Abstract
Materials synthesis and the functioning of devices often involve liquid media. However, direct visualization of dynamic processes in liquids, especially with high spatial and temporal resolution, has been challenging. For solid materials, advances in aberration-corrected electron microscopy have made observations of atomic-level features a routine practice. Here, we discuss the extent to which one can take advantage of the resolution of modern electron microscopes to image phenomena occurring in liquids. We describe the fundamentals of two different experimental approaches that use closed and open liquid cells. We illustrate the capabilities of each approach by considering processes in batteries and nucleation and growth of nanoparticles from solution. Liquid-cell electron microscopy appears to be duly fulfilling its role and promise for in situ studies of nanoscale processes in liquids, revealing physical and chemical processes that are otherwise difficult to observe.
Similar content being viewed by others
References
M. Haider, S. Uhlemann, E. Schwan, H. Rose, B. Kabius, K. Urban, Nature 392 (6678), 768 (1998).
K.W. Urban, Nat. Mater. 8, 260 (2009).
D.A. Muller, Nat. Mater. 8, 263 (2009).
A.R. Harutyunyan, G.G. Chen, T.M. Paronyan, E.M. Pigos, O.A. Kuznetsov, K. Hewaparakrama, S.M. Kim, D. Zakharov, E.A. Stach, G.U. Sumanasekera, Science 326 (5949), 116 (2009).
B.J. Kim, J. Tersoff, S. Kodambaka, M.C. Reuter, E.A. Stach, F.M. Ross, Science 322 (5904), 1070 (2008).
P.L. Hansen, J.B. Wagner, S. Helveg, J.R. Rostrup-Nielsen, B.S. Clausen, H. Topsøe, Science 295 (5562), 2053 (2002).
P. Nolte, A. Stierle, N.Y. Jin-Phillipp, N. Kasper, T.U. Schulli, H. Dosch, Science 321, 1654 (2008).
H. Yoshida, Y. Kuwauchi, J.R. Jinschek, K. Sun, S. Tanaka, M. Kohyama, S. Shimada, M. Haruta, S. Takeda, Science 335, 317 (2012).
A.M. Minor, S.A.S. Asif, Z.W. Shan, E.A. Stach, E. Cyrankowski, T.J. Wyrobek, O.L. Warren, Nat. Mater. 5 (9), 697 (2006).
H.M. Zheng, R.K. Smith, Y.W. Jun, C. Kisielowski, U. Dahmen, A.P. Alivisatos, Science 324 (5932), 1309 (2009).
H.-G. Liao, L.K. Cui, S. Whitelam, H.M. Zheng, Science 336 (6084), 1011 (2012).
J.E. Evans, K.L. Jungjohann, N.D. Browning, I. Arslan, Nano Lett. 11 (7), 2809 (2011).
H.M. Zheng, S.A. Claridge, A.M. Minor, A.P. Alivisatos, U. Dahmen, Nano Lett. 9 (6), 2460 (2009).
M.J. Williamson, R.M. Tromp, P.M. Vereecken, R. Hull, F.M. Ross, Nat. Mater. 2 (8), 532 (2003).
E.R. White, S.B. Singer, V. Augustyn, W.A. Hubbard, M. Mecklenburg, B. Dunn, B.C. Regan, ACS Nano 6 (7), 6308 (2012).
M. Gu, L.R. Parent, B.L. Mehdi, R.R. Unocic, M.T. McDowell, R.L. Sacci, W. Xu J.G. Connell, P. Xu, P. Abellan, X. Chen, Y. Zhang, D.E. Perea, J.E. Evans, L.J. Lauhon, J.-G. Zhang, J. Liu, N.D. Browning, Y. Cui, I. Arslan, C.-M. Wang, Nano Lett. 13 (12), 6106 (2013).
X. Chen, K.W. Noh, J.G. Wen, S.J. Dillon, Acta Mater. 60, 192 (2012).
U. Mirsaidov, C.-D. Ohl, P. Matsudaira, Soft Matter 8, 7108 (2012).
E.R. White, M. Mecklenburg, S.B. Singer, S. Aloni, B.C. Regan, Appl. Phys. Express 4, 055201 (2011).
