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Introducing and Controlling Water Vapor in Closed-Cell In Situ Electron Microscopy Gas Reactions

Published online by Cambridge University Press:  11 March 2020

Kinga A. Unocic ,
Franklin S. Walden ,
Nelson L. Marthe ,
Abhaya K. Datye ,
Wilbur C. Bigelow  and
Lawrence F. Allard
Kinga A. Unocic*
Affiliation:
Center for Nanophase Materials Sciences Division, Oak Ridge National Laboratory, 1 Bethel Valley Rd, Oak Ridge, TN37831, USA
Franklin S. Walden
Affiliation:
Protochips Inc., 3800 Gateway Centre Blvd, Suite 306, Morrisville, NC27560, USA
Nelson L. Marthe
Affiliation:
Protochips Inc., 3800 Gateway Centre Blvd, Suite 306, Morrisville, NC27560, USA
Abhaya K. Datye
Affiliation:
Chemical and Biological Engineering, University of New Mexico, MSC01 1120, Albuquerque, NM87131, USA
Wilbur C. Bigelow
Affiliation:
Department of Materials Science and Engineering, University of Michigan, Dow Bldg., Hayward Ave., Ann Arbor, MI48109, USA
Lawrence F. Allard
Affiliation:
Center for Nanophase Materials Sciences Division, Oak Ridge National Laboratory, 1 Bethel Valley Rd, Oak Ridge, TN37831, USA
*
*Author for correspondence: Kinga A. Unocic, E-mail: unocicka@ornl.gov
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Abstract

Protocols for conducting in situ transmission electron microscopy (TEM) reactions using an environmental TEM with dry gases have been well established. However, many important reactions that are relevant to catalysis or high-temperature oxidation occur at atmospheric pressure and are influenced by the presence of water vapor. These experiments necessitate using a closed-cell gas reaction TEM holder. We have developed protocols for introducing and controlling water vapor concentrations in experimental gases from 2% at a full atmosphere to 100% at ~17 Torr, while measuring the gas composition using a residual gas analyzer (RGA) on the return side of the in situ gas reactor holder. Initially, as a model system, cube-shaped MgO crystals were used to help develop the protocols for handling the water vapor injection process and confirming that we could successfully inject water vapor into the gas cell. The interaction of water vapor with MgO triggered surface morphological and chemical changes as a result of the formation of Mg(OH)2, later validated with mass spectra obtained with our RGA system with and without water vapor. Integrating an RGA with an in situ scanning/TEM closed-cell gas reaction system can thus provide critical measurements correlating gas composition with dynamic surface restructuring of materials during reactions.

Keywords

closed-cell gas reaction systemin situ STEMMgOresidual gas analyzerwater vapor
Type
Software and Instrumentation
Information
Microscopy and Microanalysis , Volume 26 , Issue 2 , April 2020 , pp. 229 - 239
Copyright
Copyright © Microscopy Society of America 2020

