TY - JOUR A1 - Gross, Thomas A1 - Kühn, Gerhard A1 - Unger, Wolfgang T1 - Photoelectron spectroscopy on organic surfaces: X-ray degradation of oxygen-plasma-treated and chemically reduced poly(propylene) surfaces in comparison to conventional polymers N2 - The X-ray-induced sample damage during mono XPS analysis of an oxygen-plasma-oxidized and subsequently wet-chemically reduced poly(propylene) film was investigated as a showcase for plasma-modified or plasma-deposited samples. By doing this, the degradation index approach as introduced by Beamson and Briggs in the Scienta ESCA300 high-resolution XPS database of organic polymers has been adopted. As to be expected, the sample degrades by loosing oxygen as revealed by observation of decreasing O/C and COR/Csum ratios. However, the X-ray degradation indices are definitely higher than those of conventional reference polymers. Moreover, the COR/Csum degradation index is significantly higher in comparison with one obtained for the O/C ratio. In that context, there is no difference between the plasma sample and a conventional poly(vinyl alcohol) polymer. It is concluded that for reliable quantitative surface chemical analysis, the quality of spectra in terms of acquisition times must be optimized aimed to a minimization of X-ray degradation. Finally, it is proposed to describe the photon flux of an X-ray gun in an XPS experiment, which defines the degradation rate at the end, by using the sample current simply measured with a carefully grounded sputter-cleaned reference silver sample. KW - Photoelectron spectroscopy KW - ESCA/XPS KW - Surfaces KW - Surface modification KW - Poly(propylene) (PP) KW - Plasma treatment KW - X-ray KW - Degradation PY - 2009 U6 - https://doi.org/10.1002/sia.3024 SN - 0142-2421 SN - 1096-9918 VL - 41 IS - 5 SP - 445 EP - 448 PB - Wiley CY - Chichester AN - OPUS4-19252 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wettmarshausen, Sascha A1 - Kühn, Gerhard A1 - Hidde, Gundula A1 - Mittmann, Hans-Ulrich A1 - Friedrich, Jörg Florian T1 - Plasmabromination - the Selective Way to Monotype Functionalized Polymer Surfaces N2 - In contrast to other plasma modification processes of polymer surfaces, the bromination is very selective and shows a high yield in C—Br groups. The most convenient bromination process was found using bromoform, which was thus preferred to elemental bromine, allyl bromide, vinyl bromide or tert-butylbromide. The bromoform process give yields in C—Br up to 40 C—Br or more, with only 2-3% co-introduction of O-functionalities whereas allyl bromide results in yields of about 20 C—Br and more, but in more than 10% oxygen-containing by-products. C—Br groups serve as anchoring points for grafting of molecules, oligomers and pre-polymers of diole or diamine character. KW - Functional groups KW - Grafting KW - Plasma bromination KW - Polymer surfaces KW - Selective plasma process KW - Spacer PY - 2007 U6 - https://doi.org/10.1002/ppap.200700019 SN - 1612-8850 SN - 1612-8869 VL - 4 IS - 9 SP - 832 EP - 839 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-16209 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Friedrich, Jörg Florian A1 - Kühn, Gerhard A1 - Mix, Renate A1 - Hoffmann, Katrin A1 - Resch-Genger, Ute T1 - Tailoring of polymer surfaces with monotype functional groups of variable density using chemical and plasma chemical processes N2 - Polymer surfaces were modified in low-pressure glow discharge plasmas for introduction of monotype functional groups of different type and density. For this purpose three ways are selected, (i) oxygen plasma treatment followed by wet-chemical reduction of O functional groups to OH groups, (ii) plasma bromination for introducing C - Br groups and (iii) coating by deposition of thin plasma (co-) polymerized layers of functional groups-bearing monomers with OH, NH2, COOH, epoxy etc. functionalities. Subsequently, these groups were used as anchoring points for chemical grafting of spacer molecules, oligomers, prepolymers, fluorescent labels, ionic and nucleic acid residues, employing different chemical routes. The yield in monosort functional groups at polymer surfaces ranged from 10–14 (process i), 20–40 (process ii) and 18–31 groups per 100 C atoms (process iii) as measured by XPS after derivatization. The consumption of functional groups amounted to 40–90% of all functionalities present at the surface and depended on the dimensions of grafted molecules. For infinitely variably tuning the number of functional groups process iii was performed as copolymerization of a functional group-carrying comonomer with a non-functionalized (“chain-extending”) comonomer. KW - Introduction of functional groups KW - Plasma modification KW - Reactions at Polymer surfaces PY - 2006 SN - 0340-255x SN - 1437-8027 VL - 132 SP - 62 