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Please use this identifier to cite or link to this item: http://ntour.ntou.edu.tw:8080/ir/handle/987654321/52172

Title: 溶膠凝膠法製備特殊表面形貌之氧化鋯薄膜及其光學性質之關係研究
Authors: Lee, Po-I
李柏逸
Contributors: NTOU:Institute of Materials Engineering
國立臺灣海洋大學:材料工程研究所
Keywords: 氧化鋯薄膜;表面形貌;光致發光;光催化
zirconia thin film;surface morphology;photoluminescence;photocatalysis
Date: 2018
Issue Date: 2019-05-23T06:19:41Z
Abstract: 本研究利用溶膠凝膠法製備奈米氧化鋯薄膜,過程中添加5 % PVA以增加溶液的黏滯性,並使用旋轉塗佈(Spinning coating)鍍膜,再鍍膜完成時放置於加熱盤上進行30ºC、70ºC、90ºC的加溫約30分鐘,分別成功製備出平整、編織狀(basket-wave-like)與網狀(network)氧化鋯薄膜,之後在大氣中進行400ºC、500ºC、600ºC的鍛燒,並將鍛燒完成後的樣品進行顯微結構分析與光學實驗檢測,以探討不同表面形貌和不同溫度鍛燒下的光學性質差異。本實驗使用X光繞射儀檢測其相組成並計算晶粒尺寸、掃描式電子顯微鏡觀察形貌、光致發光光譜儀檢測各樣品的光致發光強度以進行比較、光催化實驗測量樣品在不同降解時間下對亞甲基藍液的降解程度、原子力顯微鏡檢測不同形貌的粗糙度。 實驗結果顯示,透過SEM分析觀察到在加熱盤上進行加熱會使得氧化鋯膠粒產生團聚,以產生出三種不同的形貌,分別為平整、編織狀、網狀。在大氣400ºC和500ºC鍛燒後,氧化鋯薄膜皆為四方晶相,但在600ºC鍛燒後會有單斜晶相的產生。在光致發光實驗中400ºC擁有最高的光致發光強度,光致發光強度會隨著鍛燒溫度升高而降低,而在不同的形貌中,平整與網狀擁有比編織狀更高的光致發光強度。在光催化實驗中,結果顯示編織狀與網狀形貌氧化鋯薄膜因擁有較大的比表面積進行反應,因此其降解率皆比平整氧化鋯薄膜較來的好。此外,光降解率會隨溫度提高而降低。在400ºC鍛燒下編織狀形貌氧化鋯薄膜的降解率可達近乎80%。
This thesis is to synthesize nano-scale tetragonal zirconia (t-ZrO2) thin films using the sol-gel method with 5% PVA addition for increasing the adhesion of sol-gel solutions. The sol-gel solutions were subsequently spinning-coated on silicon substrates. Three specific surface morphologies, flat, basket-wave-like and network were successfully produced after baking on a hot plate separately at 30ºC, 70ºC and 90ºC for 30 min. Furthermore, these zirconia thin films were calcined at 400ºC, 500ºC and 600ºC for 2 hr in air. The calcined specimens are examined the microstructure analysis and optics properties to study the variation of the thin film with distinct surface morphology under various calcination temperatures using x-ray diffractometer (XRD), scanning electron microscope (SEM), photoluminescence (PL), photocatalysis and atomic force microscopy (AFM). Meanwhile, the crystalline sizes of t-ZrO2 in thin films were evaluated with Scherrer equation from the XRD results, and the photodegrdation time of ZrO2 thin films with distinct surface morphologies in methylene blue (MA) solution were also tested. The results shows that the flat, basket-wave-like and network morphologies are formed after baking on a hot plate separately at 30ºC, 70ºC and 90ºC for 30 min, respectively. The formation of the specific surface morphologies are attributed to the agglomeration of ZrO2-gel particles during baking. The microstructures of ZrO2 thin films after calcining at 400ºC and 500ºC both exhibited tetragonal phase, but monoclinic phase also formed in the ZrO2 thin film after 600ºC calcination. The thin film with flat morphology calcined at 400ºC showed the high PL intensity. Moreover, the PL intensity of the specimens decreased with increasing calcination temperatures, in which the thin films of flat and network morphologies displayed higher PL intensity than that of basket-wave-like morphology. For photocatalysis characterization, the basket-wave-like and network morphologies specimens both showed better photodegrdation than the flat morphology specimen. Because the basket-wave-like and network morphologies specimens exhibit larger surface roughness from AFM analysis, the two morphologies have larger surface defects leading to better photodegrdation. Besides, photodegradation degree decreased with increasing calcination temperatures. The photodegradation ratio of the ZrO2 thin film with basket-wave-like morphology calcined at 400ºC could reach to near 80%.
URI: http://ethesys.lib.ntou.edu.tw/cgi-bin/gs32/gsweb.cgi?o=dstdcdr&s=G0010555016.id
http://ntour.ntou.edu.tw:8080/ir/handle/987654321/52172
Appears in Collections:[材料工程研究所] 博碩士論文

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