Presence Of Residual Moisture Research Articles

A Ceramic/Lithiophilic Metal Dual Protective Layer for Stable Lithium Metal Anodes Fabricated via Transfer-Printing Methods

Lithium metal has attracted researcher’s attention because of its superior theoretical capacity (3860mAh g-1 or 2061 mAh cm-3), which is nearly 10 times higher than commercialized anode materials, for example, graphite (372 mAh g-1). However, lithium metal is not currently used in commercial lithium metal batteries due to safety and efficiency issues that arise during long-term battery operation. The high reactivity of lithium metal causes almost all available electrolytes to be spontaneously reduced on the Li surface to form a solid-electrolyte interface (SEI) layer. Unfortunately, this passivating SEI layer is typically too fragile to withstand significant mechanical deformation of the electrode during cycling, resulting in crack formation. These cracks expose fresh Li underneath, which locally enhances Li-ion flux and promotes morphological deformation of the lithium metal surface. This often leads to dendritic Li deposition that can cause internal short circuits and compromise battery safety. Additionally, repeated failures and repairs of SEIs result in the continued loss of both Li and electrolyte, leading to low coulombic efficiency (CE) and rapid capacity decrease.To mitigate these problems, researchers have attempted to suppress lithium dendrite growth by slurry coating on the lithium metal surface such as ceramic layer and lithiophilic metal. These materials and conventional lithium metal protection coating methods partially inhibit the growth of lithium dendrites; however, they come with several significant drawbacks. The ceramic layer possesses high mechanical properties that physically inhibit the growth of lithium dendrites. However, it exhibits poor interfacial characteristics with lithium metal, leading to increased resistance. This heightened resistance results in the formation of uneven lithium deposition layers at high current densities, causing cracks in the ceramic layer. Lithiophilic metals exhibit an advantage in reducing nucleation resistance through alloying reactions with lithium prior to nucleation, thereby facilitating uniform lithium ion deposition. However, their low mechanical properties limit their potential for enhancing electrochemical performance. Furthermore, the conventional coating method used for lithium metal protection involves the direct application of solvent-containing slurries onto the lithium metal surface using slurry coating techniques. Given the inherent reactivity of lithium metal, the presence of residual moisture and impurities within the solvent may induce sub-reactions, ultimately compromising the stability of lithium metal.In this study, we propose an approach to improve the cycling stability of lithium metal through Ceramic/lithiophilic metal dual protective layer fabricated via transfer-printing methods. The dual lithium metal protection layer, consisting of Ceramic/lithiophilic, involves coating a lithiophilic metal layer between the ceramic layer and the lithium metal. This method aims to maximize electrochemical performance improvement through a synergistic effect that utilizes the high mechanical properties of ceramics and solves the problem of interfacial resistance between the ceramic layer and lithium metal through the lithiophilic metal. Furthermore, we propose a coating process for lithium metal protection layers using a method based on transfer printing. This method involves applying pressure to the lithium metal surface through transfer printing of pre-finished composite protective layers on a film, rather than directly applying slurry onto the lithium metal surface. Transfer printing offers the advantage of maintaining the stability of lithium metal by avoiding direct application of slurry onto the lithium metal surface, thereby ensuring the integrity of the protection layer.

Parametric Analysis of Donor Activation for Glycosylation Reactions.

The chemical synthesis of complex oligosaccharides relies on efficient and highly reproducible glycosylation reactions. The outcome of a glycosylation is contingent upon several environmental factors, such as temperature, acidity, the presence of residual moisture, as well as the steric, electronic, and conformational aspects of the reactants. Each glycosylation proceeds rapidly and with a high yield within a rather narrow temperature range. For better control over glycosylations and to ensure fast and reliable reactions, a systematic analysis of 18 glycosyl donors revealed the effect of reagent concentration, water content, protecting groups, and structure of the glycosyl donors on the activation temperature. With these insights, we parametrize the first step of the glycosylation reaction to be executed reliably and efficiently.

