of 1450°C for 15 min and their subsequent cooling. The comparative studies were made with conventional CGi (in wt.%: 3.70 C, 2.30 Si, 0.44 Mn, 0.054 P, 0.017 Mg, 0.015 S) and two alloys additionally containing the same amounts of 0.25 Mo, 0.1 V, 0.045 Sn and 0.032 Sb with different concentrations of Mg + Cu additions, i.e. 0.01Mg + 0.33Cu and 0.02Mg + 0.83Cu. All three CGi alloys demonstrated non-wetting behavior on the Al2o3 substrates while the contact angle values slightly decreased with increase of the Mg + Cu content in the alloy, i.e. 131° (unalloyed CGi), 130° (0.01Mg + 0.33Cu) and 125° (0.02Mg + 0.83Cu). Structural characterization of solidified couples by light microscopy and scanning electron microscopy coupled with energy dispersive X-ray spectroscopy revealed: 1) heterogeneous nucleation of discontinuous graphite layer at the drop-side interfaces and on the surface of the drops; 2) reactively formed Mg-rich oxide layer at the substrate-side interface; 3) the formation of satellite droplets on the surface of the drops during their solidification; 4) degeneration of initially compacted graphite to lamellar graphite after remelting and subsequent solidification of the drops, particularly in their surface layer. [ABSTRACT FROM AUTHOR]

Leaf wettability has an impact on a plant's ability to retain water on its leaf surface, which in turn has many environmental consequences. In the case of the potato leaf (Solanum tuberosum L.), water on the leaf surface may contribute to the development of a fungal disease. If fungal disease is caused, this may reduce the size of potato harvests, which contribute significantly to meeting global food demand. The aim of this study was to assess the leaf wettability of five potato cultivars (i.e., Bryza, Lady Claire, Rudawa, Russet Burbank, Sweet Caroline) in the context of its direct and indirect impact on potato yield. Leaf wettability was assessed on the basis of contact angle measurements using a sessile drop method with an optical goniometer. For Bryza and Rudawa cultivars, which showed, respectively, the highest and the lowest contact angle values, light microscopy as well as scanning electron microscopy analyses were performed. The results of the contact angle measurements and microscopic image analyses of the potato leaf surfaces indicated that the level of wettability was closely related to the type of trichomes on the leaf and their density. Therefore, higher resistance of the Rudawa cultivar to biotic stress conditions could be the result of the presence of two glandular trichome types (VI and VII), which produce and secrete metabolites containing various sticky and/or toxic chemicals that may poison or repel herbivores. [ABSTRACT FROM AUTHOR]

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. [ABSTRACT FROM AUTHOR]

Phase change heat transfer (e.g., boiling of water) on surfaces can be enhanced by tuning the surface wettability, which is often quantified by the contact angle and is expected to be influenced by temperature and pressure. However, the temperature (and pressure) dependence of contact angles of water on metallic surfaces remain unclear. In this study, an in situ characterization of the contact angles of water on 304 stainless steel surfaces at temperatures from room temperature to 250 °C and at pressures up to 15 MPa was performed using the sessile drop method. It was shown that three distinct regimes can be identified on the contact angle-temperature curves. A slightly-decreasing trend of the contact angles with temperature was observed below 120 °C, followed by a steeper linear decrease at higher temperatures. A further rise of the decreasing rate with temperature was observed above 210 °C. In contrast to temperature, the pressure was shown to have little effects on the contact angles. Based on the theory of surface thermodynamics, the effects of temperature (and pressure) on the contact angles were analyzed in terms of the interfacial tensions. An empirical correlation was developed to predict the contact angles as a function of temperature. [ABSTRACT FROM AUTHOR]

