喷雾燃烧制备氧化铁基纳米复合材料及其性能
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摘要
纳米复合材料由于纳米尺度和不同功能的结合具有优异的性能,是新材料的研究热点之一。氧化铁基纳米复合材料在磁分离、催化剂、磁显影、新能源、太阳能光解水等领域有着重要的应用。因此,设计和制备新型多功能氧化铁基纳米复合材料具有重要的价值。火焰喷雾燃烧法基于传统气相燃烧制备纳米材料,具有气相燃烧连续化、无后处理、低成本、易规模化等优点。采用溶液注射,拓展了前驱体的范围,在制备多组分的纳米复合材料方面具有优势。本文基于气相火焰燃烧法,针对材料结构制备,设计燃烧反应器,开发了新型喷雾燃烧反应装置,优化燃烧工艺,制备了金属性Fe和Co3Fe7纳米颗粒、γ-Fe2O3‖SiO2双面杂化颗粒、Sn02纳米晶包覆γ-Fe2O3的核壳结构、以及相分离生长的α-Fe2O3/SnO2纳米异质结构等一系列氧化铁基纳米复合材料。同时,研究了喷雾燃烧中材料的形成,结构与性能之间的关系。主要研究工作如下：
1、针对火焰喷雾燃烧过程,通过控制燃料氧气比,选择高含量的前驱体,并通过淬火环引入N2保护,优化燃烧工艺,建立了金属性纳米材料的还原火焰燃烧制备新技术,制备了金属性Fe和C03Fe7合金纳米颗粒。其中,金属颗粒(Fe和Co3Fe7)粒径为20-80nm,被3-6nm的氧化物层(Fe304和CoFe2O4)所包覆,在空气气氛中具有良好的热稳定性。有较高的比饱和磁化强度,Co3Fe7合金颗粒的比饱和磁化强度高达126.1emu/g,比单一的Fe颗粒的比饱和磁化强度提高了68%。研究了燃料氧气比、组成、材料结构和磁性能的关系。分析了金属性纳米颗粒在火焰中的形成：前驱体火焰燃烧热解、还原性气氛下的成核生长和表面氧化。
2、结合Fe2O3和SiO2双组分高温相分离生长的特点,设计了共进前驱体喷雾燃烧工艺和后续连续化改性过程,优化前驱体组成,制备了具有不对称结构的γ-Fe2O3‖SiO2双面杂化颗粒,并实现了颗粒的原位表面改性。所制备的γ-Fe2O3‖SiO2双面杂化颗粒具有非对称的组成,在外磁场作用下,可以进行磁定向排列。研究了前驱体中Fe/Si比与材料结构的关系。通过火焰反应中原位取样分析表征,结合Fe2O3和SiO2的二元相图,分析了双面杂化结构在火焰中的形成机理。在此基础上,研究了火焰共进Ni、Mn、Co/Si前驱体得到的燃烧产物结构。经后续表面改性,硅烷偶联剂(KH570)分子选择性的接枝到双面结构中SiO2表面,赋予材料的双亲双疏特性。改性后的材料稳定于油/水两相溶剂的界面,亲水疏水分子作用使得材料取向排列,自组装形成油水界面膜和磁响应的微胶囊。采用改性后的材料可以组装成新型液体磁性微球,这些微球具有体积可控、良好的力学性能和外磁场驱动特性。
3、基于火焰温度梯度的变化,采用淬火环添加另一种前驱体原位包覆的方法,在反应器的后续位置引入锡源,利用SnO2在Fe2O3表面的异相成核生长,制备了SnO2纳米晶包覆γ-Fe2O3核壳纳米结构。核为30-120m的γ-Fe2O3组成,壳由8-10m的SnO2纳米晶所组成,且SnO2壳厚度在10-15nm。改变鼓泡瓶的水浴温度调整淬火环引入锡源前驱体的量,可以控制SnO2壳厚。研究发现水浴温度30℃制备的核壳结构有高的比表面积,有最高的气敏性能,对100ppm乙醇在300℃其灵敏度达22.8,是同条件下制备的Fe2O3的3.5和SnO2的1.9倍,且对乙醇有选择性。结合核壳结构及异质界面电子传递,分析了材料对乙醇分子的气敏机理。
4、根据相分离诱导外延生长的机理,选择设计前驱体组成,采用前驱体共进料喷雾燃烧工艺,制备了α-Fe2O3/SnO2异质结构的纳米复合材料。其中,α-Fe2O3/SnO2纳米异质结构表面粗糙,尺寸在30-200nm,且具有厚度不均的SnO2壳。研究了SnO2的引入对火焰燃烧形成的Fe203组成与结构的影响。研究表明Sn02能够有效地促进火焰反应中γ-Fe2O3向α-Fe2O3的转变。当SnO2掺杂量大于5at%时,γ相Fe2O3完全转变为α相。当前驱体中锡源量继续增加时,SnO2在Fe2o3中达到饱和,在Fe2oO的表面外延生长,形成类核壳异质结构。结合燃烧反应区温度梯度及复合材料的结构演变,分析了火焰中α-Fe2O3/SnO2纳米异质结构的相分离生长机理。用所制备的α-Fe2O3/SnO2异质结构作为负极材料组装成纽扣式锂离子电池,发现相对于单组分的Fe2O3和SnO2颗粒,两种活性氧化物的异质结构可以显著地提高锂电池容量存储性能。
Recently, advanced nanomaterials have attracted more attention owing to the unique physical and chemical properties. Especially, nanocomposites with versatile morphologies have an extensive application and are one of research hot topics of novel materials, which have different compositions, diverse function and unique interfacial interaction at nanoscale. Iron oxide based nanocomposites, as an important fuctional material, have a promising application such as magnetic