3. Si based membrane chips for in-situ TEM liquid cell
3.3 Conclusions
was pasted on the container with heating on hot plate at 150oC. The bottom chip put on the container and container-bottom chip assembly was cooled to be closured the bottom part. Specimen dispersed liquid was dropped on bottom chips and top piece covered the liquid. Some of leaked liquid was wiped off with tissue. The UV epoxy was pasted on the top of container-liquid cell assembly and hardened with UV light for 1min. The advanced plasma system, Gatan-960 (Gatan, USA), was used to check the sealing of liquid in 70m torr vacuum condition for 20min. The UV epoxy effectively prevent to evaporating the liquid in cell.
The size of container was 4mm x 5.1mm. The zig containing liquid cell could be fixed on the in-situ TEM holder with high vacuum grease. It was stably sticky on the TEM holder. So it was expected that the zig would not be detached in TEM system during sample analysis.
Summary
The hybrid Na-air batteries, the seawater batteries, fabricated with the solid electrolyte that is very important component for transferring the Na+ ions. The NASICON should have chemical & physical stabilities and high ionic conductivities serving as separator and electrolyte. Before applied in seawater batteries, the characteristics of the NASICON itself were studied with much analytical equipment.
As the solid electrolyte contacted with seawater and influenced by electrochemical processes, the seawater and D.I water immersed the NASICON pellets for a long time. The hydronium NASICON generated on the NASICON surface and minor phase was dissolving from the NASICON. The platinum noble metal was effective on the OER/ORR process that should be important factors to improve the performance of seawater batteries. The NASICON was degraded by electrochemical process, in particular, charge process generating the HCl. The concentration of hydronium ions in seawater impacted on the degradation of the NASICON. I fabricated the Si based liquid cell assembly to monitor the deterioration of the NASICON.
These studies suggested not only the new insights of the NASICON properties but also the structural degradation of the NASICON solid electrolyte. The analysis of the solid electrolyte and deterioration would be fundamental for development of seawater batteries.
References
1. The UN’s ‘sustainable energy for all’ initiative is compatible with a warming limit of 2oC. Joeri Rogelj, David L.McCollum & Keywan Riahi. nature climate change 3, 545-551 (2013)
2. Towards greener and more sustainable batteries for electrical energy storage. D.Larcher, J- M.Trascon. Nature chemistry 7, 19-29 (2015)
3. Opportunities and challenges for a sustainable energy future. Steven Chu, Arun Majumdar. Nature 488, 294-303 (2012)
4. Optimum energy storage techniques for the improvement of renewable energy sources-based electricity generation economic efficiency. J.K. Kaldellis_, D. Zafirakis. Energy 32 2295ឡ2305 (2007) 5. Promise and reality of post-lithium-ions batteries with high energy densities. Choi, J. W., Aurbach D. Nat. rev. mater. 1, 16013 (2016)
6. Li-ion battery materials: present and future. Naoki Nitta, Feixiang Wu, Jung Tae Lee, Gleb Yushin Materials today 18, 5, 252-264,( 2015)
7. Batteries and fuel cells for emerging electric vehicle markets. Zachary P. Cano, Dustin Banham, Siyu Ye, Andreas Hintennach, Jun Lu, Michael Fowler and Zhongwei Chen Nature Energy 3, 279- 289 (2018)
8. Global Energy Storage Market Overview & Regional Summary Report 2015. The Energy Storage Council 978-0-646-94626-9
9. Na-ion batteries, recent advances and present challenges to become low cost energy storage systems. Verónica Palomares, Paula Serras, Irune Villaluenga, Karina B. Hueso, Javier Carretero- González and Teófilo Rojo. Energy Environ. Sci., 5, 5884-5901 (2012)
10. Sodium and sodium-ion energy storage batteries Current Opinion in Solid State and Materials.
Brian L.Ellis, Linda F.Nazar. Science 16 168-177 (2012)
11. A cost and resource analysis of sodium-ion batteries. Christoph vaalma, Daniel Buchholz, Marcel weil, Stefano passerine. Nature reviews materials 3 18013 (2018)
12. United States Geological Survey. Mineral commodity summaries 2018.
https://minerals.usgs.gov/minerals/pubs/mcs/2018/ mcs2018.pdf
13. Global lithium availability. Gruber, P. W. et al. J. Ind. Ecol. 15, 760–775 (2011).
14. Handbook of methods for the analysis of the various parameters of the carbon dioxide system in sea water. A.G. Dickson & C. Goyet. (1994)
15. Saltwater as the energy source for low-cost, safe rechargeable batteries. Sangmin Park, Baskar SenthilKumar, Kyoungho Kim, Soo Min Hwang and Youngsik Kim. J. Mater. Chem., 4, 7207 (2016) 16. Rechargeable Seawater Battery and Its Electrochemical Mechanism. Jae-Kwang Kim, Eungje Lee, Hyojin Kim, Christopher Johnson, Jaephil Cho, Youngsik Kim. ChemElectroChem, 2, 328–332,
(2015)
17. Sodium-ion hybrid electrolyte battery for sustainable energy storage applications. S.T. Senthil kumar, Mari Abirami, Junsoo Kim, Wooseok Go, Soo Min Hwang, Youngsik Kim. Journal of Power Sources 341 404-410 (2017).
