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All sources NASA NTRS DOE OSTI

DOE OSTI2022

Kinetic Model for Moisture-Controlled CO 2 Sorption

The understanding of the sorption/desorption kinetics is essential for practical applications of moisture-controlled CO 2 sorption. We introduce an analytic model of the kinetics of moisture-controlled CO 2 sorption and its interpretation in two limiting cases. In one case, chemical reaction kinetics on pore surfaces dominates, in the other case, diffusive transport through the sorbent defines the kinetics. Here, we show that reaction kinetics, which is dominant in the first case, can be expressed as a linear combination of 1st and 2nd order kinetics in agreement with the static isotherm equation derived and validated in a previous paper. The interior transport kinetics can be described by non-linear diffusion equations. By combining all carbon species into a single equation, we can eliminate — in certain limits — the source terms associated with chemical reactions. In this case, the governing equation is ∂θ/∂t = –∇ · (–D eff ∇ θ ). For a sorbent in a form of a flat sheet or a membrane, one can maintain the same functional form of a diffusion equation by introducing a generalized effective diffusivity D M that combines contributions from both surface chemical reaction kinetics and interior diffusive transport kinetics. Experimental data of transient CO 2 flux in a preconditioned commercial anion exchange membrane fit well to the 1st order model as long as very dry states are avoided, validating the theory. The observed DM for a preconditioned commercial anion exchange membrane ranges from 6.6× 10 -14 to 7.1× 10 -14 m 2 s -1 at 35°C. These small values compared to typical ionic diffusivities imply a very slow kinetics, which will be the largest issue that needs to be addressed for practical application. The collected transient CO 2 flux data are used to predict the magnitude of a continuous CO 2 pumping flux in an active membrane that transports CO 2 against a CO 2 concentration gradient. The pumped CO 2 flux is supported by water flux due to a water concentration gradient.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Moisture Sorption and Swelling of Sylgard-184

The report summarizes the quantitative assessment of moisture sorption by Sylgard-184. It is an important ingredient in many of our materials. Moisture sorption for this material has been extensively studied with data from 9 different samples available for analysis. These samples varied in size and geometry. Seven of the 9 samples were thin slabs. The remaining 2 were cylinders, one of which had comparable height and diameter and is therefore considered a 3-D sample. All the samples, except 2 (1D_slab4.06mm and 1D_Sylgard_2016_Sharma) belonged to lot number A1606324. They were all prepared by Tony Rodrigues in the plastics shop in the Summer of 2016 and tested by Hom Sharma between October 2016 and June 2017. 1D_slab4.06mm was also prepared by Tony Rodrigues in the plastics shop in Summer of 2016, however, the sample did not have a lot number. 1D_Sylgard_2016_Sharma was prepared by Hom Sharma in February 2016 and tested potentially around May - June 2016.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

M3SF-24LL010301062-Surface Complexation/Ion Exchange Data Integration for Radionuclide Sorption to Clay Minerals

This progress report (Level 3 Milestone Number M3SF-24LL010301062) summarizes research conducted at Lawrence Livermore National Laboratory (LLNL) within the Argillite International Collaborations Work Package SF-24LL01030106. The activity is focused on our long-term commitment to engaging our partners in international nuclear waste repository research. The focus of this milestone is the establishment of international collaborations for sorption modeling and the associated impacts of unlocking larger, community-based datasets. More specifically, we are developing a database framework for Spent Fuel and Waste and Science Technology (SFWST) that is aligned with the Helmholtz Zentrum Dresden Rossendorf (HZDR) and other international sorption database development groups in support of the database needs of the SFWST program.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2022

A computational pipeline to generate a synthetic dataset of metal ion sorption to oxides for AI/ML exploration

The charged mineral/electrolyte interfaces are ubiquitous in the surface and subsurface–including the surroundings of the geological disposal sites for radioactive waste. Therefore, understanding how ions interact with charged surfaces is critically important for predicting radionuclide mobility in the case of waste leakage. At present, the Surface Complexation Models (SCMs) are the most successful thermodynamic frameworks to describe ion retention by mineral surfaces. SCMs are interfacial speciation models that account for the effect of the electric field generated by charged surfaces on sorption equilibria. These models have been successfully used to analyze and interpret a broad range of experimental observations including potentiometric and electrokinetic titrations or spectroscopy. Unfortunately, many of the current procedures to solve and fit SCM to experimental data are not optimal, which leads to a non-transferable or non-unique description of interfacial electrostatics and consequently of the strength and extent of ion retention by mineral surfaces. Recent developments in Artificial Intelligence (AI) offer a new avenue to replace SCM solvers and fitting algorithms with trained AI surrogates. Unfortunately, there is a lack of a standardized dataset covering a wide range of SCM parameter values available for AI exploration and training–a gap filled by this study. Here, we described the computational pipeline to generate synthetic SCM data and discussed approaches to transform this dataset into AI-learnable input. First, we used this pipeline to generate a synthetic dataset of electrostatic properties for a broad range of the prototypical oxide/electrolyte interfaces. The next step is to extend this dataset to include complex radionuclide sorption and complexation, and finally, to provide trained AI architectures able to infer SCMs parameter values rapidly from experimental data. Here, we illustrated the AI-surrogate development using the ensemble learning algorithms, such as Random Forest and Gradient Boosting. These surrogate models allow a rapid prediction of the SCM model parameters, do not rely on an initial guess, and guarantee convergence in all cases.

