Self-assembly of maltoheptaose-b-PMMA block copolymer systems: 10 nm Resolution in thin film and bulk states

Noronha, Carolina Montanheiro; Otsuka, Issei; Bouilhac, Cécile; Rochas, C.; Barreto, Pedro Luiz Manique

doi:10.1016/j.carbpol.2017.04.029

Cited by 7 publications

(5 citation statements)

References 54 publications

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“…The saccharide-containing conjugates examined all show one detectable T g , which can be attributed to the higher- T g saccharides being the minority components. Similar observations of a single T g transition have been reported in other compositionally asymmetric oligosaccharide-containing diblock copolymers. ,, For the MT-containing conjugates, the measured T g reflects mostly that of the PS component. Their values are higher than N 3 –PS–N 3 because the PS chains are tethered on both ends to the rigid high- T g MT.…”

Section: Resultssupporting

confidence: 84%

“…Similar observa-tions of a single T g transition have been reported in other compositionally asymmetric oligosaccharide-containing diblock copolymers. 20,34,35 For the MT-containing conjugates, the measured T g reflects mostly that of the PS component. Their values are higher than N 3 −PS−N 3 because the PS chains are tethered on both ends to the rigid high-T g MT.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…Early studies on saccharide-containing block copolymers used polysaccharides and oligosaccharides. − For example, Liu and Zhang reported the synthesis of a dextran- b -poly(ε-caprolactone) diblock copolymer, then demonstrated the self-assembly of the diblock in water to form spherical micelles . Borsali and co-workers employed oligosaccharide maltoheptaose and prepared a number of block copolymers with different synthetic blocks. − Morphology characterization of these block copolymers revealed ordered microdomain morphologies with sub-10 nm periodicity. By utilizing their small feature sizes, the application of the block copolymers as nanolithography templates was also illustrated. , Satoh and co-workers reported the synthesis of triblock copolymers containing malto-oligosaccharides as the end blocks and either polystyrene (PS) or poly(δ-decanolactone) (PDL) as the mid-block. , Ordered microdomain morphologies were confirmed in the solid-state samples.…”

Section: Introductionmentioning

confidence: 99%

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Ordered Microdomain Structures in Saccharide–Polystyrene–Saccharide Hybrid Conjugates

et al. 2021

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Hybrid conjugates consist of synthetic polymers and naturally occurring saccharides, and are capable of microphase separation at small molecular weights to form ordered domain structures. In this study, we synthesize ABA triblock-like conjugates with polystyrene as the synthetic mid-segment and either trisaccharide maltotriose (MT) or disaccharide maltose (Mal) as the end unit. Hybrid conjugates of varying compositions are prepared by a combination of atom transfer radical polymerization and a click reaction, and their morphologies are examined by small-angle X-ray scattering and transmission electron microscopy. The MT-containing conjugates are found to form well-ordered domain structures with a sub-10 nm periodicity, and morphology transition from cylinders to spheres to disordered spheres is observed with decreasing saccharide weight fraction. The Mal-containing conjugates also show microphase separation. However, the observed domain morphologies lack regular packing due to the close proximity of polymer glass transition temperature and order–disorder transition temperature. The saccharide-containing conjugates are also found to undergo an irreversible morphology change at high temperatures, attributed to saccharide dehydration-induced pentablock-like structure formation.

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Section: Resultssupporting

confidence: 84%

Section: ■ Results and Discussionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Ordered Microdomain Structures in Saccharide–Polystyrene–Saccharide Hybrid Conjugates

et al. 2021

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“…The maximum solubility of lignin (99.88%) was obtained with a 7:3 volume ratio of GVL to water. This could be explained by Hildebrand solubility theory [ 44 ]; the maximum solubility of lignin should be obtained when the solubility parameter of the solvent mixture is close to the solubility parameters of lignin. The effects of the volume ratio of GVL to water on the particle sizes of LNPs were investigated and the results are shown in Figure 1 b.…”

