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博碩士論文 etd-0930113-220938 詳細資訊
Title page for etd-0930113-220938
論文名稱
Title
線上複合電鍍銳化法對CVD鑽石膜表面精加工特性之研究
Studies on the Finish Machining Characteristics of CVD Diamond Film Surface by Using a Composite Electro-plating In-process Sharpening Method
系所名稱
Department
畢業學年期
Year, semester
語文別
Language
學位類別
Degree
頁數
Number of pages
129
研究生
Author
指導教授
Advisor
召集委員
Convenor
口試委員
Advisory Committee
口試日期
Date of Exam
2013-06-04
繳交日期
Date of Submission
2013-10-31
關鍵字
Keywords
CVD鑽石膜、複合電鍍、正反向脈衝電流、超精密研磨
Finish machining, Pulse reversal current, Composite electroplating, CVD diamond film
統計
Statistics
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中文摘要
現今厚達數微米之鑽石膜常以化學氣相沉積法(Chemical Vapor Deposition, CVD)進行沉積。而以此法沉積出如此厚度的鑽石膜,操作參數必須精準控制,否則鑽石膜表面通常有著表面極為粗糙、表面晶粒大小不一、鍍層厚度成長不均等情況發生。所以剛沉積完成的鑽石膜通常難以直接應用而必須進行後續的研磨加工。
本研究首先以線上複合電鍍銳化研磨法對鑽石膜研磨加工之可行性進行探討。研究過程中以鎳金屬為陽極,銅盤為陰極,將兩者浸入含粒徑10μm的鑽石磨粒之鎳電鍍液中並接上直流電源,因此銅盤表面可以不斷沉積出具銳利磨粒的鎳基鑽石複合鍍層。研究結果發現,與傳統研磨法相比,此法不僅可以有效地提升磨盤對鑽石膜材料移除率達3.8倍,且磨盤表面的鍍層厚度也可以維持甚至微幅增加。
本研究接著改變不同的操作條件如電流密度、鍍液配方以及鑽石磨粒粒徑,藉此了解上述的操作條件對本加工法之影響。研究中發現,鑽石磨粒於複合鍍層中之分布可以視為體心正方(body-centered tetragonal)之結構。此外,在加工過程中,將電流密度調整到2.5至7.5 ASD、鍍液中氯化鎳濃度調整到30至150 g/L、以及鍍液中鑽石磨粒粒徑大於鑽石膜表面之柱狀結晶尺寸時可得到較好的研磨效果即較高的鑽石膜粗糙度變化率以及較低的鍍層成長率。為了得到類鏡面的鑽石膜表面,因此使用兩階段線上複合電鍍銳化法研磨鑽石膜。在第一階段,使用粒徑25 μm的鑽石磨粒對鑽石膜研磨加工30分鐘。在第二階段,則將粒徑改為3 μm並繼續研磨加工180分鐘。經此兩階段的加工後,可得到平均表面粗糙度約0.03 μm之類鏡面鑽石膜表面。此外,藉由觀察加工過程中磨盤表面複合鍍層以及鑽石膜的表面結構,可描繪出此法的加工機制。
為了控制磨盤表面複合鍍層的厚度,本研究將正反向脈衝電源導入本加工法。在加工過程中同時以正反向脈衝電流對磨盤表面之複合鍍層同時進行電鍍銳化以及電解削銳,因此鍍層可維持其銳利度以及厚度。實驗中探討不同正反向脈衝電流對加工後磨盤表面之鎳基鑽石複合鍍層及CVD鑽石膜表面特性的影響。由實驗結果可知,無論反向脈衝時間長短,雖然鑽石膜的最終粗糙度皆較正向脈衝電流時高,但鍍層的厚度皆可有效控制。在反向脈衝時間為1500 μs 時,鍍層厚度於加工過程中幾乎可維持零成長。
Abstract
A diamond film with thickness of several microns is usually deposited by chemical vapor deposition method. To deposit the diamond film by this method, its operating parameters have to be precisely controlled. Otherwise, the rough souface of the diamond film is grown with non-uniform thickness, resulting in limitations on the applications. Hence, a surface machining process is required.
A feasibility study to grinding diamond film is conducted by Composite Electro-plating In-process Sharpening (CEPIS) method. A nickel plate as the anode is located on the top of a copper disc horizontally as the cathode. Both are connected to DC power supply and immersed in a nickel chloride bath containing diamond grits of 10 μm as an electrolyte, so that metal ions with diamond grits are deposited onto a grinder in process to expose fresh sharp grains. Results show that the removal rate of the diamond film increases with increasing current density, and the highest removal rate is about 3.8 times higher than that of the traditional grinding method. Meanwhile, the coating thickness on the disc is maintained or slightly increased.
Next, effects of various operating parameters, such as current densities, bath compositions, and diamond grit sizes, on the grinding characteristics of CEPIS method are studied. Results show that a distribution model of the diamond grits in the coating layer is deduced, and it can be demonstrated as body-centered tetragonal structure. To promote optimum grinding efficiency, a high variation rate in the surface roughness of diamond film and a small growth rate in the coating thickness are desired. To meet this demand, a current density is in the range of 2.5 to 7.5 ASD, a concentration of nickel chloride is in the range of 30 to 150 g/L, and the diamond grit size is larger than the column size on a diamond film surface. A two-stage CEPIS grinding procedure is used to grind the diamond film. A grit size of 25 μm is selected to conduct the CEPIS grinding for 30 min. Then, the operating conditions are switched to a grit size of 3 μm and a grinding time of 180 min. Finally, a mirror-like surface on the diamond film with an average surface roughness of 0.03 μm is obtained. Moreover, the grinding mechanism is deduced by observing the coating and diamond film surface during this process.
Finally, a pulse reversal current is introduced to this method to control the coating thickness on the grinding tool. The coating can be sharpen by composite electroplating and dressed by electrolyzing simultaneously, so that both sharpness and thickness of the coating is maintained. Effect of pulse reversal current on the grinding characteristics of the coating layer and the CVD diamond film is experimentally investigated. Results show that the surface roughness of diamond film is higher than that obtained by the positive pulse current, but the coating thickness on the tool can be efficiently controlled regardless of pulse reversal duration. The thickness of the coating layer can almost maintain constant at the pulse reversal duration of 1500 μs.
目次 Table of Contents
總目錄
總目錄 i
圖目錄 iii
表目錄 ix
摘要 x
Abstract xii
第一章 總論 1
1-1研究背景 1
1-2文獻回顧 3
1-3 論文研究方向與架構 19
第二章 鑽石膜表面之研磨特性與磨盤表面的銳化機制之研究 21
2-1 前言 21
2-2 實驗設備及流程 23
2-3 實驗結果與討論 31
2-4 結論 42
第三章 氯化鎳濃度對磨盤銳化機制之影響 43
3-1 前言 43
3-2 實驗設備及流程 45
3-3 實驗結果與討論 47
3-4 結論 57
第四章 磨粒粒徑與鑽石膜的原始表面粗糙度對磨盤銳化機制之影響 58
4-1 前言 58
4-2 實驗流程與設備 59
4-3 結果與討論 61
4-4 結論 78
第五章 不同脈衝電流下之鑽石膜表面研磨特性 79
5-1 前言 79
5-2 實驗設備與流程 81
5-3 實驗結果 83
5-4 結論 98
第六章 總結及未來展望 99
6-1 總結 99
6-2 展望 101
參考文獻 102
陳泰甲學經歷簡介 110

圖目錄
Fig. 1-1 Schematic drawing of the polishing apparatus [6] 3
Fig. 1-2 Microphotographs of the CVD diamond film (a) as deposited, (b) partly polished, and (c) the method of estimating the polishing rate [6] 4
Fig. 1-3 Model of the thermochemical polishing of diamond on hot metal-solvent [10] 5
Fig. 1-4 Schematic diagram for the reaction between diamond and iron powders [11] 5
Fig. 1-5 Mechanism map of material removal in dynamic friction polishing [14] 6
Fig. 1-6 Scheme of the device for mechanochemical polishing of diamond substrates [17] 7
Fig. 1-7 Incident angles to grains after irradiation: (a) before irradiation, (b) after irradiation at 0° ,and (c) after irradiation at 80° [23] 8
Fig. 1-8 Schematic diagram for the electro-chemical discharge apparatus [27] 10
Fig. 1-9 Mechanism for diamond film of the electro-chemical discharge [27] 11
Fig. 1-10 SEM micrographs of the growth surfaces of the samples before (a: TD1, b: TF1) and after (c: TD1P, d: TF1P) polishing [29] 12
Fig. 1-11 Scheme of the two-step deposition process 17
Fig. 1-12 The five stages in the codeposition of a particle 18
Fig. 1-13 Thesis Structure 20
Fig. 2-1 Grinding apparatus with composite electroplating in-process sharpening method (a) schematic diagram, (b) photograph 24
Fig. 2-2 Geometry and size of copper disc 25
Fig. 2-3 SEM micrographs for CVD diamond film before the grinding process: (a) x1000, and (b) x5000 26
Fig. 2-4 Evaluation of the coating thickness (a) Before deposition, and (b) After deposition 29
Fig. 2-5 SEM micrographs for Ni-Diamond composite coating of the grinding tool after electroplating 15 min: (a) SEI, (b) BEI, and (c) Binarization 30
Fig. 2-6 Variation for the coating thickness of the grinding tool at different current densities during the grinding process 32
Fig. 2-7 Variation for the amount of the diamond film removed under different current densities during the grinding process 32
Fig. 2-8 (a) Rate of variation of the coating thickness of the grinding tool, and (b) removal rate of diamond film at different current densities 34
Fig. 2-9 Variation for the profile of diamond film at different current densities during the grinding process: (a) 0 ASD, and (b) 7.5 ASD 35
Fig. 2-10 Variation for the surface roughness of diamond film at different current densities during grinding process 36
Fig. 2-11 SEM micrographs of the CVD diamond film after a grinding time of 30 min at 7.5 ASD: (a) x1000, and (b) x5000 36
Fig. 2-12 SEM micrographs of the composite coating surface of the grinding tool at 0 ASD after a grinding time of: (a) 20 min, (b) 30 min 38
Fig. 2-13 SEM micrographs of the composite coating surface of the grinding tool at 7.5 ASD after a grinding time of: (a) 20 min, and (b) 30 min 38
Fig. 2-14 SEM micrographs of the cross-section of a coated grinding tool at different current densities after a grinding time of 30 min: (a) 0 ASD, and (b) 7.5 ASD 40
Fig. 2-15 Wear mechanism of Ni-diamond composite coating of the grinding tool at 0 ASD during the grinding process: (a) original, and (b) worn away 40
Fig. 2-16 Sharpening mechanism of Ni-diamond composite coating of the grinding tool during the CEPIS grinding process: (a) original, (b) worn away, and (c) depositing a new layer during each rotation of the grinding tool, where t is the incremental amount of the coating in thickness, and its actual value is much smaller than shown here (t is about 0.05 m/rev at 7.5 ASD). The coating thickness and the active grits density increase with increasing current 41
Fig. 3-1 SEM micrographs of the CVD diamond film under different initial surface roughness, Ra: (a) 1.1 m, and (b) 0.2 m 46
Fig. 3-2 Variation for the coating thickness of the grinding tool under different concentrations of the nickel chloride of the plating bath 48
Fig. 3-3 Growth rate of the coating thickness of the grinding tool under different concentrations of the nickel chloride of the plating bath 48
Fig. 3-4 SEM micrographs for Ni-Diamond composite coating of the grinding tool at a current density of 7.5 ASD after electroplating 30 min under different concentrations of the nickel chloride of the plating bath: (a) 10 g/L, (b) 30 g/L, and (c) 75 g/L 49
Fig. 3-5 Variation for the coating thickness of the grinding tool under different concentrations of the nickel chloride of the plating bath and different current densities during the grinding process 51
Fig. 3-6 Growth rate of the coating thickness of the grinding tool under different concentrations of the nickel chloride of the plating bath and different current densities during the grinding process 51
Fig. 3-7 Variation for the surface roughness of diamond film under different concentrations of the nickel chloride of the plating bath and different current densities during the grinding process 52
Fig. 3-8 Surface profile histories of the diamond film at the current density of 7.5 ASD, and the grinding time of 180 min under different concentrations of the nickel chloride of the plating bath during the grinding process: (a) 10 g/L and (b) 75 g/L 53
Fig. 3-9 SEM micrographs of Ni-Diamond composite coating on the grinding tool surface after grinding 180 min under 0 ASD at different concentrations of the nickel chloride: (a) 10 g/L, (b) 30 g/L, and (c) 75 g/L 55
Fig. 3-10 SEM micrographs of Ni-Diamond composite coating on the grinding tool surface after grinding 180 min under 7.5 ASD at different concentrations of the nickel chloride: (a) 10 g/L, (b) 30 g/L, and (c) 75 g/L 56
Fig. 4-1 Variations for the average coating thickness on the grinding tool during the electroplating process 62
Fig. 4-2 SEM micrographs of the coating layer on the grinding tool under different diamond grit sizes: (a) 3 μm, (b) 10 μm, and (c) 25 μm 63
Fig. 4-3 Weight loss of an anode during the electroplating process 64
Fig. 4-4 Variation for the covered area ratio of the diamond grits to the surface area Fig. 4-5 (a) Schematic diagram of the distribution of diamond grits in the Ni-Diamond composite coating layer, and (b) edge length for the experiments of the BCT unit cell 65
Fig. 4-6 Thickness variations for the composite coating on the grinding tool under different degrees of surface roughness in the initial diamond film and diamond grit sizes in the CEPIS grinding process 71
Fig. 4-7 SEM micrographs of the coating layer on the grinding tool under different initial surface roughness of diamond films and diamond grit sizes: (a) 3 μm, (b) 10 μm, and (c) 25 μm 72
Fig. 4-8 Variation for the average surface roughness of the diamond film under different initial surface roughness of diamond films and diamond grit sizes 73
Fig. 4-9 SEM micrographs of the composite coating after grinding 30 min at the current density of 0 ASD under different particle sizes: (a) 3 μm, (b) 10 μm, and (c) 25 μm 74
Fig. 4-10 The CEPIS grinding mechanisms under different grit sizes: (a) When the diamond grit size is smaller than the column size on the diamond film, and (b) When the diamond grit size is larger than the column size on the diamond film 75
Fig. 4-11 Variations for the average surface roughness of the diamond film at a disc speed of 50 rpm, a work-piece speed of 400 rpm using a two-stage CEPIS grinding process 76
Fig. 4-12 SEM micrographs of the CVD diamond film at a grinding time of 210 min 77
Fig. 5-1 Schematic diagram of the grinding apparatus with modified composite electroplating in-process sharpening method 81
Fig. 5-2 Variation fot the coating thickness of the grinding tool under different pulse current during the electroplating process 83
Fig. 5-3 Weight loss of an anode under different impulse current during the electroplating process 84
Fig. 5-4 Variation for the coating thickness of the grinding tool under different pulse current during the grinding process 85
Fig. 5-5 Variation for the surface roughness of diamond film under different pulse current during grinding process 86
Fig. 5-6(a) Rate of variation of the coating thickness of the grinding tool under different pulse current, and (b) final surface roughness of diamond film 87
Fig. 5-7 Variation for the coating thickness of the grinding tool under different pulse reverse current during the grinding process 88
Fig. 5-8 Variation for the surface roughness of diamond film under different pulse reverse current during grinding process 89
Fig. 5-9(a) Rate of variation of the coating thickness of the grinding tool under different pulse reverse current, and (b) final surface roughness of diamond film 90
Fig. 5-10 Real growth rate of the coating thickness of the grinding tool under different pulse current 91
Fig. 5-11 SEM micrographs of the coating of the grinding tool at different pulse current after a grinding time of 60 min (a) No current, (b) DC, (c)3750/750 μs, (d)1500/750 μs, (e)750/750 μs 92
Fig. 5-12 Real growth rate of the coating thickness of the grinding tool under different pulse reverse current 94
Fig. 5-13 SEM micrographs of the coating of the grinding tool at different pulse reverse current after a grinding time of 60 min (a) 3750/750 μs, (b) 3750/750 μs;750/750 μs, (c)3750/750 μs;1500/750 μs, (d)3750/750 μs;3750/750 μs 94
Fig. 5-14 Variations for the coating thickness on the grinding tools using a two-stage Composite electroplating and electrolytic in-process sharping grinding process 96
Fig. 5-15 Variations for the average surface roughness of the diamond film using a two-stage Composite electroplating and electrolytic in-process sharping grinding process 97
Fig. 5-16 SEM micrographs of the CVD diamond film at a grinding time of 240 min (a) Before, and (b) After grinding 97

表目錄
Table 1-1 Various diamond polishing techniques 14
Table 2-1 Operating parameters 31
Table 3-1 Operating parameters 45
Table 4-1 Composition of the electrolyte 59
Table 4-2 Operating parameters 60
Table 4-3 Coating thickness and the surface roughness of the diamond film under different operating conditions after grinding 30 min 69
Table 5-1 Operating parameters 82
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