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Stones are traditionally used in construction and architectural applications as building elements due to their aesthetic and technical/structural performance. Like other environmental factors (rain, humidity, moisture, salt presence, biological activity, etc.), heating–cooling and freeze–thaw cycles significantly threaten the longevity of stone materials. Hence, considering the socio-economic and cultural value of stones, preventive actions such as hydrophobic coatings are applied to prevent or mitigate damage. The scope of this study is the performance assessment of limestones with different characteristics and the efficiency of various commercial silane/siloxane-based hydrophobic coatings when exposed to thermal variation and freeze–thaw. For that purpose, the standards EN 14066:2013 (determination of resistance to aging by thermal shock) and EN 12371:2010 (determination of frost resistance) were followed. Open porosity and static contact angles were estimated to assess the stone durability and water protection capabilities of the hydrophobics. Additionally, sound speed propagation velocity, quality of building material index, elastic modulus and flexural strength were measured to evaluate the variation of mechanical properties. Static contact angle revealed that the coatings maintained an efficient level of hydrophobicity even after thermal-shock and freeze–thaw weathering tests. The study also revealed a critical interaction between freeze–thaw cycles, hydrophobic coatings and structural integrity of the stones, mostly on more porous ones. When they are subjected to harsh environmental conditions, untreated porous limestones keep structural cohesion, allowing for the natural absorption and release of water during freezing and thawing. On the contrary, when limestones are treated, the hydrophobic coatings can moderately obstruct the water release due to the partial saturation of the porous framework by the products. It also probably resulted from the different mechanical behavior between the inner matrix and layer of stone coated, resulting in a premature breakout and mechanical damage of the stone.
The use of selected organosilicon compounds for the preparation of silicon based ceramic materials is discussed in terms of processing microstructure-property relationships. The mechanisms operative in the formation of gel derived silicate glasses and glass ceramics are reasonably well understood, but this is not true for silicon carbide/nitride based ceramics. The properties of organosilicon precursors and the mechanism of pyrolysis affect the microstructural features of the ceramic. Reaction mechanisms are proposed and the microstructural features and properties of organosilazane derived ceramics discussed.
Addition polyimide oligomers have been synthesized from bis(gamma-aminopropyl) tetramethyldisiloxane and 3, 3', 4, 4'-benzophenonetetracarboxylic dianhydride using a variety of latent crosslinking groups as endcappers. The prepolymers were isolated and characterized for solubility (in amide, chlorinated and ether solvents), melt flow and cure properties. The most promising systems, maleimide and acetylene terminated prepolymers, were selected for detailed study. Graphite cloth reinforced composites were prepared and properties compared with those of graphite/Kerimid 601, a commercially available bismaleimide. Mixtures of the maleimide terminated system with Kerimid 601, in varying proportions, were also studied.
Acetylene terminated polyimide oligomers having a range of molecular weights have been synthesized by reacting bis (gamma-aminopropyl) tetramethyldisiloxane, aminophenylacetylene and 3, 3', 4, 4' benzophenonetetracarboxylic dianhydride in different molar ratios. The prepolymers were isolated and characterized for melt flow and cure properties. They show promise as adhesives for bonding titanium to titanium and as matrix resins for graphite cloth reinforced composites. The most promising system has been blended in varying proportions with Thermid 600, a commercially available acetylene terminated polyimide oligomer, and the mixtures have been tested for application as composite matrix resins.
Laminates show increased impact resistances and other desirable mechanical properties. Bismaleamic acid extended by reaction of diaminosiloxane with maleic anhydride in 1:1 molar ratio, followed by reaction with half this molar ratio of aromatic dianhydride. Bismaleamic acid also extended by reaction of diaminosiloxane with maleic anhydride in 1:2 molar ratio, followed by reaction with half this molar ratio of aromatic diamine (Michael-addition reaction). Impact resistances improved over those of unmodified bismaleimide, showing significant increase in toughness. Aromatic addition polyimides developed as both matrix and adhesive resins for applications on future aircraft and spacecraft.
