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- ItemSynthesis of High Crystalline TiO2 Nanoparticles on a Polymer Membrane to Degrade Pollutants from Water(Basel : MDPI, 2018-9-5) Fischer, Kristina; Schulz, Paulina; Atanasov, Igor; Abdul Latif, Amira; Thomas, Isabell; Kühnert, Mathias; Prager, Andrea; Griebel, Jan; Schulze, AgnesTitanium dioxide (TiO2) is described as an established material to remove pollutants from water. However, TiO2 is still not applied on a large scale due to issues concerning, for example, the form of use or low photocatalytic activity. We present an easily upscalable method to synthesize high active TiO2 nanoparticles on a polyethersulfone microfiltration membrane to remove pollutants in a continuous way. For this purpose, titanium(IV) isopropoxide was mixed with water and hydrochloric acid and treated up to 210 °C. After cooling, the membrane was simply dip-coated into the TiO2 nanoparticle dispersion. Standard characterization was undertaken (i.e., X-ray powder diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy, water permeance, contact angle). Degradation of carbamazepine and methylene blue was executed. By increasing synthesis temperature crystallinity and photocatalytic activity elevates. Both ultrasound modification of nanoparticles and membrane pre-modification with carboxyl groups led to fine distribution of nanoparticles. The ultrasound-treated nanoparticles gave the highest photocatalytic activity in degrading carbamazepine and showed no decrease in degradation after nine times of repetition. The TiO2 nanoparticles were strongly bound to the membrane. Photocatalytic TiO2 nanoparticles with high activity were synthesized. The innovative method enables a fast and easy nanoparticle production, which could enable the use in large-scale water cleaning.
- ItemThin film deposition using energetic ions(Basel : MDPI, 2010) Manova, D.; Gerlach, J.W.; Mändl, S.One important recent trend in deposition technology is the continuous expansion of available processes towards higher ion assistance with the subsequent beneficial effects to film properties. Nowadays, a multitude of processes, including laser ablation and deposition, vacuum arc deposition, ion assisted deposition, high power impulse magnetron sputtering and plasma immersion ion implantation, are available. However, there are obstacles to overcome in all technologies, including line-of-sight processes, particle contaminations and low growth rates, which lead to ongoing process refinements and development of new methods. Concerning the deposited thin films, control of energetic ion bombardment leads to improved adhesion, reduced substrate temperatures, control of intrinsic stress within the films as well as adjustment of surface texture, phase formation and nanotopography. This review illustrates recent trends for both areas; plasma process and solid state surface processes. © 2010 by the authors.
- ItemIncreased biocompatibility and bioactivity after energetic PVD surface treatments(Basel : MDPI, 2009) Mändl, S.Ion implantation, a common technology in semiconductor processing, has been applied to biomaterials since the 1960s. Using energetic ion bombardment, a general term which includes conventional ion implantation plasma immersion ion implantation (PIII) and ion beam assisted thin film deposition, functionalization of surfaces is possible. By varying and adjusting the process parameters, several surface properties can be attuned simultaneously. Extensive research details improvements in the biocompatibility, mainly by reducing corrosion rates and increasing wear resistance after surface modification. Recently, enhanced bioactivity strongly correlated with the surface topography and less with the surface chemistry has been reported, with an increased roughness on the nanometer scale induced by self-organisation processes during ion bombardment leading to faster cellular adhesion processes. © 2009 by the authors;.
