Theory Instrumentation Applications Theory Instrumentation Applications SurPASS Electrokinetic...
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Transcript of Theory Instrumentation Applications Theory Instrumentation Applications SurPASS Electrokinetic...
Theory
Instrumentation
Applications
Theory
Instrumentation
Applications
SurPASS Electrokinetic AnalyzerZeta Potential Measurement for Solid Samples
SurPASS Electrokinetic AnalyzerZeta Potential Measurement for Solid Samples
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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
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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)
electrodeelectrode
sampleflowingliquid
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+ + + + + + + +Electrochemical double layer at equilibrium
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++ + + + + + + +
Fluid Flow
Electrolyte flow forced across solid surface
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++
++ ++ + +
Fluid Flow
Ion accumulation causes potential difference
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++
++ ++ + +
Backflow Current
Potential difference causes backflow current
Mechanism of Streaming Potential
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SurPASS Measurement Set-Up
RS 232
VisioLab for SurPASS
SurPASS Electrokinetic Analyzer
ConductivitypH
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Cylindrical Cell
Natural and technical fibres Hair Textile fibres and fabrics Powder samples with > 25 µm size Particle and granular samples
electrolyteinlet/outlet
electrolyteinlet/outlet
perforateddisc
sample
electrode
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Clamping Cell
25 5 mm2
electrolyteinlet/outlet
spacersample
Flat membranes Foils Polymer sheets Rigid samples of different thickness
and shape with a flat surface
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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
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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.
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Textile purification
Fibre swelling
Hydrophobicity
Particle retention
Glass fibre finishing
Characterization of sizing agents
Surfactant interaction
etc.
Textile and Technical Fibres
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Solution with SurPASSTime resolved measurement of treated polyester fibres in Cylindrical Cell
Characterization of Polyester Fibre Preparation
SurfactantZeta potential (mV)
T = 0 min T = 15 min T = 60 min
untreated -35.10 -34.93
anionic-55.49 -57.49
-48.68 -51.75 -48.36
cationic
-22.22 -28.22 -32.24
-24.92 -29.41
-18.32 -18.15 -16.8
-13.17 -16.11
non-ionic -37.32 -36.87
Field of ApplicationTreatment of synthetic fibres with surface-active compounds after spinning to assure textile processing
ChallengeCharacterization of these surface-active compounds to forecast textile processibility of fibres
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100 150 200 250 300
Adhesive Length (10-6 N/tex)
Zet
a P
oten
tial (
mV
)
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Glass Fibre Finishing
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2 3 4 5 6 7 8 9 10 11
pH (in 10-3 M KCl)
Zet
a P
ote
ntia
l (m
V)
untreated
sized
AMEO
0
20
40
60
80
100
120
140
15 25 35 45 55 65 75
lv (mJ/m2)
K
lv c
os
sv = 49.6 mJ/m2
sv = 47.8 mJ/m2
Electrokinetic measurement shows higher sensitivity to changes in surface chemistry of glass fibres than contact angle measurement
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Un
trea
ted
Sh
ampo
o
Rin
se
Co
ndi
tion
er
Rin
se
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0
10
20
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Ze
ta P
ote
ntia
l (m
V)
Zeta Potential of Human Hair
Source: E.D.Goddard, P.S.Leung, Sonderdruck aus Parfümerie und Kosmetik 68 (1987)
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Surface modification
Lacquer adhesion
Composite materials
Hydrophobic vs. hydrophilic behaviour
Protein adsorption in biomaterials engineering
Wetting and de-wetting behaviour
etc.
Polymer Characterization
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Hydrophilisation of Polyolefines
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pH
Zet
a P
oten
tial (
mV
)
untreated 1 min
2 min 3 min
4 min 5 min
0
20
40
60
80
100
0 1 2 3 4 5Treatment Time (min)
Con
tact
Ang
le (
°)
Aim Modification of the polymer surface
properties with retention of the bulk behaviour
Example
Introduction of acidic surface groups
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Plastics for Medical Application
Field of ApplicationMembrane material for haemodialysis
ChallengeCompatibility of membrane material with human organism
Solution with SurPASSZeta potential determination of capillary membranes in Cylindrical Cell and flat membranes in Clamping Cell
Examination of plastics surface in natural aqueous environment
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Zet
a P
oten
tial (
mV
)
untreat w/o hep
amine-mod w/o hep
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2 3 4 5 6 7 8 9 10 11pH
Zet
a P
oten
tial (
mV
)
untreat w/ hep
amine-mod w/ hep
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Metal Oxide and Semiconductor Processes
Photoresist coating
Silicon wafer cleaning
Metal layer characterization
Chemical Mechanical Polishing
Particle adhesion
etc.
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pH
Zet
a P
oten
tial (
mV
)
alkaline pickled/boiled
alkaline pickled
alkaline/acid pickled
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 pHSource: C. Bellmann et al, Fresenius J Anal Chem 358 (1997) 255
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pH
Zet
a P
oten
tial (
mV
)
alkaline pickled/boiled
alkaline pickled
alkaline/acid pickled
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
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0
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2 3 4 5 6 7 8 9 10
pH
Pa
rtic
le n
o.
on
wa
fer
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Ze
ta P
ote
ntia
l (mV
)
Conc. of PSL
Piranha
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Zet
a P
oten
tial (
mV
)
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a P
oten
tial (
mV
)
Piranha
Piranha + BOE
Piranha, BOE + H3PO4
RCA 1
Particle Deposition on Si3N4 Wafer
Sample TreatmentRatio
IEPSi/N Si/O N/O
Piranha 0.77 2.99 3.88 3.7
Piranha + BOE 0.81 3.78 4.66 5.3
Piranha, BOE + H3PO4 0.80 2.53 3.16 3.5
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)
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CMP Slurry / Cu Surface Interaction
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0
5
10
15
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25
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1E-07 1E-06 1E-05 1E-04 1E-03 1E-02surfactant concentration in 10-4 M KCl (mol/l)
Zet
a P
oten
tial (
mV
)
cationic
non-ionic
anionic
cationic dodecyl trimethyl ammounium bromide
non-ionic Marlipal O13/100 (C13-alcohol polyethylene glycol ether)
anionic sodium dodecyl sulphate
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