γ-氧化铝和尖晶石型偏铝酸锌纳米结构的离子液体辅助水热法可控合成研究
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摘要
金属氧化物纳米材料因其优异的光、电、热、磁性能,成为化学、材料、物理等领域的重要研究方向之一。科学研究表明,材料的性能和应用取决于其晶型、形貌、尺寸和组成等,因此,金属氧化物纳米材料结构和形貌的控制合成不仅具有重要的理论意义,而且在很多方面还有很大的应用价值。其中氧化铝和尖晶石型偏铝酸锌均为廉价而有用的工业材料,引起人们广泛的关注。本论文在γ-氧化铝和尖晶石型偏铝酸锌ZnAl2O4纳米材料的离子液体辅助水热合成新途径及调控合成新方法等方面进行了探索性研究。
离子液体是在室温下完全由离子组成的有机溶剂,由于其特殊的物理和化学性能在无机纳米材料合成方面引起人们广泛的关注。在离子液体辅助下,开发新的合成方法,同时对γ-氧化铝和尖晶石型偏铝酸锌ZnAl2O4纳米结构形貌进行控制合成是本论文的重点。具体的研究内容包括：
(1)碱式醋酸铝为前驱物离子液体辅助水热法合成Y-氢氧化氧铝和Y-氧化铝纳米结构研究。首先,以乙酸钾和氯化铝为反应物,以离子液体氯代1-丁基-2,3-二甲基咪唑([Bdmim][Cl)])为模板剂,通过水热法制备了不同形貌的碱式醋酸铝(CH3COO)2Al(OH)纳米晶,包括树叶状、纤维状、花状、多面体和纳米棒。在制备过程中,以离子液体为模板剂,通过调节离子液体浓度,反应物浓度和反应温度即可有效地对产物的形貌进行调控。研究发现,离子液体浓度对具有不同形貌的前驱物碱式醋酸铝纳米结构的形成起到了关键的作用。吸附在前驱物晶体表面的离子液体阳离子使纳米结构稳定,随着离子液体量增加可以制备一、二、三维纳米结构。通过前驱物在高温下煅烧,即可得到形貌保持不变的γ-氢氧化氧铝和γ-氧化铝纳米结构。表面性能研究表明所得γ-氧化铝纳米结构显示良好的表面和气孔性能,得到的γ-氧化铝纳米结构具有250-380m2/g的比表面积和大约3.5nm的孔径。
(2)以碱式醋酸铝为前驱物,通过前驱物分解与络合物生成反应的耦合反应,一步合成γ-氢氧化氧铝纳米结构的新途径研究。在一样的反应体系中,通过加一定量的Zn(NO3)2,即可直接得到花状γ-氢氧化氧铝钠米结构。添加的Zn2+离子为一种耦合反应驱动剂,对γ-氢氧化氧铝的形成起到关键的作用。另外,离子液体作为模板剂,对产物的形貌起到非常重要的作用,随着离子液体量增大,花状结构的尺寸变小,而构成花儿的纳米叶的长宽比变大了。最后得到的花状γ-氧化铝纳米结构具有150m2/g左右的比表面积和3.6nm的孔径。
(3)离子液体辅助水热法制备碱式碳酸铝钠NaAl(OH)2CO3 (Na-Dowsonite)纳米棒以及高能电子束辐射制备纳米管。首先以氯化铝和碳酸氢钠为反应物,以离子液体氯代1-丁基-2,3-二甲基咪唑([Bdmim][Cl)])为模板剂,在水热体系中制备出直径为25nm,长度为200nm的碱式碳酸铝钠纳米棒,产物不仅大小均匀而且分散性良好。然后以碱式碳酸铝钠为前驱物,通过高能电子束辐射制备出纳米管。在电子束分解过程当中,前驱物碱式碳酸铝钠的分解过程与普通热分解过程完全不一样。在热分解过程,分解产物为偏铝酸钠(NaA102),而电子束分解产物是表面为氢氧化氧铝(AlOOH)和内部为碳酸钠(Na2CO3)的两层结构。
(4)以碱式碳酸铝钠为前驱物在低温下Zn2+离子交换制备偏铝酸锌ZnAl2O4纳米结构的新途径。首先通过Zn2+离子交换反应得到中间体Al2O3·H20和Zn6Al2(OH)16·CO3·4H2O混合晶体的纳米片,然后在700℃煅烧2h所得偏铝酸锌(ZnAl2O4)纳米片。其纳米片由直径为约20nm的纳米颗粒组成,颗粒之间存在有气孔。这些气孔是在煅烧过程当中因中间体分解脱水而形成的。研究结果表明ZnAl2O4纳米片产物具有245m2/g的比较高的比表面积。离子液体在纳米片的生长过程中起到模板剂的作用。
(5)以碳酸铵为碱源离子液体辅助水热法γ-氧化铝纳米结构调控合成。在相同的反应体系当中,随着温度变化得到不同物相和形貌的产物。在75℃下得到竹叶状碱式碳酸铝铵纳米结构,而在120℃下得到γ-AlOOH纳米棒或者纳米线。当温度为150℃时,产物的形貌六角形纳米片。在不同合成条件下,离子液体对产物形貌的影响明显。
总之,本文主要研究了关于氧化铝和偏铝酸锌纳米材料的简便且环境友好的离子液体辅助水热合成法,证明了离子液体的使用使制备的材料具有新颖的形貌和优化的性能,并且可能为更多无机纳米材料的可控合成提供一个新的思路。
Most recently, metal oxides nanomaterials have become one of the most important research directions of chemistry, materials, and physics because of their excellent optical, electrical, thermal, and magnetic properties. Moreover, several researches indicated that the performance and application of the nanomaterials are decided by their phases, morphologies, sizes, and compositions. Thus, structure and shape controlled synthesis of nanoscale metal oxides will not only bring the theoretically progresses, but also extend the corresponding application field. Among them aluminum oxide, aluminum oxide hydroxide and zinc aluminate spinel compound are low cost materials widely used in industries, therefore have attracted interest. In this dissertation, a valuable research has been carried out to explore the new ionic liquid-assisted hydrothermal routes to y-aluminum oxide and ZnAl2O4 spinel nanostructures.
