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J Materiomics xxx (2017) 1e7

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J Materiomics

journal homepage: www.journals .e lsevier .com/journal-of -mater iomics/

High throughput materials research and development for lithium ionbatteries

Parker Liu a, Bingkun Guo b, Tanglin An c, Hui Fang c, Genxiang Zhu c, Chris Jiang a,Xiaoping Jiang a, c, *

a MTI Corporation, 860 South 19th Street, Richmond, CA 94804, USAb Shanghai University, 99 Shangda Road, Baoshan District, Shanghai 200444, Chinac Kejing Materials Technology Co. Ltd., 10 Kexueyuan Road, Hefei, Anhui 230088, China

a r t i c l e i n f o

Article history:Received 1 July 2017Received in revised form26 July 2017Accepted 28 July 2017Available online xxx

Keywords:High throughputMaterials synthesisLithium-ion battery

* Corresponding author.E-mail address: xpj@mtixtl.com (X. Jiang).Peer review under responsibility of The Chinese C

http://dx.doi.org/10.1016/j.jmat.2017.07.0042352-8478/© 2017 The Chinese Ceramic Society. Pcreativecommons.org/licenses/by-nc-nd/4.0/).

Please cite this article in press as: Liu P, et a(2017), http://dx.doi.org/10.1016/j.jmat.2017

a b s t r a c t

Development of next generation batteries requires a breakthrough in materials. Traditional one-by-onemethod, which is suitable for synthesizing large number of sing-composition material, is time-consuming and costly. High throughput and combinatorial experimentation, is an effective method tosynthesize and characterize huge amount of materials over a broader compositional region in a shorttime, which enables to greatly speed up the discovery and optimization of materials with lower cost. Inthis work, high throughput and combinatorial materials synthesis technologies for lithium ion batteryresearch are discussed, and our efforts on developing such instrumentations are introduced.© 2017 The Chinese Ceramic Society. Production and hosting by Elsevier B.V. This is an open access article

under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction

Ever since the first commercialization by Sony in 1991, lithiumion batteries(LIBs) have been ubiquitously used as power sourcesfor most of today's portable electronic devices, hand tools andelectric vehicles. Recently, LIBs have been considered as one of thebest candidates for large-scale energy storage applications due totheir high energy density, long service life and low environmentalimpact [1e4]. Although the overall performance of LIBs has beensignificantly improved compared to the original Sony LIBs, currentLIBs still cannot meet the growing demand in energy density andsafety.

Much effort has been put to further improve the performance ofLIBs. It is well recognized that searching for new electrode mate-rials is crucial. A number of Ni-base layered structure cathodes,such as LiNi0.8Co0.15Al0.05O2 (NCA) [5], LiNi1/3Mn1/3Co1/3O2(NMC-333) [6] and NMC-532 [7], have been widely studied and replacingCo with Ni results in a higher reversible capacity (over 200 mAh/g)and better structural stability. However, the reactivity of the highNi-content electrodes with electrolyte and the thermal instability

eramic Society.

roduction and hosting by Elsevie

l., High throughput material.07.004

at high charging state, which results in capacity fading and safetyissues, is still a concern [8]. For the anode materials, Si has beenconsidered as one of the most attractive anode materials because ofits high capacity (theoretical capacity: 4200mAh/g) and abundance[9]. However, Si suffers from rapid capacity fading due to largevolume expansion during lithiation, which hampers its application[10].

Next generation batteries with higher energy density, lowercost, better safety, and better environmental compatibility requirethe discovery of new electrode/electrolyte materials and rapidoptimization of processing techniques. Compared to traditionalone-by-one method, high-throughput experimentation enables tosynthesize and characterize a large number of compositionallyvarying samples in a very short time, which can speed up the dis-covery and optimization process of materials. In this work, highthroughput and combinatorial materials synthesis methods forlithium ion battery research are discussed, and our efforts on highthroughput instrumentation development are also introduced.

2. Thin film combinatorial methods

Thin-film synthesis is a typical technique to create combinato-rial libraries and composition spreads, which has been great de-velopments in the high-throughput materials synthesis [11]. Thepreparation process for thin-film samples typically contains two

r B.V. This is an open access article under the CC BY-NC-ND license (http://

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steps: deposition of multiple solid state materials as thin films invarying ratios on substrates and thermal processing of the samplesto mix the materials and form either stable or metastable com-pounds [12]. The combination of thin film deposition has beenremarked as the method of the combinatorial approach for batteryresearch.

Co-sputtering technique can be traced to early research on alloyphase diagram in the 1960s [13], which is a facile method to pre-pare gradient film without need of shadow masks. Whitacre et al.[14] fabricated hundreds of batch-fabricated cells with slightlydifferent cathode compositions using a co-sputtering technique(radio frequency planar magnetron sputter system) in less than 10work hours. To fabricate a compositional gradient, the substratewas placed between the two targets of LiMn2O4 and LiNiO2 duringdeposition, as shown in Fig. 1. After deposition, the substrates wereannealed for 30 min at 700 �C in air for inter-diffusion and crys-tallization of the cathode materials. Full test cells were subse-quently produced by sputtering LiPON electrolyte and evaporatingLi metal on the cathodes, respectively. The thin film cathodes hadsimilar structural and electrochemical properties as bulk-fabricatedpowder electrodes, which demonstrated that the combinatorialapproach may serve as a powerful tool in the discovery and opti-mization of the electrode materials.

Dahn et al. [15] developed a multi-target sputtering machinewith specially designed stationary masks and rotating substratetable, which can create two orthogonal compositional gradients onup to five substrates by rotating the substrate table. A broad rangeof negative electrode material, such as Al-Si-Sn and Si-Sn-Mn, havebeen produced by the modified sputtering machine and charac-terizedwith a 64-channel combinatorial cell. Ludwig et al. [16] useda similar combinatorial sputtering system as Dahn to fabricate Li-Ni-Mn-Co-O thin film library. Han et al. [17] developed a

Fig. 1. (a) Schematic of combinatorial sputter deposition process whereby two sputtercathodes of different compositions are used. A centrally located substrate leads to afilm with a variant composition. (b) Schematic of a 400 Si wafer with defined activecathode areas. The region examined in this study (three longest cell rows parallel todirection of composite variation) is indicated [14].

Please cite this article in press as: Liu P, et al., High throughput material(2017), http://dx.doi.org/10.1016/j.jmat.2017.07.004

sputtering system (AJA International) with five targets to create Li-Ni-Co-Mn-O thin film library in a single sample. A clear relationshipbetween mechanical properties and electrochemical cyclability forLi[NixCoyMnz]O2 was found and Li[Ni0.33Co0.30Mn0.34]O2 showedoptimized electrochemical and mechanical properties.

Besides sputtering technique, pulsed laser deposition (PLD)have been used for combinatorial synthesis. Matsumoto et al. [18]using PLD with a combinatorial moving mask synthesizedLi2CO3�CoO composition spread thin film, as shown in Fig. 2.Single-phase LiCoO2 thin film was obtained in a very narrowcomposition region and the LiCoO2 thin film with a stoichiometricLi:Co ratio exhibited a good electrochemical performance.

3. Combinatorial robot system

The combinatorial robot systems have been successfully appliedto find promising materials in the fields of pharmaceutical andbiomaterial. The automatic robot can ensure accuracy and repeat-ability in the experimental process, which is a suitable techniquefor oxide powder synthesis with liquid starting raw materials.

Yanase et al. [19] have developed a combinatorial robot systemfor LiCo1-xMnxO2 powder synthesis, as show in Fig. 3. The robot armwith an automatic micropipette (Fig. 3a) was used to dispense andmix starting solution or slurry materials. Themixture samples weredistributed to a sample plate, and subsequently dried and heated athigh temperature to produce the desired combinatorial samples.Carey and Dahn [20] used a combinatorial solutions-processingrobot for combinatorial study of the Li-Ni-Mn-Co oxide pseudo-quaternary system and nearly 800 distinct compositions wereprepared to screen for single-phase cathode materials. Takada et al.[21] used the similar method to create an electrode array with 16samples and evaluated them within 3 h.

Fujimoto et al. [22] developed a combinatorial electrostaticspray deposition system via combining a robot system with high-voltage power supply, as shown in Fig. 4. The liquid mixture ofstarting materials was fed into a stainless steel nozzle, which wasfixed on the robot arm and charged with a high-voltage, andatomized from the nozzle onto a substrate. A series of layered-typepseudo four-component Li-Ni-Co-Ti oxides were prepared by thecombinatorial preparation system and reaction phase diagramswere established.

Automatic robot systems have been also applied to the parallelpreparation and screening of cathode electrodes for optimizingcontents of binder and carbon black in lithium ion batteries[23a,23b]. The mixtures with desired ratio of active material,binder, acetylene black and cyclopentanone were used as inks, andwere distributed on the corresponding current collectors of a 64-channel cell by a Multiprobe II automated liquid handling system(Perkin-Elmer Life Sciences). 64-electrodes were cycled simulta-neously and results on the effect of carbon black in the electrodesmatched that of conventional experiments in the same condition,showing that the electronic percolation threshold is at 3% byvolume.

4. Our high throughput materials synthesis technologies

We have developed multiple combinatorial deposition systemsthat can be applied to new materials discovery for lithium ionbattery development. Our combinatorial magnetron sputteringsystem (Fig. 5a) with 5 independent sputtering sources (AC or DC)and a rotatable 16-sample mask, is designed for quinary thin filmdeposition for lithium ion battery cathode, anode, or solid elec-trolyte research [25]. Our combinatorial spray pyrolysis techniquecan be used for rapid screening of cathode materials and solidelectrolytes (Fig. 5b) [26]. Take inorganic-polymer composite

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Fig. 2. (a, b) Schematic illustration of the Li2CO3�CoO composition spread thin film and its optical microscope image (the white dotted lines indicate the edge of substrate clampsand the red crossed lines are the scale bar). (c) XRF Co Ka intensity variationwith the sample position X. (d) Out-of-plane XRD image plot. (e, f) XRD peak intensities of LCO(104) andCo3O4(400) normalized by that of STO(002) and their d-spacing values plotted against the sample position X. (g) Raman peak intensity variations of LCO (~593 cm�1) and Co3O4

(~689 cm�1) with the sample position X [18].

Fig. 3. Combinatorial robot system for mixing starting raw materials such as inorganic aqueous solution [19].

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electrolyte for example. By varying the ratio between polymerelectrolyte and ceramic electrolyte, a balance between compositeelectrolyte‘s electrical and mechanical properties can be achievedthrough the high throughput screening [24]. Various polymer

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hosts, liquid electrolytes, and solid inorganic electrolyte powdersuspensions are loaded into different channels of themulti-channelsyringe pump, and concurrently pumped and mixed at differentratios. The mixture is atomized by the ultrasonic spray nozzle, and

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Fig. 4. Schematic image (a) and photograph (b) of the M-ist Combinatory system based on an electrostatic atomization method [22].

Fig. 5. (a) 5-source combinatorial magnetron sputtering system. (b) Schematic of combinatorial spray pyrolysis system for rapid screening of battery materials.

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sprayed onto the heated stage with the assistance of the com-pressed gas. An adjustable aperture is mounted below the nozzle todefine the spray coating area. Beside the in-situ preparation at asingle temperature by the heating stage, the samples can be pro-cessed ex-situ at various temperatures with a high throughput tubefurnace, such as our 16-channel tube furnace up to 1100 �C, for

Please cite this article in press as: Liu P, et al., High throughput material(2017), http://dx.doi.org/10.1016/j.jmat.2017.07.004

rapid process optimization [27].A high throughput battery materials synthesis production line,

which incorporates high throughput dispensing, mixing/milling,pressing, heat processing, and coating, is developed by us (Fig. 6)[28]. Compared to the combinatorial thin film deposition or lowvolume powder synthesis techniques, this production line enables

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Fig. 6. Our high throughput materials synthesis production line, which includes high throughput dispensing, mixing/milling, pressing, heat processing, and coating.

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automatic, higher volume (several gram or ml) synthesis and pro-cessing of powder/slurry materials, and fabrication of cathode/anode foils or solid electrolyte discs in high throughput approaches.It allows newmaterial screening in a setting closer to practical use,such as in a crimped coin cell or in an assembled split cell.

Our high throughput materials synthesis production line savetime and labor, reduce operator fatigue, and minimize human er-rors. It consists of instruments for 5 processing steps:

(1) Dispense e high throughput, automatic dispensing of solidpowders and liquid precursors for electrode/electrolytepowder synthesis. For solid powder dispensing, four or morepowder dispensing heads and balances, with one dispensinghead for each material component, are integrated with acarousel type sample changer for automatic powderdispensing with varying ratios between different materialcomponents [29]. Up to 32 samples with�10 gweight can beprepared with 0.01 g resolution. For liquid dispensing, anautomatic pipette robot is integrated with a XYZ stage,enabling up to 96 samples preparation with �2 ml volumeand 0.2 ml resolution [30].

(2) Milling/Mixing e high throughput ball milling of the as-dispensed powder samples, and high throughput homoge-nizing of high viscosity cathode/anode slurry samples. With

Table 1Equipment capability of our high throughput materials synthesis production line.

Process Equipment Capability

Deposition 5-Target CombinatorialMagnetron Sputtering

5 sputtering targets with adtilt and 16-sample mask

6-Channel Combinatorial SprayPyrolysis

Automatic 6-source spray pysubstrate heating

Dispensing 32-Sample Powder Dispensing Automatic powder dispensin0.01 g resolution

96-Sample Liquid Dispensing Automatic liquid dispensing0.2 ml resolution

Milling/Mixing 16-Sample Planetary Ball Mill Planetary ball milling of 16 s6-Sample Planetary CentrifugalMixer

Planetary centrifugal mixing5 ml

Pressing 16-Position Hydraulic Press 10 ton electric hydraulic prerotary working plate

Heat Processing 4-Channel Tube Furnace Compact, atmosphere contro1700 �C with 100 OD tube

16-Channel Tube Furnace withQuenching

Atmosphere controlled quen1100 �C with 100 OD tube

Coating Tape Casting With 4-ChannelApplicator

Parallel 4-channel tape castiwidth) with 10 mm accuracy

Please cite this article in press as: Liu P, et al., High throughput material(2017), http://dx.doi.org/10.1016/j.jmat.2017.07.004

4 sets of 4 cavities milling jars, totally 16 parallel ball millingexperiments of 2ml samples can be carried out in a planetaryball mill machine [31]. Similarly, with two 3-syringe holders,the existing planetary centrifuge mixer can be modified intoa high throughput equipment, mixing 6 different high vis-cosity samples of 5 ml in one automatic run.

(3) Pressinge high throughput pellet pressing of cathode, anode,or solid electrolyte powders for sintering process. A 10 tonelectric hydraulic press is integrated with a carrousel typesample changer for high throughput pellet pressing. The as-prepared pellets are then placed inside tube furnace for heatprocessing in a controlled gas environment, or used for coincell assembly.

(4) Heating e multi-channel high temperature furnace with at-mosphere control for high throughput sintering, annealing,or quenching operations of electrode/inorganic solid elec-trolyte powder or pellets. The existing instruments includesa 16-channel tube furnace up to 1100 �C with 100 OD pro-cessing tubes and quenching options [27], and a compact,4-channel tube furnace up to 1700 �C with 100 OD processingtubes [32]. Up to 100 g sample can be heat processed in eachfurnace channel, either in a controlled gas environment or invacuum.

Ar GloveBox Compatibility

# of ParallelExperiment

# of Experimentin One Run

justable power and Yes 1 16

rolysis with 500 �C Yes 1 16

g up to 10 g with Yes 4 32

up to 2 ml with Yes 1 96

amples up to 2 ml Yes 16 16of 6 samples up to Yes 6 6

ss with 16-position Yes 1 16

lled furnace up to No 4 4

ching furnace up to No 16 16

ng (150 mm total Yes 4 4

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(5) Coating emulti-channel coating of electrode slurry or com-posite electrolyte slurry onto the foil substrate. With additionof a 4-channel film applicator, existing doctor blade coatercan bemodified into a high-throughput equipment [33]. Fourstrips of different slurry coatings can be fabricated in oneautomatic coating operation. The as-prepared coatings arethen passed onto heated roller press for solvent evaporationand thickness reduction, and coin cell die cutter for highthroughput preparation of cathode, anode, or flexible com-posite electrolyte discs.

5. Summary

In summary, high throughput and combinatorial materialssynthesis technologies for lithium ion battery research, includingthin film coating methods and combinatorial robot methods, arereviewed and discussed. Thousands of compounds with differentcompositions are able to be rapidly prepared for subsequent anal-ysis of physical and electrochemical properties in a short time bythese methods. Our high throughput capabilities of above-mentioned experimental instruments are summarized in Table 1,and discussed in terms of sample handling capacity, number ofparallel experiments, number of total experiments in one auto-matic operation, and Ar gas glove box compatibility. The Ar gasglove box compatibility is crucible for synthesis of moisture/ni-trogen sensitive battery materials, such as lithiummetal anode andLi-S solid electrolyte. These experimental instruments enable thescale-up transition from the low volume combinatorial materialssynthesis technique to a high throughput materials production linewhich includes dispensing, mixing/milling, pressing, heat pro-cessing, and coating. It further increases the productivity and re-duces time and cost for new material discovery of lithium ionbattery research.

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[25] Customized 5 heads RF plasma magnetron sputtering coater for MGI thin filmresearch. 2017. http://www.mtixtl.com/VTC-5RF.aspx.

[26] Bench-top automatic ultrasonic spray pyrolysis coating unit with 6” � 6”heating plate up to 500�C. 2017. http://www.mtixtl.com/MSK-USP-02.aspx.

[27] 16 channels tube furnace (1' O.D, 1100C Max.) for high throughput annealing& quenching research. 2017. http://www.mtixtl.com/GSL-1200X-MGI-16.aspx.

[28] High throughput research for Li-ion battery. 2017. http://www.mtixtl.com/highthroughputresearchforli-ionbattery.aspx.

[29] Automatic powder dispenser with analytical balance (1 mg - 5 g @ 0.05 mg)for high throughput solid dispensing up to 30 samples. 2017. http://www.mtixtl.com/ProgrammableLiquidDistributingStationwith18-Ports-MSK-18PE.aspx.

[30] High-throughput liquid distributing robot with 1mL pipette, microplates, tube& tip refilling racks. Laptop & Softw 2017. http://www.mtixtl.com/ProgrammableLiquidDistributingStationwith18-Ports-MSK-18PE.aspx.

[31] High throughput planetary ball mill with 16 channel SS milling jars (10ml/channel). 2017. http://www.mtixtl.com/MSK-SFM-13S.aspx.

[32] 4 channel compact tube furnace (1” alumina tube, 1700oC Max) for Hi-throughout annealing. 2017. http://www.mtixtl.com/GSL-1700X-MGI-4.aspx.

[33] Compact tape casting coater with vacuum chuck (8“Wx14”L), adjustable filmapplicator & optional dryer cover. 2017. http://www.mtixtl.com/CompactTapeCastingFilmCoater-MSK-AFA-III.aspx.

Dr. Chris Jiang received B.S and M.S. degrees in Metal-lurgy and Ph.D. degree in Materials Science and Engineerfrom Institute of Metal Research (IMR), Chinese Academyof Sciences near the end of last millennium. He hasworked in Max-Planck-Institute for Iron Research in Dus-seldorf, Germany(1year), Department of Metallurgy andMaterials Engineering in Catholic University Leuven,Belgium(3 years), and Department of Materials Scienceand Engineering in University of California at Davis(8years). Before joining MTI, he worked for a startup com-pany in silicon valley(2 years) as a senior Scientist and En-gineer focusing on scientific and engineering solutions tomass production challenges in energy storage application.He is currently in charge of R&D programs in MTICorporation.

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Dr. Bingkun Guo is a professor in the Materials GenomeInstitute at Shanghai University, China. He received hisPhD from the Institute of Physics, Chinese Academy ofSciences in 2009, which was followed by three yearspostdoctoral research at Oak ridge National Laboratory.After a postdoc at The University of Texas at Austin, Hejoined Shanghai University in 2015 and is working onsynthesis of nanostructured materials for energy storageapplication and solid lithium ion batteries.

Please cite this article(2017), http://dx.doi.o

Parker Liu received M.S. degree in Electrical Engineeringfrom San Jose State University in 2009. He is currentlyworking as the Manager of Technical Support Departmentin MTI Corporation.

Tanglin An is an Application Engineer in Kej-ing Materials Technology Co. Ltd. (KMT), whichis a division of MTI Corporation.

in pressrg/10.101

as: Liu P, et al., High throughput material6/j.jmat.2017.07.004

Hui Fang is a Chief Engineer in Kejing Materials Tech-nology Co. Ltd. (KMT), which is a division of MTICorporation.

s research and develop

Genxiang Zhu received M.S. degree in Materials Engi-neering from Hefei University of Technology in 2010. Heis currently working as the General Manager in KejingMaterials Technology Co. Ltd. (KMT), which is a divisionof MTI Corporation.

Dr. Xiaoping Jiang is a material scientist and founder ofMTI Corporation. He received Ph.D. degree in MaterialsScience and Engineer from Institute of Metal Research(IMR), Chinese Academy of Sciences in 1988, and trainedat Massachusetts Institute of Technology as a post-doctoral research associate from 1988 - 1991. Dr. Jianghad ~40 papers published in international journals. MTICorporation, which he found in California, USA, hasbeen producing advanced lab equipment for materialsresearch since 1994.

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