應用物理氣相沉積法製備低電阻高透光氧化物/銀複合薄膜之研究

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研究生：	林自威 Tzu-wei Lin
論文名稱：	應用物理氣相沉積法製備低電阻高透光氧化物/銀複合薄膜之研究 Low resistance and high visible transmittance of transition metal oxide/silver composites through physical vapor deposition
指導教授：	李勝偉 Sheng-Wei Lee
口試委員:
學位類別：	博士 Doctor
系所名稱：	工學院 - 材料科學與工程研究所 Graduate Institute of Materials Science & Engineering
論文出版年：	2017
畢業學年度：	105
語文別：	英文
論文頁數：	130
中文關鍵詞：	透明導電氧化物、透明導電薄膜、介電層-金屬-介電層
外文關鍵詞：	TCO films, dielectric-metal-dielectric
相關次數：	點閱：9 下載：0
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以濺鍍法輔以活性電漿O2/Ar氣體比例為6％製備的非晶相的MoOx層，表現出高的可見光透射率和2.7eV大的能帶間隙。對於雙層A(10)M，適當的電漿O2/Ar氣體比例作用下可以提高可見光透光率並降低紅外線穿透率。在嵌入Ag層厚度> 10nm的情況下，MAM三層結構具有優異的導電性，高可見光透光率及低近紅外線透射率。插入的10nm 銀層可以有效地將MAM層結構電阻降低到4.83Ω/ sq，於可見波長為550nm的MA(10)M的品質係數可以達5.3×10-2-1，MoOx層的光學和電學性質是MoOx介電層厚度的函數。本研究結果顯示，具有最佳Ag和MoOx厚度的MoOx多層結構是可應用於透明導電氧化物和熱反射鏡。將銀層暴露於電漿O2/Ar氣體比例為6％混合物下，該方法能有效地調控MAM的可見光透射率而不降低導電率。這種MoOx / Ag / MoOx堆疊結構可望成為透明導電電極於一般玻璃或柔性基板上的應用。
以濺鍍法輔以活性電漿O2/Ar氣體比例為1％製備的ITO層及非晶相ITO/Ag多層結構，表現出高可見光透光率及3.62eV大能帶間隙。在IAI多層中，由HRTEM展現Ag和ITO層之間的界面明顯邊界。當嵌入的Ag層> 10nm時，所製備的IAI三層結構在波長550nm和600nm的波長下表現出優異的導電性和高的可見光透光率。插入的10nm Ag層可以有效地降低I(60)A(10)I(60)堆疊層的電阻降至5.8Ω/ sq，IA(10)I在可見波長為550nm及600 nm的品質係數分別可達1.09×10-1-1和1.28×10-1-1。此對稱結構IAI於可見光透光率隨著ITO厚度的減小而呈現藍位移。在退火溫度小於400 oC ，IAI的Rs隨著RTA溫度升高而降低；退火溫度大於 400℃時的透光率顯示沒有下降並產生藍位移，此歸因於RTA後ITO層的結晶改善。在400℃退火處理後，可見光波長為550nm的IA(10)I的品質係數可達1.56×10-1-1。本研究結果顯示，具有最佳Ag和ITO厚度的ITO多層結構可望作為透明導電氧化物和藍色發光二極管電極上之應用。
TAW和WAW多層膜在室溫下以電子束蒸鍍在PES上，研究結晶度、微觀結構、電學和光學特性。觀察到在TAW堆疊層中具有(111)面的優選取向的多晶Ag層。不對稱結構TAW多層於HRTEM展示Ag/TiOx與Ag/WO3 BL之間有明顯的邊界，並且不會形成氧化物。在嵌入的Ag層> 15nm的情況下，T(40)A(15)W(40)三層結構在波長550nm處具有夠高的可見光(93.7％)及低近紅外光透光率(14.4％)並表現出優異的導電性。插入的15nmAg層可以有效地將TAW堆疊層的電阻降低至3.93Ω/ sq，而在可見光波長為550 nm時，最佳TA(15)W有最高品質係數可達到1.210-1 -1，優於文獻的值[2,19-22]。由於上層TiOx有較佳的抗濕能力，TAW層比WAW層有較佳的濕度穩定性。本研究結果顯示，非對稱結構多層的TA(15)W是可望作為透明導電氧化物和熱反射鏡於柔性基底之應用