recyclable catalysts, magnetic resonance imaging, lithium ion battery, solar light splitting water and so on. Therefore, it is still a challenge that how to design and synthesize multifunctional iron oxide based nanocomposites effectively. Flame spray pyrolysis technology has been demonstrated to be an effective, continuous, easily scalable approach for production of nanomaterials. Liquid-feeding route could offer more chocies for employing versatile precursor and make flame spray pyrolysis method possess more advantages in the construction of nanocomposites with multicomposition and diverse morphologies. In this thesis, combining flame reactor designing, optimum process control and the design of structured materials, Iron oxide based nanocomposites, such as oxides stabilized metallic Fe and Co3Fe7alloy core-shell nanoparticles, double faced γ-Fe2O3‖SiO2nanhybrids, γ-Fe2O3‖SiO2core-shell nanostructures and α-Fe2O3/SnO2nanoheterostructures, have been prepared by a facile flame spray pyrolysis approach. The flame process, materials structures and properties have been investigated in detail. The major contents have been summarized as follows.
1. Air stable, metallic Fe and Co3Fe7nanoparticles have been synthesized via one-step flame spray pyrolysis of an organicmetal precursor solution under stronger reducing atmosphere. The as-synthesized nanoparticles with diameters of20-80nm showed a typical core shell structure and high stability for one month in air, which metallic Fe or Co3Fe7cores were protected against oxidation by a surface shell of about3-6nm oxides (Fe3O4and CoFe2O4). The ratio of metallic Fe/Co alloy nanoparticles was7:3. The alloy nanoparticles exhibited enhanced saturation magnetization (126.1emu/g), compared with flame sprayed iron nanoparticles with the same conditions. By investigating the relationship between the ratio of fuel to oxygen, the morphology and composition of obtained materials and magnetic properties, reducing flame synthesis process is created for the synthesis of novel nanomaterials. Moreover, the formation mechanism of metal and alloy nanoparticles with core-shell structure was investigated in detail, which included three stages:flame combustion, reducing and surface oxidation during flame process. It is reckoned that such a continuous production approach an effective way to produce the stable advanced nanomaterials with a reduced valence state.
2. Double faced γ-Fe2O3‖SiO2nanohybrids (NHs) and their in-situ selective modification on silica faces with the3-Methacryloxypropyltrimethoxysilane molecules have been successfully prepared by a simple, rapid and scalable flame aerosol route. The double faced NHs perfectly integrates magnetic hematite hemispheres and non-magnetic silica parts into an almost intact nanoparticle as a result of phase segregation during the preparation process. The unique feature allows us to easily manipulate these particles into one-dimension chain-like nanostructures. By tailoring the mole ratio of Fe and Si in precursor, Janus nanoparticles with different volume of segregated SiO2hemisphere could be designed. The high temperature phase segregation mechanism based on thermal dynamic control is proposed to explain the formation of double faced γ-Fe2O3‖SiO2NHs in flame. Furthermore, the co-oxidation of different precursor (Ni, Mn, Co) and silica resource in flame eventually leads to the products with different composition and morphologies, indicating that the final morphology undergoing a high temperature aerosol process are independent of the bulk physiochemical features of the corresponding metal oxides. On the other hand, in situ selectively modificated double faced γ-Fe2O3‖SiO2NHs possess excellent interfacial activities, which can assemble into many interesting architectures, such as interfacial film, magnetic responsive capsules, novel magnetic liquid marbles and so forth. The modified NHs prefers to assemble at the interface of water/oil or oil/water systems. It is believed that the highly interfacial active NHs is not only beneficial for the development of interface reaction in a miniature reactor, but also very promising functional materials for other smart applications.
3. Core-shell γ-Fe2O3‖SiO2nanohybrids were fabricated via a simple flame-assisted spray pyrolysis (FASP). The shell layer composed of SnO2nanocrystals (8-10nm) was in-situ grown on the pristine Fe2O3nanoparticles with a tailored thickness ranging from6-20nm. The construction of such intriguing structure thus provided a rational and efficient combination of two kinds of gas sensitive materials, resulting in a remarkably enhanced sensing sensitivity (Ra/Rg) of22.8to100ppm ethanol vapor at300℃with high selectivity, compared to the pure Fe2O3and SnO2materials synthesized by FASP, respectively. The enhancement can be mainly attributed to the synergistic effects, i.e. the change of heterojunction barrier height at the interface between them. In addition, the in-situ flame coating process provides a promising and versatile choice for the synthesis of core-shell nanostructures with multifunctional composition.
4. Novel core-shell α-Fe2O3/SnO2heterostructures (HSs) are successfully prepared by a one-step flame-assisted spray copyrolysis of iron and tin precursor. The effect of SnO2component is investigated for the evolution of phase composition and morphology in detail. For the first time, it is noted that SnO2as a dopant can effectively promote the phase transition of γ-Fe2O3to α-Fe2O3during flame synthesis. A phase-segregation induced growth mechanism is proposed to explain the formation of unique core-shell structure. Such core-shell HSs as LIB anode materials exhibits an enhanced lithium storage capacity in comparison to pure Fe2O3and SnO2. This enhancement could be ascribed to the synergetic effect of both single components as well as the unique core-shell HSs.
