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At least 19 records

Chemical compatibility of hollow ceramic cenospheres as thermal insulation for high-temperature thermal energy storage applications with molten nitrate salt

An effective insulation material that is both thermally and chemically stable in molten salts could transform the design of molten-salt-based thermal energy storage (TES) tanks. Most current molten salt TES tanks hold the metallic tank structure in direct contact with hot salt inventory, a design which leads to thermal expansion of the tank and triggers stresses that can lead to thermomechanical failures. With an internal insulation to lower the temperature at the tank structure, the extent of thermal expansion can be reduced, thereby reducing expansion-induced stresses and allowing for consideration of lower-cost tank structure materials. Conventional insulation materials are either 1) too porous and allow molten salts to permeate into the matrix, which significantly increases the thermal conductivity or 2) too dense and have a thermal conductivity that cannot provide sufficient thermal insulation. This paper presents an alternative thermal insulation concept using cenospheres which have an alumino-silicate structure. The cost analysis suggests that the low-density cenospheres can be one of the cheapest materials to provide cost-effective thermal insulation. The chemical compatibility of cenospheres is investigated in molten 60 wt% NaNO3/40 wt% KNO3 salt which is close to industrial-grade Solar Salt. This paper shows that diffusion of the sodium and potassium cations from the salt into the cenospheres occurs based on weight analysis, energy dispersive spectroscopy (EDS), X-ray diffraction (XRD) and Fourier-transform infrared (FTIR) spectroscopy. The cation diffusion breaks the bridging oxygen bonds and causes volume expansion of the microstructure which is responsible for the failure of the cenosphere particles. The chemical composition of the cenospheres is found to affect their compatibility with molten nitrate salt. A cenosphere product with low iron content showed the best compatibility with an average survival rate of 77.9% +/- 9.8% after 7 days of immersion in the molten nitrate salt. While even the low-iron cenospheres appear to require protection from direct molten salt contact, their slow degradation rate, closed-cell porosity, and low cost hold potential for effective use as internal tank insulation.

14 SOLAR ENERGY↗

ECAR-6588 Chemical Compatibility of MARVEL Components: Project # 33526

This ECAR serves to demonstrate the compatibility of MARVEL Reactor materials in contact with the two molten metal coolants, sodium potassium eutectic and lead. Operational requirements are determined, and recommendations for material treatment or replacement are presented.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

RH-TRU Waste Streams: HFDA Crucibles Create New Complex Waste Stream

This project focuses on the removal of the Hot Fuel Dissolution Apparatus (HFDA) crucibles from the Hot Fuel Examination Facility’s (HFEF) hot cells to create space for upcoming projects. The project team has created a crucible and pyro-salt non-debris waste stream that can be disposed of at Waste Isolation Pilot Plant (WIPP). Chemical Compatibility Examinations (CCEs) must be performed on candidate waste by reviewing the types of chemicals used in the experiments, information found in INL Process Knowledge Summary Reports (PKSRs), and Environmental Protection Agency guides on chemical compatibility. The CCEs identify which chemicals can be safely combined to ensure adverse reactions do not occur in the waste packages. The CCEs are then used to update the PKSR, Basis of Knowledge, and Acceptable Knowledge documents and demonstrate compliance with the WIPP Waste Acceptance Criteria. Once documents are finalized, they are reviewed and approved by the WIPP Central Characterization Project (CCP) to ensure proper waste stream characterization. After the documents are approved, the crucibles can be packaged and shipped to the Idaho Nuclear Technical and Engineering Center for storage awaiting certification. CCP will certify the waste using the approved documents and a series of confirmatory testing before being shipped and disposed in WIPP’s deep geological repository. Currently, the CCE is in progress and the PKSRs are being updated.

Basis of Knowledge↗

A high-performance organic cathode customized for sulfide-based all-solid-state batteries

All-solid-state batteries (ASSBs) have become increasingly attractive recently due to their better safety and prospective long-term stability compared with conventional liquid batteries. However, obtaining a sustainable cathode candidate to match the solid electrolyte with regards to operating potential, chemical compatibility, and mechanical property is still an open challenge. In this work, the chemical incompatibility of quinone-based active materials and sulfide-based electrolyte were unveiled for the first time through a heteroconjugate addition reaction mechanism. To develop a quinone cathode customized for sulfide-based ASSBs, poly-(anthraquinonyl sulfide)-graphene (PAQS-G) nanocomposite was reported. The stable polymer framework of PAQS can protect the quinone redox center by preventing nucleophilic attack from sulfide-based solid electrolytes. The graphene additives can ameliorate redox kinetics and improve active material utilization. The PAQS-G cathode exhibited a specific capacity of ~178 mAh g -1 and a high material utilization of ~79%. Excellent cycling stability was achieved with 94 % capacity after 200 cycles in lithium batteries and 95.5 % capacity after 300 cycles in sodium batteries at 0.1C rate, respectively. A promising potential for energy storage applications was demonstrated.

