Imaging Polymer Morphology using Atomic Force Microscopy

Schönherr, Holger

doi:10.1002/9781118892756.ch6

Cited by 4 publications

(1 citation statement)

References 35 publications

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“…AFM applications in polymers include the study of polymer morphologies at micro and nanoscale level, the identification of molecular order in single crystals and oriented samples, individual polymer chains and branches, filled polymer systems and composites, polymer blends and block copolymers. [8][9][10] AFM has been used to detect microphase-separated morphologies of block copolymers. Block copolymers display different morphologies depending on three main factors: copolymer composition and architecture, melt segregation strength, and thermal transitions (e.g., order-disorder, crystallization, and glass transition temperatures).…”

Section: Introductionmentioning

confidence: 99%

Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy

Palacios

Zhang

et al. 2020

Polymer

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In this work, we provide a detailed description of the tri-lamellar nanoscale morphology of a triple crystalline PEO-b-PCL-b-PLLA triblock terpolymer obtained by Hot-Stage Atomic Force microscopy (AFM) imaging and Wide Angle X-ray scattering (WAXS) analysis for the first time. The precursor PCL-b-PLLA diblock copolymer has also been included in the study for comparison purposes. A two-step crystallization protocol has been applied to create a distinct lamellar morphology. Both WAXS and AFM revealed the double crystalline nature of the diblock copolymer. However, the identification of multiple crystalline phases in the triblock terpolymer by AFM and WAXS at room temperature is not straightforward. The advantages of hot-stage AFM allowed following the evolution of the lamellar morphology and the successive melting of the tricrystalline PEO-b-PCL-b-PLLA sample during heating. Taking into account the melting temperature of each crystalline block, the existing lamellar populations were clearly identified. At 45 °C, the thinnest lamellae disappeared, due to the melting of PEO crystals. The medium size lamellae disappeared at 60 °C when PCL crystals melt. At that temperature, the only remaining crystals are those of the PLLA block. AFM mechanical modulus images provide further evidence of the lamellar self-assembly of the triblock terpolymer. The nanoscale arrangement includes lamellae of PCL, PEO, or both in between the PLLA lamellae. Hot-Stage AFM is a valuable technique to elucidate the morphological features of complex multi-crystalline systems.

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Section: Introductionmentioning

confidence: 99%

Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy

Palacios

Zhang

et al. 2020

Polymer

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Detailed thermal analysis of crystallization kinetics and band morphology for future blending of absorbable poly(p‐dioxanone) monofilament surgical suture with poly(ε‐caprolactone)

Mamun

2020

Polymer International

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The thermal effects on crystallization kinetics and the band morphology of absorbable poly(p-dioxanone) (PDS) were studied in detail with TGA, AFM, DSC and polarized optical microscopy techniques. The polymer film was crystallized with isothermal and non-isothermal conditions over a wide temperature range, cooling from the melt at 140°C (beyond the equilibrium melting temperature but below the degradation temperature). With the isothermal crystallization process, a well-defined spherulitic morphology of the PDS polymer, linearly growing in all directions with time, was observed. A microstructure analysis by polarized optical microscopy and AFM revealed that the crystallized PDS shows large spherulites with band morphology, the nucleation density decreases and the spacing between the band increases with crystallization temperature. The periodic band morphology of the spherulites is related to edge-on and flat-on lamella orientation. The crystallization temperature dependent spherulite growth rate displayed a bell-shaped curve, showing a highest spherulite growth rate at 60°C, explained by classical nucleation theory. These results allowed a good understanding of the thermal and morphological properties of the PDS polymer over a wide temperatures range in both isothermal and non-isothermal conditions. Additionally, the crystallization and melting behaviors of the PDS polymer were studied and compared for the future application of blending with other compatible polymers, e.g. poly(ε-caprolactone).

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Effect of a cryogenic treatment in the microstructure, functional and flow properties of soy protein isolate

et al. 2021

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Imaging Polymer Morphology using Atomic Force Microscopy

Cited by 4 publications

References 35 publications

Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy

Direct identification of three crystalline phases in PEO-b-PCL-b-PLLA triblock terpolymer by In situ hot-stage atomic force microscopy

Detailed thermal analysis of crystallization kinetics and band morphology for future blending of absorbable poly(p‐dioxanone) monofilament surgical suture with poly(ε‐caprolactone)

Effect of a cryogenic treatment in the microstructure, functional and flow properties of soy protein isolate

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