本研究係以恆溫沈澱法及非恆溫沈澱法製備CeO2奈米微粉。文中探討各製備變因，包括反應溫度、氣氛、溶劑、前驅鹽種類等對所得微粉形狀、粒徑、晶態、光學性質等特性之影響，並由粒子之演化過程探討微粉之生成機制。另外，以製備之CeO2微粉作觸媒進行CO氧化反應，比較各觸媒之催化活性，並針對CeO2微粉特性對催化活性之影響來加以探討。

　　實驗結果發現，以恆溫沈澱法製備CeO2微粉，所得產物多為顆粒狀，粒徑約在5-20 nm之間，且隨反應溫度之降低而減小，其UV吸收峰出現藍位移，能隙則呈現量子限量化效應。當反應溫度由30 oC升至90 oC，以TEM觀察到產物形狀由四邊形變為六角形，此乃因{111}晶面在高溫下佔優勢所致。以醇-水溶液作反應系溶劑時，發現所得微粉粒徑依序為：pure water > MeOH/water > EtOH/water ≒ n-PrOH/water ≒ i-PrOH/water ≒ t-BuOH/water > EG/water，且隨醇添加量之增加，微粉粒徑減小。由於溶液之介電常數隨溶劑種類及組成而變，文中提出粒徑與介電常數之關係(1/dp = A + B/ε)，可合理解釋本實驗之結果。另外，改變反應氣氛N2-O2混合氣流中氧氣濃度來進行微粉製備，結果發現，當氧氣濃度大於50 %時，會有針狀CeO2出現，且氧氣濃度愈高時，針狀產物比例愈高。

　　觀察CeO2微粉在恆溫沈澱中粒子之演化情形，發現在高溫 (> 50 oC)時，初始沈澱物Ce(OH)3為針狀，低溫(< 50 oC)時則為極細微粉凝成之膠狀物。針狀Ce(OH)3中間產物會隨反應進行而逐漸裂解、剝離出3-5 nm之微晶，再經OA、OR模式而長成顆粒狀晶體。低溫下極細之Ce(OH)3中間產物則隨時間逐漸成長為顆粒狀CeO2。

　　以非恆溫沈澱法製備CeO2微粉，係將製程分成不同操作溫度之沈澱(反應初期5分鐘)與熟成(20小時)兩階段。在高溫沈澱(70-90 oC)、低溫熟成(0 oC)製程下，針狀Ce(OH)3中間產物會轉變為針狀CeO2奈米微粉，且微粉表面具有較高比例之{100}及{110}晶面，推測係因針狀Ce(OH)3中間產物依類結構(topotactic)機制所生成。因此，針狀Ce(OH)3中間產物對最終微粉之形狀具有極為關鍵之角色。實驗中並發現，針狀CeO2奈米微粉僅能由Ce3+前驅鹽獲得，無法以Ce4+前驅鹽得之。

　　以N-0(針狀)、CN-0(鍛燒過之針狀)、P-90(顆粒狀)、CP-90(鍛燒過之顆粒狀)及CERAC(商用粉體)五種CeO2微粉作觸媒，比較其CO氧化反應之催化活性。結果發現，各觸媒之催化活性依序為：CN-0 > N-0 > CP-90 > P-90 > CERAC。經600 oC鍛燒6小時之觸媒(CN-0, CP-90)催化活性較未鍛燒處理(N-0, P-90)之催化活性高，且針狀CN-0觸媒之活性最佳，在275 oC下反應之轉化率較商用微粉提升約3.5倍。另由氫氣程溫還原分析結果顯示，CN-0觸媒之表面氧比例最高，與其催化活性相符。由於CN-0觸媒表面以高活性之{110}及{100}晶面居多，較易釋放表面之氧參與反應，故其催化活性最高。另外，CO程溫脫附及紅外線吸收光譜分析亦顯示，CN-0觸媒對CO之吸附能力較CP-90強。此即顯示CeO2微粉晶形對其反應催化活性影響甚鉅，亦提供未來針狀CeO2奈米微粉在催化應用之一發展方向。

　In this study, CeO2 nanoparticles are synthesized by isothermal and non-isothermal precipitations, respectively. The effects of solvents, temperatures, atmospheres and precursors, on the particle size, shape, crystalline structure, optical properties are investigated. The CeO2 particle evolutions at various temperatures are also explored. Furthermore, the catalytic activities for CO oxidation over various CeO2 nanoparticles are studied.

　Experimental results show that, via isothermal precipitation, the particle sizes of resulting products are decreased from 20 to 5 nm by decreasing the reaction temperature, which also results in the blueshift of UV absorption due to quantum size effect. As the reaction temperature increases from 30 to 90 oC, the particle shape observed from TEM images transforms from tetragonal to hexagonal attributed to the preferable {111} planes at higher temperature. Moreover, for the CeO2 synthesis in alcohol-water systems, the particle size of resulting products decreases in order as pure water > MeOH/water > EtOH/water ≒ n-PrOH/water ≒ i-PrOH/water ≒ t-BuOH/water > EG/water. Also, the particle size decreases with increasing the amount of alcohol. Since the dielectric constant of reaction medium plays an important role on the nucleation of particles, a comprehensive model correlated between final particle size (dp) and dielectric constant (ε) in mixed solvents (1/dp = A+ B/ε) is obtained. In addition, high oxygen-containing atmosphere, e.g., O2 concentration above 50 %, needle-like CeO2 nanoaprticles are found in the final products.

　From the evolutions of CeO2 particles at reaction temperatures of 0-90 oC, it is found that the initial Ce(OH)3 precipitate is needle-like at the stage of precipitation above 50 oC. Whereas Ce(OH)3 tiny nanoparticles are precipitated below 50 oC. Afterwards, the Ce(OH)3 needles are broken into nanocrystals and then transformed to be hexagonal-shaped via orientated attachment (OA) and Ostwald ripening (OR) mechanisms.

　The non-isothermal preparation includes two stages, i.e., precipitating at a given temperature for 5 min, and followed by aging at alternative temperature for 20 hr. The results show that, the final products, synthesized by precipitating at higher temperature (70-90 oC) and then aging at very low temperature (0 oC), are needle-like which are via topotactic mechanism. It is worth to note, the surfaces of CeO2 nanoneedles are preferrably composed of {100} and {110} facets. In addition, the CeO2 nanoneedles can only be obtained starting from the Ce3+ precursor, which can not be formed from the Ce4+ precursor.

　Furthermore, CO oxidation is used as the model reaction to compare the catalytic activity of various CeO2 nanoparticles. The results show that the activities of catalysts decrease in order as CN-0 (calcined nanoneedles) > N-0(nanoneedles) > CP-90(calcined nanohexagons) > P-90 (nanohexagons) > CERAC(commercial powders). It reveals the activity of catalyst can be enhanced by means of calcination treatment due to the higher degree of crytallinity. Among five catalysts, CN-0 exhibits highest catalytic activity. For example, the CO conversion for CN-0 at 275 oC is about 3.5 times higher than that for commercial powders. This result can be comprehended from the temperature programming reduction (TPR) result of CN-0 catalyst which provides the most surface oxygen sites preferably composed of higher active {110} and {100} facets. In addition, the results of temperature programming desorption (TPD) and IR absorption spectra indicate that stronger adsorption of CO is found for CN-0 than CP-90. Therefore, the morphological manipulation of CeO2 nanoparticles is quite important for determining their catalytic oxidation activity, which also reveals the promise of needle-like CeO2 in future uses.

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