The AMPIX electrochemical cell: a versatile apparatus for in situ X-ray scattering and spectroscopic measurements

Borkiewicz, Olaf J.; Shyam, Badri; Wiaderek, Kamila M.; Kurtz, Charles; Chupas, Peter J.; Chapman, Karena W.

doi:10.1107/S0021889812042720

The AMPIX electrochemical cell: a versatile apparatus for in situ X-ray scattering and spectroscopic measurements

Journal Article · Thu Nov 15 04:00:00 EST 2012 · Journal of Applied Crystallography

DOI:https://doi.org/10.1107/S0021889812042720· OSTI ID:1386775

Borkiewicz, Olaf J.; Shyam, Badri; Wiaderek, Kamila M.; Kurtz, Charles; Chupas, Peter J.; Chapman, Karena W.

This article presents a versatile easy-to-use electrochemical cell suitable forin operando,in situmeasurements of battery materials during electrochemical cycling using a variety of X-ray techniques. Argonne's multi-purposein situX-ray (AMPIX) cell provides reliable electrochemical cycling over extended periods owing to the uniform stack pressure applied by rigid X-ray windows and the formation of a high-fidelity hermetic seal. The suitability of the AMPIX cell for a broad range of synchrotron-based X-ray scattering and spectroscopic measurements has been demonstrated with studies at eight Advanced Photon Source beamlines to date. Compatible techniques include pair distribution function analysis, high-resolution powder diffraction, small-angle scattering and X-ray absorption spectroscopy. These techniques probe a broad range of electronic, structural and morphological features relevant to battery materials. The AMPIX cell enables experiments providing greater insight into the complex processes that occur in operating batteries by allowing the electrochemical reactions to be probed at fine reaction intervals with greater consistency (within the charge–discharge cycle and between different methodologies) with potential for new time-dependent kinetic studies or studies of transient species. Representative X-ray and electrochemical data to demonstrate the functionality of the AMPIX cell are presented.

Research Organization:: Energy Frontier Research Centers (EFRC) (United States). Northeastern Center for Chemical Energy Storage (NECCES)

Sponsoring Organization:: USDOE SC Office of Basic Energy Sciences (SC-22)

DOE Contract Number:: SC0001294

OSTI ID:: 1386775

Journal Information:: Journal of Applied Crystallography, Journal Name: Journal of Applied Crystallography Journal Issue: 6 Vol. 45; ISSN JACGAR; ISSN 0021-8898

Publisher:: International Union of Crystallography

Country of Publication:: United States

Language:: English

References (27)