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References

Allard, L, Overbury, SH, Katz, MB, Bigelow, WC, Nackashi, D & Damiano, J (2012 b). Innovative closed-cell reactor permits in situ heating and gas reactions with atomic resolution at atmospheric pressure. Microsc Microanal 18, 1118–1119.CrossRefGoogle Scholar
Allard, LF, Bigelow, WC, Wu, Z, Overbury, SH, Unocic, KA, Chi, M, Carpenter, WB, Walden, FS, Thomas, RL, Gardiner, DS, Jacobs, BW, Nackashi, DP & Damiano, J (2015). Computer-controlled in situ gas reactions via a MEMS-based closed-cell system. Microsc Microanal 21, 97–98.CrossRefGoogle Scholar
Allard, LF, Bigelow, WC, Zhang, S, Pan, X, Wu, Z, Overbury, SH, Carpenter, WB, Walden, FS, Thomas, RL, Gardiner, DS, Jacobs, BW, Nackashi, DP & Damiano, J (2014). Controlled in situ gas reaction studies of catalysts at high temperature and pressure with atomic resolution. Microsc Microanal 20, 1572–1573.CrossRefGoogle Scholar
Allard, LF, Overbury, SH, Bigelow, WC, Katz, MB, Nackashi, DP & Damiano, J (2012 a). Novel MEMS-based gas-cell/heating specimen holder provides advanced imaging capabilities for in situ reaction studies. Microsc Microanal 18, 656–666.CrossRefGoogle ScholarPubMed
Anderson, PJ & Morgan, PL (1964). Effects of water vapour on sintering of MgO. Trans Faraday Soc 60, 930–937.CrossRefGoogle Scholar
Burke, MG, Bertali, G, Prestat, E, Scenini, F & Haigh, SJ (2017). The application of in situ analytical transmission electron microscopy to the study of preferential intergranular oxidation in Alloy 600. Ultramicroscopy 176, 46–51.CrossRefGoogle Scholar
Cassidy, C, Yamashita, M, Cheung, M, Kalale, C, Adaniya, H, Kuwahara, R & Shintake, T (2017). Water without windows: Evaluating the performance of open cell transmission electron microscopy under saturated water vapor conditions, and assessing its potential for microscopy of hydrated biological specimens. PLOS ONE 12, e0186899.CrossRefGoogle ScholarPubMed
Chen, Y, An, Z & Chen, M (2018). Competition mechanism study of Mg + water and MgO + water reaction. Mater Sci Eng 394, 1–5.CrossRefGoogle Scholar
Creemer, JF, Helveg, S, Hoveling, GH, Ullmann, S, Molen-broek, AM, Sarro, PM & Zandbergen, HW (2008). Atomic-scale electron microscopy at ambient pressure. Ultramicroscopy 108(9), 993–998.CrossRefGoogle ScholarPubMed
Crozier, PA & Chenna, S (2011). In situ analysis of gas composition by electron energy-loss spectroscopy for environmental transmission electron microscopy. Ultramicroscopy 111, 177–185.CrossRefGoogle ScholarPubMed
Dai, S, Zhang, S, Katz, MB, Graham, GW & Pan, X (2017). In Situ observation of Rh-CaTiO3 catalysts during reduction and oxidation treatments by transmission electron microscopy. ACS Catal 7, 1579–1582.CrossRefGoogle Scholar
Ehlers, J, Young, DJ, Smaardijk, EJ, Tyagi, AK, Penkalla, HJ, Singheiser, L & Quadakkers, WJ (2006). Enhanced oxidation of the 9%Cr steel P91 in water vapour containing environments. Corros Sci 48, 3428–3454.CrossRefGoogle Scholar
Flowers, P, Theopold, K, Langley, R & Robinson, WR (2015). Liquids and solids. In Chemistry, pp. 539–540. Houston, Texas: OpenStax Rice University.Google Scholar
Gleeson, B (2018). Still plenty to explore. Nat Mater 17, 574–576.CrossRefGoogle ScholarPubMed
Hansen, TW & Wagner, JB (2014). Catalysts under controlled atmospheres in the transmission electron microscope. Ultramicroscopy 4, 1673–1685.Google Scholar
