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SiH8(CI)4 is Protactinium-like structured and crystallizes in the orthorhombic P2_12_12_1 space group. The structure is zero-dimensional and consists of eight tetrakis(iodomethyl)silane molecules.
N2SiF4 is Cyanogen Chloride-derived structured and crystallizes in the orthorhombic Immm space group. The structure is zero-dimensional and consists of twelve ammonia molecules and six silane, tetrafluoro- molecules.
SiH8(CBr)4 is Silicon tetrafluoride-derived structured and crystallizes in the tetragonal P-42_1c space group. The structure is zero-dimensional and consists of two tetrakis(bromomethyl)silane molecules. Si4+ is bonded in a tetrahedral geometry to four equivalent C2- atoms. All Si–C bond lengths are 1.89 Å. C2- is bonded to one Si4+, two H1+, and one Br1- atom to form distorted corner-sharing CSiH2Br tetrahedra. There is one shorter (1.09 Å) and one longer (1.10 Å) C–H bond length. The C–Br bond length is 1.97 Å. There are two inequivalent H1+ sites. In the first H1+ site, H1+ is bonded in a single-bond geometry to one C2- atom. In the second H1+ site, H1+ is bonded in a single-bond geometry to one C2- atom. Br1- is bonded in a single-bond geometry to one C2- atom.
This report summarizes the current actives in FY21 related to the effort by Sandia National Laboratories to identify and test coating materials for the prevention, mitigation, and repair of spent nuclear fuel dry storage canisters against potential chloride-induced stress corrosion cracking. This work follows up on the details provided in Sandia National Laboratories FY20 report on the same topic, which provided a detailed description of the specific coating properties desired for application and implementation on spent nuclear fuel canisters, as well as provided detail into several different coatings and their applicability to coat spent nuclear fuel canisters. In FY21, Sandia National Laboratories has engaged with private industry to create a Memorandum of Understanding and established a collaborative R&D program building off the analytical and laboratory capabilities at Sandia National Laboratories and the material design and synthesis capabilities of private industry. The resulting Memorandum of Understanding included four companies to date (Oxford Performance Materials, White Horse R&D, Luna Innovations, and Flora Coating) proposing six different coating technologies (polyetherketoneketone, modified polyimide/polyurea, modified phenolic resin, silane-based polyurethane hybrid with and without a Znrich primer, and a quasi-ceramic sol-gel polyurethane hybrid) to be tested, evaluated, and optimized for their potential use for this application. This report provides a detailed description of each of the coating systems proposed by the participating industry partners. It also provides a description of the planned experimental actives to be performed by Sandia National Laboratories including physical tests, electrochemical tests, and characterization methods. These analyses will be used to identify specific ways to further improve coating technologies toward their application and implementation on spent nuclear fuel canisters. In FY21, Sandia National Laboratories began baseline testing of the base metal material in according with activities of the Memorandum of Understanding. In FY22, Sandia National Laboratories will receive coated coupons from each of the participating industry partners and begin characterization, physical, and electrochemical testing following the test plan described herein.
This report summarizes the activities performed by Sandia National Laboratories in FY22 to identify and test coating materials for the prevention, mitigation, and/or repair of potential chloride-induced stress corrosion cracking in spent nuclear fuel dry storage canisters. This work continues efforts by Sandia National Laboratories that are summarized in previous reports in FY20 and FY21 on the same topic. The previous work detailed the specific coating properties desired for application and implementation to spent nuclear fuel canisters (FY20) and identified several potential coatings for evaluation (FY21). In FY22, Sandia National Laboratories, in collaboration with four industry partners through a Memorandum of Understanding, started evaluating the physical, mechanical, and corrosion-resistance properties of 6 different coating systems (11 total coating variants) to develop a baseline understanding of the viability of each coating type for use to prevent, mitigate, and/or repair potential stress corrosion on cracking on spent nuclear fuel canisters. This collaborative R&D program leverages the analytical and laboratory capabilities at Sandia National Laboratories and the material design and synthesis capabilities of the industry collaborators. The coating systems include organic (polyetherketoneketone, modified polyimide/polyurea, modified phenolic resin), organic/inorganic ceramic hybrids (silane-based polyurethane hybrid and a quasi-ceramic sol-gel polyurethane hybrid), and hybrid systems in conjuncture with a Zn-rich primer. These coatings were applied to stainless steel coupons (the same coupons were supplied to all vendors by SNL for direct comparison) and have undergone several physical, mechanical, and electrochemical tests. The results and implications of these tests are summarized in this report. These analyses will be used to identify the most effective coatings for potential use on spent nuclear fuel dry storage canisters, and also to identify specific needs for further optimization of coating technologies for their application on spent nuclear fuel canisters. In FY22, Sandia National Laboratories performed baseline testing and atmospheric exposure tests of the coating samples supplied by the vendors in accordance with the scope of work defined in the Memorandum of Understanding. In FY23, Sandia National Laboratories will continue evaluating coating performance with a focus on thermal and radiolytic stability.
