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Shaping Macroporous Ceramics: templated synthesis, X-ray tomography and permeability
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). (Materials chemistry)
2011 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Macroporous ceramic materials have found widespread technological application ranging from particulate filters in diesel engines, tissue engineering scaffolds, and as support materials in carbon capture processes. This thesis demonstrates how the pore space of macroporous alumina can be manipulated, analysed in three-dimensions (3D) using visualisation techniques, and functionalised with a CO2-adsorbing material.

A novel method was developed to produce macroporous alumina materials: by combining sacrificial templating with thermally expandable polymeric microspheres and gel-casting of an alumina suspension. This method offers a versatile production of macroporous ceramics in which the level of porosity and the pore size distribution can easily be altered by varying the amount and type of spheres. The permeability to fluid flow could be regulated by controlling the connectivity of the pore space and the size of the smallest constrictions between the pores. Sacrificial templating with particle-coated expandable spheres significantly increased the fraction of isolated pore clusters and reduced both the sizes and the numbers of connections between neighbouring pores, compared to templating with un-coated spheres.

The macroporous alumina materials were characterised with X-ray micro-computed tomography (μ-CT). The 3D data-sets obtained by X-ray μ-CT were used to calculate the spatial variation in porosity, the throat and pore size distributions and to calculate the permeability to fluid flow. The throat and pore size distributions were also able to be accurately quantified in only one extrusion and intrusion cycle with water-based porosimetry; a relatively novel and simple characterisation technique. The pore walls of the macroporous alumina materials were also coated with zeolite films by a colloidal processing technique. The CO2-uptake of the coated alumina materials and of hierarchically porous monoliths of zeolites was evaluated and compared.

Place, publisher, year, edition, pages
Stockholm: Department of Materials and Environmental Chemistry, Stockholm University , 2011. , 60 p.
Keyword [en]
Alumina, ceramic, CO2 capture, colloidal processing, expandable microspheres, gel casting, layer-by-layer, macroporosity, near-net shape, non-destructive evaluation, permeability, porosity, sacrificial templating, X-ray computed tomography
National Category
Chemical Sciences
Research subject
Materials Chemistry
Identifiers
URN: urn:nbn:se:su:diva-54677ISBN: 978-91-7447-180-9 (print)OAI: oai:DiVA.org:su-54677DiVA: diva2:396718
Public defence
2011-03-11, Magnélisalen, Kemiska övningslaboratoriet, Svante Arrhenius väg 16 B, Stockholm, 13:00 (English)
Opponent
Supervisors
Note
As the time of the doctoral defense, the following papers were unpublished and had a status as follows: Paper 2: Submitted. Paper 4: Accepted. Paper 5: Manuscript. Paper 6: Submitted.Available from: 2011-02-17 Created: 2011-02-10 Last updated: 2011-02-11Bibliographically approved
List of papers
1. Three-dimensional structure analysis by X-ray micro-computed tomography of macroporous alumina templated with expandable microspheres
Open this publication in new window or tab >>Three-dimensional structure analysis by X-ray micro-computed tomography of macroporous alumina templated with expandable microspheres
2010 (English)In: Journal of the European Ceramic Society, ISSN 0955-2219, E-ISSN 1873-619X, Vol. 30, no 12, 2547-2554 p.Article in journal (Refereed) Published
Abstract [en]

The three-dimensional (3D) structures of macroporous alumina, produced by a novel method that combines gel casting with expandable polymericmicrospheres as a sacrificial templating material, have been characterised by X-ray micro-computed tomography (µ-CT). The grey-scale intensitytomogram data produced by the X-ray µ-CT was segmented into porous and solid phases and the individual pores were identified. We comparedtwo-dimensional slices of the analysed data with the corresponding scanning electron microscopy images and showed that the structural featuresof the pores were well reproduced in the X-ray µ-CT images. 3D visualisations of the pore structure and the pore network were also shown. Theopen porosity obtained from X-ray µ-CT corresponded well with the porosity derived from mercury porosimetry for pores larger than the voxeldimension (3 µm). The quantitative analysis also yielded information on the spatial variations in porosity and the number of connected neighboursof pores. The 3D data was used to relate the calculated permeability to the open porosity.

