本研究中，我們以電噴灑式氣相奈米粒子電移動度分析儀 (Electrospray-differential mobility analyzer, ES-DMA) 此氣相電泳法作為基礎，建立一高解析度的分析技術與方法，用於進行溶劑熱法製備功能膠體奈米材料之研究。藉由其他儀器的數據輔助，加以分析膠體材料合成時所涉及的配方化學以及界面化學效應，此有助於後續開發其他的新型功能膠體材料以優化材料的性能表現，進一步用於催化或是能源環境之應用。
首先，本研究的第一部分，我們針對金屬-有機骨架 (Metal-organic framework, MOF) 膠體粒子於溶劑熱合成過程中之生長情形進行研究。我們選用HKUST-1此銅基MOF作為代表性材料，並透過ES-DMA量測所得之數據，探討隨著合成溫度、合成時間以及有機配體前驅物濃度等合成條件改變，其電移動度粒徑分布與數量濃度等基本性質的變化。我們分別利用粉末X光繞射儀 (X-ray diffraction analyzer, XRD) 和比表面積與孔隙度分析儀 (Brunauer-Emmett-Teller analyzer, BET) 量測MOF材料的結晶程度與孔洞結構變化情形，以提供相輔之分析結果，以了解合成參數與材料特性之間的關聯性。結果指出，HKUST-1膠體奈米粒子的電移動度粒徑、結晶度、比表面積與孔體積，都會隨著合成時間增加而提升，並呈現正相關趨勢，進一步提高合成溫度時，也能夠觀察到類似現象且更加明顯。此外，透過改變有機配體前驅物濃度，結果顯示電移動度粒徑會隨著前驅物濃度增加而提升，綜合上述可歸納出電移動度粒徑與結晶度呈正相關，而結晶度增加也會使得材料比表面積增加。同時，我們也將合成的HKUST-1材料於常溫常壓 (1 atm, 35℃) 進行CO2吸附能力量測，由結果得知其電移動度粒徑大小大致與CO2吸附量呈一次方的正比關係。因此，我們除了能透過控制合成條件製備不同尺寸大小、晶徑與比表面積的HKUST-1奈米粒子，也能藉由ES-DMA量測得到電移動度粒徑分布並對應其CO2吸附量 (即在溶劑熱合成過程中量化HKUST-1於CO2捕捉的吸附量，對於開發或是優化MOF材料於CO2捕捉應用提供一定量且快速評估之方法。
本研究的第二部分，則針對葡萄糖衍生碳球 (Glucose-derived carbon nanosphere, GCNS) 進行研究。首先，藉由改變合成時間與結構導向劑濃度對以溶劑熱法製備的預碳化碳球進行研究。利用ES-DMA量測數量濃度、電移動度粒徑分布等基本性質的變化，觀察合成參數對於尺寸大小和膠體穩定性的影響，了解合成條件與材料性質之間的關聯性。此外，藉由掃描式電子顯微鏡 (Scanning electron microscopy, SEM)、穿透式電子顯微鏡 (Transmission electron microscopy, TEM) 以及比表面積與孔隙度分析儀 (Brunauer-Emmett-Teller analyzer, BET) 的數據觀察材料的型態、比表面積與孔洞結構。另外透過加入不同比例的氫氧化鉀 (Potassium hydroxide, KOH) 進行煅燒活化，於表面產生孔洞結構以提升材料的比表面積，結果顯示當KOH相對於預碳化碳球的重量比達到3倍時，因為材料的高比表面積與孔隙度，其電容表現可以達到最大電容值162 F/g。在此階段的工作中，我們成功在定量的基礎上鑑定以溶劑熱法製備的膠體奈米碳材，並透過定量分析深入探討預碳化碳球的生成機制與觀察粒徑的變化，有望優化多孔奈米碳材的重要材料性能，進一步提升用於電化學領域之電極材料的性能表現。

In this study, we demonstrate a high-resolution characterization method, electrospray-differential mobility analysis (ES-DMA) based on the gas-phase electrophoretic method for understanding the solvothermal synthesis of the functional nanomaterial colloids. The analyses from other instruments are employed complementarily to the ES-DMA. The understanding correlated to the interfacial phenomena of colloidal materials are useful for the development of other functional nanomaterial colloids for their performance optimization in catalytic and energy applications.
In the first part of this work, we focus on the solvothermal growth process of metal-organic framework (MOF) colloids. HKUST-1 is selected as the representative copper-based MOF material, and ES-DMA is used for the analysis of synthesis parameters versus the fundamental material properties. Mobility size distributions and number concentrations of MOF versus the synthetic temperature, synthetic time and the concentrations of precursor in the solvothermal process are successfully characterized on a quantitative basis. To know the relationship between the synthesis parameters and the material properties, the crystallinity variation of MOF material and the consequent changes in pore structure are analyzed by using powder x-ray diffraction analyzer (XRD) and the Brunauer-Emmett-Teller (BET) surface area measurement, respectively. The results show that the physical sizes and the crystallinity variation, the specific surface area and pore volume of HKUST-1 colloids increase with synthetic temperature and synthetic time. Moreover, the physical sizes of HKUST-1 colloids also increase with the concentrations of the organic ligand precursors. In addition, we measure the CO2 uptake capacity of the synthesized HKUST-1 colloids at normal pressure and temperature (i.e., 1 atm, 35 °C). From the results, we found the CO2 uptake capacity is proportional to the mobility size of the synthesized MOF colloids. The work provides a proof of concept for controlled synthesis of MOF colloids supported by a fast, quantitative characterization. The proposed approach is shown to be useful for the development and optimization of CO2 uptake capacity through the development of MOF colloids for the applications of CO2 capture and utilization.
In the second part of this work, we focus on glucose-derived carbon nanosphere (GCNS) colloids. First, we investigate the solvothermal growth process of the pre-carbonized nanosphere. The effect of synthetic time and concentrations of the structure directing agent on the cluster size and colloidal stability are investigated through a quantitative characterization of mobility size distributions by ES-DMA. Scanning electron microscopy (SEM), transmission electron microscopy (TEM) and the Brunauer-Emmett-Teller (BET) surface area analyzer are employed complementarily for the determination of morphology, specific surface area and pore structure of the materials. Subsequently, potassium hydroxide (KOH) is used as the activating agent to produce the micropore structure increasing the specific surface area and porosity of the carbon materials. The results show that GCNS has the maximum specific capacitance capacity of 162 F/g was achieved when the ratio of KOH to pre-carbonized carbon reaches 3 times, in corresponding to high surface area and porosity. The work demonstrates a prototype study of fabricating nanocarbon porous colloidal material with the support of quantitative characterization. The mechanistic understanding developed by the quantitative analysis shows promise for a further optimization of the critical material properties of nanocarbon porous colloidal material to further improve the performance in electrochemistry application.

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