Considerations in applying neutron depth profiling (NDP) to Li-ion battery research

Lyons, Daniel J.; Weaver, Jamie L.; Co, Anne C.

doi:10.1039/d1ta09639g

Cited by 9 publications

(8 citation statements)

References 32 publications

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Section: Resultsmentioning

confidence: 99%

“…Furthermore, electrochemical testing does not necessarily activate all the materials inside the sample, suggesting the observed capacity would not always match actual Li amount in cathode. [62] NDP results indicate an increased Li concentration at the LNMO/LiPON interface. One possible source of this increase is overlithiation of the LNMO surface.…”

Section: Concentration Gradient Across Lnmo/lipon Interfacementioning

confidence: 90%

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Unraveling the Stable Cathode Electrolyte Interface in all Solid‐State Thin‐Film Battery Operating at 5 V

Shimizu

Cheng

Weaver

et al. 2022

Advanced Energy Materials

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Spinel‐type LiNi0.5Mn1.5O4 (LNMO) is one of the most promising 5 V‐class cathode materials for Li‐ion batteries that can achieve high energy density and low production costs. However, in liquid electrolyte cells, the high voltage causes continuous cell degradation through the oxidative decomposition of carbonate‐based liquid electrolytes. In contrast, some solid‐state electrolytes have a wide electrochemical stability range and can withstand the required oxidative potential. In this work, a thin‐film battery consisting of an LNMO cathode with a solid lithium phosphorus oxynitride (LiPON) electrolyte is tested and their interface before and after cycling is characterized. With Li metal as the anode, this system can deliver stable performance for 600 cycles with an average Coulombic efficiency >99%. Neutron depth profiling indicates a slight overlithiated layer at the interface prior to cycling, a result that is consistent with the excess charge capacity measured during the first cycle. Cryogenic electron microscopy further reveals intimate contact between LNMO and LiPON without noticeable structure and chemical composition evolution after extended cycling, demonstrating the superior stability of LiPON against a high voltage cathode. Consequently, design guidelines are proposed for interface engineering that can accelerate the commercialization of a high voltage cell with solid or liquid electrolytes.

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Section: Resultsmentioning

confidence: 99%

Section: Concentration Gradient Across Lnmo/lipon Interfacementioning

confidence: 90%

Unraveling the Stable Cathode Electrolyte Interface in all Solid‐State Thin‐Film Battery Operating at 5 V

Shimizu

Cheng

Weaver

et al. 2022

Advanced Energy Materials

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“…NDP has been demonstrated to provide invaluable insights into Li transport and immobile Li growth that enables improved battery designs. [6][7][8][9] The concentration depth profile of 6 Li have been determined in LIB materials such as solid and liquid based electrolytes and electrodes. 9,10 The non-destructive nature of the technique has also allowed for relevant in situ and operando experiments for the LIB community such as varying the applied potential or current.…”

Section: Applications Of Ndp For Studying Lithium-ion Batteriesmentioning

confidence: 99%

“…[6][7][8][9] The concentration depth profile of 6 Li have been determined in LIB materials such as solid and liquid based electrolytes and electrodes. 9,10 The non-destructive nature of the technique has also allowed for relevant in situ and operando experiments for the LIB community such as varying the applied potential or current. 2,6,8,9,11 This study looked at a prospective electrolyte for an all-solid-state LIB, e.g., Li 6 PS 5 Cl 0.5 Br 0.5 .…”

Section: Applications Of Ndp For Studying Lithium-ion Batteriesmentioning

confidence: 99%

A demonstration study of lithium-ion battery by neutron depth profiling with a low flux neutron source

Wood,

Bisbee,

Maier

et al. 2023

Hard X-Ray, Gamma-Ray, and Neutron Detector Physics XXV

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Neutron Depth Profiling (NDP) is an analytical neutron technique that continues to grow in popularity for the quantification of Li ions in lithium-ion battery (LIB) materials. Most investigations occur at high flux neutron sources, i.e. cold or thermal neutron beam facilities, offered by high-power (10-20 MW) research reactors and employing multiple NDP energy and concentration standards. This work aims to develop a feasible method using NDP facilities with less intense neutron flux at lower power research reactors to quantitatively determine the Li concentration in LIB materials, while also applying a “thick” energy and concentration standard. Here, we describe a methodology for processing and calibrating NDP data collected using a multi-detector (i.e., 7-detector setup), which is essential to increase the detection efficiency. The Li concentration of a Li6PS5Cl0.5Br0.5 solid-state electrolyte was determined to be 2.2×1022 Li atoms cm−3. This value deviated by less than 3% of the expected Li atom concentration using a “thick” LiF single crystal wafer as a concentration standard. The method described in this work can be applied to other low-power reactors and other NDP-sensitive isotopes to further increase the application and availability of user-based NDP facilities.

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“…This breakthrough not only enabled the precise monitoring of lithium variations during the battery charging and discharging processes but also facilitated a deeper understanding of the electrochemical behavior within these batteries. Subsequently, the NDP technique has been widely employed for measurements in various fields such as lithium-ion batteries, semiconductors, and nuclear materials. − …”

Section: Introductionmentioning

confidence: 99%

Measurement of Nanoscale Film Thickness Using Neutron Depth Profiling Technique

Zhao

Xiao

Yao

et al. 2023

ACS Appl. Mater. Interfaces

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Determination of geometric parameters for thin film materials has always been a critical concern in scientific research. This paper proposes a novel approach for high-resolution and nondestructive measurement of nanoscale film thickness. In this study, the neutron depth profiling (NDP) technique was employed to accurately measure the thickness of nanoscale Cu films, achieving an impressive resolution of up to 1.78 nm/keV. The measurement results exhibited a deviation from the actual thickness of less than 1%, highlighting the accuracy of the proposed method. Additionally, simulations were conducted on graphene samples to demonstrate the applicability of NDP in measuring the thickness of multilayer graphene films. These simulations provide a theoretical foundation for subsequent experimental measurements, further enhancing the validity and practicality of the proposed technique.

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Considerations in applying neutron depth profiling (NDP) to Li-ion battery research

Abstract: Li distribution within micron-scale battery electrode materials is quantified with neutron depth profiling (NDP). This method allows the determination of intra- and inter-electrode parameters such as lithiation efficiency, electrode morphology...

Cited by 9 publications

References 32 publications

Unraveling the Stable Cathode Electrolyte Interface in all Solid‐State Thin‐Film Battery Operating at 5 V

Unraveling the Stable Cathode Electrolyte Interface in all Solid‐State Thin‐Film Battery Operating at 5 V

A demonstration study of lithium-ion battery by neutron depth profiling with a low flux neutron source

Measurement of Nanoscale Film Thickness Using Neutron Depth Profiling Technique

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