Skip to main content
×
Home

In situ transmission electron microscopy and spectroscopy studies of interfaces in Li ion batteries: Challenges and opportunities

  • C.M. Wang (a1), W. Xu (a2), J. Liu (a3), D.W. Choi (a2), B. Arey, L.V. Saraf (a1), J.G. Zhang, Z.G. Yang (a2), S. Thevuthasan, D.R. Baer (a1) and N. Salmon (a4)...
Abstract

Transmission electron microscopy (TEM) and spectroscopy have been evolved to a stage such that they can be routinely used to probe the structure and composition of the materials with the resolution of a single atomic column. However, a direct in situ TEM observation of structural evolution of the materials in a lithium ion battery during dynamic operation of the battery has never been reported. In this paper, we report the results of exploring the in situ TEM techniques for observation of interfaces in the lithium ion battery during the operation of the battery. A miniature battery was fabricated using a single nanowire and an ionic liquid electrolyte. The structure and composition of the interface across the anode and the electrolyte was studied using TEM imaging, electron diffraction, and electron energy-loss spectroscopy. In addition, we also explored the possibilities of carrying out in situ TEM studies of lithium ion batteries with a solid state electrolyte.

Copyright
Corresponding author
a)Address all correspondence to this author. e-mail: Chongmin.Wang@pnl.gov
References
Hide All
1.Tarascon J.M., Armand M.Issues and challenges facing rechargeable lithium batteries. Nature 414, 359 (2001)
2.Dedryvere R., Martinez H., Leroy S., Lemordant D., Bonhomme F., Biensan P., Gonbeau D.Surface film formation on electrodes in a LiCoO2/graphite cell: A step by step XPS study. J. Power Sources 174, 462 (2007)
3.Kong F., Kostecki R., Nadeau G., Song X., Zaghib K., Kinoshita K., McLarnon F.In situ studies of SEI formation. J. Power Sources 97–98, 58 (2001)
4.Bryngelsson H., Stjerndahl M., Gustafsson T., Edstrom K.How dynamic is the SEI? J. Power Sources 174, 970 (2007)
5.Chen G.Y., Song X.Y., Richardson T.J.Electron microscopy study of the LiFePO4 to FePO4 phase transition. Electrochem. Solid-State Lett. 9, (6)A295 (2006)
6.Eswaramoorthy S.K., Howe J.M., Muralidharan G.In situ determination of the nanoscale chemistry and behavior of solid-liquid systems. Science 318, 1437 (2007)
7.Brazier A., Dupont L., Dantras-Laffront L., Kuwata N., Kawamura J., Tarascon J.M.First cross-section observation of an all solid-state lithium-ion “nanobattery” by tramsmission electron microscopy. Chem. Mater. 20, 2352 (2008)
8.Lux S.F., Schmuck M., Rupp B., Kern W., Appetecchi G.B., Passerini S., Winter M., Balducci A.Mixtures of ionic liquids in combination with graphite electrodes: The role of Li-salt. ECS Transactions 16, (35)45 (2009)
9.Lewandowski A., Świderska-Mocek A.Properties of the graphite-lithium anode in N-methyl-N-propylpiperidinium bis(trifluoromethanesulfonyl)imide as an electrolyte. J. Power Sources 171, (2)938 (2007)
10.Retoux R., Brousse T., Schleich D.M.High-resolution electron microscopy investigation of capacity fade in SnO2 electrodes for lithium-ion batteries. J. Electrochem. Soc. 146, (7)2472 (1999)
11.Delmas C., Maccario M., Croguennec L., Cras F.L., Weill F.Lithium deintercalation in LiFePO4 nanoparticles via a Domoni-Cascade model. Nat. Mater. 7, 665 (2008)
12.Gibot P., Casas-Cabanas M., Laffont L., Levasseur S., Carlach P., Hamelet S., Tarascon J.M., Masquelier C.Room-temperature single-phase Li insertion/extraction in nanoscale LixFePO4. Nat. Mater. 77, 741 (2008)
13.Laffont L., Delacourt C., Gibot P., Wu M.Y., Kooyman P., Masquelier C., Marie Tarascon J.Study of the LiFePO4/FePO4 two-phase system by high-resolution electron energy loss spectroscopy. Chem. Mater. 18, 5520 (2006)
