A novel SAXS model for multi-texture systems: application to CaCO3 calcination using in-situ USAXS-SAXS-WAXS

Strumendo, Matteo matteo.strumendo@unipd.it; Segre, Carlo U.; Ilavsky, Jan; Kuzmenko, Ivan

doi:10.1016/j.apmt.2022.101568

A novel SAXS model for multi-texture systems: application to CaCO₃ calcination using in-situ USAXS-SAXS-WAXS

Journal Article · Thu Jun 30 00:00:00 EDT 2022 · Applied Materials Today

DOI:https://doi.org/10.1016/j.apmt.2022.101568· OSTI ID:1902634

^[1]; ^[2]; ^[3]; Kuzmenko, Ivan ^[3]

Univ. degli Studi di Padova (Italy)
Illinois Institute of Technology, Chicago, IL (United States)
Argonne National Lab. (ANL), Argonne, IL (United States)

SAXS models, used to calculate the micro-textural properties (porosity, specific surface, correlation length, correlation function) of porous materials, are especially relevant for in-situ material characterization. Certain classes of porous materials, including those generated during solid decompositions, are characterized by distinct regions with different micro-textures. Classical SAXS models cannot be applied directly to such multi-texture systems, thus a novel SAXS model for multi-texture systems is proposed in this work and validated by using measurements of micro-textural properties of a calcined CaCO₃ powder, obtained using time-resolved in-situ synchrotron radiation USAXS, SAXS and WAXS data. The proposed model, in contrast to the direct application of classical SAXS models, is capable of correctly predicting the expected linear trend of the particle internal porosity with respect to the CaCO₃ conversion and provides a complete description of the micro-textural properties, in very close agreement with experimental data available in the literature. In the reaction product region the correlation function, as well as the other micro-textural properties, is essentially constant during the solid decomposition, and is accurately represented by a two-parameter model. Based on the proposed SAXS model, a simplified expression of the differential scattering cross section, as a product of the CaO mass fraction times a time-independent function of the correlation function, is obtained; such expression can reliably predict the experimental scattering intensity profiles over time.

View Accepted Manuscript (DOE)

Research Organization:: Argonne National Laboratory (ANL), Argonne, IL (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES). Scientific User Facilities Division

Grant/Contract Number:: AC02-06CH11357

OSTI ID:: 1902634

Journal Information:: Applied Materials Today, Journal Name: Applied Materials Today Vol. 29; ISSN 2352-9407

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

References (59)