The MoOx layers with amorphous phases fabricated by reactive sputtering with plasma at an O2/Ar of 6% for the reactive gas exhibited a high visible transmittance and a large optical band gap of 2.7 eV. For the A(10)M bilayer, an appropriate O2/Ar plasma can improve the transparency and reduce the IR transmittance. With an embedded Ag layer > 10 nm, the MAM sandwiched layers exhibit superior conductivity with sufficiently high visible and low NIR transmittance. The inserted 10-nm Ag layer can effectively reduce the resistance of the MAM stacked layer down to 4.83 Ω/sq, and the FOM of MA(10)M at a visible wavelength of 550 nm can reach 5.310-2. The optical and electrical properties of the MoOx layer are a function of the thickness of the MoOx dielectric layer. Our results suggest that a MoOx multilayer with appropriate Ag and MoOx thicknesses is a promising candidate for application as a TCO and heat mirror. The Ag layer was exposed to plasma induced by an in-situ 6% O2/Ar mixture, and this approach was demonstrated to tune the visible transmittance of MAM effectively without degradation of the Rs. Such a MoOx/Ag/MoOx stacked structure might be a promising electrode in potential applications of transparent conductive oxides on conventional glass or flexible substrate.
The ITO layers and ITO/Ag multi-layers with amorphous phases fabricated by reactive sputtering with plasma through O2/Ar mixture of 1% severed as the reactive gas exhibited high visible transmittance and a large optical band gap of 3.62 eV. In the IAI multilayer, the interface between the Ag and ITO layer revealed by HRTEM shows a distinct boundary. With an embedded Ag layer > 10 nm, the as-prepared IAI sandwiched layers exhibit superior conductivity with high visible transmittance at the wavelength of 550 and 600 nm. The inserted 10-nm Ag layer can effectively reduce the resistance of the I(60)A(10)I(60) stacked layer down to 5.8 Ω/sq, and the FOM of IA(10)I at a visible wavelength of 550 and 600 nm can reach up to ~ 1.09×10-1 and 1.28×10-1. The visible transmittance of symmetric IAI sample shows a blue-shift with a decreasing in the ITO thicknesses. The Rs of IAI sample reduced as an increasing RTA temperature < 400 oC. The transmittance without degradation in the annealed samples > 400 oC also showed blue-shift, which is attributed to the crystallization of ITO layer after RTA. The FOM of IA(10)I at a visible wavelength of 550 nm can reach up to ~ 1.56×10-1-1 after annealing treatment at 400 oC. Our results suggest that a ITO multilayer with appropriate Ag and ITO thicknesses is a promising electrode candidate for application as a TCO and blue light emitting diode.
The crystallinity, microstructure, and electrical and optical properties of TAW and WAW multilayers on PES or glass through E-beam evaporation at room temperature were studied. The polycrystalline Ag layer with preferred orientation along the (111) plane in the TAW stacked layers were observed. In the asymmetrical TAW multilayer as revealed by HRTEM, both of the interface between the Ag/TiOx capping layer and Ag/WO3 BL show distinct boundaries and no oxide formation. With an embedded Ag layer > 15 nm, the T(40)A(15)W(40) sandwiched layers exhibit superior conductivity with sufficiently high visible (> 93.7%) at the wavelength of 550 nm and low NIR transmittance (14.4%). The inserted 15-nm Ag layer can effectively reduce the resistance of the TAW stacked layer down to 3.93 Ω/sq, and the highest FOM of the optimal TA(15)W at a visible wavelength of 550 nm can reach as high as 1.210-1 -1, which is higher than the value of the previous report [2, 19-22]. The TAW layer also shows better moisture stability than that of the WAW sandwiched layer owing to the suppression of moisture by the TiOx top layer. Our results suggest that an asymmetrical TA(15)W multilayer is a promising candidate for application as a robust TCO and heat mirror on flexible substrate.

Abstract        I
Contents    VI
Chapter 1 Introduction    1
1 Brief review of progress in transparent conductive electrode    1
2 Requirement and applications in transparent conductive oxide    3
3 Motivation of this work    3
Chapter 2 Background of transparent electrode    5
1 Review of TCO    5
2 Categories of TCO    7
1.1 Carbon nanotube/graphene    7
2.2 A thin layer of metal and metal grids    9
2.3 Metal nanowires    11
2.4 Metal oxide    12
3 Principle and fabrication of dielectric/metal/dielectric    13
4 The applications of DMD in TCO    20
5 The approaches of enhanced FOM in DMD    21
6 Evolution of silver morphology under plasma exposure    23
Chapter 3 Experimental Procedures and characterization equipments    25
1 Sputtering deposition process    25
2 Electron beam physical vapor deposition process    26
3 Surface profiler    27
4 X-ray diffraction    27
5 Transmission electron microscopy    29
6 Scanning electron microscopy    29
7Atomic force microscopy    30
8 X-ray photo-electron spectroscopy    31
9 Four point probe and Hall effect    31
10. Ellipsometer    32
11. UV/Vis/NIR spectrometer    33
Chapter 4Tailoring transparence in MoOx/Ag/MoOx electrode through Ag by O2/Ar plasma exposure    34
1 Motivation of MoOx/Ag/MoOx electrode    34
2 Preparation of MoOx/Ag/MoOx through sputtering    35
3 Structural and optical properties of MoOx films fabricated by reactive sputtering    37
4 Structural, electrical and optical properties of AM and MAM stacked layer with O2/Ar plasma treatments    37
5 Microstructures, optical, and electrical properties of AM and MAM stacked layer with different Ag thickness    40
6 Optical, and electrical properties of symmetric and asymmetric MAM multilayers with different MoOx thickness in configuration    42
7 Summary of MoOx/Ag composites through Ag by O2/Ar plasma exposure    43
Chapter 5  High transparent ITO/Ag/ITO electrode with Ag layer under O2/Ar plasma exposure    44
1 Motivation of ITO/Ag/ITO    44
2. Experimental    45
3. Results and Discussion    47
3.1 Structure and optical properties of ITO films fabricated by reactive sputtering with different O2/Ar ratio    47
3.2 Structure, electrical and optical properties of AI stacked layer prepared with Ag under O2/Ar plasma exposure    47
3.3 Structure, optical, and electrical properties of symmetrical IAI stacked layer with different Ag thickness    49
3.4 Thermal stability of IAI multi-layers with different annealing temperature    52
4. Conclusions    53
Chapter 6 Indium-free transparent TiOx/Ag/WO3 stacked composite electrode with improved moisture resistance    55
1 Motivation of TiOx/Ag/WO3 stacking layer    55
2. Experimental details of preparation of TiOx/Ag/WO3 by E-gun    56
3. Structure properties of TiOx, WO3, and TiOx/Ag/WO3    57
4. Optical and electrical properties of TiOx, WO3, and TiOx/Ag/WO3    59
5. Damped test of TiOx/Ag/WO3 and WO3/Ag/WO3    61
6. Summary of TiO2/Ag/WO3 stacking layer    61
Chapter 7 Conclusions and future prospects    63
1 Conclusions    63
2 Future prospects    65
References    66
Figure Captions    81
Table Captions    86
Related Publication    119

                                

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