臺灣博碩士論文加值系統

在這日新月異的社會，產品的生命週期是非常短暫，所以就要以最短時間與最少的成本損失來加速產品的改進及新產品的開發，而實驗設計就能以最少的實驗次數來找到實驗的顯著因子。本實驗是利用 部份因子找出銀粉合成的重要因子。銀粉是利用氨銀當前驅物，聯氨當還原劑，在批式反應器中進行化學還原反應來合成。由於影響銀粉合成的因子包括銀離子濃度（wt%）、聯氨濃度（wt%）、界面活性劑濃度（wt%）、氨銀溶液起始酸鹼值（pH）、反應溫度（℃）、進料流速（g/min）。我們將這6個因子用 部份因子設計需要8組實驗數，每組實驗數再重複做一次，共進行16組實驗數，接著將實驗數據以ANOVA分析來判斷主效應對銀粉性質的顯著性，並以回歸模式找到各銀粉性質之模式。
我們以摺疊（Folding Over）方式來了解主效應與交互效應對銀粉各性質的影響程度有多大。在本研究中實驗結果顯示部份因子設計可以較少的實驗次數找到影響銀粉性質（銀粉平均粒徑、銀粉比表面積、振實密度以及回收率）的主效應及交互因子效應，以本研究較有把握的實驗結果說明了主效應因子：銀離子濃度、聯氨濃度、界面活性劑濃度、反應溫度和進料流速，與交互因子效應：銀離子濃度與反應溫度、銀離子濃度與界面活性劑濃度對銀粉平均粒徑影響較大。以及主效應因子：銀離子濃度、聯氨濃度、界面活性劑濃度、反應溫度和氨銀溶液起始酸鹼值，與交互因子效應：銀離子濃度與聯氨濃度、銀離子濃度與界面活性劑濃度、銀離子濃度與反應溫度對銀粉回收率有顯著影響。

The valid period of a product is so transient in the competitive and progressing society that the improvement and exploitation of products under the increased efficiency and reduced cost are eagerly pursued. The purpose of experimental design is to find the significant factors via least experiments. The fractional factorial design is applied in this experiment to the synthesis of silver particles for particle size and recovery optimization. Ammonia silver solution was used as the precursor in the batch reactor to accomplish the chemical effects of silver powder synthesis. Concentration of silver ions(wt%), concentration of hydrazine hydrate(wt%), concentration of surfactant(wt%), initial pH value of ammonia silver solution(pH), temperature during reaction process (℃), and flow rate of materials(g/min) are influential factors in silver powder synthesis. The six factors were estimated via fractional factorial design requiring the execution of 8 distinct experiments, which were duplicated afterwards. The statistics of the altogether 16 experiments was analyzed by ANOVA to ascertain the significance of the main effect on silver powder properties. Next, regression model was built for each output reflecting the property of silver powder.
Folding over technique was utilized to realize the influence of main effects and interactive effects on the powder property. In the work, the experimental results reveal that the fractional factorial designs enable us to find out the concerned main effects and interactive factors on silver powder qualities (average size, surface area, tap density and recovery) based on the fewest numbers of experiments.
The most assured experimental results in this research prove that the main effective factors: concentration of silver ions, and of hydrazine hydrate, and of surfactant, reaction temperature and feeding rate, and the interaction effects: between concentration of silver ions and of surfactant, between concentration of silver ions and reaction temperature, are the most significant on the mean particle size of silver powder. Recovery rate, another focus in this work, is demonstrated to be most significant under the conditions of main effects: concentration of silver ions, and of hydrazine hydrate, and of surfactant, and initial pH of ammonia silver solution, and interaction effects: concentration of silver ions and of hydrazine hydrate, concentration of silver ions and of surfactant, concentration of silver ions and reaction temperature, are the most significant on the recovery rate of silver powder.

CONTENTS
ACKNOWLEDGMENTS i
ABSTRACT (in English) ii
ABSTRACT (in Chinese) iv
CONTENTS vi
TABLE OF CONTENTS viii
LIST OF FIGURES ix
LIST OF TABLES x
NOTATION xiv
CHAPTER 1 INTRODUCTION 1
1.1 Background and Motives 1
1.2 Objectives and Contents 5
1.3 Introduction of the Chapters 6
CHAPTER 2 REVIEW OF LITERATURE AND THERETICAL EXPLANATION OF EXPERIMENTAL DESIGN 8
2.1 The Synthesis of Metal Particles 8
2.1.1 Reduction Method of Reducing Agents 10
2.2 The Production Model of Silver Powders 14
2.3 Powder Qualities 15
2.4 Experimental Design Method 16
2.5 Fractional Factorial Design 18
2.6 Analysis of Variance 29
2.7 Estimation of the Parameters in Linear Regression Models 33
CHAPTER 3 EXPERIMENTAL 36
3.1 Materials 36
3.2 Apparatus Specifications 37
3.3 Analysis Instrumentation for Properties of Silver Particles 44
3.4 Statistics Software 45
3.5 Experimental Procedures 46
3.5.1 Ammonia Silver Solution Preparation 46
3.5.1.1 Preparation of Ammonia Silver (with 5wt%
Silver Ions ) of Respective pH Values of 4 and 9 46
3.5.1.2 Preparation of Ammonia Silver (with 3wt% Silver Ions ) of Respective pH Values of 4 and 9 47
3.5.2 Reducing Agent and Surfactant Preparation 47
3.5.2.1 Preparation of Hydrazine hydrate (8wt%) with
Surfactant 47
3.5.2.2 Preparation of Hydrazine hydrate (8wt%) with Surfactant 48
3.5.3 The Experiment Design of Silver Powder Synthesis 48
3.5.4 Silver Powder Estimation 52
3.6 Experimental Flow Sheet 53
CHAPTER 4 THE EXPERIMENTAL DESIGH APPLIED TO SYNTHESIS OF SILVER POWDER 55
4.1 Experimental Designs 55
4.1.1 The Influence of Each Main Effect toward Specific Properties of Silver Powders 57
4.1.2 Construction of Regression Model for Synthesis of Sliver Powders 63
4.2 Folding Over Design 65
CHAPTER 5 CONCLUSIONS 79
REFERENCES 83
LIST OF FIGURES
Figure 2.1 The two one half fractions of the design 20
Figure 2.2 Projection of a design into three designs 21
Figure 2.3 Treatment combination of design 30
Figure 3.1 Schematic diagram of the experimental apparatus 43
Figure 3.2 Experimental process 54
LIST OF TABLES
Table 2.1 Various Techniques for Synthesizing Nanopowders 9
Table 2.2 Plus and Minus Signs of the Factorial Design 19
Table 2.3 Three Factors of Linear Combinations 24
Table 2.4 The Designs of the Generators I=ABD, I=ACE, and I=BCF 25
Table 2.5 The Design of the Generators I=-ABD, I=-ACE, and I=-BCF 27
Table 2.6 Six Factors of Linear Combinations 28
Table 2.7 Data for Multiple Linear Regression 33
Table 3.1 Materials 37
Table 3.2 A Jacketed Reactor with An Agitator 38
Table 3.3 The Weighting Measurement 38
Table 3.4 The Feed-Rate Control Apparatus 39
Table 3.5 Equipment of Control Temperature 39
Table 3.6 The Temperature Measurement Apparatus 40
Table 3.7 The pH Measurement Apparatus 41
Table 3.8 The Separation Apparatus 41
Table 3.9 Measurement Instrumentation for The Particle Size Distributions 44
Table 3.10 Measurement Instrumentation for the Specific Surface Area 44
Table 3.11 Measurement Instrumentation for the Tap Density 45
Table 3.12 Temperature Recording Software 45
Table 3.13 Data Analysis Software 46
Table 3.14 Arrangement of Experiment by Fractional Factorial Design 49
Table 3.15 Arrangement of Experiment by Folding Over of Fractional Factorial Design 50
Table 4.1 Factor and Level of Fractional Factorial Design for Synthesis of Silver Powders 56
Table 4.2 Fractional Factorial Design for Synthesis of Silver Powders 56
Table 4.3 ANOVA of the Significance of Each Factor on the Mean Particle Size of Silver Powders 58
Table 4.4 Estimates of Effect and Alias structures for the Mean Particle Size of Silver Powders 59
Table 4.5 ANOVA of the Significance of Each Factor on the Specific Surface of Silver Powders 60
Table 4.6 Estimates of Effect and Alias for the Specific Surface of Silver Powders 60
Table 4.7 ANOVA of the Significance of Each Factor on the Tap Density of Silver Powders 61
Table 4.8 Estimates of Effect and Alias for the Tap Density of Silver Powders 62
Table 4.9 ANOVA of the Significance of Each Factor on the Recovery Rate of Silver Powders 63
Table 4.10 Estimates of Effect and Alias for the Recovery Rate of Silver Powders 63
Table 4.11 Value of Each Property of Silver Powders 65
Table 4.12 The Folding Over of Fractional Factorial Design for Synthesis of Silver Powders 66
Table 4.13 The Folding Over Applied to Estimates of Effect and Alias for the Mean Particle Size of Silver Powders 67
Table 4.14 Linear Combination for the Mean Particle Size of Silver Powders 67
Table 4.15 The Folding Over Applied to Estimates of Effect and Alias for the Specific Surface Area of Silver Powders 67
Table 4.16 Linear Combination for Specific Surface Area of Silver Powder 68
Table 4.17 The Folding Over Applied to Estimates of Effect and Alias for the Tap Density of Silver Powders 68
Table 4.18 Linear Combination for the Tap Density of Silver Powders 68
Table 4.19 The Folding Over Applied to Estimates of Effect and Alias for the Recovery Rate of Silver Powders 69
Table 4.20 Linear Combination for Recovery Rate of Silver Powders 69
Table 4.21 ANOVA on the Mean Particle Size of Silver Powders 70
Table 4.22 ANOVA on the Specific Surface Area of Silver Powders 71
Table 4.23 ANOVA on the Tap Density of Silver Powders 72
Table 4.24 ANOVA on Recovery Rate of Silver Powders 74
Table 4.25 Significant Factors for Producing the Silver Powders 74

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