TY - CONF A1 - Baier, Jennifa A1 - Beck, Uwe A1 - Hidde, Gundula A1 - Hielscher, Stefan A1 - Lange, Thorid A1 - Mix, Renate T1 - Plasmagestützte Oberflächenfunktionalisierung von Polypropylen (PP) N2 - Polypropylen (PP) ist als Niedrigenergie-Polymer ohne nass- und plasmachemische Vorbehandlung weder haftfest zu beschichten noch verbundfest zu kleben. Typische Haft- bzw. Klebfestigkeiten liegen für die unbehandelte Polymeroberfläche bei maximal 0,5 MPa. Hinzu kommt, dass bei der Bestimmung von Haft- und Klebfestigkeiten der unmodifizierten Oberfläche mit großen Streuungen zu rechnen ist, die bezogen auf die Spannweite durchaus einem Faktor 5 entsprechen können. Generell besteht bei Prüfung der Haftfestigkeit mittels Stirnabzugsversuch und bei der Prüfung der Klebfestigkeit die Notwendigkeit eines statistisch validierten Herangehens. Hierzu sind zeitaufwändige Ein-Proben-Klebungen und -Prüfungen nur eingeschränkt geeignet. Zudem ist, insbesondere für geringe Haft- bzw. Klebfestigkeiten, ein querkraftfreies Prüfen Grundvoraussetzung. Im vorliegenden Beitrag werden verschiedenartige plasmagestützte Oberflächenfunktionalisierungen von PP sowie das Mehr-Proben-Konzept zur Klebung/Prüfung von bis zu acht Proben vorgestellt. Dazu werden ein BAM-Funktionsmuster einer Mehr-Proben-Kleb-Vorrichtung und eine kommerzielle analytische Zentrifuge zum Prüfen verwendet. T2 - 24. Workshop des Anwenderkreises Atmosphärendruckplasma "Haftung durch Oberflächenfunktionalisierung" CY - Erfurt, Germany DA - 11.11.2015 KW - Plasmamodifizierung KW - Polypropylen KW - Haftfestigkeit KW - Klebfestigkeit KW - Mehr-Proben-Kleben/-Prüfen PY - 2015 SP - 1 EP - 6 PB - Anwenderkreis Atmosphärendruckplasma CY - Jena AN - OPUS4-34838 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beck, Uwe A1 - Baier, Jennifa A1 - Hidde, Gundula A1 - Hielscher, Stefan A1 - Kittler-Packmor, Kai A1 - Lange, Thorid A1 - Mix, Renate A1 - Weise, Matthias T1 - Multiple-sample approach: reliable ranking and validated statistics of bonding and adhesive strength N2 - Bonding strength of adhesive-bonded joints and adhesive strength of coatings have been exclusively determined in single-sample tests using a tensile testing machine. Necessarily, the single-sample approach was also applied to the corresponding bonding procedure. As a consequence, reliability and reproducibility of results were restricted. By applying the newly introduced centrifuge technology, the multiple-sample approach was realized for simultaneous tensile testing of up to eight samples under identical conditions without any disturbing shear-force effects. In order to introduce the multiple-sample approach into the bonding procedure, a hydraulic bonding set-up was developed which enables identical bonding pressure also for slightly different heights of sample assemblies. Both sample approaches were compared for various application examples: ranking of different classes of adhesives, validated statistics of adhesive-bonded joints using one particular adhesive and effects of cleaning and plasma-treatment on the adhesive strength of coatings. The investigated systems included glass, metals and polymer substrates, different adhesives, metallic and dielectric coatings on polymers. KW - Bonding strength KW - Adhesive strength KW - Multi-sample approach KW - Centrifuge technology PY - 2014 SN - 978-3-944261-28-7 SN - 978-3-944261-36-2 SN - 978-3-944261-52-2 VL - 5 SP - 1 EP - 5 AN - OPUS4-31310 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Baier, Jennifa A1 - Hidde, Gundula A1 - Hielscher, Stefan A1 - Kittler-Packmor, Kai A1 - Lange, Thorid A1 - Mix, Renate A1 - Weise, Matthias T1 - Multiple-sample approach: reliable ranking and validated statistics of bonding and adhesive strength N2 - Bonding strength of adhesive-bonded joints and adhesive strength of coatings have been exclusively determined in single-sample tests using a tensile testing machine. Necessarily, the single-sample approach was also applied to the corresponding bonding procedure. As a consequence, reliability and reproducibility of results were restricted. By applying the newly introduced centrifuge technology, the multiple-sample approach was realized for simultaneous tensile testing of up to eight samples under identical conditions without any disturbing shear-force effects. In order to introduce the multiple-sample approach into the bonding procedure, a hydraulic bonding set-up was developed which enables identical bonding pressure also for slightly different heights of sample assemblies. Both sample approaches were compared for various application examples: ranking of different classes of adhesives, validated statistics of adhesive-bonded joints using one particular adhesive and effects of cleaning and plasma-treatment on the adhesive strength of coatings. The investigated systems included glass, metals and polymer substrates, different adhesives, metallic and dielectric coatings on polymers. T2 - EURADH 2014 - 10th European Adhesion Conference CY - Alicante, Spain DA - 22.04.2014 KW - Bonding strength KW - Adhesive strength KW - Multi-sample approach KW - Centrifuge technology PY - 2014 SN - 978-84-616-9067-1 SN - 84-616-9067-2 SP - Paper 49, 211 EP - 214 AN - OPUS4-31309 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mix, Renate A1 - Friedrich, Jörg Florian A1 - Neubert, Dietmar A1 - Inagaki, N. T1 - Response of linear, branched or crosslinked polyethylene structures on the attack of oxygen plasma N2 - Linear, branched and crosslinked polyethylenes (PE) were exposed to the low-pressure oxygen plasma for 2–120 s. In the following the samples were washed with solvents to remove low-molecular weight oxidized material and to excavate the subjacent polymer structure for microscopic characterization. X-ray photoelectron spectroscopy (XPS) measurements provided information about changes in elemental composition and chemical structure of PE after plasma exposure and washing. The calculation of the concentration of tertiary C atoms using XPS data was a measure of branches and crosslinking in the polymer before and after exposure to oxygen plasma. Linear PE was most sensitive towards oxygen plasma and showed the highest concentration in tertiary C atoms after plasma exposure. On the other hand branched PE types, which possess originally more tertiary carbon atoms, have lost two-third of them after 2 s oxygen plasma exposure. Branched PE show also topological changes at their surface as detected by atomic force microscopy. Differential scanning calorimetry measurements confirmed strong changes in crystallinity and molecular orientation of linear PE already after 120 s exposure to the oxygen plasma interpreted as amorphization. These effects should be interpreted as result of crosslinking caused