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Fabrication, Characterization and Application of Organic/Inorganic Film Membranes and Advanced Materials

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A special issue of Membranes (ISSN 2077-0375). This special issue belongs to the section "Membrane Surfaces and Interfaces".

Deadline for manuscript submissions: closed (10 July 2022) | Viewed by 21090

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Dr. Elena Kalinina

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1. Laboratory of Complex Electrophysic Investigations, Institute of Electrophysics, Ural Branch, Russian Academy of Sciences, Yekaterinburg 620016, Russia
2. Department of Physical and Inorganic Chemistry, Institute of Natural Sciences and Mathematics, Ural Federal University, Yekaterinburg 620002, Russia
Interests: solid oxide fuel cells (SOFC); thin-film technology; electrophoretic deposition (EPD); stable suspensions; nanoscale materials; electrochemical properties
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Dear Colleagues,

We would like to invite you to submit your works to a Special Issue “Fabrication, Characterization and Application of Organic/Inorganic Film Membranes and Advanced Materials”. The purpose of this Special Issue is to present the latest experimental and theoretical developments in the application of organic/inorganic membranes based on new functional materials. Authors are invited to submit their latest results; both original research papers and reviews are welcome. Topics of interest include but are not limited to:

Development of methods for producing organic/inorganic membranes, including physical vacuum deposition technologies such as magnetron deposition, pulsed laser deposition, and chemical vapor deposition as well as electrochemical methods, ceramic and solution technologies, etc.

Application of organic/inorganic membranes in devices for energy production, conversion and storage (fuel cells, batteries, supercapacitors, electrolyzers); chemical sensors; MEMS devices; and catalytic reactors.

3D printing and additive manufacturing for the formation of membrane film structures.

Promising materials for the production of organic/inorganic membranes; ion-conductive materials, proton-conductive materials; and metal, semiconductor, dielectric, and piezo materials.

Methods for obtaining promising nanostructured and composite membrane materials.

Dr. Elena Kalinina
Guest Editor

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Membranes is an international peer-reviewed open access monthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2700 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

thin-film technology
organic/inorganic film membranes
electrophoretic deposition
membranes for energy conversion and storage
fuel cells
membrane materials
membrane fabrication

Published Papers (9 papers)

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Research

16 pages, 7581 KiB

Open AccessArticle

A Proton Battery Stack Real-Time Monitor with a Flexible Six-in-One Microsensor

by Chi-Yuan Lee, Chia-Hung Chen, Yun-Hsiu Chien and Zhi-Yu Huang

Membranes 2022, 12(8), 779; https://doi.org/10.3390/membranes12080779 - 13 Aug 2022

Cited by 2 | Viewed by 1360

Abstract

A proton battery is a hybrid battery produced by combining a hydrogen fuel cell and a battery system in an attempt to obtain the advantages of both systems. As the battery life of a single proton battery is not good, the proton battery stack is developed by connecting in parallel, which can greatly improve the battery life of proton batteries. In order to obtain important information about the proton battery stack in real time, a flexible six-in-one microsensor is embedded in the proton battery stack. This study has successfully developed a health diagnostic tool for a proton battery stack using micro-electro-mechanical systems (MEMS) technology. This study also focused on the innovatively developed hydrogen microsensor, and integrated the voltage, current, temperature, humidity, and flow microsensors, as previously developed by our laboratory, to complete the flexible six-in-one microsensor. Six important internal physical parameters were simultaneously measured during the entire operation of the proton battery stack. It also established a complete database and monitor system in real time to detect the internal health status of the proton cell stack and observe if there were problems, such as water accumulation, aging, or failure, in order to understand the changes and effects of the various physical quantities of long-term operation. The study found that the proton batteries exhibited significant differences in the hydrogen absorb rates and hydrogen release rates. The ceramic circuit board used in the original sensor is replaced by a flexible board to improve problems such as peeling and breaking. Full article

(This article belongs to the Special Issue Fabrication, Characterization and Application of Organic/Inorganic Film Membranes and Advanced Materials)