- ItemIon Beam Assisted Deposition of Thin Epitaxial GaN Films(Basel : MDPI, 2017-6-23) Rauschenbach, Bernd; Lotnyk, Andriy; Neumann, Lena; Poppitz, David; Gerlach, Jürgen W.The assistance of thin film deposition with low-energy ion bombardment influences their final properties significantly. Especially, the application of so-called hyperthermal ions (energy <100 eV) is capable to modify the characteristics of the growing film without generating a large number of irradiation induced defects. The nitrogen ion beam assisted molecular beam epitaxy (ion energy <25 eV) is used to deposit GaN thin films on (0001)-oriented 6H-SiC substrates at 700 °C. The films are studied in situ by reflection high energy electron diffraction, ex situ by X-ray diffraction, scanning tunnelling microscopy, and high-resolution transmission electron microscopy. It is demonstrated that the film growth mode can be controlled by varying the ion to atom ratio, where 2D films are characterized by a smooth topography, a high crystalline quality, low biaxial stress, and low defect density. Typical structural defects in the GaN thin films were identified as basal plane stacking faults, low-angle grain boundaries forming between w-GaN and z-GaN and twin boundaries. The misfit strain between the GaN thin films and substrates is relieved by the generation of edge dislocations in the first and second monolayers of GaN thin films and of misfit interfacial dislocations. It can be demonstrated that the low-energy nitrogen ion assisted molecular beam epitaxy is a technique to produce thin GaN films of high crystalline quality.
- ItemBiocatalytic Self-Cleaning Polymer Membranes(Basel : MDPI, 2015) Schulze, Agnes; Stoelzer, Astrid; Striegler, Karl; Starke, Sandra; Prager, AndreaPolymer membrane surfaces have been equipped with the digestive enzyme trypsin. Enzyme immobilization was performed by electron beam irradiation in aqueous media within a one-step method. Using this method, trypsin was covalently and side-unspecific attached to the membrane surface. Thus, the use of preceding polymer functionalization and the use of toxic solvents or reagents can be avoided. The resulting membranes showed significantly improved antifouling properties as demonstrated by repeated filtration of protein solutions. Furthermore, the biocatalytic membrane can be simply “switched on” to actively degrade a fouling layer on the membrane surface and regain the initial permeability. The membrane pore structure (pore size and porosity) was neither damaged by the electron beam treatment nor blocked by the enzyme loading, ensuring a stable membrane performance.
- ItemCharge Separating Microfiltration Membrane with pH-Dependent Selectivity(Basel : MDPI, 2018-12-20) Breite, Daniel; Went, Marco; Prager, Andrea; Kuehnert, Mathias; Schulze, AgnesMembrane filters are designed for selective separation of components from a mixture. While separation by size might be the most common approach, other characteristics like charge can also be used for separation as presented in this study. Here, a polyether sulfone membrane was modified to create a zwitterionic surface. Depending on the pH value of the surrounding solution the membrane surface will be either negatively or positively charged. Thus, the charged state can be easily adjusted even by small changes of the pH value of the solution. Charged polystyrene beads were used as model reagent to investigate the pH dependent selectivity of the membrane. It was found that electrostatic forces are dominating the interactions between polystyrene beads and membrane surface during the filtration. This enables a complete control of the membrane’s selectivity according to the electrostatic interactions. Furthermore, differently charged beads marked with fluorescent dyes were used to investigate the selectivity of mixtures of charged components. These different components were successfully separated according to their charged state proving the selectivity of the invented membrane.
- ItemTailoring Membrane Surface Charges: A Novel Study on Electrostatic Interactions during Membrane Fouling(Basel : MDPI, 2015) Breite, Daniel; Went, Marco; Prager, Andrea; Schulze, AgnesIn this work we aim to show that the overall surface potential is a key factor to understand and predict anti-fouling characteristics of a polymer membrane. Therefore, polyvinylidene fluoride membranes were modified by electron beam-induced grafting reactions forming neutral, acidic, alkaline or zwitterionic structures on the membrane surface. The differently charged membranes were investigated regarding their surface properties using diverse analytical methods: zeta potential, static and dynamic water contact angle, scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). Porosimetry measurements proved that there is no pore blocking due to the modifications. Monodisperse suspensions of differently charged polystyrene beads were synthesized by a radical emulsion polymerization reaction and were used as a model fouling reagent, preventing comparability problems known from current literature. To simulate membrane fouling, different bead suspensions were filtered through the membranes. The fouling characteristics were investigated regarding permeation flux decline and concentration of model fouling reagent in filtrate as well as by SEM. By considering electrostatic interactions equal to hydrophobic interactions we developed a novel fouling test system, which enables the prediction of a membrane’s fouling tendency. Electrostatic forces are dominating, especially when charged fouling reagents are present, and can help to explain fouling characteristics that cannot be explained considering the surface wettability.
