skip to main content
OSTI.GOV title logo U.S. Department of Energy
Office of Scientific and Technical Information

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

Journal Article · · Chemical Engineering Journal
 [1];  [2];  [3];  [1]
  1. Univ. of Padova, Padova (Italy). Dept. of Industrial Engineering
  2. Argonne National Lab. (ANL), Argonne, IL (United States). X-ray Science Division
  3. Illinois Inst. of Technology, Chicago, IL (United States). Dept. of Physics & CSRRI
+ Show Author Affiliations

Here in this work, the micro-textural properties of CaO-based CO2 sorbents prepared in a thermo-gravimetric reactor were investigated by ex situ synchrotron-based Small Angle X-ray Scattering (SAXS), Ultra Small Angle X-ray Scattering (USAXS) and Wide Angle X-ray Scattering (WAXS). Six sorbent samples were produced by calcination in vacuum at different temperatures and durations of the heating step; additionally, four partially carbonated samples were produced, after calcination in vacuum, at different CaO conversions. The scattering intensity profiles were analyzed by means of the Unified Fit model. Bimodal pore size distributions (micro-pores and meso-pores) were identified and the micro-textural properties (porosity, specific surface and pore radius of gyration) of each of the two pore populations were quantified both for the calcined and for the carbonated samples. The micro-textural properties of a few calcined samples were compared with N2-adsorption measurements. For each pore population, the trends of porosity, specific surface and pore radius of gyration, in addition to the pore number density and sphericity factor, were obtained versus time during the calcination and versus the CaO conversion during the carbonation. The relevance of micro-pores with respect to macro-pores was assessed both as far as the porosity impact on the CO2 capture capacity and as far as the specific surface impact on the carbonation kinetics. For the calcined samples, the micro-textural properties of a partially calcined sample were compared with those of the completely calcined samples, and pore correlation distances were determined. Finally, for the carbonated samples, the specific surface per unit of particle volume results linearly dependent on the CaO conversion and, if expressed per unit of mass of unreacted CaO, does not change significantly for most of the CaO carbonation.

Research Organization:
Argonne National Lab. (ANL), Argonne, IL (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
Grant/Contract Number:
AC02-06CH11357
OSTI ID:
1491801
Alternate ID(s):
OSTI ID: 1702993
Journal Information:
Chemical Engineering Journal, Vol. 355; ISSN 1385-8947
Publisher:
ElsevierCopyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 17 works
Citation information provided by
Web of Science

References (62)

