导　　师： 杨秋华

学科专业： G0301

授予学位： 硕士

作　　者： ;

机构地区： 天津大学

摘　　要： 本文分别采用回流法和溶剂热法合成了复合氟化物KAlF/_4，NH/_4AlF/_4，Li/_3AlF/_6和Na/_3AlF/_6，考查了反应物的选择、配比、反应时间、反应温度、反应液的填充度等因素对产物的影响，并利用XRD，TEM，XPS等技术对其结构、形貌、粒径大小以及表面氧含量进行了表征，结果表明回流法和溶剂热法在适当的反应条件下均能合成单一相结构的复合氟化物，且粒径均小于100 nm，属于纳米颗粒，所合成的产物不含晶格氧，且吸附氧含量较低，该方法具有工艺简单、反应时间短、不腐蚀设备、不需要煅烧直接生产晶相等优点，具有广阔的开发应用前景。 此外，本文利用乙二醇回流法合成了NH/_4MgAlF/_6，LiSrAlF/_6，KFeF/_3及几种掺杂Ce~/(3+/)的复合氟化物KAlF/_4：Ce~/(3+/)，NH/_4MgAlF/_6：Ce~/(3+/)，KFeF/_3：Ce~/(3+/)。经XRD检测表明掺杂少量的Ce~/(3+/)离子并没有使晶体结构发生明显的变化，XRD的测试数据与标准卡片的数据基本吻合，没有杂质峰出现，产物仍具有单一晶相。通过对KAlF/_4：Ce~/(3+/)和NH/_4MgAlF/_6：Ce~/(3+/_的荧光光谱分析发现：KAlF/_4：Ce~/(3+/)的发射光谱中最大发射峰位于326 nm处，发射带属于Ce~/(3+/)的5d→4f跃迁。NH/_4MgAlF/_6：Ce~/(3+/)的发射光谱中，发射峰从300 nm延展到400 nm，最大发射峰位于335 nm，发射半宽峰约为60 nm，其特点是吸收和发射都是宽带，这表明KAlF/_4和NH/_4MgAlF/_6可作为优质的荧光基质材料。 Nano complex fluorides KAlF/_4, NH/_4AlF/_4, Li/_3AlF/_6, Na/_3AlF/_6 were synthesized byreflux method and solvent-thermal method。The influence of different synthesisconditions such as reactants, ratio of reactants, reaction time and the kind of solventswere investigated in the paper. The structure, size and oxygen content of samples wereanalysized by means of X-ray powder diffraction, TEM and X-ray photoelectronspectrometry technology. It is found that reflux and solvent-thermal method cansynthsize complex fluorides with single-phase structure. The resluts showed that thesize of particles were smaller than 100 nm which belonged to namoparticle. Using Xrayphotoelectron spectrometry, it is confirmed that the samples does not contain theoxyfluoride and that the superficial oxygen content is low. Compared with solventthermalmethod, the reflux method has many advantages such as simple technology,mild conditions, fast phase-transformation rate and so on. The method can be usedfully in the future. KAlF/_4, NH/_4AlF/_4, Li/_3AlF/_6, Na/_3AlF/_6, KAlF/_4:Ce~/(3+/), NH/_4MgAlF/_6:Ce~/(3+/) andKFeF/_3:Ce~/(3+/) had been synthesized with refluent glycol extraction method. The resultsXRD indicate that the value for the sample is similar to the data standard of cardand no impure peaks appear. This shows that the crystal structure don’t changesignificantly by doping a small amount of Ce~/(3+/) ions. The product is single phase. Inthe emission of KAlF/_4:Ce~/(3+/) powders, there is one sharp line emission located at 326nm, which is arisen from 5d-4f transition of Ce~/(3+/) in KAlF/_4 lattice. In the emissionspectrum of NH/_4MgAlF/_6:Ce~/(3+/), there is one broad range of 300-400 nm with amaximum center located 335 nm, and their absorption and emission characteristics arebroadband. The result shows that the complex fluorides KAlF/_4:