D. Li, M.H. Nielsen, J.R. Lee, C. Frandsen, J.F. Banfield, J.J. De Yoreo, Science 336 (6084), 1014 (2012).
T.W. Huang, S.Y. Liu, Y.J. Chuang, H.Y. Hsieh, C.Y. Tsai, W.J. Wu, C.T. Tsai, U. Mirsaidov, P. Matsudaira, C.S. Chang, F.G. Tseng, F.R. Chen, Soft Matter 9 (37), 8856 (2013).
M.T. Proetto, A.M. Rush, M.-P. Chien, P. Abellan Baeza, J.P. Patterson, M.P. Thompson, N.H. Olson, C.E. Moore, A.L. Rheingold, C. Andolina, J. Millstone, S.B. Howell, N.D. Browning, J.E. Evans, N.C. Gianneschi, J. Am. Chem. Soc. 136 (4), 1162 (2014).
N. de Jonge, D.B. Peckys, G.J. Kremers, D.W. Piston, Proc. Natl. Acad. Sci. U.S.A. 106 (7), 2159 (2009).
U.M. Mirsaidov, H.M. Zheng, Y. Casana, P. Matsudaira, Biophys. J. 102 (4), L15 (2012).
J.E. Evans, K.L. Jungjohann, P.C.K. Wong, P.-L. Chiu, G.H. Dutrow, I. Arslan, N.D. Browning, Micron 43 (11), 1085 (2012).
N. de Jonge, F.M. Ross, Nat. Nano technol. 6 (11), 695 (2011).
K. Degen, M. Dukes, J.R. Tanner, D.F. Kelly, RSC Adv. 2, 2408 (2012).
E.A. Ring, N. de Jonge, Microsc. Microanal. 16, 622 (2010).
K. Tai, Y. Liu, S.J. Dillon, Microsc. Microanal. 20, 330 (2014).
H.-G. Liao, D. Zherebetskyy, H.L. Xin, C. Czarnik, P. Ercius, H. Elmlund, M. Pan, L.W. Wang, H.M. Zheng, Science 345 (6199), 916 (2014).
T.J. Woehl, K.L. Jungjohann, J.E. Evans, I. Arslan, W.D. Ristenpart, N.D. Browning, Ultramicroscopy 127, 53 (2013).
K.L. Jungjohann, J.E. Evans, J.A. Aguiar, I. Arslan, N.D. Browning, Microsc. Microanal. 18 (03), 621 (2012).
R.F. Egerton, Ultramicroscopy 127, 100 (2013).
N. de Jonge, D.B. Peckys, G.J. Kremers, D.W. Piston, Proc. Natl. Acad. Sci. U.S.A. 106, 2159 (2009).
T.J. Woehl, J.E. Evans, I. Arslan, W.D. Ristenpart, N.D. Browning, ACS Nano 6 (10), 8599 (2012).
D.A. Welch, R. Faller, J.E. Evans, N.D. Browning, Ultramicroscopy 135, 36 (2013).
K.L. Jungjohann, J.E. Evans, J.A. Aguiar, I. Arslan, N.D. Browning, Microsc. Microanal. 18 (3), 621 (2012).
J.F. Creemer, S. Helveg, G.H. Hoveling, S. Ullmann, A.M. Molenbroek, P.M. Sarro, H.W. Zandbergen, Ultramicroscopy 108, 993 (2008).
J.M. Grogan, H.H. Bau, J. Microelectromech. Syst. 19, 885 (2010).
E. Jensen, A. Burrows, K. Mølhave, Microsc. Microanal. 20, 445 (2014).
J.M. Yuk, J. Park, P. Ercius, K. Kim, D.J. Hellebusch, M.F. Crommie, J.Y. Lee, A. Zettl, A.P. Alivisatos, Science 336 (6077), 61 (2012).
C.M. Wang, W. Xu, J. Liu, D.W. Choi, B. Arey, L.V. Saraf, J.G. Zhang, Z.G. Yang, S. Thevuthasan, D.R. Baer, N. Salmon, J. Mater. Res. 25, 1541 (2010).