Holcomb, GR, Carney, C & Dogan, ON (2016). Oxidation of alloys for energy applications in supercritical CO2 and WATER. Micron 109, 22–35.Google Scholar
Li, P, Liu, J, Nag, N & Crozier, PA (2009). In situ preparation of Ni–Cu/TiO2 bimetallic catalysts. J Catal 262, 73–82.CrossRefGoogle Scholar
Li, Y, Zakharov, D, Zhao, S, Tappero, R, Jung, U, Elsen, A, Baumann, P, Nuzzo, RG, Stach, EA & Frenkel, AI (2015). Complex structural dynamics of nanocatalysts revealed in Operando conditions by correlated imaging and spectroscopy probes. Nat Commun 6, 7583.CrossRefGoogle ScholarPubMed
Likith, SRJ, Farberow, CA, Manna, S, Abdulslam, A, Stevanovi, V, Ruddy, DAO, Schaidle, JA, Robichaud, DJ & Ciobanu, CVO (2017). Thermodynamic stability of molybdenum oxycarbides formed from orthorhombic Mo2C in oxygen-rich environments. J Phys Chem C 122, 1223–1233.CrossRefGoogle Scholar
Liu, X, Zhang, C, Li, Y, Niemantsverdriet, JW, Wagner, JB & Hansen, TW (2017). Environmental transmission electron microscopy (ETEM) studies of single iron nanoparticle carburization in synthesis gas. ACS Catal 7, 4867–4875.CrossRefGoogle Scholar
Luo, L, Su, M, Yan, P, Zou, L, Schreiber, DK, Baer, DR, Zhu, Z, Zhou, G, Wang, Y, Bruemmer, SM, Xu, Z & Wang, C (2018). Atomic origins of water-vapour-promoted alloy oxidation. Nat Mater 17, 514–518.CrossRefGoogle ScholarPubMed
McKelvy, MJ, Sharma, R, Chizmeshya, AVG, Carpenter, RW & Streib, K (2001). Magnesium hydroxide dehydroxylation: In situ nanoscale observations of Lamellar nucleation and growth. Chem Mater 13, 921–926.CrossRefGoogle Scholar
Mortazavi, N, Geers, C, Esmaily, M, Babic, V, Sattari, M, Lindgren, K, Malmberg, P, Jönsson, B, Halvarsson, M, Svensson, JE, Panas, I & Johansson, LG (2018). Interplay of water and reactive elements in oxidation of alumina-forming alloys. Nat Mater 17, 610–617.CrossRefGoogle ScholarPubMed
Onal, K, Maris-Sida, MC, Meier, GH & Pettit, FS (2003). Water vapor effects on the cyclic oxidation resistance of alumina forming alloys. Mater High Temp 20, 327–337.CrossRefGoogle Scholar
Opila, EJ (2004). Volatility of common protective oxides in high-temperature water vapor: Current understanding and unanswered questions. Int J Basic Appl Sci IJBAS-IJENS 461–464, 765–774.Google Scholar
Pint, BA, Haynes, JA, Unocic, KA & Zhang, Y (2012). The effect of water vapor and superalloy composition on thermal barrier coating lifetime. 12th International Symposium on Superalloys, Huron, ES, Reed, RC, Hardy, MC, Mills, MJ, Montero, RE, Portella, PD & Telesman, J (Eds.), pp. 723–732. Hoboken, New Jersey: John Wiley & Sons, Inc.Google Scholar
Rackauskas, S, Jiang, H, Wagner, JB, Shandakov, SD, Hansen, TW, Kauppinen, EI & Nasibulin, AG (2014). In situ study of noncatalytic metal oxide nanowire growth. Nano Lett 14, 5810–5813.CrossRefGoogle ScholarPubMed
Simonsen, SB, Dahl, S, Johnson, E & Helveg, S (2008). Ceria-catalyzed soot oxidation studied by environmental transmission electron microscopy. J Catal 255, 1–5.CrossRefGoogle Scholar
Sturkey, L & Frevel, LK (1945). Refraction effects in electron diffraction. Phys Rev 68, 56–57.CrossRefGoogle Scholar
Taheri, ML, Stach, EA, Arslan, I, Crozier, PA, Kabius, BC, LaGrange, T, Minor, AM, Takeda, S, Tanase, M, Wagner, JB & Sharma, R (2016). Current status and future directions for in situ transmission electron microscopy. Ultramicroscopy 170, 86–95.CrossRefGoogle ScholarPubMed