25 ENERGY STORAGE↗

Chemical interaction and compatibility of uranium mononitride and alumina forming austenitic stainless steel

Uranium mononitride (UN) and alumina forming austenitic (AFA) stainless steel are a potential fuel-cladding combination for the lead-cooled fast reactor (LFR). Chemical compatibility between UN and AFA steel needs to be verified before implementation in a nuclear reactor. Diffusion couple experiments at 823 K and 1023 K were conducted for nonirradiated UN samples in contact with as-cast (no thermally grown Al 2 O 3 ) and preoxidized (with thermally grown Al 2 O 3 ) AFA for 500 and 1000 h in an inert environment. Preoxidized AFA exhibited little to no interaction with all UN samples tested at both 823 K and 1023 K, displaying the stability and capability of the Al 2 O 3 layer to prevent chemical interaction and inter-diffusion with UN. Chemical interaction occurs between UN and as-cast AFA. At 1023 K, an aluminum and nitrogen rich phase (likely AlN) formed along the interface of as-cast AFA and UN samples. At 823 K the AlN phase was not prominently observed due to the reduced diffusivity of aluminum through AFA. The aluminum and nitrogen-enriched phase was also observed in a high temperature pressure-assisted test sample of UN and as-cast AFA thermally treated at 1373 K. Finally, in UN samples doped with a low weight percent of UO 2 (< 3 wt%), AlN was not detected along the interface at either temperatures, and an Al 2 O 3 layer likely formed along the interface and prevented further chemical interaction between UN and as-cast AFA.

36 MATERIALS SCIENCE↗

Post-irradiation Examination Status for the BSU-269 Project

High-density uranium inter-metallic uranium silicide (U 3 Si 2 ) was initially considered as a potential advanced nuclear fuel for light water reactor (LWR) systems due to several advantages it demonstrated in thermophysical properties, chemical, and irradiation stability. In addition to understanding the basic thermophysical and mechanical properties of U 3 Si 2 under LWR irradiation conditions, it is important to assess its performance with advanced claddings such as FeCrAl, SiC, or conventional Zr-based claddings. Several aspects of the fuel cycle and fuel performance are being evaluated for U 3 Si 2 coupled with different types of claddings. To thoroughly characterize the U 3 Si 2 -cladding system, their chemical compatibilities and the potential for fuel-cladding chemical interaction (FCCI) must be addressed. Interdiffusion studies have been performed between U 3 Si 2 /Zry-4 and U 3 Si 2 /FeCrAl using diffusion couples. For the U 3 Si 2 /Zry-4 system, ZrSi 2 was the primary interdiffusion product observed at 800°C in addition to other secondary phases from the Zr alloying elements such as Fe and Cr. Low melting point U 6 Fe was also observed at 1000°C. For the U 3 Si 2 /FeCrAl system, at temperatures above 500°C, chemical diffusion Fe-U and Fe-U-Si was observed, increasing with rising temperatures. Although information from these non-irradiated tests is a fundamental first assessment, follow-up with focused irradiation tests is necessary. Irradiation can significantly alter the structure and evolution of the FCCI layers compared to the non-irradiated conditions.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Examining Graphite Degradation in Molten Salt Environments: A Chemical, Physical, and Material Analysis

Molten-salt reactors (MSRs) are Generation IV nuclear reactors that use liquid salt as a coolant and/or fuel. In several MSR designs, graphite serves as a moderator and/or reflector. However, due to limited experimental data and operational experience, our understanding of graphite behavior in molten salt environments remains incomplete. This report aims to identify the degradation mechanisms of nuclear graphite in MSRs, detail the mechanisms of each factor, and provide an initial assessment of their impact on the structural integrity of graphite components. This assessment is based on an extensive literature review and insights from subject matter experts. Furthermore, given the limited data, a modeling strategy using existing Grizzly software is proposed for a more thorough analysis where appropriate. Additionally, it presents mitigation strategies where applicable. The report covers physical degradation mechanisms such as infiltration, erosion, and abrasion, as well as chemical degradation mechanisms including fluorination, intercalation, corrosion, and oxidation. Molten salt can infiltrate the porous structure of graphite, leading to several detrimental effects. Entrapment of fissile products within the graphite pores can cause radiation damage and could pose challenges in the handling and disposal of contaminated components. The differential thermal expansion between the infiltrated salt and graphite, along with internal stress from pressurized molten salt and volumetric heating, can compromise the structural integrity of graphite. To mitigate these effects, employing ultra-fine graphite grades and applying sealants and coatings are effective strategies. A computational model based on coupled solid mechanics and heat transfer phenomena could be used to predict the internal stresses using Grizzly software. In pebble-bed MSRs, graphite fuel pebbles can cause abrasion against reactor components due to friction and wear. The severity of wear is influenced by various factors such as temperature, environment, and the presence of lubricants. Tribological studies reveal that higher temperatures and molten salt environments, such as FLiBe, significantly reduce wear rates compared to dry conditions. Additionally, the chemical composition of the salt can further optimize graphite's tribological performance. Long-term wear effects can be modeled by incorporating surface defects into the geometry and predict stresses under thermal and radiation effects using Grizzly software. Chemical degradation of graphite in a molten salt environment can occur through fluorination and intercalation. Fluorination can occur via replacement of hydrogen or oxygen atoms, or at the active sites, but does not cause structural degradation. Intercalation, on the other hand, can lead to exfoliation, where layers of graphite separate and peel away, damaging the graphite. Protective coatings can enhance graphite's resistance to intercalation. Graphite generally exhibits good chemical stability in molten salt environments, though it can corrode under specific conditions, particularly in the presence of impurities or oxidants. Studies have shown that protective coatings, such as plasma-sprayed partially stabilized zirconia (PSZ), can effectively prevent such degradation. Corrosion behavior varies significantly with different graphite grades and coating applications, underscoring the need for detailed studies on uncoated and coated graphite to understand and mitigate corrosion mechanisms in MSRs. Research indicates that the presence of oxidants and impurities can accelerate graphite degradation in molten salts, making it essential to explore acceptable impurity limits. Oxidation is another critical degradation mechanism, leading to weight loss and structural damage due to the formation of CO and CO 2 from the reaction of carbon atoms with oxygen. This process creates new porosity and compromises graphite's integrity. While extensive research on graphite oxidation has been conducted for gas-cooled reactors, studies specific to MSRs are limited. Findings from the coal industry suggest that molten alkali metal salts can significantly accelerate graphite oxidation, a hypothesis worth exploring for fluoride salts in MSRs. Understanding oxidation behavior in MSRs is vital for developing protective measures. The analysis of post-irradiated graphite from the MSRE experiment demonstrated exceptional chemical compatibility with molten fluoride salt, suggesting that the extent of chemical attack on graphite largely depends on the salt's infiltration capability. Therefore, the use of ultra-fine grade graphite could help mitigate chemical degradation effects. Existing oxidation modeling capabilities in Grizzly, which use reaction-diffusion equations to model graphite-air interactions, could be adapted to simulate the chemical degradation effects of graphite in molten salt environments.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

TRISO Fuel for High-Temperature Passively-Safe Nuclear Reactors

The poster entitled "TRISO Fuel for High-Temperature Passively-Safe Nuclear Reactors" presents reasons why TRISO fuel is a safe nuclear fuel. The poster contains four blocks: Multiple barriers to fission product release, Thermal stability, Chemical compatibility and Safety and Performance. Each block present information on the TRISO fuel in terms of the mechanical, chemical and thermal properties. In summary the safety and performance of the TRISO fuel based on the experimental results is shown.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Joint LLNL & SNL Material Compatibility Study Commences

The fundamental goal of the W80-4 Life Extension Program (LEP) is the design and production of a safe and reliable system. Ensuring long-term viability and chemical compatibility of the materials in the warhead is paramount to its success. To that end, the material and aging compatibility team, which includes researchers from Lawrence Livermore and Sandia National Laboratories (SNL), has launched the LEP’s most comprehensive compatibility test to date.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Solid-State Side-Chain Functionalization of Conjugated Polymers for Expanded Chemical and Functional Versatility