J.Y. Huang, L. Zhong, C.M. Wang, J.P. Sullivan, W. Xu, L.Q. Zhang, S.X. Mao, N.S. Hudak, X.H. Liu, A. Subramanian, H. Fan, L. Qi, A. Kushima, J. Li, Science 330 (6010), 1515 (2010).
X.H. Liu, H. Zheng, L. Zhong, S. Huang, K. Karki, L.Q. Zhang, Y. Liu, A. Kushima, W.T. Liang, J.W. Wang, J.-H. Cho, E. Epstein, S.A. Dayeh, S.T. Picraux, T. Zhu, J. Li, J.P. Sullivan, J. Cumings, C.-M. Wang, S.X. Mao, Z.Z. Ye, S. Zhang, J.Y. Huang, Nano Lett. 11 (8), 3312 (2011).
X.H. Liu, S. Huang, S.T. Picraux, J. Li, T. Zhu, J.Y. Huang, Nano Lett. 11 (9), 3991 (2011).
Y. Liu, N.S. Hudak, D.L. Huber, S.J. Limmer, J.P. Sullivan, J.Y. Huang, Nano Lett. 11 (10), 4188 (2011).
A. Kushima, X.H. Liu, G. Zhu, Z.L. Wang, J.Y. Huang, J. Li, Nano Lett. 11, (11), 4535 (2011).
X.H. Liu, J.W. Wang, Y. Liu, H. Zheng, A. Kushima, S. Huang, T. Zhu, S.X. Mao, J. Li, S. Zhang, W. Lu, J.M. Tour, J.Y. Huang, Carbon 50 (10), 3836 (2012).
Y. Liu, H. Zheng, X.H. Liu, S. Huang, T. Zhu, J. Wang, A. Kushima, N.S. Hudak, X. Huang, S. Zhang, S.X. Mao, X. Qian, J. Li, J.Y. Huang, ACS Nano 5 (9), 7245 (2011).
M.M. Islam, T. Bredow, J. Phys. Chem. C 113, 672 (2009).
F. Wang, H.-C. Yu, M.-H. Chen, L. Wu, N. Pereira, K. Thornton, A. Van der Ven, Y. Zhu, G.G. Amatucci, J. Graetz, Nat. Commun. 3, 1201 (2012).
H.-G. Liao, H. Zheng, J. Am. Chem. Soc. 135 (13), 5038 (2013).
K.L. Jungjohann, S. Bliznakov, P.W. Sutter, E.A. Stach, E.A. Sutter, Nano Lett. 13 (6), 2964 (2013).
O. Akhavan, E. Ghaderi, J. Phys. Chem. C 113 (47), 20214 (2009).
A.B. Panda, G. Glaspell, M.S. El-Shall, J. Am. Chem. Soc. 128 (9), 2790 (2006).
X.-H. Liao, N.-Y. Chen, S. Xu, S.-B. Yang, J.-J. Zhu, J. Cryst. Growth 252, (4), 593 (2003).
Z. Li, L. Peng, Y. Fang, Z. Chen, D. Pan, M. Wu, Radiat. Phys. Chem. 80, (12), 1333 (2011).
F. Zhou, R. Zhou, X. Hao, X. Wu, W. Rao, Y. Chen, D. Gao, Radiat. Phys. Chem. 77 (2), 169 (2008).
R. Divan, Q. Ma, D. Mancini, D. Keane, Rom. J. Inf. Sci. Technol. 11 (1), 71 (2008).
J. Rojas, C. Castano, Radiat. Phys. Chem. 81 (1), 16 (2012).
Y. Mishra, D. Avasthi, P. Kulriya, F. Singh, D. Kabiraj, A. Tripathi, J. Pivin, I. Bayer, A. Biswas, Appl. Phys. Lett. 90 (7), 073110 (2007).
H.L. Xin, H. Zheng, Nano Lett. 12 (3), 1470 (2012).
A. Radisic, P.M. Vereecken, J.B. Hannon, P.C. Searson, F.M. Ross, Nano Lett. 6, 238 (2006).
A. Radisic, F.M. Ross, P.C. Searson, J. Phys. Chem. B 110, 7862 (2006).
A. Radisic, P.M. Vereecken, P.C. Searson, F.M. Ross, Surf. Sci. 600, 1817 (2006).
M. den Heijer, I. Shao, A. Radisic, M.C. Reuter, F.M. Ross, APL Mater. 2, 022101 (2014).
J.M. Grogan, N.M. Schneider, F.M. Ross, H.H. Bau, J. Indian Inst. Sci. 92, 295 (2012).
