電漿電解質氧化軟性火花區及電弧區在AZ91D鎂合金鍍膜之行為分析

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研究生：	馮法納 Fofana Muhammed S.
論文名稱：	電漿電解質氧化軟性火花區及電弧區在AZ91D鎂合金鍍膜之行為分析 Soft Sparking and Arcing Regime Behaviors of Plasma Electrolytic Oxidation (PEO) Coatings on AZ91D Magnesium Alloy
指導教授：	周振嘉 Chen-Chia Chou
口試委員:	蔡大翔 Dah-Shyang Tsai 李志偉 Jyh-Wei Lee
學位類別：	碩士 Master
系所名稱：	工程學院 - 機械工程系 Department of Mechanical Engineering
論文出版年：	2019
畢業學年度：	107
語文別：	英文
論文頁數：	122
中文關鍵詞：	鎂合金、電漿電解質氧化、電弧放電、軟性火花區、電流比、電荷比
外文關鍵詞：	Magnesium, Plasma electrolytic oxidation, arcing regime, soft sparking regime, current ratio, charge ratio
相關次數：	點閱：348 下載：1
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上一筆

本論文在雙極脈衝模式下研究了AZ91D 鎂合金在鋁酸鹽基電解質中電漿電解質
氧化 (PEO)的軟性火花區和電弧區行為。
在PEO 研究中，氧化層生長動力學對氧化物的形貌、特性具有顯著影響。至今
為止，軟性火花和電弧區特性行為的研究少之又少，本研究中我們使用可能影
響軟性火花和電弧發生的的參數進行研究。舉例來說像是電流比IR (IR=I+/I−)
代表陽極氧化與陰極還原電流的比率，以及電荷比CR (CR=Q+/Q−) 代表一個脈
衝週期內陽極氧化與陰極還原電荷的比率。在定電流模式下，藉由調整負電流
使IR範圍= [0.63~2.40] 以及陰極工作週期使CR= [0.65~2.00] 。
實驗結果表明IR<1.0 時形成的塗層在陽極時的電阻不高，這可歸因於在負
脈衝期間氧化物被氫還原，相較於其他團隊的結果，我們發現不論CR值如何，
在IR<1.0 參數中的塗層中發生軟性火花現象，其原因為較大的負電流與較長的
負極脈衝波形影響氧擴散機制與電漿反應型態，有助於用較軟的火花取代反應
較為劇烈的強火花。進而比較發現當IR<1.0,CR<1.0 時，相較IR<1.0,CR>1.0 軟
性火花發生得更早，其原因為CR<1.0 時氫的總含量多於CR>1.0，而氫會破壞膜
層的絕緣性，故提早發生軟火花現象。另一方面在IR>1.0,CR>1.0 的塗層中觀
察到電弧放電增長現象；IR>1.0;CR<1.0 時，塗層生長的電壓頻繁且急劇地下
降，出現軟性火花、微放電、聲音光線驟減現象。
在軟性火花狀態下形成的膜層的微觀結構顯示出均勻的塗層，可以觀察到
氧化層向內生長的行為；而在電弧狀態下形成的膜層明顯看到一些放電通道、
孔洞、裂紋等，在XRD 中可以分析出試片具有高的結晶度，故機械性質如納米
硬度、彈性模數都會比經由軟性火花狀態下的膜層性質好。
在本研究中運用Mott-Schottky 評估所有塗層都具有n 型半導體行為。另外
由於氧化物膜層中的氫引起的氧空缺，我們觀察到軟火花形成的塗層的載子濃
度遠高於電弧放電塗層。結果亦與氧化物被氫氣還原現象一致。

This study investigated the soft sparking and arcing regime behaviors of plasma
electrolytic oxidation (PEO) on AZ91D magnesium alloys in aluminate-based
electrolyte under constant current DC bipolar pulse mode. In PEO, the coating growth
dynamics has a significant influence on the oxide coatings and characteristics. Both
the soft sparking and arcing regime behavior of PEO coatings on Mg alloys are rarely
studied. In this work, we performed experiments by considering factors that may
influence the occurrence of soft sparking and/or arcing regime. We investigated the
effect of electrical parameters like the current ratio parameter (IR) representing ratio
of anodic oxidation to cathodic reduction current ratio (IR = I+/I−) and the electrical
charge ratio parameter (CR) representing the ratio of the anodic oxidation to cathodic
reduction charge quantity over one current pulsed period (CR = Q+/Q−) under
constant current density on the occurrence of the soft sparking and arc regime. Several
IR values ranging from [0.63~2.40] were selected by only varying the cathodic current
over a fixed anodic current. Similarly several CR values ranging from [0.65~2.00]
were selected by only varying the negative current pulses over a fixed anodic current
pulse.
It seems that the oxide coatings formed at IR<1.0 is not highly resistive to the anodic
current which is likely attributed to the oxygen being reduced by hydrogen during the
negative pulse. As a result, contrary to reports from various PEO studies, we found
out that soft sparking growth phenomenon occurs in coatings at IR<1.0 due to the
larger negative current and longer duration of cathodic pulses that influences the
oxygen diffusion mechanism and plasma reaction characteristics contributing to
replacing the strong sparks with softer ones irrespective of the various selected
CR values. It is found that soft sparking regime occurred earlier when (IR <1.0;
CR<1.0) than when (IR<1.0; CR>1.0). It was observed that at a constant IR value,
varying the CR values as a result of adjusting the cathodic polarization influences the
soft sparking regime occurrence time. On the other hand, an arcing regime growth
phenomenon was observed in coatings at IR>1.0 irrespective of the various selected
CR values. The obtained results shows that the coating growth was distinguished by
frequent sharp sudden brief drops in the voltage followed by soft sparks,
II
microdischarges, decreased in voltage, reduced acoustics and light emissions when
(IR>1.0; CR<1.0).
Comparatively, the microstructure of ceramic oxide coatings formed at soft sparking
regime shows uniform and porous coatings. The coatings can be observed to grow
inwards and the outside layer appears smooth and plain. Arcing regime coatings on
the other hand were distinguished by visible discharge channels, holes, microcracks
and micro-pores. The higher intensity and sharpness of the peaks from the XRD
results shows that coatings at arcing regime demonstrate better degree of crystallinity.
As a result, nano-hardness and elastic modulus of the ceramic oxide coatings were
found to be comparatively higher with arcing regime coatings and reduces with soft
sparking regime coatings.
The Mott-Schottky evaluation results exhibited an n-type semiconducting behaviors
for all the ceramic oxide coatings in this study. As a result of oxygen deficiency
vacancy caused by hydrogen in the oxide film layer, it was observed that donor
concentration for soft regime coatings were much higher than the arcing regime
coatings. The oxide coating characteristics and corrosion resistance performance
could be improved by altering working parameters such as applied the current during
PEO.