This report summarizes the activities performed by Sandia National Laboratories in FY23 to identify and test coating materials for the prevention, mitigation, and/or repair of potential chloride-induced stress corrosion cracking in spent nuclear fuel dry storage canisters. This work continues efforts by Sandia National Laboratories that are summarized in previous reports from FY20 through FY22 on the same topic. In FY23, Sandia National Laboratories, in collaboration with five industry partners through a memorandum of understanding, evaluated the physical, mechanical, and corrosion-resistance properties of eight different coating systems. The evaluation included thermal and radiation environments relevant to various time periods of storage for spent nuclear fuel canisters. The coating systems include polymeric (polyetherketoneketone, modified polyimide/polyurea, modified phenolic resin, epoxy), organic/inorganic ceramic hybrids (silane-based polyurethane hybrid and a quasi-ceramic sol-gel polyurethane hybrid), and coatings utilizing a Zn-rich primer applied to stainless steel coupons. The results and implications of these tests are summarized in this report. These analyses will be used to identify the most effective coatings for potential use on spent nuclear fuel dry storage canisters and to identify specific needs for further optimization of coating technologies for application on spent nuclear fuel canisters.
Direct air capture (DAC) has received significant attention this decade as a viable solution to limit global warming, although large-scale deployment is currently not economically feasible. To reach the ambitious cost target set by the U.S. of $100/ton CO2 captured and stored, significant improvements must be made to sorbent lifetime and capacity. Aminosilanes grafted onto silica supports are promising candidates for deployment in DAC systems due to their relatively high oxidative stability and low regeneration temperature. Despite myriad advancements in the field, there still exists a fundamental knowledge gap relating sorbent structure to performance. In this work, we grafted various aminosilanes onto the highly porous silica SBA-15 and characterized both oxidative stability and CO2 capacity. Material properties systematically investigated included amine moiety (primary vs. secondary), silane group structure, number of linkages to the silica support, and co-addition of impregnated amines (e.g., PEI), among others. A fixed bed system was used to execute accelerated degradation studies in the presence of humidity and varying temperatures to simulate realistic operating conditions. Atomistic simulations were combined with the experimental results to gain mechanistic insight, ultimately informing the design of next-generation materials
Each year, roughly 8 million tons of glass are landfilled in the United States. Vitriform3D, in collaboration with Oak Ridge National Laboratory through the Innovation Crossroads program, is developing an additive manufacturing approach to transform post-consumer glass into engineered stone building materials. A custom UV-curable binder jetting system was commissioned to enable recycled glass printing without energy-intensive oven curing. While this printer is still under development, the team pursued a parallel research track using ORNL equipment and a polyethyleneimine (PEI) binder. Printed parts were thermally post-cured and infiltrated with epoxy, with the resulting material exceeding fiber cement board performance. Silane treatment of the glass particles further improved glass–epoxy adhesion, yielding an additional 24% strength gain over the epoxy-glass composite, achieving nearly 3x the fiber cement benchmark. Ongoing research is focused on reducing epoxy content to improve cost and recycled content while retaining mechanical performance. This work demonstrates a scalable, low-carbon pathway to convert glass waste into high-value, locally produced construction materials.
Cage topology controlled at the nanometer length scale is expected to enable original functionalities, e.g., in catalysis and therapeutics. Cages are fundamental structural motifs of clathrates and their topological duals, Frank-Kasper phases, and are constituents of mesoporous silica frameworks. However, with one exception, they have not been synthesized as discrete particles. By varying reactant ratios of surfactant, oil, and silane, we report the discovery of 5(12)6(2) and 5(12)6(8) amorphous silica polyhedra, each coexisting with the previously identified 5(12) cage, using combined cryo-transmission electron microscopy (cryo-TEM) and single-particle reconstruction (SPR). Notably, the 5(12)6(8) polyhedron represents a topology not previously observed in mesoporous silica frameworks. Control over structural features is demonstrated, and insights into cage formation mechanisms are provided. Structural outcomes are summarized in a ternary morphology diagram alongside prior results, bridging serendipitous discovery and intentional design of silica cages displaying a level of control over silica polymerization rivaling nature.