Li, Chunhui↗

NASA NTRS1986

Dynamic design of gas sorption J-T refrigerator

A long-life Joule-Thomson refrigerator which is heat powered, involves no sealing, and has few mechanical parts is desirable for long-term sensor cooling in space. In the gas-sorption J-T refrigerator, cooling is achieved by gas sorption (either adsorption or absorption) processes. Currently, a modular, single-stage refrigerator is being designed and built to be operated at 20 K. The design was analyzed using a dynamic model, which is described here. The model includes the kinetics of the compressors and the heat switches, the heat transfer of the pre-coolers and the heat exchangers, the on/off ratio of the check valves, and the impedance of the J-T valve. The cooling power, the cycle time, and the operating conditions were obtained in terms of the power input, the heat sink temperature, and the J-T impedance.

Chan, C. K.↗

NASA NTRS1988

Sorption cryogenic refrigeration - Status and future

The operation principles of sorption cryogenic refrigeration are discussed. Sorption refrigerators have virtually no wear-related moving parts, have negligible vibration, and offer extremely long life (at least ten years), making it possible to obtain efficient, long life and low vibration cooling to as low as 7 K for cryogenic sensors. The physisorption and chemisorption systems recommended for various cooling ranges down to 7 K are described in detail. For long-life cooling at 4-5 K temperatures, a hybrid chemisorption-mechanical refrigeration system is recommended.

Jones, Jack A.↗

NASA NTRS1988

Iodine sorption study on the proposed use of Viton A in a shuttle galley water accumulator

The installation of a Viton A accumulator in the Shuttle galley has been proposed to prevent overpressurization of the hot water supply system. A laboratory study has been conducted to determine if there would be any interaction between the Viton A material and the iodine used to disinfect the water. Coupons of Viton A were exposed for 24 hours to aqueous iodine solutions similar in quality to the Shuttle's potable water. Changes in the iodine residual were monitored to determine the rate of iodine sorption by the coupon. Total organic carbon (TOC) was monitored to determine the rate of desorption of organic materials from the Viton A. The same coupons were then soaked in reagent-grade water for 24 hours, and iodine was monitored to determine the rate of iodine desorption. The coupons were again exposed to iodine solutions for 24 hours and iodine and TOC were monitored. No significant change in the iodine sorption rate was detected between the first and second exposures. A triangle taste test indicated at a 1 percent confidence level that the water exposed to Viton A had a different taste which was less acceptable to the panelists.

Gibbons, Randall E.↗

NASA NTRS1991

Mixed-Gas Sorption Joule-Thomson Refrigerator

Proposed mixed-gas sorption Joule-Thomson refrigerator provides cooling down to temperature of 70 K. Includes only one stage and no mechanical compressor. Simpler, operates without vibrating, and consumes less power in producing same amount of cooling. Same sorption principle of operation applicable in compressor that chemisorbs oxygen or hydrogen from mixture with helium, neon, and/or other nonreactive gases.

Jones, Jack A.↗

NASA NTRS1990

Regenerative sorption compressors for cryogenic refrigeration

Dramatic efficiency improvements for sorption coolers appear possible with use of compressor heat regeneration techniques. The general theory of sorption compressor heat regeneration is discussed in this paper, and several design concepts are presented. These designs result in long-life, low-vibration cryocoolers that potentially have efficiencies comparable to Stirling refrigerators for 65 to 90 K spacecraft instrument cooling applications.

Bard, Steven↗

NASA NTRS1994

Simpler Three-Stage Regenerative Sorption Cooler

Three-stage regenerative sorption cooler simpler version of one described in "Three-Stage Regenerative Sorption Cooler Reaches 65 K" (NPO-18366). In exchange for simplification, requires about 1 1/2 times input power of more-complicated version.