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19 pages, 7108 KiB

Open AccessArticle

Direct Electrophoretic Deposition and Characterization of Thin-Film Membranes Based on Doped BaCeO₃ and CeO₂ for Anode-Supported Solid Oxide Fuel Cells

by Elena Pikalova, Denis Osinkin and Elena Kalinina

Membranes 2022, 12(7), 682; https://doi.org/10.3390/membranes12070682 - 30 Jun 2022

Cited by 13 | Viewed by 1784

Abstract

In this work, a technology was developed for the formation of BaCe_0.8Sm_0.2O₃+1 wt% CuO (BCS-CuO)/Ce_0.8Sm_0.2O_1.9 (SDC) thin-film electrolyte membranes for intermediate-temperature solid oxide fuel cells (IT-SOFCs) on porous NiO-BCS-CuO anode substrates using direct electrophoretic deposition (EPD). The effect of increasing the zeta potential when modifying the base suspension of a micro-sized SDC-gn powder (glycine–nitrate method) with the addition of a SDC-lec nanopowder (laser evaporation–condensation) was investigated. Dependences of the current strength on the deposition time and the deposited weight on the EPD voltage were obtained, and evolution of the morphology of the coatings during the modification of the SDC-gn suspension and a suspension of BCS-CuO powder was studied. The compatibility of the shrinkage kinetics of the SDC, the BCS-CuO electrolyte coatings and the NiO-BCS-CuO anode substrate was studied during the high-temperature sintering. Dense BCS-CuO/SDC films of different thicknesses were obtained for the first time on porous NiO-BCS-CuO anode substrates and comprehensive microstructural and electrochemical studies were carried out. The developed technology can be applied to the formation of anode-supported SOFCs with thin-film electrolyte membranes. Full article

(This article belongs to the Special Issue Fabrication, Characterization and Application of Organic/Inorganic Film Membranes and Advanced Materials)

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14 pages, 5582 KiB

Open AccessArticle

Influence of Deposition Modes and Thermal Annealing on Residual Stresses in Magnetron-Sputtered YSZ Membranes

by Andrey Solovyev, Sergey Rabotkin, Anna Shipilova, Dmitrii Agarkov, Ilya Burmistrov and Alexander Shmakov

Membranes 2022, 12(3), 346; https://doi.org/10.3390/membranes12030346 - 19 Mar 2022

Cited by 3 | Viewed by 2143

Abstract

Thin-film electrolyte made of 8-mol% yttria stabilized zirconia (8YSZ) for solid oxide fuel cells (SOFCs) was fabricated on anode substrates using reactive magnetron sputtering of Zr-Y targets in a mixture of Ar and O₂ gases. The deposition of 4–6 µm thin-film electrolyte was in the transition or oxide modes differing by the oxygen concentration in the sputtering atmosphere. The half-cell bending of the anode-supported SOFCs was measured to determine the residual stresses in the electrolyte films after the deposition and thermal annealing in air. The dependences were studied between the deposition modes, residual stresses in the films, and the SOFC performance. At 800 °C, the maximum power density of SOFCs ranged between 0.58 and 1.2 W/cm² depending on the electrolyte deposition mode. Scanning electron microscopy was carried out to investigate the surface morphology and structure of the YSZ electrolyte films after thermal annealing. Additionally, an X-ray diffraction analysis of the YSZ electrolyte films was conducted for the synchrotron radiation beam during thermal annealing at different temperatures up to 1300 °C. It was found that certain deposition modes provide the formation of the YSZ electrolyte films with acceptable residual stresses (<1 GPa) at room temperature, including films deposited on large area anodes (100 × 100 mm²). Full article

(This article belongs to the Special Issue Fabrication, Characterization and Application of Organic/Inorganic Film Membranes and Advanced Materials)

