臺灣博碩士論文加值系統

金屬奈米顆粒的製備方式以往大多是採用化學法，添加懸浮劑控制奈米顆粒之粒徑與濃度。本論文利用放電加工機(EDM)，以電火花放電法(ESDM)，透過電弧(Arc)將金屬材料熔融成奈米等級之顆粒，製造過程中無需添加化學藥劑，僅利用純水作為介電液，設定製程參數及放電脈寬時間(TON-TOFF)，即可製備出懸浮於介電液中之奈米等級的金屬顆粒，其製程簡單且快速可大量製造、低成本、對環境汙染較小，此方法對於奈米材料的製備極具貢獻。
本論文提出奈米鉍之研究，係利用脈衝火花放電 (Pulsed Spark Discharge)在去離子水(DI-water)中製備奈米鉍膠體溶液，藉由調整放電加工機的TON、TOFF及放電電流IP值，使鉍金屬線在去離子水中產生脈衝火花放電以製備奈米鉍膠體溶液，並使用穿透式電子顯微鏡(Transmission electron microscope,TEM)、能量色散X射線譜(Energy-dispersive X-ray spectroscopy,EDX)、以及光散射儀(Zetasizer)、紫外光可見光分光光譜儀(Ultraviolet–Visible Spectroscopy,UV-Vis)等儀器去分析在不同的放電參數下所製備奈米鉍膠體溶液的結果，藉以得到以脈衝火花放電加工法製備奈米鉍的較優化參數。本論文結果顯示成功以電火花製備出奈米鉍膠體溶液，並佐以TEM及EDX分析找到奈米鉍在UV-Vis的吸收峰值為234~237nm，另外，本研究為了探討以微型放電加工機製備奈米鉍膠體溶液的製備參數，此微型放電加工機的製備參數即比例-積分-微分(Proportional Integral Derivative,PID)的控制參數，經詳細分析微型放電加工機的系統架構後，也成功推導出微型放電加工機(Micro Electrical Discharge Machine, Micro EDM)的數學模型，藉由Matlab軟體輔助分析找到PID參數並帶入Micro EDM實驗，相比較於線上調適法的放電成功率(36%)、Ziegler-Nichols(ZN)法的調適參數法(36.451%)，使製備奈米銀的放電成功率提升至84.4773%，而製備奈米鉍膠體溶液的放電成功率也可以達到74.1876%。

In the past, the preparation of metal nanoparticles has been carried out by a chemical method, and a suspension agent is added to control the particle size and concentration of the nanoparticles. In this dissertation, an electric discharge machine (EDM) or a Micro EDM is used to melt metal materials into nanometer-scale particles by arc discharge. No chemical is added during the manufacturing process, and pure water is used as the medium. Electro-hydraulic, set process parameters and discharge pulse width time (TON-TOFF), can prepare nano-grade metal particles suspended in dielectric liquid, the process is simple and fast, can be mass-produced, low cost, environmental pollution Smaller, this method contributes greatly to the preparation of nanomaterials.
In this dissertation, the study of nano-small is carried out by using pulsed spark discharge (Pulsed Spark Discharge) method to prepare nano-Bi colloidal solution in deionized water (DI-water) by adjusting the TON, TOFF and discharge current IP of the EDM. The value causes the Bismuth wire to generate a pulsed spark discharge in deionized water to prepare a nano-Bi colloidal solution, then the Transmission Electron Microscope(TEM), Energy-dispersive X-ray spectroscopy(EDX), Zetasizer, Ultraviolet–Visible Spectroscopy (UV-Vis) and other instruments were used to analyze the results of the nano-Bi colloidal prepared under different discharge parameters, so as to obtain the optimized parameters of the preparation of nano-Bi by pulse spark discharge machine. The results of this dissertation show that the nano-Bismuth colloidal solution was successfully prepared by EDM and the absorption peak of UV–Vis was found at 234~237 nm. In addition, in order to find out the Proportional Integral Derivative (PID) control parameter while using the Micro EDM to prepare the Bismuth colloid, the mathematical model of Micro EDM was successfully derived, the PID parameters were found by Matlab software-assisted analysis and put them into the Micro EDM for experiment, compared with the discharge success rate of the online adaptation method (36%), and the Ziegler-Nichols (ZN) method. (36.451%), the discharge success rate of preparing nano silver was increased to 84.4773%, and the discharge success rate of preparing nano-Bismuth colloid solution can reach 74.1876%.

摘　要 i
Abstract iii
誌 謝 v
Contents vii
List of Tables x
List of Figures xi
Chapter 1 Introduction 1
1.1 Background 1
1.2 Research motives and objectives 3
1.3 Dissertation organization 5
Chapter 2 Literature review of Bismuth nanoparticle and analysis 7
2.1 Introduction of Bismuth Particle 7
2.1.1 The fundamental properties of Bismuth 7
2.1.2 .Bismuth Particle 12
2.1.3 Special physical and chemical property of Bismuth 16
2.1.4 Applications of Bismuth 16
2.2 Optical properties of Nano Metal Particle 17
2.3 Nano Particles Preparation 18
2.3.1 Chemical methods 18
2.3.2 Physical methods 20
2.4 Suspension mechanism and dispersion theory 22
2.4.1 Brownian motion 22
2.4.2 Electric double layer theory 24
2.4.3 DLVO theory 25
2.5 The aggregation and dispersion of nano suspension 28
2.5.1 The formation of colloid surface charge 28
2.5.2 The aggregation of nano-suspension 30
2.5.3 The dispersion of nano-suspension 31
2.5.4 Physical dispersion 32
2.5.5 Chemical dispersion 33
2.6 Surface modification of nanoparticles and suspended 35
Chapter 3 Principles of Electric Spark Discharge and EDM 36
3.1 Introduction of spark discharge 36
3.1.1 Origin of life 36
3.1.2 Classification of discharge 38
3.2 Plasma Basic Theory 41
3.3 Introduction of electric discharge machine 43
3.3.1 Background of EDM 43
3.3.2 Melting points of different metal bulk material 44
3.3.3 Electric spark (PSDM) heat source system 45
3.3.4 Nucleation and growth of the nanoparticles 48
3.3.5 Feature of EDM 50
3.4 Nanoparticles formation mechanism via spark discharge 52
3.5 Advantages of Spark discharge 56
3.6 Large-scale electric discharge machine 57
3.6.1 Architecture of the Large-scale electric discharge machine 57
3.6.2 Discharge time and rest time (Ton:Toff) and discharge current (Ip) of electrical parameters 59
3.6.3 Control panel parameter setting 60
3.6.4 Preparation Process of nano metal colloid with large-scale EDM 62
3.7 MicroEDM 63
3.7.1 Micro EDM mechanism 64
3.7.2 Hardware Circuit System 65
3.7.3 Discharge circuit 66
3.7.4 Motor control and feedback circuit 67
3.7.5 logic determination circuit 68
3.7.6 VisSim Monitoring System 69
Chapter 4 Research Method and Analytic Instruments 71
4.1 Bismuth Materials 71
4.2 Preparation of the Bismuth Particals with Large-scale EDM 72
4.2.1 Materials 72
4.2.2 Flow chart of experiment 73
4.2.3 Environmental parameter settings 74
4.3 Micro EDM Preparation Process Optimization 76
4.3.1 System Control Principle 76
4.3.2 Electrode discharge gap and PID control 78
4.3.3 Manual Tuning 81
4.3.4 Ziegler-Nichols method(ZN Method) 85
4.3.5 Matlab Aided Analysis 87
4.4 Micro EDM Control System Modeling 89
4.4.1 System Parameters of the Micro EDM 89
4.4.2 Mathematic Model of the Micro EDM Control System 98
4.5 Analytic Instruments for Bismuth Colloid 99
4.5.1 Zetasizer Nano System 99
4.5.2 UV-Visible Spectrophotometer 101
4.5.3 Transmission Electron Microscope 102
Chapter 5 Experimental Results and Discussion 105
5.1 Analyses of 50% duty cycle for preparing Nano-Bismuth colloid 105
5.1.1 Zeta Sizer and Zeta potential of 10-10 μs 105
5.1.2 Zeta Sizer and Zeta potential of 20-20 μs 106
5.1.3 Zeta Sizer and Zeta potential of 40-40 μs 108
5.1.4 Zeta Sizer and Zeta potential of 80-80 μs 110
5.1.5 Zeta Sizer and Zeta potential of100-100 μs 111
5.1.6 Summary of analyses for preparing nano-Bismuth colloid with 50% duty cycle 113
5.2 Analyses for preparing Bismuth colloid with Ton=10μs 113
5.2.1 Zeta Sizer and Zeta potential of 10-10 μs 114
5.2.2 Zeta Sizer and Zeta potential of 10-30 μs 115
5.2.3 Zeta Sizer and Zeta potential of 10-50 μs 117
5.2.4 Zeta Sizer and Zeta potential of 10-100 μs 119
5.2.5 Zeta Sizer and Zeta potential of 10-300 μs 120
5.2.6 Summary of analyses for preparing Bismuth colloid with fixed Ton=10μs 122
5.3 Analyses of Bismuth colloid with UV-Vis 123
5.3.1 Absorption of Nano Bismuth Analysis using UV-Vis 123
5.3.2 Peak Absorption of Nano Bismuth of UV-Vis 125
5.3.3 Summary of Analyses of Bismuth colloid with UV-Vis 126
5.4 Analyses of Bismuth colloid with TEM and EDX 126
5.4.1 Analyses with Transmission electron microscope (TEM) 127
5.4.2 Analyses with Energy dispersive X-ray spectroscopy (EDX) 127
5.4.3 Summary of analyses of Bismuth colloid with TEM and EDX 130
5.5 Analyses of Micro EDM Control System 130
5.5.1 On Line Manual Tuning 131
5.5.2 Ziegler–NicholsTunig Method 132
5.5.3 Micro EDM Mathematic Model and Matlab Aided Analysis 133
5.5.4 Discussion of the ZN Tuning Method Again 141
5.5.5 Summary of analyses of Micro EDM System with Modeling 143
5.6 Results and Discussion of Others 144
Chapter 6 Conclusions and Future Works 146
6.1 Conclusions 146
6.2 Future works 147
References 149
Author’s Introduction 159
Publication List a

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