Surface and Interface Characterization of Polymer Films
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1 Surface and Interface Characterization of Polymer Films Jeff Shallenberger, Evans Analytical Group 104 Windsor Center Dr., East Windsor NJ Copyright 2013 Evans Analytical Group
2 Outline Introduction to surface chemical techniques X-ray photoelectron spectroscopy (XPS/ESCA) Time-of-flight secondary ion mass spectrometry (TOF-SIMS) Selected examples from polymer surfaces Identification of Defects on Metallized Polymer-PSA Laminate Failed Heat Seal from medical packaging Examining the sub-surface New technology available Copyright 2013 Evans Analytical Group 2
3 Surface chemistry related phenomena Wetting (hydrophobic vs. hydrophillic) Corrosion/oxidation Coatings Appearance (stains, hazes, residues, etc.) Adhesion Blooming, additive migration 3 Copyright 2010 Evans Analytical
4 What tools are available to probe the surface? 1. Microscopy SEM, AFM, TEM, optical microscopy Copyright 2010 Evans Analytical Group LLC 4
5 What tools are available to probe the surface? 2. Physical properties hardness, wear resistance, scratch resistance, contact angle, etc Images courtesy of 5 Copyright 2010 Evans Analytical
6 C*F2 COO What tools are available to probe the surface? CF 2 Intensity (CPS) 1/75/10, 90 -CF 3 C-C C*COO C-O and C*H-CF 2 Relative concentration 3. Surface chemistry XPS, Auger, TOF-SIMS Binding energy (ev) 100 Sample 114, run #2 first derivative 10 O Ti Nb Yb Pb Pt Si not acquired in SiO 2 layer 1 E N(E) Kinetic Energy (ev) EMS/MatSci/Trolier-McKinstry/114b.opj Depth (nm) Copyright 2010 Evans Analytical Group LLC 6
7 Other techniques Indirect surface techniques Extraction approaches followed by GC/MS, ICP, ICP-MS, etc. Bulk techniques XRF, SEM-EDS, XRD, ICP-MS, FTIR, Raman. 7 Copyright 2010 Evans Analytical
8 EAG Bubble Chart 8 Copyright 2010 Evans Analytical
9 Comparing Analytical Techniques Depth of Analysis ~ ~ ~ ~ 9 Copyright 2010 Evans Analytical
10 XPS XPS can detect and quantify all elements except for H and He, and provide chemical state information; making it a powerful survey analysis technique ~ 10 Copyright 2010 Evans Analytical
11 XPS Process (Photoelectric Effect) X-ray * * 11 Copyright 2010 Evans Analytical
12 Typical Data- Plasma treated polystyrene Copyright 2013 Evans Analytical Group 12
13 Typical Data- Plasma treated polystyrene Sample Carbon Nitrogen Oxygen Treated polystyrene Untreated polystyrene Copyright 2013 Evans Analytical Group 13
14 XPS Summary Strengths Elemental identification of all elements except H and He Chemical state identification (oxidation state) Quantitative analysis Can analyze insulating samples Limitations Detection limits typically ~500 ppm Smallest analytical area ~10 µm Limited organic information UHV technique Copyright 2012 Evans Analytical Group 14
15 TOF-SIMS TOF-SIMS is a very surface sensitive technique providing full elemental and molecular analysis with excellent detection limits. 15 Copyright 2013 Evans Analytical
16 Ion Induced Desorption Ejected Species: Atoms, Molecules, Clusters, Ions/Neutrals (+/-) Source for this image? 16 Copyright 2010 Evans Analytical
17 Typical Data O O C O C 149 O C H 2 C H m/z O O O C C O C H 2 C H Negative Spectrum of PET m/z 17 Copyright 2010 Evans Analytical
18 Typical Data TOF-SIMS Imaging of Alumina-Zirconia-Silica Materials Region 1 Spectrum Primary Ion Beam Chemical Map 1 m/z Total Ion Image Total Area Spectrum Chemical Map 2 m/z Region 2 Spectrum Sample m/z 18 Copyright 2010 Evans Analytical
19 Strengths TOF-SIMS Summary elemental and molecular information on thin (submonolayer) organic films/contaminants survey analysis ppm detection limits small spot size (0.2 µm) and mapping analyzes insulators and conductors Limitations organic information can be limited vacuum compatibility required at times, too surface sensitive Copyright 2012 Evans Analytical Group 19
20 Selected examples from polymer surfaces Identification of Defects on Metallized Polymer-PSA Laminate A laminate consisting of an acrylic-based pressure sensitive adhesive (PSA) on a polyester film bonded to a metallized PET with a silicone release layer experienced isolated defects that were µm in size. PET Copyright 2013 Evans Analytical Group 20
21 Identification of Defects on Metallized Polymer-PSA Laminate c/s Was there something on the surface of the PET prior to metallization that Y0BCY spe: hindered V6C adhesion? Apr 20 Al mono 12.5 W 50.0 µ ev e+003 max min Su1s/Point1: Metal side larger feature/ Y0BCY spe O C C O Si Binding Energy (ev) Copyright 2013 Evans Analytical Group 21
22 c/s Identification of Defects on Metallized Polymer-PSA Laminate Finding of silicone on PET surface under metallization seems suspicious. However, silicone release layer surrounded defect and silicones are notoriously mobile. Y0BCY spe: Underside V6C of PSA failure confirms locus of failure is at Al-PET interface 2011 Apr 20 Al mono 12.5 W 50.0 µ ev e+002 max min Al2p/Point3: Pigment side of failure/1 (Shft) Y0BCY spe Aluminum 2p Al Area C O Al Si Metal side of defect PSA side of defect Release layer Al 2 O What is this carbon due to? Binding Energy (ev) Copyright 2013 Evans Analytical Group 22