by the recombination of dangling bond sites. KW - Linear and branched polyethylene KW - Oxygen plasma KW - Functionalization KW - Crosslinking PY - 2014 UR - http://link.springer.com/article/10.1007%2Fs11090-014-9558-9/fulltext.html DO - https://doi.org/10.1007/s11090-014-9558-9 SN - 0272-4324 VL - 34 IS - 5 SP - 1199 EP - 1218 PB - Plenum Publ. Corp. CY - New York, NY, USA AN - OPUS4-30741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H.R. A1 - Mix, Renate A1 - Weidner, Steffen T1 - Poly(ester urethane)s derived from lactide, isosorbide, terephthalic acidm abd various diisocyanates N2 - Isosorbide-initiated oligomerizations of ʟ-lactide were preformed in bulk using SnCl2 as catalyst. The resulting telechelic OH-terminated oligoesters were in situ subjected to simultaneous polycondensation and polyaddition with mixtures of terephthaloyl chloride and diisocyanates. Most polymerizations were conducted with 4,4'-diisocyanatodiphenyl methane and 2,4-diisocyanato toluene. The consequences of excess diisocyanate and four different catalysts were studied. The isosorbide/lactide ratio and the terephthalic acid/diisocyanate ratio were varied. Number average molecular weights up to 15 kDa with polydispersities around 3–5 were obtained. Depending on the chemical structure of the copolyester and on the feed ratio, incorporation of urethane groups may reduce or enhance the glass-transition temperature, but the thermal stability decreases dramatically regardless of composition. KW - Cyclization KW - Isosorbide KW - Lactide KW - Polyaddition KW - Polycondensation KW - Polyesters KW - Polyurethanes PY - 2014 DO - https://doi.org/10.1002/pola.27069 SN - 0360-6376 SN - 0887-624X VL - 52 IS - 6 SP - 867 EP - 875 PB - Wiley CY - Hoboken, NJ AN - OPUS4-30299 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Mix, Renate A1 - Friedrich, Jörg Florian A1 - Inagaki, N. ED - Thomas, M. ED - Mittal, K.L. T1 - Permanence of functional groups at polyolefin surfaces introduced by dielectric barrier discharge pretreatment in presence of aerosols N2 - A convenient way to overcome the chemical inertness of polyolefin surfaces is to expose them to the atmospheric air plasma of a dielectric barrier discharge (DBD). To improve the efficiency in formation of polar groups at the polyolefin surface, different liquids such as water and ethanol were sprayed as aerosol into the plasma zone between the powered electrode and the polyolefin surface. Both sprayed liquids as well as the polyolefin surface were simultaneously activated; thus, the formation of different functional groups at the polyolefin surface was realized. The type of aerosol-sprayed additive, exposure time, power etc. have been found to determine the efficiency with respect to introduction of polar groups. KW - PE KW - PP KW - Surface modification KW - Aerosol-assisted DBD PY - 2013 SN - 978-1-118-59621-0 DO - https://doi.org/10.1002/9781118747308.ch4 N1 - Serientitel: Adhesion and Adhesives: Fundamental and applied aspects – Series title: Adhesion and Adhesives: Fundamental and applied aspects IS - Part 1 / Chapter 4 SP - 131 EP - 156 PB - Wiley AN - OPUS4-28657 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Friedrich, Jörg Florian A1 - Mix, Renate T1 - Combination of plasma-chemical and wet-chemical processes - a simple way to optimize interfaces in metal-polymer composites for maximal adhesion N2 - Different surface treatments of polypropylene (PP) were tested to improve the peel strength of aluminium-PP systems. Plasma exposure followed by chemical grafting of spacers with -SiOH endgroups and thin adhesion promoting layers deposited by aerosol-assisted DBD using aqu. solutions of classic polymers were compared. Both methods were effective, however, –SiOH terminated spacers effected no peeling also after ageing. T2 - ISPC 21 - 21st International Symposium on Plasma Chemistry CY - Cairns, QLD, Australia DA - 2013-08-02 KW - Adhesion polypropylene-aluminium KW - Tailored interface structures KW - Aerosol-assisted DBD PY - 2013 UR - http://www.ispc-conference.org/ispcproc/ispc21/ID549.pdf SP - Paper 549, 1 EP - 4 AN - OPUS4-28661 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fahmy, A. A1 - Mix, Renate A1 - Schönhals, Andreas A1 - Friedrich, Jörg Florian T1 - Structure of plasma-deposited copolymer films prepared from acrylic acid and styrene: Part II variation of the comonomer ratio N2 - Copolymers of acrylic acid and styrene (AA/S) were prepared by pulsed plasma deposition technique. Their structure–property relationships were studied in dependence on the comonomer ratio. Both, the regularity of the structure and the composition of the thin copolymer films were investigated by bulk-sensitive (dielectric spectroscopy, FTIR, and differential scanning calorimetry) as well as surface-sensitive methods such as X-ray photoelectron spectroscopy (XPS). For an unambiguous identification of the functionality of the deposited films the COOH groups were estimated by derivatization with trifluoroethanol and subsequent XPS measurement as well as by the quantitative analysis of the FTIR data. As a result, the concentration of COOH groups on the surface and in the bulk is increasing with the fraction of AA in precursor mixture in a non-monotonous way but similar to the dependence obtained by conventional free radical polymerization. KW - Acrylic acid-styrene copolymer KW - Bulk properties KW - Dielectric properties KW - Plasma polymerization KW - Surface functionalization PY - 2013 DO - https://doi.org/10.1002/ppap.201200110 SN - 1612-8850 SN - 1612-8869 VL - 10 IS - 9 SP - 750 EP - 760 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-29096 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mix, Renate A1 - Hielscher, Stefan A1 - Beck, Uwe A1 - Friedrich, Jörg F. T1 - Adhesion Promotion in Aluminium Polypropylene Composites Measured by Peel test and Centrifuge technology T2 - 19th International Vacuum Congress (IVC-19) CY - Paris, France DA - 2013-09-09 PY - 2013 AN - OPUS4-29552 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Mix, Renate A1 - Yin, Huajie A1 - Friedrich, Jörg Florian ED - Gutowski, W. ED - Dodiuk, H. T1 - Aerosol-based DBD - A simple way to provide polymers with functional groups for adhesion promotion N2 - Polypropylene (PP) foils were exposed to the plasma of an atmospheric dielectric barrier discharge (DBD) in presence of different aerosols. Pure liquids such as water, ethanol, and 1/1 mixtures ethanol/water (v/v) or aqueous Solutions of acetic acid, poly(acrylic acid), poly(vinyl alcohol), and ethylene glycolpoly(vinyl alcohol) copolymer were introduced into the DBD. Surface composition, the number of functional groups per 100 C atoms, and water contact angles were correlated with the energy density of