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  3D Micromachined Polyimide Mixing Devices for in Situ X-ray Imaging of Solution-Based Block Copolymer Phase Transitions

Vakili, M., Merkens, S., Gao, Y., Gwozdz, P. V., Vasireddi, R., Sharpnack, L., et al. (2019). 3D Micromachined Polyimide Mixing Devices for in Situ X-ray Imaging of Solution-Based Block Copolymer Phase Transitions. Langmuir, 35(32), 10435-10445. doi:10.1021/acs.langmuir.9b00728.

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Item Permalink: http://hdl.handle.net/21.11116/0000-0004-9049-7 Version Permalink: http://hdl.handle.net/21.11116/0000-0004-904A-6
Genre: Journal Article


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Vakili, M.1, Author
Merkens, S.1, Author
Gao, Y.1, 2, Author              
Gwozdz, P. V.3, Author
Vasireddi, R.1, Author
Sharpnack, L.4, Author
Meyer, A.5, Author
Blick, R. H.3, 6, Author
Trebbin, M.1, 7, Author
1Centre for Ultrafast Imaging (CUI) University of Hamburg, ou_persistent22              
2International Max Planck Research School for Ultrafast Imaging & Structural Dynamics (IMPRS-UFAST), Max Planck Institute for the Structure and Dynamics of Matter, Max Planck Society, ou_2266714              
3Center for Hybrid Nanostructures (CHyN), University of Hamburg, ou_persistent22              
4Beamline ID02, European Synchrotron Radiation Facility (ESRF), ou_persistent22              
5Institute for Physical Chemistry, University of Hamburg, ou_persistent22              
6Department of Materials Sciences and Engineering, University of Wisconsin- Madison, ou_persistent22              
7Department of Chemistry, BioXFEL, RENEW and Hauptman-Woodward Medical Research Institute (HWI), State University of New York at Buffalo, ou_persistent22              


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 Abstract: Advances in modern interface- and material sciences often rely on the understanding of a system’s structure–function relationship. Designing reproducible experiments that yield in situ time-resolved structural information at fast time scales is therefore of great interest, e.g., for better understanding the early stages of self-assembly or other phase transitions. However, it can be challenging to accurately control experimental conditions, especially when samples are only available in small amounts, prone to agglomeration, or if X-ray compatibility is required. We address these challenges by presenting a microfluidic chip for triggering dynamics via rapid diffusive mixing for in situ time-resolved X-ray investigations. This polyimide/Kapton-only-based device can be used to study the structural dynamics and phase transitions of a wide range of colloidal and soft matter samples down to millisecond time scales. The novel multiangle laser ablation three-dimensional (3D) microstructuring approach combines, for the first time, the highly desirable characteristics of Kapton (high X-ray stability with low background, organic solvent compatibility) with a 3D flow-focusing geometry that minimizes mixing dispersion and wall agglomeration. As a model system, to demonstrate the performance of these 3D Kapton microfluidic devices, we selected the non-solvent-induced self-assembly of biocompatible and amphiphilic diblock copolymers. We then followed their structural evolution in situ at millisecond time scales using on-the-chip time-resolved small-angle X-ray scattering under continuous-flow conditions. Combined with complementary results from 3D finite-element method computational fluid dynamics simulations, we find that the nonsolvent mixing is mostly complete within a few tens of milliseconds, which triggers initial spherical micelle formation, while structural transitions into micelle lattices and their deswelling only occur on the hundreds of milliseconds to second time scale. These results could have an important implication for the design and formulation of amphiphilic polymer nanoparticles for industrial applications and their use as drug-delivery systems in medicine.


Language(s): eng - English
 Dates: 2019-07-152019-03-122019-07-182019-08-13
 Publication Status: Published in print
 Pages: 11
 Publishing info: -
 Table of Contents: -
 Rev. Method: Peer
 Identifiers: DOI: 10.1021/acs.langmuir.9b00728
 Degree: -



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Project name : The authors are grateful to the ESRF for providing synchrotron beam time and thank Theyencheri Narayanan and his team at the ID02 beamline for technical assistance. Furthermore, they thank Stephan Fleig and Bernd Krambeer from the mechanical workshop of the University of Hamburg for technical support in the fabrication of the sample holder. Tobias Gerling and Robert Seher (University of Hamburg) are thanked for fruitful discussions on microfluidic device and sample holder designs. Diana Monteiro and Florian Kopf (University of Hamburg) are thanked for fruitful discussions on fluid dynamic simulations. Further, they thank Matthew Derry (University of Sheffield) for very helpful discussions on SAXS data modeling. Moreover, the authors express their gratitude to Claudia Leopold (University of Hamburg) for enabling pycnometry measurements; the NMR team of the Institute for Organic Chemistry (University of Hamburg); Felix Scheliga, Stefen Bleck, and Katrin Rehmke for GPC and DSC measurements; as well as Sven Bettermann for access to the DLS Zetasizer. They also thank Yannig Gicquel (University of Hamburg) and Michael Heymann (Max Planck Institute of Biochemistry, Martinsried) for fruitful discussions about surface functionalization. This work was supported by the Cluster of Excellence “The Hamburg Centre for Ultrafast Imaging” of the Deutsche Forschungsgemeinschaft (DFG) - EXC 1074 - project ID 194651731.
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Source 1

Title: Langmuir
  Abbreviation : Langmuir
Source Genre: Journal
Publ. Info: Columbus, OH : American Chemical Society
Pages: - Volume / Issue: 35 (32) Sequence Number: - Start / End Page: 10435 - 10445 Identifier: ISSN: 0743-7463
CoNE: https://pure.mpg.de/cone/journals/resource/954925541194