Efficient simultaneous reverse Monte Carlo modeling of pair-distribution functions and extended x-ray-absorption fine structure spectra of crystalline disordered materials Németh, Károly; Chapman, Karena W.; Balasubramanian, Mahalingam The Journal of Chemical Physics, Vol. 136, Issue 7 https://doi.org/10.1063/1.3684547	journal	February 2012
In situ structural characterization of electrochemical systems using synchrotron-radiation techniques Marco, Roland De; Veder, Jean-Pierre TrAC Trends in Analytical Chemistry, Vol. 29, Issue 6 https://doi.org/10.1016/j.trac.2010.01.011	journal	June 2010
An In Situ Small-Angle X-Ray Scattering Study of Sodium Insertion into a Nanoporous Carbon Anode Material within an Operating Electrochemical Cell Stevens, D. A.; Dahn, J. R. Journal of The Electrochemical Society, Vol. 147, Issue 12 https://doi.org/10.1149/1.1394081	journal	January 2000
Dual Lithium Insertion and Conversion Mechanisms in a Titanium-Based Mixed-Anion Nanocomposite Dambournet, Damien; Chapman, Karena W.; Chupas, Peter J. Journal of the American Chemical Society, Vol. 133, Issue 34 https://doi.org/10.1021/ja204284h	journal	August 2011
A comparative study on structural changes of LiCo1/3Ni1/3Mn1/3O2 and LiNi0.8Co0.15Al0.05O2 during first charge using in situ XRD Yoon, Won-Sub; Chung, Kyung Yoon; McBreen, James Electrochemistry Communications, Vol. 8, Issue 8 https://doi.org/10.1016/j.elecom.2006.06.005	journal	August 2006
Nano-sized transition-metal oxides as negative-electrode materials for lithium-ion batteries Poizot, P.; Laruelle, S.; Grugeon, S. Nature, Vol. 407, Issue 6803, p. 496-499 https://doi.org/10.1038/35035045	journal	September 2000
Structural Evolution of Li[sub x]Mn[sub 2]O[sub 4] in Lithium-Ion Battery Cells Measured In Situ Using Synchrotron X-Ray Diffraction Techniques Mukerjee, S. Journal of The Electrochemical Society, Vol. 145, Issue 2 https://doi.org/10.1149/1.1838286	journal	January 1998
A Swagelok-type in situ cell for battery investigations using synchrotron radiation Nikolowski, Kristian; Baehtz, Carsten; Bramnik, Natalia N. Journal of Applied Crystallography, Vol. 38, Issue 5 https://doi.org/10.1107/S0021889805022302	journal	September 2005
A Cell for In Situ X-Ray Diffraction Based on Coin Cell Hardware and Bellcore Plastic Electrode Technology Richard, M. N. Journal of The Electrochemical Society, Vol. 144, Issue 2 https://doi.org/10.1149/1.1837447	journal	January 1997
In situ X-ray diffraction techniques as a powerful tool to study battery electrode materials Morcrette, M.; Chabre, Y.; Vaughan, G. Electrochimica Acta, Vol. 47, Issue 19 https://doi.org/10.1016/S0013-4686(02)00233-5	journal	July 2002
Nanomaterials for Rechargeable Lithium Batteries Bruce, Peter G.; Scrosati, Bruno; Tarascon, Jean-Marie Angewandte Chemie International Edition, Vol. 47, Issue 16, p. 2930-2946 https://doi.org/10.1002/anie.200702505	journal	April 2008
In situ X-ray diffraction and X-ray absorption studies of high-rate lithium-ion batteries Balasubramanian, M.; Sun, X.; Yang, X. Q. Journal of Power Sources, Vol. 92, Issue 1-2, p. 1-8 https://doi.org/10.1016/S0378-7753(00)00493-6	journal	January 2001
A continuous X-ray diffraction study of the electrochemical behavior of a plastic Li-ion cell Gérand, B.; Blyr, A.; Du Pasquier, A. Journal of Power Sources, Vol. 81-82 https://doi.org/10.1016/S0378-7753(99)00242-6	journal	September 1999
Nanostructured materials for advanced energy conversion and storage devices Aricò, Antonino Salvatore; Bruce, Peter; Scrosati, Bruno Nature Materials, Vol. 4, Issue 5, p. 366-377 https://doi.org/10.1038/nmat1368	journal	May 2005
Electrochemical in situ reaction cell for X-ray scattering, diffraction and spectroscopy Braun, A.; Shrout, S.; Fowlks, A. C. Journal of Synchrotron Radiation, Vol. 10, Issue 4 https://doi.org/10.1107/S090904950300709X	journal	June 2003
Modeling the Structure and Composition of Nanoparticles by Extended X-Ray Absorption Fine-Structure Spectroscopy Frenkel, Anatoly I.; Yevick, Aaron; Cooper, Chana Annual Review of Analytical Chemistry, Vol. 4, Issue 1 https://doi.org/10.1146/annurev-anchem-061010-113906	journal	July 2011
Microstructural defects in nanocrystalline iron probed by x-ray-absorption spectroscopy Di Cicco, Andrea; Berrettoni, Mario; Stizza, Sergio Physical Review B, Vol. 50, Issue 17 https://doi.org/10.1103/PhysRevB.50.12386	journal	November 1994
Interpretation of EXAFS Data Gurman, S. J. Journal of Synchrotron Radiation, Vol. 2, Issue 1 https://doi.org/10.1107/S0909049594009179	journal	January 1995
Glassy Carbon as an Absolute Intensity Calibration Standard for Small-Angle Scattering Zhang, Fan; Ilavsky, Jan; Long, Gabrielle G. Metallurgical and Materials Transactions A, Vol. 41, Issue 5 https://doi.org/10.1007/s11661-009-9950-x	journal	August 2009
Beyond Intercalation-Based Li-Ion Batteries: The State of the Art and Challenges of Electrode Materials Reacting Through Conversion Reactions Cabana, Jordi; Monconduit, Laure; Larcher, Dominique Advanced Materials, Vol. 22, Issue 35 https://doi.org/10.1002/adma.201000717	journal	August 2010
Orthorhombic LiMnO[sub 2] as a High Capacity Cathode for Li-Ion Cells Koetschau, I. Journal of The Electrochemical Society, Vol. 142, Issue 9 https://doi.org/10.1149/1.2048663	journal	January 1995
Structural and Mechanistic Revelations on an Iron Conversion Reaction from Pair Distribution Function Analysis Shyam, Badri; Chapman, Karena W.; Balasubramanian, Mahalingam Angewandte Chemie International Edition, Vol. 51, Issue 20 https://doi.org/10.1002/anie.201200244	journal	April 2012
Recent advances in rechargeable battery materials: a chemist’s perspective Palacín, M. Rosa Chemical Society Reviews, Vol. 38, Issue 9 https://doi.org/10.1039/b820555h	journal	January 2009
In Situ Energy Dispersive X-ray Diffraction Study of LiNi _0.8 Co _0.2 O ₂ Cathode Material for Lithium Batteries Ronci, F.; Scrosati, B.; Albertini, V. Rossi The Journal of Physical Chemistry B, Vol. 105, Issue 4 https://doi.org/10.1021/jp0024827	journal	February 2001
PDFfit2 and PDFgui: computer programs for studying nanostructure in crystals Farrow, C. L.; Juhas, P.; Liu, J. W. Journal of Physics: Condensed Matter, Vol. 19, Issue 33 https://doi.org/10.1088/0953-8984/19/33/335219	journal	July 2007
In Situ SAXS Studies of the Structural Changes of Sepiolite Clay and Sepiolite−Carbon Composites with Temperature Sandí, G.; Winans, R. E.; Seifert, S. Chemistry of Materials, Vol. 14, Issue 2 https://doi.org/10.1021/cm010627w	journal	February 2002
Simple cell for in situ X-ray absorption spectroelectrochemistry Farley, N. Electrochemistry Communications, Vol. 1, Issue 10 https://doi.org/10.1016/S1388-2481(99)00088-0	journal	October 1999

Similar Records

A radially accessible tubular in situ X-ray cell for spatially resolved operando scattering and spectroscopic studies of electrochemical energy storage devices

Journal Article · Fri Sep 16 00:00:00 EDT 2016 · Journal of Applied Crystallography (Online) · OSTI ID:1391936

The AUREX cell: a versatile operando electrochemical cell for studying catalytic materials using X-ray diffraction, total scattering and X-ray absorption spectroscopy under working conditions

Journal Article · Thu Sep 19 20:00:00 EDT 2024 · Journal of Applied Crystallography (Online) · OSTI ID:2447508

Recent advances in characterization of rechargeable battery materials via scanning probe microscopy

Journal Article · Mon Feb 17 19:00:00 EST 2025 · Journal of Materials Chemistry. A · OSTI ID:2500997

Related Subjects

energy storage (including batteries and capacitors)
defects
charge transport
materials and chemistry by design
synthesis (novel materials)

The AMPIX electrochemical cell: a versatile apparatus for in situ X-ray scattering and spectroscopic measurements

Citation Formats

References (27)

Similar Records

Related Subjects