Conjugated polymers that integrate diverse chemical functionalities with high electronic performance are essential for advanced organic electronic, optoelectronic, and biointerfaced technologies. Achieving such multifunctionality typically requires grafting functional units onto polymer side chains. However, conventional solution-phase approaches remain constrained by solubility limitations, side-chain-induced packing disruptions, and challenges in preserving charge transport. Here, we introduce a solid-state side-chain functionalization strategy that exploits a swellable polar side-chain architecture and azide–alkyne click chemistry to enable efficient molecular diffusion and reaction throughout predeposited polymer thin films. This approach substantially broadens the chemical compatibility of graftable units and mitigates the adverse effects on the electrical property. Moreover, the method supports spatially selective functionalization within a continuous film, enabling the patterned incorporation of chemically distinct groups to produce spatially defined optical properties. Here, this solid-state strategy thus provides a versatile platform for constructing conjugated polymers with expanded chemical versatility, preserved electronic performance, and programmable spatial functionality.

Conjugated polymers↗

Direct Air Capture-Compatible Azolate and Amino Acid Ionic Liquids for Electrochemical CO 2 Reduction to CO on a Silver Cathode

Direct air capture (DAC) compatible ionic liquids (ILs) are attractive for integrating CO 2 capture and conversion due to their high CO 2 solubility at low partial pressures, tunable chemisorption mechanisms, low volatility, and wide electrochemical windows. However, very few ILs have high CO 2 uptake at DAC conditions (420 ppm CO 2 ), and even fewer have been evaluated for chemical compatibility and mechanistic continuity for combined capture and electrochemical CO 2 reduction (eCO 2 RR). We demonstrate that two representative DAC-capable ILs, [P 4444 ][Val] (amino acid-based) and [P 66614 ][5-Me-Imd] (azolate-based), exhibit favorable electrochemical reduction behavior. CO and H 2 were the dominant gas-phase products by GC, while 1 H and 13 C NMR confirmed negligible liquid-phase HCOOH. Chronoamperometry at moderate applied potentials (−2.0 to −2.5 V vs Ag/AgCl) in a two-compartment H-cell with a Ag coated carbon paper as the working electrode yielded steady-state current densities of ∼10 mA cm −2 with CO FE of 96% for [P 4444 ][Val] and 95% for [P 66614 ][5-Me-Imd], highlighting the role of viscosity and chemically absorbed CO 2 -IL species to provide highly selective CO formation while suppressing H 2 evolution.

amino acid ionic liquid↗

Demonstration of an All-Refractory Corrosion-Resistant Molten Salt Pumping and Storage Infrastructure Up to 950 degrees C

Concentrating solar power (CSP) with thermal energy storage (TES) has an estimated cost similar to solar photovoltaics (PV) with lithium-ion batteries (LIB), but CSP + TES has the potential for significantly reduced cost by operating above 700 degrees C. However, this requires a TES medium and containment infrastructure which are chemically compatible and do not degrade above 700 degrees C. MgCl2-KCl-NaCl (MKN) salt is a promising medium, but when MKN salt has small amounts of water and oxygen dissolved in it, it excessively corrodes conventional commercial alloys. Here, we consider refractory materials including graphite, carbon-carbon composite (C/C), and molybdenum because they maintain high mechanical strength at elevated temperatures and are expected to resist corrosion by MKN salt. While selection of refractory materials is often constrained by the need to remain chemically stable in air, this work uses an enclosure filled with inert gas to allow the use of materials like graphite and molybdenum. Notably, graphite components can seal against liquids unlike many brittle refractory materials. We demonstrate a centrifugal pump and mechanical seals made of refractory materials in a laboratory-scale circulation loop, which successfully operated continuously for more than 49 h at temperatures ranging from 750 degrees C to 950 degrees C with no mechanical failures or chemical degradation of the refractory materials. To the best of our knowledge, this is the highest temperature molten salt circulation loop that has been successfully developed, and this refractory infrastructure allows for operation at even much higher temperatures (<1600 degrees C) if a storage medium with a lower vapor pressure is used. The principles of this architecture are relevant to other applications with high temperature flowing metals and salts including Generation IV nuclear fission reactors for power production and molten salt electrolysis reactors for metallurgical processing.