DBD plasma exposure. The wettability of the treated surfaces was investigated for different storage times. Peel strength of the thermally deposited aluminum layer to modified polymer surfaces revealed that the aerosol introduction strongly improves the adhesion between aluminum and polypropylene. KW - Aerosol-assisted DBD KW - Functional groups KW - Surface modification PY - 2013 SN - 978-90-04-20173-6 SN - 978-90-04-20174-3 SP - Chapter 8, 155 EP - 170 PB - CRC Press AN - OPUS4-30035 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ramanujam, Maalolan A1 - Mix, Renate A1 - Wagner, M. A1 - Friedrich, Jörg Florian T1 - Effect of Br gassing after Ar plasma treatment of polyolefins N2 - For simulation and acceleration of artificial polymer ageing, polyolefin foils were exposed to low-pressure Ar plasma. Plasma particle bombardment and irradiation induce C–C and C–H bond scissions by σ→σ* excitations on the surface and in near-surface layers. Consequently, radicals are generated. They react by recombination, cross-linking, metastable trapping of the radical site or formation of olefinic double bonds. The long-living and metastable trapped C-radicals as well as double bonds in polyolefins were immediately exposed to bromine vapour without breaking the vacuum after switching-off the plasma. These reactive sites rapidly react with the molecular bromine under formation of C–Br bonds. For 5 min of argon plasma exposure, the elemental concentration of bromine was 13% for polyethylene and 22% Br/C for polypropylene as analysed by X-ray photoelectron spectroscopy. Nevertheless, not all C radical sites have reacted with bromine. Later on, when the polyolefins brought in contact with ambient air, an additional post-plasma reaction of the remaining trapped radicals with oxygen was observed. The oxygen concentrations were lower after bromine gassing, thus repressing partially the post-plasma oxidation in the analysed layer (ca. 6 nm) by radical quenching. Such bromination took place either at the surface or in near-surface layers because the Attenuated Total Reflectance (ATR)-FTIR spectra (sampling depth ca. 2500 nm) did not show significant changes for argon plasma-treated PE foils with and without bromine vapour exposure. Further addition of bromine may also occur on C=C double bonds. KW - Ageing of polyolefins KW - Argon plasma KW - Radical formation KW - Formation of double bonds PY - 2013 DO - https://doi.org/10.1080/01694243.2012.762326 SN - 0169-4243 SN - 1568-5616 VL - 27 IS - 6 SP - 1828 EP - 1839 PB - VNU Science Press CY - Utrecht AN - OPUS4-30572 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fahmy, A. A1 - Mix, Renate A1 - Schönhals, Andreas A1 - Friedrich, Jörg Florian T1 - Structure of plasma-deposited copolymer films prepared from acrylic acid and styrene: Part I dependence on the duty cycle N2 - Copolymers of acrylic acid and styrene (AA/S) were prepared by pulsed plasma deposition and their structures were studied in dependence on the duty cycle (DC) for a fixed composition of 1:1. As a result, low values of DC doses preserve the structure of monomers in the plasma deposited polymers while high DC leads to a higher degree of fragmentation and a loss in regular structure. Regarding plasma copolymerisation as a feasible method to finish surfaces with a definite number of functional groups it is necessary to characterize both, the chemical nature and the physical properties of the deposited layer. Therefore, a combination of different methods was employed for the characterization of thin plasma copolymer films (FTIR, dielectric spectroscopy, differential scanning calorimetry, X-ray photoelectron spectroscopy (XPS)). Special attention was paid on the unambiguous identification of COOH groups at the surface after derivatization with trifluoroethanol by XPS and in the volume by FTIR. The glass transition temperature of the copolymer system is lower than that for the both plasma deposited homopolymers and increases with the DC in difference to plasma deposited poly(acrylic acid). The dielectric measurements showed that the plasma deposited films were not thermally stable and underwent an undesired post-plasma chemical reaction. The results obtained by dielectric spectroscopy are discussed in detail in comparison with the data from FTIR and XPS measurements. KW - Plasmapolymerisation KW - Copolymerisation KW - Acrylic acid–styrene copolymer KW - Dynamic mobility KW - Plasma copolymerisation KW - Surface functionalization KW - Thin film properties PY - 2012 DO - https://doi.org/10.1002/ppap.201100117 SN - 1612-8850 SN - 1612-8869 VL - 9 IS - 3 SP - 273 EP - 284 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-25654 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mix, Renate A1 - Friedrich, Jörg Florian A1 - Inagaki, N. T1 - Modification of branched polyethylene by aerosol-assisted dielectric barrier discharge N2 - Three polyethylene (PE) types with different branching structures were subjected to air, water and ethanol aerosol-assisted dielectric barrier discharges (DBD) for surface modification. Using the air DBD the incorporated oxygen concentration was found to be independent on the branching of PE in contrast to the introduction of OH groups, which was PE-2 > PE-1 > PE-3. For water-aerosol DBD the succession of OH concentration was in the order of PE-1 > PE-2 > PE-3. Ethanol aerosol-assisted DBD produced the lowest concentration of OH groups also independent on the branching of PE. The chemical nature of introduced oxygen functional groups was inspected by X-ray photoelectron spectroscopy (XPS) and assigned as C–O, >C=O/CHO/O–C–O and O=C–O. KW - PE KW - Surface modification KW - Aerosol-assisted DBD PY - 2012 DO - https://doi.org/10.1002/ppap.201100052 SN - 1612-8850 SN - 1612-8869 VL - 9 IS - 4 SP - 406 EP - 416 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-25748 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mix, Renate A1 - Hielscher, Stefan A1 - Beck, Uwe A1 - Friedrich, Jörg Florian T1 - Plasma meets chemistry: Combined methods for tailored interface design in metal-polymer composites by selective chemical reactions on plasma modified surfaces N2 - The applicability of polymer-metal composites is mainly determined by the durability of the adhesive strength between both components. Aluminium (Al) deposited on polypropylene (PP) exemplifies different options of interface design. By deposition of plasma polymers on PP the effect of the type of the functionality was investigated. Spacer insertion was accomplished to position the functional group away from the topmost surface. A further kind of interface design involved a partial condensation of functional groups. Hydroxyl and carboxyl groups were most effective to improve adhesion in Al-PP