Section: Resultsmentioning

confidence: 99%

Preparation of Lignin-Based Nanoparticles with Excellent Acidic Tolerance as Stabilizer for Pickering Emulsion

Wang,

Kang,

Zhang

et al. 2023

Polymers

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In this work, novel lignin-based nanoparticles (LβNPs) with high acidic tolerance were successfully prepared via electrostatic interaction between β-alanine and lignin nanoparticles. The effects of the mass ratio of lignin nanoparticles to β-alanine and pH value on the morphology and particle sizes of LβNPs were investigated with the aim of obtaining the ideal nanoparticles. The optimized LβNPs were spherical in shape with an average particle size of 41.1 ± 14.5 nm and exhibited outstanding structure stability under high acidic conditions (pH < 4). Subsequently, Pickering emulsions stabilized by LβNPs were prepared using olive oil as the oil phase. Additionally, the effects of pH value, droplet size, morphology, and storage stability on Pickering emulsions were also analyzed. The emulsions displayed excellent stability, and were stable against strongly acidic conditions (pH < 4) after 30 days of storage. The study presented a promising approach to preparing lignin-based nanoparticles with high acidic tolerance (an ideal type of stabilizer to prepare emulsions), and exhibited extremely high potential application values in the fields of drug delivery, food additives, and oily wastewater treatment.

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“…Additionally, Cushen et al linked MH to poly( para -trimethylsilylstyrene) (PTMSS) in MH- b -PTMSS with an N of 22, and this copolymer also phase separated into cylinders of L 0 = 8.3 nm. Noronha et al demonstrated that MH- b -PMMA with an N of 34 could phase separate into a cylindrical morphology with an L 0 = 8.3 nm. Additionally, Sakai-Otsuka and colleagues linked poly(3-hexylthiophene) with peracetylated maltoheptose in P3HT- b -AcMal 7 with an M n of 5670 g mol –1 and demonstrated phase separation into a lamellar morphology with an L 0 = 12.2 nm.…”

Section: Introductionmentioning

confidence: 99%

Galactose-Based Block Copolymers with Switchable χ Parameters for Tuning Phase Separated Morphology

et al. 2023

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Block copolymer (BCP) self-assembly has emerged over the past two decades as a promising method for generation of features for manufacture of integrated circuits and memory devices. Low-molecular-weight BCPs with blocks that are highly immiscible can generate features of dimensions below 10 nm. However, it is often challenging to select a common good solvent for high-χ BCPs to allow spin coating. In addition, controlling the alignment of phase separated morphologies with respect to the wafer and at the air interface may be challenging. Here, we prepare a series BCPs of polystyrene (PS) and poly-6-O-methacryloyl-Dgalactopyranose (PMAGal), where the polar galactose has been protected with more hydrophobic acetonides. The acetonide protecting groups could be deprotected with trifluoroacetic acid to yield the more polar galactose repeat units to increase the incompatibility of the sugar-containing block with the PS blocks. The bulk morphology of the protected and deprotected versions was studied using small-angle X-ray scattering, where the morphology could be switched from disordered for the protected BCP to either cylindrical or lamellar for the deprotected version or between two ordered phases. Finally, we demonstrate phase separation on the wafer via solvent vapor annealing with H 2 O/THF, resulting in lamellar patterning with domains as small as 14 nm.

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Self-assembly of maltoheptaose-b-PMMA block copolymer systems: 10 nm Resolution in thin film and bulk states

Cited by 7 publications

References 54 publications

Ordered Microdomain Structures in Saccharide–Polystyrene–Saccharide Hybrid Conjugates

Ordered Microdomain Structures in Saccharide–Polystyrene–Saccharide Hybrid Conjugates

Preparation of Lignin-Based Nanoparticles with Excellent Acidic Tolerance as Stabilizer for Pickering Emulsion

Galactose-Based Block Copolymers with Switchable χ Parameters for Tuning Phase Separated Morphology

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