銅鈀奈米粒子之合成及其在無電鍍銅之應用｜國立清華大學博碩士論文庫

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研究生：	羅曉筠 Hsiao-Yun Lo
論文名稱：	銅鈀奈米粒子之合成及其在無電鍍銅之應用 The Synthesis of Cu/Pd Nanoparticles and Its Application to Electroless Copper Deposition
指導教授：	王詠雲 Yung-Yun Wang 萬其超 Chi-Chao Wan
口試委員:
學位類別：	博士 Doctor
系所名稱：	工學院 - 化學工程學系 Department of Chemical Engineering
論文出版年：	2008
畢業學年度：	96
語文別：	英文
論文頁數：	114
中文關鍵詞：	奈米粒子、無電鍍銅、觸媒、X光吸收光譜
外文關鍵詞：	nanoparticle, electrless copper deposition, catalyst, EXAFS
相關次數：	點閱：4 下載：0
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Cu/Pd bimetallic nanoparticles have been successfully synthesized in the ambient condition with the aid of complexing agent, trisodium citrate and EDTA. XRD and XPS results show low degree of oxidation in Cu/Pd nanoparticles in citrate and EDTA systems. The TEM images reveal that the synthesized nanoparticles were well-dispersed and about 5 nm in diameter. The quenched XANES method was employed to investigate the formation mechanism of Cu/Pd nanoparticles with citric complexing agent. Two-stage and three-stage mechanisms were proposed for Cu/Pd molar ratio = 1/1 and 1/2 systems, respectively. The former was expected to have more Cu on surface while the latter had Pd enriched on surface. The Cu/Pd nanoparticles synthesized with citric complexing agent in different molar ratios were further tested as activator for electroless copper deposition. The nanoparticles with Cu/Pd = 1/2 was found to have catalytic ability comparable to traditional Pd/Sn colloid or pure Pd activator among all the bimetallic Cu/Pd systems. The most concerned long-term stability of Cu/Pd nanoparticles was investigated by XANES. Although slow Pd oxidation and Cu dissolution were found in Cu/Pd colloidal solution when exposed to air, the stability of these Cu/Pd nanoparticles was still acceptable in industrial application. In short, stable Cu/Pd nanoparticles have been successfully synthesized with citric complexing agent and showed high potential to be applied as activator in electroless copper deposition.

本文主要探討水溶液中銅鈀奈米粒子的合成，此合成方法是透過添加檸檬酸或EDTA錯合劑至前驅鹽溶液中，使形成穩定的金屬錯合離子後，以甲醛還原金屬錯合離子成奈米級金屬微粒，以高分子型(PVP)保護劑形成立體障礙防止合成的粒子聚集沉澱。錯合劑除了改變金屬離子的還原電位外，亦可有效防止氫氧化物雜質的產生。
經過穿透式電子顯微鏡的觀察，以檸檬酸錯合劑合成的銅鈀奈米粒子分散尤其良好，並具有均一的粒徑分布(3 nm ~ 4 nm)，X光粉末繞射結果發現此奈米粒子確實是以雙金屬的型態存在。根據電子能譜儀的結果顯示，合成的銅鈀奈米粒子在表面上有些微的氧化，其氧化可能的原因為與保護劑的化學鍵結或是受氧氣的氧化所造成，然此奈米粒子的內部仍維持金屬的還原態。經過X光吸收光譜的分析，可以推測出可能的金屬錯合離子還原機構，不同的金屬前驅鹽比例會以不同的機制進行還原反應。在銅鈀比為1：2的系統中，還原反應主要可分為三部分，第一為鈀錯離子的成核，第二階段為銅錯離子還原及少量的鈀金屬還原，待大量的銅離子還原完後，進入還原反應的第三個階段，溶液中只剩鈀錯離子可繼續進行反應，最終有效形成較多鈀分布在表面的奈米粒子，此種奈米粒子具有較低的貴金屬鈀含量而仍具有鈀金屬的高催化活性。在銅鈀比為1：1的系統中，還原反應主要可分為二步驟，先為鈀核的形成而後為銅離子在鈀核上還原，因而形成以銅金屬為主的外層結構。
將此種銅鈀奈米粒子應用在無電鍍銅的催化上，可以較簡便的流程進行無電鍍銅之催化反應，除了鈀金屬的含量之外，奈米粒子的外層結構或是PVP層包覆的型態亦有可能影響最終的催化鍍銅效果。銅鈀比為1:2的系統具有最高的催化活性，其催化鍍銅效率與傳統錫鈀膠體或是純鈀金屬相當。此外，此種銅鈀奈米粒子具有相當的穩定度，曝露在空氣中雖會有緩慢的鈀氧化與銅溶解現象，但仍具有穩定的懸浮能力與催化活性。整體而言，以檸檬酸錯合劑合成之銅鈀奈米粒子具有相當高的應用潛力。

誌謝辭    I
ABSTRACT    II
摘要    III
TABLE OF CONTENTS    V
LIST OF TABLES    VIII
LIST OF FIGURES    IX
CHAPTER 1
INTRODUCTION TO NANOPARTICLES AND THEIR POTENTIAL APPLICATION    1
1 INTRODUCTION    1
2 SYNTHESIS OF METAL NANOPARTICLES    2
2.1 Electrochemical Synthesis    2
2.2 Sonochemical synthesis    4
2.3 photochemical synthesis    5
2.4 Wet-Chemical Synthesis with Reducing Agent    8
2.5 Synthesis of bimetallic nanoparticles    12
3 STABILIZATION MECHANISM OF METAL NANOPARTICLES    14
3.1 Electrostatic Stabilization    14
3.2 Streric Stabilization    16
4 CHARACTERIZATIONS OF METAL NANOPARTICLES    23
4.1 Ultraviolet/Visible Absorption Spectroscopy (UV/vis spectroscopy)    23
4.2 Fourier Transform Infrared (FT-IR) spectroscopy    24
4.3 Transmission Electron Microscopy (TEM) Observation    26
4.4 X-ray Diffraction Method    27
4.5 X-ray Photoelectron Spectroscopy    29
4.6 X-ray Scattering Method    31
4.7 X-ray Absorption Method    33
5 APPLICATION OF METAL NANOPARTICLES    37
5.1 Application for C-C coupling reactions    37
5.2 Application for Hydrogenation reactions    40
6 BRIEF REVIEW ON THE SYNTHESIS AND APPLICATION OF METAL NANOPARTICLES IN THE ELECTROCHEMISTRY LAB OF TSING-HUA UNIVERSITY    42
6.1 Electroless Copper Deposition    42
6.2 Application to Fuel Cell and Solar Cell    46
7 MOTIVATION    48

CHAPTER 2
SYNTHESIS OF CU/PD BIMETALLIC NANOPARTICLES WITH COMPLEXING AGENT    50
1 INTRODUCTION    50
2 EXPERIMENTS    52
2.1 Preparation of Cu/Pd Nanoparticles    52
2.2 Characterization of Cu/Pd Nanoparticles    52
2.3 Electroless Copper Deposition and Determination of Catalytic Ability    53
3 RESULTS AND DISCUSSIONS    55
3.1 Confirmation of Complexation between Metal Ions and Complexing Agents    55
3.2 Preparation and Characterization of the Cu/Pd Nanoparticles    56
3.3 Catalytic Ability of Cu/Pd Nanoparticles for Electroless Copper Deposition    67
4 CONCLUSION    72
CHAPTER 3
XAS STUDY ON FORMATION MECHANISM AND PARTICLE STRUCTURE    73
1 INTRODUCTION    73
2 EXPERIMENTS    75
2.1 Sample Preparation for quenched XANES Measurements    75
2.2 XAS Measurements    75
3 RESULTS AND DISCUSSIONS    77
3.1 XANES investigation on metal complexing ions    77
3.2 Formation mechanism of Cu/Pd (1/2) Nanoparticles from quenched XANES    78
3.3 Formation mechanism of Cu/Pd (1/1) Nanoparticles from quenched XANES    82
4 CONCLUSIONS    86
CHAPTER 4
FEASIBILITY AND LONG-TERM STABILITY TESTS OF CU/PD NANOPARTICLES FOR ELECTROLESS COPPER DEPOSITION    87
1 INTRODUCTION    87
2 EXPERIMENTS    89
2.1Preparation of Nanoparticles    89
2.2 Electroless Copper Deposition    89
2.3 Electrochemical Measurements    90
2.4 Sampling and Characterization Method of Long-term Stability    90
3 RESULTS AND DISCUSSIONS    92
3.1 Electroless Copper Deposition    92
3.2 Electrochemical measurement    98
3.3 Long-term Stability and Long-term Catalytic Ability    99
4 CONCLUSIONS    105
CHAPTER 5    106
CONCLUSIONS AND FUTURE WORK    106
1 CONCLUSIONS    106
2 FUTURE WORK    108
REFERENCE    109
ABOUT THE AUTHOR    114

                                

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