14.Mauchamp V., Moreau P., Moncondut L., Doublet M.L., Boucher F., Ouvrard G.Determination of lithium insertion sites in LixTiP4 (x = 2–11) by electron energy-loss spectroscopy. J. Phys. Chem. C 111, 3996 (2007)
15.Wang D., Choi D., Yang Z., Viswanathan V.V., Nie Z., Wang C.M., Song Y., Zhang J.G., Liu J.Synthesis and Li ion insertion properties of highly crystalline mesoporous rutile TiO2. Chem. Mater. 20, 3435 (2008)
16.Hightower A., Ahn C.C., Fultz B., Rez P.Electron energy-loss spectroscopy on lithiated graphite. Appl. Phys. Lett. 77, (2)238 (2000)
17.Chen G., Li C., Xu X., Li J., Kolb U.Electronic structure of Li(CO0.7-xAl0.3)MgxO2 studied by electron energy-loss spectroscopy. Appl. Phys. Lett. 83, (6)1142 (2003)
18.Gabrisch H., Yazami R., Fultz B.The character of dislocationsin LiCoO2. Electrochem. Solid-State Lett. 5, (6)A111 (2002)
19.Nishimura S.I., Kobayashi G., Ohoyama K., Kanno R., Yashima M., Yamada A.Experimental visulization of lithium diffusion in LixFePO4. Nat. Mater. 7, 707 (2008)
20.Harutyunyan A.R., Chen G.G., Paronyan T.M., Pigos E.M., Kuznetsov O.A., Hewaparakrama K., Kim S.M., Zakharov D., Stach E.A., Sumanasekera G.U.Preferential growth of single-walled carbon nanotubes with metallic conductivity. Science 326, (5949)116 (2009)
21.Kim B.J., Tersoff J., Kodambaka S., Reuter M.C., Stach E.A., Ross F.M.Kinetics of individual nucleation events observed in nanoscale vapor-liquid-solid growth. Science 322, (5904)1070 (2008)
22.Hansen P.L., Wagner J.B., Helveg S., Rostrup-Nielsen J.R., Clausen B.S., Topsoe H.Atom-resolved imaging of dynamic shape changes in supported copper nanocrystals. Science 295, (5562)2053 (2002)
23.Shan Z.W., Mishra R.K., Asif S.A.S., Warren O.L., Minor A.M.Mechanical annealing and source-limited deformation in submicrometre-diameter Ni crystals. Nat. Mater. 7, (2)115 (2008)
24.Minor A.M., Asif S.A.S., Shan Z.W., Stach E.A., Cyrankowski E., Wyrobek T.J., Warren O.L.A new view of the onset of plasticity during the nanoindentation of aluminium. Nat. Mater. 5, (9)697 (2006)
25.Zheng H.M., Smith R.K., Jun Y.W., Kisielowski C., Dahmen U., Alivisatos A.P.Observation of single colloidal platinum nanocrystal growth trajectories. Science 324, (5932)1309 (2009)
26.Williamson M.J., Tromp R.M., Vereecken P.M., Hull R., Ross F.M.Dynamic microscopy of nanoscale cluster growth at the solid-liquid interface. Nat. Mater. 2, (8)532 (2003)
27.de Jonge N., Peckys D.B., Kremers G.J., Piston D.W.Electron microscopy of whole cells in liquid with nanometer resolution. Proc. Natl. Acad. Sci. U.S.A. 106, (7)2159 (2009)
28.Wang J.X., Liu D.F., Yan X.Q., Yuan H.J., Ci L.J., Zhou Z.P., Gao Y., Song L., Liu L.F., Zhou W.Y., Wang G., Xie S.S.Growth of SnO2 nanowires with uniform branched structures. Solid State Commun. 130, 89 (2004)
29.Pan Z.W., Dai Z.R., Wang Z.L.Nanobelts of semiconducting oxides. Science 291, 1947 (2001)
30.Courtney I.A., Dahn J.R.Electrochemical and in situ x-ray diffraction studies of the reaction of lithium with tin oxide composites. J. Electrochem. Soc. 144, 2045 (1997)
Recommend this journal

Email your librarian or administrator to recommend adding this journal to your organisation's collection.

Journal of Materials Research
  • ISSN: 0884-2914
  • EISSN: 2044-5326
  • URL: /core/journals/journal-of-materials-research
Please enter your name
Please enter a valid email address
Who would you like to send this to? *
×

Keywords:

Metrics

Full text views

Total number of HTML views: 2
Total number of PDF views: 221 *
Loading metrics...

Abstract views

Total abstract views: 406 *
Loading metrics...

* Views captured on Cambridge Core between September 2016 - 19th November 2017. This data will be updated every 24 hours.