- ItemControlled electron-beam synthesis of transparent hydrogels for drug delivery applications(Basel : MDPI, 2019) Glass, Sarah; Kühnert, Mathias; Abel, Bernd; Schulze, AgnesIn this study, we highlight hydrogels prepared by electron-beam polymerization. In general, the electron-beam-polymerized hydrogels showed improved mechanical and optical transmittances compared to the conventional UV-cured hydrogels. They were more elastic and had a higher crosslinking density. Additionally, they were transparent over a broader wavelength range. The dependence of the mechanical and optical properties of the hydrogels on the number of single differential and total irradiation doses was analyzed in detail. The hydrogels were prepared for usage as a drug delivery material with methylene blue as a drug model. In the first set of experiments, methylene blue was loaded reversibly after the hydrogel synthesis. Electron-beam-polymerized hydrogels incorporated twice as much methylene blue compared to the UV-polymerized gels. Furthermore, the release of the model drug was found to depend on the crosslinking degree of the hydrogels. In addition, electron-beam polymerization enabled the irreversible binding of the drug molecules if they were mixed with monomers before polymerization.
- ItemWater softening using a light-responsive, spiropyran-modified nanofiltration membrane(Basel : MDPI, 2019) Das, Rasel; Kuehnert, Mathias; Sadat Kazemi, Asieh; Abdi, Yaser; Schulze, AgnesA novel technique for the covalent attachment of a light-responsive spiropyran onto polyamide thin film composite nanofiltration (NF) membranes in a one-step reaction using low-energy electron beam technology is described. The effect of illumination of the immobilized spiropyran was studied, as well as the resulting membrane properties with respect to MgSO4 retention, water permeability rate, and chlorine resistance. Electron beam irradiation showed a direct effect on the transformation of the rough PA NF membrane surface into a ridge-and-valley structure. Upon UV light irradiation, the spiropyran transformed into zwitterionic merocyanine, which had shown MgSO4 removal of >95% with water permeation rates of 6.5 L/(m2·h·bar). Alternatively, visible light was used to convert merocyanine to spiropyran, which achieved >95% of MgSO4 retention with a water flux of around 5.25 L/(m2·h·bar). The modified NF membranes showed higher chlorine resistance as well as a higher normalized water flux as compared to the reference membrane, without a loss of ion retention. All the NF membranes were characterized by scanning electron microscopy and X-ray photoelectron spectroscopy. This study demonstrates a simple and inexpensive method for the immobilization of molecules onto polymeric membranes, which may be applied in water softening.
- ItemBio-Inspired Polymer Membrane Surface Cleaning(Basel : MDPI, 2017-3-9) Schulze, Agnes; Breite, Daniel; Kim, Yongkyum; Schmidt, Martin; Thomas, Isabell; Went, Marco; Fischer, Kristina; Prager, AndreaTo generate polyethersulfone membranes with a biocatalytically active surface, pancreatin was covalently immobilized. Pancreatin is a mixture of digestive enzymes such as protease, lipase, and amylase. The resulting membranes exhibit self-cleaning properties after “switching on” the respective enzyme by adjusting pH and temperature. Thus, the membrane surface can actively degrade a fouling layer on its surface and regain initial permeability. Fouling tests with solutions of protein, oil, and mixtures of both, were performed, and the membrane’s ability to self-clean the fouled surface was characterized. Membrane characterization was conducted by investigation of the immobilized enzyme concentration, enzyme activity, water permeation flux, fouling tests, porosimetry, X-ray photoelectron spectroscopy, and scanning electron microscopy.