Effects of Residual Solvent Molecules Facilitating the Infiltration Synthesis of ZnO in a Nonreactive Polymer

Ye, Xinyi; Kestell, John; Kisslinger, Kim; Liu, Mingzhao; Grubbs, Robert B.; Boscoboinik, J. Anibal; Nam, Chang-Yong

doi:10.1021/acs.chemmater.7b01222

Title: Effects of Residual Solvent Molecules Facilitating the Infiltration Synthesis of ZnO in a Nonreactive Polymer

Journal Article · Thu May 04 00:00:00 EDT 2017 · Chemistry of Materials

DOI:https://doi.org/10.1021/acs.chemmater.7b01222· OSTI ID:1376164

Ye, Xinyi ^[1]; Kestell, John ^[1]; Kisslinger, Kim ^[1]; Liu, Mingzhao ^[1]; Grubbs, Robert B. ^[2]; Boscoboinik, J. Anibal ^[1];

^[1]

Brookhaven National Lab. (BNL), Upton, NY (United States). Center for Functional Nanomaterials (CFN)
Stony Brook Univ., NY (United States). Dept. of Chemistry

Infiltration synthesis, the atomic-layer-deposition-based organic–inorganic material hybridization technique that enables unique hybrid composites with improved material properties and inorganic nanostructures replicated from polymer templates, is shown to be driven by the binding reaction between reactive chemical groups of polymers and perfusing vapor-phase material precursors. Here in this paper, we discover that residual solvent molecules from polymer processing can react with infiltrating material precursors to enable the infiltration synthesis of metal oxides in a nonreactive polymer. The systematic study, which combines in situ quartz crystal microgravimetry, polarization-modulated infrared reflection–absorption spectroscopy, X-ray photoelectron spectroscopy, and transmission electron microscopy, shows that the ZnO infiltration synthesis in nominally nonreactive SU-8 polymer is mediated by residual processing solvent cyclopentanone, a cyclic ketone whose Lewis-basic terminal carbonyl group can react with the infiltrating Lewis-acidic Zn precursor diethylzinc (DEZ). In addition, we find favorable roles of residual epoxy rings in the SU-8 film in further assisting the infiltration synthesis of ZnO. Lastly, the discovered rationale not only improves the understanding of infiltration synthesis mechanism, but also potentially expands its application to more diverse polymer systems for the generation of unique functional organic–inorganic hybrids and inorganic nanostructures.

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Research Organization:: Brookhaven National Laboratory (BNL), Upton, NY (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: SC0012704

OSTI ID:: 1376164

Report Number(s):: BNL-114135-2017-JA

Journal Information:: Chemistry of Materials, Vol. 29, Issue 10; ISSN 0897-4756

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 23 works

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References (56)