Measurement and Importance of Volatile Matter in Coals and Biofuels

Abstract Volatile matter values for solid fuels are used to assess their burning rates and, thus, provide a basis for the buying and selling of these fuels. The major factors that affect volatile matter yields are the type of fuel, moisture contents, and the heating rates used in the tests. This paper reports the results of experiments designed to improve the reliability and application of test methods for the determination of volatile matter in various solid fuels. The macro thermogravimetric analysis studies described herein include the rapid drying of analysis samples of coal and the effect on volatile matter yields, the heating of various chars at high temperatures to reach a state of constancy, the measuring of decomposition moisture, an “elusive” constituent in coal, and the cocombustion of coals and other solid fuels. The presence of residual moisture and decomposition moisture in the coal during the volatile matter tests increases the measured volatile matter yields even though the residual moisture has been factored out. The rates of heating solid fuels during volatile matter tests affect the volatile matter yields because of the presence of different types of moisture in the fuel that are released at different temperatures. The heating rates used in volatile matter tests affect the type of compounds released and the total volatile matter yields of coals and biofuels. The experiments reported in this paper were instrumental in the decision of ASTM Committee D05 on Coal and Coke to recently revise the classic volatile matter standard test method D3175 to change the temperature for drying sparking coals from 600°C to 107°C. The role volatile matter plays in the combustion of fuel blends is discussed in this article.

Thermal-Vacuum Method for Obtaining Nanodispersed Zirconium Dioxide

An energy-efficient thermal-vacuum method for continuous production of nanodispersed powder of amorphous zirconium dioxide from zirconium hydroxide has been developed. This approach is based on a principle of creating an aerodynamic flow with an initial powder-like material in the cavity of the heating element of a thermal-vacuum installation. In this way, short-term contacts of particles of zirconium hydroxide with the inner surface of the heating element made in the form of the winding helical are created. As a result, the crushing of the particles is carried out due to the high thermal stresses in the particles contacted. This process is aggravated by the presence of residual moisture in the original powdery material. Transformations of the zirconium hydroxide in the process of thermal-vacuum treatment have been investigated. Amorphous dioxide has been obtained. The study of structural composition of the material in the initial state and processed in a thermal-vacuum installation was carried out using X-ray analysis and scanning microscopy. Experimental data on the structural-phase composition of the original material and data on the closest structural prototypes of crystalline-impurity compounds are presented. They are also given data on the volume of crystal cells and estimates of the molar concentration of the components. A mass spectrometric assessment of the elemental composition of the obtained zirconium dioxide is given. Thermal-vacuum method allows toobtain highly dispersed zirconium dioxide in its amorphous state directly from zirconium hydroxide without using liquid media and, moreover, in a short time – within 15...20 s.

Mono- and dinuclear CuII complexes of the benzyldipicolylamine (BDPA) ligand: crystal structure, synthesis and characterization.

The crystal structures of mono- and dinuclear CuII trifluoromethanesulfonate (triflate) complexes with benzyldipicolylamine (BDPA) are described. From equimolar amounts of Cu(triflate)2 and BDPA, a water-bound CuII mononuclear complex, aqua(benzyldipicolylamine-κ3N,N',N'')bis(trifluoromethanesulfonato-κO)copper(II) tetrahydrofuran monosolvate, [Cu(CF3SO3)2(C19H19N3)(H2O)]·C4H8O, (I), and a triflate-bridged CuII dinuclear complex, bis(μ-trifluoromethanesulfonato-κ2O:O')bis[(benzyldipicolylamine-κ3N,N',N'')(trifluoromethanesulfonato-κO)copper(II)], [Cu2(CF3SO3)4(C19H19N3)2], were synthesized. The presence of residual moisture in the reaction medium afforded water-bound complex (I), whereas dinuclear complex (II) was synthesized from an anhydrous reaction medium. Single-crystal X-ray structure analysis reveals that the CuII centres adopt slightly distorted octahedral geometries in both complexes. The metal-bound water molecule in (I) is involved in intermolecular O-H...O hydrogen bonds with triflate ligands and tetrahydrofuran solvent molecules. In (II), weak intermolecular C-H...F(triflate) and C-H...O(triflate) hydrogen bonds stabilize the crystal lattice. Complexes (I) and (II) were also characterized fully using FT-IR and UV-Vis spectroscopy, cyclic voltammetry and elemental analysis.