14 SOLAR ENERGY↗

Investigation of Solid Particle Reactors for Nonoxidative Dehydrogenation of Ethane: Toward Solar Thermal Ethylene Production

Concentrating solar power plants can generate renewable heat at temperatures well above those of most industrial processes. Ceramic particles irradiated with concentrated sunlight can store high-quality sensible heat and transfer this to power generation systems. These concepts and materials hold great potential to also enable thermal processes in the chemical industry, but effective strategies for transferring heat from thermal energy storage media into chemical reactors are still under development. This present work evaluated the thermal and chemical compatibility of various solid particle media (including quartz, bauxite, and alumina particles) integrated directly into tube reactors and the subsequent effects on reactor performance for the nonoxidative dehydrogenation of ethane reaction. Empty tube reactors without loaded particles (representing conventional ethane cracking coils) showed significant heat transfer limitations as the tube diameter was scaled. The incorporation of media into the reactor significantly aided heat transfer to the gaseous ethane reactant and increased its conversion by as much as 10% at similar space velocities. Despite direct contact with hydrocarbon gases, alumina and quartz media showed negligible coke formation. Even during reaction in 100% ethane feed gas at 825 °C, the average selectivity of the coke product was only 0.57% when using the quartz media. These materials further demonstrated excellent thermal stability during subsequent reoxidation in air at 800 °C, which simulated the reheating of particles in a circulating particle solar receiver. Conversely, high rates of coke formation, with a product selectivity of 27.5%, were observed on sintered bauxite particles during the reaction, likely promoted by transition metal constituents. These particles fractured upon reoxidation due to exotherms generated from coke combustion. In conclusion, while the use of cofed steam could mitigate attrition of redox-active particles, the ability of inert metal oxide particles to efficiently transfer heat to concentrated ethane reactant gas while suppressing side reactions or degradation suggests that these media could effectively couple solar thermal plants to reactors for next-generation production of ethylene and other critical chemicals.

Hydrocarbons↗

Ionic Liquid-Mediated Scanning Probe Electro-Oxidative Lithography as a Novel Tool for Engineering Functional Oxide Micro- and Nano-Architectures

Functional oxides have extensively been investigated as a promising class of materials in a broad range of innovative applications. Harnessing the novel properties of functional oxides in micro- to nano-scale applications hinges on establishing advanced fabrication and manufacturing techniques able to synthesize these materials in an accurate and reliable manner. Oxidative scanning probe lithography (o-SPL), an atomic force microscopy (AFM) technique based on anodic oxidation at the water meniscus formed at the tip/substrate contact, not only combines the advantages of both “top-down” and “bottom-up” fabrication approaches, but also offers the possibility of fabricating oxide nanomaterials with high patterning accuracy. While the use of self-assembled monolayers (SAMs) broadened the application of o-SPL, significant challenges have emerged owing to the relatively limited number of SAM/solid surface combinations that can be employed for o-SPL, which constrains the ability to control the chemistry and structure of oxides formed by o-SPL. Here, in this work, a new o-SPL technique that utilizes room-temperature ionic liquids (RTILs) as the functionalizing material to mediate the electrochemistry at AFM tip/substrate contacts is reported. The results show that the new IL-mediated o-SPL (IL-o-SPL) approach allows sub-100 nm oxide features to be patterned on a model solid surface, namely steel, with an initiation voltage as low as -2 V. Moreover, this approach enables high tunability of both the chemical state and morphology of the patterned iron oxide structures. Owing to the high chemical compatibility of ILs, which derives from the possibility of synthesizing ILs able to adsorb on a wide variety of solid surfaces, IL-o-SPL can be extended to other material surfaces and provide the opportunity to accurately tailor the chemistry, morphology, and electronic properties within nanoscale domains, thus opening new pathways to the development of novel micro- and nano-architectures for advanced integrated devices.

36 MATERIALS SCIENCE↗

Generalizable Porous Aromatic Framework‐Included Polymer Membranes for Diffusion‐Enhanced Gas Separations

Industrial separation processes account for 10-15% of global energy consumption. Membrane-based processes are less energy-intensive than traditional gas separation technologies; however, enhanced material separation performance and stability for numerous gas mixtures are needed for widespread industrial adoption. This work presents a generalizable strategy for preparing mixed-matrix gas separation membranes exceeding the performance upper bounds of existing polymer membranes for a wide variety of industrial gases. By incorporating robust porous aromatic framework (PAF) particles into various dense commercial polymer matrices, gas diffusivity and solubility can be enhanced. For diverse gas mixtures (e.g., CO2/N2, O2/N2, He/CH4, H2/N2, and C2H4/C2H6), the resulting composite membranes exhibit enhanced gas permeabilities-by as much as 520%-and largely unchanged selectivities even after 6 years of aging under simulated flue gas conditions. These improvements arise from the ultrahigh porosity, excellent chemical compatibility, and unique physicochemical properties of the embedded PAF particles. Functionalizing the PAFs with polyamines also enables composite membranes that achieve among the highest reported performances against plasticization, a common obstacle in commercializing gas separation membranes. Significantly, the PAF-1 particles are readily dispersible in various common membrane casting solvents, suggesting their broader utility as a filler for designing high-performance membranes for many industrial gas separations.

