LED用碱金属碱土金属硼酸盐荧光粉的制备及其热力学性质研究

Because the preparation process of alkali and alkaline earth borate phosphor for LED was simple,the control lab preparation study on the product`composition and structure was few and there were no reports on their thermodynamic properties, this project intends to do the synthesis and thermodynamic studies of the rare earth (Eu3+) doped alkali and alkaline earth borate phosphor. There are two preparation steps, the hydrated rare earth (Eu3 +) doped alkali and alkaline earth borates (precursor) were prepared by wet chemical method firstly, then the final products were obtained by heat the precursors. The thermodynamic properties of precursors and final products were studied by calorimetric method. Combined their thermodynamic properties with their composition and structure, the influence of precursor' structure, composition and heat treatment conditions on the products' composition, structure were studied and obtained. In addition, the relationship between the precursors and final products' structure and their thermodynamic properties were obtained. On the basis of obtained influence rules and mechanisms, the preparation process and preparation condition of precursor and heat treated products were predicted by thermodynamic method, and the predicted results were validated by experiment. Finally, the thermodynamic prediction method for the preparation process of this kind phosphors were established. The research results will provide scientific guidance and reference for the controlled synthesis of rare earth (Eu3+) doped alkali and alkaline earth borate phosphors with specific composite and structure.

针对当前LED用碱金属碱土金属硼酸盐基质荧光粉的制备工艺单一、组成与结构可控研究少和热力学性质尚未开展研究的现状，本项目拟开展稀土（Eu3+）掺杂碱金属碱土金属硼酸盐荧光粉的制备和热力学性质研究。本项目采用湿化学法分两步进行产品制备研究，先制备水合稀土（Eu3+）掺杂碱金属碱土金属硼酸盐（前躯体），后将前躯体热处理的方法来制备目标产品。主要利用量热法对前躯体和不同热处理条件下产品的热力学性质进行研究，并结合它们的组成、结构，研究前躯体结构、组成和热处理条件对产品组成、结构的影响规律及机理，研究前躯体和热处理产品的组成、结构与其热力学性质的关系及规律，并在此基础上，对前躯体和热处理后产品的合成工艺、条件进行热力学预测和实验验证，最终建立利用湿化学法合成系列产品的合成工艺、条件的热力学预测方法，为特定组成、结构的稀土掺杂碱金属碱土金属硼酸盐荧光粉的可控合成提供科学指导。

针对当前LED用碱金属碱土金属硼酸盐基质荧光粉的制备工艺单一、组成与结构可控研究少和热力学性质尚未开展研究的现状，本项目主要开展5个方面的工作:1）稀土离子掺杂的水合碱金属碱土金属硼酸盐（前躯体）的制备及表征；2)前躯体的热处理及热处理后产品的表征；3)前躯体和热处理后产品的热力学性质研究；4)热处理过程产物结构变化规律、过程研究；5)对合成工艺、条件的热力学预测研究。.本项目取得的研究结果主要有：（1）首次利用湿化学法分两步（两步法）制备得到了5种稀土（Eu3+）掺杂水合碱金属、碱土金属硼酸盐（前驱体）、5种具有8不同形貌的稀土（Eu3+）掺杂水合碱土金属硼酸盐荧光粉（2）利用量热法对7种前躯体和6种热处理后产品的热力学数据（ΔfHmө）进行了测定，并对其热力学数据（ΔfGmө、Smө）进行了估算；（3）获得了9种水合Eu3+掺杂硼酸盐基质荧光粉的热分解（即第二步）物相(组成、结构）随温度变化过程；（4）从反应体系物质组成、结构和热力学性质两方面开展了产品制备工艺、条件预测研究，基本建立了预测方法;(5)项目资助发表SCI论文5篇、核心论文1篇。..整体研究结果为特定组成、结构的稀土掺杂碱金属、碱土金属硼酸盐荧光粉的可控（物相可控）合成提供科学依据与参考，达到了预定目标。