TABLE OF CONTENTS
Abstract ......................................................................................................................... I
摘要.............................................................................................................................. III
ACKNOWLEDGEMENT ......................................................................................... IV
LIST OF FIGURES ................................................................................................ VIII
LIST OF TABLES .................................................................................................. XIV
CHAPTER 1 ................................................................................................................. 1
1.1 Introduction ..................................................................................................... 1
1.2 Research Objectives ........................................................................................ 2
CHAPTER 2 ................................................................................................................. 5
LITERATURE REVIEW ........................................................................................... 5
2.1 Magnesium Alloy ................................................................................................. 5
2.1.1 History and Properties of Magnesium alloys ................................................ 5
2.1.2 Corrosion Behavior of Magnesium and its alloys ......................................... 7
2.2 Plasma Electrolytic Oxidation (PEO) .................................................................. 8
2.2.1 History of the PEO Process ........................................................................... 8
2.2.2 Technology of PEO as a Coating Technique ................................................. 8
2.2.3 PEO Ceramic Oxide Coating Formation ..................................................... 10
2.2.4 PEO Processing Parameters ......................................................................... 11
2.2.5 PEO Process Regimes Coating Growth ....................................................... 15
2.2.6 PEO Oxide Semiconducting Property: Mott–Schottky Theory .................. 25
CHAPTER 3 ............................................................................................................... 27
EXPERIMENTAL PROCEDURES ........................................................................ 27
3.1 MATERIALS ..................................................................................................... 27
3.2 ELECTROLYTES ............................................................................................. 27
VI
3.3 Plasma Electrolytic Oxidation (PEO) Treatment ............................................... 28
3.4 Electrical Parameters .......................................................................................... 29
3.5 COATINGS CHARACTERIZATION METHODS .......................................... 30
3.5.1 X-Ray Diffraction (XRD) ............................................................................ 31
3.5.2 Scanning Electron Microcopy (SEM) ......................................................... 31
3.5.3 Electrochemical Corrosion Test .................................................................. 31
3.5.4 Mott-Schottky Test ...................................................................................... 32
3.5.4 Hardness Test .............................................................................................. 33
3.5.5 Roughness Test ............................................................................................ 33
Chapter 4 .................................................................................................................... 34
Results and Discussions ............................................................................................. 34
4.1 Soft sparking and arcing regime oxide coating growth behavior at a constant
??>1.0. ..................................................................................................................... 34
4.1.1 Coating growth behavior at CR = 1.50 and IR>1.0 .................................... 34
4.1.2 Coating growth behavior at CR = 1.50 and IR<1.0 .................................... 45
4.2 Soft sparking and arcing regime coating growth behavior at a constant CR<1.0.
.................................................................................................................................. 55
4.2.1 Coating growth behavior at CR = 0.65 and IR>1.0 .................................... 55
4.2.2 Coating growth behavior at CR = 0.65 and IR<1.0 .................................... 64
4.3 Soft sparking regime coating growth behavior under IR<1.0 ............................ 73
4.3.1 Effect of CR >1.0 on the soft sparking regime oxide coatings growth
behavior at IR = 0.86. .......................................................................................... 73
4.3.2 Effect of CR <1.0 on the soft sparking regime oxide coatings growth
behavior at IR = 0.86. .......................................................................................... 82
4.4 Influence of soft sparking and arcing regime on nano-mechanical properties of
the ceramic oxide PEO coatings............................................................................... 89
4.4.1 Effect of soft sparking regime coating growth on hardness properties of the
oxide layer ............................................................................................................ 89
VII
4.4.2 Effect of arcing regime coating growth on hardness properties of the oxide
layer ...................................................................................................................... 91
4.5 Influence of soft sparking and arcing regime on the semiconductive properties
of the oxide coatings (Mott- Schottky) .................................................................... 93
CHAPTER 5 ............................................................................................................... 96
CONCLUSIONS ........................................................................................................ 96
REFERENCES ........................................................................................................... 98
                                

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