摘要
本研究利用水熱法結合多孔性陽極氧化鋁模板(PAM)輔助合成硫化銅奈米線。藉由電壓控制、二階段陽極處理等製備條件，探討對PAM模板孔洞大小與規則度的影響。再將模板置於高壓釜中，水熱生成一維CuS奈米線。結果顯示，孔洞的直徑會隨著施加電壓升高而變大，孔洞間距也會增大。而阻障層移除的時間越長則會使第二次陽極處理的孔洞增大，並縮小孔洞間距。在沒有陽極氧化鋁模板孔洞的侷限之下， 水熱生成CuS實驗結果顯示，在反應溫度<,'Times New Roman'; font-family:'新細明體',serif,新細明體">℃，其結構為圓球狀，且成份為富銅相之Cu9S5。而反應溫度≧130℃，會於圓球狀結構表面生成為片狀結構的CuS晶體，形成花狀結構。而CuS奈米線的合成，在反應溫度70℃時，是為非晶的奈米線。而當反應溫度≧100℃時，其奈米線結晶情形分為兩種，顆粒狀與線狀。反應溫度達到190℃時，則全部結晶相只剩單一的線狀。而經由TEM的繞射分析，能做初步判斷其為CuS的成份。而會造成這種原因，我們推測是水熱反應在有限的模板孔洞中所產生的結果。所以本實驗成功使用陽極氧化鋁模板輔助水熱法合成硫化銅奈米線陣列。
關鍵詞：硫化銅奈米線、多孔陽極氧化鋁模版、水熱法，陽極處理
Abstract
In this study, copper sulfide nanowires arrays were synthesized by using hydrothermal method assisted with porous anodized alumina membrane (PAM) template. Various pore sizes were prepared by controlling the voltage and anodizing stages. The results showed that the diameter and spacing of the pore increased as the voltage increases. If the time for removing barrier layer is longer, it will prepare PAM template with larger pore sizes and smaller pore distances. Without the confinement of the PAM template, the copper sulfide is spherical Cu9S5 phase as the hydrothermal temperature becomes smaller than 130℃. When the temperature becomes higher than 130℃, the flower-like CuS powder will be formed. By the assistance of PAM, the CuS nanowire is amorphous as the reaction temperature is 70℃ and the CuS crystallizes when the temperature becomes higher than 100℃. The crystalline CuS nanowires confirmed by TEM diffraction are divided into granular and wire structures. When the temperature becomes higher than 190℃, the morphology of CuS is wire-like crystal. It could be attributed to the fact that the crystal has grown in a limited holes of the template. Therefore, in this study, we successfully prepared CuS nanowires arrays by hydrothermal synthesis assisted by PAM template.
Keywords: Copper Sulfide Nanowires, Porous Anodized Alumina Membrane, Hydrothermal Synthesis, Anodization.