• Experimentally investigated high-temperature interaction of liquid Mg with solid Cu. • Wettability of liquid magnesium on the solid metallic copper. • A very good wetting and spreading of liquid magnesium on solid copper (θ less than 90°). • The SEM/TEM/EDS analysis of the Mg/Cu couple after sessile drop test. For the first time, experimental results of the high-temperature interaction of liquid magnesium with pure copper are presented. The investigation was performed using the sessile drop method and capillary purification procedure allowing both non-contact heating of the Mg/Cu couple and in situ cleaning of the Mg drop from a native oxide film. The test was done under isothermal conditions at 710 °C in a protective atmosphere, which was a mixture of Ar + 5 wt% H 2. The images of the Mg/Cu couple collected during the high-temperature measurements were used to determine the time-dependent values of the contact angle (θ) formed between the liquid magnesium drop and the copper substrate. The solidified couple was subjected to detailed microstructural observations by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), both coupled with energy-dispersive X-ray spectroscopy (EDS). Under the applied measurement conditions, immediately after contact with the Cu substrate, the liquid Mg drop showed a very good wetting (θ 0 ∼ 22°), followed by rapid spreading over the substrate, forming a final contact angle θ f ∼ 11°. However, SEM/EDS analysis revealed that θ f is an apparent angle due to the deep crater (∼200 μm) formed in the substrate under the Mg drop by the dissolution of Cu in liquid Mg. The comparative SEM/TEM/EDS analysis suggests that good wetting and rapid spreading in the Mg/Cu couple are dominated by the reactive wetting mechanism due to the dissolution of the Cu substrate in the liquid Mg drop and its saturation with a high amount of dissolved Cu. Consequently, the microstructure of the solidified drop was composed of large Cu-rich primary MgCu 2 crystals surrounded with a two-phase eutectic mixture (MgCu 2 + Mg 2 Cu) formed at the final stage of cooling. In addition, the MgCu 2 phase was also nucleated and grown at the Mg/Cu interface to form a continuous layer. [ABSTRACT FROM AUTHOR]

Leaf wettability has an impact on a plant’s ability to retain water on its leaf surface, which in turn has many environmental consequences. In the case of the potato leaf (Solanum tuberosum L.), water on the leaf surface may contribute to the development of a fungal disease. If fungal disease is caused, this may reduce the size of potato harvests, which contribute significantly to meeting global food demand. The aim of this study was to assess the leaf wettability of five potato cultivars (i.e., Bryza, Lady Claire, Rudawa, Russet Burbank, Sweet Caroline) in the context of its direct and indirect impact on potato yield. Leaf wettability was assessed on the basis of contact angle measurements using a sessile drop method with an optical goniometer. For Bryza and Rudawa cultivars, which showed, respectively, the highest and the lowest contact angle values, light microscopy as well as scanning electron microscopy analyses were performed. The results of the contact angle measurements and microscopic image analyses of the potato leaf surfaces indicated that the level of wettability was closely related to the type of trichomes on the leaf and their density. Therefore, higher resistance of the Rudawa cultivar to biotic stress conditions could be the result of the presence of two glandular trichome types (VI and VII), which produce and secrete metabolites containing various sticky and/or toxic chemicals that may poison or repel herbivores.

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 (θ > 90°) forming a high contact angle of θ = 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. [ABSTRACT FROM AUTHOR]

The sessile drop method was implemented to calculate the values of the surface tension coefficient of liquid metals. Appropriate software was developed to increase the data processing efficiency and the accuracy of the obtained results. This paper provides information on the structure and applications of the designed programs as well as the underlying mathematical models used during computations. Since the determination of the surface tension coefficient in this study is based on the recognition of drop outlines from a digital image, the problems of calibration and appropriate photography mode adjustments are mentioned in this paper. In addition, the methods of controlling the research equipment using Arduino shields are described. Finally, the research results are presented in the form of graphs which show the temperature dependence of the studied parameters of metallic samples and compared with the literature data.

Research of the last years pointed out that most soils are neither completely hydrophilic nor hydrophobic, but exhibit a subcritical level of water repellency (i.e. contact angle, CA > 0° and < 90°). Soil water repellency (SWR) is mainly caused by organic compounds of different origin and structure, showing the relevance of biofilms and organic coatings present at many particle surfaces. Despite the importance of SWR for hydraulic processes like preferential flow phenomena, generation of heterogeneous moisture patterns, or surface run-off generation, detailed investigations on the spatial variability of SWR at various scales have rarely been carried out. We introduce a new and easy-to-apply operation for measuring the spatial distribution of SWR using a modified sessile drop method for direct optical assessment of CA at a small scale. The specific objectives of this paper are to apply a sampling and preparation technique that preserves the original spatial arrangement of soil particles and to characterize soil wettability in terms of CA at a high spatial resolution. Results revealed that the sampling and preparation technique allows determination of CA at the millimeter scale using droplets of 1 μL volume. Direct measurement on grain surfaces of the sand fraction is possible for grain sizes > 300 μm using drop volumes down to 0.1 μL. Geostatistical evaluation showed that the measurement grid scale is below the range of spatial dependency for droplets of 1 μL volume, but not for measurements on single grains (pure nugget effect). Results show further that the small-scale differences in wettability, especially for CA < 90°, cannot be detected by the conventional WDPT test. From these findings it can be concluded that the proposed technique allows the identification of small-scale variations in wettability that may promote the formation of heterogeneous flow fields and moisture patterns in soil under unsaturated conditions.

