Intermittent Contact Alternating Current Scanning Electrochemical Microscopy: A Method for Mapping Conductivities in Solid Li Ion Conducting Electrolyte Samples

Intermittent contact alternating current scanning electrochemical microscopy (ic-ac-SECM) has been used to determine the electrochemical response to an ac signal of several types of materials. A conductive gold foil and insulating Teflon sheet were first used to demonstrate that the intermittent con...

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Main Authors: Samantha Raisa Catarelli, Daniel eLonsdale, Lei eCheng, Jaroslaw S Syzdek, Marca eDoeff
Format: Article
Language:English
Published: Frontiers Media S.A. 2016-03-01
Series:Frontiers in Energy Research
Subjects:
Online Access:http://journal.frontiersin.org/Journal/10.3389/fenrg.2016.00014/full
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author Samantha Raisa Catarelli
Daniel eLonsdale
Lei eCheng
Lei eCheng
Jaroslaw S Syzdek
Marca eDoeff
author_facet Samantha Raisa Catarelli
Daniel eLonsdale
Lei eCheng
Lei eCheng
Jaroslaw S Syzdek
Marca eDoeff
author_sort Samantha Raisa Catarelli
collection DOAJ
description Intermittent contact alternating current scanning electrochemical microscopy (ic-ac-SECM) has been used to determine the electrochemical response to an ac signal of several types of materials. A conductive gold foil and insulating Teflon sheet were first used to demonstrate that the intermittent contact function allows the topography and conductivity to be mapped simultaneously and independently in a single experiment. Then a dense pellet of an electronically insulating but Li-ion conducting garnet phase, Al-substituted Li7La3Zr2O12 (LLZO), was characterized using the same technique. The polycrystalline pellet was prepared by classical ceramic sintering techniques and was comprised of large (~150 μm) grains. Critical information regarding the contributions of grain and grain boundary resistances to the total conductivity of the garnet phase was lacking due to ambiguities in the impedance data. In contrast, the use of the ic-ac-SECM technique allowed spatially resolved information regarding local conductivities to be measured directly. Impedance mapping of the pellet showed that the grain boundary resistance, while generally higher than that of grains, varied considerably, revealing the complex nature of the LLZO sample.
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spelling doaj.art-e2f64a2b89594cefb4a317f0d57ce99c2022-12-21T20:36:18ZengFrontiers Media S.A.Frontiers in Energy Research2296-598X2016-03-01410.3389/fenrg.2016.00014185139Intermittent Contact Alternating Current Scanning Electrochemical Microscopy: A Method for Mapping Conductivities in Solid Li Ion Conducting Electrolyte SamplesSamantha Raisa Catarelli0Daniel eLonsdale1Lei eCheng2Lei eCheng3Jaroslaw S Syzdek4Marca eDoeff5Uniscan Instruments, LtdUniscan Instruments, LtdLawrence Berkeley National LaboratoryUniversity of California, BerkeleyBio-Logic USA LLCLawrence Berkeley National LaboratoryIntermittent contact alternating current scanning electrochemical microscopy (ic-ac-SECM) has been used to determine the electrochemical response to an ac signal of several types of materials. A conductive gold foil and insulating Teflon sheet were first used to demonstrate that the intermittent contact function allows the topography and conductivity to be mapped simultaneously and independently in a single experiment. Then a dense pellet of an electronically insulating but Li-ion conducting garnet phase, Al-substituted Li7La3Zr2O12 (LLZO), was characterized using the same technique. The polycrystalline pellet was prepared by classical ceramic sintering techniques and was comprised of large (~150 μm) grains. Critical information regarding the contributions of grain and grain boundary resistances to the total conductivity of the garnet phase was lacking due to ambiguities in the impedance data. In contrast, the use of the ic-ac-SECM technique allowed spatially resolved information regarding local conductivities to be measured directly. Impedance mapping of the pellet showed that the grain boundary resistance, while generally higher than that of grains, varied considerably, revealing the complex nature of the LLZO sample.http://journal.frontiersin.org/Journal/10.3389/fenrg.2016.00014/fullsolid electrolytegarnetLithium lanthanum zirconium oxideGrain boundaries.intermittent contact alternating current scanning electrochemical microscopy
spellingShingle Samantha Raisa Catarelli
Daniel eLonsdale
Lei eCheng
Lei eCheng
Jaroslaw S Syzdek
Marca eDoeff
Intermittent Contact Alternating Current Scanning Electrochemical Microscopy: A Method for Mapping Conductivities in Solid Li Ion Conducting Electrolyte Samples
Frontiers in Energy Research
solid electrolyte
garnet
Lithium lanthanum zirconium oxide
Grain boundaries.
intermittent contact alternating current scanning electrochemical microscopy
title Intermittent Contact Alternating Current Scanning Electrochemical Microscopy: A Method for Mapping Conductivities in Solid Li Ion Conducting Electrolyte Samples
title_full Intermittent Contact Alternating Current Scanning Electrochemical Microscopy: A Method for Mapping Conductivities in Solid Li Ion Conducting Electrolyte Samples
title_fullStr Intermittent Contact Alternating Current Scanning Electrochemical Microscopy: A Method for Mapping Conductivities in Solid Li Ion Conducting Electrolyte Samples
title_full_unstemmed Intermittent Contact Alternating Current Scanning Electrochemical Microscopy: A Method for Mapping Conductivities in Solid Li Ion Conducting Electrolyte Samples
title_short Intermittent Contact Alternating Current Scanning Electrochemical Microscopy: A Method for Mapping Conductivities in Solid Li Ion Conducting Electrolyte Samples
title_sort intermittent contact alternating current scanning electrochemical microscopy a method for mapping conductivities in solid li ion conducting electrolyte samples
topic solid electrolyte
garnet
Lithium lanthanum zirconium oxide
Grain boundaries.
intermittent contact alternating current scanning electrochemical microscopy
url http://journal.frontiersin.org/Journal/10.3389/fenrg.2016.00014/full
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