本文選題：類普魯士藍 + 介晶��； 參考：《華東師范大學》2015年碩士論文

【摘要】：在近幾年的研究中,類普魯士藍(PBA)這一類金屬有機框架物的應用越來越受到關注。而將其作為一種前驅(qū)體通過熱轉化得到形貌各異,結構多樣,用途廣泛的各類金屬氧化物也取得大量的研究成果。本工作選取一類鉍系的含氧酸鹽和氧化物作為目標產(chǎn)物,特別是多功能性的BiFeO3和Bi2O3,研究了含鉍類普魯士藍向這類化合物的熱轉換過程,及目標產(chǎn)物的應用。具體工作主要分為以下三個方面：1.X片狀類普魯士藍介晶向單晶多孔鈣鈦礦結構金屬氧化物的低溫熱轉化通過在酸性條件下,以檸檬酸三鈉(Sc)和聚乙烯吡咯烷酮(PVP)作為減速劑,通過硝酸鉍和鐵氰化鉀室溫共沉淀的方法,得到X型片狀結構的純相Bi-Fe PBA介晶。通過對不同反應時段樣品SEM圖表明Bi-Fe PBA是由納米級單晶快速取向聚集形成超大的介晶顆粒。將得到的Bi-Fe PBA介晶在400℃條件下煅燒2h得到純相的鈣鈦礦結構BiFeO3。通過SEM結果顯示煅燒后產(chǎn)物形貌與前驅(qū)體保持一致,并產(chǎn)生多孔結構。,TEM分析顯示煅燒后產(chǎn)物為單晶。研究表明,這種介晶到單晶的轉換經(jīng)歷了無定型的中間過程。這有效地避免了較高的能耗,相較于傳統(tǒng)固相反應法,合成溫度降低了將近400℃,這對于工業(yè)化具有潛在的商業(yè)價值。該發(fā)現(xiàn)提供了一種制備單晶介孔材料的新途徑。以這種單晶多孔結構BiFeO3作為光催化劑對羅丹明B有機物進行降解,發(fā)現(xiàn)在4h內(nèi)降解了97%的有機物,表現(xiàn)出良好的催化效率。2.單分散的摻鑭Bi-Fe PBA的合成及其熱轉化產(chǎn)物Bi1-xLaxFeO3的介電響應在室溫條件下,以前一體系的合成方法為基礎,在硝酸鉍的酸溶液中添加不同摩爾比例的硝酸鑭。與鐵氰化鉀的酸溶液均勻混合得到摻鑭的Bi-Fe PBA。通過SEM發(fā)現(xiàn)不同摻鑭比的樣品的形貌結構相同,呈棱柱狀微米級顆粒。TEM可發(fā)現(xiàn)樣品均為典型的介晶顆粒。在空氣氣氛中,400℃條件下煅燒前驅(qū)物得到純相的Bi1-xLaxFeO3。通過SEM, TEM發(fā)現(xiàn)樣品均保持與前驅(qū)物的形貌一致,同樣為介晶顆粒,并存在多孔結構。這說明,利用這種單晶到單晶熱轉化的方法可作為一種有效的摻雜途徑。BET和VSM測試顯示隨著摻鑭比的增加,樣品的比表面積和磁性有所增加,這說明通過鑭的摻入對晶體結構有一定的影響,有助于BiFeO3內(nèi)稟磁性的釋放。作為一種典型的鈣鈦礦結構氧化物,BiFeO3是少數(shù)能夠在室溫下鐵磁性和鐵電性共存的多鐵材料,這種多孔結構Bi1-xLaxFeO3存在一定的介電響應。3. Bi-Co PBA多晶向多孔Bi2-xCoxO3的熱轉化及其光催化性能研究通過按摩爾計量比稱量的硝酸鉍的酸溶液均勻混合到含有鈷氰化鉀的酸性溶液,室溫條件下恒溫6h得到得到純相的Bi-Co PBA。通過SEM圖像分析說明Bi-Co PBA顆粒為長方形塊狀,表面粗糙。在500℃,空氣氣氛條件下煅燒2h得到黑色的粉末。對比XRD標準卡和EDS確定產(chǎn)物為高比例Co摻雜的(Bi2-xCoxO3),摻雜量為x≈0.5。而這種高比例的摻雜量并未發(fā)生相分離,這在文獻中少見報道。通過紫外可見光吸收光譜發(fā)現(xiàn),相對于商業(yè)Bi2O3,樣品Bi2-xCoxO3的吸收峰發(fā)生了紅移,并且在整個可見光范圍都有吸收作用。通過對比商業(yè)Bi2O3, Co3+的摻雜使得Bi2O3的具有微弱的鐵磁性。在對于有機物羅丹明B的光催化效果方面,樣品表現(xiàn)出了相對較好的降解性能。
[Abstract]:In recent years, the application of the metal like organic frame like Prussian blue (PBA) has attracted more and more attention, and a large number of research results have been obtained as a precursor of various kinds of metal oxides with different morphologies, various structures and wide uses. As the target products, especially the multi-functional BiFeO3 and Bi2O3, the thermal conversion process of bismuth Prussian blue to these compounds and the application of the target products are studied. The specific work is mainly divided into three aspects: the low temperature thermal transformation of the 1.X plate-like Prussian Lan Jiejing to the single crystal porous calcium titanium structure metal oxide. Under the acid condition, the pure phase Bi-Fe PBA mesophase of X type sheet structure was obtained by the method of co precipitation of bismuth nitrate and polyvinylpyrrolidone (PVP) as decelerator, through the co precipitation of bismuth nitrate and potassium ferricyanide at room temperature. Through the SEM diagram of the samples at different reaction periods, the Bi-Fe PBA was formed by the rapid orientation of the nanoscale single crystal to form the super large PBA. Mesocrystalline particles. The Bi-Fe PBA mesocrystalline was calcined at 400 centigrade to get the perovskite structure of the pure phase, and the perovskite structure of the pure phase was obtained by the SEM result. The results showed that the morphology of the product was consistent with the precursor and produced the porous structure. The TEM analysis showed that the calcined product was single