Calcination Heterogeneity in Li-Rich Layered Oxides: A Systematic Study of Li2CO3 Particle Size

Busse, Grace M.; Csernica, Peter M.; Lim, Kipil; Lee, Junghwa; Jiang, Zhelong; Rivera, Diego F.; Kim, Young Jin; Shapiro, David A.; Gent, William E.; Chueh, William C.

doi:10.1021/acs.chemmater.3c02404

Title: Calcination Heterogeneity in Li-Rich Layered Oxides: A Systematic Study of Li₂CO₃ Particle Size

Journal Article · 13 December 2023 · Chemistry of Materials

DOI: https://doi.org/10.1021/acs.chemmater.3c02404 · OSTI ID:2404886

^[1]; Csernica, Peter M. ^[2]; Lim, Kipil ^[3]; Lee, Junghwa ^[2];

^[4]; Rivera, Diego F. ^[2]; Kim, Young Jin ^[5]; Shapiro, David A. ^[6];

^[2];

^[7]

Stanford Univ., CA (United States); SLAC
Stanford Univ., CA (United States)
Stanford Univ., CA (United States); SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States). Stanford Institute for Materials and Energy Science (SIMES); SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States). Stanford Synchrotron Radiation Lightsource (SSRL)
Stanford Univ., CA (United States); SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States). Stanford Synchrotron Radiation Lightsource (SSRL)
Baden Aniline and Soda Factory (BASF) (Germany)
Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States). Advanced Light Source (ALS)
Stanford Univ., CA (United States); SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States). Stanford Institute for Materials and Energy Science (SIMES)

Li- and Mn-rich (LMR) layered oxide positive-electrode materials exhibit high energy density and have earth-abundant compositions relative to conventional Ni-, Mn-, and Co-oxides (NMCs). The lithiation of coprecipitated precursors is a key part of the synthesis and offers opportunities for tuning the properties of LMR materials. Whereas the morphology of transition metal precursors has received substantial attention, that of Li sources has not. Using Li_1.14Mn_0.57Ni_0.29O₂ as a model system, in this work, we establish a detailed understanding of LMR calcination pathways via in situ and ex situ diffraction, spectroscopy, microscopy, and thermogravimetry. Our work shows that a large Li₂CO₃ particle size modulates a previously misunderstood thermogravimetric feature present at the Li₂CO₃ melting point during layered oxide calcination and causes heterogeneity at larger length scales (inter-secondary particle) than previously reported (intra-secondary particle). We found that electrochemical performance is largely insensitive to this heterogeneity. Finally, this work highlights the sensitivity of layered oxide calcination pathways to synthesis conditions and suggests design rules to minimize calcination heterogeneity in layered oxides beyond LMR.

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Research Organization:: SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES). Materials Sciences & Engineering Division (MSE); USDOE Office of Science (SC), Basic Energy Sciences (BES). Scientific User Facilities (SUF)

Grant/Contract Number:: AC02-76SF00515

OSTI ID:: 2404886

Journal Information:: Chemistry of Materials, Journal Name: Chemistry of Materials Journal Issue: 24 Vol. 35; ISSN 0897-4756

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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Title: Calcination Heterogeneity in Li-Rich Layered Oxides: A Systematic Study of Li₂CO₃ Particle Size