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A Comparative Study on Physiochemical, Thermomechanical, and Electrochemical Properties of Sulfonated Poly(Ether Ether Ketone) Block Copolymer Membranes with and without Fe₃O₄ Nanoparticles.

ABSTRACT: The composite structure, good porosity, and electrochemical behavior of proton exchange membranes (PEMs) are important characteristics, which can improve the performance of polymer electrolyte fuel cells (PEFCs). In this study, we designed and synthesized an XY block copolymer via a polycondensation reaction that contains sulfonated poly(ether ether ketone) (SPEEK) (X) as a hydrophilic unit and a fluorinated oligomer (Y) as a hydrophobic unit. The prepared XY block copolymer is composed of Fe₃O₄ nanoparticles to create composite architecture, which was subsequently treated with a 1 M H₂SO₄ solution at 70 °C for 1 h to eliminate Fe₃O₄ and generate a pores structure in the membrane. The morphological, physiochemical, thermomechanical, and electrochemical properties of bare XY, XY/Fe₃O₄-9 and XY(porous)-9 membranes were measured and compared in detail. Compared with XY/Fe₃O₄-9 composite, the proton conductivity of XY(porous)-9 membrane was remarkably enhanced as a result of the existence of pores as nano-conducting channels. Similarly, the XY(porous)-9 membrane exhibited enhanced water retention and ion exchange capacity among the prepared membranes. However, the PEFC power density of XY(porous)-9 membrane was still lower than that of XY/Fe₃O₄-9 membrane at 60 °C and 60% relative humidity. Also, the durability of XY(porous)-9 membrane is found to be lower compared with pristine XY and XY/Fe₃O₄-9 membranes as a result of the hydrogen crossover through the pores of the membrane.

SUBMITTER: Kim AR

PROVIDER: S-EPMC6473931 | biostudies-literature |

REPOSITORIES: biostudies-literature

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Composite Sulfonated Polyether-Ether Ketone Membranes with SBA-15 for Electrochemical Energy Systems.

Project description:The aim of this work is the evaluation of a Sulfonated Poly Ether-Ether Ketone (S-PEEK) polymer modified by the addition of pure Santa Barbara Amorphous-15 (SBA-15, mesoporous silica) and SBA-15 previously impregnated with phosphotungstic acid (PWA) fillers (PWA/SBA-15) in order to prepare composite membranes as an alternative to conventional Nafion® membranes. This component is intended to be used as an electrolyte in electrochemical energy systems such as hydrogen and methanol Proton Exchange Membrane Fuel Cell (PEMFC) and Electrochemical Hydrogen Pumping (EHP). The common requirements for all the applications are high proton conductivity, thermomechanical stability, and fuel and oxidant impermeability. The morphology of the composite membranes was investigated by Scanning Electron Microscopy- Energy Dispersive X-ray Spectroscopy (SEM-EDS) analysis. Water Uptake (Wup), Ion Exchange Capacity (IEC), proton conductivity, methanol permeability and other physicochemical properties were evaluated. In PEMFC tests, the S-PEEK membrane with a 10 wt.% SBA-15 loading showed the highest performance. For EHP, the inclusion of inorganic materials led to a back-diffusion, limiting the compression capacity. Concerning methanol permeability, the lowest methanol crossover corresponded to the composites containing 5 wt.% and 10 wt.% SBA-15.

| S-EPMC7178128 | biostudies-literature

Nanocomposite Based on Functionalized Gold Nanoparticles and Sulfonated Poly(ether ether ketone) Membranes: Synthesis and Characterization.