1、针对火焰喷雾燃烧过程,通过控制燃料氧气比,选择高含量的前驱体,并通过淬火环引入N2保护,优化燃烧工艺,建立了金属性纳米材料的还原火焰燃烧制备新技术,制备了金属性Fe和C03Fe7合金纳米颗粒。其中,金属颗粒(Fe和Co3Fe7)粒径为20-80nm,被3-6nm的氧化物层(Fe304和CoFe2O4)所包覆,在空气气氛中具有良好的热稳定性。有较高的比饱和磁化强度,Co3Fe7合金颗粒的比饱和磁化强度高达126.1emu/g,比单一的Fe颗粒的比饱和磁化强度提高了68%。研究了燃料氧气比、组成、材料结构和磁性能的关系。分析了金属性纳米颗粒在火焰中的形成：前驱体火焰燃烧热解、还原性气氛下的成核生长和表面氧化。
2、结合Fe2O3和SiO2双组分高温相分离生长的特点,设计了共进前驱体喷雾燃烧工艺和后续连续化改性过程,优化前驱体组成,制备了具有不对称结构的γ-Fe2O3‖SiO2双面杂化颗粒,并实现了颗粒的原位表面改性。所制备的γ-Fe2O3‖SiO2双面杂化颗粒具有非对称的组成,在外磁场作用下,可以进行磁定向排列。研究了前驱体中Fe/Si比与材料结构的关系。通过火焰反应中原位取样分析表征,结合Fe2O3和SiO2的二元相图,分析了双面杂化结构在火焰中的形成机理。在此基础上,研究了火焰共进Ni、Mn、Co/Si前驱体得到的燃烧产物结构。经后续表面改性,硅烷偶联剂(KH570)分子选择性的接枝到双面结构中SiO2表面,赋予材料的双亲双疏特性。改性后的材料稳定于油/水两相溶剂的界面,亲水疏水分子作用使得材料取向排列,自组装形成油水界面膜和磁响应的微胶囊。采用改性后的材料可以组装成新型液体磁性微球,这些微球具有体积可控、良好的力学性能和外磁场驱动特性。
3、基于火焰温度梯度的变化,采用淬火环添加另一种前驱体原位包覆的方法,在反应器的后续位置引入锡源,利用SnO2在Fe2O3表面的异相成核生长,制备了SnO2纳米晶包覆γ-Fe2O3核壳纳米结构。核为30-120m的γ-Fe2O3组成,壳由8-10m的SnO2纳米晶所组成,且SnO2壳厚度在10-15nm。改变鼓泡瓶的水浴温度调整淬火环引入锡源前驱体的量,可以控制SnO2壳厚。研究发现水浴温度30℃制备的核壳结构有高的比表面积,有最高的气敏性能,对100ppm乙醇在300℃其灵敏度达22.8,是同条件下制备的Fe2O3的3.5和SnO2的1.9倍,且对乙醇有选择性。结合核壳结构及异质界面电子传递,分析了材料对乙醇分子的气敏机理。
4、根据相分离诱导外延生长的机理,选择设计前驱体组成,采用前驱体共进料喷雾燃烧工艺,制备了α-Fe2O3/SnO2异质结构的纳米复合材料。其中,α-Fe2O3/SnO2纳米异质结构表面粗糙,尺寸在30-200nm,且具有厚度不均的SnO2壳。研究了SnO2的引入对火焰燃烧形成的Fe203组成与结构的影响。研究表明Sn02能够有效地促进火焰反应中γ-Fe2O3向α-Fe2O3的转变。当SnO2掺杂量大于5at%时,γ相Fe2O3完全转变为α相。当前驱体中锡源量继续增加时,SnO2在Fe2o3中达到饱和,在Fe2oO的表面外延生长,形成类核壳异质结构。结合燃烧反应区温度梯度及复合材料的结构演变,分析了火焰中α-Fe2O3/SnO2纳米异质结构的相分离生长机理。用所制备的α-Fe2O3/SnO2异质结构作为负极材料组装成纽扣式锂离子电池,发现相对于单组分的Fe2O3和SnO2颗粒,两种活性氧化物的异质结构可以显著地提高锂电池容量存储性能。
Recently, advanced nanomaterials have attracted more attention owing to the unique physical and chemical properties. Especially, nanocomposites with versatile morphologies have an extensive application and are one of research hot topics of novel materials, which have different compositions, diverse function and unique interfacial interaction at nanoscale. Iron oxide based nanocomposites, as an important fuctional material, have a promising application such as magnetic recyclable catalysts, magnetic resonance imaging, lithium ion battery, solar light splitting water and so on. Therefore, it is still a challenge that how to design and synthesize multifunctional iron oxide based nanocomposites effectively. Flame spray pyrolysis technology has been demonstrated to be an effective, continuous, easily scalable approach for production of nanomaterials. Liquid-feeding route could offer more chocies for employing versatile precursor and make flame spray pyrolysis method possess more advantages in the construction of nanocomposites with multicomposition and diverse morphologies. In this thesis, combining flame reactor designing, optimum process control and the design of structured materials, Iron oxide based nanocomposites, such as oxides stabilized metallic Fe and Co3Fe7alloy core-shell nanoparticles, double faced γ-Fe2O3‖SiO2nanhybrids, γ-Fe2O3‖SiO2core-shell nanostructures and α-Fe2O3/SnO2nanoheterostructures, have been prepared by a facile flame spray pyrolysis approach. The flame process, materials structures and properties have been investigated in detail. The major contents have been summarized as follows.
