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无机晶体结晶过程研究

The Study on Crystallization Process of Inorganic Crystals

【作者】 赵旭

【导师】 薛冬峰;

【作者基本信息】 大连理工大学 , 功能材料化学与化工, 2009, 硕士

【摘要】 结晶过程是化工过程中的一个重要操作单元,也是完成化工产品生产的重要环节。对结晶过程进行有效地控制,是制备高纯度、高品质功能晶体材料的关键,制约材料科学的发展与工业化应用。为了探索影响结晶生长过程的因素,挖掘晶体生长的本质,实现无机晶体材料的可控合成,本论文对氧化亚铜和磷酸二氢钾晶体的结晶行为进行了系统研究。基于单晶生长的化学键合理论,设计了合理的结晶生长路线,系统地考察了各种因素对最终产物结晶形貌的影响。以氧化-还原法为合成策略,设计了乙二胺四乙酸钠辅助的水热结晶工艺,获得了多形貌的氧化亚铜微晶。在独立实验中,用扫描电子显微镜和X射线衍射对氧化亚铜不同生长环境下的形貌和性能进行了分析表征。同时论文对制备过程中影响最终产物形貌的外在因素进行了考察。并从化学键合的角度合理地阐述了多面体形貌和枝化形貌形成的原因。对氧化亚铜结晶过程的理论研究和实际的工业化生产起到了积极的指导作用。磷酸二氢钾具有优良的铁电、压电性能,在光学器件中具有极其广泛的应用。通过研究磷酸二氢钾的结晶学特征,运用化学键合理论模拟了磷酸二氢钾的理想形貌。并通过设计不同过饱和度下的结晶实验,利用扫描电子显微镜和X射线衍射对产物进行了表征,获得了磷酸二氢钾随过饱和度改变的形貌演变趋势。指出过饱和度的改变导致晶面生长机制的变化,引起磷酸二氢钾柱面和锥面相对生长速率的改变。同时,该实验对磷酸二氢钾的工业结晶具有指导作用。论文探索了控制结晶过程的新方法,考察了结晶过程中的各种因素对无机晶体结晶习性的影响,并结合理论对结晶生长机制进行了合理的解释。当前的工作对指导无机晶体的可控合成具有借鉴意义。

【Abstract】 Crystallization process is one of the most important operation units in chemical engineering process,as well as an essential component in the manufacture of chemical products.Effective control on crystallization process is critical to the fabrication of functional crystal materials with high purity and high quality,which influences the development of materials science and industrial application.In order to investigate the factors during crystal growth process,dig the nature of crystal growth and realize the controlled fabrication of inorganic crystal materials,the crystallization behaviors of cuprous oxide(Cu2O) and potassium dihydrogen phosphate(KDP) crystals have been systematically studied in this thesis.Based on the chemical bonding theory of single crystal growth,the crystal growth routes have been reasonably designed to investigate the influences of various factors on the crystallization morphologies of final products.Starting from the self-oxidation-reduction synthesis strategy,the EDTANaa-assisted hydrothermal crystallization technique has been designed to obtain polymorphological Cu2O microcrystals.The morphology and structure information of the as-grown crystals have been characterized by scanning electron mi roscope(SEM) and X-ray powder diffraction(XRD). From the chemical bonding viewpoint,the growth mechanisms of polyhedral morphology and branch growth behavior have been reasonably interpreted,which can further guide the theoretical research and industrial preparation of Cu2O crystals.For the unique ferro-and piezo-electric properties,KDP crystals are highly desirable in optical devices.From the study of crystallization character of KDP,the ideal morphology has been simulated by using chemical bonding theory.The final products obtained from different supersaturation have been characterized by SEM and XRD.The variation in solution supersaturation can effectively change the growth mechanisms of different crystal faces.In the thesis,new methods for controlling crystallization process have been designed; several factors that influence the growth habit of inorganic crystals have been investigated; the growth mechanisms have been reasonably interpreted according to the crystal growth theory.The current work can guide the shape-controlled synthesis of inorganic crystals.

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