M.E. Holtz, Y. Yu, D. Gunceler, J. Gao, R. Sundararaman, K.A. Schwarz, T.S.A. Arias, H.C.D. Abruña, D.A. Muller, Nano Lett. 14, 1453 (2014).
R.L. Sacci, N.J. Dudney, K.L. More, L.R. Parent, I. Arslan, N.D. Browning, R.R. Unocic, Chem. Commun. 50, 2104 (2014).
Z. Zeng, W.-I. Liang, H.-G. Liao, H.L. Xin, Y.-H. Chu, H. Zheng, Nano Lett. 14, 1745 (2014).
R.R. Unocic, R.L. Sacci, G.M. Brown, G.M. Veith, N.J. Dudney, K.L. More F.S. Walden II, D.S. Gardiner, J. Damiano, D.P. Nackashi, Microsc. Microanal. 20, 452 (2014).
D. Morgan, A. Van der Ven, G. Ceder, Electrochem. Solid-State Lett. 7 (2), A30–A32 (2004).
P. Gibot, M. Casas-Cabanas, L. Laffont, S. Levasseur, P. Carlach, S. Hamelet, J.M. Tarascon, C. Masquelierk, Nat. Mater. 7 (9), 741 (2008).
R. Malik, F. Zhou, G. Ceder, Nat. Mater. 10 (8), 587 (2011).
Y. Zhu, J.W. Wang, Y. Liu, X. Liu, A. Kushima, Y. Liu, Y. Xu, S.X. Mao, J. Li, C. Wang, J.Y. Huang, Adv. Mater. 25, 5461 (2013).
K. Kang Xu, A. von Cresce, U. Lee, Langmuir 26 (13), 11538 (2010).
J.M. Grogan, N.M. Schneider, F.M. Ross, H.H. Bau, Nano Lett. 14, 359 (2014).
J. Belloni, M. Mostafavi, H. Remita, J.L. Marignier, M.O. Delcourt, New J. Chem. 22 (11), 1239 (1998).
J. Belloni, Catal. Today 113 (3–4), 141 (2006).
P. Abellan, B.L. Mehdi, L.R. Parent, M. Gu, C. Park, W. Xu, Y. Zhang, I. Arslan, J.-G. Zhang, C.-M. Wang, J.E. Evans, N.D. Browning, Nano Lett. 14, 1293 (2014).
Acknowledgements
C.-M.W. acknowledges the support of the Assistant Secretary for Energy Efficiency and Renewable Energy, Office of Vehicle Technologies, of the US Department of Energy (DOE) under Contract DE-AC02-05CH11231, Subcontract 18769, under the Batteries for Advanced Transportation Technologies program. The in situ TEM capability is developed under the Chemical Imaging Initiative at Pacific Northwest National Laboratory (PNNL). C.-M.W. also acknowledges the support of the William R. Wiley Environmental Molecular Sciences Laboratory, a national scientific user facility sponsored by DOE’s Office of Biological and Environmental Research and located at PNNL. PNNL is operated by Battelle for the DOE under Contract DE-AC05-76RL01830. H.-G.L. was supported by the DOE Office of Science Early Career Research Program under the supervision of Dr. Zheng at Lawrence Berkeley National Laboratory (LBNL). H.-G.L. also acknowledges the facility support of the National Center for Electron Microscopy at LBNL, which is supported by the Office of Basic Energy Sciences, Division of Materials Sciences and Engineering, of the US DOE under Contract DE-AC02-05CH11231.
Author information
Authors and Affiliations
Rights and permissions
About this article
Cite this article
Wang, CM., Liao, HG. & Ross, F.M. Observation of materials processes in liquids by electron microscopy. MRS Bulletin 40, 46–52 (2015). https://doi.org/10.1557/mrs.2014.283
Published:
Issue Date:
DOI: https://doi.org/10.1557/mrs.2014.283