Unocic, KA, Choi, J-S, Ruddy, DA, Yang, C, Kropf, J, Miller, J, Krause, TR & Habas, S (2018 a). In situ S/TEM reduction reaction of Ni-Mo2C catalyst for biomass conversion. Microsc Microanal 24, 322–323.CrossRefGoogle Scholar
Unocic, KA, Datye, AK, Bigelow, WC & Allard, LF (2017 a). Water vapor in closed-cell in situ gas reactions: Initial experiments. Microsc Microanal 23, 940–941.CrossRefGoogle Scholar
Unocic, KA, Elsentriecy, HH, Brady, MP, Meyer, HM III, Song, GL, Fayek, M, Meisner, RA & Davis, B (2014 a). Transmission electron microscopy study of aqueous film formation and evolution on magnesium alloys. JECS 161, C302–C311.Google Scholar
Unocic, KA, Essuman, E, Dryepondt, S & Pint, BA (2012). Effect of environment on the scale formed on oxide dispersion strengthened FeCrAl at 1050°C and 1100°C. Mater High Temp 29, 171–180.CrossRefGoogle Scholar
Unocic, KA, Kolbus, LM, Dehoff, RR, Dryepondt, SN & Pint, BA (2014 b). High-temperature performance of UNS N07718 processed by additive manufacturing. CORROSION 2014 Paper No. 4478, March 9–14, 2014, San Antonio, Texas, USA. Houston, Texas: NACE International.Google Scholar
Unocic, KA, Meyer, HM, Walden, FS, Marthe, NL, Bigelow, WC & Allard, LF (2018 b). Controlling water vapor in gas-cell microscopy experiments. Microsc Microanal 24, 286–287.CrossRefGoogle Scholar
Unocic, KA & Pint, BA (2013 a). Effect of water vapor on thermally grown alumina scales on bond coatings. Surf Coat Technol 215, 30–38.CrossRefGoogle Scholar
Unocic, KA & Pint, BA (2013 b). Oxidation behavior of co-doped NiCrAl alloys in dry and wet air. Surf Coat Technol 237, 8–15.CrossRefGoogle Scholar
Unocic, KA & Pint, BA (2013 c). Effect of water vapor on thermally grown alumina scales on bond coatings. Surf Coat Technol 215, 30–38.CrossRefGoogle Scholar
Unocic, KA, Shin, D, Unocic, RR & Allard, LF (2017 b). NiAl oxidation reaction processes studied in situ using MEMS-based closed-cell gas reaction transmission electron microscopy. Oxid Metals 88, 495–508.CrossRefGoogle Scholar
Vendelbo, SB, Elkjær, CF, Falsig, H, Puspitasari, I, Dona, P, Mele, L, Morana, B, Nelissen, BJ, van Rijn, R, Creemer, JF, Kooyman, PJ & Helveg, S (2014). Visualization of oscillatory behaviour of Pt nanoparticles catalysing CO oxidation. Nat Mater 13, 884–890.CrossRefGoogle ScholarPubMed
Wu, YA, Li, L, Li, Z, Kinaci, A, Chan, MKY, Sun, Y, Guest, JR, McNulty, I, Rajh, T & Liu, Y (2016). Visualizing redox dynamics of a single Ag/AgCl heterogeneous nanocatalyst at atomic resolution. ACS Nano 10, 3738–3746.CrossRefGoogle ScholarPubMed
Xie, Y, Zhang, J, Young, DJ & Zheng, W (2019). Effect of Fe on corrosion of Ni-20Cr and Ni-30Cr alloys in wet CO2 gas at 650 and 700°C. Corros Sci 154, 129–143.CrossRefGoogle Scholar
Young, D (2008). Effects of water vapour on oxidation, chapter 10. In High Temperature Oxidation and Corrosion of Metals, pp. 455–496. Elsevier Science.CrossRefGoogle Scholar
Zhang, L, Miller, BK & Crozier, PA (2013). Atomic level in situ observation of surface amorphization in anatase nanocrystals during light irradiation in water vapor. Nano Lett 13, 679–684.CrossRefGoogle ScholarPubMed
Zhong, XL, Schilling, S, Zaluzec, NJ & Burke, MG (2016). Sample preparation methodologies for in situ liquid and gaseous cell analytical transmission electron microscopy of electropolished specimens. Microsc Microanal 22, 1350–1359.CrossRefGoogle ScholarPubMed