臺灣博碩士論文加值系統

光觸媒係屬於高級氧化程序(advanced oxidation processes)中的一環，常見的光觸媒材料為TiO2、ZnO、CdS、WO3、SnO2及Fe2O3等，以TiO2與ZnO最為廣泛研究。由於光觸媒材料應用上最大的困難為光觸媒的固定化技術，利用熔膠凝膠法、濺鍍法或燒鍍法較難製備大面積的塗層。相關研究結果與討論分為三部份來說明，首先本研究係利用大氣電漿熔射(atmosphere/air plasma spray, APS)技術將ZnO-3wt.%Al2O3 (代號I-APS AZO)殼型微米造粒結構之材料噴覆於玻璃基板表面，針對該氧化鋅複合粉末利用UV光(λ = 365 nm)降解亞甲基藍水溶液之光觸媒特性進行研究。研究結果顯示熔射後塗層表面形貌多為奈米結構，電漿熔射I-APS AZO之塗層其表面形貌多為奈米球狀氧化鋅，熔射過程發現較多高表面能結晶面，雖然降低硬度接近理想值c軸晶面之一半，但能有效提高氧化鋅塗層觸媒效率；X射線繞射(XRD)分析顯示熔射I-APS AZO之塗層其特徵峰向右偏移，表示鋁及氫可能有摻雜進氧化鋅結構，並壓縮ZnO純相之晶格。光觸媒特性顯示，經UV光照24 h，能將亞甲基藍水溶液降解為透明水溶液，電漿熔射I-APS AZO塗層光照12 h降解率為61%。綜合分析結果顯示，塗層表面結構與光觸媒材料影響光觸媒降解率，進行降解亞甲基藍(methylene blue, MB)水溶液，厚膜I-APS AZO塗層較薄膜AIP AZO塗層(代號AIP-Ref AZO，其中AIP表示電弧離子鍍膜/arc ion plating製程)效率佳，因為塗層中產生較多高表面能結晶面之ZnO相，會因高濃度氧空缺，形成電子電洞再結合中心之能障，導致其光觸媒效率較佳。
第二部份有關於電漿熔射以自製造粒粉末並沉積在玻璃基材之雙摻雜Al與C之ZnO鍍膜(代號II-APS AZO)，其厚度只有有13 μm，對應商用造粒粉末所製備之I-APS AZO 鍍膜，II-APS AZO在玻璃基板之膜層厚度，於噴塗相同趟數下，它的噴塗效率明顯較低。II-APS AZO鍍層結晶性，低於它的造粒餵粉狀態，且顯示為無織構性。高倍率下之II-APS AZO鍍層的表面型態顯示與I-APS AZO鍍層並不同(例如無發現奈米棒型態在Al,C:AZO試片上)，這結果強化解釋I-APS AZO鍍層在該電漿製程所製備出具新穎之層次結構(hierarchical morphology)。這些特性促使光觸媒特性優異，並高於先前所述之AIP-Ref AZO與TiO2 sprayer試片。另外，由於II-APS AZO試片以未除膠之PVA黏結劑當成C源模板，經電漿噴塗而成為Al與C雙摻雜之ZnO鍍層，經相同光觸媒測試條件下，光觸媒效率比I-APS AZO高出一倍。
最後部份是關於火焰熔射(Flame spray) F-AZO-Al2O3沉積在AISI 304不銹鋼基板之實驗，鍍膜厚度隨添加Al2O3含量(由F-30AO、F-50AO變化至F-70AO)增加而增加。而純火焰熔射Al2O3沉積在304不銹鋼基板(F-Al2O3，代號F-AO)，鍍膜厚度接近700 µm。SEM表面型態顯示奈米群顆粒聚集在微米顆粒上，並且黏結其上，這種奈米群顆粒可以幫助催化反應，特別在F-50AO (added 50 wt.% Al2O3)試片上發現有奈米與微米薄板(nano- and microplatelet morphology)之型態顆粒簇立於塗層表面。火焰熔射F-AZO-Al2O3試片顯示為多相沉積，而I-APS AZO與II-APS AZO試片顯示僅為wurzite相之ZnO沉積。這個多相反應使F-AZO-Al2O3試片之能隙隨當添加越多Al2O3 (由30 wt.%變化至70 wt.%)，具有藍偏移，並使之具有良好之光觸媒特性。
F-AZO-Al2O3試片經過72 h亞甲基藍浸泡並以UV光照射實驗中，顯示也有著相同近100%光觸媒效率(photocatalytic efficiency)，然而試片F- Al2O3 僅有30%光觸媒效率。特別是光照前6 h時，F-50AO試片之光觸媒效率快於F-30AO試片與F-70AO試片。對比F-AZO，F-70AO與F-AO (pure Al2O3)試片，顯示F-30AO試片與F-50AO試片3次循環測試實驗(cycling test of photocatalytic efficiency)，3次曲線均呈現穩定之趨勢。這結果顯示Al2O3一定含量(i.e., 50 wt.%)對AZO試片之光觸媒效果有正面幫助，另外F-AZO-Al2O3試片均有近140°之接觸角，顯示為疏水性(hydrophobic)，疏水性材料在光觸媒自清潔應用極為廣泛。

The aim of this study is to prepare the aluminum zinc oxide (AZO) coating onto glass and AISI 304 stainless steel substrates by thermal spraying, respectively. The research is mainly divided into three sections. The first two sections are related to plasma spraying AZO coating onto the glass substrate by using commercial agglomeration (I-APS AZO sample) and home-made agglomeration (II-APS AZO sample) feedstock powders. In plasma spraying with home-made agglomeration feedstock powder, a novel approach is applied and the chemical decomposed reaction from adhesive agent (polyvinyl acetate, PVA) of home-made agglomeration feedstock powder into plasma jet was started, carbon was then produced and doped into AZO coating. PVA was used as carbon source template in the feedstock powder, II-APS AZO sample thus had two dopant elements of Al and C. The final section is related to flame spraying AZO coating onto the AISI 304 stainless steel substrate by using of mixing aluminum oxide and aluminum zinc oxide. Here, Al2O3 was used as catalytic carrier and Al doping source. F-AZO-AO samples included F-AZO, F-30AO, F-50AO, and F-70AO samples. The composition of Al2O3 powder was 30 wt.% (F-30AO sample), 50 wt.% (F-50AO sample), and 70 wt.% (F-70AO sample). Those powders were added to mix with AZO powder in 3D mixer, respectively. And the mixed powder fed into flame jet to react with its own inside AZO powder and then deposited on 304 stainless steel substrates. All AZO samples were used as photocatalysts for the degradation of methylene blue (MB) dye chosen as an organic water pollutant soultion.
In the first section, AZO was deposited on a glass substrate using plasma spraying technique. Hierarchical nanostructured morphology is observed, for the first time, in plasma spraying coatings. Nanorod and nanosphere adhere to micro spherical particle to form hierarchical structure, however, is only reported by chemical synthesis method. Through XRD and SEM analysis, it is found that the morphology of coating can improve the formation of defects greatly. After UV-A light testing, photocatalytic efficiency of degradation methylene blue coating was analyzed using UV-Vis spectrometer. Combined with photoluminescence and X-ray photoelectron spectroscopy analysis, the results indicates that I-APS AZO coating is with good enhanced photocatalytic properties. This phenomenon suggests that I-APS AZO crystallites consist of multiple facets with high surface-energy planes. The measured water contact angle of about 7° indicates that I-APS AZO coating is with high hydrophilic characteristic and has very good practical applications in industry. This study thus paves a new way for environmental pollution control. In the second section, the research of II-APS AZO feedstock powder with agglomeration for spray drying experiment is further conducted to understand the surface morphology differences between I-APS AZO and II-APS AZO coating during plasma spraying process. The microstructure and shape of I-APS AZO coating with hierarchical characteristic is quite different from that of II-APS AZO coating with nano particle agglomeration. And, this hierarchical nanostructured morphology of the thicker I-APS AZO film also results in lower contact angle. However, the photocatalytic efficient of II-APS AZO coating is almost twice higher than that of I-APS AZO coating due to the carbon added into II-APS AZO sample.
In the final section, F-AO (pure Al2O3) coating sample was identified by XRD and its coating consists of lower temperature Al2O3 phase (e.g., γ-Al2O3, θ-Al2O3) and their energy gaps are lower than that of α-Al2O3. Catalytic property of these low temperature Al2O3 phases is rather good. Therefore, F-AZO-AO samples are with almost the same photocatalytic efficiency (near 98%) after 72 h test. The energy gap of I-APS AZO sample is decreased, whereas the energy gap of the F-AZO-AO samples (from F-AO, F-30AO and F-50AO transfer to F-70AO) is inecreased. From SEM and X-ray photoelectron spectroscopy analysis, the results shows that the F-AZO-AO coatings at appropriate amount of Al2O3 are with good enhanced photocatalytic properties. In addition, F-50AO (added with 50 wt.% Al2O3) sample is found to with a nano- and microplatelet morphology in its coating, comparing with F-30AO (added with 30 wt.% Al2O3) and F-70AO (added with 70 wt.% Al2O3) samples. The measured water contact angle of about 140° indicates that F-AZO-AO coatings is with high hydrophobic characteristic and thus has very good practical applications in self-cleaning industry.

摘要.................................i
ABSTRACT.............................iii
目錄.................................vi
表目錄...............................ix
圖目錄...............................x
第1章 緒論............................1
1.1. 前言.............................1
1.2. 文獻回顧.........................2
1.2.1. ZnO材料特性....................2
1.2.2. 熔射技術原理...................3
1.2.3. 電漿熔射技術...................5
1.2.4. 火焰熔射技術...................6
1.2.5. 熔射材料與應用.................9
1.2.6. 光觸媒簡介.....................10
1.3. 研究動機.........................23
1.3.1. 研究目的.......................23
1.3.2. 研究內容.......................25
1.4. 參考資料.........................26
第2章 電漿熔射商用鋁摻雜氧化鋅粉末與其塗層之製備並探討其塗層微結構以及降解亞甲基藍之光催化性能研究....................................33
2.1. 前言.............................33
2.2. 實驗方法與步驟...................34
2.3. 結果與討論.......................40
2.3.1. OM與SEM分析....................40
2.3.2. X-ray相分析與XPS分析...........42
2.3.3. UV-vis DRS 與PL分析............47
2.3.4. 光觸媒分析與親疏水分析.........52
2.3.5. 白光下AZO塗層之抗菌分析........55
2.3.6. 本實驗製造AZO層次塗層之構想....................................56
2.3.7. 結論............. .............57
2.4. 參考資料.........................74
第3章 自製鋁摻雜氧化鋅熔射粉末及其電漿熔射塗層之製備並探討其塗層微結構以及降解亞甲基藍之光催化性能研究....................................79
3.1. 前言.............................79
3.2. 實驗方法與步驟...................82
3.3. 自製熔射粉末與塗層分析...........83
3.3.1. 結論...........................95
3.3.2. 參考資料.......................96
第4章 火焰熔射商用鋁摻雜氧化鋅粉末與其塗層之製備並探討其塗層微結構以及降解亞甲基藍之光催化性能研究...........98
4.1.1. 前言......................................98
4.1.2. 實驗方法與步驟............................104
4.1.3. 火焰熔射塗層分析..........................106
4.1.4. 結論......................................128
4.1.5. 參考文獻..................................129
第5章 總結.......................................133
電漿熔射商業粉末與塗層分析.......................133
電漿熔射自製造粒粉末與塗層分析...................133
火焰熔射自製造粒粉末與塗層分析...................134

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