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2. Stabilized Nickel‐Rich‐Layered Oxide Electrodes for High‐Performance Lithium‐Ion Batteries.

Author

Ahaliabadeh, Zahra, Miikkulainen, Ville, Mäntymäki, Miia, Colalongo, Mattia, Mousavihashemi, Seyedabolfazl, Yao, Lide, Jiang, Hua, Lahtinen, Jouko, Kankaanpää, Timo, and Kallio, Tanja

Subjects
ATOMIC layer deposition, OXIDE electrodes, PROTECTIVE coatings, ELECTRIC vehicle batteries, ENERGY density
Abstract

Next‐generation Li‐ion batteries are expected to exhibit superior energy and power density, along with extended cycle life. Ni‐rich high‐capacity layered nickel manganese cobalt oxide electrode materials (NMC) hold promise in achieving these objectives, despite facing challenges such as capacity fade due to various degradation modes. Crack formation within NMC‐based cathode secondary particles, leading to parasitic reactions and the formation of inactive crystal structures, is a critical degradation mechanism. Mechanical and chemical degradation further deteriorate capacity and lifetime. To mitigate these issues, an artificial cathode electrolyte interphase can be applied to the active material before battery cycling. While atomic layer deposition (ALD) has been extensively explored for active material coatings, molecular layer deposition (MLD) offers a complementary approach. When combined with ALD, MLD enables the deposition of flexible hybrid coatings that can accommodate electrode material volume changes during battery operation. This study focuses on depositing TiO2‐titanium terephthalate thin films on a LiNi0.8Mn0.1Co0.1O2 electrode via ALD‐MLD. The electrochemical evaluation demonstrates favorable lithium‐ion kinetics and reduced electrolyte decomposition. Overall, the films deposited through ALD‐MLD exhibit promising features as flexible and protective coatings for high‐energy lithium‐ion battery electrodes, offering potential contributions to the enhancement of advanced battery technologies and supporting the growth of the EV and stationary battery industries. [ABSTRACT FROM AUTHOR]

Published
2024
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9. Understanding the Stabilizing Effects of Nanoscale Metal Oxide and Li–Metal Oxide Coatings on Lithium-Ion Battery Positive Electrode Materials

Author

Ahaliabadeh, Zahra, primary, Miikkulainen, Ville, additional, Mäntymäki, Miia, additional, Mousavihashemi, Seyedabolfazl, additional, Lahtinen, Jouko, additional, Lide, Yao, additional, Jiang, Hua, additional, Mizohata, Kenichiro, additional, Kankaanpää, Timo, additional, and Kallio, Tanja, additional

Published
2021
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18. TiO2 Photocatalyzed Oxidation of Drugs Studied by Laser Ablation Electrospray Ionization Mass Spectrometry

Author

Van Geenen, Fred A.M.G., Franssen, Maurice C.R., Miikkulainen, Ville, Ritala, Mikko, Zuilhof, Han, Kostiainen, Risto, Nielen, Michel W.F., Van Geenen, Fred A.M.G., Franssen, Maurice C.R., Miikkulainen, Ville, Ritala, Mikko, Zuilhof, Han, Kostiainen, Risto, and Nielen, Michel W.F.

Abstract

In drug discovery, it is important to identify phase I metabolic modifications as early as possible to screen for inactivation of drugs and/or activation of prodrugs. As the major class of reactions in phase I metabolism is oxidation reactions, oxidation of drugs with TiO2 photocatalysis can be used as a simple non-biological method to initially eliminate (pro)drug candidates with an undesired phase I oxidation metabolism. Analysis of reaction products is commonly achieved with mass spectrometry coupled to chromatography. However, sample throughput can be substantially increased by eliminating pretreatment steps and exploiting the potential of ambient ionization mass spectrometry (MS). Furthermore, online monitoring of reactions in a time-resolved way would identify sequential modification steps. Here, we introduce a novel (time-resolved) TiO2-photocatalysis laser ablation electrospray ionization (LAESI) MS method for the analysis of drug candidates. This method was proven to be compatible with both TiO2-coated glass slides as well as solutions containing suspended TiO2 nanoparticles, and the results were in excellent agreement with studies on biological oxidation of verapamil, buspirone, testosterone, andarine, and ostarine. Finally, a time-resolved LAESI MS setup was developed and initial results for verapamil showed excellent analytical stability for online photocatalyzed oxidation reactions within the set-up up to at least 1 h.

