TY - JOUR A1 - Farag, Zeinab Ramadan A1 - Friedrich, Jörg Florian A1 - Krüger, Simone A1 - Hidde, Gundula A1 - Moustapha, M. E. T1 - Adhesion promotion of thick polyphosphate-poly(allylamine) films onto polyolefin substrates by plasma polymers N2 - The adhesion of thick poly(allylamine)-polyphosphate layers (1 µm) deposited by the wet-chemical layer-by-layer technique (LbL) onto polyethylene or polystyrene (each 100 µm) was very low. To promote the adhesion of these LbL layers the polyolefin substrates were oxidized at the surface by short exposure to the oxygen plasma (2 or 5 s) and subsequently coated with an interlayer of plasma-deposited poly(allylamine) or poly(allyl alcohol) (100 nm). The plasma polymer interlayers have improved strongly the adhesion between polyolefin substrates and polyphosphate coatings. Such phosphate coatings are interesting for life sciences (nucleotide formation) but also for fire retardancy in combination with N-rich compounds such as melamine. The intention was to prefer chemical and hydrogen bonds for adhesion promoting because of their high binding energy. Therefore, the introduced oxygen-containing groups at the polyolefin surface could interact with the OH or NH2 groups of the adhesion-promoting plasma polymer interlayer. These groups were also able to interact strongly with the poly(allylamine)-polyphosphate topcoating. The coated polyolefins were investigated using Fourier Transform Infrared Spectroscopy in Attenuated Total Reflectance mode (FTIR-ATR), X-ray Photoelectron Spectroscopy (XPS), Thermo-Gravimetric Analyses (TGA) and Atomic Force Spectroscopy (AFM) and 90° peel test. KW - Plasma-polymerized poly(allylamine) KW - Adhesion KW - Layer-by-layer deposition KW - Plasma polymerization PY - 2016 UR - http://www.tandfonline.com/doi/abs/10.1080/01694243.2015.1095626 DO - https://doi.org/10.1080/01694243.2015.1095626 SN - 1648-4142 VL - 30 IS - 3 SP - 231 EP - 246 PB - Taylor & Francis AN - OPUS4-35885 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mohamed, Zeinab A1 - Friedrich, Jörg Florian A1 - Krüger, Simone A1 - Farouk, M. A1 - Moustapha, M.E. T1 - Plasma deposition of adhesion-promoting polymer layers onto polypropylene for subsequent covering with thick fire retardant coatings N2 - Melamine resins were used as 50-µm-thick fire retardant coatings for polypropylene (PP). Preceding deposition, low-pressure plasma polymer films of allyl alcohol were coated onto PP to improve the adhesion between PP and melamine resin coatings. The efficiency of such fire retardant coatings was confirmed by flame tests. The plasma-deposited polymer and the dip-coated melamine resin films were characterized by Fourier transform infrared-attenuated total reflectance spectroscopy and X-ray photoelectron spectroscopy (XPS). The adhesion of coatings was measured using a 90° peel test with a doubled-faced adhesive tape. To detect the locus of failure, the peeled layer surfaces were inspected using optical microscopy and XPS. Thermal properties of PP thick melamine resin-coated films were analyzed by thermogravimetric analysis. KW - Polymer KW - Plasma KW - Polypropylene KW - Fire retardant KW - Melamine precursors KW - Plasma polymerization KW - Allyl alcohol KW - Flame retardants KW - Curing PY - 2015 DO - https://doi.org/10.1080/01694243.2015.1033878 SN - 0169-4243 SN - 1568-5616 VL - 29 IS - 14 SP - 1522 EP - 1533 PB - VNU Science Press CY - Utrecht AN - OPUS4-33112 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mohamed, Zeinab A1 - Friedrich, Jörg Florian A1 - Krüger, Simone T1 - Cured melamine systems as thick fire-retardant layers deposited by combination of plasma technology and dip-coating N2 - Melamine and melamine resins are widely used as fire-retardants for polymer building materials. Cured melamine systems are used in heat-sensitive items, such as furniture and window frames and sills. In this work, differently cured methylated poly(melamine-co-formaldehyde) (cmPMF) resins were used as fire-retardant coverage for poly(styrene) (PS) and poly(ethylene) (PE) building materials. Such polymer layers should have several tenths of