Dimethylsilanediol (DMSD) has been identified as a problematic organic contaminant aboard the ISS. This contaminant was initially identified in humidity condensate and in the Water Processor Assembly (WPA) product water in 2010 when routine water quality monitoring an increasing total organic carbon (TOC) trend in the WPA product water. Although DMSD is not a crew health hazard at the levels observed in the product water, it can degrade the WPA catalytic reactor's effectiveness and cause early replacement of Multifiltration Beds. DMSD may also degrade the performance of the Oxygen Generation System (OGS) which uses the WPA product water for electrolysis. An investigation into the source of DMSD has determined that polydimethylsiloxane (PDMS) compounds are likely hydrolyzing in the Condensing Heat Exchangers (CHX) to form DMSD. PDMS compounds are prevalent aboard ISS from a variety of sources, including crew hygiene products, adhesives, caulks, lubricants, and various nonmetallic materials. PDMS compounds are also known to contribute to CHX hydrophilic coating degradation by rendering it hydrophobic and therefore adversely affecting its ability to effectively transmit water to the condensate bus. Eventually this loss in performance results in water droplets in the air flow exiting the CHX, which may lead to microbial growth in the air ducts and may impact the performance of downstream systems. Several options have been evaluated to address these concerns. Modifications to the Water Processor Multifiltration Beds and Catalytic Reactor for removal of DMSD were not considered viable, and did not address the issue with PDMS compound degradation of the CHX coating. Design concepts are now in development for removing PDMS compounds from the air stream before they can reach the CHX coating, thus preventing coating degradation and hydrolysis of the PDMS compounds to DMSD. This paper summarizes the current status of the effort to treat these contaminants on ISS.
Dimethylsilanediol (DMSD) has been identified as a problematic chemical contaminant aboard ISS. This contaminant was initially identified in the ISS condensate and in the Water Processor Assembly (WPA) product water in 2010 when an increasing total organic carbon (TOC) trend was detected in the water produced by the WPA. DMSD is not a crew health hazard at the levels observed in the product water, but it may degrade the performance of the Oxygen Generation System (OGS) which uses product produced by the WPA for electrolysis. In addition, DMSD can prevent the effective operation of the WPA catalytic reactor, and necessitates early replacement of Multifiltration Beds in the WPA. An investigation into the source of DMSD has determined that polydimethylsiloxanes (PDMSs) are hydrolyzing in the Condensing Heat Exchanger (CHX) to form DMSD. PDMSs are prevalent aboard ISS from a variety of sources, including crew hygiene products, adhesives, caulks, lubricants, and various nonmetallics. TPDMSs are also implicated in CHX hydrophilic coating degradation, rendering it hydrophobic and adversely affecting its ability to effectively transmit water to the condensate bus. Eventually this loss in performance results in water droplets in the air flow out of the CHX core, which can lead to microbial growth in the air ducts and can impact the performance of downstream systems. Design concepts have now been developed for removing PDMS in the air stream before it can reach the CHX core, thus preventing degradation of the coating and decomposition of the PDMS to DMSD. This paper summarizes the current status of the effort to deliver filters to ISS for removing PDMSs from the atmosphere before they can adversely impact the performance of the CHX coating and the WPA.
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Ultra-high temperature, light-weight, ceramic insulation such as ceramic tile is obtained by pyrolyzing a siloxane gel derived from the reaction of at least one organo dialkoxy silane and at least one tetralkoxy silane in an acid or base liquid medium. The reaction mixture of the tetra- and dialkoxy silanes may contain also an effective amount of a mono- or trialkoxy silane to obtain the siloxane gel. The siloxane gel is dried at ambient pressures to form a siloxane ceramic precursor without significant shrinkage. The siloxane ceramic precursor is subsequently pyrolyzed, in an inert atmosphere, to form the black ceramic insulation comprising atoms of silicon, carbon and oxygen. The ceramic insulation, can be characterized as a porous, uniform ceramic tile resistant to oxidation at temperatures ranging as high as 1700.degree. C. and is particularly useful as lightweight tiles for spacecraft and other high-temperature insulation applications.
Ultra-high temperature, light-weight, black ceramic insulation having a density ranging from about 0.12 g/cc. to 0.6 g/cc. such as ceramic tile is obtained by pyrolyzing siloxane gels derived from the reaction of at least one organo dialkoxy silane and at least one tetralkoxy silane in an acid or base liquid medium. The reaction mixture of the tetra- and dialkoxy silanes also may contain an effective amount of a mono- or trialkoxy silane to obtain the siloxane gels. The siloxane gels are dried at ambient temperatures and pressures to form siloxane ceramic precursors without significant shrinkage. The siloxane ceramic precursors are subsequently pyrolyzed, in an inert atmosphere, to form the black ceramic insulation comprising atoms of silicon, carbon and oxygen. The ceramic insulation can be characterized as a porous, uniform ceramic tile resistant to oxidation at temperatures ranging as high as 1700.degree. C., and particularly useful as lightweight tiles for spacecraft and other high-temperature insulation applications.
