Novel Method for High-Spatial-Resolution Chemical Analysis of Buried Polymer-Metal Interface: Atomic Force Microscopy-Infrared (AFM-IR) Spectroscopy with Low-Angle Microtomy
Restricted accessResearch articleFirst published online July, 2021
Novel Method for High-Spatial-Resolution Chemical Analysis of Buried Polymer-Metal Interface: Atomic Force Microscopy-Infrared (AFM-IR) Spectroscopy with Low-Angle Microtomy
There is a great need for the analysis of the chemical composition, structure, functional groups, and interactions at polymer-metal interfaces in terms of adhesion, corrosion, and insulation. Although atomic force microscopy-based infrared (AFM-IR) spectroscopy can provide chemical analysis with nanoscale spatial resolution, it generally requires to thin a sample to be placed on a substrate that has low absorption of infrared light and high thermal conductivity, which is often difficult for samples that contain hard materials such as metals. This study demonstrates that the combination of AFM-IR with low-angle microtomy (LAM) sample preparation can analyze buried polymer-metal interfaces with higher spatial resolution than that with the conventional sample preparation of a thick vertical cross-section. In the LAM of a polymer layer on a metal substrate, the polymer layer is tapered to be thin in the vicinity of the interface, and thus, sample thinning is not required. An interface between an epoxyacrylate layer and copper wire in a flexible printed circuit cable was measured using this method. A carboxylate interphase layer with a thickness of ∼130 nm was clearly visualized at the interface, and its spectrum was obtained without any signal contamination from the neighboring epoxyacrylate, which was difficult to achieve on a thick vertical cross-section. The combination of AFM-IR with LAM is a simple and useful method for high-spatial-resolution chemical analysis of buried polymer-metal interfaces.
J. Friedrich. Metal–Polymer Systems: Interface Design and Chemical Bonding. Weinheim, Germany: Wiley-VCH Verlag GmbH and Co. KGaA, 2018.
2.
PletincxS.FockaertL.L.I.MolJ.M.C., et al.“Probing the Formation and Degradation of Chemical Interactions from Model Molecule/Metal Oxide to Buried Polymer/Metal Oxide Interfaces”. NPJ Mater. Degrad. 2019, 3: 23-. doi: 10.1038/s41529-019-0085-2.
3.
J.F. Watts. “The Interfacial Chemistry of Adhesion: novel Routes to the Holy Grail?”. In: W. Possart, editor. Adhesion–Current Research and Application. Weinheim, Germany: Wiley-VCH Verlag GmbH and Co. KGaA, 2005. Chap. 1, Pp. 1–16. doi: 10.1002/3527607307.ch1.
4.
FockaertL.-L.I.Ganzinga-JurgD.VersluisJ., et al.“Studying Chemisorption at Metal−Polymer Interfaces by Complementary Use of Attenuated Total Reflection−Fourier Transform Infrared Spectroscopy (ATR-FT-IR) in the Kretschmann Geometry and Visible−Infrared Sum-Frequency Generation Spectroscopy (SFG)”. J. Phys. Chem. C. 2020, 124(13): 7127–7138. doi: 10.1021/acs.jpcc.9b10775.
5.
GrundmeierG.StratmannM.“Adhesion and De-Adhesion Mechanisms at Polymer/Metal Interfaces: Mechanistic Understanding Based on in Situ Studies of Buried Interfaces”. Annu. Rev. Mater. Res. 2005, 35: 571–615. doi: 10.1146/annurev.matsci.34.012703.105111.
6.
NagaiN.HironakaT.ImaiT., et al.“Study of Interaction Between Polyimide and Cu Under a High-Humidity Condition”. Appl. Surf. Sci. 2001, 171(1–2): 101–105. doi: 10.1016/S0169-4332(00)00539-0.
7.
OkumuraH.TakedaK.NagaiN.“Depth Profile Analysis of Structures in ArF Resists by 172nm VUV Curing and Dry Etching Process Using μ-FT-IR with Gradient Shaving Preparation”. J. Photopolym. Sci. Technol. 2004, 17(4): 535–540. doi: 10.2494/photopolymer.17.535.
8.
H. Seki. Characterization of the Chemical Bonding at the Interfaces of SiO2-Related Materials Using Microscopic Infrared Spectroscopy and Attenuated Total Reflection. [Ph.D. Thesis]. Sanda, Hyogo, Japan: School of Science and Technology, Kwansei Gakuin University, 2017.
9.
TonozukaY.ShohjiI.KoyamaS., et al.“Degradation Behaviors of Adhesion Strength Between Epoxy Resin and Copper Under Aging at High Temperature”. Procedia Eng. 2017, 184: 648–654. doi: 10.1016/j.proeng.2017.04.132.
