廢料之復活：利用鍍膜及電漿表面改質技術於回收矽/碳化矽之複合材與其鋰離子電池之應用

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研究生：	陳秉宏 Chen, Bing Hong
論文名稱：	廢料之復活：利用鍍膜及電漿表面改質技術於回收矽/碳化矽之複合材與其鋰離子電池之應用 A Revival of Waste: Surface Modification via Coating and Plasma Jet in Recycled Si/SiC Composite for Lithium Ion Batteries
指導教授：	杜正恭 Duh, Jenq Gong
口試委員:	胡啟章 Hu, Chi Chang 石東益 Shih, Toung Yi 劉偉仁 Liu, Wei Ren 蕭立殷 Hsiao, Li Yin
學位類別：	博士 Doctor
系所名稱：	工學院 - 材料科學工程學系 Materials Science and Engineering
論文出版年：	2017
畢業學年度：	105
語文別：	英文
論文頁數：	200
中文關鍵詞：	鋰離子電池、矽、廢料回收、大氣電漿、表面改質、鍍膜
外文關鍵詞：	Lithium ion batteries, Silicon, Recycled waste, Atmospheric pressure plasma, Surface modification, Coating
相關次數：	點閱：1 下載：0
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在過去數十年，鋰離子電池的發展被視為一開發的主流來解決能源儲存裝置之議題。在此相關產業蓬勃發展的同時，高電容密度以及低環境影響的條件已被當作鋰離子電池正負極活物選用時的基本要求。現今負極活性材料，多採用碳材為主而限制了其高電容量之發展性。其中矽基負極材料，因充放電過程中形成Li15Si4合金所貢獻之理論電容量高達3590 mAh/g 可吻合高電容量的條件，被認定為最具潛力來取代傳統碳基電池的潛力材料，但卻因其合金化過程所造成的體積膨脹與伴隨的固態電解質生成相，造成電容量之衰減而影響其應用端的發展。為了克服矽基電池的缺點，大部份的研究致力於 (1) 合成各種特殊形貌來縮小矽粉體至奈米尺度， (2) 包覆或混合添加物於粉體上或漿料中，或 (3) 加入電解液添加劑等方法。然而，上述等方法往往與商業化之低成本以及環保之低污染源的需求大相逕庭。
本論文擬開發低成本且環境友善之矽基高容量鋰電池負極材料。材料端選用自太陽能切削廢液，回收純化後所得之回收矽廢料為活性材料，其微米尺度粉體遠大於一般效能較好之奈米尺度粉體，且其表面含有豐富的有機鍵結與原生氧化層。有別於傳統之方法，多種表面改質技術於本論文中提出，其技術包含表面碳薄膜鍍製與大氣電漿處理，係作用於矽基電池極片表面，由介面著手優化其表面鍵結組態，來抑制固態電解液相之生成。此外，更佐以整體電池極片之空間佈局，並配合添加劑以及導電劑之調控，增加矽基回收廢料之循環壽命。本論文中所開發之技術相較於其他化學合成方法來說，除了簡易、快速、低成本且環境友善外，更可有效地達到優異電性的表現，預期所開之各種表面改質技術能推廣至更多不同電池材料系統中。咸信本文所選用之廢料回收之負極材料，可適用於未來高電容量之商業化發展鋰離子電池中。

In the past decade, the rising development of lithium ion batteries (LIBs) has been recognized as a tidal current for solving energy storage related issues. Under this technical billow, the demands of active materials with lower environmental impact and higher energy density are considered as the criteria for LIBs materials. Especially for anodic material, the present carbon-based electrode is limited in the potential applications with high capacity because of its theoretic capacity (372 mAh/g). To achieve the goal for high capacity anodes, silicon (Si) with 3590 mAh/g theoretical capacity meets the requirement by forming Li15Si4 phase during cycling processes to replace present conventional carbon-based batteries. However, the capacity fading caused by the intrinsic drawbacks of volumetric expansion and continuous formation of solid electrolyte interphase hinders the dissemination of Si-based LIBs. To overcome the disadvantages of Si, numerous studies have endeavored (1) to shrink Si particles to nanometer scales by using various morphology-chemical synthesis techniques, (2) to wrap or mix conductive additives onto particles or into slurries, and (3) to add electrolyte additives. Unfortunately, the as-mentioned methods mostly fail to accommodate the cost-effectiveness of commercialization and low pollution of environmental friendliness.
In the pursuit of low cost and high environmental friendly anode material, a distinct resource of Si-based anode material is explored in this study. The recycled material is extracted from the cutting waste fluid produced in solar panel industry. After purification technology of chemical rinsing and physical separation, the obtained composites show much larger particle size than commonly nanolized Si particles, and possess the abundant organic bonds and native oxide on the surface of particle. Unlike conventional methods to focus on the synthesis process of powder, the as-prepared electrodes will be treated via various surface modifications, including techniques of carbon deposition and atmospheric pressure plasma jet. The combined processing reduces the capacity degradation by interfacial control to convert the surface bonds with the effectiveness to suppress the growth of SEI, and then maintain the stabilization of electrode during cycling. In addition, the entire electrode collocates with conductive agent and electrolyte additive to provide the conductivity and to improve the internal SEI formation. Overall, the developed techniques of surface modifications are not only scalable, simple, low-cost and environmental friendly but also effective to achieve the excellent performance with high capacity. It is expected for similar potential usage in others battery system. The selected recycled waste for anodic material should be applicable and suitable for the future blueprint in the commercialization for LIBs.

Contents    1
Figures    6
Tables……………………………………………………………………14
Chapter 1    15
1 Background    15
2 Motivations and Objectives    17
3 Stages for Reviving Wafer Waste    18
3.1 Stage I. Carbon (C) Additives and Pitch Wrapping Technique (PWT)    18
3.2 Stage II. Carbon Assisted Technique (CAT by sputtering)    18
3.3 Stage III. Nitrogen-Atmospheric Pressure Plasma Jet (N-APPJ)    19
3.4 Stage IV. Multiple Surface Modification by Plasma Enhanced Carbon Veil (PEC-veil)    19
3.5 Stage V. Synergistic Fusion of Spatial and Interfacial Control40    20
Chapter 2 Literature Survey    21
1 Environmental issues    21
2 Renewable energies    22
3 Silicon Wafer Waste    23
4 Lithium Ion Batteries (LIBs)    27
4.1 Evolution of LIBs    27
4.2 The Reaction Mechanism of LIBs    32
4.3 Evolution of Anode Materials    36
5 Si-based Anode Materials    40
5.1. Basic Concept of Si-based Anode    40
5.2 Particle Size Effects in Si-based Lithium-ion Battery    46
5.3 Spatial Control: Architectural Designs of Si/C Hybrid Anode Materials    49
5.5 Si-N compounds and Li-N matrix    56
6 Methodologies of Micro-sized Si/SiC Composites from Wafer Waste    59
Chapter 3 Experimental Details    61
1 Material Preparation    61
1.1 Waste from Solar Industry    61
1.2 Carbon Assisted Method(CAT) and Pitch Wrapping Technique (PWT)    61
1.3 Nitrogen Atmospheric Pressure Plasma Jet (N-APPJ)    62
1.4 Carbon Veil (C-veil) and Plasma Enhanced C-veil (PEC-veil)    63
1.5 Double-Plasma Enhanced Carbon Shield (D-PECS)    63
2 Characterization an Analysis    64
2.1 Phase Identification    64
2.2 Compositional Evaluation and Element Mapping    64
3.3 Morphology Observation    64
3 Electrochemical Analysis    65
3.1 Electrode Parameters and Battery Assembly    65
1.2 Cyclability and Rate Capability Measurement    65
3.3 Cyclic Voltammetry (CV) and Electrochemical Impedance Spectroscopy (EIS)    66
Results and Discussions    67
Chapter 4  Preliminary Examinations of Si/SiC composites    67
1 Phase Identifications, Morphologies and Particle Distribution    68
2 Wafer Orientation and Native Oxide    71
3 Surface bonds of Pristine Powder from Waste    73
4 Performance of Recycled Waste without Treatment    75
5 Stage I. Carbon Additives and Pitch Wrapping    77
Chapter 5 Interfacial Control for Si/SiC Composites by Carbon Assisted Technique (CAT)    85
1 Simplify the Waste-based Electrode    85
2 Development of Stage II. Carbon Assisted Technique (CAT)    85
3 Characteristics of Carbon Assisted Technique (CAT) for Modified Electrode    86
4 Optimum Thickness of Carbon Assisted Technique (CAT)    89
5 Comparison of Carbon Assisted Technique (CAT) and Pitch Wrapping Technique (PWT)    90
6 Investigation of Electrochemical Behaviors    95
7 Summaries of Stage II. Carbon Assisted Technique (CAT)    98
Chapter 6 Interfacial Control for Si/SiC Composites by Nitrogen-Atmospheric Pressure Plasma Jet (N-APPJ)    99
1 Preface    99
2 Chemical Compositions of Surface Bonds    100
3 Qualitative and Quantitate Analysis for N-APPJ    104
4 Plasma Mechanism of N-APPJ and Electrochemical Behaviors after N-APPJ    111
5 Investigation of Formed SEI and Electrodes after First Cycle    118
6 Summaries of Stage III. Nitrogen-Atmospheric Pressure Plasma Jet (N-APPJ)    126
Chapter 7 Interfacial Control for Si/SiC Composites by Stage IV. Multiple Surface Modifications (C-veil and PEC-veil)    127
1 Preface    127
2 Schematic Diagram of Stage IV. C-veil and PEC-veil    128
3 Characteristics and Optimized Thickness of C-veil and PEC-veil    129
4 Qualitative and Quantitate Analysis for C-veil and PEC-veil    134
5 Electrochemical Behaviors after the Modifications of C-veil and PEC-veil    139
6 Investigation of Formed SEI and Electrodes after First Cycle    146
7 Summaries of Stage IV. Multiple Surface Modifications: C-veil and PEC-veil    153
Chapter 8 Stage V. Synergetic Fusion Of Spatial & Interfacial Control    155
1 Preface    155
2 Infrastructure of Stage V. Synergetic Fusion of Spatial & Interfacial Control    157
3 Spatial Control: Active/Inactive/Conductive Additives    160
4 Interfacial Control: Internal/External/Fusion electrode modifications    165
5 Rate Performance of Micro-Sized Si Electrodes and Impedance Analysis    169
6 Homogeneity and Effects of D-PECS Electrode Modification    172
7 Investigation of Formed SEI and Electrodes after First Cycle    176
8 Summaries of Stage V. Synergetic Fusion of Spatial and Interfacial Control    181
Chapter 9 Conclusions    183
References    187


                                

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