18. Eco-friendly Energy storage system : seawater and ionic liquid electrolyte. Jae-Kwang Kim, Franziska Mueller, Hyojin Kim, Sangsik Jeong, Jeong-Sun Park, Stefano Passerini, and Young sik Kim. ChemSusChem, 9,42–49, (2016)
19. Development of coin-type cell and engineering of its compartments for rechargeable seawater batteries. Jinhyup Han, Soo Min Hwanga, Wooseok Go, S.T. Senthilkumara, Dong hoon Jeon, Young sik Kim. Journal of Power Sources 374, 24–30, (2018)
20. Na ion- Conducting Ceramic as Solid Electrolyte for Rechargeable Seawater Batteries. Yongil Kima, Hyojin Kima, Sangmin Parka, Inseok Seob, Youngsik Kim. Electrochimica Acta 191 1–7 (2016).
21. Hybrid seawater desalination-carbon capture using modified seawater battery system. Hyuntae Bae, Jeong-Sun Park, S.T.Senthil kumar, Soo Min Hwang, Young sik Kim. Journal of Power Sources 15–31, 99-105, (2019).
22. Reliable seawater battery anode: controlled sodium nucleation via deactivation of the current collector surface. Do Hyeong Kim, Hongkyw Choi, Dae Yeon Hwang, Jaehyun Park, Keun Soo Kim, Seokhoon Ahn, Youngsik Kim, Sang Kyu Kwak, Young-Jun Yu and Seok Ju Kang. J. Mater. Chem.
A, 6, 19672-19680, (2018)
23. Rechargeable aqueous Na–air batteries: Highly improved voltage efficiency by use of catalysts.
Sun Hye Sahgong, S.T. Senthilkumar, Kyoungho Kim, Soo Min Hwang, Youngsik Kim.
Electrochemistry Communications 61, 53–56, (2015)
24. The role of separator in lithium ion cell safety. Christopher J. Oren dorff. The electrochemical society interface 2012
25. CRYSTAL STRUCTURES AND CRYSTAL CHEMISTRY IN THE SYSTEM Nal+xZr2SixP3_xO12. H.Y-P.Hong. Mat. Res. Bull. II, 173-182, (1976)
26. High temperature sodium batteries: status, challenges and future trends. Karina B. Hueso, Michel Armand and Te´ ofilo Rojo. Energy Environ. Sci., 6, 734, (2013)
27. Understanding Na Mobility in NASICON Materials: A Rietveld, 23Na and 31P MAS NMR, and Impedance Study. Enrique R. Losilla, Miguel A. G. Aranda, Sebastián Bruque. Chem. Mater., 10, 665–673, (1998)
28. Relation structure – fast ion conduction in the NASICON solid solution. J.P.Boilot, G.Collin, Colomban. Journal of solid state chemistry 73, 160-171, (1988)
29. Capacily Fading on Cycling of 4 V Li/LiMn2O4 Cells Yongyao Xia, Yunhong Zhou,° and Masaki Yoshio. J Electrochem. Soc., 8, 144, (1997)
30. Simulation of capacity fade in lithium-ion batteries. R.Spotnitz. Journal of power sources 113, 72- 80, (2003)
31. Theory of SEI Formation in Rechargeable Batteries: Capacity Fade, Accelerated Aging and Lifetime Prediction. Matthew B. Pinson1 and Martin Z. Bazant. Massachusetts Institute of Technology, Cambridge, MA 02139
32. Study on lithium/air secondary batteries—Stability of NASICON-type lithium ion conducting glass–ceramics with water. Satoshi Hasegawa, Nobuyuki Imanishi, Tao Zhang, Jian Xie, Atsushi Hirano, Yasuo Takeda, Osamu Yamamoto. Journal of Power Sources 189, 371-377, (2009)
33. Water Durable Lithium Ion Conducting Composite Membranes from the Li2O-Al2O3-TiO2- P2O5 Glass-Ceramic. Joykumar S. Thokchom, and Binod Kumar Journal of The Electrochemical Society, 154, A331-A336 (2007)
34. Reaction of NASICON with water R.O. Fuentes, F. Figueiredo, F.M.B. Marques a , J.I. Franco Solid State Ionics, 139, 309–314, (2001)
35. Characterization of protonically exchanged NASICON. P.G Komorowski, S.A argyropoulos solid state ionics 48, 295-301, (1991)
36. Reactivity of NASICON with water and interpretation of the detection limit of a NASICON based Na+ ion selective electrode F. Mauvy, E. Siebert *, P. Fabry. Talanta 48, 293–303, (1999)