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13 pages, 3404 KiB

Open AccessArticle

Synthesis of Nanocomposite TiSiCN Coatings by Titanium Evaporation and Organosilicon Compound Activation in Hollow Cathode Arc Discharge

by Andrey I. Menshakov, Yulia A. Bruhanova, Andrey I. Kukharenko and Ivan S. Zhidkov

Membranes 2022, 12(3), 321; https://doi.org/10.3390/membranes12030321 - 12 Mar 2022

Cited by 3 | Viewed by 2313

Abstract

TiSiCN coatings have been obtained by anode evaporation of titanium and the decomposition of hexamethyldisilazane in an arc discharge, using a self-heated hollow cathode, at the pressure rate of 1 mTorr of the Ar+N₂ gas mixture. The proposed method makes it possible to independently and widely change the amount of metal and precursor vapor flows, the pressure and composition of the vapor-gas mixture and the degree of ionic interaction on the surface of the growing coating within a single discharge system. The paper presents the method and the results of the effect of a current discharge (10–50 A), and the flux of precursor vapours (0–1 g/h), on deposition rates, compositions, and properties of TiSiCN coatings deposited by an advanced combined PVD+PECVD method. Dense homogeneous TiSiCN coatings up to 6 µm thick and up to 27.5 GPa in hardness were obtained at 7.5 µm/h. The composition of the obtained coatings has been studied by X-ray diffraction and X-ray photoelectron spectroscopy, and it has been shown that the presented methods can form nanocomposite coatings with nanocrystallites TiC, TiN, and TiC_xN_1−x 3–10 nm in the amorphous matrix based on SiCN. Full article

(This article belongs to the Special Issue Fabrication, Characterization and Application of Organic/Inorganic Film Membranes and Advanced Materials)

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19 pages, 6440 KiB

Open AccessArticle

Electrophoretic Deposition and Characterization of the Doped BaCeO₃ Barrier Layers on a Supporting Ce_0.8Sm_0.2O_1.9 Solid-State Electrolyte

by Elena Kalinina, Kirill Shubin and Elena Pikalova

Membranes 2022, 12(3), 308; https://doi.org/10.3390/membranes12030308 - 09 Mar 2022

Cited by 11 | Viewed by 2276

Abstract

In this study, the technology of electrophoretic deposition (EPD) micrometer barrier layers based on a BaCe_0.8Sm_0.19Cu_0.1O₃ (BCSCuO) protonic conductor on dense carrying Ce_0.8Sm_0.2O_1.9 (SDC) solid-state electrolyte substrates is developed. Methods for creating conductive sublayers on non-conductive SDC substrates under EPD conditions, such as the synthesis of a conductive polypyrrole (PPy) layer and deposition of a layer of finely dispersed platinum from a suspension of its powder in isopropanol, are proposed. The kinetics of disaggregation, disperse composition, electrokinetic potential, and the effect of adding iodine to the BCSCuO suspension on these parameters as factors determining the preparation of stable suspensions and successful EPD processes are explored. Button cells based on a carrying SDC electrolyte of 550 μm in thickness with BCSCuO layers (8–35 μm) on the anode, cathode, and anode/cathode side, and Pt electrodes are electrochemically tested. It was found that the effect of blocking the electronic current in the SDC substrate under OCV conditions was maximal for the cells with barrier layers deposited on the anode side. The technology developed in this study can be used to fabricate solid oxide fuel cells with doped CeO₂ electrolyte membranes characterized by mixed ionic–electronic conductivity (MIEC) under reducing atmospheres. Full article

(This article belongs to the Special Issue Fabrication, Characterization and Application of Organic/Inorganic Film Membranes and Advanced Materials)

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19 pages, 4418 KiB

Open AccessArticle

A High-Durability Graphitic Black Pearl Supported Pt Catalyst for a Proton Exchange Membrane Fuel Cell Stack

by Bing Li, Meng Xie, Kechuang Wan, Xiaolei Wang, Daijun Yang, Zhikun Liu, Tiankuo Chu, Pingwen Ming and Cunman Zhang