The purpose of this project is to investigate the wetting behaviors of Sn3-xAg0:5CuxIn (SAC-In) (x = 0:5 wt%, 1 wt%, and 2 wt%) alloys at various temperatures (250 °C, 280 °C, and 310 °C) on copper (Cu) substrate in argon (Ar) atmosphere. The contact angles (θ) of alloys were gaged by sessile drop technique. The alloys' microstructures were examined by scanning electron microscopy/energy dispersive spectroscopy. Intermetallic compounds of Cu3Sn, Cu6Sn5, and Ag3Sn were observed at the interface of SAC-In/Cu. The results of wetting tests represent that the addition of 1 wt% In improves the wetting properties of the Sn-3 wt%Ag-0.5 wt%Cu (SAC305) alloy. The lowest θ was obtained as 35:55° for Sn-2 wt%Ag-0.5 wt%Cu-1 wt%In alloy at 310 °C. [ABSTRACT FROM AUTHOR]

Abstract In this paper, the experimental performance of a new testing device designed for investigating the high temperature properties of molten Mg is presented. The newly developed device allows examining high temperature wetting behavior and thermophysical properties of molten Mg (and Mg alloys) by using various experimental procedures (e.g. classical sessile drop, pendant drop, dispensed drop and drop sucking). High temperature wettability tests at temperatures up to 1000 °C in an inert gas atmosphere or under high vacuum (up to 10−7 hPa) are now possible. It has been documented that the application of the classical sessile drop method combined with a capillary purification procedure successfully eliminates the problem of magnesium oxidation that traditionally affects obtained results. Selected examples of high temperature experiments carried out for molten Mg in contact with various refractories are presented in order to show a wide range of analytical possibilities of the new device. The results obtained by using the new device are important from both a high theoretical and practical perspective regarding liquid phase assisted fabrication and processing of Mg-based alloys and metal-matrix composites. [ABSTRACT FROM AUTHOR]

Surface tension and density measurements of liquid Ag-Sb-Sn alloys were carried out over a wide temperature range by using the sessile drop method. The surface tension experimental data were analyzed by the Butler thermodynamic model in the regular solution approximation. The wetting characteristics of these alloys on Cu and Ni substrates have been also determined. The new experimental results were compared with the calculated values as well as with data available in the literature.

The wettablity at a liquid of pure-Al or Al-Mg alloys/ Al2O3 interface wasevaluated by the sessile drop method at 700oC and with a vacuum pressure of10-4Pa. The value of contact angle varies (decreases) with time of contact withAl2O3 substrate. The reduction in θ of the Al-Mg alloy was proportional to thereduction in surface tension γlv of Al, and to reactions that took place at the Alalloy/Al2O3 interface.

The contact angle measured using the sessile drop method is typically an advancing contact angle, which is often used for the evaluation of wettability. However, the precise measurement of the contact angle on rough substrates has been required for developing various industrial processes. In this study, a new measuring method by achieving the minimum total free energy by ultrasonic vibration (USV) was developed. The new method has been demonstrated for different rough surfaces, droplet volumes, and wettability conditions. The advancing contact angle significantly decreased when the USV is applied, but it immediately increased after stopping the USV. In order to capture the droplet behavior at the beginning and end of the USV, a high-speed camera was used. The contact angle was apparently a receding contact angle after stopping the ultrasonic vibration. Accordingly, the intrinsic contact angle was estimated using the values of the advancing contact angles obtained before applying the ultrasonic vibration and the receding contact angles obtained after stopping the ultrasonic vibration. [ABSTRACT FROM AUTHOR]

