Time-resolved GISAXS and cryo-microscopy characterization of block copolymer membrane formation

Handle URI:
http://hdl.handle.net/10754/563422
Title:
Time-resolved GISAXS and cryo-microscopy characterization of block copolymer membrane formation
Authors:
Marques, Debora S.; Dorin, Rachel Mika; Wiesner, Ulrich B.; Smilgies, Detlef Matthias; Behzad, Ali Reza; Vainio, Ulla; Peinemann, Klaus-Viktor ( 0000-0003-0309-9598 ) ; Nunes, Suzana Pereira ( 0000-0002-3669-138X )
Abstract:
Time-resolved grazing-incidence small-angle X-ray scattering (GISAXS) and cryo-microscopy were used for the first time to understand the pore evolution by copolymer assembly, leading to the formation of isoporous membranes with exceptional porosity and regularity. The formation of copolymer micelle strings in solution (in DMF/DOX/THF and DMF/DOX) was confirmed by cryo field emission scanning electron microscopy (cryo-FESEM) with a distance of 72 nm between centers of micelles placed in different strings. SAXS measurement of block copolymer solutions in DMF/DOX indicated hexagonal assembly with micelle-to-micelle distance of 84-87 nm for 14-20 wt% copolymer solutions. GISAXS in-plane peaks were detected, revealing order close to hexagonal. The d-spacing corresponding to the first peak in this case was 100-130 nm (lattice constant 115-150 nm) for 17 wt% copolymer solutions evaporating up to 100 s. Time-resolved cryo-FESEM showed the formation of incipient pores on the film surface after 4 s copolymer solution casting with distances between void centers of 125 nm. © 2014 Elsevier Ltd. All rights reserved.
KAUST Department:
Physical Sciences and Engineering (PSE) Division; Materials Science and Engineering Program; Imaging and Characterization Core Lab; Biological and Environmental Sciences and Engineering (BESE) Division; Environmental Science and Engineering Program; Water Desalination and Reuse Research Center (WDRC); Advanced Nanofabrication, Imaging and Characterization Core Lab; Advanced Membranes and Porous Materials Research Center; Chemical and Biological Engineering Program; Core Labs; Nanostructured Polymeric Membrane Lab
Publisher:
Elsevier BV
Journal:
Polymer
Issue Date:
Mar-2014
DOI:
10.1016/j.polymer.2013.11.010
Type:
Article
ISSN:
00323861
Sponsors:
We thank Yibei Gu, Cornell Materials Science, for assistance with the GISAXS measurements at CHESS. CHESS is supported by the National Science Foundation. The authors at Cornell were supported by the National Institutes of Health and General Medical Sciences via NSF award DMR-0936384. SAXS measurements were carried out at the light source DORIS III at DESY, a member of the Helmholtz Association (HGF). We further thank the National Science Foundation (DMR-1104773) for financial support.
Appears in Collections:
Articles; Advanced Membranes and Porous Materials Research Center; Environmental Science and Engineering Program; Advanced Nanofabrication, Imaging and Characterization Core Lab; Physical Sciences and Engineering (PSE) Division; Chemical and Biological Engineering Program; Materials Science and Engineering Program; Water Desalination and Reuse Research Center (WDRC); Biological and Environmental Sciences and Engineering (BESE) Division

Full metadata record

DC FieldValue Language
dc.contributor.authorMarques, Debora S.en
dc.contributor.authorDorin, Rachel Mikaen
dc.contributor.authorWiesner, Ulrich B.en
dc.contributor.authorSmilgies, Detlef Matthiasen
dc.contributor.authorBehzad, Ali Rezaen
dc.contributor.authorVainio, Ullaen
dc.contributor.authorPeinemann, Klaus-Viktoren
dc.contributor.authorNunes, Suzana Pereiraen
dc.date.accessioned2015-08-03T11:51:04Zen
dc.date.available2015-08-03T11:51:04Zen
dc.date.issued2014-03en
dc.identifier.issn00323861en
dc.identifier.doi10.1016/j.polymer.2013.11.010en
dc.identifier.urihttp://hdl.handle.net/10754/563422en
dc.description.abstractTime-resolved grazing-incidence small-angle X-ray scattering (GISAXS) and cryo-microscopy were used for the first time to understand the pore evolution by copolymer assembly, leading to the formation of isoporous membranes with exceptional porosity and regularity. The formation of copolymer micelle strings in solution (in DMF/DOX/THF and DMF/DOX) was confirmed by cryo field emission scanning electron microscopy (cryo-FESEM) with a distance of 72 nm between centers of micelles placed in different strings. SAXS measurement of block copolymer solutions in DMF/DOX indicated hexagonal assembly with micelle-to-micelle distance of 84-87 nm for 14-20 wt% copolymer solutions. GISAXS in-plane peaks were detected, revealing order close to hexagonal. The d-spacing corresponding to the first peak in this case was 100-130 nm (lattice constant 115-150 nm) for 17 wt% copolymer solutions evaporating up to 100 s. Time-resolved cryo-FESEM showed the formation of incipient pores on the film surface after 4 s copolymer solution casting with distances between void centers of 125 nm. © 2014 Elsevier Ltd. All rights reserved.en
dc.description.sponsorshipWe thank Yibei Gu, Cornell Materials Science, for assistance with the GISAXS measurements at CHESS. CHESS is supported by the National Science Foundation. The authors at Cornell were supported by the National Institutes of Health and General Medical Sciences via NSF award DMR-0936384. SAXS measurements were carried out at the light source DORIS III at DESY, a member of the Helmholtz Association (HGF). We further thank the National Science Foundation (DMR-1104773) for financial support.en
dc.publisherElsevier BVen
dc.subjectBlock copolymer assemblyen
dc.subjectMembranesen
dc.subjectTime-resolved GISAXSen
dc.titleTime-resolved GISAXS and cryo-microscopy characterization of block copolymer membrane formationen
dc.typeArticleen
dc.contributor.departmentPhysical Sciences and Engineering (PSE) Divisionen
dc.contributor.departmentMaterials Science and Engineering Programen
dc.contributor.departmentImaging and Characterization Core Laben
dc.contributor.departmentBiological and Environmental Sciences and Engineering (BESE) Divisionen
dc.contributor.departmentEnvironmental Science and Engineering Programen
dc.contributor.departmentWater Desalination and Reuse Research Center (WDRC)en
dc.contributor.departmentAdvanced Nanofabrication, Imaging and Characterization Core Laben
dc.contributor.departmentAdvanced Membranes and Porous Materials Research Centeren
dc.contributor.departmentChemical and Biological Engineering Programen
dc.contributor.departmentCore Labsen
dc.contributor.departmentNanostructured Polymeric Membrane Laben
dc.identifier.journalPolymeren
dc.contributor.institutionDepartment of Material Science and Engineering, Cornell University, Ithaca, NY 14853-1501, United Statesen
dc.contributor.institutionCornell High Energy Synchrotron Source, Cornell University, Ithaca, NY 14853-1501, United Statesen
dc.contributor.institutionHASYLAB at Deutsches Elektronen-Synchrotron (DESY), Notkestr. 85, 22607 Hamburg, Germanyen
kaust.authorMarques, Debora S.en
kaust.authorBehzad, Ali Rezaen
kaust.authorPeinemann, Klaus-Viktoren
kaust.authorNunes, Suzana Pereiraen
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