Membranes 2022, 12(3), 301; https://doi.org/10.3390/membranes12030301 - 07 Mar 2022

Cited by 5 | Viewed by 2823

Abstract

Graphitized black pearl (GBP) 2000 supported Pt nanoparticle catalysts is synthesized by a formic acid reduction method. The results of a half-cell accelerated degradation test (ADT) of two protocols and a single-cell ADT show that, Pt/GBP catalyst has excellent stability and durability compared with commercial Pt/C. Especially, the survival time of Pt/GBP-membrane electrode assembly (MEA) reaches 205 min, indicating that it has better reversal tolerance. After the 1003-hour durability test, the proton exchange membrane fuel cell (PEMFC) stack with Pt/GBP presents a slow voltage degradation rate of 5.19% and 36 μV h⁻¹ at 1000 mA cm⁻². The durability of the stack is improved because of the durability and stability of the catalyst. In addition, the post morphology characterizations indicate that the structure and particle size of the Pt/GBP catalyst remain unchanged during the dynamic testing protocol, implying its better stability under dynamic load cycles. Therefore, Pt/GBP is a valuable and promising catalyst for PEMFC, and considered as an alternative to classical Pt/C. Full article

(This article belongs to the Special Issue Fabrication, Characterization and Application of Organic/Inorganic Film Membranes and Advanced Materials)

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16 pages, 3490 KiB

Open AccessArticle

Investigation of NH₃ Desorption Kinetics on the LTA and SOD Zeolite Membranes

by Natalya E. Gordina, Tatyana N. Borisova, Ksenya S. Klyagina, Irina A. Astrakhantseva, Alexander A. Ilyin and Ruslan N. Rumyantsev

Membranes 2022, 12(2), 147; https://doi.org/10.3390/membranes12020147 - 25 Jan 2022

Cited by 5 | Viewed by 2561

Abstract

The acidity characteristics of zeolite are highly significant, and understanding the acidic properties is essential for developing new types of zeolite catalysts. Zeolite membranes were synthesized using metakaolin, sodium hydroxide, and alumina with a molar ratio of 6Al₂Si₂O₇:12NaOH:2Al₂O₃ as the starting ingredients. X-ray diffraction, scanning electron microscopy, and infrared spectroscopy were used for this study. N₂ adsorption measurements determined the surface areas of the SOD zeolite membrane (115 m²/g) and the LTA membrane (150 m²/g). The units of absorbed water vapor were 40 and 60 wt% for the SOD membrane and the LTA membrane, respectively. The strength and number of acid sites of the synthesized LTA and SOD zeolite membranes were determined by temperature-programmed desorption of ammonia. As a result, the value of the total acidity of the LTA zeolite membrane is in the range of 0.08 × 10¹⁹ units/m² while that of the sodalite membrane is an order of magnitude lower and is 0.006 × 10¹⁹ units/m². The apparent activation energy values for desorption of ammonia from LTA and SOD zeolite membranes were calculated using data on the kinetics of desorption of ammonia at different heating rates. It was found that at temperatures below 250 °C, the degree of conversion of the activation energy values is no more than 35 kJ/mol, which corresponds to the desorption of physically bound ammonia. An increase in the activation values up to 70 kJ/mol (for SOD) and up to 80 kJ/mol (for LTA) is associated with the desorption of chemically bound ammonia from the samples. Full article

(This article belongs to the Special Issue Fabrication, Characterization and Application of Organic/Inorganic Film Membranes and Advanced Materials)

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12 pages, 4543 KiB

Open AccessArticle

Synthesis of Lithium Phosphorus Oxynitride (LiPON) Thin Films by Li₃PO₄ Anodic Evaporation in Nitrogen Plasma of a Low-Pressure Arc Discharge

by Nikolay Gavrilov, Alexander Kamenetskikh, Petr Tretnikov, Alexey Nikonov, Leonid Sinelnikov, Denis Butakov, Viktor Nikolkin and Andrey Chukin

Membranes 2022, 12(1), 40; https://doi.org/10.3390/membranes12010040 - 28 Dec 2021

