Skip to main content
U.S. Department of Energy
Office of Scientific and Technical Information

Multilevel Morphology of Complex Nanoporous Materials

Journal Article · · Langmuir
This work exploits gas adsorption and small-angle X-ray scattering (SAXS) to determine the morphology of complex nanoporous materials. We resolve multiple classes of porosity including previously undetected large-scale texture that significantly compromises the canonical interpretation of gas adsorption. Specifically, a UVM-7 class mesoporous silica was synthesized that has morphological features on three length scales: macropores due to packing of 150 nm globules, 1.9 nm radius spherical mesopores inside the globules, and >7 nm pockets on and between the globules. The total and external surface areas, as well as the mesopore volume, were determined using gas adsorption (αs-plot) and SAXS. A new approach was applied to the SAXS data using multilevel fitting to determine the surface areas on multiple length scales. The SAXS analysis code is applicable to any two-phase system and is freely available to the public. The total surface area determined by SAXS was 12% greater than that obtained by gas adsorption. The macropore interfacial area, however, is only 30% of the external surface area determined by the αs-plot. The overestimation of the external surface area by the αs-plot method is attributed to capillary condensation in nanoscale surface irregularities. Here, the discrepancy is resolved assuming that the macropore–globule interfaces harbor fractally distributed nooks and crannies, which lead to gas adsorption at pressures above the mesopore filling pressure.
Research Organization:
Argonne National Laboratory (ANL), Argonne, IL (United States)
Sponsoring Organization:
NSF
OSTI ID:
1455249
Journal Information:
Langmuir, Journal Name: Langmuir Journal Issue: 23 Vol. 34; ISSN 0743-7463
Publisher:
American Chemical SocietyCopyright Statement
Country of Publication:
United States
Language:
ENGLISH

References (31)

A Stable and Highly Active Hybrid Mesoporous Solid Acid Catalyst journal August 2005
A comprehensive analysis of the BET area for nanoporous materials journal August 2017
Commercial applications of porous Si: optical filters and components journal May 2007
Characterization of Porous Solids and Powders: Surface Area, Pore Size and Density book September 2004
Ultra-Small-Angle X-ray Scattering Instrument at the Advanced Photon Source: History, Recent Development, and Current Status journal October 2012
Origin of porosity in resorcinol-formaldehyde aerogels journal June 1995
Monitoring of the structure of siliceous mesoporous molecular sieves tailored using different synthesis conditions journal November 1997
The use of nitrogen adsorption for the characterisation of porous materials journal August 2001
Mesoporous silica nanoparticles as controlled release drug delivery and gene transfection carriers journal August 2008
Characterization of porous materials using combined small-angle X-ray and neutron scattering techniques journal September 2011
Control of ordered structure and morphology of large-pore periodic mesoporous organosilicas by inorganic salt journal April 2006
Fabrication and structural analysis of mesoporous silica–titania for environmental purification journal December 2013
Bases for the synthesis of nanoparticulated silicas with bimodal hierarchical porosity journal August 2006
Expanding the atrane route: Generalized surfactant-free synthesis of mesoporous nanoparticulated xerogels journal May 2008
Sol–Gel with Phase Separation. Hierarchically Porous Materials Optimized for High-Performance Liquid Chromatography Separations journal September 2007
Gas Adsorption Characterization of Ordered Organic−Inorganic Nanocomposite Materials journal October 2001
Structure of Arylene-Bridged Polysilsesquioxane Xerogels and Aerogels journal April 2004
On the Controllable Soft-Templating Approach to Mesoporous Silicates journal July 2007
Pore Size Determination of MCM-51 Mesoporous Materials by means of 1H NMR Spectroscopy, N2 adsorption, and HREM. A Preliminary Study journal April 1995
Characterization of Pore Size Distributions of Mesoporous Materials from Adsorption Isotherms journal October 2000
Pore Size Determination in Ordered Mesoporous Materials Using Powder X-ray Diffraction journal August 2013
An isotherm equation for adsorption on fractal surfaces of heterogeneous porous materials journal November 1989
Adsorption-Induced Deformation of Mesoporous Solids: Macroscopic Approach and Density Functional Theory journal June 2011
Structural Characterization of MCM-41 over a Wide Range of Length Scales journal March 1999
Standard Nitrogen Adsorption Data for Characterization of Nanoporous Silicas journal August 1999
Silica-based powders and monoliths with bimodal pore systemsElectronic supplementary information (ESI) available: UV–Vis spectrum of sample 3. See http://www.rsc.org/suppdata/cc/b1/b110883b/ journal February 2002
Density functional theories and molecular simulations of adsorption and phase transitions in nanopores journal June 2001
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
Interpretation of small-angle scattering curves proportional to a negative power of the scattering vector journal October 1982
Fractal Pores or a Distribution of Pore sizes: Alternative Interpretations of Power-Law Small-Angle Scattering journal January 1986

Cited By (1)

Insight into the nanostructure of anisotropic cellulose aerogels upon compression journal January 2019

Similar Records

SANS coupled with fluid invasion approaches for characterization of overall nanopore structure and mesopore connectivity of organic-rich marine shales in China
Journal Article · Mon Nov 18 19:00:00 EST 2019 · International Journal of Coal Geology · OSTI ID:1779160

Controlled release of ibuprofen by meso–macroporous silica
Journal Article · Fri Feb 14 23:00:00 EST 2014 · Journal of Solid State Chemistry · OSTI ID:22274222

Development of mesopores in superfine grain graphite neutron-irradiated at high fluence
Journal Article · Tue Oct 02 20:00:00 EDT 2018 · Carbon · OSTI ID:1479761