Project description:Gold nanoparticles, capped by 3-mercapto propane sulfonate (Au-3MPS), were synthesized inside a swollen sulfonated poly(ether ether ketone) membrane (sPEEK). The formation of the Au-3MPS nanoparticles in the swollen sPEEK membrane was observed by spectroscopic and microscopic techniques. The nanocomposite containing the gold nanoparticles grown in the sPEEK membrane, showed the plasmon resonance λmax at about 520 nm, which remained stable over a testing period of three months. The size distribution of the nanoparticles was assessed, and the sPEEK membrane roughness, both before and after the synthesis of nanoparticles, was studied by AFM. The XPS measurements confirm Au-3MPS formation in the sPEEK membrane. Moreover, AFM experiments recorded in fluid allowed the production of images of the Au-3MPS@sPEEK composite in water at different pH levels, achieving a better understanding of the membrane behavior in a water environment; the dynamic hydration process of the Au-3MPS@sPEEK membrane was investigated. These preliminary results suggest that the newly developed nanocomposite membranes could be promising materials for fuel cell applications.

| S-EPMC5503356 | biostudies-literature

Effect of Covalent Organic Frameworks Containing Different Groups on Properties of Sulfonated Poly(ether ether ketone) Matrix Proton Exchange Membranes.

Project description:The rich -SO3H groups enable sulfonated poly (ether ether ketone) (SPEEK) to possess excellent proton conductivities in proton exchange membrane (PEM), but cause excessive water absorption, resulting in the decline of dimensional stability. It is a challenge to resolve the conflict between conductivity and stability. Owing to its unique structural designability, covalent organic frameworks (COFs) have been used to regulate the performances of PEMs. The authors propose the use of COFs with acidic and basic groups for meeting the requirements of proton conductivity and dimensional stability. Herein, COFs containing different groups (sulfoacid, pyridine, and both) were uniformly dispersed into the SPEEK matrix by in situ synthesis, and the effects on the properties of SPEEK matrix PEMs were revealed. The sulfoacid group significantly improves proton conductivities. At 60 °C, under 95% RH, the conductivity of the SPEEK/TpPa-SO3H-20 composite membrane was 443.6 mS·cm-1, which was 3.3 times that of the pristine SPEEK membrane. The pyridine group reduced the swelling ratio at 50 °C from 220.7% to 2.4%, indicating an enhancement in dimensional stability. Combining the benefits of sulfoacid and pyridine groups, SPEEK/TpPa-(SO3H-Py) composite membrane has a conductivity of 360.3 mS·cm-1 at 60 °C and 95% RH, which is 1.86 times that of SPEEK, and its swelling ratio is 11.8%, about 1/20 of that of SPEEK membrane. The method of in situ combination and regulation of groups open up a way for the development of SPEEK/COFs composite PEMs.

| S-EPMC9565559 | biostudies-literature

Synthesis and characterization of a novel crosslinkable side-chain sulfonated poly(arylene ether sulfone) copolymer proton exchange membranes.

Project description:A series of novel crosslinkable side-chain sulfonated poly(arylene ether sulfone) copolymers (S-SPAES(x/y)) was prepared from 4,4'-biphenol, 4,4'-difluorodiphenyl sulfone, and a new difluoro aromatic monomer 1-(2,6-difluorophenyl)-2-(3,5-dimethoxyphenyl)-1,2-ethanedione (DFDMED) via co-polycondensation, demethylation, and further nucleophilic substitution of 1,4-butane sultone. Meanwhile, quinoxaline-based crosslinked copolymers (CS-SPAES(x/y)) were obtained via cyclo-condensation between S-SPAES(x/y) and 3,3'-diaminobenzidine. Both the crosslinkable and crosslinked copolymer membranes exhibit good mechanical properties and high anisotropic membrane swelling. Crosslinkable S-SPAES(1/2) with an ion exchange capacity (IEC) of 2.01 mequiv. g-1 displays a relatively high proton conductivity of 180 mS cm-1 and acceptable single-cell performance, which is attributed to its good microphase separation resulting from the side-chain sulfonated copolymer structures. Compared with S-SPAES(1/1) (IEC of 1.68 mequiv. g-1), crosslinked CS-SPAES(1/2) with a comparable IEC exhibits a larger conductivity of 157 mS cm-1, and significantly higher oxidative stability and lower membrane swelling, suggesting a distinct performance improvement due to the quinoxaline-based crosslinking.

| S-EPMC9055182 | biostudies-literature

Phosphonate poly(vinylbenzyl chloride)-Modified Sulfonated poly(aryl ether nitrile) for Blend Proton Exchange Membranes: Enhanced Mechanical and Electrochemical Properties.

