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SurPASS Electrokinetic Analyzer Zeta Potential Measurement for Solid Samples. Theory Instrumentation Applications. Surface and Interface Analysis. Spectroscopy Secondary Ion Mass Spectrometry X-ray Photoelectron Spectroscopy Energy Dispersive X-ray fluorescence Raman spectroscopy
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SurPASS Electrokinetic AnalyzerZeta Potential Measurement for Solid Samples Theory Instrumentation Applications
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 Interfaceanalysis • 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
flowingliquid sample electrode electrode 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)
+ + + + + + + + Electrochemical double layer at equilibrium - - - - - - - - - - - Fluid Flow + + + + + + + + + - - - - - - - - - - - Fluid Flow + + + + + + + + - - - - - - - - - - - Backflow Current + + + + + + + + - - - - - - - - - - - Mechanism of Streaming Potential Electrolyte flow forced across solid surface Ion accumulation causes potential difference Potential difference causes backflow current
RS 232 VisioLab for SurPASS pH Conductivity SurPASS Measurement Set-Up SurPASS Electrokinetic Analyzer
Cylindrical Cell electrolyte inlet/outlet electrode sample perforateddisc • Natural and technical fibres • Hair • Textile fibres and fabrics • Powder samples with > 25 µm size • Particle and granular samples electrolyte inlet/outlet
25 5 mm2 electrolyte inlet/outlet spacer sample Clamping Cell • Flat membranes • Foils • Polymer sheets • Rigid samples of different thickness and shape with a flat surface
dU dp = 0 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
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.
Textile and Technical Fibres Textile purification Fibre swelling Hydrophobicity Particle retention Glass fibre finishing Characterization of sizing agents Surfactant interaction etc.
Characterization of Polyester Fibre Preparation 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 Solution with SurPASS Time resolved measurement of treated polyester fibres in Cylindrical Cell
Glass Fibre Finishing • Electrokinetic measurement shows higher sensitivity to changes in surface chemistry of glass fibres than contact angle measurement sv = 47.8 mJ/m2 sv = 49.6 mJ/m2
Zeta Potential of Human Hair Untreated Shampoo Rinse Rinse Conditioner Source: E.D.Goddard, P.S.Leung, Sonderdruck aus Parfümerie und Kosmetik 68 (1987)
Polymer Characterization Surface modification Lacquer adhesion Composite materials Hydrophobic vs. hydrophilic behaviour Protein adsorption in biomaterials engineering Wetting and de-wetting behaviour etc.
Hydrophilisation of Polyolefines Aim • Modification of the polymer surface properties with retention of the bulk behaviour Example Introduction of acidic surface groups
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
Metal Oxide and Semiconductor Processes • Photoresist coating • Silicon wafer cleaning • Metal layer characterization • Chemical Mechanical Polishing • Particle adhesion • etc.
Electrokinetic Measurement of Aluminium Sheets Treatment • Alkaline pickled with NaOH and Na2CO3 and boiled in H20 for 10 min • Alkaline pickled only • Alkaline and then acid pickled with H2SO4 and H2O2 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
Electrokinetic Measurement of Aluminium Sheets Treatment • Alkaline pickled with NaOH and Na2CO3 and boiled in H20 for 10 min • Alkaline pickled only • Alkaline and then acid pickled with H2SO4 and H2O2 • 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
Particle Deposition on Si3N4 Wafer • Zeta potential depends on cleaning treatment of LPCVD Si3N4 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. 3rd Int. Symp. on Cleaning Technology in Semiconductor Device Manufacturing (1993)
CMP Slurry / Cu Surface Interaction cationic dodecyl trimethyl ammounium bromide non-ionic Marlipal O13/100 (C13-alcohol polyethylene glycol ether) anionic sodium dodecyl sulphate