23 Identification of Defects on Metallized Polymer-PSA Laminate High resolution C 1s spectrum from underside of defect equal intensity C-O and O-C=O indicative of ester functional groups Could this be transfer of PET? Carbon 1s C-C O=C-O C-O Binding Energy (ev) Copyright 2013 Evans Analytical Group 23
24 Identification of Defects on Metallized Polymer-PSA Laminate 3.98 ev 1.54 ev 1.79 ev 4.27 ev Copyright 2013 Evans Analytical Group 24
25 Identification of Defects on Metallized Polymer-PSA Laminate C 1s peak positions are consistent with aliphatic ester, not PET PET surface was contaminated with some aliphatic ester prior to metallization Silicones contaminated the PET after the adhesion failure Copyright 2013 Evans Analytical Group 25
26 Failed Heat Seal from medical packaging Background: A medical device sterile package experienced adhesion failure at a polyethylene-ethylene acrylic acid (co-polymer) heat seal to polyethylene interface. EAA was added at 3% to improve adhesion and lower % of crystallinity. Adhesion problems can lead to loss of sterility. Analytical Approach: Examine good and bad surfaces prior to heat sealing to look for evidence of impurities with XPS and TOF-SIMS Copyright 2013 Evans Analytical Group 26
27 Failed Heat Seal from medical packaging Sample Carbon Oxygen Good PE-EAA surface Failed PE-EAA surface %EAA-PE, theory CH 2 Good Bad O-C=O Binding energy (ev) CH 2 O-C=O Binding Energy (ev) Copyright 2013 Evans Analytical Group 27
28 Failed Heat Seal from medical packaging XPS only finds only C-C and O-C=O Measurable difference in amount of total O suggests either: (a) difference in the amount of EAA at the surface or, (b) presence of some other O-C=O containing compound on the surface of the bad heat seal XPS unable to distinguish between these two scenarios Copyright 2013 Evans Analytical Group 28
29 Failed Heat Seal from medical packaging We use the better molecular specificity inherent to TOF-SIMS to look for foreign species. Copyright 2013 Evans Analytical Group 29
30 Failed Heat Seal from medical packaging Series of more intense peaks observed on Bad seal surface Peaks are characteristic of hydroxyhydrocinnamate compounds such as Irganox 1010 or amu = C 15 H 23 O amu = C 16 H 25 O amu = C 17 H 23 O 2 + Copyright 2013 Evans Analytical Group 30
31 Failed Heat Seal from medical packaging XPS flagged the higher O levels, but could not determine the root cause of the problem TOF-SIMS found clear evidence of hydroxyhydrocinnamate compounds on Bad surface Low levels of hydroxyhydrocinnamate found on Good surface Copyright 2013 Evans Analytical Group 31
32 Examining the sub-surface Copyright 2013 Evans Analytical Group 32
33 Examining the sub-surface What do we do when these techniques are too surface sensitive? - buried interfaces, extraneous surface contamination, etc. Copyright 2013 Evans Analytical Group 33
34 Basics of sputtering process 3 kv Ar + impinging Ni{001} Simulation courtesy of Barbara Garrison, PSU Chemistry Sputtered green and red atoms Bond breakage, atomic rearrangement in sub-surface Copyright 2013 Evans Analytical Group 34
35 Typical Depth Profile: Metallized PP Copyright 2013 Evans Analytical Group 35
36 c/s aimcal105.pro: AIMCAL research Aluminum Spectra 2013 Sep 10 Al mono 50.1 W µ ev e+003 max min Al2p/Point3: Al coated polymer/1 (Shft) Al2p Al Al 2 O Al 2 O Binding Energy (ev) Copyright 2013 Evans Analytical Group 36
37 What about profiling organics? PET After ~10 nm of sputtering Copyright 2013 Evans Analytical Group 37
38 What about profiling organics? Copyright 2013 Evans Analytical Group 38
39 Producing higher mass projectiles to increase sputter yield and decrease damage depth SF 5+, m = 127 Au 3+, m = 591 C 60+, m = 720 Cluster Ion Beams Most recent creation Ar 10,000+, m = 40,000!
40 Counts Erucamide Chemical Mapping-Surface 300 µm X 300 µm field of view 200 C 22 H 44 NO M/Z 40X Mass-to-charge Copyright 2013 Evans Analytical Group 40
41 Erucamide Chemical Mapping-Sub-Surface 300 µm X 300 µm field of view C 22 H 44 NO M/Z Mass-to-charge Copyright 2013 Evans Analytical Group 41
42 Erucamide Chemical Mapping-Different Depths Copyright 2013 Evans Analytical Group 42
43 Summary Surface Technique XPS/ESCA TOF-SIMS Typical applications Corona/plasma treatments Adhesion failures Additive blooming studies Reverse engineering of nm coatings Surface contaminants Defect analysis Adhesion failures Additive blooming Surface contaminants Signal detected photoelectrons sputtered ions Elements detected Li-U Molecular identification on surfaces H-U (including isotopes) and molecular species Organic info Yes, nearest neighbor bonding Yes, molecular info Quantitative Yes Qualitative Detection limits atom% ppm Sampling depth 1-10nm 1-2 monolayers Depth profiling Yes, limited info on organics Yes, for most organics Imaging/mapping Yes-limited Yes, elemental and molecular imaging Spatial resolution 10,000 nm (10 µm) 200 nm Copyright 2013 Evans Analytical Group 43
44 Questions Welcome Copyright 2013 Evans Analytical Group 44
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