scholarly journals Structural, thermal and surface characterization of thermoplastic polyurethanes based on poly(dimethylsiloxane)

2014 ◽  
Vol 79 (7) ◽  
pp. 843-866 ◽  
Author(s):  
Marija Pergal ◽  
Ivan Stefanovic ◽  
Dejan Godjevac ◽  
Vesna Antic ◽  
Vesna Milacic ◽  
...  
Keyword(s):  
Surface Properties ◽  
Surface Characterization ◽  
Soft Segment ◽  
Hydrophobic Surface ◽  
Sem Analysis ◽  
Degree Of Crystallinity ◽  
Water Contact ◽  
Thermoplastic Polyurethanes ◽  
Melting Temperatures ◽  
Soft Segments

In this study, the synthesis, structure and physical properties of two series of thermoplastic polyurethanes based on hydroxypropyl terminated poly(dimethylsiloxane) (HP-PDMS) or hydroxyethoxy propyl terminated poly(dimethylsiloxane) (EO-PDMS) as a soft segment, and 4,4?-methylenediphenyl diisocyanate and 1,4-butanediol as a hard segment were investigated. Each series is composed of samples prepared with a different soft segment. The polyurethanes were synthesized by two-step polyaddition in solution. The effects of the type and content of PDMS segments on the structure, thermal and surface properties of copolymers were studied by 1H NMR, 13C NMR and two-dimensional NMR (HMBC and ROESY) spectroscopy, GPC, DSC, TGA, WAXS, SEM, water contact angle and water absorption measurements. Thermal properties investigated by DSC indicated that the presence of soft PDMS segments lowers the glass transition and melting temperatures of the hard phase as well as the degree of crystallinity. SEM analysis of copolymers with a lower soft segment content confirmed the presence of spherulite superstructures, which arise from the crystallization of the hard segments. When compared with polyurethanes prepared from HP-PDMS, copolymers synthesized from EO-PDMS with the same content of the soft segments have higher degree of crystallinity, better thermal stability and less hydrophobic surface. Our results show that the synthesized polyurethanes have good thermal and surface properties, which could be further modified by changing the type or content of the soft segments.

scholarly journals Surface Characterization of Asymmetric Bi-Soft Segment Poly(ester urethane urea) Membranes for Blood-Oxygenation Medical Devices

2012 ◽  
Vol 2012 ◽  
pp. 1-9 ◽  
Author(s):  
Mónica Faria ◽  
Vítor Geraldes ◽  
Maria Norberta de Pinho
Keyword(s):  
Cross Sections ◽  
Surface Characterization ◽  
Soft Segment ◽  
Surface Characteristics ◽  
Contact Angles ◽  
Sem Analysis ◽  
Blood Oxygenation ◽  
Water Contact ◽  
Streaming Potentials ◽  
Zeta Potentials

Asymmetric bi-soft segment poly(ester urethane urea) (PEUU) membranes containing polycaprolactone (PCL) as a second soft segment are synthesized with PCL-diol ranging from 0% to 15% (w/w). Bulk and surface characteristics of the PEUU membranes were investigated by scanning electron microscopy (SEM), static water contact angles, and surface streaming potentials and were correlated to hemocompatibility properties, namely, hemolysis and thrombosis degrees. SEM analysis reveals PEUU membranes with asymmetric cross-sections and top dense surfaces with distinct morphologies. The increase in PCL-diol content yields PEUU membranes with blood-contacting surfaces that are smoother, more hydrophilic, and with higher maximum zeta potentials. The results obtained in this work give no evidence of a correlation between hydrophilicity/zeta potentials and the hemolysis/thrombosis degree of blood-contacting surfaces of the PEUU membranes. In contrast, other hemocompatibility aspects reveal that the more hydrophilic membranes are associated with lower platelet deposition and inhibition of extreme states of platelet activation.

scholarly journals Investigation of the morphology and surface properties of crosslinked poly(urethane-ester-siloxane)s