10.
V.G. Gregoriou, S.E. Rodman, B.R. Nair, et al. “Studying the Viscoelastic Behavior of Liquid Crystalline Polyurethanes Using Static and Dynamic FT-IR Spectroscopy”. In: V.G. Gregoriou, M.S. Braiman, editors. Vibrational Spectroscopy of Biological and Polymeric Materials. Boca Raton, FL: CRC Press, 2006. Chap. 1, Pp. 1–34.
11.
L. Bokobza. “Some Applications of Vibrational Spectroscopy for the Analysis of Polymers and Polymer Composites”. Polymers. 2019. 11(7): 1159. doi: 10.3390/polym11071159.
12.
E. Wessel, C. Vogel, O. Kolomiets, et al. “FT-IR and NIR Spectroscopic Imaging: Principles, Practical Aspects and Applications in Material and Pharmaceutical Sciences”. In: R. Salzer, H. W. Siesler, editors. Infrared and Raman Spectroscopic Imaging. Weinheim, Germany: Wiley-VCH, 2009. Chap. 9, Pp. 312–318.
13.
NagaiN.OkumuraH.ImaiT., et al.“Depth Profile Analysis of the Photochemical Degradation of Polycarbonate by Infrared Spectroscopy”. Polym. Degrad. Stab. 2003, 81(3): 491–496. doi: 10.1016/S0141-3910(03)00135-6.
14.
McClureD.J.OuderkirkA.J.HillJ.B., et al.“Depth Profiling of Polymer Thin Films by Infrared Spectroscopy”. J. Vac. Sci. Technol. A. 1990, 8(3): 2295–2299. doi: 10.1116/1.576753.
15.
TatsumiD.YamauchiT.“Application of ATR–FT-IR Spectroscopy Combined with Sputter Etching for Depth Profiling of a Chemical Additive Within a Pulp Fiber”. J. Appl. Polym. Sci. 1998, 69(3): 461–468. doi: 10.1002/(SICI)1097-4628(19980718)69:3<461::AID-APP5>3.0.CO;2-E.
16.
HinderS.J.LoweC.MaxtedJ.T., et al.“The Morphology and Topography of Polymer Surfaces and Interfaces Exposed by Ultra-Low-Angle Microtomy”. J. Mater. Sci. 2005, 40(2): 285–293. doi: 10.1007/s10853-005-6081-7.
17.
S. Ochiai, H. Seki. “Infrared Microspectroscopic Measurements”. In: M. Tasumi, A. Sakamoto, editors. Introduction to Experimental Infrared Spectroscopy: Fundamentals and Practical Methods. West Sussex, UK: John Wiley and Sons, Ltd., 2015. Chap. 16, Pp. 223–240.
18.
OkumuraH.TakahagiT.NagaiN., et al.“Depth Profile Analysis of Polyimide Film Treated by Potassium Hydroxide”. J. Polym. Sci. Part B. 2003, 41(17): 2071–2078. doi: 10.1002/polb.10572.
19.
ItohH.“Depth Profiling Analysis of Organic Materials by Using ToF-SIMS and Gradient Shaving Preparation”. J. Surf. Anal. 2009, 15(3): 235–238. doi: 10.1384/jsa.15.235.
20.
ManN.OkumuraH.OizumiH., et al.“Depth Profile Analysis of Chemically Amplified Resist by Using TOF–SIMS with Gradient Shaving Preparations”. Appl. Surf. Sci. 2004, 231–232: 353–356. doi: 10.1016/j.apsusc.2004.03.093.
21.
DazziA.PraterC.“AFM-IR: Technology and Applications in Nanoscale Infrared Spectroscopy and Chemical Imaging”. Chem. Rev. 2017, 117(7): 5146–5173. doi: 10.1021/acs.chemrev.6b00448.
22.
DazziA.PraterC.B.HuQ., et al.“AFM–IR: Combining Atomic Force Microscopy and Infrared Spectroscopy for Nanoscale Chemical Characterization”. Appl. Spectrosc. 2012, 66(12): 1365–1384. doi: 10.1366/12-06804.
23.
DazziA.PrazeresR.GlotinF., et al.“Local Infrared Microspectroscopy with Subwavelength Spatial Resolution with an Atomic Force Microscope Tip Used as a Photothermal Sensor”. Opt. Lett. 2005, 30(18): 2388–2390. doi: 10.1364/OL.30.002388.
24.