Insight on the SU-8 resist as passivation layer for transparent Ga2O3–In2O3–ZnO thin-film transistors Olziersky, Antonis; Barquinha, Pedro; Vilà, Anna Journal of Applied Physics, Vol. 108, Issue 6 https://doi.org/10.1063/1.3477192	journal	September 2010
Systematic study of trimethyl aluminum infiltration in polyethylene terephthalate and its effect on the mechanical properties of polyethylene terephthalate fibers Padbury, Richard P.; Jur, Jesse S. Journal of Vacuum Science & Technology A: Vacuum, Surfaces, and Films, Vol. 33, Issue 1 https://doi.org/10.1116/1.4898435	journal	January 2015
Sequential Vapor Infiltration of Metal Oxides into Sacrificial Polyester Fibers: Shape Replication and Controlled Porosity of Microporous/Mesoporous Oxide Monoliths Gong, Bo; Peng, Qing; Jur, Jesse S. Chemistry of Materials, Vol. 23, Issue 15 https://doi.org/10.1021/cm200694w	journal	August 2011
Temperature-dependent reaction between trimethylaluminum and poly(methyl methacrylate) during sequential vapor infiltration: experimental and ab initio analysis Dandley, Erinn C.; Needham, Craig D.; Williams, Philip S. J. Mater. Chem. C, Vol. 2, Issue 44 https://doi.org/10.1039/C4TC01293C	journal	January 2014
Strategies for Inorganic Incorporation using Neat Block Copolymer Thin Films for Etch Mask Function and Nanotechnological Application Cummins, Cian; Ghoshal, Tandra; Holmes, Justin D. Advanced Materials, Vol. 28, Issue 27 https://doi.org/10.1002/adma.201503432	journal	January 2016
General Introduction To Plastics Analysis Lobo, Hubert; Bonilla, Jose Handbook of Plastics Analysis https://doi.org/10.1201/9780203911983.ch1	book	June 2003
Emerging trends in metal-containing block copolymers: synthesis, self-assembly, and nanomanufacturing applications Ramanathan, Muruganathan; Tseng, Yu-Chih; Ariga, Katsuhiko Journal of Materials Chemistry C, Vol. 1, Issue 11 https://doi.org/10.1039/c3tc00930k	journal	January 2013
Sequential Infiltration Synthesis of Doped Polymer Films with Tunable Electrical Properties for Efficient Triboelectric Nanogenerator Development Yu, Yanhao; Li, Zhaodong; Wang, Yunming Advanced Materials, Vol. 27, Issue 33 https://doi.org/10.1002/adma.201502546	journal	July 2015
In Situ Raman Spectroscopic Study of Al-Infiltrated Spider Dragline Silk under Tensile Deformation Lee, Seung-Mo; Pippel, Eckhard; Moutanabbir, Oussama ACS Applied Materials & Interfaces, Vol. 6, Issue 19 https://doi.org/10.1021/am5041797	journal	September 2014
Tuning the Tensile Strength of Cellulose through Vapor-Phase Metalation Gregorczyk, Keith E.; Pickup, David F.; Sanz, Miren Garcia Chemistry of Materials, Vol. 27, Issue 1 https://doi.org/10.1021/cm503724c	journal	December 2014
Mechanism of Metal Oxide Deposition from Atomic Layer Deposition inside Nonreactive Polymer Matrices: Effects of Polymer Crystallinity and Temperature Obuchovsky, Stas; Frankenstein, Hadar; Vinokur, Jane Chemistry of Materials, Vol. 28, Issue 8 https://doi.org/10.1021/acs.chemmater.6b00159	journal	April 2016
A Route to Nanoscopic Materials via Sequential Infiltration Synthesis on Block Copolymer Templates Peng, Qing; Tseng, Yu-Chih; Darling, Seth B. ACS Nano, Vol. 5, Issue 6, p. 4600-4606 https://doi.org/10.1021/nn2003234	journal	May 2011
Atmospheric pressure synthesis of photoluminescent hybrid materials by sequential organometallic vapor infiltration into polyethylene terephthalate fibers Akyildiz, Halil I.; Mousa, Moataz Bellah M.; Jur, Jesse S. Journal of Applied Physics, Vol. 117, Issue 4 https://doi.org/10.1063/1.4906406	journal	January 2015