Project description:Blend proton exchange membranes (BPEMs) were prepared by blending sulfonated poly(aryl ether nitrile) (SPAEN) with phosphorylated poly(vinylbenzyl chloride) (PPVBC) and named as SPM-x%, where x refers to the proportion of PPVBC to the weight of SPAEN. The chemical complexation interaction between the phosphoric acid and sulfonic acid groups in the PPVBC-SPAEN system resulted in BPEMs with reduced water uptake and enhanced mechanical properties compared to SPAEN proton exchange membranes. Furthermore, the flame retardancy of the PPVBC improved the thermal stability of the BPEMs. Despite a decrease in ion exchange capacity, the proton conductivity of the BPEMs in the through-plane direction was significantly enhanced due to the introduction of phosphoric acid groups, especially in low relative humidity (RH) environments. The measured proton conductivity of SPM-8% was 147, 98, and 28 mS cm-1 under 95%, 70%, and 50% RH, respectively, which is higher than that of the unmodified SPAEN membrane and other SPM-x% membranes. Additionally, the morphology and anisotropy of the membrane proton conductivities were analyzed and discussed. Overall, the results indicated that PPVBC doping can effectively enhance the mechanical and electrochemical properties of SPAEN membranes.

| S-EPMC10421228 | biostudies-literature

Hydration, Prediction of the pK a, and Infrared Spectroscopic Study of Sulfonated Polybenzophenone (SPK) Block-Copolymer Hydrocarbon Membranes and Comparisons with Nafion.

Project description:We used long-range-corrected density functional theory to investigate the hydration, pK a values, and harmonic vibrational spectroscopy of sulfonated polybenzophenone (SPK) block-copolymer hydrocarbon membranes to ascertain the reasons why this gives comparable or higher proton conductivities against Nafion over a wide range of humidity. It was found that a minimum of three water molecules are required for proton dissociation in both membranes. From natural population analysis, it was noticed that the proton dissociation of SPK membranes is nearly comparable to Nafion at relatively low water content. Next, we explored the applicability of the appropriate treatment for pK a and proton's energy with a benchmark set (AKB) scheme to compute the pK a values for these membranes. These results indicate that the proton dissociative abilities of sulfonic acid groups of the SPK membrane are higher than those of Nafion. This could be one of the reasons for the SPK membrane to show higher proton conductivities at high relative humidity. Furthermore, the effect of hydration on the proton conductivity of membranes illustrates that asymmetric stretching of the SO3 - mode was in agreement with Nafion ones but opposite trends were found in the case of symmetric stretching of the SO3 - mode upon hydration.

| S-EPMC8655912 | biostudies-literature

Block Copolymer Membranes for Efficient Capture of a Chemotherapy Drug.

Project description:We introduce the use of block copolymer membranes for an emerging application, "drug capture". The polymer is incorporated in a new class of biomedical devices, referred to as ChemoFilter, which is an image-guided temporarily deployable endovascular device designed to increase the efficacy of chemotherapy-based cancer treatment. We show that block copolymer membranes consisting of functional sulfonated polystyrene end blocks and a structural polyethylene middle block (S-SES) are capable of capturing doxorubicin, a chemotherapy drug. We focus on the relationship between morphology of the membrane in the ChemoFilter device and efficacy of doxorubicin capture measured in vitro. Using small-angle X-ray scattering and cryogenic scanning transmission electron microscopy, we discovered that rapid doxorubicin capture is associated with the presence of water-rich channels in the lamellar-forming S-SES membranes in aqueous environment.

| S-EPMC4989249 | biostudies-literature

MXene potassium titanate nanowire/sulfonated polyether ether ketone (SPEEK) hybrid composite proton exchange membrane for photocatalytic water splitting.

