Высокоэнергоемкие катодные материалы для литий-ионных аккумуляторов на основе модифицированных Ni-обогащенных слоистых оксидов переходных металлов (High-energy-density cathode materials for Li-ion batteries based on modified Ni-rich layered transition metal oxides) тема диссертации и автореферата по ВАК РФ 00.00.00, кандидат наук Орлова Елена Дмитриевна

• Орлова Елена Дмитриевна
• кандидат наук
• 2024

Оглавление диссертации кандидат наук Орлова Елена Дмитриевна

Table of contents

Introduction

Chapter 1. Literature review

1.1. Lithium-ion batteries and their market overview

1.2. High-energy-density cathode materials

1.3. Ni-rich layered transition metal oxides

1.3.1. Crystal and electronic structure of Ni-rich NMCs and their evolution

1.3.2. Reasons of Ni-rich NMC cathodes' electrochemical properties degradation

1.4. Approaches for Ni-rich NMCs modification

1.4.1. Cation doping

1.4.2. Surface coating

1.4.3. Core-shell and gradient structures

1.4.4. Grain boundaries modification

1.4.5. Microstructure engineering

1.5. Synthesis approaches

1.6. Literature review conclusions

Chapter 2. Methodology and techniques

2.1. Synthesis methods

2.2. Characterization methods

Chapter 3. Studying the co-precipitation synthesis conditions influence on Li+/Ni2+ cation disordering

in Ni-rich NMC at different spatial scales

Chapter 4. Composite cathode material based on NMC811 and Li2SO4 at the grain boundaries

Chapter 5. Composite cathode material based on NMC811 modified by boron

Chapter 6. Development of microwave-assisted hydrothermal synthesis

Chapter 7. Conclusions

List of symbols, abbreviations

Bibliography

Appendix A. Supplementary figures and tables

Acknowledgements

Введение диссертации (часть автореферата) на тему «Высокоэнергоемкие катодные материалы для литий-ионных аккумуляторов на основе модифицированных Ni-обогащенных слоистых оксидов переходных металлов (High-energy-density cathode materials for Li-ion batteries based on modified Ni-rich layered transition metal oxides)»

Introduction

The modern strategy for the development of megalopolises involves improving transport infrastructure and the environmental situation through the transition to ecologically friendly electric transport, as well as the rational use of energy resources through "smart" power grids, including large-scale energy storage systems. In that light, the development of high-energy, safe, and affordable batteries for a new generation is a challenging but essential task. Emerging demand for battery-electric (EVs) and hybrid-electric vehicles (HEVs) is currently covered by lithium-ion batteries (LIBs). As the electric cars industry constantly calls for faster charging and longer driving ranges, the elaboration of high energy-density cathodes is highly demanded because they are known to be a limiting factor in both the performance and cost of the battery.

Layered transition metal oxides of nickel, manganese, and cobalt with high nickel content, so-called Ni-rich NMC, are considered to be promising candidates for high-energy cathode materials, delivering a high practical capacity of ~200-210 mAh/g and energy density of more than 800 Wh/kg. However, electrodes with high Ni concentration have several drawbacks, such as fast capacity fade over the battery life and heat/gas release during electrochemical cycling, that obstacle the application of Ni-rich NMCs in commercial LIBs. Generally, limitations of Ni-rich NMC practical application are associated with oxygen evolution from Ni-rich NMC cathode materials, both during heating and electrochemical cycling, and irreversible structural changes, which represent a crucial and urgent scientific problem. Despite numerous chemical and engineering approaches aimed at the enhancement of Ni-rich NMCs electrochemical properties, the problem of finding the optimal way towards the modification of high-energy-density cathode materials is only partially solved, since the majority of proposed in literature methods provide only trade-off solutions, where enhancement of one electrochemical characteristic leads to deterioration of others. Besides, the modification route should be implemented in a sustainable and efficient way to enable large-scale production of such high-energy-density cathodes. Therefore, the present dissertation's aim is the development of a proper modification route for Ni-rich NMCs in order to controllably improve electrochemical properties such as capacity, stability, and rate capability.

The relevance of the dissertation lies in the fact that it addresses the existing Ni-rich NMCs' challenges to ensure their improvement through the robust and cost-effective synthetic routes, supplying the rapidly developing LIBs market with high-performance and cost-effective cathode materials for EVs and other electrochemical energy storage devices and systems.

To achieve the aim of the present dissertation, the following objectives of the present dissertation work were established:

1. Modified composite high-energy-density active cathode materials based on Ni-rich NMCs, synthesized by co-precipitation and microwave-assisted hydrothermal synthesis followed by high-temperature lithiation in different atmospheres;

2. Methodology of Li+/Ni2+ cation disordering assessment in Ni-rich NMCs at different spatial scales;

3. Correlations among synthesis conditions, micro- and macro-structure, and electrochemical properties for Ni-rich NMC cathode materials.

To achieve the goals, the methodology of the present research was identified, which corresponds to the main dissertation chapters:

1. Synthesis of Ni-rich NMC with composition LiNi0.8Mn0.1Co0.1O2 (NMC811) through hydroxide and carbonate co-precipitation from transition metal sulfates and acetates and annealing with lithium source in air or oxygen atmosphere;

2. Study the influence of co-precipitation synthesis conditions on Ni2+/Li+ cation disordering in Ni-rich NMC at different spatial scales;

3. Study of physicochemical and electrochemical properties of composite material based on NMC811 and Li2SO4 at the grain boundaries as a cathode material for Li-ion batteries;

4. Synthesis and study of physicochemical and electrochemical properties of composite material based on NMC811 modified by boron as a cathode material for Li-ion batteries;

5. Development of microwave-assisted hydrothermal synthesis for NMC811;

6. Synthesis and study of physicochemical and electrochemical properties of material based on mixed fractions of NMC811, prepared by co-precipitation and microwave-assisted hydrothermal synthesis, as a cathode material for Li-ion batteries.

The work used a combination of modern physicochemical methods of analysis: powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), transmission electron microscopy (selected area electron diffraction (SAED), electron diffraction tomography (EDT), high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM), electron energy loss spectroscopy (EELS), energy-dispersive X-ray spectroscopy (EDS)), X-ray photoelectron spectroscopy (XPS), thermogravimetry and differential thermal analysis (TG-DTA), mass-spectrometry with inductively coupled plasma (ICP-MS), galvanostatic cycling, electrochemical impedance spectroscopy (EIS). The obtained results are confirmed by theoretical calculations with density functional theory (DFT).

The following statements disclose the scientific novelty of the present dissertation work.

1. The Li+/Ni2+ cation disordering in Ni-rich NMC at unit cell scale was for the first time quantitatively assessed using atomic-resolution images treatment with model-based parameter estimation, the regions with different defects content were firstly computationally distinguished.

2. The composite materials of (1-x) LiNi0.8Mn0.1Co0.1O2 - x Li2SO4, where the amorphous Li2SO4 binder located at the grain boundaries and intergranular contacts, were for the first time synthesized, characterized by physicochemical methods and studied as cathode materials with enhanced electrochemical properties for lithium-ion batteries.

3. The misconception of boron doping, validated by computational and experimental methods, as well as direct visualization of Li3BO3 coating formation at plate-like primary particles of NMC811 cathode materials and its positive influence on the reversibility of high-voltage phase transitions were for the first time demonstrated.

4. For the first time, microwave-assisted hydrothermal synthesis was applied to NMC811 material, shortening its precursor fabrication time to less than one hour. The samples, synthesized by microwave-assisted hydrothermal synthesis, were for the first time characterized by physicochemical methods and studied as cathode materials for lithium-ion batteries and used as a space filler for enhancement of volumetric energy density of NMC811 cathode material for lithium-ion batteries.

The practical value of obtained results consists in that the studied composite materials based on NMC811 represent a highly promising high-energy-density cathode materials for next-generation lithium-ion batteries as they deliver enhanced electrochemical characteristics such as capacity, stability, and rate capability. Besides, the composites' fabrication procedure was optimized and requires no additional operation steps, making those composite cathode materials appealing for large-scale production. Elaborated fast and facile microwave-assisted hydrothermal synthesis for highly ordered and electrochemically efficient NMC811 enables the sufficient reduction of hydroxide precursors' production time to dozens of minutes. Additionally, the results of this study provide important guidelines for Li+/Ni2+ cation disordering assessment at different spatial scales, highlighting the influence of synthesis conditions on the redistribution of the regions with different defect content. So, the developed Li+/Ni2+ cation disordering assessment methodology could be used for further development of high-energy-density cathode materials, susceptible to cation defects formation, in particular, Ni-rich NMC with higher nickel content and LiNiO2.

The statements to be defended in the dissertation can be summarized as follows:

1. The reliable assessment methodology of Li+/Ni2+ cation disordering at bulk, submicron crystal and unit cell scales was established through comprehensive comparative analysis of semi-quantitative parameters, such as I003/I104 integral intensity ratio, c/V6a ratio and unit cell volume, and quantitative approaches, based on Rietveld refinement of powder X-ray diffraction, electron diffraction tomography

and analysis of atomic-resolution scanning transmission electron microscopy images using model-based parameter estimation.

2. High-energy-density composite cathode materials (1-x) LiNi0.8Mn0.1Co0.1O2 - x Li2SO4 (x < 0.005) for lithium-ion batteries, where amorphous Li2SO4 solid electrolyte binder is located at the grain boundaries and intergranular contacts of the primary crystallites, demonstrating growth in discharge capacity and capacity retention due to improved mechanical integrity and increased interfacial fracture toughness of the secondary agglomerates upon prolonged cycling.

3. High-energy-density boron-modified composite material for lithium-ion batteries, based on LiNi0.8Mn0.1Co0.1O2, with plate-like primary particles, coated by Li3BO3 1-2 nm, delivering high rate capability and enhanced capacity retention due to nearly radial alignment of lithium layers within the cathodes' agglomerates and better reversibility of the H2^H3 phase transitions.

4. The microwave-assisted hydrothermal synthesis followed by high-temperature lithiation of well-crystalline and low-defect LiNi0.8Mn0.1Co0.1O2 cathode material for lithium-ion batteries.

5. LiNi0.8Mn0.1Co0.1O2 cathode material for lithium-ion batteries, consisting of different fractions of materials, prepared by co-precipitation and microwave-assisted hydrothermal synthesis, with elevated tap density of 2.9 g/cm3 and volumetric energy density of 2100 mWh/cm3.

The author's personal contribution includes setting goals, planning experimental activities, and systematizing and analyzing literature data. The author has carried out synthesis, analysis of the crystal structure and composition of (1-x) LiNi0.8Mn0.1Co0.1O2 - x Li2SO4, boron-modified composite material, and LiNi0.8Mn0.1Co0.1O2, synthesized by microwave-assisted hydrothermal method, measurements of their electrochemical properties, processing, and interpretation of obtained scientific results. The author performed studies using modern methods of transmission electron microscopy, including atomic-resolution HAADF-STEM imaging, electron diffraction tomography, and electron energy loss spectroscopy. The author conducted a quantitative analysis of Li+/Ni2+ cation defects. The author participated in the preparation and presentation of oral and poster presentations at scientific conferences, writing articles for international peer-reviewed scientific journals.

The work was done at the Center for Energy Science and Technology of the Skolkovo Institute of Science and Technology. Assistance in the synthesis and characterization was provided by I. Skvortsova and Dr. A.A. Savina (Skolkovo Institute of Science and Technology, Moscow, Russia). Assistance in TEM measurements was provided by A.V. Morozov (Skolkovo Institute of Science and Technology, Moscow, Russia). The AFM study was done by Dr. S.Yu. Luchkin (Skolkovo Institute of Science and Technology, Moscow, Russia). TG-DTA-MS measurements were conducted by Dr. I.A. Trussov (Skolkovo Institute of Science and Technology, Moscow, Russia). Slice&View and EBSD images of boron-modified NMC811 were acquired by I.A. Moiseev (Skolkovo Institute of Science and Technology, Moscow, Russia). X-ray photoelectron spectra were measured by

E.M. Pazhetnov (Skolkovo Institute of Science and Technology, Moscow, Russia). The Li and B content via ICP-MS was studied by Dr. D.I. Petukhov (Lomonosov MSU, Moscow, Russia). Theoretical studies and DFT calculations were carried out by Dr. D.A. Aksyonov and Dr. A.O. Boev (Skolkovo Institute of Science and Technology, Moscow, Russia).

The validity and reliability of the results and conclusions are ensured using a wide range of complementary physicochemical and electrochemical methods of analysis as well as their consistency with literature data. The results reproducibility of electrode materials study in electrochemical cells was confirmed by conducting at least three experiment trials with high accuracy and precision. To validate electron microscopy studies, at least three crystals for each sample were investigated and at least three images for each crystal with different magnifications were acquired. The statements and conclusions formulated in the dissertation have received qualified approbation at international and national scientific conferences. The credibility is also confirmed by the publication of research results in peer-reviewed scientific journals. The dissertation materials were published in 14 works, including 5 articles in high-ranking international peer-reviewed scientific journals, 1 book chapter, 2 patents, and 6 abstracts at international and national scientific conferences.

List of conferences:

1. Orlova E.D., Savina A.A., Abakumov A.M. "High-energy cathode materials for lithium-ion batteries based on layered transition metal oxides with a low Li+/Ni2+ disorder". International scientific conference for undergraduate, graduate students and young scientists "Lomonosov-2021" (Lomonosov MSU, Moscow, Russia, April 12-23, 2021).

2. Orlova E.D. "Comprehensive study of Ni-rich NMCs synthesis conditions influence on Li+/Ni2+ antisite defects". International scientific student conference ISSC 2021 (NSU, Novosibirsk, Russia, April 12-23, 2021).

3. Orlova E.D., Savina A.A., Abakumov A.M. "Study of Li+/Ni2+ cation disordering by electron diffraction tomography". X National crystal chemistry conference (Kabardino-Balkarian republic, Russia, July 5-9, 2021).

4. Orlova E.D., Savina A.A., Abakumov A.M. "Composite cathode materials based on Ni-rich layered oxides for Li-ion batteries". IV Baikal materials science forum (Ulan-Ude, Lake Baikal, Russia, July 1-7, 2022).

5. Orlova E.D., Savina A.A., Abakumov A.M. "Quantitative local analysis of Li+/Ni2+ cation disordering in Ni-rich layered oxides". XXIX Russian Conference on Electron Microscopy (Moscow, Russia, August, 29-31, 2022).

6. Orlova E.D., Skvortsova I., Dolzhikova E.A., Sitnikova L.A. "Boron-modified cathode materials based on Ni-rich layered oxides for Li-ion batteries". International scientific student conference ISSC 2023 (NSU, Novosibirsk, Russia, April 17-26, 2023).

Список литературы диссертационного исследования кандидат наук Орлова Елена Дмитриевна, 2024 год

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