Electrochemical Synthesis of Sn-based Anode Materials in Li Secondary Batteries

Electrochemical Synthesis of Sn-based Anode Materials in Li Secondary Batteries

Li#+2-.Sn01*)("2,$&/%'

July, 2014

Moongook JEONG

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Electrochemical Synthesis of Sn-based Anode Materials in Li Secondary Batteries

Li #+2-. Sn 01*)("2,$&/%'

July, 2014

Waseda University

Graduate School of Advanced Science and Engineering Department of Applied Chemistry

Research on Applied Electrochemistry

Moongook JEONG

Supervisor: Prof. Dr. Tetsuya Osaka (Waseda University) Referees: Prof. Dr. Kazuyuki Kuroda (Waseda University)

Prof. Dr. Yoshiyuki Sugahara (Waseda University) Prof. Dr. Takayuki Homma (Waseda University) Prof. Dr. Toshiyuki Momma (Waseda University)

I sincerely appreciate their reviewing this dissertation.

Preface

Growing attention on rechargeable batteries has been accelerated due to its application for energy sources of portable electronics, such as mobile phone, lap top, camcorder and so on. Furthermore, the current issues on environment and energy problems have promoted a number of interests in the development on sustainable energy systems and green vehicles, which requires advanced rechargeable battery system for stable operation. Among various candidates for the rechargeable battery systems, lithium ion batteries (LIBs) have considered as the most attractive one since lithium metal is the lightest and the most electropositive (-3.04 V vs. SHE) metal, which accomplishes high energy density both the gravimetric (Wh kg^-1) and volumetric (Wh L^-1).

Since the LIBs were first commercialized in 1991, the conventional LIBs have been composed of transition metal oxide cathode and graphite anode. To meet the growing needs for development on LIBs delivering high energy density, a Sn based anode material has recently attracted attention as a promising candidate for an anode material substituting the graphite since it can reversibly alloy and dealloy with lithium, delivering fairly higher theoretical capacity (Li4.4Sn: 940 mAh g^-1) than that of graphite (C6Li: 372 mAh g^-1). However, there is profound drawback against its practical application for LIBs since the outstanding capacity rapidly fades within initial electrochemical charge/discharge process, causing poor cycle life. During cycling, enormous volume expansion (-400%) occurs with lithiation process followed by contraction after delithiation process, causing cracks on the active material. Finally, the electrode suffered from pulverization and peeling off of the active material from the substrate by further cycles, resulting in rapid capacity fade. Recently, many efforts to overcome the poor cycle life have focused on enduring the server volume change by introducing nano sized active material with free volume to effectively accommodate the expanded volume, multiphase active/inactive Sn-M (M = Co, Cu, Mn, Fe, Mg and so on) composite acting as a buffer matrix and composite with carbonaceous materials, i.e., carbon nanotubes, graphene, amorphous carbon, mesoporous carbon.

In previous work, electrochemical synthesis of the Sn-O-C composite anode was accomplished by the galvanostatic electrodeposition technique from an organic carbonate solvent, which delivered a discharge capacity of 465 mAh gof Sn-1after the 100th cycle showing 80% capacity retention against the first cycle. During the electrodeposition process, Sn deposition and decomposition of the organic carbonate solvent were

simultaneously carried out. Consequently, the Sn-O-C composite containing polycrystalline Sn phase surrounded by the decomposed products of an organic carbonate solvent with inter-particle void spaces was successfully achieved, and the unique structure would act as a buffer effectively enduring volume expansion, resulting in a stable cycle performance with high capacity. During the deposition process, a multi-plateau was observed in galvanostatic potential transients, which was derived from an increase in overpotential caused by variation on concentrations of active specie near the electrodes with a further deposition time. It is assumed that the varied overpotential resulted in different arising electrochemical reactions which probably influenced the unique structure of the Sn-O-C composite and its battery performances as an anode material.

In this thesis, the electrodeposition process of the Sn-O-C composite from organic carbonate solvent was suggested in order to comprehensively understand the electrochemical reactions where the different potential plateaus were obtained from the galvanostatic potential transients in the previous work. Comprehensive understanding on the electrodeposition process is required to synthesize the anode material showing desired properties such as high capacity, fine coulombic efficiency for Li secondary batteries. On the basis of the suggested deposition process, the Sn-O-C composite was prepared by potentiostatic deposition technique including three steps with controlling diffusion-layer thickness. The morphological and chemical characteristics of the Sn-O-C composite was able to be modified by implementing agitation of the electrolyte with simple magnetic stirring during the electrodeposition process, causing increase in initial capacity and coulombic efficiency.

Outline of this thesis is as follow.

Chapter 1 introduces history and its principles of development on LIBs, in particular Sn-based anode material. Furthermore, this chapter closely declares material properties and cycle performance of the Sn-O-C composite anode. Chapter 2 investigates electrochemical process of the Sn-O-C composite deposition process from organic carbonate solvent. The contribution of the deposition process on the anode performance is also thoroughly examined. Chapter 3 describes influence of the diffusion-layer thickness during electrodeposition on synthesis of nano Sn-O-C composite and their anode performances. Chapter 4 reports effect of electrolyte on cycle performances of the electrodeposited Sn-O-C composite as anode materials. Conclusion and future aspects are given in chapter 5.

Contents

Preface

Chapter 1 – General Introduction

1.1 Background 2

1.2 History of Development on Anode Materials 3

1.2.1 Drawbacks of Li metal anode 3

1.2.2 Emergence of Li ion batteries 5

1.2.3 Breakthrough of the conventional graphite anode material 5

1.3 Sn based anode material 12

1.3.1 Properties and characteristics of Sn based anode material 12

1.3.2 Sn-based oxide material 14

1.3.3 Sn-M intermetallic compound 16

1.3.4 Sn-M-carbon composite 18

1.4 Electrodeposited Sn based anode material 20 1.4.1 Electrochemical synthesis of Sn-based anode material 20 1.4.2 Electrodeposition of Sn-O-C composite form organic solvent 21

1.5 Summary 25

References 27

Chapter 2 – Analysis of an Electrodeposition process of Sn-O-C Composite from an Organic Electrolyte

2.1 Introduction 34

2.2 Experimental 36

2.3 Results and Discussion 38

2.3.1 Investigation on deposition mechanism 38

2.3.2 Anode performances dependent on deposition condition 53

2.4 Summary 59

References 60

Chapter 3 – Influence of the diffusion-layer thickness during electrodeposition on synthesis of nano core/shell Sn-O-C composite as an anode of Li secondary batteries

3.1 Introduction 64

3.2 Experimental 66

3.3 Results and Discussion 68

3.3.1 Influences of electrolyte agitation 68

3.3.2 Material properties 71

3.3.3 Electrochemical anode performances 83

3.3.4 Electrochemical investigation on lithiation/delithiation reaction 85

3.4 Summary 91

References 92

Chapter 4 – Effect of electrolyte on cycle performances of the electrodeposited Sn-O-C composite anode of Li secondary batteries

4.1 Introduction 96

4.2 Experimental 98

4.3 Results and Discussion 100

4.3.1 Electrochemical anode performances 100

4.3.2 Electrochemical behaviors 101

4.3.3Material characteristics 104

4.4 Summary 108

References 109

Chapter 5 – General Conclusion

5.1 Conclusions 112

5.2 Future aspects 114

List of Achievement

Acknowledgement

Chapter 1:

General Introduction

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Table 1.2.24IFOG?=B;HA?I@;FFIS;HI>?G;N?LC;FM>OLCHA=S=FCHAI@NB?@OFF=;J;=CNS 1JLCHA?L L?JLCHN?>QCNBJ?LGCMMCIH

3 HFCNBC;N?>=IGJIOH> * CNBC;N?>=IGJIOH> 4IFOG?=B;HA?

F * C F

C * C. C

! > * C.! >

.< * C/)/.<

1H * C/)/1H

1C * C/1C

8H * C8H

! * C!1

'HMJCN? I@NB? =LCNC=;F>CG?HMCIH;FCHMN;<CFCNSL?MOFNCHACHJIIL=S=F?FC@? NB? * C

;FFIS G;N?LC;FM Q?L? MNCFFL?A;L>?> ;M ;NNL;=NCP? =;H>C>;N?M IQCHA NI NB?CLBCAB =B;LA?

>?HMCNS @;CLFS@CH? * C^&GI<CFCNSCH* CLC=BJB;M?M ;H>;==?JN;<F? =OLL?HN>?HMCNS>OLCHA

=B;LA?>CM=B;LA? =S=F? ^{,4' .4(/,} 2 B?L?@IL? ; HOG<?L I@ L?M?;L=B?M NI IP?L=IG? NB?

>CG?HMCIH;FCHMN;<CFCNSB;M ;NN?GJN?> 2 B? >CG?HMCIH;FMN;<CFCNSI@* C ;FFISG;N?LC;FM CM MCAHC@C=;HNFS ;@@?=N?> @LIG NB?CL G?N;FFOLAC=;F MNLO=NOL? ;H> GILJBIFIAS ^/-(/0 2 BOM NBC=E F;S?L?F?=NLI>? CM CHMO@@C=C?HNFS @F?RC<F? =;OMCHA G?=B;HC=;F>?AL;>;NCIH >OLCHA

=S=FCHA 2 BCH F;S?L =IGJIM?> I@ MG;FF J;LNC=F? MCT? QCNB MO<GC=LI IL H;HIG;N?LC;FM CM L?A;L>?> ;M IH? ;JJLI;=B NI MOJJL?MM NB? G?=B;HC=;F>?AL;>;NCIH 'H NBCM =;M? NB? IP?L;FFP;LC;NCIHIHNB? J;LNC=F? >CG?HMCIHM =;H<? GCHCGCT?> =;OMCHANI MOJJL?MMJ;LNC=F?=L;=ECHA;H>JOFP?LCT;NCIH$ CA

HINB?L ;JJLI;=B NI ?H>OL? >CG?HMCIH;F CHMN;<CFCNS CM NI MSHNB?MCM G;NLCR

=IGJIMCN? I@* C ;FFISM QCNBF?MM ;=NCP? ILHIH;=NCP? G;N?LC;F^/. =IH>O=NCP? JIFSG?L

;JILIOM G?G<L;H?^/3 ;H CH?LNG?N;F=IGJIMCN?^.. IL;HINB?LG;NLCR=IH>O=NIL^/4 Q?L? =IHMC>?L?>;M =;H>C>;N?M @ILNB? MOCN;<F? G;NLCRG;N?LC;F $ CA CM NB? M=B?G?

MBIQCHA NB? C>?; BIQ NB? G;NLCR G;N?LC;F J?L@ILGM NI MOJJL?MM NB? >CG?HMCIH;F

>?AL;>;NCIH >OLCHA =S=FCHA ;MC=;FFS NB? L?;=N;HNJB;M? CH CHN?L G?N;FFC= =IGJIMCN?

OH>?LAI?M PIFOG? =B;HA? <S ;==?JNCHA * C^& CIHM 5 BCF? INB?LJB;M?M CH NB? =IGJIMCN?

;L? CH;=NCP? ILF?MM ;=NCP? ;A;CHMN* C^& CIHM QBC=B F?NM NB?G J?L@ILG?> <O@@?L;A;CHMN PIFOG? ?RJ;HMCIH >OLCHA =S=FCHA^,4' $ CH? >CMJ?LMCIH I@ NB? MG;FFJ;LNC=F? MCT? I@

Fig. 1.2.4+ I>?F MNFCNBC;NCIHCM MN;FFISCHAQCNBFCNBCOG I@;FIIM?FSJ;=E?>MG;FFJ;LNC=F?MCT?

G?N;FFC=G;N?LC;F #P?H #FM?PC?L L?JLCHN?>QCNBJ?LGCMMCIH ^/0

NB? L?;=N;HNG;N?LC;FCHNB? G;NLCR=IGJIMCN? CM JL?@?L;<FSL?KOCL?>CHIL>?LNI?HB;H=?

NB??@@?=NMI@CHN?LG?N;FFC=G;NLCR=IGJIMCN?^/0

* C ;FFISG;N?LC;FM MO=B;M MCFC=IH^0,ILMCFP?L^0-=IGJIMCNCHAQCNB=;L<IH;=?IOM G;N?LC;FM Q?L? ;FMI MOAA?MN?> ;M ;H ?@@?=NCP? MIFONCIH NI IP?L=IG? PIFOG? =B;HA?

JLI<F?G @ILCGJLIP?G?HNI@=S=F?FC@?

+ ?;HQBCF? HIP?FNCH<;M?> ;HI>? G;N?LC;FM C? NCH =IGJIMCN? IRC>? 2 ! - AF;MM QBC=B Q;M L?JILN?> <S $ ODC@CFG ! ?FFN?=B ! I * N> B;> L?=?CP?> =IHMC>?L;<F?

;NN?HNCIH >O? NI CNM @;CLFS MN;<F? =S=F? FC@? IONMN;H>CHA L?P?LMC<F? =;J;=CNS QCNB <INB AL;PCG?NLC=;F BEA^(, ;H>PIFOG?NLC= B* ^(, QBC=B;L? GIL? NB;H NQC=? =IGJ;L?> NI =IHP?HNCIH;FAL;JBCNC= =;L<IH ;HI>? $ CA = ^0. '>IN;-; )3 L?JILN?> ;GILJBIOM MN;N? I@ AF;MMS G;N?LC;FMBIQCHA S?FFIQCMB =IFILQCNB @ILGOF;I@

Md,)+<+)01J+)/+FW+)/-I.)1 MI=;FF?> 2 ! - ;M MBIQH CH $ CA ; ;H> < 2BCM

;GILJBIOM MNLO=NOL? G;CHFS =IHMCMNM I@ 1H ;H> IRSA?H <IH>CHA QCNB INB?L AF;MMS

?F?G?HNM 2 B? 1H J?L@ILGM ;M ; L?;=N;HNJB;M? NI ;FFIS>?;FFIS QCNB * C^& CIHM QBC=B L?MOFNM CH BCAB =;J;=CNS 2 B? IRSA?H <IH>CHA FCGCNM 1H =FOMN?LM MCT? QBC=B =;OM?M @;MN

* CCIH >C@@OMCIH ;H> >?FI=;FCT?M NB? 1H L?;=N;HNJB;M?^0/ M NB? L?MOFN NB?S ;=BC?P?>

L?G;LE;<F?=S=F?L?N?HNCIHMBIQCHA;JJLIRCG;N?FS ;@N?LNB? NB=S=F?;A;CHMNNB?

MN=S=F? $ CA > & IQ?P?L NB? 2 ! - MBIQ?> JIILCHCNC;F=IOFIG<C= ?@@C=C?H=S NB;H=LSMN;FFCH?NCH<?=;OM?I@CLL?P?LMC<F?L?;=NCIHNI@ILG * C-- @LIG 1H- ^0/

Fig. 1.2.5+ I>?F MNLIHA?RJ;HMCIHMI@NB?VL?;=N;HNW>IG;CHM>O?NIFCNBC;NCIH=;H<?<O@@?L?Z

<SNB? CH;=NCP? ILF?MM ;=NCP? VG;NLCRW >IG;CHM NBOM E??JCHANB? ?RN?HNI@=L;=E@ILG;NCIHCd NB?IP?L;FFGOFNCJB;M?G;N?LC;FMG;FF #FM?PC?L L?JLCHN?>QCNBJ?LGCMMCIH ^{/0' 0+}

Fig. 1.2.6 ; OFE NCH<;M?> =IGJIMCN? IRC>? 2 ! - ;=NCP? G;N?LC;FF?@N 'NCM ;S?FFIQCM^ NL;HMJ;L?HNAF;MM QCNB ;>?HMCNS I@ A=G^. ! LOMBCHA NB? AF;MM JLIPC>?M ;QBCN? JIQ>?LI\

;=NCP? G;N?LC;F LCABN =;J;<F? I@ * C CHM?LNCIH @IL OM? CH NB? H?A;NCP? ?F?=NLI>? I@ * CCIH L?=B;LA?;<F?<;NN?LC?M < 2 B?RL;S>C@@L;=NCIHMJ?=NLOGI@2 ! - OH>?L! O) ;L;>C;NCIH - HFS

;Q?;E>C@@L;=NCIH>CMNLC<ONCIHCMI<M?LP?>QCNB;J?;E;N+ \ NI \ QBC=BCM;=B;L;=N?LCMNC=

I@1H- =IHN;CHCHAAF;MM;H>L?@F?=NM;>CMNLC<ONCIHI@1H1H>CMN;H=?MCHNB?;HCMINLIJC=G;NLCR

= ! S=FCHA I@ ?F?=NLI=B?GC=;F * C CHM?LNCIH =B;LA? ;H> L?F?;M? >CM=B;LA? IH 2 ! -

$Md,)+<+)01J+)/+;b+)/-I.)1 ;N;=IHMN;HN=OLL?HNI@ G J?L GAI@2 ! - =IH>O=N?>;NLIIc N?GJ?L;NOL?<?NQ??HNB?PIFN;A?FCGCNMI@ 4 CHM?LNCIH ;H> 4 L?F?;M? P?LMOM;* C =IOHN?h

?F?=NLI>? > ! S=F;<CFCNSI@;2! - ;HI>? #! "#! * C.$ * C! I--=;NBI>? XLI=ECHA=B;CLY NSJ?I@<;NN?LSMIFC>FCH? 2 B?<;NN?LSQ;M=B;LA?>CM=B;LA?=S=F?>IP?L;=?FFPIFN;A?QCH>IQ I@<?NQ??H 4 =B;LA? ;H> 4 >CM=B;LA? ;N;=IHMN;HN=OLL?HN=ILL?MJIH>CHANI ! 2B? G?LC=;H MMI=C;NCIH@ILNB? >P;H=?G?HNI@1=C?H=? L?JLCHN?>QCNBJ?LGCMMCIH ^0.

1H<;M?>;HI>?G;N?LC;F

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2CH >?FCP?LM BCAB =;J;=CNS I@ <INB AL;PCG?NLC= ;H> PIFOG?NLC= ;M ;H ;HI>?

G;N?LC;FCH* ' M $ CA ;H> 2;<F? ^-- 'H J;LNC=OF;L CNM PIFOG?NLC==;J;=CNS

;<ION G B=G^(. CM ?P?HBCAB?LNB;H* C G?N;F;H>=IGJ;L;<F? NI1C^./(.2 5 B?H G?N;FFC=NCH?F?=NLI=B?GC=;FFSL?;=NM QCNB* C CNA?H?L;FFSI<N;CHM P;LCIOM JB;M?M MO=B;M F_-Md0 * C1H * C2Md. * C0Md- * C,.Md0 * C2Md- ;H>* C--Md0 $ CA ;H> N NB? @OFFS FCNBC;N?> MN;N? NB? G;RCGOG AL;PCG?NLC= =;J;=CNS ;H> QILECHA JIN?HNC;F

=ILL?MJIH> NI G B A^(, ;H> ;<ION 4 PM * C* C^& L?MJ?=NCP?FS^0/ & IQ?P?L ;M

;@IL?G?HNCIH?> CNMO@@?LM@LIG M?LP?LPIFOG?=B;HA?L?MOFNCHACHJIIL=S=F?FC@? QBC=B B;>?R;GCH?><SCHMCNO;NIGC=@IL=?GC=LIM=IJS $ + ⁰¹;H>MNL?MMG?;MOL?G?HNM⁰²

Fig. 1.3.1* C1HJB;M?>C;AL;G 1JLCHA?L L?JLCHN?>QCNBJ?LGCMMCIH ⁰⁰

Fig. 1.3.2 ! B;L;=N?LCMNC= =B;LA? =OLP? I@ ?F?=NLIJF;N?> 1H CH + * C! F-/.! M G =G^(-)

#FM?PC?L L?JLCHN?>QCNBJ?LGCMMCIH ^/0

Fig. 1.3.3.FINMMBIQCHA>CG?HMCIH;F=B;HA?M I@; =B;HA?CH;L?; < J?L=?HN;A?=B;HA?CH B?CABN = J?L=?HN;A?=B;HA?CHPIFOG?I@NB?

MCHAF? J;NN?LH?> MJINI@ 1H<;M?> ;HI>? ;HZ

> =?FFPIFN;A? PM <INB NCG? ;H> $ + M=;H HOG<?L;H;FST?>@LIG5 : 1;< $ + N?=BHCKO?

2 B? #F?=NLI=B?GC=;F 1I=C?NS ;ME?> @Ih L?JLCHNCHAQCNBJ?LGCMMCIH ⁰¹

1H<;M?>IRC>?G;N?LC;F

1CH=? >CM=IP?LS I@ 2 ! - <S $ ODC@CFG ! ?FFN?=B ! I * N> ^0. 1H<;M?> IRC>?

G;N?LC;FM =IHN;CHCHA1H- IL1H--B;P? L?=?CP?>;FINI@;NN?HNCIH;M ;JLIGCMCHA;HI>?

G;N?LC;F 'NM<;MC=?F?=NLI=B?GC=;FL?;=NCIHCMCH>C=;N?>CH#KO;NCIH ;H> ^0/

MdI- * C^& ?⁽(1H * C-- * C^& ?⁽( B=B C $ @ E#!%!#F 1H- * C^& ?⁽(1H * C-- * C^& ?⁽( B=B C @ E#!%!$F

2 B? IRSA?H <IH>?> NI 1H CM L?F?;M?> <S NB? CHM?LN?> * C^& CIHM ;H> ?F?=NLIHM QBC=B CLL?P?LMC<FS @ILGM * C-- JB;M?M FFIS>?;FFIS L?;=NCIH <?NQ??H NB? >CMMI=C;N?>

G?N;FFC=1H;H>* C^&CM L?P?LMC<FS=;LLC?>IONNI@ILG * Cn1HJB;M? $R$ L?;FCTCHA BCAB NB?IL?NC=;F =;J;=CNS ⁰³ 1CH=? NB? ?F?=NLI=B?GC=;FFS HIH;=NCP? * C-- JB;M?M ;L?

@CH?FS>CMJ?LM?>QCNBCHNB?G?N;FFC=1HJB;M? NB?* C-- JB;M?M=;H?@@C=C?HNFSJ?L@ILG ;M

<O@@?LG;NLCR QBC=B =;H ?H>OL? NB? PIFOG? =B;HA? M NB? L?MOFN NB? 1H<;M?> IRC>?

G;N?LC;F=;H;=BC?P? CGJLIP?G?HNI@=S=F? L?N?HNCIH=IGJ;L?>NIG?N;FFC=1H;HI>?^0/

& IQ?P?L >OLCHA @OLNB?L=S=F?M NB? G?N;FFC= 1H JB;M?M ;AAL?A;N? ?;=B INB?L =;OMCHA F;LA? MCT? J;LNC=F?M $ OLNB?LGIL? NB? * C-- G;NLCR JB;M?M MOLLIOH>CHA G?N;FFC= 1H ;L?

>?MNLIS?><SNB??HF;LA?>1HJ;LNC=F?M $ CH;FFS NB?=S=F?FC@?CM>?N?LCIL;N?>⁰⁴

+ ?;HQBCF? CN Q;M @IOH> NB;N JBSMC=;F GI>C@C=;NCIH QIOF> <? ?@@?=NCP? NI CGJLIP? =;J;=CNS L?N?HNCIH I@ 1H<;M?> IRC>? G;N?LC;F - H? I@ NBCM JLIJIM;F CM NI JL?J;L? H;HIMCT?>1H--J;LNC=F?M MCH=? NB? GCHCGCT?>J;LNC=F? MCT? =;HL?>O=? ;<MIFON?

PIFOG? =B;HA?¹⁺ 2 B? H;HIMNLO=NOL?>1H<;M?>IRC>? G;N?LC;F @ILCHMN;H=? H;HILI>M BIFFIQMJB?L?M H;HIQCL?M ;H> H;HINO<?M ;NN;CH?> CGJLIP?G?HNIH=;J;=CNSL?N?HNCIH NB;H NB;NI@ <OFE 1H-- ^1,(11 HINB?L;JJLI;=B CM NI I@@?L@L?? PIFOG? CH <?NQ??H NB?

;=NCP? G;N?LC;FM MI NB;NNB? @L?? PIFOG? J?L@ILGM ;M <O@@?LNI ;==IGGI>;N? PIFOG?

=B;HA?M ¹² 'N Q;M L?JILN?> NB;N ;H IL>?L?> G?MIJILIOM MNLO=NOL? ¹² H;HINO<OF;L MNLO=NOL? ;H> 1H- BIFFIQ GC=LIH;HIMJB?L? ;=BC?P?> CGJLIP?G?HN IH

=S=F?L?N?HNCIH $ CA

FNBIOAB NB?L? B;> <??H GO=B JLIAL?MM?M QCNB =S=F? L?N?HNCIH ;H> BCAB

=;J;=CNS QCNB 1H<;M?> IRC>? G;N?LC;F CNM JL;=NC=;F ;JJFC=;NCIH NI L?JF;=? AL;JBCNC=

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>OLCHA NB? MNFCNBC;NCIH JLI=?MM >?LCP?> @LIG CLL?P?LMC<F? L?;=NCIH NI @ILG NB? * C-- JB;M?

Fig. 1.3.4; $ #1#+ CG;A?MI@NB?1H--H;HINO<?M G?LC=;H! B?GC=;F1I=C?NS L?JLCHN?>QCNB J?LGCMMCIH ^1, < 2 #+ CG;A?M I@ NB? =LSMN;FFCH? =;L<IH BIFFIQ MJB?L?M G?LC=;H ! B?GC=;F 1I=C?NS L?JLCHN?>QCNBJ?LGCMMCIH ^1- = 2 #+ CG;A?I@NB?1H--H;HILI>M G?LC=;H! B?GC=;F 1I=C?NS L?JLCHN?>QCNBJ?LGCMMCIH ^1. > 1#+ CG;A?I@1H--H;HIQCL?M(IBH5 CF?S;H>1IHM L?JLCHN?> QCNB J?LGCMMCIH ^1/ ? @ 2SJC=;F2 #+ CG;A? I@ 1H--(Cd-I. H;HIQCL?M G?LC=;H

! B?GC=;F1I=C?NS L?JLCHN?>QCNBJ?LGCMMCIH ¹⁰ A CG;A?MI@2 #+ ;H>M?F?=N?>;L?;>C@@L;=NCIH 1 #" J;NN?LHMI@1H--H;HIQCL?M ;H>@ 2 #+ ;H>$ $ 2 CG;A?MI@1H--H;HIJIQ>?LM (IBH 5 CF?S;H>1IHM L?JLCHN?>QCNBJ?LGCMMCIH ¹¹

1H+ CHN?LG?N;FFC==IGJIOH>

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Gn1H + ! I ! O + H $ ? ! ? + A 1< IGWU Q?L? MOAA?MN?> NI MO<MNCNON? IRSA?H

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CH#KO;NCIH ;H> <?FIQ^0/

Gn1H * C^& ?⁽(R+ * C/)-01H R+ * C/)-01HD+ n1H 1H * C ?⁽

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NB? #KO;NCIH CM @IL NB? G?=B;HCMG >OLCHA NB? MN >?FCNBC;NCIH JLI=?MM ;H> NB?

MO<M?KO?HN=S=F?M NNB? MNFCNBC;NCIH JLI=?MM MCGCF;LL?;=NCIH NI NB? 1H<;M?> IRC>?

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1H+ =;L<IH=IGJIMCN?

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0 ?@?L?H=?M

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5 6 ( 5 ;HA $ "CHA 6 ! B?H # , ;MS<OFCH 7 8B;HA' (% 8B;HA 5-9/?

5=1965 $ +1 7

+ 7IMBCI ) IT;Q; 0 ( LI>> CH * CNBCOGCIH ;NN?LC?M #>M + 7IMBCI 0 ( LI>> ) IT;Q; 1JLCHA?L , ?Q7ILE

& ) CG % (?IHA 73 ) CG (& ) CG ! + .;LE & ( 1IBH 0 -4 $ 6+ #-=

42

$ - LMCHC "O.;MKOC?L ?;O>ICH (+ 2;L;M=IH + 2L?HNCH , * ;HA?HBOCT?H #

"? ??L . , INN?H " 6>-9 $ 6<9+-: 76

2 - M;E;2 + IGG;7 + ;NMOGINI 7 3 =BC>; 3-+;96+0 -4$ 6+ 14 3 PIH1;=E?H # , I>Q?FF 1OH>B?L$ 631, : ;);- 651+: 69

" OL<;=B * 5 ?CMMG;H CH , IH;KO?IOM #F?=NLI=B?GCMNLS #>M " OL<;=B + ;L=?F"?EE?L , ?Q7ILE )

, "?S # ( 0 O>> 3-+;96+0 -4 $ 6+ 121 0 " 0 ;OB 1 LOGG?L 3-+;96+0 14 +;) 22 ) + <L;B;G 3-+;96+0 14 +;) 38

8' 2;E?B;L; " 6>-9 $ 6<9+-: 68

" OL<;=B # 8CHCAL;>7 ! IB?H & 2?FF?L$ 631, $ ;);- 651+: 148 # .;F?> ( 3-+;96+0 -4 $ 6+ 126

" OL<;=B " 6>-9 $ 6<9+-: 89

+ * ;TT;LC 1=LIM;NC 3-+;96+0 -4 $ 6+ 127

+ LG;H> CH + ;N?LC;FM @IL >P;H=?> ;NN?LC?M #>M " 5 + OLJBS(

LI;>B?;> ! & 1N??F? .F?HOG , ?Q7ILE

+ 5 CHN?L ( - ?M?HB;L> + # 1J;BL . , IP` E ,= );-9 10 ) + CTOMBCG; .! (IH?M .( 5 CM?G;H ( % II>?HIOAB ); #-: <33 15

, "?S 3-+;96+0 -4 $ 6+ 118

% (?IHA 73 ) CG & ) CG 7( ) CG & ( 1IBH 5-9/? 5=1965 $ +1 4

+ * 0 ;I 0 5 $ L;H=CM & 5 ! BLCMNIJB?L 3-+;96+0 -4 $ 6+ 124 + % ;LL?;O ( 2 B?P?HCH + $ ?ECL " 6>-9 $ 6<9+-: 9

0 4 + IMBN?P . 8F;NCFIP; .OL?MB?P; 4 + ;H?P ) IT;Q; " 6>-9 $ 6<9+-:

51

+ + ILCN; 7 - E;>; 7 + ;NMO>; 3-+;96+0 -4 $ 6+ 134 1 C;FFIT;L + * C?>?L 3-+;96+0 -4 $ 6+ 140

' #J?F<ICH + $ LIG?HN + % ;LL?;O ( 2 B?P?HCH " 5 ;LCH 3-+;96+0 -4 $ 6+

127

2 0 (IQ ! ! * C;HA 3-+;96+0 -4 $ 6+ 129

. 8F;NCFIP; ' ;FE;HIP 7 % ?LIHIP " 6>-9 $ 6<9+-: 24

(- ?M?HB;L> . ) IG?H>; .;RCHIM # 5 O>S$ 631, : ;);- 651+: 18 ( 7;HA + 5 CHN?L (- ?M?HB;L>$ 631, : ;);- 651+: 90

(- ?M?HB;L> + & ?MM . ) IG?H>;$ 631, $ ;);- 651+: 40 " $ ;ON?OR 0 ) IEM<;HA 773 0 -4 23

0 5 & IFG?M CH.LI=??>CHAM I@NB? #! 1 1SGJIMCOG IH* CNBCOG ;NN?LC?M ?>CN?>

<S , "?S .?HHCHANIH , ( 3 1

( 5 ;HA . ) CHA;H>0 & OAACHM$ 631, $ ;);- 651+: 20 0 7;T;GC .B 2IOT;CH " 6>-9 $ 6<9+-: 9

( - ?M?HB;L> ( % dLNF?L. ) IG?H>; CH! B?GC=;F.BSMC=MI@'HN?L=;F;NCIH ?>CN?>

<S . * ?AL;H>;H>1 $ F;H>LICM , 2- 1' 1?LC?M 1?LC?M .BSMC=M .F?HOG.L?MM , ?Q7ILE

(- ?M?HB;L> & . $ LCNT 3-+;96+0 14 +;) 20

H;HC 1 ! LIO=B ;E?L 0 & OAACHM 3-+;96+0 -4 $ 6+ 134 ! ( 5 ?H IOE;GJ 0 & OAACHM 5 5 ?JJH?L 3-+;96+0 -4 $ 6+

126

(- ?M?HB;L> ( 7;HA + 5 CHN?L " 6>-9 $ 6<9+-: 68

IOE;GJ % ! * ?MB 0 & OAACHM 3-+;96+0 -4 $ 6+ 128 ( 0 - Q?H 5 ! + ;ME?FF ! & 1N??F? 2 1 , C?FM?H - 2 1b L?HM?H$ 631, $ ;);-

8RQMGV 13

+ 5 CHN?L ( - ?M?HB;L> 3-+;96+0 14 +;) 45

+ + ;R@C?F> 2 0 (IQ 1 % IOF> + % 1?Q=BI=E * 5 1B;=EF?NN? 3-+;96+0 -4

@RG& 135

+ + ;R@C?F> 2 0 (IQ + % 1?Q=BI=E * 5 1B;=EF?NN? " 6>-9 $ 6<9+-:

26

(- ?M?HB;L> + & ?c ( & OMF;A? ) (OL?QC=T 3 ) L?<<?L " 6>-9 $ 6<9+-:

44

0 & OAACHM " 6>-9 $ 6<9+-: 26

(- ?M?HB;L> + 5 CHN?L ( 7;HA + 5 ;=BNF?L 0 H>L?;OM 5 1CNN? ' 0 IG CH .LI=??>CHAMI@ NB HHO;F+ ??NCHAI@'1# ) CN;ESOMBO (;J;H

+ 5 CFMIH (0 ";BH 3-+;96+0 -4 $ 6+ 142

( L;A;H? ) + ;NMOC & H>IB 1 1OTOEC & $ OE;>; & 'E?S; ) ) CN;<; 0 'MBCE;Q; " 6>-9 $ 6<9+-: 68

7 '>IN; 2 ) O<IN; + ;NMO@ODC 7 + ;?E;Q; 2 + CS;M;E; @GMIQGI 276

! + .;LE (& ) CG & ) CG & ( 1IBH 0 -4 $ 6+ #-= 39 ( 1;HAMN?L ! 5 ;F? " 0 ): - 8 <131* 19

* 7 ?;OFC?O 2 " & ;N=B;L> IH;E>;LJIOL+ " $ F?CM=B;O?L;H>( 0 ";BH 3-+;96+0 -4 $ 6+ 150

& + OE;C<I 2 + IGG; 7 1B;=B;G"C;G;H> 2 - M;E; + ) I>;CL; 3-+;96+0 -4

$ 631, $ ;);- -;; 10

' ! IOLNH?S ( 0 ";BH 3-+;96+0 -4 $ 6+ 144

' ! IOLNH?S 5 0 + =) CHHIH;H>( 0 ";BH 3-+;96+0 -4 $ 6+ 146 ) CG + , IB + ! BIC ( ! BI;H> .;LE 0 -4 );-9 17

7 5 ;HA ( 7 * ??;H>& ! 8?HA 0 -4 );-9 17 7 5 ;HA $ 1O ( 7 * ??;H>6 1 8B;I 0 -4 );-9 18 7 5 ;HA;H>( 7 * ?? " 0 ?: 0 -4 108

+ 1 .;LE % 6 5 ;HA 7+ ) ;HA " 5 ?RF?L 16 "IO & ) * CO 5/->

0 -4 5; , 46

"5 ) CG '1 & Q;HA 1 ( ) QIH & 7 ) ;HA ) 1 .;LE 7( ! BIC ) ( ! BIC

;H>(% .;LE! )56 -;; 7

+ 1 .;LE 7+ ) ;HA % 6 5 ;HA 16 "IO;H>& ) * CO ,= <5+; );-9 18

# ) CG " 1IH 2% ) CG ( ! BI .;LE ) 1 0 SO 1 & ! B;HA 5/-> 0 -4 5; , 43

1 & ;H (;HA 2 ) CG 1 + - B;H>2 & S?IH ,= <5+; );-9 15 + 5 ;=BNF?L + 5 CHN?L;H>( - ?M?HB;L> " 6>-9 $ 6<9+-: 94 & ) CG 7( ) CG " % ) CG & ( 1IBH;H>2 ) ;HA$ 631, $ ;);- 651+: 144

" * ;L=B?L 1 .L;E;MB ( 1;CHN + + IL=L?NN? (+ 2;L;M=IH 0 -4 );-9 16

( 7 * ?? 0 8B;HA;H>8 * CO " 6>-9 $ 6<9+-: 90

' % LCAILC;HNM * 1IGCHMEC & * C ' '@;LA;H " OL<;=B % ?>;HE?H 0 -4 3RPPXQ&

2 (C;HA 1 8B;HA 6 / CO 5 8BO;;H>* ! B?H " 6>-9 $ 6<9+-: 166 ( * ;H>C + ( % ;HN?L ! " ! L?MM 0 "C* ?I 0 . 0 ;@@;?FF? 5-9/? 5=1965

@GM& 2

+ , IB 7 ) QIH & * ?? ( ! BI 7 ) CG ;H>+ % ) CG 0 -4 );-9 17

% "?LLC?H ( & ;MMIOH 1 .;H?LI;H> 1=LIM;NC ,= );-9 19 ( ! ! F;OMM?H " $ L;HEFCH O & ;KO? " + .ILN?L!?F> 2 1 $ CMB?L $ ! )56

3

. 0 ;H>;LO ! )56: +1 ! )56;-+0 563 7

* . 8;H?FFI 8B;I & & O 0 ! & ;>>IH! )56 -;; 6

. .b NM=BE? 2 H>L?M 2 4 CFFGIQ 1 .?A?F & LdHCA ) ) I<;MBC " $ CM=B?L *

& ` OMMF?L 6476: $ +1 % -+0 563 70

5 6 ! B?H ( 7 * ??;H>8 * CO3EUFRQ 41

8 . % OI 8 5 8B;I & ) * CO;H>1 6 "IO3EUFRQ 43 7 5 ;HA & ! 8?HA;H>( 7 * ?? ,= );-9 18

7 5 ;HA ( 7 * ?? 5/-> 0 -4 5; , 45 7 5 ;HA + 5 O 8 (C;I ( 7 * ?? 0 -4 );-9 21 & 'MBCB;L; 1 + CTON;HC & 'HIO? 3 1 .;N

/ $ ;H . ( ! BOJ;M + 1 5 BCNNCHAB;G 3-+;96+0 -4 $ 631, $ ;);- -;; 10

( 0 ";BH 0 # + ;L;H> <IOT?C> 3-+;96+0 -4 $ 6+ 153 " 5 2I>> 0 # + ;L;H>( 0 ";BH 3-+;96+0 -4 $ 6+ 153 " 5 2I>> 0 # + ;L;H>( 0 ";BH 3-+;96+0 -4 $ 6+ 154 ( & ;MMIOH 1 .;H?LI % + OF;M;H> 1=LIM;NC " 6>-9 $ 6<9+-: 171 1' * ?? 1 7IIH ! + .;LE (+ * ?? & ) CG " 'G 1% "II;H>& ( 1IBH

3-+;96+0 14 +;) 54

1 7IIH (+ * ?? & ) CG " 'G 1% "II;H>& ( 1IBH 3-+;96+0 14 +;) 54

. . $ ?LAOMIH + * + ;LNCH? # % ?ILA? ;H>( 0 ";BH " 6>-9 $ 6<9+-:

194

, * C & 1IHA & ! OC % 7;HA ! 5 ;HA );-9 0 -4 2

6 * C 7 8BIHA + ! ;C + . ;FIAB " 5 ;HA 7 8B;HA 0 * C 6 1OH 3-+;96+0 14 1GWE 89

! ( * CO $ & 6 O? & & O;HA 6 & 7O ! ( 6 C? + 1 1BC % 8 ! ;I 7% (OHA 6 * "IHA 3-+;96+0 14 +;) 129

5 .O 6 & ? ( 0 ?H ! 5 ;H ! (C;HA 3-+;96+0 14 +;) 50 ( & ;MMIOH 1 .;H?LI 1=LIM;NC " 6>-9 $ 6<9+-: 160 / (C;HA 0 6 O? + (C; 773 $ <9. $ +1 258

(5 .;LE (7 #IG & 1 ) QIH 3-+;96+0 -4 644<5 11

1" 1?I % & * ?? & * CG ) + + CH (! ) CG & 5 1BCG ) 1 .;LE

"5 ) CG#$ ,= 2

( "IHA>IHA + 6 C;IBO; $ 7;H<;I 773 3-+;96+0 -4 42

+ 3 SM;F & % OF FJ & E<OFON 'HN ( ?,96/-5 5-9/? In press DCDBS>?H?

+ 3 SM;F 2 ! ?NCHE;S; FJ & E<OFON 773 $ <9. $ +1 290 5 5 ?C 6 ! OC 5 ! B?H " % 'P?S " 0 ?: 0 -4 112

! 7O;H * 7;HA * & IO * 1B?H 6 8B;HA 6 5 * IO 5-9/? 5=1965 $ +1 5

" 2 ";G 6 5 ;HA (+ * ??#$ ,= 2

1 2IGCH;E; 2 + IGG; 2 - M;E; 3-+;96+0 14 +;) 53

1 2IGCH;E; 2 & ;S;MBC 7 , ;E;GOL; 2 - M;E; );-9 0 -4 20 1 2IGCH;E; 7 , ;E;GOL; 2 - M;E; " 6>-9 $ 6<9+-: 195

7 " % ;G<OLA % 8;HA;LC 2 B?ILS ;H> .L;=NC=? I@ + ?N;F #F?=NLI>?JIMCNCIH 1JLCHA?L

( 2;HA ) TOGC 3-+;96+0 14 +;) 56

2' * ?IHA 72 & MC?B '5 1OH 3-+;96+0 14 +;) 56 . % CLC>B;L 1 8?CH#F <?>CH $ #H>L?M 3-+;96+0 14 +;) 70

. , ;LNF?NN " ! IIE ! & ) ??M >?% LIIN * & ?=NIL0 & O;HA (IFF?SM % . ) CMMFCHA 5 * ?P;MIH 1 ( .?;L=? % 0 ?C>#$ ,= 3

) 'TONMO #F?=NLI=B?GCMNLSCH, IH;KO?IOM 1IFONCIHM 5 '* #74 ! & 4 ?LF;A% G<&

! I ) % ; 1?=IH> 0 ?PCM?>;H>#HF;LA?>#>CNCIH

2 + IGG; + (?IHA 2 7IEIMBCG; & , ;L; 2ISI>; 2 - M;E; " 6>-9

$ 6<9+-: 242

Chapter 2:

Analysis of an Electrodeposition

process of Sn-O-C Composite from

an Organic Electrolyte