Published
2019

19. Intercalation of Lithium Ions from Gaseous Precursors into β-MnO2 Thin Films Deposited by Atomic Layer Deposition

Author

Nieminen, Heta-Elisa, primary, Miikkulainen, Ville, additional, Settipani, Daniel, additional, Simonelli, Laura, additional, Hönicke, Philipp, additional, Zech, Claudia, additional, Kayser, Yves, additional, Beckhoff, Burkhard, additional, Honkanen, Ari-Pekka, additional, Heikkilä, Mikko J., additional, Mizohata, Kenichiro, additional, Meinander, Kristoffer, additional, Ylivaara, Oili M.E., additional, Huotari, Simo, additional, and Ritala, Mikko, additional

Published
2019
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21. Effect of precursor chemistry on residual stress of ALD Al2O3 and TiO2 films

Author

Miikkulainen, Ville, Nieminen, Heta, Ylivaara, Oili, Mizohata, Kenichiro, Puurunen, Riikka L., and Ritala, Mikko

Subjects
Al203, Atomic Layer Deposition, ALD, TiO2, residual stress, precursors
Abstract

Deposited thin films carry residual stress that can be classified into two categories. One is thermal stress that results from differences in thermal expansion coefficients between the substrate and the film, and the other is so called intrinsic stress that is a result of the deposition process itself. Stress can be either compressive or tensile. In extreme case, films under excessive stress can lead to cracking, buckling or delamination of the film. In polycrystalline films, the residual intrinsic stress originates from morphology, such as grain coalescence, crystallization and phase transformation, and from impurities and voids, and development of these parameters during the deposition process. In amorphous films, residual stress also occurs but its sources are more difficult to elucidate. Residual stress of ALD films has been studied for example for Al2O3, TiO2, and the hybrid material alucone.1-4 These studies have focused on effects of deposition temperature, pulsing parameters, film thickness, and post-deposition annealing temperature. In the present paper we report results on how the precursor chemistry affects the residual stress of ALD Al2O3 and TiO2 films deposited at 250 °C to 50 nm thickness onto 150 mm Si wafers. We employed several metal precursors, such as AlMe3, AlCl3, TiCl4 and Ti(OiPr)4 as well as different oxygen sources (H2O, O3, CH3OH) and studied the effect of both the metal precursor and oxygen source on the residual stress of the deposited films. In addition to stress measurements, film characterization was done by X-ray diffraction, scanning electron microscopy and Time-of-Flight Elastic Recoil Detection Analysis for fundamental morphological and compositional properties. Characterization data will be discussed with the residual stress results. Notably large differences in the residual stress were found as a function of precursor chemistry, for both Al2O3 and TiO2.

Published
2016

27. TiO2Photocatalysis–DESI-MS Rotating Array Platform for High-Throughput Investigation of Oxidation Reactions

Author

Ruokolainen, Miina, Miikkulainen, Ville, Ritala, Mikko, Sikanen, Tiina, Kotiaho, Tapio, and Kostiainen, Risto

Abstract

We present a new high-throughput platform for studying titanium dioxide (TiO2) photocatalytic oxidation reactions by performing reactions on a TiO2-coated surface, followed by direct analysis of oxidation products from the surface by desorption electrospray ionization mass spectrometry (DESI-MS). For this purpose, we coated a round glass wafer with photocatalytically active anatase-phase TiO2using atomic layer deposition. Approximately 70 aqueous 1 μL samples can be injected onto the rim of the TiO2-coated glass wafer, before the entire wafer is exposed to UV irradiation. After evaporation of water, the oxidation products can be directly analyzed from the sample spots by DESI-MS, using a commercial rotating sample platform. The method was shown to provide fast photocatalytic oxidation reactions and analysis with throughput of about four samples per minute. The feasibility of the method was examined for mimicking phase I metabolism reactions of amodiaquine, buspirone and verapamil. Their main photocatalytic reaction products were mostly similar to the products observed earlier in TiO2photocatalysis and in in vitro phase I metabolism assays performed using human liver microsomes.

Published
2024
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30. Intercalation of Lithium Ions from Gaseous Precursors into β-MnO2Thin Films Deposited by Atomic Layer Deposition

Author

Nieminen, Heta-Elisa, Miikkulainen, Ville, Settipani, Daniel, Simonelli, Laura, Hönicke, Philipp, Zech, Claudia, Kayser, Yves, Beckhoff, Burkhard, Honkanen, Ari-Pekka, Heikkilä, Mikko J., Mizohata, Kenichiro, Meinander, Kristoffer, Ylivaara, Oili M.E., Huotari, Simo, and Ritala, Mikko

Abstract

LiMn2O4is a promising candidate for a cathode material in lithium-ion batteries because of its ability to intercalate lithium ions reversibly through its three-dimensional manganese oxide network. One of the promising techniques for depositing LiMn2O4thin-film cathodes is atomic layer deposition (ALD). Because of its unparalleled film thickness control and film conformality, ALD helps to fulfill the industry demands for smaller devices, nanostructured electrodes, and all-solid-state batteries. In this work, the intercalation mechanism of Li+ions into an ALD-grown β-MnO2thin film was studied. Samples were prepared by pulsing LiOtBu and H2O for different cycle numbers onto about 100 nm thick MnO2films at 225 °C and characterized with X-ray absorption spectroscopy, X-ray diffraction, X-ray reflectivity, time-of-flight elastic recoil detection analysis, and residual stress measurements. It is proposed that for <100 cycles of LiOtBu/H2O, the Li+ions penetrate only to the surface region of the β-MnO2film, and the samples form a mixture of β-MnO2and a lithium-deficient nonstoichiometric spinel phase LixMn2O4(0 < x< 0.5). When the lithium concentration exceeds x≈ 0.5 in LixMn2O4(corresponding to 100 cycles of LiOtBu/H2O), the crystalline phase of manganese oxide changes from the tetragonal pyrolusite to the cubic spinel, which enables the Li+ions to migrate throughout the whole film. Annealing in N2at 600 °C after the lithium incorporation seemed to convert the films completely to the pure cubic spinel LiMn2O4.

Published
2019
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32. TiO2 Photocatalysis--DESI-MS Rotating Array Platform for High-Throughput Investigation of Oxidation Reactions.

Author

Ruokolainen, Miina, Miikkulainen, Ville, Ritala, Mikko, Sikanen, Tiina, Kotiaho, Tapio, and Kostiainen, Risto

Subjects
*TITANIUM dioxide, *OXIDATION-reduction reaction, *PHOTOCATALYSIS, *DESORPTION electrospray ionization, *METABOLISM
Abstract

We present a new high-throughput platform for studying titanium dioxide (TiO2) photocatalytic oxidation reactions by performing reactions on a TiO2-coated surface, followed by direct analysis of oxidation products from the surface by desorption electrospray ionization mass spectrometry (DESI-MS). For this purpose, we coated a round glass wafer with photocatalytically active anatase-phase TiO2 using atomic layer deposition. Approximately 70 aqueous 1 μL samples can be injected onto the rim of the TiO2-coated glass wafer, before the entire wafer is exposed to UV irradiation. After evaporation of water, the oxidation products can be directly analyzed from the sample spots by DESI-MS, using a commercial rotating sample platform. The method was shown to provide fast photocatalytic oxidation reactions and analysis with throughput of about four samples per minute. The feasibility of the method was examined for mimicking phase I metabolism reactions of amodiaquine, buspirone and verapamil. Their main photocatalytic reaction products were mostly similar to the products observed earlier in TiO2 photocatalysis and in in vitro phase I metabolism assays performed using human liver microsomes. [ABSTRACT FROM AUTHOR]

Published
2017
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40. Studies of the Electrochemical Behavior of LiNi0.80Co0.15Al0.05O2 Electrodes Coated with LiAlO2

Author

Srur, Onit, Miikkulainen, Ville, Markovsky, Boris, Grinblat, Judith, Talianker, Michael, Fleger, Yafit, Cohen, Gili, Mor, Albert, Tal, Yosef, and, Yosef, and Aurbach, Doron

Abstract

In this paper, we studied the influence of LiAlO2 coatings of 0.5, 1 and 2 nm thickness prepared by Atomic Layer Deposition onto LiNi0.8Co0.15Al0.05O2 electrodes, on their electrochemical behavior at 30 and 60degC. It was demonstrated that upon cycling, 2 nm LiAlO2 coated electrodes displayed [?]3 times lower capacity fading and lower voltage hysteresis comparing to bare electrodes. We established a correlation among the thickness of the LiAlO2 coating and parameters of the self-discharge processes at 30 and 60degC. Significant results on the elevated temperature cycling and aging of bare and LiAlO2 coated electrodes at 4.3 V were obtained and analyzed for the first time. By analyzing of X-ray diffraction patterns of bare and 2 nm coated LiNi0.8Co0.15Al0.05O2 electrodes after cycling, we concluded that cycled materials preserved their original structure described by R-3m space group and no additional phases were detected.

Published
2017

47. Atomic layer deposition of functional films for Li-ion microbatteries.

Author

Nilsen, Ola, Miikkulainen, Ville, Gandrud, Knut B., Østreng, Erik, Ruud, Amund, and Fjellvåg, Helmer

Subjects
*ATOMIC layer deposition, *CONDUCTIVITY of electrolytes, *THIN films, *IONS spectra, *SOLID state batteries
Abstract

The lithium ion battery concept is a promising energy storage system, both for larger automotive systems and smaller mobile devices. The smallest of these, the microbatteries, are commonly based on the all-solid state concept consisting of thin layers of electroactive materials separated by a solid state electrolyte. The fact that solid state electrolytes are required puts rather severe constraints on the materials in terms of electronic and ionic conductivity, as well as lack of pinholes otherwise leading to self-discharge. The atomic layer deposition (ALD) technology is especially suitable for realization of such microbatteries for the Li-ion technology. ALD has an inherent nature to deposit conformal and pinhole free layers on complex geometrical shapes, an architecture most commonly adopted for microbattery designs. The current paper gives an overview of ALD-type deposition processes of functional battery materials, including cathodes, electrolytes, and anodes with the aim of developing all-solid-state batteries. Deposition of Li-containing materials by the ALD technique appears challenging and the status of current efforts is discussed. [ABSTRACT FROM AUTHOR]

Published
2014
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49. Atomic Layer Deposition of Spinel Lithium Manganese Oxide by Film-Body-Controlled Lithium Incorporation for Thin-Film Lithium-Ion Batteries

Author

Miikkulainen, Ville, Ruud, Amund, Østreng, Erik, Nilsen, Ola, Laitinen, Mikko, Sajavaara, Timo, and Fjellvåg, Helmer

Abstract

Lithium manganese oxide spinels are promising candidate materials for thin-film lithium-ion batteries owing to their high voltage, high specific capacity for storage of electrochemical energy, and minimal structural changes during battery operation. Atomic layer deposition (ALD) offers many benefits for preparing all-solid-state thin-film batteries, including excellent conformity and thickness control of the films. Yet, the number of available lithium-containing electrode materials obtained by ALD is limited. In this article, we demonstrate the ALD of lithium manganese oxide, LixMn2O4, from Mn(thd)3, Li(thd), and ozone. Films were polycrystalline in their as-deposited state and contained less than 0.5 at. % impurities. The chemical reactions between the lithium precursor and the film were found not to be purely surface-limited but to include a bulk component as well, contrary to what is usually found for ALD processes. In addition, we show a process for using Li(thd)/ozone and LiOtBu/water treatments to transform ALD-MnO2and ALD-V2O5into LixMn2O4and LixV2O5, respectively. The formed LixMn2O4films were characterized electrochemically and found to show high electrochemical capacities and high cycling stabilities.

Published
2014
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50. (Invited) ALD of Thin Films for Lithium-Ion Batteries

Author

Aaltonen, Titta, Miikkulainen, Ville, Bjarne, Knut, Pettersen, Anders, Nilsen, Ola, and Fjellvaag, Helmer

Abstract

Atomic layer deposition (ALD) technique is a thin film deposition method that provides highly conformal films on 3D structured supports, including powder materials. The technique relies on sequential self-limiting gas-to-surface reactions which enable control of thin film depositions even down to the atomic level on complex surface geometries. Even if ALD technique has been used in the semiconductor industry in production scale for several years now, there are rather few reports on ALD of battery materials. However, the recent development in processes for lithium containing films clearly opens up new possibilities. Promising applications of ALD include 3D structured all-solid-state batteries and surface modification of electrode powders. The present paper presents an overview of the present status in application of ALD in the field of lithium ion batteries.

Published
2011

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