The effect of CaO sintering on cyclic CO2 capture in energy systems Sun, P.; Grace, J. R.; Lim, C. J. AIChE Journal, Vol. 53, Issue 9 https://doi.org/10.1002/aic.11251	journal	January 2007
Novel model for the sintering of ceramics with bimodal pore size distributions: Application to the sintering of lime Maya, Juan C.; Chejne, Farid; Bhatia, Suresh K. AIChE Journal, Vol. 63, Issue 3 https://doi.org/10.1002/aic.15446	journal	August 2016
Effect of the product layer on the kinetics of the CO2-lime reaction Bhatia, S. K.; Perlmutter, D. D. AIChE Journal, Vol. 29, Issue 1 https://doi.org/10.1002/aic.690290111	journal	January 1983
Catalyzed Sintering of Regenerated CaO Induced by Partition Evolution of Calcium Carbonate Niu, Jiaming; Li, Mingchun; Wang, Baoting Chemical Engineering & Technology, Vol. 44, Issue 3 https://doi.org/10.1002/ceat.202000368	journal	January 2021
The reversibility of the reaction CaCO3 ⇄ CaO+CO2 Barker, Ronald Journal of Applied Chemistry and Biotechnology, Vol. 23, Issue 10 https://doi.org/10.1002/jctb.5020231005	journal	October 1973
Ultra-Small-Angle X-ray Scattering Instrument at the Advanced Photon Source: History, Recent Development, and Current Status Ilavsky, J.; Zhang, F.; Allen, A. J. Metallurgical and Materials Transactions A, Vol. 44, Issue 1 https://doi.org/10.1007/s11661-012-1431-y	journal	October 2012
Sintering of nascent calcium oxide H. Borgwardt, Robert Chemical Engineering Science, Vol. 44, Issue 1 https://doi.org/10.1016/0009-2509(89)85232-7	journal	January 1989
Small-angle X-ray study of particulate reinforced composites Wu, Wen-li Polymer, Vol. 23, Issue 13 https://doi.org/10.1016/0032-3861(82)90216-6	journal	December 1982
Preparation of nanocrystalline Na2ZrO3 for high-temperature CO2 acceptors: chemistry and mechanism Zhao, Tiejun; Rønning, Magnus; Chen, De Journal of Energy Chemistry, Vol. 22, Issue 3 https://doi.org/10.1016/S2095-4956(13)60050-9	journal	May 2013
Nano CaO grain characteristics and growth model under calcination Zhu, Yanqing; Wu, Sufang; Wang, Xieqing Chemical Engineering Journal, Vol. 175 https://doi.org/10.1016/j.cej.2011.09.084	journal	November 2011
Calcination–carbonation durability of nano CaCO3 doped with Li2SO4 Lu, Shangqing; Wu, Sufang Chemical Engineering Journal, Vol. 294 https://doi.org/10.1016/j.cej.2016.02.100	journal	June 2016
Characterization of potassium doped Li2ZrO3 based CO2 sorbents: Stability properties and CO2 desorption kinetics Peltzer, D.; Mùnera, J.; Cornaglia, L. Chemical Engineering Journal, Vol. 336 https://doi.org/10.1016/j.cej.2017.10.177	journal	March 2018
Analysis of textural properties of CaO-based CO2 sorbents by ex situ USAXS Benedetti, Alberto; Ilavsky, Jan; Segre, Carlo Chemical Engineering Journal, Vol. 355 https://doi.org/10.1016/j.cej.2018.07.164	journal	January 2019
Polyetheramine improves the CO2 adsorption behavior of tetraethylenepentamine-functionalized sorbents Wang, Xia; Zeng, Wulan; Song, Mingjun Chemical Engineering Journal, Vol. 364 https://doi.org/10.1016/j.cej.2019.02.008	journal	May 2019
Investigation of CaO–CO2 reaction kinetics by in-situ XRD using synchrotron radiation Biasin, A.; Segre, C. U.; Salviulo, G. Chemical Engineering Science, Vol. 127 https://doi.org/10.1016/j.ces.2014.12.058	journal	May 2015
The calcium looping cycle for CO2 capture from power generation, cement manufacture and hydrogen production Dean, C. C.; Blamey, J.; Florin, N. H. Chemical Engineering Research and Design, Vol. 89, Issue 6 https://doi.org/10.1016/j.cherd.2010.10.013	journal	June 2011
Comparative techno-economic analysis for steam methane reforming in a sorption-enhanced membrane reactor: Simultaneous H2 production and CO2 capture Lee, Hyunjun; Lee, Boreum; Byun, Manhee Chemical Engineering Research and Design, Vol. 171 https://doi.org/10.1016/j.cherd.2021.05.013	journal	July 2021