Determination of the Critical Product Layer Thickness in the Reaction of CaO with CO 2 journal June 2005
Studies of Ca-based high temperature sorbents for CO2 capture journal January 2013
The reversibility of the reaction CaCO3 ⇄ CaO+CO2 journal October 1973
Approximations Leading to a Unified Exponential/Power-Law Approach to Small-Angle Scattering journal December 1995
Particle size distributions from small-angle scattering using global scattering functions journal July 2004
Experimental setup for in situ X-ray SAXS/WAXS/PDF studies of the formation and growth of nanoparticles in near- and supercritical fluids journal May 2010
A SAXS-WAXS study of the endothermic transitions in amorphous or supercooled liquid itraconazole journal November 2016
Characterization of the Porous CaO Particles Formed by Decomposition of CaCO3 and Ca(OH)2 in Vacuum journal July 1980
Rearrangement of Porous CaO Aggregates During Calcite Decomposition in Vacuum journal December 1983
A random pore model for fluid-solid reactions: II. Diffusion and transport effects journal March 1981
Analysis of distributed pore closure in gas-solid reactions journal April 1985
A random pore model for fluid-solid reactions: I. Isothermal, kinetic control journal May 1980
Effect of the product layer on the kinetics of the CO2-lime reaction journal January 1983
Unified treatment of structural effects in fluid-solid reactions journal March 1983
Investigation of CaO–CO2 reaction kinetics by in-situ XRD using synchrotron radiation journal May 2015
CaCO 3 Crystallite Evolution during CaO Carbonation: Critical Crystallite Size and Rate Constant Measurement by In-Situ Synchrotron Radiation X-ray Powder Diffraction journal October 2015
The calcium looping cycle for large-scale CO2 capture journal April 2010
Sintering of nascent calcium oxide journal January 1989
Calcium oxide sintering in atmospheres containing water and carbon dioxide journal April 1989
Synthesis of Highly Efficient, Ca-Based, Al2O3-Stabilized, Carbon Gel-Templated CO2 Sorbents journal May 2012
Small-angle X-ray scattering analysis of porous powders of CaCO 3 journal August 2012
A versatile sample-environment cell for non-ambient X-ray scattering experiments journal July 2008
The calcium looping cycle for CO2 capture from power generation, cement manufacture and hydrogen production journal June 2011
Enhanced hydrogen production from biomass with in situ carbon dioxide capture using calcium oxide sorbents journal January 2008
Application of the random pore model to the carbonation cyclic reaction journal May 2009
Sorption-Enhanced Hydrogen Production: A Review journal September 2008
CRC Handbook of Chemistry and Physics, 76th edition journal July 1996
Characterization of porous materials using combined small-angle X-ray and neutron scattering techniques journal September 2011
Characterization of Complex Thermal Barrier Deposits Pore Microstructures by a Combination of Imaging, Scattering, and Intrusion Techniques journal July 2009
Irena : tool suite for modeling and analysis of small-angle scattering journal February 2009
Ultra-small-angle X-ray scattering at the Advanced Photon Source journal April 2009
Ultra-Small-Angle X-ray Scattering Instrument at the Advanced Photon Source: History, Recent Development, and Current Status journal October 2012
An iterative method of slit-correcting small angle X-ray data journal August 1967
Dehydration Effect on the Pore Size, Porosity, and Fractal Parameters of Shale Rocks: Ultrasmall-Angle X-ray Scattering Study journal October 2014
A rate equation theory for the pore size distribution of calcined CaCO 3 in calcium looping journal January 2016
Synthesis of Sintering-Resistant Sorbents for CO 2 Capture journal March 2010
High-resolution small-angle X-ray scattering camera for anomalous scattering journal February 1991
Novel model for the sintering of ceramics with bimodal pore size distributions: Application to the sintering of lime journal August 2016
On the modeling of the co 2 -catalyzed sintering of calcium oxide journal March 2017
Economics of CO 2 Capture Using the Calcium Cycle with a Pressurized Fluidized Bed Combustor journal March 2007
Investigation of the Enhanced Water Gas Shift Reaction Using Natural and Synthetic Sorbents for the Capture of CO 2 journal September 2009
Characterization of accessible and inaccessible pores in microporous carbons by a combination of adsorption and small angle neutron scattering journal July 2012
The Calcium-Looping technology for CO2 capture: On the important roles of energy integration and sorbent behavior journal January 2016
Die Röntgenkleinwinkelstreuung von dichtgepackten kolloiden Systemen: I. Teil journal November 1951
Calcium Looping Process (CLP) for Enhanced Noncatalytic Hydrogen Production with Integrated Carbon Dioxide Capture journal August 2010
Thermal decomposition of calcite: Mechanisms of formation and textural evolution of CaO nanocrystals journal April 2009
A Twin Fluid-Bed Reactor for Removal of CO2 from Combustion Processes journal January 1999
Reporting physisorption data for gas/solid systems with special reference to the determination of surface area and porosity (Recommendations 1984) journal January 1985
Mathematical modelling of gas-solid reactions with solid product journal January 1985
Analysis of the small-angle intensity scattered by a porous and granular medium journal March 2003
Phenomenological model of anisotropic peak broadening in powder diffraction journal April 1999
Solution of PBE by MOM in finite size domains journal May 2008
Solution of Population Balance Equations by the Finite Size Domain Complete Set of Trial Functions Method of Moments (FCMOM) for Inhomogeneous Systems journal April 2010
The effect of CaO sintering on cyclic CO2 capture in energy systems journal January 2007
A discrete-pore-size-distribution-based gas–solid model and its application to the CaO+CO2 reaction journal January 2008
Determination of intrinsic rate constants of the CaO–CO2 reaction journal January 2008
Review of hydrogen-enriched gas production from steam gasification of biomass: The prospect of CaO-based chemical looping gasification journal February 2014
Volume, Shape, and Roundness of Quartz Particles journal April 1935
Note on a Method of Determining the Distribution of Pore Sizes in a Porous Material journal April 1921
Glassy Carbon as an Absolute Intensity Calibration Standard for Small-Angle Scattering journal August 2009
Investigation on a novel CaO–Y2O3 sorbent for efficient CO2 mitigation journal May 2014
Nano CaO grain characteristics and growth model under calcination journal November 2011

Cited By (1)

Phase Evolution and Textural Changes during the Direct Conversion and Storage of CO2 to Produce Calcium Carbonate from Calcium Hydroxide journal November 2018

Figures / Tables (29)

Table 1(p. 22)table Table 1
Table 2(p. 22)table Table 2
Table 3(p. 22)table Table 3
Table 4(p. 23)table Table 4
Table 5(p. 23)table Table 5
Table 6(p. 23)table Table 6
Table 7(p. 23)table Table 7
Figure 1(p. 24)figure Figure 1
Table 8(p. 24)table Table 8
Figure 2a(p. 25)figure Figure 2a
Figure 2b(p. 26)figure Figure 2b
Figure 2c(p. 26)figure Figure 2c
Figure 2d(p. 27)figure Figure 2d
Figure 3(p. 27)figure Figure 3
Figure 4(p. 28)figure Figure 4
Figure 5(p. 29)figure Figure 5
Figure 6(p. 30)figure Figure 6
Figure 7(p. 31)figure Figure 7
Figure 8(p. 32)figure Figure 8
Figure 9(p. 33)figure Figure 9
Figure 10(p. 34)figure Figure 10
Figure 11(p. 35)figure Figure 11
Figure 12(p. 36)figure Figure 12
Figure 13(p. 37)figure Figure 13
Figure 14(p. 38)figure Figure 14
Figure 15(p. 39)figure Figure 15
Figure 16(p. 40)figure Figure 16
Figure 17(p. 41)figure Figure 17
Figure 18(p. 42)figure Figure 18

Similar Records

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 · OSTI ID:1491801
+1 more
SO{sub 2} Retention by CaO-Based Sorbent Spent in CO{sub 2} Looping Cycles
Journal Article · Wed Jul 15 00:00:00 EDT 2009 · Industrial and Engineering Chemistry Research · OSTI ID:1491801
Comparison of different natural sorbents for removing CO{sub 2} from combustion gases, as studied in a bench-scale fluidized bed
Journal Article · Sat Nov 15 00:00:00 EST 2008 · Energy and Fuels · OSTI ID:1491801
+3 more

Related Subjects

36 MATERIALS SCIENCE
42 ENGINEERING
CaO-based CO2 sorbents
Synchrotron radiation
X-ray small angle scattering
Micro-textural properties
Bimodal pore size distributions
Reaction model