A. Dazzi. “Photothermal Induced Resonance. Application to Infrared Spectromicroscopy”. In: S. Volz, editor. Thermal Nanosystems and Nanomaterials, Topics in Applied Physics. Berlin, Germany: Springer-Verlag, 2009. Pp. 469–503.
25.
CentroneA.“Infrared Imaging and Spectroscopy Beyond the Diffraction Limit”. Annu. Rev. Anal. Chem. 2015, 8(1): 101–126. doi: 10.1146/annurev-anchem-071114-040435.
26.
N. Baden, M. Yasuda, A. Yoshida, et al. “New Method for Chemical Characterization of Polymer Materials in Industrial Devices: AFM-IR with FIB Sample Preparation”. Paper presented at: 2015 IEEE 22nd International Symposium on the Physical and Failure Analysis of Integrated Circuits. Hsinchu, Taiwan; Jun 29–Jul 2, 2015.
27.
MorschS.LiuY.MalaninM., et al.“Exploring Whether a Buried Nanoscale Interphase Exists within Epoxy–Amine Coatings: Implications for Adhesion, Fracture Toughness, and Corrosion Resistance”. ACS Appl. Nano Mater. 2019, 2(4): 2494–2502. doi: 10.1021/acsanm.9b00387.
28.
SangJ.HiraharaH.AisawaS., et al.“Direct Bonding of Polypropylene to Aluminum Using Molecular Connection and the Interface Nanoscale Properties”. ACS Appl. Polym. Mater. 2019, 1(9): 2450–2459. doi: 10.1021/acsapm.9b00568.
29.
CavezzaF.PletincxS.RevillaR.I., et al.“Probing the Metal Oxide/Polymer Molecular Hybrid Interfaces with Nanoscale Resolution Using AFM-IR”. J. Phys. Chem. C. 2019, 123(43): 26178–26184. doi: 10.1021/acs.jpcc.9b04522.
30.
KhorasaniM.G.Z.ElertA.-M.HodoroabaV.-D., et al.“Short- and Long-Range Mechanical and Chemical Interphases Caused by Interaction of Boehmite (γ-AlOOH) with Anhydride-Cured Epoxy Resins”. Nanomaterials. 2019, 9(6): 853–872. doi: 10.3390/nano9060853.
31.
S. Morsch, S. Lyon, S. Gibbon. “Spectroscopic Insights into Adhesion Failure at the Buried Epoxy–Metal Interphase Using AFM-IR”. Surf. Interface Anal. 2020. 52(12): 1139--1144. doi:10.1002/sia.6795.
32.
KurouskiD.DazziA.ZenobiR., et al.“Infrared and Raman Chemical Imaging and Spectroscopy at the Nanoscale”. Chem. Soc. Rev. 2020, 49(11): 3315–3347. doi: 10.1039/c8cs00916c.
33.
QuaroniL.“Imaging and Spectroscopy of Domains of the Cellular Membrane by Photothermal-Induced Resonance”. Analyst. 2020, 145(17): 5940–5950. doi: 10.1039/D0AN00696C.
34.
LahiriB.HollandG.CentroneA.“Chemical Imaging Beyond the Diffraction Limit: Experimental Validation of the PTIR Technique”. Small. 2013, 9(3): 439–445. doi: 10.1002/smll.201200788.
35.
WangC.-T.JiangB.ZhouY.-W., et al.“Exploiting the Surface-Enhanced IR Absorption Effect in the Photothermally Induced Resonance AFM-IR Technique Toward Nanoscale Chemical Analysis”. Anal. Chem. 2019, 91(16): 10541–10548. doi: 10.1021/acs.analchem.9b01554.
36.
RamerG.AksyukV.A.CentroneA.“Quantitative Chemical Analysis at the Nanoscale Using the Photothermal Induced Resonance Technique”. Anal. Chem. 2017, 89(24): 13524–13531. doi: 10.1021/acs.analchem.7b03878.
37.
M. Belkin, F. Lu, V.V. Yakolev, et al. High Frequency Deflection Measurement of IR Absorption. US Patent US8869602B2. Filed 2011. Issued 2014.
38.
MorozovskaA.N.EliseevE.A.BorodinovN., et al.“Photothermoelastic Contrast in Nanoscale Infrared Spectroscopy”. Appl. Phys. Lett. 2018, 112(3): 033105-doi: 10.1063/1.4985584.
39.
WaeytensJ.DoneuxT.NapolitanoS.“Evaluating Mechanical Properties of Polymers at the Nanoscale Level via Atomic Force Microscopy−Infrared Spectroscopy”. ACS Appl. Polym. Mater. 2019, 1(1): 3−7-doi: 10.1021/acsapm.8b00243.