Recent developments and consideration issues in solid adsorbents for CO2 capture from flue gas Nie, Lijuan; Mu, Yuanyuan; Jin, Junsu Chinese Journal of Chemical Engineering, Vol. 26, Issue 11 https://doi.org/10.1016/j.cjche.2018.07.012	journal	November 2018
Thermally-Induced morphological evolution of spherical silica nanoparticles using in-operando X-ray scattering measurements Asgar, Hassnain; Semeykina, Viktoriya; Hunt, Mikaila Colloids and Surfaces A: Physicochemical and Engineering Aspects, Vol. 586 https://doi.org/10.1016/j.colsurfa.2019.124260	journal	February 2020
Contrasting thermally-induced structural and microstructural evolution of alumino-silicates with tubular and planar arrangements: Case study of halloysite and kaolinite Asgar, Hassnain; Jin, Jiaqi; Miller, Jan Colloids and Surfaces A: Physicochemical and Engineering Aspects, Vol. 613 https://doi.org/10.1016/j.colsurfa.2020.126106	journal	March 2021
CaO carbonation kinetics determined using micro-fluidized bed thermogravimetric analysis Li, Ye; Li, Zhenshan; Wang, Hui Fuel, Vol. 264 https://doi.org/10.1016/j.fuel.2019.116823	journal	March 2020
Role of particle size on the multicycle calcium looping activity of limestone for thermochemical energy storage Durán-Martín, Jonatan D.; Sánchez Jimenez, Pedro E.; Valverde, José M. Journal of Advanced Research, Vol. 22 https://doi.org/10.1016/j.jare.2019.10.008	journal	March 2020
Performance of Na2CO3-CaO sorbent in sorption-enhanced steam methane reforming Santos, Dyovani Bruno Lima; Oliveira, Ana Caroline Pereira; Hori, Carla Eponina Journal of CO2 Utilization, Vol. 51 https://doi.org/10.1016/j.jcou.2021.101634	journal	September 2021
Theoretical approaches in hot CO2 capture using modified CaO-based sorbents: Review Tiwary, Shishir; Bhaumik, Soubhik Kumar Journal of CO2 Utilization, Vol. 57 https://doi.org/10.1016/j.jcou.2021.101875	journal	March 2022
The effect of the Li:Na molar ratio on the structural and sorption properties of mixed zirconates for CO2 capture at high temperature Peltzer, Diana; Múnera, John; Cornaglia, Laura Journal of Environmental Chemical Engineering, Vol. 7, Issue 2 https://doi.org/10.1016/j.jece.2019.102927	journal	April 2019
The calcium looping cycle for large-scale CO2 capture Blamey, J.; Anthony, E. J.; Wang, J. Progress in Energy and Combustion Science, Vol. 36, Issue 2 https://doi.org/10.1016/j.pecs.2009.10.001	journal	April 2010
Reactivity of calcined cement raw meals for carbonation Plou, J.; Martínez, I.; Grasa, G. Powder Technology, Vol. 354 https://doi.org/10.1016/j.powtec.2019.05.084	journal	September 2019
Detailed modeling of sorptive and textural properties of CaO-based sorbents with various porous structures Bazaikin, Ya. V.; Malkovich, E. G.; Prokhorov, D. I. Separation and Purification Technology, Vol. 255 https://doi.org/10.1016/j.seppur.2020.117746	journal	January 2021
CaCO ₃ Crystallite Evolution during CaO Carbonation: Critical Crystallite Size and Rate Constant Measurement by In-Situ Synchrotron Radiation X-ray Powder Diffraction Biasin, A.; Segre, C. U.; Strumendo, M. Crystal Growth & Design, Vol. 15, Issue 11 https://doi.org/10.1021/acs.cgd.5b00563	journal	October 2015
CO₂ Capture at Medium to High Temperature Using Solid Oxide-Based Sorbents: Fundamental Aspects, Mechanistic Insights, and Recent Advances Dunstan, Matthew T.; Donat, Felix; Bork, Alexander H. Chemical Reviews, Vol. 121, Issue 20 https://doi.org/10.1021/acs.chemrev.1c00100	journal	August 2021