37. Platinum−Gold Nanoparticles: A Highly Active Bifunctional Electrocatalyst for Rechargeable Lithium−Air Batteries. Yi-Chun Lu, Zhichuan Xu, Hubert A. Gasteiger, Shuo Chen, Kimberly Hamad-Schifferli, Yang Shao-Horn. J. Am. Chem. Soc., 132 (35), 12170-12171 (2010)
38. Controlling the Catalytic Activity of PlatinumǦMonolayer Electrocatalysts for Oxygen Reduction with Different Substrates. Junliang Zhang, Miomir B. Vukmirovic Dr, Ye Xu, Manos Mavrikakis, Radoslav R. Adzic. Angewandte chemie 14, 117, 2170-2173, (2005)
39. Mechanical properties of the solid electrolyte Al-substituted Li7La3Zr2O12 (LLZO) by utilizing micro-pillar indentation splitting test . An-Ni Wang, Juliane Franciele Nonemacher, Gang Yan, Martin Finsterbusch, Jürgen Malzbender, Manja Krüger. Journal of the European Ceramic Society 38, 9, 3201-3209 (2018)
40. Cleaning and surface properties M. Taborelli CERN, Geneva, Switzerland
41. Synthesis, processing and characterization of nasicon solid electrolytes for CO2 sensing applications Minghua Zhou Aftab Ahmad. Sensors and Actuators B 122 419–426 (2007)
42. Progressive Assessment on the Decomposition Reaction of Na Superionic Conducting Ceramics.
Jae-Il Jung, Daekyeom Kim, Hyojin Kim, Yong Nam Jo, Jung Sik Park, Youngsik Kim ACS Appl.
Mater. Interfaces 9, 304−310, (2017)
43. Co3O4 nanocrystals on graphene as a synergistic catalyst for oxygen reduction reaction. Yongye Liang, Yanguang Li, HailiangWang, Jigang Zhou, JianWang, Tom Regier, Hongjie Dai1 NATURE MATERIALS 10, 780-786, (2011)
44. A class of non-precious metal composite catalysts for fuel cells. Rajesh Bashyam, Piotr Zelenay, NATURE, 443 7, 63-66, (2006)
45. Measuring oxygen reduction/evolution reactions on the nanoscale. Amit Kumar, Francesco Ciucci, Anna N. Morozovska, Sergei V. Kalinin1, Stephen Jesse NATURE CHEMISTRY, 3, (2011)
46. A Bifunctional Nonprecious Metal Catalyst for Oxygen Reduction and Water Oxidation. Yelena Gorlin, Thomas F. Jaramillo. J. AM. CHEM. SOC. 132, 13612–13614, (2010)
47. Hybrid Na–air flow batteries using an acidic catholyte: effect of the catholyte pH on the cell Performance. Soo Min Hwang, Wooseok Go, Hyein Yu, Youngsik Kim. J. Mater. Chem. A, 5, 11592, (2017).
48. Coating Methods for Use with the Platinum Metals. Christopher Hood. Platinum Metal Rev., 2, 20, 48-52, (1976)
49. Trace degradation analysis of lithium ion battery components. Paul Voelker, ReD magazine, www.RDmag.com, (2014).
50. Predictive modeling of battery degradation and greenhouse gas emissions from U.S. state-level electric vehicle operation. Fan Yang, Yuanyuan Xie, Yelin Deng, Chris yuan. nature communications, 9, 2429 (2018)
51. Aging investigations of a lithium-ion battery electrolyte from a field-tested hybrid electric vehicle.
Martin Grützke, Vadim Kraft, Björn Hoffmann, Sebastian Klamor, Jan Diekmann, Arno Kwade, Martin Winter, SaschaNowak. Power Sources, 273, 1, 83-88, (2015)
52. Understanding ageing in Li-ion batteries: a chemical issue. M.Rosa Palacin. Chem. Soc. Rev.,47, 4924, (2018)
53. Thermal stability studies of Li-Ion cells and components. Hossein Maleki, Guoping Deng, Anaba Anani, Jason Howard. Journal of the Electrochemical Society, 146 (9) 3224-3229 (1999)
54. Review of Lithium Ion Battery Degradation Mechanisms, Models, and their Economic Implications. Andrew W. Thompson. VEDECOM, working paper V1
55. Liquid cell transmission electron microscopy. Hong-gang liao and haimei Zheng Annu. Rev. Phys.
Chem. 67, 719-47, (2016)
56. Imaging gas-solid interactions in an atomic resolution environmental TEM. Xiao Feng Zhang, Takeo Kamino. Microscopy today September 2006, hitachi.