micrometers thickness to produce sufficient fire retardancy. These thick layers were produced by dip-coating. To promote sufficient adhesion of such thick coating to the polyolefin substrates, also in the case of high temperatures occurring at fire exposure, the polymer substrates were firstly coated with a few hundred nanometer thick adhesion-promoting plasma polymer layer. Such thin plasma polymer layers were deposited by low-pressure plasma polymerization of allyl alcohol (ppAAl). It was assumed that the hydroxyl groups of ppAAl interact with the melamine resin; therefore, ppAAl was well suited as adhesion promoter for thick melamine resin coatings. Chemical structure and composition of polymer films were investigated using infrared-attenuated total reflectance and X-ray photoelectron spectroscopy (XPS). Peel strengths of coatings were measured. After peeling, the peeled polymer surfaces were also investigated using optical microscopy and XPS the layers for identification of the locus of peel front propagation. Thermal properties were analyzed using TGA (thermo-gravimetric analyses). Finally, the fire-retardant properties of such thick coated polymers were evaluated by exposure to flames. KW - Plasma polymerization KW - Dip-coating KW - Curing KW - Methylated poly(melamine-co-formaldehyde) KW - Polystyrene KW - Polyethylene KW - Flame retardancy KW - Polymer KW - Plasma KW - Melamine resin KW - Fire retardant PY - 2015 DO - https://doi.org/10.1080/01694243.2014.995911 SN - 0169-4243 SN - 1568-5616 VL - 29 IS - 9 SP - 807 EP - 820 PB - VNU Science Press CY - Utrecht AN - OPUS4-32795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mohamed, Zeinab A1 - Friedrich, Jörg Florian A1 - Krüger, Simone T1 - Adhesion promotion of thick fire-retardant melamine polymer dip-coatings at polyolefin surfaces by using plasma polymers N2 - Melamine and melamine resins are widely used as fire retardants for polymer materials used in pharmaceutical, plastic, textile, rubber, and construction industry. Melamine-based flame retardants act by blowing off intumescent layers, char formation, and emission of quenching ammonia gas and diluent molecular nitrogen. Special advantages are: low cost, low smoke density and toxicity, low corrosive activity, safe handling, and environmental friendliness. Methylated poly(melamine-co-formaldehyde) (mPMF) was used as thick (≥40 µm) fire-retardant coating for plasma pretreated polymers. A combined low-pressure plasma pretreatment consisting of oxygen plasma exposure followed by deposition of thin poly(allylamine) (ppAAm) and poly(allyl alcohol) (ppAAl) plasma polymers as adhesion promoters have improved the adhesion of thick mPMF coatings strongly. Chemical structure and composition of deposited polymer films were characterized by infrared-attenuated total reflectance and X-ray photoelectron spectroscopy (XPS). After peeling, the peeled layer surfaces were also investigated for identification of the locus of failure and their topography using optical microscopy and XPS. Often the adhesion promotion was so efficient that the peeling of coating was not possible. Thermal properties of plasma polymers and dip-coating films were analyzed by thermogravimetric analysis. Significant improvement of fire-retardant properties of coated polymers was confirmed by flame tests. KW - Adhesion KW - Thick melamine layers KW - Plasma polymerization KW - Dip-coating KW - Methylated poly(melamine-co-formaldehyde) KW - Polystyrene KW - Polyethylene KW - Flame retardancy KW - Fire retardant KW - Melamine resin KW - Polymer KW - Plasma PY - 2014 DO - https://doi.org/10.1080/01694243.2014.943339 SN - 0169-4243 SN - 1568-5616 VL - 28 IS - 21 SP - 2113 EP - 2132 PB - VNU Science Press CY - Utrecht AN - OPUS4-31485 LA - eng 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 - 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 - JOUR A1 - Swaraj, Sufal A1 - Oran, Umut A1 - Lippitz, Andreas A1 - Schulze, Rolf-Dieter A1 - Friedrich, Jörg Florian A1 - Unger, Wolfgang T1 - Surface Analysis of Plasma-Deposited Polymer Films, 2: Analysis of Post-Plasma Air Reacted Plasma