systems. Approximately 7-10 carboxyl or 25-27 hydroxyl groups per 100 C atoms were necessary to increase the peel strength up to ~700 N/m. In this range, the failure of the composite propagated along the interface Al-tape (no peeling of the metal). Spacer molecules between surface and functional groups provoked the effect that the number of needed functional groups for maximum adhesion was strongly reduced. Linking of the functional groups resulted in non-peelable Al-PP laminates. Two adhesion tests were applied - the peel test and the centrifuge technology. For PP foils modified with chemically bonded and additionally linked silanol groups (no peeling) an adhesive strength of (2.5 ± 0.2) N/mm² was determined by centrifuge technology. XPS inspection of both fracture surfaces indicated a sub-surface failure in the polymer. T2 - HTPP-12 - 12th High-tech plasma processes conference CY - Bologna, Italy DA - 2012-06-24 KW - Adhesion PP-Al KW - Modified surfaces KW - Interface design PY - 2012 DO - https://doi.org/10.1088/1742-6596/406/1/012004 SN - 1742-6588 SN - 1742-6596 VL - 406 SP - 012004-1 - 012004-11 PB - IOP Publ. CY - Bristol, UK AN - OPUS4-28658 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ramanujam, Maalolan A1 - Wachtendorf, Volker A1 - Purohit, Purv A1 - Mix, Renate A1 - Schönhals, Andreas A1 - Friedrich, Jörg Florian T1 - A detailed dielectric relaxation spectroscopy study of artificial UV weathered low density polyethylene N2 - Artificial weathering of LDPE under dry conditions (<10% of relative humidity) by UV radiation was monitored by dielectric spectroscopy. For an apolar polymer like LDPE, dielectric study yields information about the change in structure and dynamics of the system. The fluctuations of the polar groups which are generated as a result of photooxidation such as carbonyl groups can be monitored as characteristic relaxation processes like the αc or β mode. The dielectric loss characterized by typical dielectric parameters like the activation energy and dielectric strength are strongly dependent upon changes induced by photooxidation in the amorphous and crystalline domains. This paper discusses in detail how the foil reached its mechanical disintegration. It was found that initial stages of weathering induce chain scission and/or crosslinking in the amorphous domains of the polymer and the motional processes in the crystalline regions are not affected. After this induction period, an increase in the degree of crystallization was observed by employing differential calorimetry. The increasing crystallinity is considered as one of the reasons for embrittlement which finally leads to the complete loss of the structural integrity. KW - Artificial weathering KW - UV radiation KW - Dielectric relaxation KW - LDPE PY - 2012 DO - https://doi.org/10.1016/j.tca.2011.12.003 SN - 0040-6031 SN - 1872-762X VL - 530 SP - 73 EP - 78 PB - Elsevier CY - Amsterdam AN - OPUS4-25547 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fahmy, A. A1 - Mix, Renate A1 - Schönhals, Andreas A1 - Friedrich, Jörg Florian T1 - Surface and bulk structure of thin spin coated and plasma-polymerized polystyrene films N2 - Polystyrene (PS) spin coated thin films were modified by O2 and Ar plasma as well as by UV irradiation treatments. The modified PS samples were compared with plasma polymerized and commercial polystyrene. The effects of plasma (O2 and Ar) and UV irradiation treatments on the surface and the bulk properties of the polymer layers were discussed. The surface properties were evaluated by X-ray Photoelectron Spectroscopy and Contact angle measurements and the bulk properties were investigated by FTIR and dielectric relaxation spectroscopy. As a result only one second treatment time was sufficient to modify the surface. However, this study was also dedicated to understand the effect of plasma and plasma irradiation on the deposited layers of plasma polymers. The dielectric measurements showed that the plasma deposited films were not thermally stable and underwent an undesired post-plasma chemical oxidation. KW - Surface and bulk characterization KW - Plasma polymerization KW - Polystyrene KW - Surface modification KW - Thermal stability KW - Plasma polymers PY - 2012 DO - https://doi.org/10.1007/s11090-012-9372-1 SN - 0272-4324 VL - 32 IS - 4 SP - 767 EP - 780 PB - Plenum Publ. Corp. CY - New York, NY, USA AN - OPUS4-26264 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mix, Renate A1 - Friedrich, Jörg F. T1 - New Plasma Processes for Promotion of Adhesive Properties of Polymers T2 - The 5th International Symposium of PLACIA, Japan CY - Nagoya, Japan DA - 2012-10-24 PY - 2012 AN - OPUS4-26881 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mix, Renate A1 - Friedrich, Jörg F. T1 - Tailored interphase design - the key for effective application in the field of metal-polyolefin composites T2 - 11th APCPST (Asia Pacific Conference on Plasma Science and Technology) and 25th SPSM (Symposium on Plasma Science for Materials) CY - Kyoto, Japan DA - 2012-10-02 PY - 2012 AN - OPUS4-26864 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Hielscher, Stefan A1 - Weise, Matthias A1 - Mix, Renate A1 - Lerche, D. A1 - Rietz, U. T1 - Progress in quantitative adhesion testing of films and coatings by means of centrifuge technology - present state of the art N2 - Standardised conventional adhesion tests are time-consuming single-sample tests. Moreover, except for the pull-off test, all these tests provide only qualitative or semi-quantitative (ranking, respectively measurement of an adhesion-correlated quantity) information on adhesion. Sometimes, adhesion is evaluated even under compressive stress conditions (e.g. cross-cut and scratch test), which itself is a contradiction to adhesive strength as defined in terms of tensile force per area. For optical coatings it has been shown that the pull-off test in a centrifuge is definitely a promising alternative with respect to the reliable, fast and quantitative determination of adhesive strength in N/mm2. The force-controlled centrifuge test is the only multiple-sample test which provides reliable quantitative information on the adhesive strength in agreement with DIN EN 15870 and DIN EN ISO 4624 on a statistical basis for up to eight samples simultaneously tested under identical testing conditions. T2 - PSE 2012 - 13th International conference on plasma surface engineering CY - Garmisch-Partenkirchen, Germany DA - 10.09.2012 KW - Adhesion KW - Centrifuge test KW - Plasma modification KW - Tensile strength PY - 2012 UR - http://www.pse-conferences.net/tl_files/pse2012/abstractupload/PSE2012-OR2601-ext.pdf SP - 1 EP - 4 AN - OPUS4-27305 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mix, Renate A1 - Ramanujam, Maalolan