Theory Instrumentation Applications Theory Instrumentation Applications SurPASS Electrokinetic Analyzer Zeta Potential Measurement for Solid Samples

© Anton Paar GmbH 2006 Surface and Interface Analysis Spectroscopy  Secondary Ion Mass Spectrometry  X-ray Photoelectron Spectroscopy  Energy Dispersive X-ray fluorescence  Raman spectroscopy  Ion Scattering Spectroscopy  IR, UV/VIS spectroscopy Microscopy  Scanning Electron Microscopy  Transmission Electron Microscopy  Atomic Force Microscopy  Confocal Laser Scanning Microscopy  Light microscopy Interface analysis  Contact angle (static, dynamic)  Surface tension  Streaming potential  Surface spectroscopy  Gas adsorption Analysis of …  … chemical composition of surface  … surface topography  … morphology of interfaces  … surface energy and (de-)wetting

© Anton Paar GmbH 2006 Streaming Potential Method Liquid phase (electrolyte solution) pumped through the measuring cell (containing sample)  pressure difference  relative movement of the charges in the electrochemical double layer  detection of streaming potential  U =  U(  p) electrode sample flowing liquid

© Anton Paar GmbH Electrochemical double layer at equilibrium Fluid Flow Electrolyte flow forced across solid surface Fluid Flow Ion accumulation causes potential difference Backflow Current Potential difference causes backflow current Mechanism of Streaming Potential

© Anton Paar GmbH 2006 SurPASS Measurement Set-Up RS 232 VisioLab for SurPASS SurPASS Electrokinetic Analyzer Conductivity pH

© Anton Paar GmbH 2006 Cylindrical Cell Natural and technical fibres Hair Textile fibres and fabrics Powder samples with > 25 µm size Particle and granular samples electrolyte inlet/outlet electrolyte inlet/outlet perforated disc sample electrode

© Anton Paar GmbH 2006 Clamping Cell 25  5 mm 2 electrolyte inlet/outlet spacer sample Flat membranes Foils Polymer sheets Rigid samples of different thickness and shape with a flat surface

© Anton Paar GmbH 2006 Pressure Ramp Measurement  Electrolyte flow from left  right  Measurement of streaming potential at various differential pressure  Reversal of flow direction  Linear regression for evaluation of “pressure ramp” slope  =   dU dp    0  0

© Anton Paar GmbH 2006 SurPASS Applications in... Polymer industry Synthetic fibre and textile industry Processing of non-metallic, inorganic materials Mining industry Printing industry Membrane and filtration technology Biomaterials Semiconductor industry Paint and varnish industry Cosmetics industry etc.

© Anton Paar GmbH 2006 Textile purification Fibre swelling Hydrophobicity Particle retention Glass fibre finishing Characterization of sizing agents Surfactant interaction etc. Textile and Technical Fibres

© Anton Paar GmbH 2006 Solution with SurPASS Time resolved measurement of treated polyester fibres in Cylindrical Cell Characterization of Polyester Fibre Preparation Surfactant Zeta potential (mV) T = 0 minT = 15 minT = 60 min untreated anionic cationic non-ionic Field of Application Treatment of synthetic fibres with surface- active compounds after spinning to assure textile processing Challenge Characterization of these surface-active compounds to forecast textile processibility of fibres

© Anton Paar GmbH 2006 Glass Fibre Finishing  sv = 49.6 mJ/m 2  sv = 47.8 mJ/m 2 Electrokinetic measurement shows higher sensitivity to changes in surface chemistry of glass fibres than contact angle measurement

© Anton Paar GmbH 2006 Untreated Shampoo Rinse Conditioner Rinse Zeta Potential of Human Hair Source: E.D.Goddard, P.S.Leung, Sonderdruck aus Parfümerie und Kosmetik 68 (1987)

© Anton Paar GmbH 2006 Surface modification Lacquer adhesion Composite materials Hydrophobic vs. hydrophilic behaviour Protein adsorption in biomaterials engineering Wetting and de-wetting behaviour etc. Polymer Characterization

© Anton Paar GmbH 2006 Hydrophilisation of Polyolefines Aim Modification of the polymer surface properties with retention of the bulk behaviour Example Introduction of acidic surface groups

© Anton Paar GmbH 2006 Plastics for Medical Application Field of Application Membrane material for haemodialysis Challenge Compatibility of membrane material with human organism Solution with SurPASS Zeta potential determination of capillary membranes in Cylindrical Cell and flat membranes in Clamping Cell Examination of plastics surface in natural aqueous environment

© Anton Paar GmbH 2006 Metal Oxide and Semiconductor Processes Photoresist coating Silicon wafer cleaning Metal layer characterization Chemical Mechanical Polishing Particle adhesion etc.

© Anton Paar GmbH 2006 Electrokinetic Measurement of Aluminium Sheets Treatment  Alkaline pickled with NaOH and Na 2 CO 3 and boiled in H 2 0 for 10 min  Alkaline pickled only  Alkaline and then acid pickled with H 2 SO 4 and H 2 O 2 Results  Alkaline pickling and boiling introduces only few dissociable surface groups  with no plateau in zeta potential  and IEP in the neutral range  Procedure produces AlOOH (Böhmit) on Al(OH) 3 (Bayerit) layer  More dissociable surface groups without boiling  plateau in zeta potential at low pH  IEP shifted towards higher pH Source: C. Bellmann et al, Fresenius J Anal Chem 358 (1997) 255

© Anton Paar GmbH 2006 Electrokinetic Measurement of Aluminium Sheets Treatment  Alkaline pickled with NaOH and Na 2 CO 3 and boiled in H 2 0 for 10 min  Alkaline pickled only  Alkaline and then acid pickled with H 2 SO 4 and H 2 O 2  Application of organic oligomer material with acidic functional groups Results  IEP changes to lower pH  Ion adsorption processes dominate  Oligomer removed for alkaline/acid pickled Al surface at pH > 7 Source: C. Bellmann et al, Fresenius J Anal Chem 358 (1997) 255

© Anton Paar GmbH 2006 Particle Deposition on Si 3 N 4 Wafer Sample Treatment Ratio IEP Si/NSi/ON/O Piranha Piranha + BOE Piranha, BOE + H 3 PO Zeta potential depends on cleaning treatment of LPCVD Si 3 N 4 wafers Correlation between N/O ratio (XPS data) and IEP Contamination of wafer surface with Polystyrene particles follows the zeta potential Source: D.Jan, S.Raghavan, Proc. 3 rd Int. Symp. on Cleaning Technology in Semiconductor Device Manufacturing (1993)

© Anton Paar GmbH 2006 CMP Slurry / Cu Surface Interaction cationicdodecyl trimethyl ammounium bromide non-ionicMarlipal O13/100 (C 13 -alcohol polyethylene glycol ether) anionicsodium dodecyl sulphate

© Anton Paar GmbH 2006 Partial List of EKA Customers