40.
FeltsJ.R.ChoH.YuM.-F., et al.“Atomic Force Microscope Infrared Spectroscopy on 15 nm Scale Polymer Nanostructures”. Rev. Sci. Instrum. 2013, 84(2): 023709-doi: 10.1063/1.4793229.
41.
LuF.JinM.BelkinM.A.“Tip-Enhanced Infrared Nanospectroscopy via Molecular Expansion Force Detection”. Nat. Photonics. 2014, 8(4): 307–312. doi: 10.1038/nphoton.2013.373.
42.
LuF.BelkinM.A.“Infrared Absorption Nano-Spectroscopy Using Sample Photoexpansion Induced by Tunable Quantum Cascade Lasers”. Opt. Express. 2011, 19(21): 19942–19947. doi: 10.1364/OE.19.019942.
43.
QuaroniL.“Understanding and Controlling Spatial Resolution, Sensitivity, and Surface Selectivity in Resonant-Mode Photothermal-Induced Resonance Spectroscopy”. Anal. Chem. 2020, 92(5): 3544–3554. doi: 10.1021/acs.analchem.9b03468.
44.
TangF.BaoP.SuZ.“Analysis of Nanodomain Composition in High-Impact Polypropylene by Atomic Force Microscopy-Infrared”. Anal. Chem. 2016, 88(9): 4926–4930. doi: 10.1021/acs.analchem.6b00798.
45.
MathurinJ.PancaniE.Deniset-BesseauA., et al.“How to Unravel the Chemical Structure and Component Localization of Individual Drug-Loaded Polymeric Nanoparticles by Using Tapping AFM-IR”. Analyst. 2018, 143(24): 5940–5949. doi: 10.1039/C8AN01239C.
46.
PiergiesN.DazziA.Deniset-BesseauA., et al.“Nanoscale Image of the Drug/Metal Mono-Layer Interaction: Tapping AFM-IR Investigations”. Nano Res. 2020, 13(4): 1020–1028. doi: 10.1007/s12274-020-2738-4.
47.
ZhaoW.JohnsonC.M.“Perspective–Nano Infrared Microscopy: Obtaining Chemical Information on the Nanoscale in Corrosion Studies”. J. Electrochem. Soc. 2019, 166(11): C3456–C3460. doi: 10.1149/2.0531911jes.
48.
P. McLeod. A Review of Flexible Circuit Technology and Its Applications. Loughborough, UK: Prime Faraday Partnership, 2003.
49.
NothdurftP.RiessG.KernW.“Copper/Epoxy Joints in Printed Circuit Boards: Manufacturing and Interfacial Failure Mechanisms”. Materials. 2019, 12(3): 550-doi:10.3390/ma12030550. doi: 10.3390/ma12030550.
50.
LeeH.-Y.QuJ.“Microstructure, Adhesion Strength, and Failure Path at a Polymer/Roughened Metal Interface”. J. Adhes. Sci. Technol. 2003, 17(2): 195–215. doi: 10.1163/156856103762302005.
51.
LeeH.-N.HanY.LeeJ., et al.“Aging Effect on Adhesion Strength between Electroless Copper and Polyimide Films”. Mater. Trans. 2013, 54(6): 1040–1044. doi: 10.2320/matertrans.M2013044.
52.
HoP.S.HahnP.O.BarthaJ.W., et al.“Chemical Bonding and Reaction at Metal/Polymer interfaces”. J. Vac. Sci. Technol. A. 1985, 3(3): 739–745. doi: 10.1116/1.573298.
53.
DengD.QiT.ChengY., et al.“Copper Carboxylate with Different Carbon Chain Lengths as Metal–Organic Decomposition Ink”. J. Mater. Sci.: Mater. Electron. 2014, 25(1): 390–397. doi: 10.1007/s10854-013-1599-y.
54.
ŽerjavG.MiloševI.“Carboxylic Acids as Corrosion Inhibitors for Cu, Zn, and Brasses in Simulated Urban Rain”. Int. J. Electrochem. Sci. 2014, 9(5): 2696–2715.
55.
EliaA.De WaelK.DowsettM., et al.“Electrochemical Deposition of a Copper Carboxylate Layer on Copper as Potential Corrosion Inhibitor”. J. Solid State Electrochem. 2012, 16(1): 143–148. doi: 10.1007/s10008-010-1283-6.
56.
J.V. Koleske. “Photochemistry of Cycloaliphatic Epoxides and Epoxy Acrylates”. In: M.L. Minges, editor. Electronic Materials Handbook: Packaging. Boca Raton, FL: CRC Press, 1989. Vol. 1, Pp. 854–858.