Place, publisher, year, edition, pages
Amsterdam, Netherlands: Elsevier, 2010
Keyword
Porosity; X-ray methods; Non-destructive evaluation; Al2O3; Expandable microspheres
National Category
Inorganic Chemistry
Research subject
Materials Chemistry
Identifiers
urn:nbn:se:su:diva-46705 (URN)10.1016/j.jeurceramsoc.2010.05.003 (DOI)000280029400016 ()
Projects
Berzelii center EXSELENT on porous materials are acknowledged
Funder
Swedish Research Council
Available from: 2010-11-26 Created: 2010-11-24 Last updated: 2017-12-12Bibliographically approved
2. Evaluating pore space in macroporous ceramics with water-based porosimetry
Open this publication in new window or tab >>Evaluating pore space in macroporous ceramics with water-based porosimetry
2013 (English)In: Journal of The American Ceramic Society, ISSN 0002-7820, E-ISSN 1551-2916, Vol. 96, no 6, 1916-1922 p.Article in journal (Refereed) Published
Abstract [en]

We show that water-based porosimetry (WBP), a facile, simple, and nondestructive porosimetry technique, accurately evaluates both the pore size distribution and throat size distribution of sacrificially templated macroporous alumina. The pore size distribution and throat size distribution derived from the WBP evaluation in uptake (imbibition) and release (drainage) mode, respectively, were corroborated by mercury porosimetry and X-ray micro-computed tomography (μ-CT). In contrast with mercury porosimetry, the WBP also provided information on the presence of “dead-end pores” in the macroporous alumina.

Keyword
intrusion methods, porous materials, ceramics, x-ray methods, pore volume distribution
National Category
Materials Engineering Ceramics
Research subject
Materials Chemistry
Identifiers
urn:nbn:se:su:diva-54661 (URN)10.1111/jace.12223 (DOI)000320036600041 ()
Note

AuthorCount: 4;

Available from: 2011-02-10 Created: 2011-02-10 Last updated: 2017-12-11Bibliographically approved
3. Gas-filled microspheres as an expandable sacrificial template for direct casting of complex-shaped macroporous ceramics
Open this publication in new window or tab >>Gas-filled microspheres as an expandable sacrificial template for direct casting of complex-shaped macroporous ceramics
2008 (English)In: Journal of the European Ceramic Society, ISSN 0955-2219, E-ISSN 1873-619X, Vol. 28, no 15, 2815-2821 p.Article in journal (Refereed) Published
Abstract [en]

Expandable microspheres have been used as a sacrificial template to produce macroporous ceramic materials by a gel-casting process. The temperature range for the gel-casting process has been tuned to allow the gas-filled polymer spheres to expand prior to the setting of the powder body. It is demonstrated that by controlling the amount and size of the expandable microspheres it is possible to tune and tailor the porosity up to 86% and the pore size distribution from 15 up to 150 mu m. The expandable microspheres add a relatively low amount of organic material that allows rapid and facile burn-out. The temperature-induced expansion of the microspheres and the associated volume increase of the suspension has been used as a simple zero-pressure near-net shaping method to yield complex-shaped macroporous alumina bodies.

Keyword
gel-casting; macroporosity; Al2O3; near-net shape; expandable microspheres
National Category
Natural Sciences
Identifiers
urn:nbn:se:su:diva-15278 (URN)10.1016/j.jeurceramsoc.2008.04.020 (DOI)000259758800001 ()
Available from: 2008-11-26 Created: 2008-11-26 Last updated: 2017-12-13Bibliographically approved
4. Permeability, pore connectivity and critical pore throat control of expandable polymeric sphere templated macroporous alumina
Open this publication in new window or tab >>Permeability, pore connectivity and critical pore throat control of expandable polymeric sphere templated macroporous alumina
2011 (English)In: Acta Materialia, ISSN 1359-6454, E-ISSN 1873-2453, Vol. 59, no 3, 1239-1248 p.Article in journal (Refereed) Published
Abstract [en]

We have regulated the permeability in macroporous alumina materials by manipulating the connectivity of the pore phase and the sizes of the smallest constrictions between connected pores. Templating with particle-coated expandable polymeric spheres (EPS) significantly increased the fraction of isolated pore clusters, and reduced both the sizes and the number of connections with neighboring pores, as determined by three-dimensional evaluation with X-ray micro-computed tomography. The stable particle coating, applied onto the EPS surfaces using polyelectrolyte multilayers, reduced the volume expansion and the coalescence of the EPS at elevated temperatures, which reduced the simulated permeability by as much as two orders of magnitude compared to templating with uncoated EPS in materials of similar porosities. We show that the Katz-Thompson model accurately predicts the permeability for the macroporous alumina materials with porosities of 46-76%. This suggests that the permeability to fluid flow in these materials is governed by the smallest constrictions between connected pores: the critical pore throat diameter.

Keyword
X-ray computed tomography, Permeability, Porous material, Alumina (alpha-Al(2)O(3)), Expandable polymeric spheres
National Category
Inorganic Chemistry
Research subject
Materials Chemistry
Identifiers
urn:nbn:se:su:diva-46708 (URN)10.1016/j.actamat.2010.10.056 (DOI)000286690100038 ()
Available from: 2010-11-24 Created: 2010-11-24 Last updated: 2017-12-12Bibliographically approved
5. Colloidal processing and CO2-capture performance of hierarchically porous Al2O3-zeolite 13X composites
Open this publication in new window or tab >>Colloidal processing and CO2-capture performance of hierarchically porous Al2O3-zeolite 13X composites
2012 (English)In: Journal of Ceramic Science and Technology, ISSN 2190-9385, Vol. 3, no 1, 9-16 p.Article in journal (Refereed) Published
Abstract [en]

Hierarchically porous composites for CO2-capture have been produced by coating the inner walls of foam-like macroporous alumina monoliths, produced by templated synthesis, with microporous zeolite 13X particles. Homogeneous and dense coatings of the particulate adsorbent were obtained when the impregnation process was performed at a pH above 9. At this pH-level the colloidally stable suspensions of the negatively charged zeolite 13X particles could fill all the voids of the highly connected pore space of the alumina supports and attach to the monolith walls, which had been pre-coated with poly(ethylene imine). A CO2-uptake as high as 5 mmol CO2/g zeolite 13X was achieved for alumina-zeolite 13X composites through minimisation of the added inorganic binder, kaolin, to only 3.0 wt% with respect to zeolite content, and through optimisation of the thermal treatment.

Keyword
CO2 uptake, adsorption, zeolite, macroporous, porosity, colloids, dispersions, ceramic, processing
National Category
Materials Chemistry
Research subject
Materials Chemistry
Identifiers
urn:nbn:se:su:diva-54662 (URN)10.4416/JCST2012-00039 (DOI)
Available from: 2011-02-10 Created: 2011-02-10 Last updated: 2017-12-11Bibliographically approved
6. Colloidal processing and CO2 capture performance of sacrificially templated zeolite monoliths
Open this publication in new window or tab >>Colloidal processing and CO2 capture performance of sacrificially templated zeolite monoliths
2012 (English)In: Applied Energy, ISSN 0306-2619, E-ISSN 1872-9118, Vol. 97, 289-296 p.Article in journal (Other academic) Published
Abstract [en]

Sacrificial templating of suspension cast and subsequently thermally treated zeolite monoliths with glassy carbon spheres and fibers yielded zeolite 13X and silicalite-1 monoliths with macroporosities up to 50 vol%. Homogeneous distribution of the macroporosity in hierarchically porous monoliths was obtained by tailoring the surface chemistry of the carbon particles by polyelectrolyte-assisted adsorption of zeolite particles. The effect of amount of kaolin binder and temperature for the thermal treatment on the monoliths strength, surface area and CO2 uptake was studied by diametral compression tests, electron microscopy, X-ray diffraction and gas adsorption. Cyclic adsorption and regeneration measurements showed that zeolite 13X monoliths display a high CO2 uptake while the silicalite-1 monoliths could be regenerated with a relatively low energy penalty.

Keyword
porous, zeolite, 13X, carbon, colloidal processing, adsorbent, CO2 capture, sacrificial templating, kaolin
National Category
Materials Chemistry
Research subject
Materials Chemistry
Identifiers
urn:nbn:se:su:diva-54663 (URN)10.1016/j.apenergy.2011.12.064 (DOI)000307196000034 ()
Conference
Third International Conference on Applied Energy, May 16-18, 2011, Perugia, Italy
Available from: 2011-02-10 Created: 2011-02-10 Last updated: 2017-12-11Bibliographically approved

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