微纳米结构氧化铝粉体合成与应用研究
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摘要
微纳米结构的γ-Al2O3和-Al2O3因为微观上保持了纳米材料的特性，宏观上又克服了纳米材料的不足，而应用于吸附剂、发光材料和催化等领域，因此，其制备方法受到研究者的广泛关注。本论文通过沉淀法制备了形貌规则的六角片状-Al2O3，同时，采用水热法制备了球形、棒状和三维花状的γ-Al2O3和-Al2O3，并研究了其在吸附、发光和导热领域的应用。
沉淀法是常用的制备纳米氧化铝粉体的方法，但是在低温下制备形貌规则的六角片状微纳米结构的-Al2O3仍然存在困难。本论文采用沉淀法首先制备出纳米级不同形貌的碳酸铝铵(AACH)前驱体。实验表明-Al2O3的形貌和相转变点的温度与制备前驱体的形貌和颗粒大小等密切相关,而反应温度和反应体系影响着前驱体的形貌和颗粒大小。将0.2mol/L的硫酸铝铵(AAS)溶液缓慢地滴加到2.0mol/L的碳酸氢铵(AHC)溶液中，同时，控制去离子水反应体系的pH值为9～10，温度为5°C~50°C，并加入PEG2000作为分散剂，可以得到纳米尺寸的颗粒、一维纤维、和三维簇状结构的AACH前驱体。但是当以醇水混合溶液作为反应体系时，可以得到纳米颗粒和束状纤维的AACH前驱体。
为了在低温下制备微纳米结构的片状-Al2O3，本文以一定浓度的HF作酸化剂。通过改变HF的浓度和AACH前驱体在HF中的酸化时间，经煅烧，在低温下制备出直径约为1μm六角片状-Al2O3。实验结果显示，在酸化处理过程中，当HF的浓度为5wt%，酸化处理时间为6h，生成了新物质(NH4)AlF6，形貌呈片状，经700°C煅烧后，转化为棱角分明的规则六角片状θ-Al2O3，当煅烧温度升高至850°C时，前驱体完全转化为菱角圆滑的片状-Al2O3。
氧化铝的应用与其形貌密切相关，为了得到均匀分散，形貌可控的微纳米氧化铝粉体，本论文采用水热法制备微纳米氧化铝粉体。实验结果发现水热温度是前驱体形貌生长的内在控制因素。当水热温度为90°C时AlOOH前驱体形貌为球形；在120°C时，其形貌变为一维纤维状；当温度升高至150°C时，前驱体形貌演变成三维花状结构。基于此，我们提出了γ-AlOOH前驱体形貌生长机理模拟图。同时分析了水热时间对于前驱体相组成的影响，研究发现当水热温度为120°C时，水热时间延长至24h后，经XRD和FT-IR测试结果显示，前驱体的晶型为AACH，但是SEM观察结果显示，前驱体的形貌并未随着时间的延长而改变。此方法确定了以AAS和尿素为原料制备AlOOH前驱体的生长机理，为控制-Al2O3和γ-Al2O3的形貌提供了方向。
本论文还研究了微纳米结构的-Al2O3和γ-Al2O3的应用。研究了六角片状-Al2O3和纤维状-Al2O3，作为环氧树脂的填料在导热材料中的应用。实验结果表明：当填充60wt%的氧化铝粉体时，环氧树脂的导热系数达到最大值，填充了六角片状-Al2O3的环氧树脂导热系数达到了0.81W/m K，而填充了纤维状-Al2O3的环氧树脂的导热系数是0.72W/m K，说明了以六角片状的-Al2O3作填料时的导热性优于纤维状-Al2O3。
此外，还讨论了水热法制备的微纳米γ-Al2O3粉体在吸附和光致发光领域的应用。以刚果红作为被吸附溶液，通过紫外结果显示三维花状结构的微纳米γ-Al2O3的吸附性能优异。光致发光谱分析结果发现，随着煅烧温度的升高，光致发光谱的相对强度减弱，然而800°C煅烧得到的γ-Al2O3样品，发光强度最大，发光谱在410cm-1和460cm-1处。这是因为γ-Al2O3本身存在的缺陷，促使它的晶体场发生变化，从而影响了电子的跃迁。
The micro/nanostructured alumina has been widely used as adsorbent, luminescence andcatalyst etc, due to its excellent advantages of nano and micro structure. In this dissertation,plate-like-Al2O3is prepared by precipitation method, and the micro/nanostructuredspherical, fiber-like and3dimensional (3D) flower-like alumina are obtained successfully byhydrothermal method. Besides, the applications in the fields of adsorption, luminescent andthe thermal conduction are investigated.
The precipitation is most common method to prepared nano-alumina powder, but it isstill a challenge for obtain the micro/nanostructured alumina at a lower temperature. In thisresearch, the nano-sized-Al2O3with different morphologies is synthesized bydecomposition of AACH precursor. The results present that the morphology andtransformation temperature of-Al2O3is determined by the morphology and grain size of theprecursor which are affected by the reaction temperature and the reaction system. In thedeionized water system, nano-sized pherical, fiber-like and3D flower-like AACH precursoris synthesized by adjusting reaction temperature in the range of5~50°C. While in ethanol-water system, the micro-sized spherical and fiber bundle-like AACH are obtained bycontrolling reaction temperature.