57.
M.L. Jackson. Investigation of Adhesive and Electrical Performance of Waterborne Epoxies for Interlayer Dielectric Material. [Ph.D. Dissertation]. Blacksburg, VA, US: Materials Engineering Science Department, Virginia Polytechnic Institute and State University, 1999.
58.
EscaigB.“Binding Metals to Polymers. A Short Review of Basic Physical Mechanisms”. J. Phys. IV. 1993, 3(C7): 753–761. doi: 10.1051/jp4:19937120.
59.
WanH.SongD.LiX., et al.“Failure Mechanisms of the Coating/Metal Interface in Waterborne Coatings: The Effect of Bonding”. Materials. 2017, 10(4): 397-doi: 10.3390/ma10040397.
60.
TheryS.JacquetD.MantelM.“A Study of Chemical Interactions at the Stainless Steel/Polymer Interface by Infrared Spectroscopy. Part 2: Mechanical Properties and Study of the Interphase”. J. Adhes. 1996, 56(1–4): 15–25. doi: 10.1080/00218469608010496.
61.
W.M. Moreau. Semiconductor Lithography Principles, Practices, and Materials. New York, NY, US: Plenum Press, 1988. Chap. 2, Pp. 29–80.
62.
SemotoT.TsujiY.YoshizawaK.“Molecular Understanding of the Adhesive Force between a Metal Oxide Surface and an Epoxy Resin”. J. Phys. Chem. C. 2011, 115(23): 11701–11708. doi: 10.1021/jp202785b.
63.
SemotoT.TsujiY.YoshizawaK.“Molecular Understanding of the Adhesive Force between a Metal Oxide Surface and an Epoxy Resin: Effects of Surface Water”. Bull. Chem. Soc. Jpn. 2012, 85(6): 672–678. doi: 10.1246/bcsj.20120028.
64.
ZhangY.X.HuangM.LiF., et al.“Controlled Synthesis of Hierarchical CuO Nanostructures for Electrochemical Capacitor Electrodes”. Int. J. Electrochem. Sci. 2013, 8(6): 8645–8661.
65.
P.A. Schroeder. “Infrared Spectroscopy in Clay Science”. In: A. Rule, S. Guggenheim, editors. CMS Workshop Lectures, Vol. 11: Teaching Clay Science. Aurora, CO: The Clay Mineral Society, 2002. Vol. 11, Pp. 181–206. doi: 10.1346/CMS-WLS-11.11.
66.
D.L. Allara, C.W. White. “Microscopic Mechanisms of Oxidative Degradation and Its Inhibition at a Copper–Polyethylene Interface”. In: D.L. Allara, W.L. Hawkins, editors. Stabilization and Degradation of Polymers. Washington, DC: American Chemical Society, 1978. Vol. 169, Pp. 273–292. doi: 10.1021/ba-1978-0169.ch023.
67.
AllaraD.L.WhiteC.W.MeekR.L., et al.“Mechanism of Oxidation at a Copper–Polyethylene Interface. II. Penetration of Copper Ions in the Polyethylene Matrix”. J. Polym. Sci., Polym. Chem. Ed. 1976, 14(1): 93–104. doi: 10.1002/pol.1976.170140109.
68.
JellinekH.H.G.WeiY.C.“Diffusion of Cu2+ Catalysts from Cu–Metal Polymer or Cu–Oxide/Polymer Interfaces into Isotactic Polypropylene”. J. Polym. Sci. 1986, 24(3): 503–510. doi: 10.1002/polb.1986.090240303.
69.
D.L. Allara. “The Study of Thin Polymer Films on Metal Surfaces using Reflection–Absorption Spectroscopy: Oxidation of Poly(1-Butene) on Gold and Copper”. In: L.-H. Lee, editor. Characterization of Metal and Polymer Surfaces, Vol. 2: Polymer Surfaces. New York, NY: Academic Press, Inc., 1977. Vol. 2, Pp. 193–206.
70.
WangL.WangH.WagnerM., et al.“Nanoscale Simultaneous Chemical and Mechanical Imaging via Peak Force Infrared Microscopy”. Sci. Adv. 2017, 3(6): e1700255-doi: 10.1126/sciadv.1700255.
Supplementary Material
Please find the following supplemental material available below.
For Open Access articles published under a Creative Commons License, all supplemental material carries the same license as the article it is associated with.
For non-Open Access articles published, all supplemental material carries a non-exclusive license, and permission requests for re-use of supplemental material or any part of supplemental material shall be sent directly to the copyright owner as specified in the copyright notice associated with the article.
