TY - CONF A1 - Kunze, Ralf A1 - Neubert, Dietmar A1 - Brademann-Jock, Kerstin T1 - TG/MS-Untersuchungen an geschäumten Polymeren T2 - Symposium on Thermal Analysis in Industry and Research ; 27e Journées de Calorimétrie et d'Analyse Thermique (AFCAT) ; 22. Jahrestagung der Gesellschaft für Thermische Analyse e.V. (GEFTA) CY - Freiburg, Deutschland DA - 1996-09-24 KW - Polymer, geschäumt KW - Thermogravimetrie, TG KW - Massenspektrometer, MS KW - Dämmstoff PY - 1996 SP - 166 EP - 168 PB - GEFTA Office CY - Freiburg AN - OPUS4-692 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Kunze, Ralf A1 - Neubert, Dietmar A1 - Tidjani, Adams T1 - ZnS as fire retardant in plasticised PVC N2 - The flame retardant effect of zinc sulphide (ZnS) in plasticised poly(vinyl chloride) (PVC-P) materials was investigated. PVC-P containing different combinations of additives such as 5% ZnS, 5% of antimony oxide (Sb2O3) and 5% of mixtures based on Sb2O3 and ZnS were compared. The thermal degradation and the combustion behaviour were studied using thermogravimetry (TG), coupled with FTIR (TG-FTIR) or with mass spectroscopy (TG-MS), and a cone calorimeter, respectively. A detailed and unambiguous understanding of the decomposition and release of the pyrolysis products was obtained using both TG-MS and TG-FTIR. The influence of ZnS, Sb2O3 and the corresponding mixtures on the thermal decomposition of PVC-P was demonstrated. Synergism was observed for the combination of the two additives. The combustion behaviour (time to ignition, heat release, smoke production, mass loss, CO production) was monitored versus external heat fluxes between 30 and 75 kW m-2 with the cone calorimeter. Adding 5% of ZnS has no significant influence on the fire behaviour of PVC-P materials beyond a dilution effect, whereas Sb2O3 works as an effective fire retardant. Synergism of ZnS and Sb2O3 allows the possibility of replacing half of Sb2O3 by ZnS to reach equivalent fire retardancy. KW - PVC KW - ZnS KW - Fire retardancy KW - TG-FTIR KW - Cone calorimeter PY - 2002 U6 - https://doi.org/10.1002/pi.845 SN - 0959-8103 SN - 1097-0126 SN - 0007-1641 VL - 51 IS - 3 SP - 213 EP - 222 PB - Wiley InterScience CY - Chichester, West Sussex AN - OPUS4-1291 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schartel, Bernhard A1 - Kunze, Ralf A1 - Neubert, Dietmar T1 - ZnS as Fire Retardant in PVC-P T2 - 2nd International Conference on Polymer Modification, Degradation and Stabilisation (MoDeSt) CY - Budapest, Hungary DA - 2002-06-30 PY - 2002 VL - 82 IS - 2 PB - Elsevier CY - Orlando, Fla. AN - OPUS4-2437 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Witke, Klaus A1 - Kunze, Ralf A1 - Neubert, Dietmar A1 - Mehner, Hartmut A1 - Feist, M. A1 - Kemnitz, E. T1 - Two oxidation states and four different coordinations of iron in an unusual chloro complex: TG-MS, Raman and Mössbauer spectroscopic investigations of the thermal behaviour N2 - Conventional simultaneous thermal analysis, capillary-coupled TG–MS, in situ and ex situ Raman and Mössbauer spectroscopy, as well as chemical analysis have been used for the investigation of the first decomposition step of the mixed valence chloroferrate (dmpipzH2)6[Fe(II)Cl4]2[Fe(III)Cl4]2[Fe(II)Cl5][Fe(III)Cl6]. Under argon at ca. 200°C, an almost complete reduction proceeds in a solid state reaction forming Fe(II). It is accompanied by the release of HCl and, to a minor degree, carbon containing species. A multi-phase product with at least two chloroferrate species, coke, and C,H,N-containing polymers is formed. Binuclear iron complexes, such as (dmpipzH)2[Fe(II)2Cl6], and small amounts of (dmpipzH)[Fe(III)Cl4] have been proposed to be the major and minor component of the product mixture, respectively. KW - Mixed valence chloroferrate KW - Thermal decomposition KW - Intramolecular reduction PY - 2000 U6 - https://doi.org/10.1016/S0040-6031(00)00546-3 SN - 0040-6031 SN - 1872-762X VL - 361 IS - 1-2 SP - 53 EP - 60 PB - Elsevier CY - Amsterdam AN - OPUS4-988 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gajewski, Sven A1 - Maneck, Heinz-Eberhard A1 - Knoll, Uta A1 - Neubert, Dietmar A1 - Dörfel, Ilona A1 - Mach, Reinhard A1 - Strauß, Birgid A1 - Friedrich, Jörg Florian T1 - Purification of single walled carbon nanotubes by thermal gas phase oxidation N2 - Single walled carbon nanotubes (SWNT) have been produced in an electric arc discharge by using a graphite rod as anode which is filled with a powder mixture of graphite and metallic catalysts like nickel and yttrium. The soot material containing approximately a third of SWNT was collected from the cathode region as a soft, voluminous material. The main by-products in this process are amorphous carbon and graphitic nanoparticles which have to be removed by an appropriate purification process. The as-produced soot material was purified by gas phase oxidation in air at 355 °C. The oxidation of amorphous carbon in air is advantageous against wet chemical methods because it is better controllable. Thermogravimetric analysis and electron microscopy were used to investigate the oxidation behavior of the different kinds of carbon. Oxidation of SWNT and amorphous carbon occurs simultaneously even at moderate temperatures, whereas amorphous carbon is more rapidly oxidized than SWNT. For optimizing the purification procedure by gas phase oxidation, kinetic studies were used to determine the oxidation time for each component in the soot at a given temperature. So it is possible to remove the amorphous carbon quantitatively with minimal losses of SWNT. But it was found that graphitic nanoparticles have the highest stability against oxidation and could therefore not be quantitatively removed by this method without the complete destruction of SWNT. Therefore, the electric arc discharge process has to be a controlled process for minimum production of graphitic nanoparticles to obtain a material with a high content of SWNT. KW - Nanotubes KW - Cathodic arc discharge KW - Amorphous carbon KW - Oxidation PY - 2003 U6 - https://doi.org/10.1016/S0925-9635(02)00362-X SN - 0925-9635 VL - 12 IS - 3-7 SP - 816 EP - 820 PB - Elsevier CY - New York, NY AN - OPUS4-2516 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Kunze, Ralf A1 - Neubert, Dietmar T1 - Red Phosphorus-Controlled Decomposition for Fire Retardant PA 66 N2 - The thermal degradation and the combustion behavior of glass fiber-reinforced PA 66 materials containing red phosphorus were investigated. Thermogravimetry (TG), TG coupled with FTIR, and TG coupled with mass spectroscopy were used to investigate the thermal decomposition. The flame retardant red phosphorus was investigated with respect to the decomposition kinetics and the release of volatile products. The combustion behavior was characterized using a cone calorimeter. Fire risks and fire hazards were monitored versus external heat fluxes between 30 and 75 kW/m2. Red phosphorus acts in the solid phase and its efficiency depends on the external heat flux. The use of red phosphorus results in an increased amount of residue and in a corresponding decrease in total heat release. The decrease of the mass loss rate peak results in a corresponding decrease of the peak heat release. With increasing external heat flux applied the first effect on the total heat release decreases linearly, whereas the second effect on the peak heat release expands linearly. The investigation provides insight into the mechanisms of how the fire retardant PA 66 is achieved by red phosphorus controlling the degradation kinetics. Taking into account that a decrease of the volatile products also leads to a decrease of heat production in the flame zone and that the char acts as heat transfer barrier, a reduced pyrolysis temperature is suggested as a further feedback effect. T2 - 8th European Conference on fire retardant polymers CY - Alessandria, Italy DA - 2001-06-24 KW - PA 66 KW - Red phosphorus KW - Fire retardancy KW - TG-FTIR KW - Cone calorimeter PY - 2002 U6 - https://doi.org/10.1002/app.10144 SN - 0021-8995 SN - 1097-4628 VL - 83 IS - 10 SP - 2060 EP - 2071 PB - Wiley InterScience CY - Hoboken, NJ AN - OPUS4-1234 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schartel, Bernhard A1 - Kunze, Ralf A1 - Neubert, Dietmar A1 - Braun, Ulrike ED - Lewin, M. T1 - Mechanistic Studies on PA-66 Fire Retarded with Red Phosphorus T2 - 13th Conference on Recent Advances in Flame Retardancy of Polymeric Materials ; 13th Annual BCC Conference on Flame Retardancy CY - Stamford, CT, USA DA - 2002-06-03 PY - 2002 SN - 1-569-65890-0 VL - 13 SP - 93 EP - 103 PB - BCC CY - Norwalk, Conn. AN - OPUS4-1562 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Kunze, Ralf A1 - Bartholmai, Matthias A1 - Neubert, Dietmar A1 - Schriever, Robert T1 - TG-MS and TG-FTIR applied for an unambiguous thermal analysis of intumescent coatings N2 - Thermogravimetry (TG), thermogravimetry coupled with mass spectroscopy (TG-MS) and thermogravimetry coupled with Fourier transform infrared spectroscopy (TG-FTIR) were used to characterise the thermo-oxidative behaviour of two intumescent coating materials. The temperature dependence, the corresponding volatile products and the amount of residue of the different processes were determined. Using both TG-MS and TG-FTIR results in an unambiguous interpretation of the volatile products. Characteristics such as the influence of endothermic reactions, the release of non-flammable gases, the dehydrogenation enhancing the char formation and the stability of the cellular char were discussed in detail. It was demonstrated, that TG, TG-MS and TG-FTIR are powerful methods to investigate mechanisms in intumescent coatings and that they are suitable methods in respect to quality assurance and unambiguous identification of such materials. KW - Intumescent coating materials KW - TG KW - TG-FTIR KW - TG-MS PY - 2002 U6 - https://doi.org/10.1023/A:1022272707412 SN - 1388-6150 SN - 1418-2874 SN - 0368-4466 SN - 1572-8943 VL - 70 IS - 3 SP - 897 EP - 909 PB - Kluwer Academic Publ. CY - Dordrecht AN - OPUS4-2133 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Braun, Ulrike A1 - Knoll, Uta A1 - Bartholmai, Matthias A1 - Goering, Harald A1 - Neubert, Dietmar A1 - Pötschke, P. T1 - Mechanical, Thermal, and Fire Behavior of Bisphenol A Polycarbonate/Multiwall Carbon Nanotube Nanocomposites N2 - Nanocomposites of bisphenol A polycarbonate with 2, 4, 6, and 15 wt% multiwall carbon nanotubes (MWNT) and their use in fire retardancy are investigated. Their thermal behavior and pyrolysis are characterized using thermogravimetry, differential scanning calorimeter, oscillatory shear rheology, and dynamic mechanical analysis. The flammability is addressed using LOI and UL 94; the fire behavior, with a cone calorimeter using different irradiation. With increasing MWNT content the storage modulus is increased (10-20%) and melt viscosity increases by several orders of magnitude, particularly for low shear rates. The melt flow, dripping, and deformation during fire are hindered, which influences UL 94 and cone calorimeter results. The peak heat release rate is reduced up to 40-50% due to an improved barrier for small amounts (2 wt%) of MWNT and for low irradiation, whereas the effect is reduced for increasing irradiation and nearly vanishes for increasing filling. Adjuvant but also deleterious mechanisms result in the complex dependency on the MWNT content. Significant flame retardancy effects are specific and limited to only some fire properties. This study allows the materials' potential for implementation in different fire scenarios and tests to be assessed and provides insight into active mechanisms. KW - Flame retardancy KW - Nanocomposite KW - Carbon multiwall nanotube (MWNT) KW - Cone Caorimeter KW - Flammability PY - 2008 U6 - https://doi.org/10.1002/pen.20932 SN - 0032-3888 SN - 1548-2634 VL - 48 IS - 1 SP - 149 EP - 158 PB - Wiley CY - Hoboken, NY AN - OPUS4-16365 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Braun, Ulrike A1 - Knoll, Uta A1 - Neubert, Dietmar A1 - Schartel, Bernhard ED - Schartel, Bernhard T1 - Fire Retarding Mechanisms of Red Phosphorus in Polybutylenterephthalate (PBT) in Combination with Melamine Cyanurate or Zinc Oxide KW - Fire retardancy KW - Polyester KW - Red phosphorus KW - Thermal analysis KW - Cone calorimeter PY - 2007 SN - 978-3-8334-8873-3 SP - 35 EP - 49 PB - Books on Demand GmbH CY - Norderstedt AN - OPUS4-17662 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 U6 - 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 - Sickfeld, Jürgen A1 - Neubert, Dietmar A1 - Groß, Dieter T1 - Thermogravimetrie von Vulkanisaten PY - 1983 SN - 0022-9520 SN - 0948-3276 IS - 9 SP - 760 EP - 765 PB - Hüthig CY - Heidelberg AN - OPUS4-37790 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -