模板介入法制备纳米氧化铝及其应用研究
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摘要
纳米Al2O3由于具有良好的耐磨性、抗腐蚀性、光学稳定性、电学性、催化性以及良好的生物相容性,在耐磨、绝缘、阻燃、催化、微电子元件等领域具有特殊的用途,成为一种应用最广、需求最迫切的纳米材料。目前制备性能优越的纳米γ-Al2O3粉体已经有比较成熟的工艺,但要想制备小粒径、窄分布的纳米α-Al2O3却比较困难,其原因在于γ-Al2O3必需在高温下才能转变为α相,在转相过程中颗粒极易发生硬团聚,因此很难得到分布窄的纳米α-Al2O3粉体,而纳米粒子的均一性正是良好应用性能的关键。如何制备小粒径、窄分布、分散性好、无团聚的纳米α-Al2O3一直是世界范围内科研工作者努力的目标。
本论文首先在传统结晶理论的基础上探讨了纳米晶核生长的特殊性。与常规定向有序结晶相比,纳米氧化铝前驱体的成核阶段,由于凝结速度远大于定向速度,因而分子或离子以无序或近无序的方式堆积;胶核生长阶段,一方面存在着扩散控制的生长模式, 另一方面无规则的布朗运动使两个或多个胶核碰撞产生堆垛式无序凝并,无序乱堆使部分晶核发生紧密接触,晶界曲率半径引起的化学位梯度使晶界两侧原子发生迁移, 在晶界面及周围其它原子或分子的扰动下发生结构层堆垛次序的错排,即形成堆垛层错,由此造成晶体表面原子呈一维无序及亚晶界结构。纳米粒子的壳层结构、原子排列的无序性以及材料表面固有的堆积产生的间隙微孔为这一生长模式提供了有利的佐证。
通过对已有的团聚机理的分析,系统深入地探讨了影响团聚的主要因素。研究结果表明:颗粒团聚的主要驱动力是晶粒长大前后的界面能差,而氢键、范德华力和毛细管效应则是促进粉体团聚的外界因素,团聚是内因和外因共同作用的结果,颗粒间的接触是作用的前提。因此,理想的阻隔是控制粉体团聚、获得窄分布颗粒的有效手段,微元环境的一致性是实现晶体均匀生长、粉体粒度窄分布的根本保证。
在上述理论研究的基础上,首次设计了以固态介质炭黑为模板的微元反应器, 通过模板介质、溶剂及分散方式的选择,使该反应场具有全程性的功能:在前驱体制备中模板介质控制粒子成核和长大;在后处理高温转相过程中起阻隔作用,抑制颗粒的生长。并探讨了微元反应器的作用机理,主要探讨了超声波的空化作用和模板介质的
全程阻隔作用。超声波的空化作用在前驱体制备中具有加速成核和控制晶核生长的作用,保证晶核生长的同步性,并使得生成的晶体彼此分散,避免硬团聚的发生;模板介质由于自身的结构优势在微元反应场中发挥全程阻隔作用,它是粉体均匀一致性的保证,另外模板介质的表面特性又促使超声波的空化作用得到增强,模板介质的可去除性保证了最终产品的纯度。
利用设计的微元反应场,在一定的工艺条件下合成出了尺寸可控、粒度分布均匀、晶相完整的纳米α-氧化铝粉体,并对前驱体的制备工艺和后处理工艺进行了优化,优化后的工艺参数为:超声波频率30KHz,超声波功率160W,模板介质用量20g/L, Al(NO3)3溶液浓度0.5mol.L-1,滴加速度20ml/min,溶剂为含醇60%的水,在氮气中转相,转相温度1100℃,转相时间2h,在600℃空气中煅烧1h。并采用透射电镜、红外光谱、激光粒度分析仪、X衍射仪、DSC差热分析仪等手段对合成纳米粉体性能进行了表征,结果表明:采用模板介入法可以合成出粒径小(40~50nm)、分布窄(±1.2nm)、晶相纯的纳米α-氧化铝粉体,而且工艺简单、反应条件温和、原材料价廉易得,适宜工业化生产。
论文最后对所合成的纳米氧化铝粉体的应用性能进行了初步研究,首次将纳米技术同炸药钝感技术相结合,通过安全性实验,研究了纳米氧化铝对炸药性能的影响,结果表明:纳米氧化铝较常规氧化铝能降低混合炸药的撞击感度和冲击波感度,而且对HMX热分解具有一定催化特性,使混合炸药的热分解的自加速温度有所降低,并能略微提高混合炸药的能量输出和爆速。
本课题的创新点主要表现在如下几方面:
1. 在传统结晶理论的基础上系统研究了前驱体制备过程中成核和生长机制,建立了纳米晶体生长模型,为获得窄分布纳米粉体提供了理论基础。
2. 在理论研究的基础上首次设计了以超声波、模板介质、溶剂为主体的微元反应场,并通过各项参数的优化使得该微元反应场能充分发挥全程化功能:在前驱体制备中控制粒子成核和长大;在后处理中起阻隔作用,防止颗粒的不正常生长,解决了α-氧化铝的团聚问题,保证了最终粒子的均匀一致性,并探讨了微元反应场的作用机理。
3. 首次将纳米技术同炸药钝感技术相结合,通过实验研究了纳米氧化铝对炸药撞击感度、冲击波感度以及能量输出等性能的影响。
Nano-sized alpha alumina power, which has a very high surface or interfacial area, exhibits dramatic properties, such as enhanced sinterability at low temperatures, improved UV scattering, very high hardness, smaller particle suspensions, superior optoelectronic properties, has become a kind of favorable material in applications such as high insulation material, high performance cutting tools, micro-electronics and fine porcelain.
There are a number of techniques presently available for the synthesis of nano-sized gamma alumina power, while it is relatively difficult to make perfect nano-sized alpha alumina particle with fine size, narrow distribution and high purity. The main fact is because of that the transformation process of crystal phase from gamma to alpha must be performed under high temperature above 1200-Celsius degree, at which it is very easy for nano-sized particle to agglomerate and grow. Maintaining a narrow size distribution without obvious agglomeration in the power, which is important in many applications, is not possible with a majority of conventional techniques and has become a world aim that many scientists are going in for.