Polymerized Styrene by X-Ray Photoelectron Spectroscopy and X-Ray Absorption Spectroscopy N2 - Chemical properties of plasma-polymerized styrene films can be effectively controlled by the appropriate choice of external plasma parameters, such as duty cycle, power and monomer pressure. Chemical properties here are the regularity of the primary structure, the amount of long living radicals and branching or cross-linking or both in plasma polymerized styrene films, which can be indirectly monitored by X-ray photoelectron spectroscopy (XPS) and near edge X-ray absorption fine structure (NEXAFS) spectroscopy. Principally, XPS and NEXAFS spectra of plasma-polymerized styrene show all the spectroscopic fingerprints characteristic of atactic polystyrene indicating an inherent similarity of the respective primary chemical structures. There is an increase in irregularity and radical concentration for the plasma deposited films with increasing duty cycle or power. With an increase in monomer pressure, a decreased level of monomer fragmentation and, consequently, an increase in regularity must be concluded from the experimental data. The applied power regulates the fragmentation of the monomers as monitored by spectroscopic signals correlated to the aromatic rings. A trend in the extent of the post-plasma oxygen incorporation according to the variation of the various external plasma parameters was deduced, which agrees with earlier ToF-SIMS findings KW - Chemical characterization KW - ESCA/XPS KW - NEXAFS KW - Plasma polymerization KW - Polystyrene PY - 2004 DO - https://doi.org/10.1002/ppap.200400022 SN - 1612-8850 SN - 1612-8869 VL - 1 SP - 134 EP - 140 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-6935 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Oran, Umut A1 - Swaraj, Sufal A1 - Friedrich, Jörg Florian A1 - Unger, Wolfgang T1 - Surface Analysis of Plasma-Deposited Polymer Films, 3: In situ Characterization of Plasma-Deposited Ethylene Films by ToF-SSIMS N2 - Pulsed-plasma-deposited ethylene films were studied by time-of-flight static secondary ion mass spectrometry (ToF-SSIMS) before and after exposure to ambient air. The influence of the external plasma parameters on the secondary ion mass spectra of plasma-deposited ethylene films was investigated. From these data, information on the chemical character of the plasma-deposited ethylene films was derived. The investigation of the effect of external plasma parameters on the chemical character of the plasma-deposited ethylene films revealed that there were some drastic changes in the secondary ion mass spectra of the films. It was found that fragmentation and re-arrangement of the monomer molecules in the plasma, which affects the chemical character of the deposited films, vary according to the external plasma parameters. When the plasma polymers are exposed to air, extensive oxygen incorporation occurs. The oxygen uptake is high at the beginning and then it levels of. Some indications for the formation and decay of peroxy radicals (COO) and, subsequently, hydroperoxides (COOH) are found. It was observed that the oxygen uptake of the plasma deposited ethylene films increase when the plasma conditions become harder. KW - Ageing KW - Plasma polymerization KW - Polyethylene (PE) KW - ToF-SIMS PY - 2004 DO - https://doi.org/10.1002/ppap.200400025 SN - 1612-8850 SN - 1612-8869 VL - 1 SP - 141 EP - 152 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-6936 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Friedrich, Jörg Florian A1 - Retzko, Iris A1 - Kühn, Gerhard A1 - Unger, Wolfgang A1 - Lippitz, Andreas T1 - Plasma polymers with chemically defined structures in contact with metals N2 - The retention of chemical structure and functional groups during plasma polymerization was investigated. Usually plasma polymer layers, prepared by a continuous wave radio-frequency plasma, are often chemically irregular in their structure and composition. To minimize these irregularities low wattages and the pulsed plasma technique were applied to avoid fragmentations. The first goal was to produce plasma polymers comprising