In order to prepare micro/nanostructured and plate-like-Al2O3at a lower temperature,hydrofluoric acid (HF) is used as acidifier. In this work, micro/nanostructured and plate-like
-Al2O3is sythesized at850°C by decomposition of AACH precursor treated in the HFsolution. The results indicate that (NH4)AlF6with plate-like morphology is obtained when theprecursor is treated in20mL HF solution with5wt%for6h. In the following decompositionprocess, the plate-like θ-Al2O3with sharp edges is prepared at700°C, and the plate-like-Al2O3with smooth edges is synthesized at850°C.
As the applications of alumina have a close relationship with its morphology and grainsize, the hydrothermal method is induced to prepare micro/nanostructured alumina withcontrollable morphology. The results illustrate that the hydrothermal temperature determinesthe morphology of precursor. AlOOH microspheres, microfibers and3D hierarchical structureare synthesized at hydrothermal temperature of90°C,120°C and150°C, respectively. AlOOHtransforms to γ-Al2O3with unobvious morphology change and volume shrinkage at800°C,and the mesopores are distributed evenly in γ-Al2O3structure, and γ-Al2O3is transformedcompletely to-Al2O3with morphology inherited at1150°C. Based on the experimentalresults, the temperature-dependent formation mechanism is proposed. In addition, we also find that the AlOOH precursor is tranfomed to AACH with no morphology change byprolonging the hydrothermal time. The research above makes contributions to preparingmicro/nanostructured alumina with controlling morphology.
Besides, the applications of γ-Al2O3and-Al2O3are introduced. The plate-like-Al2O3obtained by precipitation method and fiber-like-Al2O3obtained by hydrothermal method areused as thermal conductive fillers. The results indicate that the conductivity coefficient ofEpoxy with plate-like alumina is0.81W/m K when the stuffing fraction is60wt%, while theconductivity coefficient of Epoxy with fiber-like alumina is0.72W/m K, which illustratesthat plate-like alumina is a potential candidate material of thermal conductivity filler.
Meanwhile, the applications of γ-Al2O3used as absorbent and luminecent material areinvestigated. Experimental results present that hierarchically structured γ-Al2O3as absorbentcan remove about99%of Congo red for a while, which inllusrates that the obtainedhierarchically structured γ-Al2O3presents excellent adsorption property in the potentialapplication of waste water treatment. The PL spectrums of γ-Al2O3calcined at800°C presenta strong wide emission bands centred at410cm-1and460cm-1, due to the electron transition,which indicates that γ-Al2O3is a kind of excellent luminecent material.
沉淀法是常用的制备纳米氧化铝粉体的方法，但是在低温下制备形貌规则的六角片状微纳米结构的-Al2O3仍然存在困难。本论文采用沉淀法首先制备出纳米级不同形貌的碳酸铝铵(AACH)前驱体。实验表明-Al2O3的形貌和相转变点的温度与制备前驱体的形貌和颗粒大小等密切相关,而反应温度和反应体系影响着前驱体的形貌和颗粒大小。将0.2mol/L的硫酸铝铵(AAS)溶液缓慢地滴加到2.0mol/L的碳酸氢铵(AHC)溶液中，同时，控制去离子水反应体系的pH值为9～10，温度为5°C~50°C，并加入PEG2000作为分散剂，可以得到纳米尺寸的颗粒、一维纤维、和三维簇状结构的AACH前驱体。但是当以醇水混合溶液作为反应体系时，可以得到纳米颗粒和束状纤维的AACH前驱体。
为了在低温下制备微纳米结构的片状-Al2O3，本文以一定浓度的HF作酸化剂。通过改变HF的浓度和AACH前驱体在HF中的酸化时间，经煅烧，在低温下制备出直径约为1μm六角片状-Al2O3。实验结果显示，在酸化处理过程中，当HF的浓度为5wt%，酸化处理时间为6h，生成了新物质(NH4)AlF6，形貌呈片状，经700°C煅烧后，转化为棱角分明的规则六角片状θ-Al2O3，当煅烧温度升高至850°C时，前驱体完全转化为菱角圆滑的片状-Al2O3。
氧化铝的应用与其形貌密切相关，为了得到均匀分散，形貌可控的微纳米氧化铝粉体，本论文采用水热法制备微纳米氧化铝粉体。实验结果发现水热温度是前驱体形貌生长的内在控制因素。当水热温度为90°C时AlOOH前驱体形貌为球形；在120°C时，其形貌变为一维纤维状；当温度升高至150°C时，前驱体形貌演变成三维花状结构。基于此，我们提出了γ-AlOOH前驱体形貌生长机理模拟图。同时分析了水热时间对于前驱体相组成的影响，研究发现当水热温度为120°C时，水热时间延长至24h后，经XRD和FT-IR测试结果显示，前驱体的晶型为AACH，但是SEM观察结果显示，前驱体的形貌并未随着时间的延长而改变。此方法确定了以AAS和尿素为原料制备AlOOH前驱体的生长机理，为控制-Al2O3和γ-Al2O3的形貌提供了方向。
本论文还研究了微纳米结构的-Al2O3和γ-Al2O3的应用。研究了六角片状-Al2O3和纤维状-Al2O3，作为环氧树脂的填料在导热材料中的应用。实验结果表明：当填充60wt%的氧化铝粉体时，环氧树脂的导热系数达到最大值，填充了六角片状-Al2O3的环氧树脂导热系数达到了0.81W/m K，而填充了纤维状-Al2O3的环氧树脂的导热系数是0.72W/m K，说明了以六角片状的-Al2O3作填料时的导热性优于纤维状-Al2O3。
此外，还讨论了水热法制备的微纳米γ-Al2O3粉体在吸附和光致发光领域的应用。以刚果红作为被吸附溶液，通过紫外结果显示三维花状结构的微纳米γ-Al2O3的吸附性能优异。光致发光谱分析结果发现，随着煅烧温度的升高，光致发光谱的相对强度减弱，然而800°C煅烧得到的γ-Al2O3样品，发光强度最大，发光谱在410cm-1和460cm-1处。这是因为γ-Al2O3本身存在的缺陷，促使它的晶体场发生变化，从而影响了电子的跃迁。
The micro/nanostructured alumina has been widely used as adsorbent, luminescence andcatalyst etc, due to its excellent advantages of nano and micro structure. In this dissertation,plate-like-Al2O3is prepared by precipitation method, and the micro/nanostructuredspherical, fiber-like and3dimensional (3D) flower-like alumina are obtained successfully byhydrothermal method. Besides, the applications in the fields of adsorption, luminescent andthe thermal conduction are investigated.
The precipitation is most common method to prepared nano-alumina powder, but it isstill a challenge for obtain the micro/nanostructured alumina at a lower temperature. In thisresearch, the nano-sized-Al2O3with different morphologies is synthesized bydecomposition of AACH precursor. The results present that the morphology andtransformation temperature of-Al2O3is determined by the morphology and grain size of theprecursor which are affected by the reaction temperature and the reaction system. In thedeionized water system, nano-sized pherical, fiber-like and3D flower-like AACH precursoris synthesized by adjusting reaction temperature in the range of5~50°C. While in ethanol-water system, the micro-sized spherical and fiber bundle-like AACH are obtained bycontrolling reaction temperature.
In order to prepare micro/nanostructured and plate-like-Al2O3at a lower temperature,hydrofluoric acid (HF) is used as acidifier. In this work, micro/nanostructured and plate-like
-Al2O3is sythesized at850°C by decomposition of AACH precursor treated in the HFsolution. The results indicate that (NH4)AlF6with plate-like morphology is obtained when theprecursor is treated in20mL HF solution with5wt%for6h. In the following decompositionprocess, the plate-like θ-Al2O3with sharp edges is prepared at700°C, and the plate-like-Al2O3with smooth edges is synthesized at850°C.
As the applications of alumina have a close relationship with its morphology and grainsize, the hydrothermal method is induced to prepare micro/nanostructured alumina withcontrollable morphology. The results illustrate that the hydrothermal temperature determinesthe morphology of precursor. AlOOH microspheres, microfibers and3D hierarchical structureare synthesized at hydrothermal temperature of90°C,120°C and150°C, respectively. AlOOHtransforms to γ-Al2O3with unobvious morphology change and volume shrinkage at800°C,and the mesopores are distributed evenly in γ-Al2O3structure, and γ-Al2O3is transformedcompletely to-Al2O3with morphology inherited at1150°C. Based on the experimentalresults, the temperature-dependent formation mechanism is proposed. In addition, we also find that the AlOOH precursor is tranfomed to AACH with no morphology change byprolonging the hydrothermal time. The research above makes contributions to preparingmicro/nanostructured alumina with controlling morphology.
Besides, the applications of γ-Al2O3and-Al2O3are introduced. The plate-like-Al2O3obtained by precipitation method and fiber-like-Al2O3obtained by hydrothermal method areused as thermal conductive fillers. The results indicate that the conductivity coefficient ofEpoxy with plate-like alumina is0.81W/m K when the stuffing fraction is60wt%, while theconductivity coefficient of Epoxy with fiber-like alumina is0.72W/m K, which illustratesthat plate-like alumina is a potential candidate material of thermal conductivity filler.
Meanwhile, the applications of γ-Al2O3used as absorbent and luminecent material areinvestigated. Experimental results present that hierarchically structured γ-Al2O3as absorbentcan remove about99%of Congo red for a while, which inllusrates that the obtainedhierarchically structured γ-Al2O3presents excellent adsorption property in the potentialapplication of waste water treatment. The PL spectrums of γ-Al2O3calcined at800°C presenta strong wide emission bands centred at410cm-1and460cm-1, due to the electron transition,which indicates that γ-Al2O3is a kind of excellent luminecent material.
引文
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