2012 ◽  
Vol 66 (6) ◽  
pp. 813-821 ◽  
Author(s):  
Jasna Dzunuzovic ◽  
Marija Pergal ◽  
Vesna Vodnik ◽  
Milena Spírková ◽  
Rafał Poręba ◽  
...  
Keyword(s):  
Ethylene Oxide ◽  
Water Absorption ◽  
Surface Properties ◽  
Microphase Separation ◽  
Crosslinking Agent ◽  
Hydrophobic Surface ◽  
Sem Analysis ◽  
Force Microscopy ◽  
Hyperbranched Polyesters ◽  
Atomic Force

Two series of crosslinked poly(urethane-ester-siloxane)s were synthesized from ?,?-dihydroxy-(ethylene oxide-poly(dimethylsiloxane)-ethylene oxide) (EO-PDMS-EO), 4,4?-methylenediphenyl diisocyanate and Boltorn? hyperbranched polyesters of the second and third pseudo generation, by a two-step polymerization in solution. The effect of the EO-PDMS-EO content and functionality of the applied crosslinking agent on the morphology and surface properties of the prepared poly(urethane-ester-siloxane)s was investigated by FTIR spectroscopy, small-angle X-ray scattering (SAXS), atomic force microscopy (AFM), scanning electron microscopy (SEM) and water absorption measurement. Different techniques (FTIR peak deconvolution, SAXS and AFM) revealed that decrease of the crosslinking agent functionality and EO-PDMS-EO content promotes microphase separation in the synthesized poly(urethane-ester-siloxane)s. SEM analysis and water absorption experiments showed that due to the hydrophobic character of EO-PDMS-EO and its ability to migrate to the surface of poly(urethane-ester-siloxane)s, samples synthesized with higher EO-PDMS-EO content and crosslinking agent of lower functionality have more hydrophobic surface and better waterproof performances. The obtained results indicate that the synthesis of poly(urethane-ester-siloxane)s based on EO-PDMS-EO and Boltorn? hyperbranched polyesters leads to the creation of networks with interesting morphological and surface properties, which can be easily tailored by changing the content of EO-PDMS-EO segment or functionality of hyperbranched polyester.

scholarly journals Synthesis of thermoplastic poly(ester-siloxane)s in the melt and in solution

2005 ◽  
Vol 70 (12) ◽  
pp. 1469-1485 ◽  
Author(s):  
Biljana Dojcinovic ◽  
Vesna Antic ◽  
Marija Vuckovic ◽  
Jasna Djonlagic
Keyword(s):  
1H Nmr Spectroscopy ◽  
Hard Segment ◽  
Soft Segment ◽  
Weight Ratio ◽  
Thermoplastic Elastomers ◽  
Degree Of Crystallinity ◽  
Mechanical Spectroscopy ◽  
Scanning Calorimetry ◽  
Melting Temperatures ◽  
High Boiling Solvent

Two series of thermoplastic elastomers, based on poly(dimethylsiloxane) PDMS, as the soft segment and poly(butylene terephthalate), PBT, as the hard segment, were synthesized by catalyzed transesterification, from dimethyl terephthalate, DMT, silanol-terminated poly(dimethylsiloxane), PDMS-OH Mn=1750g/mol, and 1,4-butanediol, BD. The mole ratio of the starting comonomers was selected to result in a constant hard to soft weight ratio of 55:45. The first series was synthesized in order to determine the optimal mole ratio of BD and DMT for the synthesis of high molecular weight thermoplastic poly(ester-siloxane)s, TPESs. The second series was performed in the presence of the high-boiling solvent, 1,2,4-trichlorbenzene in order to increase the mixing between the extremely non-polar siloxane prepolymer and the polar reactants, DMT and BD, and, therefore, avoid phase separation during synthesis. The structure and composition of the synthesized poly(ester-siloxane)s were verified by 1H-NMR spectroscopy, while the melting temperatures and degree of crystallinity were determined by differential scanning calorimetry (DSC). The effectiveness of the incorporation of the silanol-terminated poly( dimethylsiloxane) into the polyester chains was verified by chloroform extraction. The rheological properties of the poly(ester-siloxane)s were investigated by dynamic mechanical spectroscopy (DMA).

scholarly journals Rheological behaviour of thermoplastic poly(ester-siloxane)s

2010 ◽  
Vol 64 (6) ◽  
pp. 537-545 ◽  
Author(s):  
Vesna Antic ◽  
Marija Pergal ◽  
Malisa Antic ◽  
Jasna Djonlagic
Keyword(s):  
Dynamic Viscosity ◽  
Microphase Separation ◽  
Soft Segment ◽  
Rheological Behaviour ◽  
Thermoplastic Elastomers ◽  
Degree Of Crystallinity ◽  
Mass Ratio ◽  
Complex Dynamic ◽  
Constant Length ◽  
Soft Segments

Two series of thermoplastic elastomers (TPES) based on poly(dimethylsiloxane), (PDMS) as the soft segment and poly(butylene terephthalate) (PBT) as the hard segment, were analyzed by dynamic mechanical spectroscopy. In the first TPES series the lengths of both hard and soft segments were varied while the mass ratio of the hard to soft segments was nearly constant (about 60 mass%). In the second series, the mass ratio of hard and soft segments was varied in the range from 60/40 to 40/60, with a constant length of soft PDMS segments. The influence of the structure and composition of TPESs on the rheological properties, such as complex dynamic viscosity, ?*, the storage, G?, and loss, G?, shear modulus as well as the microphase separation transition temperature, TMST, was examined. The obtained results showed that the storage modulus of the TPESs increased in a rubbery plateau region with increasing degree of crystallinity. The rheological measurements of TPESs also showed that a microphase reorganization occurred during the melting process. The microphase separation transition temperatures were in the range from 220 to 234 ?C. In the isotropic molten state, the complex dynamic viscosity increased with increasing both the content and lenght of hard PBT segments.

Topography and Wettability of Waterborne Polyurethane Coatings with Varying Amounts of Hard Segments

2013 ◽  
Vol 634-638 ◽  
pp. 3033-3037
Author(s):  
Yu Hong Qi ◽  
Zhan Ping Zhang ◽  
Yan Zhang ◽  
Mei Miao
Keyword(s):  
Laser Scanning ◽  
Hard Segment ◽  
Soft Segment ◽  
Hydrophobic Surface ◽  
Waterborne Polyurethane ◽  
Contact Angles ◽  
Water Contact ◽  
Hard Segment Content ◽  
Fouling Release ◽  
Hard Segments

Topography and wettability plays an important role to fouling release performance of a coating. Surface morphology and water contact angles (WCA) depending on time of three waterborne polyurethane (WPU) coatings were studied by laser scanning microscope and optical contact angle meter. The results show that WPU coatings with low hard segment content are consisted of hard segment domains, soft segment domains and crack-like non-cohesive regions. With increasing hard segment content, nanostructured micro-phase separated topography is easier to forming, and crack-like non-cohesive regions is reduced. A stable hydrophobic surface in the WPU system can be obtained by drying coating at 60C as well as adding hard segment content to improve fouling release performance of the coatings.

Laser-Induced Nanocarbon Formation for Tuning Surface Properties of Commercial Polymers

2020 ◽  
Author(s):  
Moataz Abdulhafez ◽  
Angela J. McComb ◽  
Mostafa Bedewy
Keyword(s):  
Contact Angle ◽  
Surface Properties ◽  
Surface Characterization ◽  
Surface Engineering ◽  
Surface Hydrophobicity ◽  
Contact Angles ◽  
Structure Property ◽  
Water Contact ◽  
Wide Range ◽  
Commercial Polymers

Abstract The growth of laser-induced nanocarbons, referred to here are LINC for short, directly on polymeric surfaces is a promising route toward surface engineering of commercial polymers. This paper aims to demonstrate how this new approach can enable achieving varied surface properties based on tuning the nanostructured morphology of the formed graphitic material on commercial polyimide (Kapton) films. We elucidate the effects of tuning laser processing parameters on the achieved nanoscale morphology and the resulting surface hydrophobicity or hydrophilicity. Our results show that by varying lasing power, rastering speed, laser spot size, and line-to-line gap sizes, a wide range of water contact angles are possible, i.e. from below 20° to above 110°. Combining water contact angle measurements from an optical tensiometer with LINC surface characterization using optical microscopy, electron microscopy, and Raman spectroscopy enables building the process-structure-property relationship. Our findings reveal that both the value of contact angle and the anisotropic wetting behavior of LINC on polyimide are dependent on their hierarchical surface nanostructure which ranges for isotropic nanoporous morphology to fibrous morphology. Results also show that increasing gap sizes lead to an increase in contact angles and thus an increase in the hydrophobicity of the surface. Hence, our work highlight the potential of this approach for manufacturing flexible devices with tailored surfaces.

scholarly journals On the Effectiveness of Oxygen Plasma and Alkali Surface Treatments to Modify the Properties of Polylactic Acid Scaffolds

Polymers ◽  
2021 ◽  
Vol 13 (10) ◽  
pp. 1643
Author(s):  
Ricardo Donate ◽  
María Elena Alemán-Domínguez ◽  
Mario Monzón
Keyword(s):  
Surface Properties ◽  
Enzymatic Degradation ◽  
Oxygen Plasma ◽  
Physicochemical Characterization ◽  
Surface Treatments ◽  
Carboxyl Groups ◽  
Scanning Calorimetry ◽  
Water Contact ◽  
Angle Measurements ◽  
3D Printed

Surface modification of 3D-printed PLA structures is a major issue in terms of increasing the biofunctionality and expanding the tissue engineering applications of these parts. In this paper, different exposure times were used for low-pressure oxygen plasma applied to PLA 3D-printed scaffolds. Alkali surface treatments were also evaluated, aiming to compare the modifications introduced on the surface properties by each strategy. Surface-treated samples were characterized through the quantification of carboxyl groups, energy-dispersive X-ray spectroscopy, water contact angle measurements, and differential scanning calorimetry analysis. The change in the surface properties was studied over a two-week period. In addition, an enzymatic degradation analysis was carried out to evaluate the effect of the surface treatments on the degradation profile of the 3D structures. The physicochemical characterization results suggest different mechanism pathways for each type of treatment. Alkali-treated scaffolds showed a higher concentration of carboxyl groups on their surface, which enhanced the enzymatic degradation rate, but were also proven to be more aggressive towards 3D-printed structures. In contrast, the application of the plasma treatments led to an increased hydrophilicity of the PLA surface without affecting the bulk properties. However, the changes on the properties were less steady over time.

scholarly journals Impact of Macrodiols on the Morphological Behavior of H12MDI/HDO-Based Polyurethane Elastomer

Polymers ◽  
2021 ◽  
Vol 13 (13) ◽  
pp. 2060
Author(s):  
Shazia Naheed ◽  
Mohammad Zuber ◽  
Mahwish Salman ◽  
Nasir Rasool ◽  
Zumaira Siddique ◽  
...  
Keyword(s):  
Molecular Weight ◽  
Contact Angle ◽  
Chain Length ◽  
Microphase Separation ◽  
Soft Segment ◽  
Group Identification ◽  
Degree Of Crystallinity ◽  
Polyurethane Elastomers ◽  
Hard Segments ◽  
Morphological Behavior