In‐situgrown silica/water‐borne epoxy shape memory composite foams prepared without blowing agent addition

ABSTRACTShape memory (SM) silica/epoxy composite foams were successfully synthesized via latex technology and prepared without blowing agent addition. Silica was synthesized via tetraethoxysilane (TEOS) hydrolysis. Silica/epoxy foams were obtained from the TEOS solution and water‐borne epoxy mixtures after freeze‐drying and foaming in the presence of residual moisture as the blowing agent under a vacuum at 110°C. The morphologies of the resulting foams were evaluated using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Compression and thermo‐mechanical cycle tests were performed to measure the mechanical and SM properties of the foams. Experimental results indicated that the micrographs and mechanical properties of the foams were closely related to freeze‐drying time. The final composite foams exhibited high shape recovery and fixity ratios and could maintain both properties at more than 90% even after five thermo‐mechanical cycles. The properties obtained in the epoxy foams may offer new opportunities for their use in future structural applications. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci.2015,132, 42599.

Comparative Study on Recovered Binder Properties Using Three Asphalt Emulsion Recovery Methods

Abstract Determining the properties of residual binders is important to the effective use of asphalt emulsion chip seals. Yet, the effect of laboratory methods on recovered binder properties used to simulate residual binders in the field is not well understood. In this research, the residues of five asphalt emulsions were compared after recovery by three methods, a Hot Oven procedure (similar to ASTM D244-04), a Stirred-Can procedure (as reported in TXDOT 0-1710), and a Warm Oven method (ASTM D7497-09). The recovered binders were tested with size exclusion chromatography (SEC) to assess the presence of residual moisture. Properties of the original base binders and the corresponding recovered binders were compared using dynamic shear rheometry and Fourier transform infrared spectrometry. The SEC results showed no residual water in any of the recovered samples, except the samples from Warm Oven recovery, which showed a small detectable amount of residual moisture. The results from statistical analysis of binder properties using ANOVA plus Tukey’s Honestly Significant Difference test suggest that recovered binders from the Warm Oven method are statistically different from their base binders. Nevertheless, considering each of the residues recovered from the three methods in paired comparisons with the other residues, none is statistically different from the others.

Structural inhomogeneity in cotton cellulose upon its interaction with water

Comparative analysis of the characteristics of supramolecular structures of dry and swollen cotton fibers makes it possible to differentiate structural regions accessible to water. The revealed features of water desorption from cotton cellulose (exceptionally low rates at the final stages, presence of residual moisture) are related to the removal of water, which is localized in the regions of the crystalline phase disorganized upon drying. The fact of incomplete moisture removal from cotton fibers at < 325 K is interpreted from the stand-point of the frozen molecular mobility in the microsurroundings of sorption sites, which are located at the defects of crystallites, at the final stage of the desorption process. A marked contribution from the recrystallization of disorganized regions in the surface layer of crystallites to the thermal effect of the interaction between water and cotton cellulose at low water content is established.

Argonne Coal Structure Rearrangement Caused by Sorption of CO2

The exposure of powdered unconfined coals to CO{sub 2} results in changes in the coals' physical structures. The presence of water changes the behavior of the coals on exposure to CO{sub 2}. The sorption of CO{sub 2} on seven Argonne premium coals was measured by using attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy as a function of time at constant CO{sub 2} pressure ({approximately} 0.62 MPa) and temperature (55{sup o}C). The depth sampled is at least 1 m, and this ensures that both the bulk and surface of the sample were interrogated. Concentrations of CO{sub 2} in the top 1-7 {mu}m of the coal were measured by using the peak area of the CO{sub 2} ATR-FTIR band near 2333 cm{sup -1}. Diffusion rates were measured by using the time dependence of the area of the 2333 cm{sup -1} band. Surface adsorption is effectively instantaneous. The coals were either extensively or briefly dried. The coals were exposed to CO{sub 2}, evacuated, and then exposed to CO{sub 2} a second time. For the extensively dried coals, removal of the CO{sub 2} under vacuum was much faster than CO{sub 2} sorption, indicating a coal structure change caused by CO{sub 2} sorption. The diffusionmore » rate of the CO{sub 2} into the coal was much faster for the second exposure, confirming that the coal underwent a physical structure rearrangement. Structure rearrangement was observed for all seven extensively dried coals and for the Pittsburgh No. 8 briefly dried coal. The presence of residual moisture in the briefly dried coal samples appeared to inhibit or block CO{sub 2} uptake as equilibrium was reached within minutes. The second exposure of the briefly dried coals universally resulted in greater CO{sub 2} uptake that was again instantaneous on our experimental time scale. 52 refs., 6 figs., 2 tabs.« less