Structural composites with metal inserts are gaining increasing interest enabling light weight design for energy efficiency, provide insulation, corrosion protection without compromising mechanical integrity. Such over molded metal-polymer composites show strong potential in many automotive and aerospace component parts, e.g. car bumper, chassis, door, brackets, fasteners, etc. Despite several advantages, metal-polymer dissimilar interface remains a weak spot in structural design, requiring further investigation to improve interfacial interlocking. The current work focuses on enhancing the metal-polymer adhesion between stainless steel inserts and polymer matrices (e.g. acrylonitrile butadiene styrene resin (ABS), and polyamide 66 (PA66) through surface treatment via chemical etching and mechanical roughening. In the chemical etching process, metal substrates were treated with aqua regia solution for different time intervals to evaluate surface roughness measured by water contact angle and morphology analysis. For mechanical roughening approach, metal inserts were subjected to blasting for surface abrasion. Treated samples were also functionalized with aminosilane coupling agent which showed successful grafting on the surface measured by water contact angle. Metal inserts with micro level surface roughness through etching exhibited significant 21% improvement in adhesion strength compared to untreated inserts; however, the effect of silane treatment on the interfacial strength was found to be highly matrix dependent.
Simultaneous fouling and pore wetting of the membrane during membrane distillation (MD) is a major concern. In this work, an electrospun bilayer membrane for enhancing fouling and wetting resistance has been developed for treating hydraulic fracture-produced water (PW) by MD. These PWs can contain over 200,000 ppm total dissolved solids, organic compounds and surfactants. The membrane consists of an omniphobic surface that faces the permeate stream and a hydrophilic surface that faces the feed stream. The omniphobic surface was decorated by growing nanoparticles, followed by silanization to lower the surface energy. An epoxied zwitterionic polymer was grafted onto the membrane surface that faces the feed stream to form a tight antifouling hydration layer. The membrane was challenged with an aqueous NaCl solution containing sodium dodecyl sulfate (SDS), an ampholyte and crude oil. In the presence of SDS and crude oil, the membrane was stable and displayed salt rejection (>99.9%). Further, the decrease was much less than the base polyvinylidene difluoride (PVDF) electrospun membrane. The membranes were also challenged with actual PW. Our results highlight the importance of tuning the properties of the membrane surface that faces the feed and permeate streams in order to maximize membrane stability, flux and salt rejection.
Primarily used as an encapsulant and soft adhesive, Sylgard 184 is an engineered, high-performance silicone polymer that has applications spanning microfluidics, microelectromechanical systems, mechanobiology, and protecting electronic and non-electronic devices and equipment. Despite its ubiquity, there are improvements to be considered, namely, decreasing its gel point at room temperature, understanding volatile gas products upon aging, and determining how material properties change over its lifespan. In this work, these aspects were investigated by incorporating well-defined compounds (the Ashby–Karstedt catalyst and tetrakis (dimethylsiloxy) silane) into Sylgard 184 to make modified formulations. As a result of these additions, the curing time at room temperature was accelerated, which allowed for Sylgard 184 to be useful within a much shorter time frame. Additionally, long-term thermal accelerated aging was performed on Sylgard 184 and its modifications in order to create predictive lifetime models for its volatile gas generation and material properties.
Glass encapsulation for semiconductor elements deposited by reaction of silane with oxygen
New process gives good yields of anilinosilane compounds that can be readily isolated in a high state of purity. S-collidine is used as an HCl acceptor. Silane compounds can be melt-condensed with aromatic diols to provide high molecular weight polyaryloxysilane materials that are of importance in polymer technology.
Silane for polycrystalline films deposition on oxidized silicon wafers, noting substrate temperature effects on preferred orientation of deposits
Infrared absorption spectra of ten individual contaminant materials and four binary mixtures of these have been studied using the internal reflection spectroscopy technique. The effect of ultraviolet radiation on these contaminants has also been studied. It has been observed that all siloxanes, silanes, and esters are drastically affected by ultraviolet irradiation. In most cases polymerization and tar formation results.
The activities of the Toxic Hazards Research Unit (THRU) for the period of June 1971 through May 1972 are reviewed in this report. Acute inhalation toxicity experiments were conducted on hydrogen chloride (HCl) gas and aerosol, ethyl bromide (C2H5Br), hydrogen bromide (HBr), hydrogen sulfide (H2S), ammonia (NH3), chlorine (CL2), and silane (SiH4). Subacute toxicity studies were conducted on chlorine pentafluoride (ClF5), dichloromethane (CH2Cl2) and coal tar volatiles. Further toxicity studies of subacute and chronic responses to inhaled monomethylhydrazine (MMH) are also described.
A method and apparatus for thermally growing stable silicon dioxide layers on silicon is disclosed. A previously etched and baked silicon nitride tube placed in a furnace is used to grow the silicon dioxide. First, pure oxygen is allowed to flow through the tube to initially coat the inside surface of the tube with a thin layer of silicon dioxide. After the tube is coated with the thin layer of silicon dioxide, the silicon is oxidized thermally in a normal fashion. If the tube becomes contaminated, the silicon dioxide is etched off thereby exposing clean silicon nitride and then the inside of the tube is recoated with silicon dioxide. As is disclosed, the silicon nitride tube can also be used as the ambient for the pyrolytic decomposition of silane and ammonia to form thin layers of clean silicon nitride.