EP - 71 PB - Springer CY - Berlin AN - OPUS4-12515 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Friedrich, Jörg Florian A1 - Kühn, Gerhard A1 - Mix, Renate T1 - Tayloring of polymer surfaces with different monotype functional groups of variable density using chemical and plasma chemical processes T2 - 10th Dresden Polymer Discussion: Characterization of Polymer Surfaces and Thin Films CY - Meißen, Germany DA - 2005-04-10 KW - Plasma modification KW - Introduction of functional groups KW - Reactions at polymer surfaces PY - 2005 SP - 34 EP - 49 PB - Leibniz-Institut für Polymerforschung Dresden CY - Meißen AN - OPUS4-11941 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mach, Reinhard A1 - Maneck, Heinz-Eberhard A1 - Röhl-Kuhn, Barbara A1 - Peplinski, Burkhard A1 - Benemann, Sigrid A1 - Strauß, Birgid A1 - Schütz, W. A1 - Kühn, Gerhard A1 - Friedrich, Jörg Florian ED - Pershin, L. T1 - Modification of graphite powders in a thermal RF induction plasma T2 - 17th International Symposium on Plasma Chemistry (ISPC-17) CY - Toronto, Canada DA - 2005-08-07 PY - 2005 SP - 1(?) EP - 6(?) CY - Toronto AN - OPUS4-11942 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Friedrich, Jörg Florian A1 - Kühn, Gerhard A1 - Mix, Renate ED - Pershin, L. T1 - Chemical synthesis at plasma modified polymer surfaces T2 - 17th International Symposium on Plasma Chemistry (ISPC-17) CY - Toronto, Canada DA - 2005-12-07 PY - 2005 SP - 1(?) EP - 6(?) CY - Toronto AN - OPUS4-11944 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Mix, Renate A1 - Kühn, Gerhard A1 - Friedrich, Jörg Florian ED - Mittal, K. L. T1 - Contribution of chemical interactions between Al atoms and different types of functional groups to the adhesion of Al-polymer systems T2 - 2nd International Symposium on Adhesion Aspects of Thin Films CY - Orlando, FL, USA DA - 2003-12-15 KW - Al-functional group interactions KW - Adhesion-promoting plasma polymer layers KW - Pulsed plasma polymerization PY - 2005 SN - 90-6764-421-8 VL - 2 SP - 123 EP - 144 PB - VSP CY - Utrecht AN - OPUS4-11156 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Friedrich, Jörg Florian A1 - Kühn, Gerhard A1 - Mix, Renate ED - D'Agostino, R. T1 - Polymer Surface Modification with Monofunctional Groups of Different Type and Density T2 - 16th International Symposium on Plasma Chemistry ; ISPC-16 CY - Taormina, Italy DA - 2003-06-22 PY - 2005 SN - 3-527-40487-2 SP - 3 EP - 21 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-7019 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Mix, Renate A1 - Friedrich, Jörg Florian A1 - Kühn, Gerhard ED - Mutlu, M. T1 - Adhesion between metal atoms and polymer surfaces fitted with different types and variable density of functional groups T2 - 3rd workshop COST 527 CY - Antalya, Turkey DA - 2004-10-07 KW - Peel strength KW - Aluminium KW - Pulsed plasma KW - Allyl alcohol KW - Allylamine KW - Acrylic acid PY - 2005 SN - 975-491194-0 SP - 106 EP - 114 PB - Hacettepe Univ. Press CY - Ankara AN - OPUS4-11042 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Friedrich, Jörg Florian A1 - Mix, Renate A1 - Kühn, Gerhard T1 - Adhesion of metals to plasma-induced functional groups at polymer surfaces N2 - The peel strength of aluminium to polypropylene and poly(tetrafluoroethylene) was determined in dependence on the type and the concentration of functional groups on the polymer surface. For this purpose the polymer surface was equipped with monotype functional groups. The first method to produce monotype functionalized surfaces was an introduction of O functional groups using an oxygen plasma treatment and converting these groups to OH groups applying a wet chemical reduction. In result of this two-step treatment the hydroxyl group concentration at the polymer surface could be increased from 3–4 to 10–14 OH groups/100 C atoms. The second method consists in the deposition of a 150 nm adhesion-promoting layer of plasmapolymers or copolymers onto the polymer surface using the pulsed plasma technique. For that purpose functional groups carrying monomers as allyl alcohol, allylamine and acrylic acid were used. Applying the plasma-initiated copolymerization and using neutral “monomers” like ethylene or butadiene the concentration of the functional groups was varied. A correlation of peel strength with the ability of forming chemical interactions between Al atoms and functional groups was found: COOH > OH >> NH2 > H(CH2–CH2). KW - Peel strength KW - Aluminium KW - Polypropylene KW - Poly(tetrafluoroethylene) KW - Pulsed plasma KW - Allyl alcohol KW - Allylamine KW - Acrylic acid KW - Plasma surface treatment KW - Adhesion PY - 2005 SN - 0257-8972 VL - 200 IS - 1-4 SP - 565 EP - 568 PB - Elsevier Science CY - Lausanne AN - OPUS4-10897 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -