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研究生：	高子軒 Kao, Tzu-Hsuan
論文名稱：	應用於下世代微電子連接點線之奈米金屬粒子相變態行為研究 Study on Phase Transformation of Metallic Nanoparticles for Next Generation Microelectronic Interconnections
指導教授：	陳引幹 Chen, In-Gann
學位類別：	博士 Doctor
系所名稱：	工學院 - 材料科學及工程學系 Department of Materials Science and Engineering
論文出版年：	2010
畢業學年度：	98
語文別：	中文
論文頁數：	142
中文關鍵詞：	金屬奈米粒子、奈米尺度效應、相變態、合金化
外文關鍵詞：	metallic nanoparticle, nanosized effect, phase transformation, alloying
相關次數：	點閱：86 下載：0
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當前微電子構裝發展重要趨勢之一，為應用奈米粒子低熔點特性，將其製備為奈米金屬墨水，經低溫熱處理即可獲得高性能之微導線與微接點。搭配高精準度噴墨技術，將可獲得所需圖案，無須使用繁複之微影製程。為傳輸電流與訊號，奈米金屬沈積物必須充份融合固化，並且須與元件接點產生緊密接合。本論文以Brust-Schiffrin兩相法所製備、以烷基硫醇為保護劑之金、銀以及銀-金合金(Ag3Au)奈米粒子為實驗材料，探討其於升溫過程中之相變現象，並系統性調查奈米粒子沈積物與常用電子金屬基材間之介面反應，期藉此開拓奈米尺寸誘發之液態金屬過冷與固化驅動力等相變態學理探討新領域。
本論文研究主題可以區分為三大部分。第一部份以奈米金粒子為實驗材料，探討奈米粒徑對金屬顆粒熔化行為效應。分別利用熱分析圖譜、微結構演變、電阻率變化以及表面電漿共振吸收行為等不同觀點驗證其奈米金屬粒子之相轉變溫度。同時藉由臨場觀察同步輻射X光繞射峰值隨溫度上升之變化，進一步證實金奈米粒子之低溫熔融與固化行為。
第二部分，探討奈米尺度效應對金奈米粒子沈積物與基材間合金化行為之影響。藉由SEM、SIMS、ESCA與拔膜測試等實驗方法，研究金奈米粒子和濺鍍金薄膜分別與不同基材介面反應組成物以及接合強度之差異，亦利用介面組成化學鍵結的位移證明此低溫合金化行為。
第三部分將系統性探討不同組成奈米金屬與合金粒子披覆物與電子金屬基材間之介面反應。將金、銀與金-銀合金奈米粒子，披覆於電子金屬基材，如銀、銅與鎳等，對金屬間互擴散與合金化行為進行系統性調查，實驗發現反應層組織相及厚度除取決於奈米金屬粒子中合金種類與比例，以及其與塊狀基材間金屬物理與化學性質差異，包括晶格匹配度、陰電性差異以及混和焓等影響。總而言之，本研究觀察奈米尺度誘發之低溫熔融以及後續發生之合金化與凝固現象，從冶金和熱力學的觀點，提出機制說明。

By utilizing the drastically reduced melting temperature of nano-sized particles (NPs), one of recent developments in microelectronic packaging is to manufacture highly conductive interconnections with metallic nanoparticle deposits subjected to a low temperature process. With the emerging technology of inkjet printing system, nano-size metallic NP suspensions can be applied to fabricate electrical line patterns without using conventional lithography. For the transportation of power and signal, the nanoparticle deposits should be consolidated and well jointed with the contacts of the devices. This study systematically investigated the low temperature melting, solidification and alloying of Au, Ag and Ag3Au nanoparticle deposits. The interaction between the metallic NPs and electronic substrates will be also explored. By doing so, the phase transformation issues such as the supercooling, latent heat difference, and driving force for solidification resulted from nanosized effects will be well understood.
This presenting thesis can be divided into three parts: First, the low temperature melting and subsequent solidification of Au nanoparticles was investigated. The temperature of phase transformation was examined by thermal analyses, microstructure evaluation, resistance measurement and surface plasma resonance shifts. Through monitoring the evolution of diffraction peaks as function of temperature using in situ synchrotron X-ray diffraction, the low temperature melting behavior of gold nanoparticles was further manifested.
Secondly, the alloying behavior between gold nanoparticle deposits and metallic substrates due to nano-sized effect was examined. The differences in interfacial products and adhesion strength between gold nanoparticles deposits and those of sputtered gold thin-film were studied by means of SIMS, ESCA and pull-off test. In addition, the chemical shifts of the reaction products proved the phenomenon of low temperature alloying.
In the third part, the interfacial reactions between nanoparticle deposits of different compositions (Au, Ag and Ag3Au) and metallic substrates of Ag, Cu and Ni were systematically investigated. It was examined that the phase and thickness of reaction layers were not only determined by the composition of the deposited nanopartilces but the differences of physical and chemical properties between the nanoparticles and substrate materials, including lattice mismatch, electronegativity difference and mixing enthalpy of the alloying systems involved. From the viewpoints of metallurgical and thermodynamic, the nano-sized induced successive behaviors of low temperature melting, alloying and solidification were demonstrated in this study.

摘要...................................I
Abstract..............................III
致謝...................................V
目錄...................................VII
表目錄.................................XII
圖目錄.................................XIII

第一章	緒論	1
1-1奈米結構簡介	1
1-2奈米粒子的特性與應用	2
1-3噴墨製程現況	4
1-4研究動機與目的	5
第二章	理論基礎與文獻回顧	11
2-1 常見的奈米金屬粒子製備方式	11
2-1-1 共沈澱合成法	11
2-1-2 溶膠合成法	13
2-1-3 微乳化合成法	14
2-1-4 模板合成法	15
2-2金屬奈米粒子的發展歷史與其應用於微電子導線之現況	17
2-2-1金奈米粒子	17
2-2-2銀奈米粒子	18
2-2-3銅奈米粒子	20
2-2-4	銅基合金與複合奈米粒子	22
2-3金屬間物理與化學性質	23
第三章 實驗流程與儀器設備	48
3-1藥品名稱	48
3-2實驗流程	50
3-2-1反應前驅物與奈米金屬粉末的合成	50
3-2-1-1合成四氯氫金	50
3-2-1-2合成以正辛基硫醇作為保護劑之金奈米粒子	51
3-2-1-3合成以正辛基硫醇作為保護劑之金-銀合金奈米粒子	52
3-2-1-4合成以正辛基硫醇作為保護劑之銀奈米粒子	53
3-2-2奈米金屬粒子旋轉批覆前基板清洗步驟與披覆參數	53
3-2-2-1矽基板	53
3-2-2-2純金屬以及金屬鍍膜基板	54
3-2-2-3旋轉披覆參數	54
3-3量測與分析設備	55
3-3-1解析型掃描穿透式電子顯微鏡	55
3-3-2掃描式電子顯微鏡	56
3-3-3原子力探針顯微鏡	56
3-3-4低掠角X光繞射儀	56
3-3-5紫外/可見吸收光譜儀	58
3-3-6臨場同步輻射X光繞射儀	58
3-3-7化學分析電子能譜儀	59
3-3-8歐傑電子能譜儀	60
3-3-9表面粗度儀	61
3-3-10熱重分析儀	62
3-3-11四點探針	62
3-3-12拔膜測試	63
3-3-13奈米壓痕測試	63
第四章 實驗結果與討論	71
4-1奈米金屬粒子性質鑑定	71
4-1-1穿透式電子顯微鏡	71
4-1-2表面電漿共振吸收	71
4-2奈米金屬粒子低溫熔融行為	73
4-2-1熱性質分析	73
4-2-1-1 金奈米粒子	73
4-2-1-2 銀奈米粒子	73
4-2-1-3 銀-金合金(Ag3Au)奈米粒子	74
4-2-2後熱處理對微結構與形貌之影響	75
4-2-3後熱處理對表面電漿共振吸收以及電阻率變化之影響	75
4-2-4臨場同步輻射X光繞射	77
4-3 奈米尺度效應對金奈米粒子沈積物與基材合金化之影響	79
4-3-1奈米尺度效應對表面型態之影響	79
4-3-2奈米尺寸效應對介面擴散反應之影響	80
4-3-2-1介面原子互擴散	80
4-3-2-2 奈米尺度效應對介面接合強度之影響	82
4-3-3介面組成與化學鍵結之關係	82
4-4不同組成奈米金屬粒子與基材介面相變態行為	85
4-4-1表面形貌及與介面接合情形觀察	85
4-4-2奈米金屬粒子沈積物與銀基材	86
4-4-3奈米金屬粒子沈積物與鎳基材	86
4-4-4奈米金屬粒子沈積物與銅基材	89
4-4-5介面反應物機械性質	90
4-5奈米尺度誘發低溫合金化行為	93
第五章 結論	127
參考文獻	…………………………………………………...130
作者自述	…………………………………………………141

 
表目錄
Table 2-1 Recent progress of metallic nanoparticles ink.	25
Table 2-2 Properties of the noble alloy systems involved.	26
Table 4-1 The thermal signals derived from DSC and TGA of different metallic NPs.	94
Table 4-2 The resistivity of NPDs film before and after different heat treatment conditions. (unit: μΩ cm)	94
Table 4-3 Average roughness (Ra) of the samples cured at various temperatures for 60 minute (unit: nm).	94
Table 4-4 Thickness of each interfacial reaction layers and ratios of atomic concentration obtained from SIMS and XPS depth profiling, respectively.	95
Table 4-5 List of referenced XPS core level binding energies and their sensitivity factors	95
Table 4-6 Electron binding energy (ΔEb) of each corresponding core level spectra measured on the surface after sputter etching	96
Table 4-7 Metallurgical features occurred in different NPD/substrate systems.	97

圖目錄
Figure 1-1 (a) The melting point of Au nanoparticles with increasing diameters and (b) Schematic diagrams of metallic nanoparticles with lower melting/sintering temperature to form conductive network with frequent surface contacts in comparison with micro-sized metallic particles (left) with less contact areas.	8
Figure 1-2 Schematic diagram of using metallic nanoparticles a interconnecting materials.	9
Figure 1-3 Simulation results of Au nanoparticles reacting with Ag substrates under 400K as function of time.	9
Figure 1-4 (Left) Relationship between the radius of the as-synthesized SnAg alloy nanoparticles and their corresponding melting points and heat of fusion, respectively. (Right) SEM image of the cross-section of the wetted SnAg alloy nanoparticles on the cleaned copper foil.	10
Figure 2-1 The structure of reverse micelle proposed by Schulman et al in 1943.	27
Figure 2-2 The chemical structure of CTAB.	27
Figure 2-3 Schematics of microemulsion synthetic method for fabricating metallic nanoparticles.	28
Figure 2-4 The evolution of the morphology of nanoparticles with increasing proportion of water phase in the system under constant concentration of Cu(AOT)2 proposed by Pileni and Tanori in 1997.	29
Figure 2-5 Schematic diagrams of supercritical fluids replacing water-oil microemulsion synthetic method.	30
Figure 2-6 Schematics of fabricating copper nanoparticles using supercritical fluids by Korgel et al.	30
Figure 2-7 The TEM images of copper oxide nanoparticles using supercritical fluids with surfactant: (a) high resolution and low resolution of (b) and (c).	31
Figure 2-8The TEM images of thiol protected copper nanoparticles using supercritical fluids: (a) high resolution and (b) low resolution .	32
Figure 2-9 The gold nanoparticles fabricated via the templates of PAH/PAA multilayer 	33
Figure 2-10 Arrangement of core-shell Au@SiO2 structure using photo-resist template 	34
Figure 2-11 Schematic diagram of Brust-Schiffrin method fabricating gold nanoparticles.	35
Figure 2-12 Schematic diagram do fabricating functionalized gold nanoparticles using different surfactants.	35
Figure 2-13 (a) Atomic force micrograph of an inkjetted line. (b) Optical micrographs of an inkjetted inductor formed on commercial polyester-based general purpose transparency plastic.	36
Figure 2-14 (a) Light microscopy images of a cured line by laser, (b) AFM scanned image of (a), and (c) its cross section.	36
Figure 2-15 TEM images of dodecanethiol-protected silver nanoparticles : (left) low magnification (right) high resolution 2-D arrangement.	37
Figure 2-16 (Left) Diagram of the piezo drop-on-demand ink-jet printing system. (Right) Optical micrograph of an ink-jet printed resonant inductive coil .	37
Figure 2-17 TEM micrographs of decanoate-protected silver nanoparticles. (a) Ensemble of silver nanoparticles with a histogram showing the respective size distribution. Selected area electron diffraction pattern is shown in the inset. (b) The top view and (c) cross section SEM morphology of the cured silver film on Si wafer.	38
Figure 2-18 (a) Schematic diagram illustrating omnidirectional printing and optical image of apparatus used (inset). (b) Transmission electron microscopy image of the synthesized silver nanoparticles and optical image of the concentrated ink (inset). (c) Shear elastic modules as a function of shear stress for silver nanoparticle inks of varying solids loading.	39
Figure 2-19 The TEM image of dodecanethiol-protected Cu nanoparticles using standard Brust-Schiffrin two phase method by Aslam et al .	40
Figure 2-20 The TEM image of hexanethiol-protected Cu nanoparticles using modified Brust-Schiffrin two phase method with organic phase of THF by Chen and Sommers et al.	41
Figure 2-21 The TEM image of octanethiol-protected Cu nanoparticles using modified Brust-Schiffrin two phase method by Chin et al .	41
Figure 2-22 (a) Resistivity of the Cu conductive film as a function of heat treatment temperature. The ink-jet printed Cu nanoparticulate films were heat-treated at various temperatures between 200oC and 325oC under vacuum (10-3 Torr). (b) SEM image showing the microstructure of the Cu film heat-treated at 325oC. The insets show high-magnification SEM images of the as-synthesized Cu nanoparticles prior to sintering. All scale bars=500 nm.	42
Figure 2-23 High resolution TEM picture of Ag/Cu alloy nanoparticles.	43
Figure 2-24 (a) HR-SEM images of the printed patterns heated under N2 at various temperatures. (b) Schematic illustration of the growing silver crystallites forming the shell. (c) The resistivity calculated for printed patterns (on glass) heated under N2 as a function of temperature.	43
Figure 2-25 (a) The comparison between the calculated packing density based on the Furnas model and the experimentally measured annealed density for the films prepared with various mixing ratios of Cu/Ag. (b) The resistivity variation as a function of annealing temperature for the mixed metal films with various Cu/Ag mixing ratios. The inset shows the resistivity of the Cu/Ag) 3:1 film prepared with larger silver nanoparticles (50 nm). (c) SEM images showing the microstructure of pure Cu (the upper) and Cu/Ag) 3:1 mixed film (the lower) annealed at 175, 250, and 325oC for 90 min. Arrows indicate the presence of Ag particles between Cu particles. All scale bars=100 nm.	44
Figure 2-26 Phase diagram of Au-Ag alloy system.	45
Figure 2-27 Phase diagram of Au-Cu alloy system.	45
Figure 2-28 Phase diagram of Ag-Cu alloy system.	46
Figure 2-29 Phase diagram of Au-Ni alloy system.	46
Figure 2-30 Phase diagram of Ag-Ni alloy system.	47
Figure 3-1 Synthesis steps of different compositions metallic nanoparticles of different compositions.	65
Figure 3-2 Experimental flow chart.	66
Figure 3-3 The diagram of measuring the average roughness at distance L .	66
Figure 3-4 The diagram displaying the relationship between lattice diffraction and Bragg Law.	67
Figure 3-5 The diagram of Grazing Incident X-ray diffraction	67
Figure 3-6 The diagram showing the excitation of surface plasmons by light is denoted as a surface plasmon resonance (SPR) for nanometer-sized metallic structures.	68
Figure 3-7 The wavelength of synchrotron radiation ranges.	69
Figure 3-8 Schematic diagrams of nanoindentation: (a) the progress of loading and unloading and (b) load-displacement curve.	70
Figure 4-1 (a) TEM image and (b) the size distribution of the Au nanoparticles used in this study.	98
Figure 4-2 (a) TEM image and (b) the size distribution of the Ag nanoparticles used in this study.	98
Figure 4-3 (a) TEM image and (b) the size distribution of the Ag3Au NPs used in this study.	98
Figure 4-4 UV-visible absorption spectra of octanthiol protected nanoparticles in chloroform with nominal formulas of Ag, Ag3Au and Au, respectively.	99
Figure 4-5 (a) TGA and (b) DSC thermal curve of the Au NPs used in this study.	100
Figure 4-6 (a) TGA and (b) DSC thermal curve of the Ag NPs used in this study.	101
Figure 4-7 (a) TGA and (b) DSC thermal curve of the Ag3Au NPs used in this study.	102
Figure 4-8 SEM morphology of spin-coated film after drying: (a) Au, (b) Ag3Au and (c)Ag nanoparticles.	103
Figure 4-9 SEM morphology of Au, Ag and Ag3Au NPs subjected to different curing temperatures for 20 minutes. The insert scale bar=200nm.	104
Figure 4-10 (a) UV-visible absorption spectra and (b) surface plasma resonance shifts with respect to sheet resistance of spin-coated Au NPs films on Si wafer as function of different curing temperatures.	105
Figure 4-11 (a) UV-visible absorption spectra and (b) surface plasma resonance shifts with respect to sheet resistance of spin-coated Ag NPs films on Si wafer as function of different curing temperatures.	106
Figure 4-12 (a) UV-visible absorption spectra and (b) surface plasma resonance shifts with respect to sheet resistance of spin-coated Ag3Au NPs films on Si wafer as function of different curing temperatures.	107
Figure 4-13 The change of Au (111) diffraction peak with respect to heating temperature.	108
Figure 4-14 TGA and DSC curves of the Au NPs and the integrated intensity of the Au (111) diffraction peak with increasing temperature.	108
Figure 4-15 AFM topography pictures of the Au deposit on the Ag substrate cured at various temperatures for 60 min: (a) 200oC, (b) 250oC and (c) 300oC.	109
Figure 4-16 AFM topography pictures of the Au deposit on the Cu substrate cured at various temperatures for 60 min: (a) 2000C, (b) 2500C and (c) 3000C.	110
Figure 4-17 AFM topography pictures of the Au deposit on the Ni substrate cured at various temperatures for 60 min: (a) 2000C, (b) 2500C and (c) 3000C.	111
Figure 4-18 Comparison of the SIMS depth profiles between the Au NP deposits and sputtered films of each system: (a) Au–Ag, (b) Au–Cu and (c) Au–Ni. (NPD: nanoparticle deposit, SF: sputtered film.)	112
Figure 4-19 Adhesion strength of the Au deposits on Cu, Ag and Ni substrates under different curing conditions in comparison with sputtered films with or without heat treatment at 300oC for 60 min. (NPD: nanoparticle deposit, SF: sputtered film.)	113
Figure 4-20 Atomic concentrations at the interface between the Au NP deposit and substrates via XPS depth profiling as a function of sputtering time and depth after different isothermal time: (a) Au–Ag, (b) Au–Cu and (c) Au–Ni.	114
Figure 4-21 Photoemission spectra of (a) Au 4f and (b) Ag 3d levels obtained from the surface after sputter-etching for 400s at the interface between the Au deposits and Ag substrates.	115
Figure 4-22 Photoemission spectra of (a) Au 4f and (b) Cu 2p levels obtained from the surface after sputter-etching for 400s at the interface between the Au deposits and Cu substrates.	116
Figure 4-23 Photoemission spectra of (a) Au 4f and (b) Ni 2p levels obtained from the surface after sputter-etching for 400s at the interface between the Au deposits and Ni substrates.	117
Figure 4-24 X-ray diffraction patterns of Au NPs deposits on Cu substrate under different curing conditions. (NPD: nanoparticle deposit.)	118
Figure 4-25 Surface and cross-sectional morphologies of the cured Au NPD on different substrates: ((a), (d)) Ag substrate; ((b), (e)) Cu substrate and ((c), (f)) Ni substrate.  The curing was performed at 300oC for 60 min.	119
Figure 4-26 Surface and cross-sectional morphologies of the cured Ag3Au NPD on different substrates: ((a), (d)) Ag substrate; ((b), (e)) Cu substrate and ((c), (f)) Ni substrate.  The curing was performed at 300oC for 60 min.	120
Figure 4-27 Surface and cross-sectional morphologies of the cured Ag NPD on different substrates: ((a), (c)) Cu substrate and ((b), (d)) Ni substrate. The curing was performed at 300oC for 60 min.	121
Figure 4-28 Atomic concentrations via AES depth profiling from the surface of the reacted Au and Ag3Au NPDs into (a) Ag, (b) Ni and (c) Cu substrates. (d) Atomic concentrations from the surface of the reacted Ag NPDs into the Cu and Ni substrates. All the data were examined after being cured at 300oC for 60 min. (NPD: nanoparticle deposit)	122
Figure 4-29 In situ XRD spectra showing Au (111) and Au3Ni (111) peaks as function of heating temperature.	123
Figure 4-30 X-ray diffraction patterns of the NPDs on Cu substrates. All the data were examined after being cured at 300oC for 60 min. (NPD: nanoparticle deposit)	123
Figure 4-31 Schematic of the calculation of the interdiffusion coefficient by the Matano method.	124
Figure 4-32 Schematic diagram of the chemical potential gradient in the apparent width of two-phase region [88].	124
Figure 4-33 Adhesion strength of NPDs on different substrates after curing under 300oC for 60minutes.	125
Figure 4-34 Hardness and Young's modulus of the reaction layers of Au, Ag and Ag3Au NPDs reacted with different substrates.	125
Figure 4-35 Schematic illustrations of the alloying behavior between the NPD and the bulk substrate at elevated temperatures.	126
                                    

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