Ionic liquids (ILs), which are liquid salts at room temperature, have attracted tremendous attention due to their unique properties. As a burgeoning field, ILs has been employed as solvents, reactants, or templates for the preparation of inorganic nanomaterials. In this paper, ILs was used to prepared y-aluminum oxide and ZnAl2O4 spinel nanostructures. The purposes are to develop new synthetic methods of y-aluminum oxide and ZnAl2O4 spinel and explore the new functions of ILs. The main points can be summarized as follows:
(1) Morphology controllable synthesis of y-alumina nanostructures via two step ionic liquid-assisted hydrothermal route. Firstly, precursor aluminum acetate hydroxide (CH3COO)2A1(OH) crystals with different morphologies, including nanoleaves, nanofibers, flowerlike nanoarchtectures, polyhedrons, and nanorods, by using ionic liquid 1-buthyl-2,3-dimethyl imidazollium chloride [Bdmim][Cl)] as a template were successfully synthesized. The morphologies of the precursor aluminum acetate hydroxide (CH3COO)2A1(OH) crystal can be controlled by simply changing the amount of ionic liquid in the reaction system, the reactant concentrations and the reaction temperature. In particular, the ionic liquid [Bdmim][Cl] plays a key role on the morphology of the products as a soft template or a capping agent by the hydrogen bond-co-π-πstack mechanism. Secondly,γ-boehmite andγ-alumina nanostructures with the same morphologies were obtained by calcining at 300℃and 600℃, respectively. BET characterization of final productγ-alumina nanostructures display spesific area of 250-380m2/g and pore dimeter of 3.5nm, indicating their excellent surface property.
(2) Noble direct synthesis of hierarchical flowerlikeγ-AlOOH nanostructures by addition of Zn salt in the same reaction system via ionic liquid-assisted hydrothermal method. We have demonstrated that Zn salt added in the reaction system plays an important role on the formation of AlOOH as a coupling agent. The ionic liquid [Bdmim][Cl] plays a key role on the morphology of the products as a soft template or a capping agent by the hydrogen bond-co-π-πstack mechanism. According to ionic liquid amount increased, the flowers of the product were decreased in size and the leaves of the flower were increased in length-to-width ratio. The hierarchical flowerlike y-Al2O3 nanostructures obtained by calcining at 600℃for 2 h display excellent surface and mesoporous properties. BET characterization of final product flowerlikeγ-alumina nanostructures display spesific area of 150m2/g and pore dimeter of 3.6nm, indicating their excellent surface property.
(3) Ionic liquid-assisted hydrothermal synthesis of Dowsonite (denoted Na-Dw) nanorod and formation of nanotube by electron beam irradiation from Dowsonite-type nanorod precursor. Firstly, well-grown Na-Dw nano rod with length of about 200 nm and diameter of about 25nm was successfully synthesized by using NaHC03 and AICl3 as reactant, and ionic liquid [Bdmim][Cl] as a template, respectively. Secondly, uniform nanotubes whose surface consisted of AlOOH were obtained by high energy electron beam irradiation. The experimental results reveal that the decomposition of Na-Dw by electron beam irradiation is absolutely different with the thermal decomposition process. In general, Na-Dw is thermal-decomposed to form NaA102, however, in present case, Na-Dw is decomposed by high energy electron beam to form A100H surface membrane and NaCO3 internal wall. Moreover, inside formed gases, i.e, H2O and CO2 are difficult to leak out because of that membrane, leading to formation of more and more expanding nanorods. In the present reaction system, ionic liquid plays a key role on the formation of well-grown Na-Dw nanorod.
(4) Preparation of ZnAl2O4 spinel nanoplate by Zn2+ ion exchange from Na-Dw parent in the ionic liquid-assisted system at low temperature. Firstly, mediate compound nanoplate consisted of Al2O3·H2O and Zn6Al2(OH)16·CO3·4H2O was successfully synthesized by ion exchange in the ionic liquid system. In this stage, ionic liquid [Bdmim][Cl] plays a key role on the formation of nanoplate. Secondly, ZnAl2O4 spinel nanoplate was obtained by clcined the mediate mixture crystal at 700℃for 2 h. TEM images exhibites that ZnAl2O4 spinel nanoplate composed of fine particles with diameter of about 20 nm. The product exhibites the specific area of about 245 m2/g, indicating its excellent surface property.
(5) Ionic liquid-assisted hydrothermal synthsis of y-alumina nanostructures by using (NH4)2CO3 as a basic source. In the same reaction system, different products and different morphologies were obtained at different temperature. NH4Al(OH)2CO3 (NH4-DW) bamboo leavelike and fiberlike nanostructures were obtained at 75℃, they thereafter converted toγ-Al2O3 with the same morphologies by calcining 500℃for 2 h. However, bamboo leavelike and fiberlike y-AlOOH nanostructures were obtained at 120℃, hexagonalγ-AlOOH nanoplates was obtained at 150℃. In the every case, ionic liquid plays key role on the morphologies of the products.
In summary, we presented some facile and environmentally friendly methods for the controllable hydrothermal synthesis ofγ-Al2O3 and ZnAl2O4 spinel nanostructures by using ionic liquid as a template in this dissertation. It has been proved that the ionic liquid possessing the extraordinary potential is favorable for the fabrication of nanomaterials with novel morphologies and improved properties; moreover, these ionic liquids-assisted routes may offer a novel pathway towards the controllable synthesis of other inorganic nanomaterials.
离子液体是在室温下完全由离子组成的有机溶剂,由于其特殊的物理和化学性能在无机纳米材料合成方面引起人们广泛的关注。在离子液体辅助下,开发新的合成方法,同时对γ-氧化铝和尖晶石型偏铝酸锌ZnAl2O4纳米结构形貌进行控制合成是本论文的重点。具体的研究内容包括：
(1)碱式醋酸铝为前驱物离子液体辅助水热法合成Y-氢氧化氧铝和Y-氧化铝纳米结构研究。首先,以乙酸钾和氯化铝为反应物,以离子液体氯代1-丁基-2,3-二甲基咪唑([Bdmim][Cl)])为模板剂,通过水热法制备了不同形貌的碱式醋酸铝(CH3COO)2Al(OH)纳米晶,包括树叶状、纤维状、花状、多面体和纳米棒。在制备过程中,以离子液体为模板剂,通过调节离子液体浓度,反应物浓度和反应温度即可有效地对产物的形貌进行调控。研究发现,离子液体浓度对具有不同形貌的前驱物碱式醋酸铝纳米结构的形成起到了关键的作用。吸附在前驱物晶体表面的离子液体阳离子使纳米结构稳定,随着离子液体量增加可以制备一、二、三维纳米结构。通过前驱物在高温下煅烧,即可得到形貌保持不变的γ-氢氧化氧铝和γ-氧化铝纳米结构。表面性能研究表明所得γ-氧化铝纳米结构显示良好的表面和气孔性能,得到的γ-氧化铝纳米结构具有250-380m2/g的比表面积和大约3.5nm的孔径。
(2)以碱式醋酸铝为前驱物,通过前驱物分解与络合物生成反应的耦合反应,一步合成γ-氢氧化氧铝纳米结构的新途径研究。在一样的反应体系中,通过加一定量的Zn(NO3)2,即可直接得到花状γ-氢氧化氧铝钠米结构。添加的Zn2+离子为一种耦合反应驱动剂,对γ-氢氧化氧铝的形成起到关键的作用。另外,离子液体作为模板剂,对产物的形貌起到非常重要的作用,随着离子液体量增大,花状结构的尺寸变小,而构成花儿的纳米叶的长宽比变大了。最后得到的花状γ-氧化铝纳米结构具有150m2/g左右的比表面积和3.6nm的孔径。
(3)离子液体辅助水热法制备碱式碳酸铝钠NaAl(OH)2CO3 (Na-Dowsonite)纳米棒以及高能电子束辐射制备纳米管。首先以氯化铝和碳酸氢钠为反应物,以离子液体氯代1-丁基-2,3-二甲基咪唑([Bdmim][Cl)])为模板剂,在水热体系中制备出直径为25nm,长度为200nm的碱式碳酸铝钠纳米棒,产物不仅大小均匀而且分散性良好。然后以碱式碳酸铝钠为前驱物,通过高能电子束辐射制备出纳米管。在电子束分解过程当中,前驱物碱式碳酸铝钠的分解过程与普通热分解过程完全不一样。在热分解过程,分解产物为偏铝酸钠(NaA102),而电子束分解产物是表面为氢氧化氧铝(AlOOH)和内部为碳酸钠(Na2CO3)的两层结构。
(4)以碱式碳酸铝钠为前驱物在低温下Zn2+离子交换制备偏铝酸锌ZnAl2O4纳米结构的新途径。首先通过Zn2+离子交换反应得到中间体Al2O3·H20和Zn6Al2(OH)16·CO3·4H2O混合晶体的纳米片,然后在700℃煅烧2h所得偏铝酸锌(ZnAl2O4)纳米片。其纳米片由直径为约20nm的纳米颗粒组成,颗粒之间存在有气孔。这些气孔是在煅烧过程当中因中间体分解脱水而形成的。研究结果表明ZnAl2O4纳米片产物具有245m2/g的比较高的比表面积。离子液体在纳米片的生长过程中起到模板剂的作用。
(5)以碳酸铵为碱源离子液体辅助水热法γ-氧化铝纳米结构调控合成。在相同的反应体系当中,随着温度变化得到不同物相和形貌的产物。在75℃下得到竹叶状碱式碳酸铝铵纳米结构,而在120℃下得到γ-AlOOH纳米棒或者纳米线。当温度为150℃时,产物的形貌六角形纳米片。在不同合成条件下,离子液体对产物形貌的影响明显。
总之,本文主要研究了关于氧化铝和偏铝酸锌纳米材料的简便且环境友好的离子液体辅助水热合成法,证明了离子液体的使用使制备的材料具有新颖的形貌和优化的性能,并且可能为更多无机纳米材料的可控合成提供一个新的思路。
Most recently, metal oxides nanomaterials have become one of the most important research directions of chemistry, materials, and physics because of their excellent optical, electrical, thermal, and magnetic properties. Moreover, several researches indicated that the performance and application of the nanomaterials are decided by their phases, morphologies, sizes, and compositions. Thus, structure and shape controlled synthesis of nanoscale metal oxides will not only bring the theoretically progresses, but also extend the corresponding application field. Among them aluminum oxide, aluminum oxide hydroxide and zinc aluminate spinel compound are low cost materials widely used in industries, therefore have attracted interest. In this dissertation, a valuable research has been carried out to explore the new ionic liquid-assisted hydrothermal routes to y-aluminum oxide and ZnAl2O4 spinel nanostructures.
Ionic liquids (ILs), which are liquid salts at room temperature, have attracted tremendous attention due to their unique properties. As a burgeoning field, ILs has been employed as solvents, reactants, or templates for the preparation of inorganic nanomaterials. In this paper, ILs was used to prepared y-aluminum oxide and ZnAl2O4 spinel nanostructures. The purposes are to develop new synthetic methods of y-aluminum oxide and ZnAl2O4 spinel and explore the new functions of ILs. The main points can be summarized as follows:
(1) Morphology controllable synthesis of y-alumina nanostructures via two step ionic liquid-assisted hydrothermal route. Firstly, precursor aluminum acetate hydroxide (CH3COO)2A1(OH) crystals with different morphologies, including nanoleaves, nanofibers, flowerlike nanoarchtectures, polyhedrons, and nanorods, by using ionic liquid 1-buthyl-2,3-dimethyl imidazollium chloride [Bdmim][Cl)] as a template were successfully synthesized. The morphologies of the precursor aluminum acetate hydroxide (CH3COO)2A1(OH) crystal can be controlled by simply changing the amount of ionic liquid in the reaction system, the reactant concentrations and the reaction temperature. In particular, the ionic liquid [Bdmim][Cl] plays a key role on the morphology of the products as a soft template or a capping agent by the hydrogen bond-co-π-πstack mechanism. Secondly,γ-boehmite andγ-alumina nanostructures with the same morphologies were obtained by calcining at 300℃and 600℃, respectively. BET characterization of final productγ-alumina nanostructures display spesific area of 250-380m2/g and pore dimeter of 3.5nm, indicating their excellent surface property.
(2) Noble direct synthesis of hierarchical flowerlikeγ-AlOOH nanostructures by addition of Zn salt in the same reaction system via ionic liquid-assisted hydrothermal method. We have demonstrated that Zn salt added in the reaction system plays an important role on the formation of AlOOH as a coupling agent. The ionic liquid [Bdmim][Cl] plays a key role on the morphology of the products as a soft template or a capping agent by the hydrogen bond-co-π-πstack mechanism. According to ionic liquid amount increased, the flowers of the product were decreased in size and the leaves of the flower were increased in length-to-width ratio. The hierarchical flowerlike y-Al2O3 nanostructures obtained by calcining at 600℃for 2 h display excellent surface and mesoporous properties. BET characterization of final product flowerlikeγ-alumina nanostructures display spesific area of 150m2/g and pore dimeter of 3.6nm, indicating their excellent surface property.
(3) Ionic liquid-assisted hydrothermal synthesis of Dowsonite (denoted Na-Dw) nanorod and formation of nanotube by electron beam irradiation from Dowsonite-type nanorod precursor. Firstly, well-grown Na-Dw nano rod with length of about 200 nm and diameter of about 25nm was successfully synthesized by using NaHC03 and AICl3 as reactant, and ionic liquid [Bdmim][Cl] as a template, respectively. Secondly, uniform nanotubes whose surface consisted of AlOOH were obtained by high energy electron beam irradiation. The experimental results reveal that the decomposition of Na-Dw by electron beam irradiation is absolutely different with the thermal decomposition process. In general, Na-Dw is thermal-decomposed to form NaA102, however, in present case, Na-Dw is decomposed by high energy electron beam to form A100H surface membrane and NaCO3 internal wall. Moreover, inside formed gases, i.e, H2O and CO2 are difficult to leak out because of that membrane, leading to formation of more and more expanding nanorods. In the present reaction system, ionic liquid plays a key role on the formation of well-grown Na-Dw nanorod.
(4) Preparation of ZnAl2O4 spinel nanoplate by Zn2+ ion exchange from Na-Dw parent in the ionic liquid-assisted system at low temperature. Firstly, mediate compound nanoplate consisted of Al2O3·H2O and Zn6Al2(OH)16·CO3·4H2O was successfully synthesized by ion exchange in the ionic liquid system. In this stage, ionic liquid [Bdmim][Cl] plays a key role on the formation of nanoplate. Secondly, ZnAl2O4 spinel nanoplate was obtained by clcined the mediate mixture crystal at 700℃for 2 h. TEM images exhibites that ZnAl2O4 spinel nanoplate composed of fine particles with diameter of about 20 nm. The product exhibites the specific area of about 245 m2/g, indicating its excellent surface property.
(5) Ionic liquid-assisted hydrothermal synthsis of y-alumina nanostructures by using (NH4)2CO3 as a basic source. In the same reaction system, different products and different morphologies were obtained at different temperature. NH4Al(OH)2CO3 (NH4-DW) bamboo leavelike and fiberlike nanostructures were obtained at 75℃, they thereafter converted toγ-Al2O3 with the same morphologies by calcining 500℃for 2 h. However, bamboo leavelike and fiberlike y-AlOOH nanostructures were obtained at 120℃, hexagonalγ-AlOOH nanoplates was obtained at 150℃. In the every case, ionic liquid plays key role on the morphologies of the products.
In summary, we presented some facile and environmentally friendly methods for the controllable hydrothermal synthesis ofγ-Al2O3 and ZnAl2O4 spinel nanostructures by using ionic liquid as a template in this dissertation. It has been proved that the ionic liquid possessing the extraordinary potential is favorable for the fabrication of nanomaterials with novel morphologies and improved properties; moreover, these ionic liquids-assisted routes may offer a novel pathway towards the controllable synthesis of other inorganic nanomaterials.
引文
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