Bard, Steven↗

NASA NTRS2000

Design Models for the Development of Helium-Carbon Sorption Crycoolers

We have developed models for predicting the performance of helium-based Joule-Thomson continuous-flow cryocoolers using charcoal-pumped sorption compressors. The models take as inputs the number of compressors, desired heat-lift, cold tip temperature, and available precooling temperature and provide design parameters as outputs. Future laboratory development will be used to verify and improve the models. We will present a preliminary design for a two-stage vibration-free cryocooler that is being proposed as part of a mid-infrared camera on NASA's Next Generation Space Telescope. Model predictions show that a 10 mW helium-carbon cryocooler with a base temperature of 5.5 K will reject less than 650 mW at 18 K. The total input power to the helium-carbon stage is 650 mW. These models, which run in MathCad and Microsoft Excel, can be coupled to similar models for hydrogen sorption coolers to give designs for 2-stage vibration-free cryocoolers that provide cooling from approx. 50 K to 4 K.

Lindensmith, C. A.↗

NASA NTRS2000

Design Models for the Development of Helium-Carbon Sorption Cryocoolers

Lindensmith, Chris A.↗

NASA NTRS2012

Reversible Ammonia Sorption for the Primary Life Support System (PLSS)

Results are presented on the development of regenerable trace-contaminant (TC) sorbent for use in Extravehicular Activities (EVAs), and more specifically in the Primary Life Support System (PLSS). Since ammonia is the most important TC to be captured, data presented in this paper are limited to ammonia sorption, with results relevant to other TCs to be reported at a later time. The currently available TC-control technology involves the use of a packed bed of acid-impregnated granular charcoal. The sorbent is non-regenerable, and its use is associated with appreciable pressure drop, i.e. power consumption. The objective of this work is to demonstrate the feasibility of using vacuum-regenerable sorbents for PLSS application. In this study, several carbon sorbent monoliths were fabricated and tested. Multiple adsorption/vacuum-regeneration cycles were demonstrated at room temperature, as well as carbon surface conditioning that enhances ammonia sorption without impairing sorbent regeneration. Depending on sorbent monolith geometry, the reduction in pressure drop with respect to granular sorbent was found to be between 50% and two orders of magnitude. Resistive heating of the carbon sorbent monolith was demonstrated by applying voltage to the opposite ends of the monolith.

Wojtowicz, Marek A.↗

NASA NTRS2017

Kinetics of Moisture Sorption and Reverse Bias Degradation in Chip Tantalum Capacitors

Exposure of chip MnO2 tantalum capacitors to humid environments might result in increased ESR, leakage currents, and first turn-on failures. However, there is a lack of literature data on the effect of moisture on reverse bias behavior of the parts. The presence of moisture can also result in pop-corning when a high water vapor pressure develops when moisture absorbed in pores of tantalum slugs vaporizes instantly during soldering process resulting in damage to capacitors. A study of kinetics of moisture ingress to and release from active elements of capacitors would allow a better understanding of degradation mechanisms and is important for preventing failures. In this work, a technique for investigation of moisture sorption and desorption in solid chip tantalum capacitors that employs tantalum slugs as a humidity sensor have been developed and kinetics of the process analyzed for different types of capacitors at temperatures from room to 125 ºC. A model that relates diffusion characteristics of polymer cases and size of the slugs to characteristic times of moisture sorption has been developed. A strong effect of moisture on long-term degradation of reverse bias currents in MnO2 cathode capacitors has been demonstrated and physical mechanisms discussed.

Teverovsky, Alexander↗

NASA NTRS2017

Kinetics of Moisture Sorption and Reverse Bias Degradation in Chip Tantalum Capacitors

Exposure of chip MnO2 tantalum capacitors to humid environments might result in increased ESR, leakage currents, and first turn-on failures. However, there is a lack of literature data on the effect of moisture on reverse bias behavior of the parts. The presence of moisture can also result in pop-corning when a high water vapor pressure develops when moisture absorbed in pores of tantalum slugs vaporizes instantly during soldering process resulting in damage to capacitors. A study of kinetics of moisture ingress to and release from active elements of capacitors would allow a better understanding of degradation mechanisms and is important for preventing failures. In this work, a technique for investigation of moisture sorption and desorption in solid chip tantalum capacitors that employs tantalum slugs as a humidity sensor have been developed and kinetics of the process analyzed for different types of capacitors at temperatures from room to 125 C. A model that relates diffusion characteristics of polymer cases and size of the slugs to characteristic times of moisture sorption has been developed. A strong effect of moisture on long-term degradation of reverse bias currents in MnO2 cathode capacitors has been demonstrated and physical mechanisms discussed.