Quantitative in situ infrared analysis of reactions between trimethylaluminum and polymers during Al2O3 atomic layer deposition Gong, Bo; Parsons, Gregory N. Journal of Materials Chemistry, Vol. 22, Issue 31 https://doi.org/10.1039/c2jm32343e	journal	January 2012
Thermal UV treatment on SU-8 polymer for integrated optics Wang, Xi-Bin; Sun, Jian; Chen, Chang-Ming Optical Materials Express, Vol. 4, Issue 3 https://doi.org/10.1364/OME.4.000509	journal	January 2014
Electrical and structural properties of ZnO synthesized via infiltration of lithographically defined polymer templates Nam, Chang-Yong; Stein, Aaron; Kisslinger, Kim Applied Physics Letters, Vol. 107, Issue 20 https://doi.org/10.1063/1.4935793	journal	November 2015
Bovine serum albumin adsorption on nano-rough platinum surfaces studied by QCM-D Dolatshahi-Pirouz, A.; Rechendorff, K.; Hovgaard, M. B. Colloids and Surfaces B: Biointerfaces, Vol. 66, Issue 1 https://doi.org/10.1016/j.colsurfb.2008.05.010	journal	October 2008
Direct fabrication of high aspect-ratio metal oxide nanopatterns via sequential infiltration synthesis in lithographically defined SU-8 templates Nam, Chang-Yong; Stein, Aaron; Kisslinger, Kim Journal of Vacuum Science & Technology B, Nanotechnology and Microelectronics: Materials, Processing, Measurement, and Phenomena, Vol. 33, Issue 6 https://doi.org/10.1116/1.4929508	journal	November 2015
Greatly Increased Toughness of Infiltrated Spider Silk Lee, S. -M.; Pippel, E.; Gosele, U. Science, Vol. 324, Issue 5926 https://doi.org/10.1126/science.1168162	journal	April 2009
Stereoselective organic reactions: catalysts for carbonyl addition processes Evans, D. Science, Vol. 240, Issue 4851 https://doi.org/10.1126/science.3358127	journal	April 1988
Lewis acid-promoted selective rearrangement of trisubstituted epoxides to aldehydes or ketones Maruoka, Keiji; Murase, Noriaki; Bureau, Ronan Tetrahedron, Vol. 50, Issue 12 https://doi.org/10.1016/S0040-4020(01)90389-8	journal	March 1994
SU8 resist for low-cost X-ray patterning of high-resolution, high-aspect-ratio MEMS Khan Malek, Chantal G. Microelectronics Journal, Vol. 33, Issue 1-2 https://doi.org/10.1016/S0026-2692(01)00109-4	journal	January 2002
Kinetics for the Sequential Infiltration Synthesis of Alumina in Poly(methyl methacrylate): An Infrared Spectroscopic Study Biswas, Mahua; Libera, Joseph A.; Darling, Seth B. The Journal of Physical Chemistry C, Vol. 119, Issue 26 https://doi.org/10.1021/jp511939j	journal	January 2015
Influence of processing conditions on the thermal and mechanical properties of SU8 negative photoresist coatings Feng, Ru; Farris, Richard J. Journal of Micromechanics and Microengineering, Vol. 13, Issue 1 https://doi.org/10.1088/0960-1317/13/1/312	journal	December 2002
A greener approach for the synthesis of 1-N-methyl-(spiro[2.3′]oxindolespiro[3.2″]/spiro[2.3′]indan-1,3-dionespiro[2.2″])cyclopentanone-4-aryl pyrrolidines Sridhar, Gowri; Gunasundari, T.; Raghunathan, R. Tetrahedron Letters, Vol. 48, Issue 2 https://doi.org/10.1016/j.tetlet.2006.11.002	journal	January 2007
Structural anisotropy in friction-deposited layers of polystyrene Elzein, Tamara; Kreim, Virginie; Ghorbal, Achraf Journal of Polymer Science Part B: Polymer Physics, Vol. 44, Issue 22 https://doi.org/10.1002/polb.20963	journal	January 2006
Enhanced Block Copolymer Lithography Using Sequential Infiltration Synthesis Tseng, Yu-Chih; Peng, Qing; Ocola, Leonidas E. The Journal of Physical Chemistry C, Vol. 115, Issue 36, p. 17725-17729 https://doi.org/10.1021/jp205532e	journal	July 2011