Cited by 6 | Viewed by 1858

Abstract

Thin amorphous films of LiPON solid electrolyte were prepared by anodic evaporation of lithium orthophosphate Li₃PO₄ in an arc discharge with a self-heating hollow cathode at a nitrogen pressure of 1 Pa. Distribution of the arc current between two electrodes having an anode potential provided independent control of the evaporation rate of Li₃PO₄ and the density of nitrogen plasma. Stabilization of the evaporation rate was achieved using a crucible with multi-aperture cover having floating potential. The existence of a threshold value of discharge current (40 A) has been established, which, upon reaching ionic conductivity over 10⁻⁸ S/cm, appears in the films. Probe diagnostics of discharge plasma were carried out. It has been shown that heating the films during deposition by plasma radiation to a temperature of 200 °C is not an impediment to achieving high ionic conductivity of the films. Dense uniform films of LiPON thickness 1 μm with ionic conductivity up to 1 × 10⁻⁶ S/cm at a deposition rate of 4 nm/min are obtained. Full article

(This article belongs to the Special Issue Fabrication, Characterization and Application of Organic/Inorganic Film Membranes and Advanced Materials)

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18 pages, 6240 KiB

Open AccessArticle

Preparation of Sodalite and Faujasite Clay Composite Membranes and Their Utilization in the Decontamination of Dye Effluents

by Abderrazek El-kordy, Abdelaziz Elgamouz, El Mokhtar Lemdek, Najib Tijani, Salman S. Alharthi, Abdel-Nasser Kawde and Ihsan Shehadi

Membranes 2022, 12(1), 12; https://doi.org/10.3390/membranes12010012 - 23 Dec 2021

Cited by 18 | Viewed by 2693

Abstract

The present work describes the deposition of two zeolite films, sodalite and faujasite, by the hydrothermal method to tune the mesopores of clay support, which are prepared from a widely available clay depot from the central region of Morocco (Midelt). The clay supports were prepared by a powder metallurgy method from different granulometries with activated carbon as a porosity agent, using uniaxial compression followed by a sintering process. The 160 µm ≤ Φ ≤ 250 µm support showed the highest water flux compared to the supports made from smaller granulometries with a minimum water flux of 1405 L.m⁻²·h⁻¹ after a working time of 2 h and 90 min. This support was chosen for the deposition of sodalite (SOM) and faujasite (FAM) zeolite membranes. The X-ray diffraction of sodalite and faujasite showed that they were well crystallized, and the obtained spectra corresponded well with the sought phases. Such findings were confirmed by the SEM analysis, which showed that SOM was crystalized as fine particles while the FAM micrographs showed the existence of crystals with an average size ranging from 0.53 µm to 1.8 µm with a bipyramidal shape and a square or Cubo octahedral base. Nitrogen adsorption analysis showed that the pore sizes of the supports got narrowed to 2.28 nm after deposition of sodalite and faujasite. The efficiencies of SOM and FAM membranes were evaluated by filtration tests of solutions containing methyl orange (MO) using a flow loop, which were developed for dead-end filtration. The retention of methylene orange (MO) followed the order: SOM > FAM > 160 µm ≤ Φ ≤ 250 µm clay support with 55%, 48% and 35%, respectively. Size exclusion was the predominant mechanism of filtration of MO through SOM, FAM, and the support. However, the charge repulsion between the surface of the membrane and the negatively charged MO have not been ruled out. The point of zero charge (pzc) of the clay support, SOM and FAM membrane were pHpzc = 9.4, pHpzc = 10.6, and pHpzc = 11.4, respectively. Filtrations of MO were carried out between pH = 5.5 and pH = 6.5, which indicated that the surface of the membranes was positively charged while MO was negatively charged. The interaction of MO with the membranes might have happened through its vertical geometry. Full article

(This article belongs to the Special Issue Fabrication, Characterization and Application of Organic/Inorganic Film Membranes and Advanced Materials)

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