Teverovsky, Alexander↗

DOE OSTI2023

CO2 Sorption in Aminopolymer-Based Direct Air Capture Composites Through Fluorescent Detection

Aminopolymer-mesoporous oxide composites are becoming widely recognized for their ability to adsorb CO2 directly from the air. However, a better fundamental understanding of the nature of these materials under different environmental operating conditions will be necessary before they become ubiquitous in industrial direct air capture (DAC) systems. For example, gas diffusion in general is coupled with polymer segmental mobility in these composites; diffusion is therefore affected by interactions of the polymer with the pore wall of the mesoporous oxide, by the relative humidity of the air, and by electrostatic crosslinks that develop as a function of CO2 sorption. Disentangling these and additional complicated effects in order to better optimize operating conditions is a major challenge for the field. Here, we present a method for quantifying the adsorption of CO2 and moisture in a polyethylenimine (PEI) - Al2O3 composite using infrared sensing while we simultaneously monitor polymer mobility with a fluorescent probe molecule doped into the composite. Both the fluorescence intensity and shape of the emission spectra are strongly dependent on the mobility of the supporting medium. We monitor the polymer mobility and CO2 adsorption kinetics across a series of different relative humidities (RH) with this technique, and we observed that the relative difference between polymer mobility and sorption kinetics from one RH to the next are quite dramatic. We interpret these results and discuss how they can be used to inform the design of more efficient DAC systems for real-world operating conditions.

carbon capture↗

DOE OSTI2025

Investigation of competitive sorption and plasticization of hyperaged CANAL ladder polymers for acid gas purification

Identifying membrane materials that have exceptional separation performance and stability to complex CO 2 -containing mixtures is a pressing topic in separation science. In this work, the membrane separation performance for a recently discovered class of contorted polymers synthesized via catalytic arene-norbornene annulation (CANAL) polymerization is presented. These CANAL polymers achieve high CO 2 /CH 4 selectivity of 68 after physical aging (up to ∼1 year), which significantly augments the size-sieving capabilities of the membranes. Binary CO 2 /CH 4 and ternary H 2 S/CO 2 /CH 4 testing result in a 41 % and 50 % enhancement in selectivities, respectively, for hyperaged (∼1 year) contorted CANAL polymers, highlighting their size-sieving capabilities. The remarkably high CO 2 /CH 4 mixed-gas and combined acid gas (CAG, (CO 2 +H 2 S)/CH 4 ) selectivities of 88 and 95, respectively, for CANAL-Me-S 5 F in particular surpass both the 2018 CO 2 /CH 4 mixed-gas and CAG upper bounds. Performance stability was also investigated for high concentrations of CO 2 , revealing a reduction in CO 2 /CH 4 mixed-gas selectivity without compromising CO 2 permeability, suggesting strong sorption of CO 2 but minimal plasticization effects for short testing periods. In addition, time-dependent plasticization shows negligible effects on CO 2 /CH 4 mixed-gas selectivity despite an increase in CO 2 permeability when exposed to high concentrations of plasticizing CO 2 over an extended period of 170 h. This study provides valuable insights into hyperaged CANAL polymers and their performance in practical industrial processes.

03 NATURAL GAS↗

DOE OSTI2025

Liquid Sorption-Enhanced Haber–Bosch Process

The use of a liquid sorbent in a traditional Haber-Bosch process enables significant improvements in energy efficiency and potential cost savings for arguably the most important chemical process on the planet. The approach presented in this report employs an incompressible liquid sorbent that absorbs and releases ammonia (NH 3 ) under specific conditions. To achieve this, we investigate reactions of ammonia and pure phosphoric acid (H 3 PO 4 , PA), which rapidly neutralize to form an equilibrated solution of monoammonium phosphate (MAP) and diammonium phosphate (DAP) that functions as a reversible and regenerable sorbent. Through intimate contact of the gas-phase Haber-Bosch reaction mixture with this liquid absorbent, complete equilibrium uptake may be achieved in an appropriately sized separator, and facile separation occurs through the use of independent liquid and gas phases. Following depressurization and release of the ammonia product, only the incompressible fluid needs to be repressurized and returned to the reactor. This study documents proof-of-concept absorption and desorption experiments carried out in 75 mL batch reactors, predominantly charged with precise MAP and DAP mixtures that equilibrate at process-relevant temperatures and pressures. We then assemble the first thermodynamic relationships that underlie this advantaged separation strategy, validated by reactive force field (ReaxFF) interatomic potential simulations, and benchmarked with traditional separation routes via process modeling and technoeconomic analysis. The scale of energy consumption in the century-old Haber-Bosch process is massive, and the elegant liquid sorption approach reported here offers opportunities to enhance its energy efficiency for the next frontier of ammonia synthesis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