double or triple bonds as precursors for electrically conducting polymers. Acetylene, ethylene, butadiene and polystyrene were used as monomers and deposited as thin polymer films by pulsed plasmas of low wattages. Styrene polymerization was strongly enhanced in the dark phase (plasma off) of a pulsed r.f. plasma caused by the reactivity of the vinyl-type double bond. This could be confirmed by a verification of a rather high chemical regularity of the film sample. The oxygen content of this film measured by X-ray photoelectron spectrometry (XPS) was in situ 0% and after 24 h exposure to air lower than 1%. Additionally, post-plasma oxidations of trapped radicals with air could be suppressed using NO gas as radical quencher. Such quenched plasma polymer layers were completely stable against oxidation for a number of weeks. During the low-wattage pulse plasma polymerization metal atoms were simultaneously or layer by layer evaporated into the growing layer and in situ measured by XPS. These metal atoms are acting as dopants. Here, Li, K, Mg and Cr were used at different concentrations providing electrical conductivity and magnetic properties for the film. KW - Pulsed plasma KW - Plasma polymerization KW - Doping with metal atoms KW - Encapsulation of nanoparticles PY - 2001 DO - https://doi.org/10.1016/S0257-8972(01)01051-9 SN - 0257-8972 VL - 142-144 SP - 460 EP - 467 PB - Elsevier Science CY - Lausanne AN - OPUS4-6972 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Oran, Umut A1 - Swaraj, Sufal A1 - Friedrich, Jörg Florian A1 - Unger, Wolfgang T1 - Surface analysis of Plasma Deposited Polymer Films, 5 - ToF-SSIMS Characterization of Plasma Deposited Allyl Alcohol Films N2 - The effect of the composite plasma parameter P/F, where P is the plasma power and F is the monomer flow rate, on the chemical character of pulsed plasma deposited allyl alcohol films was investigated by ToF-SSIMS. Information on the unsaturated character, the cross-linked and/or branched character of the plasma polymer films was derived in detail. The problem of the retention of OH groups in plasma deposited allyl alcohol films was elucidated in detail using SSIMS data. The lowest conversion rate from the monomer's hydroxyl groups to other oxygen functionalities in the plasma was concluded for the plasma polymer film produced at a P/F ratio of 0.05 W · sccm-1. It was found that the overall oxygen content of the films decreased vs. increasing P/F ratio. Because the freshly prepared films were investigated without air exposure, ageing on ambient air could be studied in detail. It was found that in the case of plasma deposited allyl alcohol films the ageing on air is probably based on two competing processes which are discussed in detail. Additionally, a review of literature data on the characterization of plasma deposited allyl alcohol films is given. KW - Ageing KW - Allyl alcohol KW - Plasma polymerization KW - ToF-SIMS PY - 2005 DO - https://doi.org/10.1002/ppap.200400075 SN - 1612-8850 SN - 1612-8869 VL - 2 IS - 7 SP - 563 EP - 571 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-11933 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Swaraj, Sufal A1 - Oran, Umut A1 - Lippitz, Andreas A1 - Friedrich, Jörg Florian A1 - Unger, Wolfgang T1 - Aging of Plasma-Deposited Films Prepared from Organic Monomers N2 - Plasma-deposited polymer films were prepared from organic molecules and investigated using near edge X-ray absorption fine structure (NEXAFS) and X-ray photoelectron spectroscopy (XPS) for aging effects after exposure to air. Results from the investigation of homopolymers are summarized. Primarily the effect of the deposition parameters duty cycle and power are dealt with. The effect of the deposition parameter pressure is briefly discussed. An example to show the effect of feed gas composition on the aging of plasma polymerized ethylene/allyl alcohol and styrene/allyl alcohol copolymer is also given. In general, change in content of unsaturated or aromatic species, change in concentration of monomer functionality, and change in the oxygen content was observed in the plasma polymerized