scholarly journals Visualization of Polymer Crystallization by In Situ Combination of Atomic Force Microscopy and Fast Scanning Calorimetry

Polymers ◽  
2019 ◽  
Vol 11 (5) ◽  
pp. 890 ◽  
Author(s):  
Rui Zhang ◽  
Evgeny Zhuravlev ◽  
René Androsch ◽  
Christoph Schick

A chip-based fast scanning calorimeter (FSC) is used as a fast hot-stage in an atomic force microscope (AFM). This way, the morphology of materials with a resolution from micrometers to nanometers after fast thermal treatments becomes accessible. An FSC can treat the sample isothermally or at heating and cooling rates up to 1 MK/s. The short response time of the FSC in the order of milliseconds enables rapid changes from scanning to isothermal modes and vice versa. Additionally, FSC provides crystallization/melting curves of the sample just imaged by AFM. We describe a combined AFM-FSC device, where the AFM sample holder is replaced by the FSC chip-sensor. The sample can be repeatedly annealed at pre-defined temperatures and times and the AFM images can be taken from exactly the same spot of the sample. The AFM-FSC combination is used for the investigation of crystallization of polyamide 66 (PA 66), poly(ether ether ketone) (PEEK), poly(butylene terephthalate) (PBT) and poly(ε-caprolactone) (PCL).

2008 ◽  
Vol 587-588 ◽  
pp. 212-216 ◽  
Author(s):  
Magdalena Jurczyk-Kowalska ◽  
Joanna Ryszkowska

Carboxyalumoxanes have been incorporated into a polyurethane matrix by in situ polymerization. The filler was dispersed in the polyurethane matrix by either both ultrasonic and mechanical mixing or by mechanical mixing alone. The physico-mechanical properties of the composites have been characterized using scanning electron microscopy (SEM), atomic force microscopy (AFM), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Using ultrasound improves the degree of dispersion of the fillers in the matrix, but it also causes changes in the structure of the polyurethane matrix.


2020 ◽  
Vol 92 (6) ◽  
pp. 977-984
Author(s):  
Mayya V. Kulikova ◽  
Albert B. Kulikov ◽  
Alexey E. Kuz’min ◽  
Anton L. Maximov

AbstractFor previously studied Fischer–Tropsch nanosized Fe catalyst slurries, polymer compounds with or without polyconjugating structures are used as precursors to form the catalyst nanomatrix in situ, and several catalytic experiments and X-ray diffraction and atomic force microscopy measurements are performed. The important and different roles of the paraffin molecules in the slurry medium in the formation and function of composite catalysts with the two types of aforementioned polymer matrices are revealed. In the case of the polyconjugated polymers, the alkanes in the medium are “weakly” coordinated with the metal-polymer composites, which does not affect the effectiveness of the polyconjugated polymers. Otherwise, alkane molecules form a “tight” surface layer around the composite particles, which create transport complications for the reagents and products of Fischer-Tropsch synthesis and, in some cases, can change the course of the in situ catalyst formation.


1999 ◽  
Vol 353 (1-2) ◽  
pp. 194-200 ◽  
Author(s):  
C. Coupeau ◽  
J.F. Naud ◽  
F. Cleymand ◽  
P. Goudeau ◽  
J. Grilhé

Polymers ◽  
2021 ◽  
Vol 13 (6) ◽  
pp. 878
Author(s):  
Krystyna Wnuczek ◽  
Andrzej Puszka ◽  
Łukasz Klapiszewski ◽  
Beata Podkościelna

This study presents the preparation and the thermo-mechanical characteristics of polymeric blends based on di(meth)acrylates monomers. Bisphenol A glycerolate diacrylate (BPA.GDA) or ethylene glycol dimethacrylate (EGDMA) were used as crosslinking monomers. Methyl methacrylate (MMA) was used as an active solvent in both copolymerization approaches. Commercial polycarbonate (PC) was used as a modifying soluble additive. The preparation of blends and method of polymerization by using UV initiator (Irqacure® 651) was proposed. Two parallel sets of MMA-based materials were obtained. The first included more harmless linear hydrocarbons (EGDMA + MMA), whereas the second included the usually used aromatic copolymers (BPA.GDA + MMA). The influence of different amounts of PC on the physicochemical properties was discussed in detail. Chemical structures of the copolymers were confirmed by attenuated total reflection–Fourier transform infrared (ATR/FT-IR) spectroscopy. Thermo-mechanical properties of the synthesized materials were investigated by means of differential scanning calorimetry (DSC), thermogravimetric (TG/DTG) analyses, and dynamic mechanical analysis (DMA). The hardness of the obtained materials was also tested. In order to evaluate the surface of the materials, their images were obtained with the use of atomic force microscopy (AFM).


Nanomaterials ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 722
Author(s):  
Ioanna Christodoulou ◽  
Tom Bourguignon ◽  
Xue Li ◽  
Gilles Patriarche ◽  
Christian Serre ◽  
...  

In recent years, Metal-Organic Frameworks (MOFs) have attracted a growing interest for biomedical applications. The design of MOFs should take into consideration the subtle balance between stability and biodegradability. However, only few studies have focused on the MOFs’ stability in physiological media and their degradation mechanism. Here, we investigate the degradation of mesoporous iron (III) carboxylate MOFs, which are among the most employed MOFs for drug delivery, by a set of complementary methods. In situ AFM allowed monitoring with nanoscale resolution the morphological, dimensional, and mechanical properties of a series of MOFs in phosphate buffer saline and in real time. Depending on the synthetic route, the external surface presented either well-defined crystalline planes or initial defects, which influenced the degradation mechanism of the particles. Moreover, MOF stability was investigated under different pH conditions, from acidic to neutral. Interestingly, despite pronounced erosion, especially at neutral pH, the dimensions of the crystals were unchanged. It was revealed that the external surfaces of MOF crystals rapidly respond to in situ changes of the composition of the media they are in contact with. These observations are of a crucial importance for the design of nanosized MOFs for drug delivery applications.


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