Thermokinetic Investigations of High Temperature Carbon Capture Using a Coal Fly Ash Doped Sorbent Sreenivasulu, Bolisetty; Sreedhar, I.; Venugopal, A. Energy & Fuels, Vol. 31, Issue 6 https://doi.org/10.1021/acs.energyfuels.7b00629	journal	June 2017
Synthesis of Sintering-Resistant Sorbents for CO ₂ Capture Liu, Wenqiang; Feng, Bo; Wu, Yueqin Environmental Science & Technology, Vol. 44, Issue 8 https://doi.org/10.1021/es903436v	journal	March 2010
Calcium oxide sintering in atmospheres containing water and carbon dioxide Borgwardt, Robert H. Industrial & Engineering Chemistry Research, Vol. 28, Issue 4 https://doi.org/10.1021/ie00088a019	journal	April 1989
Sorption-Enhanced Hydrogen Production: A Review Harrison, Douglas P. Industrial & Engineering Chemistry Research, Vol. 47, Issue 17 https://doi.org/10.1021/ie800298z	journal	September 2008
Calcium oxides of high reactivity Beruto, Dario; Searcy, Alan W. Nature, Vol. 263, Issue 5574 https://doi.org/10.1038/263221a0	journal	September 1976
Effect of distribution patterns of refractory overlayers on cyclic high temperature CO₂ capture using waste oyster shell Qin, Kun; Wang, TsingHai; Huang, Jin-Chiang RSC Advances, Vol. 6, Issue 100 https://doi.org/10.1039/C6RA20500C	journal	January 2016
Novel aqueous amine looping approach for the direct capture, conversion and storage of CO ₂ to produce magnesium carbonate Liu, Meishen; Asgar, Hassnain; Seifert, Soenke Sustainable Energy & Fuels, Vol. 4, Issue 3 https://doi.org/10.1039/C9SE00316A	journal	January 2020
Dynamics of phase transitions in Na₂TiO₃ and its possible utilization as a CO₂ sorbent: a critical analysis Blanco, Maria Valeria; Abdala, Paula Macarena; Gennari, Fabiana Reaction Chemistry & Engineering, Vol. 6, Issue 10 https://doi.org/10.1039/D1RE00125F	journal	January 2021
Use of the Langmuir method for kinetic studies of decomposition reactions: calcite (CaCO3) Beruto, Dario; Searcy, Alan W. Journal of the Chemical Society, Faraday Transactions 1: Physical Chemistry in Condensed Phases, Vol. 70, Issue 0 https://doi.org/10.1039/f19747002145	journal	January 1974
Origin of the scattering peak in microemulsions Teubner, M.; Strey, R. The Journal of Chemical Physics, Vol. 87, Issue 5 https://doi.org/10.1063/1.453006	journal	September 1987
The Scherrer Formula for X-Ray Particle Size Determination Patterson, A. L. Physical Review, Vol. 56, Issue 10 https://doi.org/10.1103/PhysRev.56.978	journal	November 1939
Small-angle scattering from three-phase samples: application to coal undergoing an extraction process Ciccariello, Salvino; Riello, Pietro Journal of Applied Crystallography, Vol. 40, Issue 2 https://doi.org/10.1107/S002188980700564X	journal	March 2007
A versatile sample-environment cell for non-ambient X-ray scattering experiments Chupas, Peter J.; Chapman, Karena W.; Kurtz, Charles Journal of Applied Crystallography, Vol. 41, Issue 4 https://doi.org/10.1107/S0021889808020165	journal	July 2008
Irena : tool suite for modeling and analysis of small-angle scattering Ilavsky, Jan; Jemian, Peter R. Journal of Applied Crystallography, Vol. 42, Issue 2 https://doi.org/10.1107/S0021889809002222	journal	February 2009
Ultra-small-angle X-ray scattering at the Advanced Photon Source Ilavsky, Jan; Jemian, Pete R.; Allen, Andrew J. Journal of Applied Crystallography, Vol. 42, Issue 3 https://doi.org/10.1107/S0021889809008802	journal	April 2009
Experimental setup for in situ X-ray SAXS/WAXS/PDF studies of the formation and growth of nanoparticles in near- and supercritical fluids Becker, Jacob; Bremholm, Martin; Tyrsted, Christoffer Journal of Applied Crystallography, Vol. 43, Issue 4 https://doi.org/10.1107/S0021889810014688	journal	May 2010
Nika : software for two-dimensional data reduction Ilavsky, Jan Journal of Applied Crystallography, Vol. 45, Issue 2 https://doi.org/10.1107/S0021889812004037	journal	March 2012
Scattering from a multiphase system Goodisman, J.; Brumberger, H. Journal of Applied Crystallography, Vol. 4, Issue 5 https://doi.org/10.1107/S0021889871007192	journal	October 1971
Scherrer after sixty years: A survey and some new results in the determination of crystallite size Langford, J. I.; Wilson, A. J. C. Journal of Applied Crystallography, Vol. 11, Issue 2 https://doi.org/10.1107/S0021889878012844	journal	April 1978
High-resolution small-angle X-ray scattering camera for anomalous scattering Long, G. G.; Jemian, P. R.; Weertman, J. R. Journal of Applied Crystallography, Vol. 24, Issue 1 https://doi.org/10.1107/S0021889890009256	journal	February 1991
Approximations Leading to a Unified Exponential/Power-Law Approach to Small-Angle Scattering Beaucage, G. Journal of Applied Crystallography, Vol. 28, Issue 6 https://doi.org/10.1107/S0021889895005292	journal	December 1995
Small-Angle Scattering from Polymeric Mass Fractals of Arbitrary Mass-Fractal Dimension Beaucage, G. Journal of Applied Crystallography, Vol. 29, Issue 2 https://doi.org/10.1107/S0021889895011605	journal	April 1996
The Nature of CaO Produced by Calcite Powder Decomposition in Vacuum and in CO2 Ewing, Jay; Beruto, Dario; Searcy, Alan W. Journal of the American Ceramic Society, Vol. 62, Issue 11-12 https://doi.org/10.1111/j.1151-2916.1979.tb12736.x	journal	November 1979
Characterization of the Porous CaO Particles Formed by Decomposition of CaCO3 and Ca(OH)2 in Vacuum Beruto, Dario; Barco, Luigi; Searcy, Alan W. Journal of the American Ceramic Society, Vol. 63, Issue 7-8 https://doi.org/10.1111/j.1151-2916.1980.tb10208.x	journal	July 1980
Surface Areas and Morphologies of CaO Produced by Decomposition of Large CaCO3 Crystals in Vacuum Powell, Elizabeth K.; Searcy, Alan W. Journal of the American Ceramic Society, Vol. 65, Issue 3 https://doi.org/10.1111/j.1151-2916.1982.tb10395.x	journal	March 1982
Rearrangement of Porous CaO Aggregates During Calcite Decomposition in Vacuum Beruto, Dario; Barco, Luigi; Searcy, Alan W. Journal of the American Ceramic Society, Vol. 66, Issue 12 https://doi.org/10.1111/j.1151-2916.1983.tb11008.x	journal	December 1983
A Twin Fluid-Bed Reactor for Removal of CO2 from Combustion Processes Shimizu, T.; Hirama, T.; Hosoda, H. Chemical Engineering Research and Design, Vol. 77, Issue 1 https://doi.org/10.1205/026387699525882	journal	January 1999
Thermal decomposition of calcite: Mechanisms of formation and textural evolution of CaO nanocrystals Rodriguez-Navarro, C.; Ruiz-Agudo, E.; Luque, A. American Mineralogist, Vol. 94, Issue 4 https://doi.org/10.2138/am.2009.3021	journal	April 2009
Phase Evolution and Textural Changes during the Direct Conversion and Storage of CO2 to Produce Calcium Carbonate from Calcium Hydroxide Liu, Meishen; Gadikota, Greeshma Geosciences, Vol. 8, Issue 12 https://doi.org/10.3390/geosciences8120445	journal	November 2018

Similar Records

Analysis of textural properties of CaO-based CO₂ sorbents by ex-situ USAXS

Journal Article · Wed Jul 25 20:00:00 EDT 2018 · Chemical Engineering Journal · OSTI ID:1491801

An in situ USAXS–SAXS–WAXS study of precipitate size distribution evolution in a model Ni-based alloy

Journal Article · Mon May 29 20:00:00 EDT 2017 · Journal of Applied Crystallography (Online) · OSTI ID:1366390

Related Subjects

CO2 solid sorbents
SAXS models
multi-texture systems
porous materials
solid decompositions

A novel SAXS model for multi-texture systems: application to CaCO3 calcination using in-situ USAXS-SAXS-WAXS

Citation Formats

References (59)

Similar Records

Related Subjects

A novel SAXS model for multi-texture systems: application to CaCO₃ calcination using in-situ USAXS-SAXS-WAXS