films on aging. KW - Plasma copolymer KW - ESCA/XPS KW - NEXAFS KW - Plasma polymerization PY - 2007 SN - 1612-8850 SN - 1612-8869 VL - 4 IS - S1 SP - S784 EP - S789 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-11934 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Swaraj, Sufal A1 - Oran, Umut A1 - Lippitz, Andreas A1 - Schulze, Rolf-Dieter A1 - Friedrich, Jörg Florian A1 - Unger, Wolfgang T1 - Surface Analysis of Plasma-Deposited Polymer Films, 4 - In situ Characterization of Plasma-Deposited Ethylene Films by XPS and NEXAFS N2 - XPS and NEXAFS spectroscopy were used for the chemical characterization of pulsed plasma-deposited ethylene films before and after exposure to ambient air. The influence of external plasma parameters on the spectroscopic results was investigated. Information on the chemical character of the plasma-polymerized films, such as the regularity of the primary structure, the amount of long-living radicals, and branching or cross-linking or both was derived from this data. Irregularity and radical concentration for post-plasma reactions of the plasma-deposited films increased with the duty cycle or power. A decreased level of monomer fragmentation and, consequently, an increase in regularity is partially concluded from the experimental data when the monomer pressure is increased. The concentration of surface radicals available for post-plasma reactions also increased with monomer pressure. The correlation found between the degree of the post-plasma oxygen incorporation and the variation of the various external parameters agreed with earlier ToF-SSIMS findings. KW - ESCA/XPS KW - NEXAFS KW - Plasma polymerization KW - Polyethylene (PE) KW - Thin films PY - 2005 DO - https://doi.org/10.1002/ppap.200400070 SN - 1612-8850 SN - 1612-8869 VL - 2 IS - 4 SP - 310 EP - 318 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-11940 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Oran, Umut A1 - Swaraj, Sufal A1 - Friedrich, Jörg Florian A1 - Unger, Wolfgang T1 - Surface analysis of plasma-deposited polymer films by Time of Flight Static Secondary Ion Mass Spectrometry (ToF-SSIMS) before and after exposure to ambient air N2 - Pulsed plasma deposited styrene and ethylene films were studied by Time of Flight Static Secondary Ion Mass Spectrometry (ToF-SSIMS) before and after exposure to ambient air. The influence of the external plasma parameters on the secondary ion mass spectra of plasma deposited films was investigated. Approaches for the interpretation of SSIMS spectra of organic materials were reviewed and applied to the evaluation of SSIMS data of plasma deposited films. From these data, information on the chemical character of the plasma deposited films was derived. When the plasma polymers are exposed to air oxygen incorporation occurs. The oxygen uptake is high at the beginning and then it levels of. A relation that “higher the regularity of the film lower is the oxygen uptake” was found. Harder plasma conditions, which could be obtained by applying higher plasma power or lower monomer flow rate, result in higher oxygen uptake and vice versa. KW - Plasma polymerization KW - Polyethylene (PE) KW - Polystyrene (PS) KW - SIMS KW - Ageing PY - 2005 DO - https://doi.org/10.1016/j.surfcoat.2005.02.032 SN - 0257-8972 VL - 200 IS - 1-4 SP - 463 EP - 467 PB - Elsevier Science CY - Lausanne AN - OPUS4-11044 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Swaraj, Sufal A1 - Oran, Umut A1 - Lippitz, Andreas A1 - Friedrich, Jörg Florian A1 - Unger, Wolfgang T1 - Study of influence of external plasma parameters on plasma polymerised films prepared from organic molecules (acrylic acid, allyl alcohol, allyl amine) using XPS and NEXAFS N2 - Plasma polymerised films of acrylic acid, allyl alcohol and allyl amine were prepared and studied by XPS (X-ray photoelectron spectroscopy) and XAS (X-ray absorption spectroscopy). The influence of external plasma parameters on certain chemical aspects of the films was investigated. The use of XPS and NEXAFS (near edge X-ray absorption fine structure) as complimentary tools in the surface characterisation of thin films has been highlighted. Certain chemical aspects of the plasma polymerised films such as presence of ROCdouble bond; length as m-dashO in the case of plasma polymerised acrylic acid films, presence of RCdouble bond; length as m-dashO and RC–OR bonds in case of plasma polymerised allyl alcohol films and presence of RCdouble bond; length as m-dashN and C?N in case of plasma polymerised allyl amine films were studied. The concentration of ROCdouble bond; length as m-dashO species was found to decrease with increase in r.f. duty cycle in the case of plasma polymerised acrylic acid films. In case of plasma polymerised allyl alcohol films there is a decrease in the concentration of RCdouble bond; length as m-dashO species and increase in the concentration of RC–OR species at higher pressures, while in the case of plasma polymerised allyl amine films the concentration of RCdouble bond; length as m-dashN and C?N increases at higher powers, with an increase in C?N more pronounced at higher powers. KW - Plasma polymerization KW - NEXAFS KW - XPS KW - Plasma parameter PY - 2005 DO - https://doi.org/10.1016/j.surfcoat.2005.01.083 SN - 0257-8972 VL - 200 IS - 1-4 SP - 494 EP - 497 PB - Elsevier Science CY - Lausanne AN - OPUS4-11045 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mix, Renate A1 - Gerstung, Vanessa A1 - Falkenhagen, Jana A1 - Schulze, Rolf-Dieter A1 - Friedrich, Jörg Florian T1 - Characterization of plasma-polymerized allyl alcohol polymers and copolymers with styrene KW - Plasma polymerization KW - Surface functionalization KW - Molar mass PY - 2007 SN - 0169-4243 SN - 1568-5616 VL - 21 IS - 5-6 SP - 487 EP - 508 PB - VNU Science Press CY - Utrecht AN - OPUS4-14765 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Swaraj, Sufal A1 - Oran, Umut A1 - Friedrich, Jörg Florian A1 - Lippitz, Andreas A1 - Unger, Wolfgang T1 - Surface Chemical Analysis of Plasma-Deposited Copolymer Films Prepared from Feed Gas Mixtures of Ethylene or Styrene with Allyl Alcohol N2 - Plasma deposited styrene/allyl alcohol and ethylene/allyl alcohol copolymer films were prepared and characterized using XPS, NEXAFS and ToF-SIMS. The relative partial flow rates of the co-monomers are used as deposition process parameters to vary and all other process parameters were constrained to conditions optimized for retention of functional groups. By doing this it is possible to control certain chemical properties of the copolymer films such as unsaturation, oxygen and hydroxyl group relative surface contents. The aging behavior of the plasma copolymer films on air was studied, too. Non-linear variations of relative oxygen contents, contents of C—OR species and contents of carbonyl species are obtained vs. variation of feed gas composition for both monomer combinations. The chemical character of the plasma copolymer films varies between the limits given by the respective plasma homopolymers. The observed non-linear correlations are discussed in terms of approaches developed for classic radical copolymerization. The aging behavior of the different plasma copolymers films depends on the feed gas composition. Principally these aging phenomena known from plasma polymer aging studies of that respective monomer which dominates the character of the plasma copolymer are observed. KW - Plasma polymers KW - Plasma copolymers KW - XPS KW - NEXAFS KW - Allyl alcohol KW - ESCA/XPS KW - Plasma polymerization KW - ToF-SIMS PY - 2007 SN - 1612-8850 SN - 1612-8869 VL - 4 IS - 4 SP - 376 EP - 389 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-14846 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Meyer-Plath, Asmus A1 - Mix, Renate A1 - Friedrich, Jörg Florian ED - Mittal, K. T1 - Aspects of amino functionalization of polypropylene surfaces for adhesion promotion of thermally-evaporated copper films KW - Plasma polymerization KW - Surface functionalization KW - Gas discharge KW - Grafting KW - Amino groups KW - Copper KW - Metallization KW - Adhesion PY - 2007 SN - 978-90-6764-455-6 SN - 90-6764-455-2 VL - 3 SP - 177 EP - 198 PB - VSP CY - Leiden AN - OPUS4-15733 