熔盐法制备一维莫来石陶瓷材料的研究
发布时间:2018-05-06 09:09
本文选题:一维陶瓷材料 + 熔盐法 ; 参考:《天津大学》2010年博士论文
【摘要】:在一定条件下,晶体沿着线性链方向生长的陶瓷材料被称为一维陶瓷材料。一维材料在其他维度方向上生长受限,因此表现出不同于传统材料的特殊性能。其中一维莫来石陶瓷由于其优异的热震性、抗蠕变性,以及高温下室温强度衰减小的特性,已经应用于晶须补强、涂层技术、过滤膜、高温催化反应器等方面。熔盐法是一种湿法化学合成方法,其优势在于合成的粉体无团聚、工艺简单;与其他液相法相比,其合成出的一维晶体质量更高。本文中,对采用熔盐法合成一维莫来石陶瓷进行了研究。 对前驱体的研究表明,采用化学活性高、溶解能力强的前驱体,有助于获得独立分散的一维莫来石晶体。以Al_2(SO_4)_3、无定形SiO_2、Na_2SO_4为原料,其配比Al/Si/Na为2/1/8(原子比)时,在1000℃保温3h条件下,HF酸洗后最终产物全部为一维莫来石晶体。XRD、EDS、HR-TEM结果表明所得的莫来石晶体为富Al组成,光致发光性能反映出富Al组成产生的氧空位缺陷。对温度制度的研究表明,快速升温有助于莫来石相的生成;合成温度过高,莫来石晶体会在1100℃左右发生分解形成NaAlSiO_4。 对莫来石晶体生长机理的研究表明。熔盐法合成过程中,当液相中不断生成的莫来石超过其过饱和度时,莫来石开始成核。在液固生长界面处,莫来石单体的沉淀是可逆的,因此生长能够按照其能量最低的原则不断进行调整,从而最大限度的保证其在c轴方向的自由生长。莫来石晶体在界面处的生长位置是由二维平台提供的,这个过程所需克服的能量壁垒大,当二维平台耗尽时,晶体即停止生长。莫来石晶体在熔盐法中的生长属于LS生长机理。 通过对B_2O_3外加剂的研究,发现莫来石晶体尺寸的减小,当B_2O_3/SiO_2达到0.04(摩尔比)时形成了纳米级别莫来石晶体,其归因于B_2O_3的加入有助于成核速率加快。通过对莫来石晶种的研究,发现晶种的加入能够在一定程度上提高熔盐法制备莫来石晶体的产率,莫来石晶体的尺寸减小、尺寸更加均匀,这是由于晶种的加入能够为莫来石晶体提供生长位点,提高了莫来石晶体初期形核速率。
[Abstract]:Under certain conditions, ceramic materials grown along linear chains are called one-dimensional ceramic materials. One-dimensional materials exhibit special properties different from traditional materials due to their limited growth in other dimensions. One-dimensional mullite ceramics have been used in whisker reinforcement coating technology filtration membrane and high temperature catalytic reactor due to their excellent thermal shock resistance creep resistance and low strength attenuation at room temperature. Molten salt method is a wet chemical synthesis method, its advantage is that the synthesized powder has no agglomeration and the process is simple. Compared with other liquid phase method, the synthesized one-dimensional crystal has higher quality. In this paper, the synthesis of one-dimensional mullite ceramics by molten salt method was studied. The study of the precursor shows that the use of the precursor with high chemical activity and strong solubility is helpful to obtain the independent dispersed one-dimensional mullite crystal. When the Al/Si/Na ratio is 2 / 1 / 8 (atomic ratio), the final product after acid washing at 1000 鈩,
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