Capturing carbon dioxide (CO2) from post-combustion gas streams is an energy-intensive process that is required prior to either converting or sequestering CO2. There are a few commercial offerings of 1st and 2nd generation aqueous amine technologies, however the cost of capturing CO2 with these technologies remains high. To decrease costs of capture, researchers are designing efficient solvent systems with the goal of being drop-in replacements for 1st and 2nd generation infrastructure. One approach has seen the development of water-lean solvents that aim to increase efficiency by reducing the water content in solution. Water-lean solvents such as GE’s GAP/TEG are promising technologies, with potential to halve the parasitic load to a coal-fired power plant, only if the intrinsically high solution viscosities and hydrolysis of the siloxane moieties could be mitigated. We present here, an integrated multidisciplinary approach to overhaul the GAP/TEG solvent system at the molecular level to mitigate hydrolysis while also reducing viscosity. We present molecular-level insights into chemical speciation of CO2-containing ions, showing that co-solvents and diluents have a negligible effect on reducing viscosity and are not needed. This finding allowed for the design of singlecomponent siloxane-free diamine derivatives with site-specific incorporation of selective chemical moieties for direct placement and orientation of hydrogen bonding to reduce viscosity. Ultimately, we present new single-component diamine formulations less susceptible to hydrolysis that exhibit up to a 98% reduction in viscosity compared to the initial GAP/TEG formulation.
A method is reported to prepare siloxane microballoons that can be loaded into a direct ink write siloxane ink for 3D printing. The resulting structure is subjected to a solvent removal and supercritical drying process to provide a final printed siloxane having both macroscopic and microscopic porosity. Core-shell particles are generated by an emulsion template and phase separation process. Intra-strand closed-cell porosities can be achieved between 10 and 40 vol% thus facilitating additional compressive strain before lockup. Here short term compression set testing highlights the excellent shape retention properties of these elastomers, which have less than 8% relative compression set under load.
Silica-supported ZnO efficiently catalyzes the nonoxidative dehydrogenation of ethanol to acetaldehyde, which is relevant for production of 1,3-butadiene from bioethanol. Characterization with in situ spectroscopies under dehydrated conditions (high sensitivity-low energy ion scattering (HS-LEIS), diffuse reflectance (DR) UV–vis, X-ray absorption spectroscopy (XAS), diffuse reflectance Fourier transform infrared spectroscopy (DRIFTS), inelastic neutron scattering (INS), and UV Raman), and ammonia adsorption probed by temperature-programmed desorption followed by DRIFTS and mass spectrometry (DRIFTS-MS NH 3 -TPD), and DFT calculations revealed that the supported ZnO x phase was present as isolated surface ZnO x sites on SiO 2 , with the vast majority coordinated by two siloxane bonds and one silicon atom with two nonbridging oxygens ((≡SiO) 2 Zn 2+ O 2 Si=), anchored at 4-, 5-, and 6-membered siloxane rings. A minor fraction of surface ZnO x sites possessed Lewis acidity, and even fewer sites possessed a Bro̷nsted acidic Zn(OH) + Si moiety. Ethanol temperature-programmed surface reaction-mass spectrometry (TPSR-MS) with various oxidative or ethanol reaction pretreatments indicated that only sites with Lewis and Bro̷nsted acidic character (Zn(OH) + Si) were active for ethanol dehydrogenation, while the majority surface (≡SiO) 2 Zn 2+ O 2 Si= sites were inactive. Greater heterogeneity among all surface ZnO x sites, as assessed by in situ DR UV–vis spectroscopy, was associated with a greater number of ZnO x sites that were active for ethanol dehydrogenation as well as lower enthalpic barriers for acetaldehyde production among the most active surface ZnO x sites. Turnover frequencies and the apparent activation energy for ethanol dehydrogenation were determined from steady-state kinetics. Together, these findings suggested that anchoring inactive surface (≡SiO) 2 Zn 2+ O 2 Si= sites on the silica support caused a greater number of active surface ZnO x sites to adopt a more strained configuration, promoting ethanol dehydrogenation catalysis. Pretreatments and catalysts that promoted desorption of ethanol during TPSR, taken as a marker of surface dehydroxylation, were associated with an increased number of the most active surface (Zn(OH) + Si) sites. Such findings suggested that inactive surface ZnO x sites were activated for ethanol dehydrogenation by dehydroxylation of the support and/or decreased coordination to hemilabile siloxane ligands.
Siloxane-based working fluids for advanced space radiators requiring direct fluid exposure to the space environment are evaluated. Isolation of five candidate fluids by vacuum distillation from existing siloxane polymers is discussed. The five fluids recovered include a polydimethylsiloxane, three phenyl-containing siloxanes, and a methylhexylsiloxane. Vapor pressures and viscosities for the five fluids are reported over the temperature range of 250 to 400 K. Use of thermal-gravimetric analysis to reliably estimate vapor pressures of 10 to the -8 power Pascals is described. Polydimethylsiloxane (PDMS) and polymethylphenylsiloxane (PMPS) are selected from the five candidate fluids based on favorable vapor pressure and viscosity, as well as perceived stability in low-Earth orbit environments. Characterization of these fluids by infrared spectroscopy, Si-29 NMR, gel-permeation chromatography, and liquid chromatography is presented. Both fluids consist of narrow molecular weight distributions, with average molecular weights of about 2500 for PDMS and 1300 for PMPS.