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Friedrich, Jörg Florian T1 - Mechanisms of plasma polymerization - reviewed from a chemical point of view N2 - Several reaction mechanisms have been proposed for the formation of plasma polymers, such as monomer fragmentation followed by poly-recombination into randomly structured and crosslinked films; fragmentation, accompanied by the formation of acetylene or other film-forming intermediates and deposition of polystyrene-like material; plasma-initiation of a radical chain-growth polymerization; and ion-molecule reactions, as well as ionic chain-growth polymerization. The bulk structure of plasma polymers is completely irregular, far from that of conventional polymers. The retention of functional groups during plasma polymerization tends to be greater than that of the entire monomer structure found again as an intact repeat unit in the resulting plasma polymer. An alternative method for depositing ultra-thin, pin-hole free coatings, ones that possess regular structures, is by electrospray ionization (ESI) of pre-fabricated polymers. KW - Fragmentation-recombination KW - Mechanism KW - Plasma polymerization KW - Pulsed plasma KW - Structure of plasma polymers PY - 2011 DO - https://doi.org/10.1002/ppap.201100038 SN - 1612-8850 SN - 1612-8869 VL - 8 IS - 9 SP - 783 EP - 802 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-24502 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 - 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 - JOUR A1 - Mohamed, Zeinab A1 - Krüger, Simone A1 - Hidde, Gundula A1 - Schimanski, A. A1 - Jäger, Christian A1 - Friedrich, Jörg Florian T1 - Deposition of thick polymer or inorganic layers with flame-retardant properties by combination of plasma and spray processes N2 - Mixtures of hexamethyldisiloxane (HMDSO) and oxygen have been used for deposition of SiO2-like layers by plasma polymerization under low-pressure conditions onto polyethylene and polystyrene used as basecoat. Water glass was cast onto these 0.5 µm plasma thick siloxane-like layers with a thickness of 5 to 40 µm. The adhesion of these bilayer systems and their flame resistance were tested. The effect of different plasma parameters such as monomer/gas ratio, pressure and power input into the discharge on the deposition rate and the composition of the formed layers was studied. Characterization and chemical composition of the formed films were performed using infrared, X-ray photoelectron and solid state nuclear magnetic resonance spectroscopy. Peel strengths of composites were measured and the locus of peel front propagation was detected. Thermal properties of composites were analyzed by thermo-gravimetric analysis. Finally, the fire-retardant properties of thick coated polymers were determined by exposure to flames and the behavior of coatings on the polymers during flaming was observed visually. KW - Plasma polymerization KW - Hexamethyldisiloxane plasma polymer KW - Polystyrene KW - Polyethylene KW - Flame retardancy PY - 2013 DO - https://doi.org/10.1016/j.surfcoat.2013.04.039 SN - 0257-8972 VL - 228 SP - 266 EP - 274 PB - Elsevier B.V. CY - Lausanne AN - OPUS4-28735 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Kühn, Gerhard A1 - Mix, Renate A1 - Friedrich, Jörg Florian T1 - Surface Controlled Fire Retardancy of Polymers Using Plasma Polymerisation N2 - Communication: Fire retardant coatings are deposited on polyamide-66 using plasma polymerisation. Chemical composition and thickness of deposits are adjusted varying the plasma treatment based on hexamethydisiloxane mixed with oxygen. The fire retardancy performances are evaluated using a cone calorimeter. The correlation between fire retardancy and thickness as well as chemical composition is discussed. KW - Cone calorimeter KW - Flame retardance KW - Heat release KW - Plasma polymerization KW - Polyamides PY - 2002 DO - https://doi.org/10.1002/1439-2054(20020901)287:9<579::AID-MAME579>3.0.CO;2-6 SN - 1438-7492 SN - 1439-2054 VL - 287 IS - 9 SP - 579 EP - 582 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-1537 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -