Novel lift-off technique for Transmission Electron Microscopy imaging of block copolymer films

Roache, Fergus J M; Radjainia, Mazdak; Williams, David E.; Gerrard, Juliet A.; Travaš-Sejdić, Jadranka; Malmström, Jenny

doi:10.1016/j.ultramic.2014.12.004

Cited by 6 publications

(9 citation statements)

References 20 publications

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“…AFM surveys only the surface of the material, and thus it is not clear if the observed structure percolates through the entire film. A recently reported process of floating films from a carbon-coated mica surface was employed to collect films for TEM and compare the image of the surface from AFM with the image through the film . Films of the SIL polymers were spin-coated onto the carbon-coated mica surface and SVA with THF was performed for 2–5 min.…”

Section: Resultsmentioning

confidence: 99%

“…The ability of S 0.40 I 0.41 L 0.19 -39 to achieve long-range order on the carbon-coated mica substrates may relate to the surface energy differences. Carbon-coated mica is more hydrophobic than bare mica or native Si and thus will have lower surface energy, more similar to HMDS-modified Si ( E surfSi = 61 mJ/m 2 ; E surf HMDS‑Si = 43 mJ/m 2 ). , The polymer blocks have lower surface energies than the HMDS-modified Si ( E surfPI = 32 mJ/m 2 ; E surfPS ≈ E surfPLA ≈ 40 mJ/m 2 ) . Thus, if the carbon-coated mica surface energy is lower and more “neutral” with respect to the block surface energy, this may improve the ordering and orientation of the domains.…”

Section: Resultsmentioning

confidence: 99%

“…The polymers were then spin-coated onto native silicon oxide, HMDS-modified silicon (HMDS = hexamethyldisilazane), and carbon-coated mica and studied with AFM. The films were also lifted from the carboncoated mica by floating in water 54 and characterized by TEM experiments after selective staining of the PI domains with OsO 4 . In both the bulk and thin film, nonlamellar morphologies were observed.…”

Section: ■ Introductionmentioning

confidence: 99%

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Morphological Consequences of Frustration in ABC Triblock Polymers

Radlauer¹,

Sinturel

Asai

et al. 2016

Macromolecules

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Three poly(styrene)-block-poly(isoprene)-block-poly-(lactide) (PS-b-PI-b-PLA, SIL) triblock terpolymers were synthesized and characterized in the bulk and as thin films. The pronounced incompatibility of the covalently connected PI and PLA led to significant frustration and the tendency to minimize their intermaterial dividing surface area. This resulted in the formation of a core−shell cylinder morphology with exaggerated nonconstant mean curvature from triblock polymers with equal block volume fractions rather than the more typical lamellar morphology. The effect of frustration was magnified in thin films by both confinement and interfacial interactions such that the PI domains became discontinuous. Selfconsistent field theory (SCFT) calculations emphasize that the marked difference in the PS/PI and PI/PLA interaction parameters promotes the formation of nonlamellar morphologies. However, SCFT predicts that lamellar morphology is more stable than the observed cylindrical morphology, demonstrating a limitation that arises from the underlying assumptions.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: ■ Introductionmentioning

confidence: 99%

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Morphological Consequences of Frustration in ABC Triblock Polymers

Radlauer¹,

Sinturel

Asai

et al. 2016

Macromolecules

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“…Carbon coated mica proved a good match of surface chemistry and enabled rapid lift-off in water after solvent annealing. 59 Fig . 5 shows the improved ordering achieved using this method and images of RuO 4 stained films acquired at different relative focus reiterate the increase in spacing and PEO size.…”

Section: Resultsmentioning

confidence: 99%

“…Polymer films were deposited on grids either by dipcoating or by floating films spun coated on carbon coated mica onto the surface of water, from where the films were picked up with the TEM grids. 59 Films were stained with RuO 4 vapour (0.5% RuO 4 in water from Electron Microscopy Sciences, US) or uranyl acetate (Sigma). TEM imaging was performed on an FEI Tecnai 12 electron microscope operated at 120 kV.…”

Section: X-ray Photoelectron Spectroscopymentioning

confidence: 99%

Protein nanorings organized by poly(styrene-block-ethylene oxide) self-assembled thin films

et al. 2015

Self Cite

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This study explores the use of block copolymer self-assembly to organize Lsmα, a protein which forms stable doughnut-shaped heptameric structures. Here, we have explored the idea that 2-D crystalline arrays of protein filaments can be prepared by stacking doughnut shaped Lsmα protein into the poly(ethylene oxide) blocks of a hexagonal microphase-separated polystyrene-b-polyethylene oxide (PS-b-PEO) block copolymer. We were able to demonstrate the coordinated assembly of such a complex hierarchical nanostructure. The key to success was the choice of solvent systems and protein functionalization that achieved sufficient compatibility whilst still promoting assembly. Unambiguous characterisation of these structures is difficult; however AFM and TEM measurements confirmed that the protein was sequestered into the PEO blocks. The use of a protein that assembles into stackable doughnuts offers the possibility of assembling nanoscale optical, magnetic and electronic structures. This study explores the use of block copolymer self-assembly to organize Lsmα, a protein which forms stable doughnut-shaped heptameric structures. Here, we have explored the idea that 2-D crystalline arrays of protein filaments can be prepared by stacking doughnut shaped Lsmα protein into the poly(ethylene oxide) blocks of a hexagonal microphase-separated polystyrene-b-polyethylene oxide (PSb-PEO) block copolymer. We were able to demonstrate the coordinated assembly of such a complex hierarchical nanostructure. The key to success was the choice of solvent systems and protein functionalization that achieved sufficient compatibility whilst still promoting assembly. Unambiguous characterisation of these structures is difficult; however AFM and TEM measurements confirmed that the protein was sequestered into the PEO blocks. The use of a protein that assembles into stackable doughnuts offers the possibility of assembling nanoscale optical, magnetic and electronic structures.

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