1. Air stable, metallic Fe and Co3Fe7nanoparticles have been synthesized via one-step flame spray pyrolysis of an organicmetal precursor solution under stronger reducing atmosphere. The as-synthesized nanoparticles with diameters of20-80nm showed a typical core shell structure and high stability for one month in air, which metallic Fe or Co3Fe7cores were protected against oxidation by a surface shell of about3-6nm oxides (Fe3O4and CoFe2O4). The ratio of metallic Fe/Co alloy nanoparticles was7:3. The alloy nanoparticles exhibited enhanced saturation magnetization (126.1emu/g), compared with flame sprayed iron nanoparticles with the same conditions. By investigating the relationship between the ratio of fuel to oxygen, the morphology and composition of obtained materials and magnetic properties, reducing flame synthesis process is created for the synthesis of novel nanomaterials. Moreover, the formation mechanism of metal and alloy nanoparticles with core-shell structure was investigated in detail, which included three stages:flame combustion, reducing and surface oxidation during flame process. It is reckoned that such a continuous production approach an effective way to produce the stable advanced nanomaterials with a reduced valence state.
2. Double faced γ-Fe2O3‖SiO2nanohybrids (NHs) and their in-situ selective modification on silica faces with the3-Methacryloxypropyltrimethoxysilane molecules have been successfully prepared by a simple, rapid and scalable flame aerosol route. The double faced NHs perfectly integrates magnetic hematite hemispheres and non-magnetic silica parts into an almost intact nanoparticle as a result of phase segregation during the preparation process. The unique feature allows us to easily manipulate these particles into one-dimension chain-like nanostructures. By tailoring the mole ratio of Fe and Si in precursor, Janus nanoparticles with different volume of segregated SiO2hemisphere could be designed. The high temperature phase segregation mechanism based on thermal dynamic control is proposed to explain the formation of double faced γ-Fe2O3‖SiO2NHs in flame. Furthermore, the co-oxidation of different precursor (Ni, Mn, Co) and silica resource in flame eventually leads to the products with different composition and morphologies, indicating that the final morphology undergoing a high temperature aerosol process are independent of the bulk physiochemical features of the corresponding metal oxides. On the other hand, in situ selectively modificated double faced γ-Fe2O3‖SiO2NHs possess excellent interfacial activities, which can assemble into many interesting architectures, such as interfacial film, magnetic responsive capsules, novel magnetic liquid marbles and so forth. The modified NHs prefers to assemble at the interface of water/oil or oil/water systems. It is believed that the highly interfacial active NHs is not only beneficial for the development of interface reaction in a miniature reactor, but also very promising functional materials for other smart applications.
3. Core-shell γ-Fe2O3‖SiO2nanohybrids were fabricated via a simple flame-assisted spray pyrolysis (FASP). The shell layer composed of SnO2nanocrystals (8-10nm) was in-situ grown on the pristine Fe2O3nanoparticles with a tailored thickness ranging from6-20nm. The construction of such intriguing structure thus provided a rational and efficient combination of two kinds of gas sensitive materials, resulting in a remarkably enhanced sensing sensitivity (Ra/Rg) of22.8to100ppm ethanol vapor at300℃with high selectivity, compared to the pure Fe2O3and SnO2materials synthesized by FASP, respectively. The enhancement can be mainly attributed to the synergistic effects, i.e. the change of heterojunction barrier height at the interface between them. In addition, the in-situ flame coating process provides a promising and versatile choice for the synthesis of core-shell nanostructures with multifunctional composition.
4. Novel core-shell α-Fe2O3/SnO2heterostructures (HSs) are successfully prepared by a one-step flame-assisted spray copyrolysis of iron and tin precursor. The effect of SnO2component is investigated for the evolution of phase composition and morphology in detail. For the first time, it is noted that SnO2as a dopant can effectively promote the phase transition of γ-Fe2O3to α-Fe2O3during flame synthesis. A phase-segregation induced growth mechanism is proposed to explain the formation of unique core-shell structure. Such core-shell HSs as LIB anode materials exhibits an enhanced lithium storage capacity in comparison to pure Fe2O3and SnO2. This enhancement could be ascribed to the synergetic effect of both single components as well as the unique core-shell HSs.
引文
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