Chemical modification of polymer surfaces for advanced triboelectric nanogenerator development Yu, Yanhao; Wang, Xudong Extreme Mechanics Letters, Vol. 9 https://doi.org/10.1016/j.eml.2016.02.019	journal	December 2016
Advanced oil sorbents using sequential infiltration synthesis Barry, Edward; Mane, Anil U.; Libera, Joseph A. Journal of Materials Chemistry A, Vol. 5, Issue 6 https://doi.org/10.1039/C6TA09014A	journal	January 2017
Temperature and Exposure Dependence of Hybrid Organic–Inorganic Layer Formation by Sequential Vapor Infiltration into Polymer Fibers Akyildiz, Halil I.; Padbury, Richard P.; Parsons, Gregory N. Langmuir, Vol. 28, Issue 44 https://doi.org/10.1021/la302991c	journal	October 2012
Fast Fourier Transform IR Characterization of Epoxy GY Systems Crosslinked with Aliphatic and Cycloaliphatic EH Polyamine Adducts Nikolic, Goran; Zlatkovic, Sasa; Cakic, Milorad Sensors, Vol. 10, Issue 1 https://doi.org/10.3390/s100100684	journal	January 2010
New Insight into the Mechanism of Sequential Infiltration Synthesis from Infrared Spectroscopy Biswas, Mahua; Libera, Joseph A.; Darling, Seth B. Chemistry of Materials, Vol. 26, Issue 21 https://doi.org/10.1021/cm502427q	journal	October 2014
The influence of hard-baking temperature applied for SU8 sensor layer on the sensitivity of capacitive chemical sensor Klanjšek Gunde, Marta; Hauptman, Nina; Maček, Marijan Applied Physics A, Vol. 95, Issue 3 https://doi.org/10.1007/s00339-008-4966-4	journal	November 2008
New Insights into Sequential Infiltration Synthesis Elam, J. W.; Biswas, M.; Darling, S. ECS Transactions, Vol. 69, Issue 7 https://doi.org/10.1149/06907.0147ecst	journal	September 2015
Photoluminescence of sequential infiltration synthesized ZnO nanostructures Ocola, Leonidas E.; Gosztola, David J.; Yanguas-Gil, Angel SPIE OPTO, SPIE Proceedings https://doi.org/10.1117/12.2209422	conference	February 2016
Chemically Enhancing Block Copolymers for Block-Selective Synthesis of Self-Assembled Metal Oxide Nanostructures Kamcev, Jovan; Germack, David S.; Nykypanchuk, Dmytro ACS Nano, Vol. 7, Issue 1 https://doi.org/10.1021/nn304122b	journal	December 2012
Photoluminescence Mechanism and Photocatalytic Activity of Organic–Inorganic Hybrid Materials Formed by Sequential Vapor Infiltration Akyildiz, Halil I.; Stano, Kelly L.; Roberts, Adam T. Langmuir, Vol. 32, Issue 17 https://doi.org/10.1021/acs.langmuir.6b00285	journal	April 2016
Investigating Sequential Vapor Infiltration Synthesis on Block-Copolymer-Templated Titania Nanoarrays Ishchenko, Olga M.; Krishnamoorthy, Sivashankar; Valle, Nathalie The Journal of Physical Chemistry C, Vol. 120, Issue 13 https://doi.org/10.1021/acs.jpcc.5b10415	journal	March 2016
Molecular Layer Deposition of Hybrid Organic-Inorganic Polymer Films using Diethylzinc and Ethylene Glycol Yoon, Byunghoon; O'Patchen, Jennifer L.; Seghete, Dragos Chemical Vapor Deposition, Vol. 15, Issue 4-6 https://doi.org/10.1002/cvde.200806756	journal	June 2009
Organometallic exposure dependence on organic–inorganic hybrid material formation in polyethylene terephthalate and polyamide 6 polymer fibers Akyildiz, Halil I.; Jur, Jesse S. Journal of Vacuum Science & Technology A: Vacuum, Surfaces, and Films, Vol. 33, Issue 2 https://doi.org/10.1116/1.4907563	journal	March 2015
Polarization Modulation FT-IR Spectroscopy of Surfaces and Ultra-Thin Films: Experimental Procedure and Quantitative Analysis Buffeteau, T.; Desbat, B.; Turlet, J. M. Applied Spectroscopy, Vol. 45, Issue 3 https://doi.org/10.1366/0003702914337308	journal	March 1991