A1 - Wachtendorf, Volker A1 - Friedrich, Jörg Florian ED - Reichert, T. T1 - New ways for early detection of polymer ageing N2 - Photo-oxidative ageing of polymers under defined exposure (UV, humidity) was investigated from two points of view: a) the ageing process Starts from the topmost surface and penetrates slowly towards bulk and b) radicals play an important role among ageing. Therefore, X-ray photoelectron (XPS) and electron spin resonance (ESR) spectroscopy were applied to show both, the progressive incorporation of oxygen during in-situ UV irradiation (XPS) and the formation of radicals (ESR) in the polymer. The intensity of ESR Signals served as measure for radical concentration. The Validation of this correlation was checked for polyethylenes (PE) equipped with different concentrations of Hostavin N30 UV stabilizer. T2 - 5th European weathering symposium - Natural and artificial ageing of polymers CY - Lisbon, Portugal DA - 21.09.2011 PY - 2011 SN - 978-3-9813136-2-8 N1 - Serientitel: CEEES Publication – Series title: CEEES Publication IS - 15 SP - 157 EP - 163 PB - GUS (Gesellschaft für Umweltsimulation) CY - Pfinztal AN - OPUS4-24535 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ramanujam, Maalolan A1 - Wachtendorf, Volker A1 - Mix, Renate A1 - Schönhals, Andreas A1 - Friedrich, Jörg Florian ED - Reichert, T. T1 - Influence of UV weathering and humidity on surface & bulk properties of LDPE N2 - The outdoor weathering of polymers is mainly due to UV radiation, water, Pollution, humidity, temperature etc. To understand the effects of weathering, simulated tests need to be undertaken in lab scale. Such tests must be quite efficient and similar to the effects of natural weathering. This paper mainly focuses on the effects of UV radiation along with humidity on LDPE. T2 - 5th European weathering symposium - Natural and artificial ageing of polymers CY - Lisbon, Portugal DA - 21.09.2011 KW - LDPE KW - UV weathering KW - Humidity PY - 2011 SN - 978-3-9813136-2-8 N1 - Serientitel: CEEES Publication – Series title: CEEES Publication IS - 15 SP - 211 EP - 218 PB - GUS (Gesellschaft für Umweltsimulation) CY - Pfinztal AN - OPUS4-24536 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mix, Renate A1 - Friedrich, Jörg Florian T1 - Improvement of adhesivity of polypropylene by its surface modification using the aerosol dielectric barrier discharge N2 - Plasma processes are used in many fields of Science and technology. While a plasma oxygen treatment produces a broad variety of different oxygen-containing functional groups, tailored - surface functionalisation demands preset functional groups in known concentration. Due to the fact that most of plasma experiments need expensive vacuum equipment increased efforts are to observe to apply atmospheric pressure plasma processes. Thus, Dielectric Barrier Discharge (DBD) and corona treatment of polymer foils have a long tradilion in industry to modify them for printing, laminating, adhesion promotion, etc. Thercibre, increasing interest is observed to make these atmospheric pressure processes more effeclive. Newly developed methods like plasma-printing were used for surfaces in biological and medical applications or for printed circuits. T2 - ADHESION `11 - 11th Triennial conference on the science and technology of adhesion and adhesives CY - York, UK DA - 07.09.2011 PY - 2011 SP - 253 EP - 256 AN - OPUS4-24337 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mix, Renate A1 - Friedrich, Jörg F. T1 - Improvement of Adhesivity of Polypropylene by Its Surface Modification Using the Aerosol Dielectric Barrier Discharge T2 - Adhesion '11, 11th International Conference on the Science and Technology of Adhesion and Adhesives CY - York, England DA - 2011-09-07 PY - 2011 AN - OPUS4-24283 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mix, Renate A1 - Yin, Huajie A1 - Friedrich, Jörg F. T1 - Special interface design for adhesion improvement T2 - ICCE-19, 19th Annual International Conference on Composites or Nano Engineering CY - Shanghai, China DA - 2011-07-24 PY - 2011 AN - OPUS4-24134 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yin, Huajie A1 - Mix, Renate A1 - Friedrich, Jörg Florian T1 - Influence of differently structured aluminium-polypropylene interfaces on adhesion N2 - Polar groups were introduced on polypropylene surfaces for increasing the surface energy and the peel strength to evaporated aluminium layers. Three kinds of plasma processes were used for introducing such functional groups to polyolefin surfaces: low-pressure radio-frequency (RF) O2 plasma exposure, atmospheric-pressure dielectric-barrier discharge (DBD) treatment in air, and the deposition of allylamine plasma polymer. The amino groups of the allylamine plasma polymer were also used as anchoring points for chemical introduction of covalently bonded spacer molecules equipped with reactive endgroups. Thus, silanol endgroups of a covalently bonded spacer were able to interact with the evaporated metal layer. The Al-PP composites achieved a maximal peel strength of 470 N/m by exposing the polymer to the lowpressure O2 plasma and 500 N/m on exposure to the atmospheric DBD plasma. After allylamine plasma polymerization and grafting of spacers, the peel strength was usually higher than 1500 N/m and the composites could not be peeled. KW - Polypropylene KW - Low-pressure RF oxygen plasma KW - Dielectric barrier discharge (DBD) KW - Pulsed plasma polymerization KW - Surface wettability KW - Peel strength PY - 2011 DO - https://doi.org/10.1163/016942410X511132 SN - 0169-4243 SN - 1568-5616 VL - 25 IS - 8 SP - 799 EP - 818 PB - VNU Science Press CY - Utrecht AN - OPUS4-23990 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fahmy, A. A1 - Mix, Renate A1 - Schönhals, Andreas A1 - Friedrich, Jörg Florian T1 - Structure of plasma-deposited poly(acrylic acid) films N2 - Poly(acrylic acid) films with a thickness of about 150?nm were deposited using a pulsed plasma onto aluminum and glass. The structure/property relationships of these samples were studied in dependence to the duty cycle (DC) of the plasma by a broad combination of different techniques and probes. For the first time, volume sensitive methods (FTIR, dielectric spectroscopy, and differential scanning calorimetry) are combined with surface analyses i.e. XPS. For an unambiguous identification of COOH groups by XPS, derivatization with trifluoroethanol was accomplished. Quantitative FTIR investigations give qualitatively a dependence of the concentration of COOH groups upon DC similar to that given by XPS investigations. The observed differences are discussed considering the different analytical depths of both methods. The dielectric measurements reveal that the structure of the plasma deposited films is different from that of the bulk material. Moreover, these measurements show also that the plasma deposited films are not thermally stable but undergo a post plasma chemical reaction during heating, where the reaction kinetics depends on DC. PY - 2011 DO - https://doi.org/10.1002/ppap.201000108 SN - 1612-8850 SN - 1612-8869 VL - 8 IS - 2 SP - 147 EP - 159 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-23478 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fahmy, A. A1 - Mix, Renate A1 - Schönhals, Andreas A1 - Friedrich, Jörg Florian T1 - Structure-property relationship of thin plasma deposited poly(allyl alcohol) films N2 - Poly(allyl alcohol) films with a thickness of about 150 nm were deposited by pulse plasma polymerization onto different substrates (inorganic and organic). The structure/property relationships of these samples were studied in dependence on the duty cycle (DC) of the plasma by a broad combination of different techniques and probes. For the first time volume sensitive methods (FTIR and dielectric spectroscopy) are combined with surface analytics by employing XPS for that system. FTIR spectroscopy gives qualitatively the same dependence of the concentration of the OH groups on DC like XPS. The observed differences are discussed considering the different analytical depths of both the methods. The dielectric measurements show that the plasma deposited films are not thermally stable but undergo a post plasma chemical reaction during heating. The results obtained by dielectric spectroscopy are discussed in detail with the data from FTIR and XPS measurements. KW - Allyl alcohol KW - Dielectric properties KW - Plasma polymerization KW - Surface and bulk characterization KW - Thermal stability PY - 2011 DO - https://doi.org/10.1007/s11090-011-9297-0 SN - 0272-4324 VL - 31 IS - 3 SP - 477 EP - 498 PB - Plenum Publ. Corp. CY - New York, NY, USA AN - OPUS4-23671 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hoffmann, Katrin A1 - Mix, Renate A1 - Friedrich, Jörg Florian A1 - Resch-Genger, Ute ED - Geddes, C.D. T1 - Spectroscopic characterization of plasma - Chemically functionalized and fluorophore-labeled polymer surfaces N2 - The potential of spectrofluorometry and fluorescence microscopy for the characterization and quantification of different functionalities like OH and NH2 groups at plasma-chemically modified polymer surfaces is assessed using traditional reactive dyes such as dansyl derivatives and a sophisticated VIS-excitable chromogenic and fluorogenic pyrylium label showing binding-induced spectral and intensity changes in absorption and emission. Aiming at an improved fluorometric surface analysis, based upon these measurements, several sources of uncertainty inherent to fluorescence measurements are illustrated ranging from environment-dependent dye absorption and emission features over spectral correction and nonspecific adsorption to the critical influence of label choice on the measured background. Solutions to these drawbacks are given thereby underlining the potential of fluorometry for surface analysis. KW - Polymer functionalization KW - Plasma modification KW - Fluorescence spectroscopy KW - Surface labeling PY - 2010 SN - 978-1-4419-0828-5 DO - https://doi.org/10.1007/978-1-4419-1260-2_6 N1 - Serientitel: Reviews in Fluorescence – Series title: Reviews in Fluorescence VL - 5 SP - 139 EP - 160 PB - Springer Science + Business Media AN - OPUS4-21274 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gross, Thomas A1 - Pippig, F. A1 - Merz, B. A1 - Merz, R. A1 - Vohrer, U. A1 - Mix, Renate A1 - Steffen, H. A1 - Bremser, Wolfram A1 - Unger, Wolfgang T1 - Determination of OH groups at plasma oxidised poly(propylene) by TFAA chemical derivatisation XPS: an inter-laboratory comparison N2 - A first inter-laboratory comparison was conducted to demonstrate and document the capability of interested laboratories to measure the fraction of C—OH species on a plasma oxidised poly(propylene) sample by using a chemical derivatisation XPS approach. This report presents the results from that inter-laboratory comparison and includes the data received for the measured values and their associated standard deviations of laboratory means, at a 95% confidence level. The measurements were guided by a protocol developed within the group before and summarised shortly in the paper. Standard deviations that may characterise the state-of-the-art for the nominally simple and rather often practised case of TFAA chemical derivatisation XPS of C—OH species on a plasma oxidised polyolefin surface are calculated following ISO 5725-2:1994. The main conclusion is that the associated degree of equivalence reached by the participating laboratories in this comparison is still low. Further research to improve chemical derivatisation XPS protocols is mandatory. KW - Chemical derivatisation KW - ESCA/XPS KW - Inter-laboratory comparison KW - Photoelectron spectroscopy (PES) KW - Poly(propylene) (PP) PY - 2010 DO - https://doi.org/10.1002/ppap.200900142 SN - 1612-8850 SN - 1612-8869 VL - 7 IS - 6 SP - 494 EP - 503 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-21678 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mix, Renate T1 - Aerosol-based DBD - a simple way to provide polymers with functional groups for adhesion promotion T2 - ACS 240th National Meeting, Symposium in Honor of Kash Mittal CY - Boston, MA, USA DA - 2010-08-22 PY - 2010 AN - OPUS4-21866 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mix, Renate A1 - Friedrich, Jörg F. A1 - Wettmarshausen, Sascha T1 - New concept for polymer metal interfaces T2 - MACRO 2010 Polymer Science in the Service of Society CY - Glasgow, Scotland DA - 2010-07-11 PY - 2010 AN - OPUS4-21847 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pfuch, A. A1 - Horn, K. A1 - Mix, Renate A1 - Ramm, M. A1 - Heft, A. A1 - Schimanski, A. ED - Suchentrunk, R. T1 - Direct and remote plasma assisted CVD at atmospheric pressure for the preparation of oxide thin films N2 - In this paper the preparation of silicon and titanium oxide thin films using an atmospheric pressure plasma process will be reported. To obtain these oxide films hexamethyldisiloxane and titanium tetraisopropoxide were used as precursor materials. Based on the different chemical reaction mechanisms the film deposition processes were carried out in the direct as well as in the remote PACVD mode. The deposition parameters were varied and the influence on different film properties was studied. The deposited oxide films were characterised by profilometry, ellipsometry, SEM, UV-VIS-NIR-transmission measurements. FT-IR spectroscopy and contact angle measurements. Additionally, first results will be presented concerning the creation of composite films using a combination of plasma and liquid dye nebulization technique. KW - FTIR KW - Ellipsometry KW - Profilometry KW - SEM KW - PACVD KW - Silicon oxide PY - 2010 SN - 978-3-87480-259-8 VL - 66 SP - 114 EP - 124 PB - Eugen G. Leuze CY - Bad Saulgau AN - OPUS4-22798 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mix, Renate A1 - Friedrich, Jörg F. T1 - Polymer surface modification by dielectric barrier discharge in presence of aerosols T2 - Plasmadays 2010 CY - Luxembourg City, Luxembourg DA - 2010-07-05 PY - 2010 AN - OPUS4-21986 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mix, Renate A1 - Friedrich, Jörg F. A1 - Yin, Huajie A1 - Rau, A. T1 - Abscheidung dünner haftvermittelnder Polymerschichten mittels Barriereentladung T2 - 5. Workshop Anwenderkreis Atmosphärendruckplasma CY - Potsdam, Germany DA - 2010-06-09 PY - 2010 AN - OPUS4-21486 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Friedrich, Jörg Florian A1 - Wettmarshausen, Sascha A1 - Hanelt, Sven A1 - Mach, Reinhard A1 - Mix, Renate A1 - Zeynalov, Eldar A1 - Meyer-Plath, Asmus T1 - Plasma-chemical bromination of graphitic materials and its use for subsequent functionalization and grafting of organic molecules N2 - Plasma-chemical bromination has been shown to be well-suited for highly selective and efficient C–Br-functionalization of polyolefin surfaces and has now been applied to graphitic materials, including highly oriented pyrolytic graphite (HOPG), natural graphite, carbon nanotubes, and graphitized carbon fibres. In contrast to the radical substitution of hydrogen by bromine at hydrogen-terminated sp3-hybridized carbon, bromination of all-carbon bound sp2-hybridized carbon in graphene requires addition to aromatic double bonds. The related change of sp2 to sp3 hybridization of the carbon atoms involved helps to explain experimental results of a loss in surface planarity on brominated HOPG. Bromine concentrations of up to 50 bromine atoms per 100 C-atoms were achieved in elemental bromine vapour under low-pressure plasma conditions using low-energetic inductively coupled radio-frequency plasma excitation. The time scale of the bromination progress was found to increase with the specific surface area of the material. The results of plasma-chemical bromination are compared to that of wet-chemical electrophilic addition reactions, which achieved 28 Br per 100 C for MWCNT. The resulting C–Br bonds from plasma-chemical processing of graphitic materials were shown to be well-suited for hydroxyl functionalization and for grafting of organic molecules by nucleophilic substitution with 1,6-diaminohexane and (3-aminopropyl)triethoxysilane. PY - 2010 DO - https://doi.org/10.1016/j.carbon.2010.06.054 SN - 0008-6223 SN - 1873-3891 VL - 48 IS - 13 SP - 3884 EP - 3894 PB - Pergamon Press CY - New York, NY AN - OPUS4-21954 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Friedrich, Jörg Florian A1 - Mix, Renate A1 - Schulze, Rolf-Dieter A1 - Rau, A. T1 - Ultra-thin polymer layer deposition by aerosol-dielectric barrier discharge (DBD) and electrospray ionization (ESI) at atmospheric pressure N2 - Polyolefins are chemically inert and do not adhere well to metals, polymers or inorganics. To overcome this problem, polyolefin surfaces were modified thermally, plasmachemically, or by flame treatment with different oxygen-containing groups, however, unfortunately, such treatments were accompanied by undesired, adhesion lowering polymer degradation. To solve this dilemma, solutions of synthetic polymers and copolymers were prepared, sprayed into the barrier discharge or electrosprayed without discharge and deposited as thin adhesion-promoting layers. The deposited polymer layers from poly(vinylamine), poly(ethylene glycol)-poly(vinyl alcohol) copolymers and poly(acrylic acid) were endowed with monotype functional groups. Using the aerosol - dielectric barrier discharge only a fraction of functional groups survived the deposition process in contrast to the electrospray in which all functional groups were retained. KW - Polymer surface modification KW - Dielectric barrier discharge KW - Polymer aerosols KW - Electrospray deposition KW - Adhesion-promoting layers PY - 2010 DO - https://doi.org/10.1163/016942409X12598231568429 SN - 0169-4243 SN - 1568-5616 VL - 24 IS - 7 SP - 1329 EP - 1350 PB - VNU Science Press CY - Utrecht AN - OPUS4-21374 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Girard-Lauriault, Pierre-Luc A1 - Retzko, Iris A1 - Swaraj, Sufal A1 - Matsubayashi, N. A1 - Gross, Thomas A1 - Mix, Renate A1 - Unger, Wolfgang T1 - Non-destructive sub-surface chemical characterization of air-exposed plasma polymers by energy-resolved XPS KW - Plasma polymers KW - Synchrotron XPS KW - Depth profiling KW - Derivatisation PY - 2010 DO - https://doi.org/10.1002/ppap.200900130 SN - 1612-8850 SN - 1612-8869 VL - 7 IS - 6 SP - 474 EP - 481 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-21711 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mix, Renate A1 - Friedrich, Jörg F. A1 - Wettmarshausen, Sascha T1 - New concept for metal-polyolefin composite interfaces T2 - MACRO 2010 Polymer Science in the Service of Society CY - Glasgow, Scotland DA - 2010-07-11 PY - 2010 AN - OPUS4-21780 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mix, Renate A1 - Falkenhagen, Jana A1 - Friedrich, Jörg F. T1 - Analytical characterization of plasma polymers and copolymers of acrylic acid T2 - MACRO 2010 Polymer Science in the Service of Society CY - Glasgow, Scotland DA - 2010-07-11 PY - 2010 AN - OPUS4-21781 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Solomun, Tihomir A1 - Mix, Renate A1 - Sturm, Heinz T1 - Immobilization of silanized DNA on glass: influence of the silane tether on the DNA hybridization N2 - Two trifunctional (trimethoxy and triethoxy) and one difunctional (methyldimethoxy) 3-mercaptopropyl-alkoxysilanes were covalently tethered to thiolated DNA oligonucleotides in solution. After deposition as microarrays onto glass, the immobilized DNA probes were tested for hybridization ability by a florescence-based method. The results demonstrate a large enhancement in the fluorescence signal when the functionality of the silane tether is reduced from three to two. An XPS analyses revealed that this is not due to a higher DNA surface density. FTIR spectra of the spin-coated silanes showed that the trifunctional silanes form branched and cyclic siloxane moieties, whereas the difunctional silane generates predominantly short straight siloxane chains. Therefore, the propensity of trifunctional silanes to form more complex networks leads to conformations of the bound DNA which are less favorable for the specific interaction with the complementary strand. The data implicate that