Moisture-uptake by the positive active material from the casting solvent and the ambient environment

It is widely recognized that the presence of residual moisture has significant detrimental effects on the performance of lithium ion batteries. Studies have shown that the positive active material can be a major source of moisture contributors to the overall cell moisture. The aim of the present study is to understand the factors affecting moisture uptake by the doped-lithium nickel cobalt oxide material from the casting solvent, acetone, and the ambient environment. As-is and the air-dried powders under various conditions (300 °C for 24 h, 500 °C for 8 h, and 500 °C for 24 h) were exposed to ambient and humid air for various lengths of time. Similarly, all these powders were exposed to extra dry (47 ppm) and wet (5789 ppm) acetone. Karl Fisher measurements at 160 °C and 290 °C show that humidity levels (80–85% relative humidity versus 20–25%) and the exposure times are the critical factors. Acetone wetness and the length of exposure in it do not contribute significantly to the moisture uptake by the active material. Cathode powder drying helps in minimizing the amount of moisture uptake from the environment.

Near infrared reflectance spectroscopy (NIRS) to predict biological parameters of maize silage: effects of particle comminution, oven drying temperature and the presence of residual moisture

Maize silage nutritive quality is routinely determined by near infrared reflectance spectroscopy (NIRS). However, little is known about the impact of sample preparation on the accuracy of the calibration to predict biological traits. A sample population of 48 maize silages representing a wide range of physiological maturities was used in a study to determine the impact of different sample preparation procedures (i.e., drying regimes; the presence or absence of residual moisture; the degree of particle comminution) on resultant NIR prediction statistics. All silages were scanned using a total of 12 combinations of sample pre-treatments. Each sample preparation combination was subjected to three multivariate regression techniques to give a total of 36 predictions per biological trait. Increased sample preparations procedure, relative to scanning the unprocessed whole plant (WP) material, always resulted in a numerical minimisation of model statistics. However, the ability of each of the treatments to significantly minimise the model statistics differed. Particle comminution was the most important factor, oven-drying regime was intermediate, and residual moisture presence was the least important. Models to predict various biological parameters of maize silage will be improved if material is subjected to a high degree of particle comminution (i.e., having been passed through a 1 mm screen) and developed on plant material previously dried at 60 °C. The extra effort in terms of time and cost required to remove sample residual moisture cannot be justified.

Adsorption of hydrocarbons by ZSM-5 zeolites with different SiO 2/Al 2O 3 ratios: a combined FTIR and gravimetric study

In metal-free ZSM-5, the decrease in the concentration of Bronsted and Lewis acid sites parallels the increase in the SiO 2/Al 2O 3 ratio. In the presence of residual moisture, the adsorption of small alkanes does not markedly depend on the SiO 2/Al 2O 3 ratio in the range from 30 to 150. The acidity is more important for the adsorption of alkenes (propene) which oligomerize following adsorption. The addition of 5 wt.% of La does not significantly affect the strength of the surface acid sites but does decrease their concentration. It causes a transformation, in a part, of the Bronsted acid sites. These new centers could perhaps be assigned to LaO(OH) or La(OH) 2 + species which may be formed on the surface in La-containing ZSM-5. La could exchange only the strongest acidic sites without inducing large changes in their total concentration. La addition has a very small effect on the adsorption of small hydrocarbons. The exchange of the protons by Cu 2+ decreases the concentration of Bronsted acid sites. At a sufficient loading of the ZSM-5 by Cu 2+, i.e. at an atomic ratio Cu/Al > 1.0, the exchange can almost totally suppress the Bronsted acidity. Another effect of the ion exchange is the suppression of the adsorption capacity of small hydrocarbons due to lowered surface area and internal pore volume. The lowered available internal pore volume also limits the extent of the oligomerization of propene.