Uliana, Adam A↗

Recent Advances in Conduction Mechanisms, Synthesis Methods, and Improvement Strategies for Li 1+ x Al x Ti 2-x (PO 4 ) 3 Solid Electrolyte for All-Solid-State Lithium Batteries

With the increasing use of Li batteries for storage, their safety issues and energy densities are attracting considerable attention. Recently, replacing liquid organic electrolytes with solid-state electrolytes (SSE) has been hailed as the key to developing safe and high-energy-density Li batteries. In particular, Li 1+ x Al x Ti 2- x (PO4) 3 (LATP) has been identified as a very attractive SSE for Li batteries due to its excellent electrochemical stability, low production costs, and good chemical compatibility. However, interfacial reactions with electrodes and poor thermal stability at high temperatures severely restrict the practical use of LATP in solid-state batteries (SSB). Herein, a systematic review of recent advances in LATP for SSBs is provided. Here, this review starts with a brief introduction to the development history of LATP and then summarizes its structure, ion transport mechanism, and synthesis methods. Challenges (e.g., intrinsic brittleness, interfacial resistance, and compatibility) and corresponding solutions (ionic substitution, additives, protective layers, composite electrolytes, etc.) that are critical for practical applications are then discussed. Last, an outlook on the future research direction of LATP-based SSB is provided.

25 ENERGY STORAGE↗

Additively manufactured polymer composites for heat exchanger applications: evaluation of critical thermophysical properties

Polymeric heat exchangers (PHXs) have been used in applications involving weight restrictions, chemical compatibility, and fouling issues. Additive manufacturing (AM) or 3D printing provide new solutions to previously inaccessible combinations of properties and geometries. There are some advancements in the PHXs by AM; however, the process and the properties of materials still need further investigation to improve the overall performance. In this study, additively manufactured polyethylene terephthalate glycol (PETG) composites reinforced with graphite and pitch-based carbon fibers were evaluated for their potential application as PHXs. The thermal conductivity, volumetric heat capacity, coefficient of thermal expansion, creep behavior, and long-term performance were studied in detail. Our results reveal that the composites have an anisotropic thermal conductivity. The thermal conductivity along the printing direction is higher than the layer building direction due to the shear-induced alignment of the fillers. The printed composites achieve good thermal stability with 80% lower CTE at room temperature than neat PETG. Creep tests suggest the creep and creep recovery were highly temperature-dependent, and the deformation can be recovered when the temperature is below glass transition. These results suggest additive manufactured composites be potentially used for heat exchanger applications at low temperatures.

36 MATERIALS SCIENCE↗

Chemistry of the interaction between an alkoxysilane-based impregnation treatment and cementitious phases

Chemical compatibility with a wide range of materials is among the features that has driven the use of alkoxysilanes as consolidants in built structures. Such compatibility is particularly important in cementitious materials where the reaction with portlandite may generate C-S-H gel, one of the main hydration phases of OPC. The cementitious matrix is a complex system, however, and the reaction of its many phases with alkoxysilanes, while poorly understood, may determine treatment efficacy. This article describes a detailed study of the individual interactions between an oligomeric alkoxysilane-based impregnation treatment previously shown to interact with the portlandite present in cement paste and the cementitious phases generated in ordinary portland cement hydration. The findings show that both portlandite and C-S-H gel interact with the silicon oligomers in the hydrolysed impregnation treatment to generate a C-S-H gel (in the case of portlandite) and a rise in C-S-H gel mean chain length (MCL). Ettringite is also altered in the presence of alkoxysilanes, transforming to gypsum and AH{sub 3}. Its transformation generates a tetrahedral aluminium that is taken up into a high silicon gel sourced from the treatment to form an amorphous aluminosilicate gel. Monocarboaluminate and katoite also partially decompose in the interaction with the product, whereas gibbsite remains unaffected.

36 MATERIALS SCIENCE↗