碳微球的溶劑熱法制備及其在修飾電極上的應(yīng)用
發(fā)布時間:2018-05-22 17:18
本文選題:碳微球 + 溶劑熱法; 參考:《湖北民族學(xué)院》2010年碩士論文
【摘要】:碳微球是碳材料的一個分支,具有許多優(yōu)良的特性,因此很多學(xué)者對其進(jìn)行了研究,包括性質(zhì)、合成方法、應(yīng)用等。 溶劑熱法制備碳微球是近幾年來興起的一種制備碳微球的有效方法,因其操作簡單和對環(huán)境友好而備受青睞。 本論文以葡萄糖為碳源,利用溶劑熱的方法對碳微球的合成進(jìn)行了探討,制得了球形和橄欖球形碳球,并對影響碳微球形貌和直徑的條件進(jìn)行了探索。實(shí)驗(yàn)數(shù)據(jù)表明,溶劑和升溫速率分別是影響碳微球形貌和直徑大小的關(guān)鍵因素。 長期以來,碳微球的應(yīng)用主要集中在復(fù)合材料模板、催化劑載體和鋰離子電池材料等方面,碳微球在修飾電極上的應(yīng)用幾乎沒有報(bào)道。本論文通過對碳微球性質(zhì)的深入分析,提出了將碳微球修飾于玻碳電極表面,制得碳微球修飾玻碳電極的構(gòu)想,實(shí)驗(yàn)證明這種構(gòu)想是可行的,在碳微球修飾玻碳電極對鎘離子的測定中修飾電極表現(xiàn)出的良好的選擇性、穩(wěn)定性、和低檢測限充分說明了這一點(diǎn)。從而拓展了碳微球的應(yīng)用領(lǐng)域。 論文主要包括以下幾個方面的內(nèi)容: 1.碳微球的溶劑熱法制備。利用溶劑熱法制備碳微球,并對碳微球進(jìn)行了表征。通過改變反應(yīng)的升溫速率和溶劑,使得碳微球的大小和形貌都分別發(fā)生了改變,實(shí)驗(yàn)表明,碳微球的直徑受反應(yīng)升溫速率的影響,而形貌則受溶劑的影響。為研究碳微球的形成機(jī)理研究提供了依據(jù)。 2.碳微球修飾玻碳電極的制備。通過對不同分散劑分散效果的對比,選擇環(huán)己醇作為分散劑,制備了碳微球修飾玻碳電極,并對修飾電極進(jìn)行了表征,掃描電鏡表面碳微球能較好地分散并修飾于玻碳電極上,碳微球的修飾對玻碳電極的性能產(chǎn)生了影響。碳微球修飾玻碳電極對鎘離子具有響應(yīng)。 3.碳微球修飾玻碳電極對鎘離子的測定及其條件的優(yōu)化。詳細(xì)研究了利用碳微球修飾玻碳電極測量鎘離子濃度的條件,采用循環(huán)伏安法研究了鎘離子在修飾電極上的伏安行為和最佳檢測條件。在所選最優(yōu)化實(shí)驗(yàn)條件下,峰電流與鎘離子濃度在5×10~(-9)-1.34×10~(-7) mol/L和1.34×10~(-7)-1×10~(-6) mol/L范圍內(nèi)呈現(xiàn)良好的線性關(guān)系,線性相關(guān)系數(shù)分別為0.9989和0.9998,檢測限為10~(-10)mol/L。該法用于模擬水樣中鎘離子的測定,結(jié)果令人滿意。
[Abstract]:Carbon microspheres are a branch of carbon materials with many excellent properties, so many scholars have studied them, including their properties, synthesis methods, applications and so on. Solvothermal preparation of carbon microspheres is an effective method for the preparation of carbon microspheres in recent years. In this paper, the synthesis of carbon microspheres using glucose as carbon source was investigated by solvothermal method. Spherical and rugby carbon spheres were prepared, and the conditions affecting the morphology and diameter of carbon microspheres were explored. Experimental data show that solvent and heating rate are the key factors affecting the morphology and diameter of carbon microspheres, respectively. For a long time, the application of carbon microspheres has been mainly focused on composite template, catalyst carrier and lithium ion battery materials, etc. The application of carbon microspheres in modified electrodes has not been reported. Based on the analysis of the properties of carbon microspheres, the idea of preparing carbon microspheres to modify glassy carbon electrodes by modifying carbon microspheres on the surface of glassy carbon electrodes is proposed in this paper, which is proved to be feasible by experiments. The good selectivity, stability and low detection limit of the modified electrode for the determination of cadmium ion at the glassy carbon electrode modified with carbon microspheres fully demonstrate this point. Thus the application field of carbon microspheres is expanded. This paper mainly includes the following aspects: 1. Preparation of carbon microspheres by solvothermal method. Carbon microspheres were prepared by solvothermal method and characterized. The size and morphology of the carbon microspheres were changed by changing the heating rate and solvent. The experimental results showed that the diameter of the carbon microspheres was affected by the reaction heating rate and the morphology was influenced by the solvent. It provides a basis for the study of the formation mechanism of carbon microspheres. 2. Preparation of glassy carbon electrode modified with carbon microspheres. By comparing the dispersion effects of different dispersants, the carbon microspheres modified glassy carbon electrodes were prepared by using cyclohexanol as dispersant, and the modified electrodes were characterized. The carbon microspheres on the surface of scanning electron microscope can be dispersed and modified onto the glassy carbon electrodes. The modification of carbon microspheres affected the performance of glassy carbon electrode. Carbon microspheres modified glassy carbon electrode are responsive to cadmium ion. 3. Determination of cadmium ion at glassy carbon electrode modified by carbon microspheres and optimization of its conditions. The conditions for the determination of cadmium ion concentration at glassy carbon electrode modified by carbon microspheres were studied in detail. The voltammetric behavior of cadmium ion on the modified electrode and the optimum detection conditions were studied by cyclic voltammetry. Under the optimized experimental conditions, the linear relationship between the peak current and the concentration of cadmium ion in the range of 5 脳 10 ~ (-9) -1.34 脳 10 ~ (-7) mol/L and 1.34 脳 10 ~ (10) ~ (-7) ~ (-1) mol/L was obtained. The linear correlation coefficients were 0.9989 and 0.9998, respectively, and the detection limit was 10 ~ (-10) mol 路L ~ (-1). The method has been applied to the determination of cadmium ion in simulated water with satisfactory results.
【學(xué)位授予單位】:湖北民族學(xué)院
【學(xué)位級別】:碩士
【學(xué)位授予年份】:2010
【分類號】:O646.54
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