further significant improvements in the DNA hybridization ability are possible by adroit choice of the silane system. KW - Silanized DNA KW - DNA immobilization KW - DNA hybridization KW - Fluorescence imaging KW - FTIRS KW - XPS PY - 2010 DO - https://doi.org/10.1021/am100263t SN - 1944-8244 SN - 0013-936X SN - 1944-8252 VL - 2 IS - 8 SP - 2171 EP - 2174 PB - ACS Publ. CY - Washington, DC, USA AN - OPUS4-22614 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Labahn, Diana A1 - Mix, Renate A1 - Schönhals, Andreas T1 - Dielectric relaxation of ultrathin films of supported polysulfone N2 - The dynamic glass transition (α relaxation, structural relaxation) of ultrathin polysulfone films prepared between aluminum electrodes is investigated by dielectric relaxation spectroscopy. As a main result, it is found that the glass transition temperature Tg does not depend on the thickness of the polymeric layer down to a thickness of 10 nm. For thicknesses lower than 10 nm, an increase of Tg is observed. A more detailed analysis of the temperature dependence of the relaxation rates reveals that the Vogel temperature increases and the fragility decreases systematically with decreasing film thickness d. Further, the dielectric strength Δε decreases with decreasing d. This is discussed by the formation of a surface layer of adsorbed polysulfone segments having a reduced molecular mobility with regard to the time scale characteristic of the glassy dynamics of bulk polysulfone. Plotted versus inverse film thickness Δε decreases linearly with 1/d and becomes zero for an extrapolated length scale of 10 nm. From that it is concluded that the thickness of the adsorbed boundary layer is about 5 nm. Contact-angle measurements were carried out to confirm the strong interaction between aluminum and polysulfone. It is also shown that preparation details like annealing conditions strongly influence the glass transition of supported ultrathin films. KW - Adsorbed layers KW - Aluminium KW - Annealing KW - Contact angle KW - Dielectric relaxation KW - Electrodes KW - Glass transition KW - Polymer films KW - Thin films PY - 2009 DO - https://doi.org/10.1103/PhysRevE.79.011801 SN - 1539-3755 SN - 1063-651X VL - 79 IS - 1 SP - 011801-1 - 011801-9 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-19050 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Wettmarshausen, Sascha A1 - Mix, Renate A1 - Meyer-Plath, Asmus A1 - Mittmann, Hans-Ulrich A1 - Friedrich, Jörg Florian ED - K.L. Mittal, T1 - Plasma Bromination - a selective way to monotype functionalized polymer surfaces KW - Functional groups KW - Polymer surfaces KW - Plasma bromination KW - Grafting KW - Spacer KW - Selective plasma process PY - 2009 SN - 978-90-04-16590-8 VL - 5 SP - 3 EP - 18 PB - Koninklijke Brill NV CY - Leiden, The Netherlands AN - OPUS4-18944 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoffmann, Katrin A1 - Mix, Renate A1 - Friedrich, Jörg Florian A1 - Buschmann, H.-J. A1 - Resch-Genger, Ute T1 - Anchoring of Fluorophores to plasma-chemically modified polymer surfaces and the effect of Cucurbit[6]uril on dye emission N2 - Polypropylene supports were functionalized by plasma-deposition of polymeric allylamine layers. The surface amino groups generated were wet-chemically reacted with xanthene dyes resulting in fluorescent polymer films. The effect of polymer-attachment of the dyes on their emission features was studied fluorometrically and different methods were tested to improve the fluorescence properties of the films. Modification with cucurbit[6]uril (CB6) yields a moderately enhanced fluorescence as well as an improved photostability. The observed effect is most likely due to CB6-induced rigidization of the linker molecules which seems to reduce fluorescence quenching dye–dye and fluorophore–surface interactions. KW - Fluorescence KW - Cucurbituril KW - Surface modification KW - Plasma functionalization KW - Polymer surface KW - Xanthene dyes PY - 2009 DO - https://doi.org/10.1007/s10895-008-0407-1 SN - 1053-0509 SN - 1573-4994 VL - 19 SP - 229 EP - 237 PB - Plenum Publ. Corp. CY - New York, NY AN - OPUS4-19154 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mix, Renate A1 - Yin, Huajie A1 - Rau, A. T1 - Adhesion Polypropylene - Aluminium by Aerosol Based DBD Treatment of Foils T2 - Third Asian Conf. on Adhesion CY - Hamamatsu, Japan DA - 2009-06-07 PY - 2009 AN - OPUS4-19439 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Mix, Renate A1 - Schulze, Rolf-Dieter A1 - Rau, A. A1 - Friedrich, Jörg Florian ED - G. Blasek, T1 - Aerosol-Barriereentladung und Elektrospray zur Polymerschichtabscheidung T2 - 17. Neues Dresdner Vakuumtechnisches Kolloquium - Beschichtung, Modifizierung und Charakterisierung von Polymeroberflächen CY - Dresden, Deutschland DA - 2009-10-21 KW - Corona KW - Barriereentladung KW - Haftvermittler KW - Schälfestigkeit PY - 2009 SN - 978-3-9812550-1-0 SP - 76 EP - 80 AN - OPUS4-20252 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Mix, Renate A1 - Falkenhagen, Jana A1 - Schulze, Rolf-Dieter A1 - Gerstung, Vanessa A1 - Friedrich, Jörg Florian ED - K.L. Mittal, T1 - Plasma homo- and copolymerization of allyl alcohol and styrene KW - Plasma polymerization KW - Surface functionalization KW - Molar masses PY - 2009 SN - 978-90-04-16590-8 VL - 5 SP - 317 EP - 340 PB - Koninklijke Brill NV CY - Leiden, The Netherlands AN - OPUS4-19606 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mix, Renate A1 - Friedrich, Jörg F. T1 - Einführung von haftvermittelnden Molekülen an plasmabehandelte Polymeroberflächen T2 - XV. Erfahrungsaustausch Oberfläachentechnologie mit Plasma- und Ionenstrahlprozessen CY - Klingenthal, Germany DA - 2008-03-04 PY - 2008 AN - OPUS4-16713 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mix, Renate A1 - Weidner, Steffen A1 - Friedrich, Jörg F. T1 - Charakterisierung der Umsetzung von OH-terminierten Oligomeren mit 3-(Isocyanatopropyl)trimethoxysilan mittels MALDI-TOF und FTIR T2 - 12. Kolloquium "MALDI und Synthetische Polymere" CY - Berlin, Germany DA - 2008-05-06 PY - 2008 AN - OPUS4-17505 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mix, Renate A1 - Friedrich, Jörg F. T1 - The influence of spacers between functional groups and metal surface on the adhesion of metal to polymers T2 - Karls-University, Prague CY - Prague, Czech Republic DA - 2008-04-28 PY - 2008 AN - OPUS4-17458 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mix, Renate A1 - Friedrich, Jörg F. T1 - Introduction of covalently bonded flexible spacers into polymer-metal interfaces T2 - 11th International Conference on Plasma Surface Engineering CY - Garmisch-Partenkirchen, Germany DA - 2008-09-15 PY - 2008 AN - OPUS4-17910 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -