臺灣博碩士論文加值系統

本研究主要探討純銅及七三黃銅於磷酸水溶液中之電解拋光行為。純銅電解拋光方面是以純鈦所製作之旋轉圓柱電極於不同硫尿含量之酸性硫酸銅鍍液中電鍍後所得之電鍍銅。研究結果顯示，所獲得之電鍍銅硬度隨鍍液中添加之硫尿添量增加而提升，此乃因鍍液添加硫尿所獲得電鍍銅具較細小晶粒所致。由顯微組織觀察時發現，於含硫尿添加劑鍍液中所得之銅鍍層組織裡有少數含富硫粒子。電鍍銅在磷酸電解液中電解拋光時，此富硫粒子會優先解離，並於銅鍍層表面生成一含磷的非結晶相。研究亦發現添加硫尿之鍍液中所得銅鍍層於電解拋光時有較高之陽極解離電流，且於拋光後可達到整平與亮化之表面，其表面粗度(Ra)值小於30 nm。
黃銅電解拋光研究方面，則採用市售之七三黃銅製成旋轉圓盤及旋轉圓柱電極試片，於70%磷酸水溶液中進行電化學測試與電解拋光，探討其電解拋光行為。旋轉圓盤電極方面，陽極極化測試結果顯示於活性解離區與極限電流區之間具有一過渡電流峰，同時於電極表面亦發現有一藍色之富銅離子層。研究結果顯示，此富銅離子層會阻礙陽極解離速率且為電解拋光時整平之必要條件。經光學顯微鏡及掃描式電子顯微鏡觀察電解拋光黃銅之表面形貌，發現於電流峰值區域之電位下電解拋光時，會產生晶界優先解離的現象。而於極限電流區中段電位下電解拋光結果則有極佳之效果。若於極限電流區後段電位下，以低轉速進行電解拋光則會於試片表面產生乳突狀及流紋形貌。此兩種表面形貌之生成主要是產生氧氣氣泡所導致，其形成可能機制亦於本研究中提出。旋轉圓柱電極之測試結果與旋轉圓盤電極相同，旋轉圓柱電極表面所形成之富銅離子層仍為整平之要素。且此富銅離子層於電解拋光時可完整包覆旋轉圓柱電極表面，因此旋轉圓柱電極之拋光效果較旋轉圓盤電極佳。當旋轉圓柱電極以每分鐘100轉以下之轉速進行電解拋光時，可觀察到此富銅離子層有爬桿的現象，此爬桿現象也在本研究中詳細討論並提出其相關之機制。

The aim of this study is to investigate the electropolishing behavior of pure Cu and cartridge brass. Pure Cu specimen was electroplated on a rotating cylindrical Ti electrode in Cu-sulphate plating baths with different thiourea contents. The hardness variation, microstructures and electropolishing behavior of the Cu deposits were studied. Experimental results show that some sulphur-rich particles were identified in the Cu deposits prepared from the thiourea-containing baths. The sulphur-rich particles dissolved preferentially during electropolishing in a 40 vol.% H3PO4 solution, forming a thin amorphous phase containing P in patches on the outer surface of the Cu deposit. The Cu deposits prepared in the baths with thiourea showed higher anodic dissolution current during electropolishing and formed a brightened and levelled surface with a surface roughness (Ra) lower than 30 nm.
The electropolishing behaviour of cartridge brass in a 70 vol.% H3PO4 solution was studied using a rotating disc electrode (RDE). Based on the results of an anodic polarization test, a transition peak varying from kinetic-controlled to diffusion-controlled dissolution was detected when a blue Cu2+-rich layer was developed on the RDE. The blue Cu2+-rich layer impedes the anodic dissolution rate of the brass-RDE and is essential for levelling during electropolishing. Potentiostatic polishing at different locations on the limiting-current plateau was studied. By polishing at the transition-peak potential, grain boundaries were preferentially etched. In contrast, a well-polished surface with a nanosized surface roughness (Ra) was achieved after electropolishing in the middle of the limiting-current plateau. By polishing at the end of the limiting-current plateau at a relatively low rotational speed, nipple-like and flow-streak features were observed. The formation of these features is attributed to the evolution of oxygen bubbles on the RDE surface. Mechanisms for the formation of the above-mentioned features were also proposed in this study.
The electropolishing behaviour of cartridge brass in a 70 vol.% H3PO4 solution was also studied using a rotating cylinder electrode (RCE). The same results of the study with RDE, the Cu2+-rich layer is necessary for leveling the brass-RCE. The electropolishing effect on the RCE is relatively easy to achieve, because a full coverage of the Cu2+-rich layer on the RCE surface was seen during electropolishing. A rod-climbing phenomenon of the Cu2+-rich layer was observed when electropolishing the brass-RCE at a rotational speed above 100 rpm. The formation mechanism of rod-climbing was discussed and proposed in this study.

Table of Contents

Chinese abstract iii
English abstract v
Table of contents vii
List of tables x
List of figures x

Chapter 1 Introduction 1
1.1 Cu and Cu alloys 1
1.2 Classification 2
1.3 Electroplated Cu deposit 3
1.4 Brass 4
1.5 Surface polishing 5
1.5.1 Mechanical polishing 5
1.5.2 Polishing facilities 7
1.5.3 Chemical mechanical polishing/planarization 7
1.6 Electrochemical polishing 8
1.6.1 General aspects of electrochemical polishing 9
1.6.2 Construction of electrochemical polishing cell 10
1.6.3 Electrochemical polishing mechanisms 11
1.7 Surface character 12
1.7.1 Roughness and waviness 13
1.7.2 Surface modification 13
1.7.3 Evaluation of a polished surface 14
1.8 Objective of the investigation 14
Chapter 2 Experimental procedure and test methods 16
2.1 Specimen preparation and cell design 16
2.2 Anodic polarization test and potentiostatic polishing 17
2.3 Surface morphology and microstructure examination 18
2.3.1 Scanning electron microscopy (SEM) 18
2.3.2 Transmission electron microscope (TEM) 19
2.3.3 Atomic force microscopy (AFM) 19

Chapter 3 The electropolishing behaviour and microstructures of electroplated Cu deposits 20
3.1 Introduction 20
3.2 Experimental procedure 21
3.3 Results and discussion 23
3.3.1 Electroplating and hardness test 23
3.3.2 Microstructure study 24
3.3.3 Electropolishing behaviour of Cu deposits 27
3.4 Conclusions 30

Chapter 4 The electropolishing behaviour of cartridge brass in a 70 vol.% H3PO4 solution 31
4.1 Introduction 31
4.2 Experimental procedure 32
4.3 Results and discussion 34
4.3.1 Electropolishing behavior of cartridge brass with RDE 34
4.3.1.1 Anodic polarisation behavior 34
4.3.1.2 Potentiostatic polishing on the limiting-current plateau 35
4.3.1.3 Formation of nipple-like and flow-streak features 37
4.3.1.4 Electropolishing mechanism 40
4.3.2 Electropolishing behavior of cartridge brass with RCE 43
4.3.2.1 Anodic polarisation behavior 43
4.3.2.2 Potentiostatic polishing on the limiting-current plateau 44
4.3.2.3 The Cu2+-rich layer on the stagnating RCE 46
4.3.2.4 The Cu2+-rich layer on the rotating RCE 48
4.3.2.4 The rod-climbing behavior 50
4.4 Conclusions 51
4.4.1 Electropolishing with brass-RDE 51
4.4.2 Electropolishing with brass-RCE 51

Chapter 5 Future work 53

Reference 54













List of tables
Table 1.1 Copper alloys and alloying elements [3] 64
Table 1.2 Generic classifications of copper alloys [3] 64
Table 3.1 Surface roughness values, Ra values, of Cu deposits prepared in the Cu-plating baths with different thiourea concentrations after electropolishing in the 40 vol.% H3PO4 solution. 65

Table 5.1 Electropolishing potentials applied to brass-RDEs at different rotational speeds 65
Table 5.2 Electropolishing potentials applied to brass-RCEs at different rotational speeds 65

List of figures
Fig. 1.1 The hardness variation of the copper deposits after 350 oC annealing for 30 min and in relation with various contents of thiourea in the plating bath [18] 66
Fig. 1.2 Schematic sketch of the structure observed for an abraded OFHC Copper surface [34] 67
Fig. 1.3 Electrochemical polishing mechanisms proposed by Jacquet [45] 68
Fig. 1.4 Electrochemical polishing mechanisms proposed by Elmore [51] 69
Fig. 1.5 Electrochemical polishing mechanisms proposed by Baumann and Ginsberg [52] 70
Fig. 1.6 Electrochemical polishing mechanisms proposed by Edward et al. [55,56,68,69] 71
Fig. 2.1 Schematic sketch of the rotating disc electrode (RDE) 72
Fig. 2.2 Schematic sketch of the rotating cylinder electrode (RCE) 73
Fig. 3.1 Variation of cathodic overpotential during electroplating at 70 Adm-2 in the Cu-sulphate plating bath 74
Fig. 3.2 Hardness and standard deviation values of Cu deposits prepared in the Cu-plating baths with different thiourea concentrations 75
Fig. 3.3 TEM observations of twin-jet etched Cu deposits prepared in plating baths (a)without and (b) with 8 ppm thiourea 76
Fig. 3.4 (a) and (b); TEM micrographs of twin-jet etched Cu deposit prepared in a bath with 3 ppm thiourea. (c) and (d) ; EDS analysis of positions of A (c), and B (d) shown in figure (b) 77
Fig. 3.5 TEM micrographs of ion-milled Cu deposits prepared in the Cu-plating baths with (a) 1, (b) 5, and (c) 8 ppm thiourea ; (d) EDX analysis on the particles indicated by arrow shown in figure (c) 78
Fig. 3.6 Anodic polarisation curves measured in the 40% H3PO4 solution for the Cu-deposited Ti-RCEs prepared in the Cu-plating baths with 0 and 8 ppm thiourea 79
Fig. 3.7 Variation of anodic current densities during potentiostatic polishing at 1.5 V in the 40 % H3PO4 solution for he Cu deposits prepared in the Cu-plating baths with different thiourea concentrations 80
Fig. 3.8 FESEM-micrographs of electropolished Cu surfaces electroplated in the Cu-plating baths (a) without ,(b) with 8 ppm thiourea 81
Fig. 3.9 AFM micrographs of electropolished Cu surfaces electroplated in the Cu-plating baths with (a) 0, (b) 1, (c) 5, and (d) 8 ppm thiourea 82
Fig. 4.1 Anodic polarisation curves of brass RDE at (a) different rotational speeds and a scan rate of 5 mV/s and (b) different scan rates and rotational speeds 83
Fig. 4.2 Surface morphologies of brass RDEs potentiostatically etched at the transition-peak potential at rotational speeds of (a) 200 and (b) 1000 rpm 84
Fig. 4.3 Surface morphologies of brass RDEs potentiostatically etched at the start of the limiting-current plateau at rotational speeds of (a) 200, (b) 500, (c) 1000, and (d) 1500 rpm 85
Fig. 4.4 Surface morphologies of brass RDEs potentiostatically etched in the middle of the limiting-current plateau at rotational speeds of (a) 200 and (b) 1500 rpm 86
Fig. 4.5 AFM micrographs of brass RDEs potentiostatically etched in the middle of the limiting-current plateau at rotational speeds of (a) 200 and (b) 1500 rpm 87
Fig. 4.6 Surface morphologies of brass RDEs potentiostatically etched on the limiting-current plateau near the oxygen-evolution reaction at rotational speeds of (a) 200, (b) 500, (c) 1000, and (d) 1500 rpm 88
Fig. 4.7 (a) Nipple-like and (b) flow-streak features on the brass RDE surface potentiostatically polished on the limiting-current plateau near the oxygen- evolution reaction 89
Fig. 4.8 Formation mechanism of nipple-like morphology 90
Fig. 4.9 Shallow craters on the RDE surface potentiostatically polished on the limiting-current plateau near the oxygen-evolution reaction 91
Fig. 4.10 Formation mechanism of a flow-streak feature 92
Fig. 4.11 Variation in the anodic current densities of brass RDEs potentiostatically polished in the middle of the limiting-current plateau 93
Fig. 4.12 (a) Variation in the anodic current densities of stagnant brass RDEs positioned upwards and downwards during potentiostatic polishing in the middle of the limiting-current plateau and the polished surface morphologies of RDEs positioned (b) upwards and (c) downwards, respectively 94
Fig. 4.13 Anodic polarisation curves of brass RDE at different rotational speeds with a scan rate of 5 mV/s. 95
Fig. 4.14 Surface morphologies of the brass RCEs potentiostatically etched at their transition peaks at rotational speeds of (a,b) 200, (c,d) 500, (e,f) 1000 and (g,h) 1500 rpm, respectively 96
Fig. 4.15 Surface morphologies of the RCEs potentiostatically etched at the start of the limiting-current plateau at rotational speeds of (a,b) 200, (c,d) 500, (e,f) 1000 and (g,h) 1500 rpm, respectively 97
Fig. 4.16 Surface morphologies of the brass-RCEs after potentiostatic polishing in the middle of the limiting-current plateau at rotational speeds of (a,b) 200, (c,d) 500, (e,f) 1000 and (g,h) 1500 rpm, respectively 98
Fig. 4.17 Surface morphologies of the brass-RCEs after potentiostatic etching at the end of the limiting-current plateau at rotational speeds of (a,b) 200, (c,d) 500, (e,f) 1000 and (g,h) 1500 rpm, respectively 99
Fig. 4.18 Variation in the anodic current densities of brass RCEs potentiostatically polished in the middle of the limiting-current plateau 100
Fig. 4.19 Schematic illustration of the Cu2+-rich layer formed on the stagnating brass-RCE during electropolishing 101
Fig. 4.20 Surface morphologies of the brass-RCEs after being potentiostatically etched in the middle of the limiting-current plateau without rotation (a) tilted RCE with light reflecting and (b) front view of the RCE showing its etched structures 102
Fig. 4.21 Optical micrograph of the rotating brass-RCE during electropolishing showing a full coverage of the Cu2+-rich layer on the RCE surface 103
Fig. 4.22 Schematic illustration of the rod-climbing phenomenon of the Cu+2-rich layer (a) initial electropolishing, (b) full coverage (c,d) rod-climbing, (e) formation a thin mushroom-shaped stream, (f) full coverage 104
Fig. 4.23 (a,b) rod-climbing of Cu2+-rich semi-sphere, and (c) a thin mushroom-shaped stream 105
Fig. 4.24 The simulated flow field combined with the electropolishing RCE in the aqueous phosphoric acid 106

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