Project description:A cross-linked sulfonated polyether ether ketone (C-SPEEK) was incorporated with MXene/potassium titanate nanowire (MKT-NW) as a filler and applied as a proton exchange membrane for photocatalytic water splitting. The prepared hybrid composite PEM had proton conductivity of 0.0097 S cm-1 at room temperature with an ion exchange capacity of 1.88 meq g-1. The hybrid composite proton exchange membrane is a reactive membrane which was able to generate hydrogen gas under UV light irradiation. The efficiency of hydrogen gas production was 0.185066 μmol within 5 h for 12% wt of MKT-NW loading. The results indicated that the MKT-NW/C-SPEEK membrane is a promising candidate for ion exchange with hydrogen gas evolution in photocatalytic water splitting and could be applied as a renewable source of energy to use in various fields of applications.

| S-EPMC8695234 | biostudies-literature

Sulfonated Pentablock Copolymer Membranes and Graphene Oxide Addition for Efficient Removal of Metal Ions from Water.

Project description:Nowadays heavy metals are among the higher environmental priority pollutants, therefore, the identification of new, effective, reusable and easy-to-handle adsorbent materials able to remove metal ions from water is highly desired. To this aim, in this work for the first time, sulfonated pentablock copolymer (s-PBC, Nexar™) membranes and s-PBC/graphene oxide (GO) nanocomposite membranes were investigated for the removal of heavy metals from water. Membranes were prepared by drop casting and their chemical, structural and morphological properties were characterized using scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy, dynamic mechanical analysis (DMA) and small-angle X-ray scattering (SAXS). The adsorption abilities and adsorption kinetics of both the polymer and the s-PBC/GO nanocomposite were investigated for the removal of different heavy metal ions (Ni2+, Co2+, Cr3+ and Pb2+) from aqueous solutions containing the corresponding metal salts at different concentrations. The investigated s-PBC membrane shows a good efficiency, due to the presence of sulfonic groups that play a fundamental role in the adsorption process of metal ions. Its performance is further enhanced by embedding a very low amount of GO in the polymer allowing an increase by at least three times of the adsorption efficiencies of the polymer itself. This can be ascribed to the higher porosity, higher roughness and higher lamellar distances introduced by GO in the s-PBC membrane, as evidenced by the SEM and SAXS analysis. Both the polymeric materials showed the best performance in removing Pb2+ ions.

| S-EPMC7353454 | biostudies-literature

Alleviating the Mechanical and Thermal Degradations of Highly Sulfonated Poly(Ether Ether Ketone) Blocks via Copolymerization with Hydrophobic Unit for Intermediate Humidity Fuel Cells.

Project description:In this contribution, sulfonated poly(ether ether ketone) (SPEEK) is inter-connected using a hydrophobic oligomer via poly-condensation reaction to produce SPEEK analogues as PEMs. Prior sulfonation is performed for SPEEK to avoid random sulfonation of multi-block copolymers that may destroy the mechanical toughness of polymer backbone. A greater local density of ionic moieties exist in SPEEK and good thermomechanical properties of hydrophobic unit offer an unique approach to promote the proton conductivity as well as thermomechanical stability of membrane, as verify from AC impedance and TGA. The morphological behavior and phase variation of membranes are explored using FE-SEM and AFM; the triblock (XYX) membranes exhibits a nano-phase separated morphology. Performance of PEFC integrated with blend and block copolymer membranes is determined at 60 °C under 60% RH. As a result, the triblock (XYX) membrane has a high power density than blend (2X1Y) membrane.

| S-EPMC6401815 | biostudies-other

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