Processing of thin SU-8 films Keller, Stephan; Blagoi, Gabriela; Lillemose, Michael Journal of Micromechanics and Microengineering, Vol. 18, Issue 12 https://doi.org/10.1088/0960-1317/18/12/125020	journal	November 2008
Asymmetric Addition of Alkylzinc Reagents to Cyclic α,β-Unsaturated Ketones and a Tandem Enantioselective Addition/Diastereoselective Epoxidation with Dioxygen Jeon, Sang-Jin; Walsh, Patrick J. Journal of the American Chemical Society, Vol. 125, Issue 32 https://doi.org/10.1021/ja036302t	journal	July 2003
Thermal analysis of γ-butyrolactone+1 butyl-3-methyl-imidazolium ionic liquids mixtures Chagnes, A.; Allouchi, H.; Carré, B. Solid State Ionics, Vol. 176, Issue 15-16 https://doi.org/10.1016/j.ssi.2005.03.005	journal	May 2005
Reactions during Atomic Layer Deposition on Polymer Films and Fibers Parsons, Gregory N.; Spagnola, Joseph; Gong, Bo ECS Meeting Abstracts, Vol. MA2010-02, Issue 20 https://doi.org/10.1149/MA2010-02/20/1411	journal	July 2010
Atomic Layer Deposition: An Overview George, Steven M. Chemical Reviews, Vol. 110, Issue 1, p. 111-131 https://doi.org/10.1021/cr900056b	journal	January 2010
Study of atomic layer epitaxy of zinc oxide by in-situ quartz crystal microgravimetry Yousfi, El Bekkaye; Fouache, Jacques; Lincot, Daniel Applied Surface Science, Vol. 153, Issue 4, p. 223-234 https://doi.org/10.1016/S0169-4332(99)00330-X	journal	January 2000
Infrared Studies of Ketones: Parameters Affecting the Induced Carbonyl Stretching Vibration by Solute/Solvent Interaction Nyquist, Richard A. Applied Spectroscopy, Vol. 44, Issue 3 https://doi.org/10.1366/0003702904086218	journal	March 1990
Cure Kinetics of Epoxy Nanocomposites Affected by MWCNTs Functionalization: A Review Saeb, Mohammad Reza; Bakhshandeh, Ehsan; Khonakdar, Hossein Ali The Scientific World Journal, Vol. 2013 https://doi.org/10.1155/2013/703708	journal	January 2013
Thermal Stability of Gold Nanoparticles Embedded within Metal Oxide Frameworks Fabricated by Hybrid Modifications onto Sacrificial Textile Templates Padbury, Richard P.; Halbur, Jonathan C.; Krommenhoek, Peter J. Langmuir, Vol. 31, Issue 3 https://doi.org/10.1021/la504094g	journal	July 2014
Infrared spectroscopy of ferrihydrite: evidence for the presence of structural hydroxyl groups Russell, J. D. Clay Minerals, Vol. 14, Issue 2 https://doi.org/10.1180/claymin.1979.014.2.03	journal	June 1979
Characterization by Fourier transform infrared spectroscopy of hydroxyapatite co-doped with zinc and fluoride Uysal, I.; Severcan, F.; Evis, Z. Ceramics International, Vol. 39, Issue 7 https://doi.org/10.1016/j.ceramint.2013.03.029	journal	September 2013
Rapid Prototyping of Microstructures with Bell-Shaped Cross-Sections and Its Application to Deformation-Based Microfluidic Valves Futai, N.; Gu, W.; Takayama, S. Advanced Materials, Vol. 16, Issue 15 https://doi.org/10.1002/adma.200400595	journal	August 2004
Catalysis of the epoxy-carboxyl reaction Blank, Werner J.; He, Z. A.; Picci, Marie Journal of Coatings Technology, Vol. 74, Issue 3 https://doi.org/10.1007/BF02720158	journal	March 2002
Sequential Infiltration Synthesis for the Design of Low Refractive Index Surface Coatings with Controllable Thickness Berman, Diana; Guha, Supratik; Lee, Byeongdu ACS Nano, Vol. 11, Issue 3 https://doi.org/10.1021/acsnano.6b08361	journal	February 2017
Nanoscopic Patterned Materials with Tunable Dimensions via Atomic Layer Deposition on Block Copolymers Peng, Qing; Tseng, Yu-Chih; Darling, Seth B. Advanced Materials, Vol. 22, Issue 45, p. 5129-5133 https://doi.org/10.1002/adma.201002465	journal	September 2010

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