In this study, we evaluated the morphological behavior of polyurethane elastomers (PUEs) by modifying the soft segment chain length. This was achieved by increasing the soft segment molecular weight (Mn = 400–4000 gmol−1). In this regard, polycaprolactone diol (PCL) was selected as the soft segment, and 4,4′-cyclohexamethylene diisocyanate (H12MDI) and 1,6-hexanediol (HDO) were chosen as the hard segments. The films were prepared by curing polymer on Teflon surfaces. Fourier transform infrared spectroscopy (FTIR) was utilized for functional group identification in the prepared elastomers. FTIR peaks indicated the disappearance of −NCO and −OH groups and the formation of urethane (NHCOO) groups. The morphological behavior of the synthesized polymer samples was also elucidated using scanning electron microscopy (SEM) and atomic force microscopy (AFM) techniques. The AFM and SEM results indicated that the extent of microphase separation was enhanced by an increase in the molecular weight of PCL. The phase separation and degree of crystallinity of the soft and hard segments were described using X-ray diffraction (XRD). It was observed that the degree of crystallinity of the synthesized polymers increased with an increase in the soft segment’s chain length. To evaluate hydrophilicity/hydrophobicity, the contact angle was measured. A gradual increase in the contact angle with distilled water and diiodomethane (38.6°–54.9°) test liquids was observed. Moreover, the decrease in surface energy (46.95–24.45 mN/m) was also found to be inconsistent by increasing the molecular weight of polyols.

scholarly journals Epoxy/alumina composite coating on welded steel 316L with excellent wear and anticorrosion properties

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Maryama Hammi ◽  
Younes Ziat ◽  
Zakaryaa Zarhri ◽  
Charaf Laghlimi ◽  
Abdelaziz Moutcine
Keyword(s):  
Electrochemical Behaviour ◽  
Sem Analysis ◽  
Water Contact ◽  
Welded Steel ◽  
Melted Zone ◽  
Angle Measurements ◽  
Contact Angle Measurements ◽  
Alumina Composite ◽  
The Cost ◽  
Good Contrast

AbstractThe main purpose of this study is to elaborate anticorrosive coatings for the welded steel 316L, since this later is widely used in industrial field. Hence, within this work we have studied the electrochemical behaviour of different zones of the welded steel 316 in 1 M HCl media. The macrography study of the welded steel has revealed the different areas with a good contrast. We have stated three different zones, namely; melted zone (MZ), heat affected zone (HAZ) and base metal zone (BM). Impedance studies on welded steel 316L were conducted in 1 M HCl solution, coating of Epoxy/Alumina composite was applied on different zones, in order to reveal the anti-corrosion efficiency in each zone. Scanning electron microscopy (SEM) analysis was undertaken in order to check how far the used coating in such aggressive media protects the studied zones and these findings were assessed by water contact angle measurements. The choice of this coating is based on the cost and the safety. We concluded that the Epoxy/Alumina composite has a good protecting effect regarding welded steel in aggressive media.

scholarly journals Tunable Crystalline Phases in UV-Curable PEG-Grafted Ladder-Structured Silsesquioxane/Polyimide Composites

Materials ◽  
2020 ◽  
Vol 13 (10) ◽  
pp. 2295 ◽  
Author(s):  
Ryung Il Kim ◽  
Ju Ho Shin ◽  
Jong Suk Lee ◽  
Jung-Hyun Lee ◽  
Albert S. Lee ◽  
...  
Keyword(s):  
Polymer Composites ◽  
Surface Properties ◽  
Weight Ratio ◽  
Hybrid Polymer ◽  
Water Contact ◽  
Uv Curable ◽  
Wide Range ◽  
Drastic Increase ◽  
Polyimide Composites ◽  
Crystalline Polyethylene

A series of UV-curable hybrid composite blends containing a carboxylic acid functionalized polyimidewith varying amounts of high molecular weight (~1 K) PEG-grafted ladder-structured polysilsesquioxanes copolymerized with methacryl groups were fabricated and their structural, thermal, mechanical, and surface properties characterized. At a composite weight ratio of polyimide above 50 wt.%, a stark shift from amorphous to crystalline polyethylene glycol (PEG) phases were observed, accompanied by a drastic increase in both surface moduli and brittleness index. Moreover, fabricated composites were shown to have a wide range water contact angle, 9.8°–73.8°, attesting to the tunable surface properties of these amphiphilic hybrid polymer composites. The enhanced mechanical properties, combined with the utility of tunable surface hydrophilicity allows for the possible use of these hybrid polymer composites to be utilized as photosensitive polyimide negative photoresists for a myriad of semiconductor patterning processes.

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