57. electron microscopy of specimens in liquid. Niels de Jonge and Frances M. Ross. Nature Nanotechnology 6 695 (2011)
58. Dynamic microscopy of nanoscale cluster growth at the solid-liquid interface. M.J willamson, R.M Tromp, P.M Vereecken, R.Hull and F.M Ross. Nature materials 2, (2003).
59. Perspectives in in situ transmission electron microscopy studies on lithium battery electrodes Hyun-wook lee, Yuzhang Li, Yi cui. Current Opinion in chemical engineering. 12, 37-43, (2016)
60. Transmission electron microscopy with a liquid flow cell. K.Lklein, I.M Anderson, N.De jonge.
Journal of microscopy 2, 242, (2011)
61. In situ observation of oscillatory growth of bismuth nanoparticles. Xin HL, Zheng H. Nano Lett.
12, 1470–74, (2012)
62. Revealing bismuth oxide hollow nanoparticle formation by the Kirkendall effect. Niu K-Y, Park J, Zheng H. Nano Lett. 13, 5715–19, (2013)
63. In situ cryogenic transmission electron microscopy for characterizing the evolution of solidifying water ice in colloidal systems. Tai K, Liu Y, Dillon SJ. Microsc. Microanal. 20, 330–37 (2014)
64. Understanding mateirals challenges for rechargeable ion batteries with in situ transmission electron microscopy. Yifei Yuan, Khalil Amine, Jun Lu, Reza shahbazian-Yassar. Nature communications 8, 15806, (2017).
65. Dependence of the properties of NASICONs on their composition and processing. A.Ahmad, T.A Wheat, A.K.Kuriakose, J.D.Canaday, A.G.Mcdonald. Solid State Ionics 24, 89 -97, (1987)
66. Basics of micro-structuring https://www.microchemicals.com/downloads/application_notes Microchemicals
67. anisotropic etching of crystalline silicon in alkaline solutions H.seidel, L.Csepregi, A.Heuberger.
J.electrochem. Soc., 11, 137, (1990)
68. Silicon anisotropic etching in alkaline solutions III: On the possibility of spatial structures forming in the course of Si (100) anisotropic etching in KOH and KOH+IPA solutions. Irena Zubel. Sensors and Actuators 84, 116–125, (2000)
69. Silicon anisotropic etching in KOH-isopropanol etchant. Irena Barycka, Irena Zubel. Sensors and Acuators A 48, 229-238, (1995)
70. Fabrication techniques of convex corners in a (1 0 0)-silicon wafer using bulk micromachining: a review. Prem Pal1, Kazuo Sato1 and Sudhir Chandra. J. Micromech. Microeng. 17, 111–133, (2007) 71. A simple and robust model to explain convex corner undercutting in wet bulk micromachining.
Prem Pal, Sajal Sagar Singh, Micro and Nano Systems Letters, 1 ,1 (2013)
72. Improvement in smoothness of anisotropically etched silicon surfaces: Effects of surfactant and TMAH concentrations Di Cheng, Miguel A.Gosálvez, Tatsuya Hori, Kazuo Sato, Mitsuhiro Shikida.
Sensors and Actuators A, 125, 2, 415-421, (2006)
73. Effects of various ion-typed surfactants on silicon anisotropic etching properties in KOH and TMAH solutions. Chii-Rong Yang, Po-Ying Chen, Cheng-Hao Yang, Yuang-Cherng Chiou, Rong- Tsong Lee. Sensors and Actuators A, 119, 1, 271-281, (2005)
74. A generalized model describing corner undercutting by the experimental analysis of TMAH/IPA H K Trieu and W Mokwa. Journal of Micromechanics and Microengineering, 8, 2
75. Corner undercutting in aniso-tropically etched isolation contours Abu-Zeid M. J. Electrochem.
Soc 131, 2138-42, (1984)
76. Compensating corner undercutting in anisotropic etching of (1 0 0) silicon Wu X P and Ko W H.
Sensors Actuators A, 18, 207–15 (1989)
77. Compensation structures for convex corner micromachining in silicon Puers B and Sansen W.
Sensors Actuators A, 23, 1036–41
78. Self-aligned wet-cell for hydrated microbiology observation in TEM. Tsu-Wei Huang, Shih-Yi Liu, Yun-Ju Chuang, Hsin-Yi Hsieh, Chun-Ying Tsai, Yun-Tzu Huang, Utkur Mirsaidov, Paul Matsudaira, Fan-Gang Tseng, Chia-Shen Changh, Fu-Rong Chen. Lab Chip, 12, 340, (2012)
79. Nanoscale Imaging of Whole Cells Using a Liquid Enclosure and a Scanning Transmission Electron Microscope. Diana B. Peckys, Gabriel M. Veith, David C. Joy, Niels de Jonge. PLoS ONE, 4, 12, 8214, (2009)