crystal. The study showed that the transformation of this kind of mesophase to single crystal has experienced an amorphous structure. The intermediate process. This effectively avoids the high energy consumption. Compared with the traditional solid state reaction method, the synthesis temperature is reduced by nearly 400 degrees C, which has potential commercial value for industrialization. The discovery provides a new way to prepare the single crystal mesoporous materials. This single crystal porous structure BiFeO3 is used as a photocatalyst to the Luo Danming B organic matter. It was found that 97% of organic matter was degraded in 4h, showing a good catalytic efficiency of.2. monodisperse lanthanum doped Bi-Fe PBA and the dielectric response of Bi1-xLaxFeO3 in the heat conversion product at room temperature. At room temperature, the synthesis method of the previous system was based on the addition of lanthanum nitrate with different molar ratios in the acid solution of bismuth nitrate and iron cyanide. The Bi-Fe PBA. of lanthanum mixed with the acid solution of the potassium chloride is obtained by SEM. The samples with different lanthanum ratio are found to have the same morphology and structure, and the prismatic micron grade particle.TEM can find that all the samples are typical mesocrystalline particles. In the air atmosphere, the calcined precursors of the calcined precursors at 400 degrees C are obtained through SEM, and TEM is found to be preserved by TEM. This shows that the method of using this single crystal to the single crystal heat conversion can be used as an effective doping method.BET and VSM test to show that the specific surface area and magnetic properties of the sample increase with the increase of the ratio of lanthanum, which indicates that the crystal structure is doped through the addition of Lanthanum. It is helpful to the release of intrinsic magnetic properties of BiFeO3. As a typical perovskite structure oxide, BiFeO3 is a few ferromagnetic materials capable of coexisting ferromagnetism and ferroelectricity at room temperature. This porous structure Bi1-xLaxFeO3 has a certain dielectric response to the thermal transformation of.3. Bi-Co PBA polycrystalline to porous Bi2-xCoxO3 and its light acceleration. The study of chemical properties is even mixed with acid solution of bismuth nitrate, which is weighed by massage, to acid solution containing cobalt cyanide. At room temperature, the Bi-Co PBA. of pure phase is obtained at constant temperature 6h to show that Bi-Co PBA particles are rectangular block and surface is rough. At 500 degrees, the calcined 2H gets black under air atmosphere. A high proportion of Co doped (Bi2-xCoxO3) is compared to the XRD standard card and EDS, and the amount of doping is x 0.5., and the high proportion of doping does not occur. This is rarely reported in the literature. A visible light range have absorption effect. By comparing the commercial Bi2O3, Co3+ doped Bi2O3 with weak ferromagnetic. In the photocatalytic effect on organic matter of rhodamine B, the sample shows relatively good performance degradation.
【學位授予單位】：華東師范大學
【學位級別】：碩士
【學位授予年份】：2015
【分類號】：TQ135.32

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