In this paper, the particularity of nano-crystal growing was discussed firstly on the base of traditional crystal theory. Comparing with general directional and regular crystallization, during the nucleating of nano-alumina precursor, molecule or ion takes on out-of-order stacking structure because of the higher concreting rate; during the growing of crystal nucleus, out-of-order stacking makes most of crystal nucleus contact closely and stacking fault is formed as a result of Brown movement and chemistry potential difference among crystal interfaces, which makes atoms in crystal take on out-of-order or sub-boundary structure. This kind of special crystal growing model can also be proved by shell structure, out-of-order property of atom array and porous surface structure of nano-particles.
Through analyzing existent agglomeration mechanisms, the main effect factors on agglomeration of nano-particles were discussed systematically and thoroughly. The results
show that the interface energy difference is the main driving force and hydrogen bond, chemical bond and capillary action force can improve the grow of the particles. The common action of intrinsic factor and exterior factor results in agglomeration. What’s more, contact among particles is the precondition of above various actions. Therefore, preventing direct contact among particles is the effective way to restrain agglomeration and grow of particles and the uniformity of microenvironment is also very important for attaining nano-sized power with narrow distribution.
On base of above theory studies, the micro-reaction unit, including mainly template medium, solvent and ultrasonic, was built in order to attain uniform nano-sized powder through combining soft-chemistry and template-chemistry technique. The micro-reaction unit has the following double functions: the one is controlling the nucleation and grow of particles during preparing process of the precursor; the other is preventing agglomeration and abnormal grow of particles during the subsequent heat-treating process acting as a kind of obstruct. Furthermore, the action mechanism of micro-reaction unit was also studied, especially on the cavitations action of ultrasonic and obstruct action of template medium .the former can accelerate nucleating and control growing of nucleus, which assures the uniformity of grow and prevent the form of hard agglomerates during preparing process of the precursor; the later exerts entire obstruct action during the whole reaction process in the advantage of its special structure, which assures the uniformity of the last nano-sized powder. What’s more, the surface characteristic of template medium also enhances the cavitations action of ultrasonic and the eliminable property of template medium also ensures the purity of final product.
Thereafter, the nano-sized alpha alumina powder with controllable size, narrow distrib
本论文首先在传统结晶理论的基础上探讨了纳米晶核生长的特殊性。与常规定向有序结晶相比,纳米氧化铝前驱体的成核阶段,由于凝结速度远大于定向速度,因而分子或离子以无序或近无序的方式堆积;胶核生长阶段,一方面存在着扩散控制的生长模式, 另一方面无规则的布朗运动使两个或多个胶核碰撞产生堆垛式无序凝并,无序乱堆使部分晶核发生紧密接触,晶界曲率半径引起的化学位梯度使晶界两侧原子发生迁移, 在晶界面及周围其它原子或分子的扰动下发生结构层堆垛次序的错排,即形成堆垛层错,由此造成晶体表面原子呈一维无序及亚晶界结构。纳米粒子的壳层结构、原子排列的无序性以及材料表面固有的堆积产生的间隙微孔为这一生长模式提供了有利的佐证。
通过对已有的团聚机理的分析,系统深入地探讨了影响团聚的主要因素。研究结果表明:颗粒团聚的主要驱动力是晶粒长大前后的界面能差,而氢键、范德华力和毛细管效应则是促进粉体团聚的外界因素,团聚是内因和外因共同作用的结果,颗粒间的接触是作用的前提。因此,理想的阻隔是控制粉体团聚、获得窄分布颗粒的有效手段,微元环境的一致性是实现晶体均匀生长、粉体粒度窄分布的根本保证。
在上述理论研究的基础上,首次设计了以固态介质炭黑为模板的微元反应器, 通过模板介质、溶剂及分散方式的选择,使该反应场具有全程性的功能:在前驱体制备中模板介质控制粒子成核和长大;在后处理高温转相过程中起阻隔作用,抑制颗粒的生长。并探讨了微元反应器的作用机理,主要探讨了超声波的空化作用和模板介质的
全程阻隔作用。超声波的空化作用在前驱体制备中具有加速成核和控制晶核生长的作用,保证晶核生长的同步性,并使得生成的晶体彼此分散,避免硬团聚的发生;模板介质由于自身的结构优势在微元反应场中发挥全程阻隔作用,它是粉体均匀一致性的保证,另外模板介质的表面特性又促使超声波的空化作用得到增强,模板介质的可去除性保证了最终产品的纯度。
利用设计的微元反应场,在一定的工艺条件下合成出了尺寸可控、粒度分布均匀、晶相完整的纳米α-氧化铝粉体,并对前驱体的制备工艺和后处理工艺进行了优化,优化后的工艺参数为:超声波频率30KHz,超声波功率160W,模板介质用量20g/L, Al(NO3)3溶液浓度0.5mol.L-1,滴加速度20ml/min,溶剂为含醇60%的水,在氮气中转相,转相温度1100℃,转相时间2h,在600℃空气中煅烧1h。并采用透射电镜、红外光谱、激光粒度分析仪、X衍射仪、DSC差热分析仪等手段对合成纳米粉体性能进行了表征,结果表明:采用模板介入法可以合成出粒径小(40~50nm)、分布窄(±1.2nm)、晶相纯的纳米α-氧化铝粉体,而且工艺简单、反应条件温和、原材料价廉易得,适宜工业化生产。
论文最后对所合成的纳米氧化铝粉体的应用性能进行了初步研究,首次将纳米技术同炸药钝感技术相结合,通过安全性实验,研究了纳米氧化铝对炸药性能的影响,结果表明:纳米氧化铝较常规氧化铝能降低混合炸药的撞击感度和冲击波感度,而且对HMX热分解具有一定催化特性,使混合炸药的热分解的自加速温度有所降低,并能略微提高混合炸药的能量输出和爆速。
本课题的创新点主要表现在如下几方面:
1. 在传统结晶理论的基础上系统研究了前驱体制备过程中成核和生长机制,建立了纳米晶体生长模型,为获得窄分布纳米粉体提供了理论基础。
2. 在理论研究的基础上首次设计了以超声波、模板介质、溶剂为主体的微元反应场,并通过各项参数的优化使得该微元反应场能充分发挥全程化功能:在前驱体制备中控制粒子成核和长大;在后处理中起阻隔作用,防止颗粒的不正常生长,解决了α-氧化铝的团聚问题,保证了最终粒子的均匀一致性,并探讨了微元反应场的作用机理。
3. 首次将纳米技术同炸药钝感技术相结合,通过实验研究了纳米氧化铝对炸药撞击感度、冲击波感度以及能量输出等性能的影响。
Nano-sized alpha alumina power, which has a very high surface or interfacial area, exhibits dramatic properties, such as enhanced sinterability at low temperatures, improved UV scattering, very high hardness, smaller particle suspensions, superior optoelectronic properties, has become a kind of favorable material in applications such as high insulation material, high performance cutting tools, micro-electronics and fine porcelain.
There are a number of techniques presently available for the synthesis of nano-sized gamma alumina power, while it is relatively difficult to make perfect nano-sized alpha alumina particle with fine size, narrow distribution and high purity. The main fact is because of that the transformation process of crystal phase from gamma to alpha must be performed under high temperature above 1200-Celsius degree, at which it is very easy for nano-sized particle to agglomerate and grow. Maintaining a narrow size distribution without obvious agglomeration in the power, which is important in many applications, is not possible with a majority of conventional techniques and has become a world aim that many scientists are going in for.
In this paper, the particularity of nano-crystal growing was discussed firstly on the base of traditional crystal theory. Comparing with general directional and regular crystallization, during the nucleating of nano-alumina precursor, molecule or ion takes on out-of-order stacking structure because of the higher concreting rate; during the growing of crystal nucleus, out-of-order stacking makes most of crystal nucleus contact closely and stacking fault is formed as a result of Brown movement and chemistry potential difference among crystal interfaces, which makes atoms in crystal take on out-of-order or sub-boundary structure. This kind of special crystal growing model can also be proved by shell structure, out-of-order property of atom array and porous surface structure of nano-particles.
Through analyzing existent agglomeration mechanisms, the main effect factors on agglomeration of nano-particles were discussed systematically and thoroughly. The results
show that the interface energy difference is the main driving force and hydrogen bond, chemical bond and capillary action force can improve the grow of the particles. The common action of intrinsic factor and exterior factor results in agglomeration. What’s more, contact among particles is the precondition of above various actions. Therefore, preventing direct contact among particles is the effective way to restrain agglomeration and grow of particles and the uniformity of microenvironment is also very important for attaining nano-sized power with narrow distribution.
On base of above theory studies, the micro-reaction unit, including mainly template medium, solvent and ultrasonic, was built in order to attain uniform nano-sized powder through combining soft-chemistry and template-chemistry technique. The micro-reaction unit has the following double functions: the one is controlling the nucleation and grow of particles during preparing process of the precursor; the other is preventing agglomeration and abnormal grow of particles during the subsequent heat-treating process acting as a kind of obstruct. Furthermore, the action mechanism of micro-reaction unit was also studied, especially on the cavitations action of ultrasonic and obstruct action of template medium .the former can accelerate nucleating and control growing of nucleus, which assures the uniformity of grow and prevent the form of hard agglomerates during preparing process of the precursor; the later exerts entire obstruct action during the whole reaction process in the advantage of its special structure, which assures the uniformity of the last nano-sized powder. What’s more, the surface characteristic of template medium also enhances the cavitations action of ultrasonic and the eliminable property of template medium also ensures the purity of final product.
Thereafter, the nano-sized alpha alumina powder with controllable size, narrow distrib
引文
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