Electrochemical machining is applied not only in die and mold fabrication, but also in the finishing process for parts manufacturing. Especially when ECM is used in finishing purposes, surface properties become more important. In this study, the wettability which is one of the surface properties was focused on and discussed. The sessile drop method and the contact angle are used to evaluate the wettability. In order to measure the contact angle based on JIS R 3257, how the contact angle changes within the allowable measurement range that JIS prescribed was experimentally examined. It was found that the contact angle changes temporally and quantitatively within the JIS allowable extent. In order to measure contact angles correctly, the measurement conditions under which the range is stricter than the JIS range was investigated and discussed. After the measurement conditions were decided, contact angles of stainless SUS304 surfaces that machined with ECM were experimentally investigated. In order to clarify the relationship between ECM conditions and the wettability of the machined surface, the change in the contact angle when varying the kind of electrolyte and the current density was examined. It was found that the surfaces machined with ECM using NaNO 3 solution as electrolyte with lower current density has a lower contact angle. When the current density increases, there appears proportional relation between the current density and the contact angle. [ABSTRACT FROM AUTHOR]

Surface Free Energy (SFE) of solids should be calculated using theoretical models. The contact angle (CA) measurement on a surface is considered the most practical way to obtain the SFE. The results of five methods based in the models are compared: the method of Zisman (ZI), the geometric mean (GM), the harmonic mean (HM), the Lifshitz-van der Waals/ Acid-Base (LW/AB) and the equation of state (ES). The SFE calculated with GM, HM and LW/AB methods change with the amount and type of liquid used, however, when water, glycerol and dimethyl sulfoxide are used together the SFE and its dispersive and polar components are similar in value for the three methods. In the case of the ES model the values of SFE change with the liquid used; finally using the ZI method the SFE values are 20% lower than the values of SFE obtained with the other methods. [ABSTRACT FROM AUTHOR]

The sessile drop method is an easy and fast method used to measure the contact angle between solids and liquids. The value of the contact angle is used in surface characterization, in particular the wettability of solid surfaces by the liquid and to calculate the surface free energy. In this work, we study the effects of the volume of the drop placed on the surface, the elapsed time between drop placing and measurement and the cleaning of the substrate (not cleaning, washed with ethanol or washed with acetone) in the value of the contact angle on Ti6Al4 V and AISI 316 stainless steel. We found that drop asymmetry is a very important parameter that must be considered in CA measurements. Anasymmetry parameter used to qualify the drop asymmetry is proposed. It was also found that the degree of cleanliness produces dispersion in the contact angle values; on the other hand no differences were found between cleaning with ethanol or acetone. CA decreases with time and increases slightly with decreasing droplet volume. [ABSTRACT FROM AUTHOR]

The surface tension of molten Sn-Ag alloys was measured using a specially developed high-accuracy sessile drop apparatus. In this apparatus, a molten sample is dropped onto a R-AlO substrate in order to prevent any reaction between the sample and substrate during the heating process. The droplet shape was recorded from two perpendicular directions to confirm its symmetry. The oxygen partial pressure ( $$ {P_{{{\text{O}}_2}}} $$ ) was controlled by a Mg furnace to a value of about 10 to 10 Pa. The sample compositions used were Sn-20Ag, Sn-50Ag, and Sn-80Ag (at.%) and were alloyed from pure Sn (99.999%) and Ag (99.99%) in the dropping tube. The accuracy of the experimental results was confirmed by an extremely small scatter. The measured temperature dependence of the surface tension of the molten Sn-50Ag (at.%) alloy indicated a characteristic curve that changed from positive to negative with increasing temperature. Furthermore, the surface tension of the molten Sn-20Ag (at.%) alloy has a temperature dependence that changes from flat to negative, while the Sn-80Ag (at.%) alloy has a negative temperature dependence across the whole temperature range. Based on a theoretical discussion using Butler's equation, these temperature dependencies can be determined by negative straight lines when assuming the surface composition. [ABSTRACT FROM AUTHOR]

The study involved measurements of surface tension of liquid binary copper-bismuth alloys with respect to their chemical composition and temperature as well as investigations of the liquid alloy - refractory material - gaseous phase system wettability using usual refractory materials, i.e. aluminium oxide, magnesium oxide and graphite. The experiments were performed with the use of sessile drop method and a high-temperature microscope coupled with a camera and a computer was utilised. [ABSTRACT FROM AUTHOR]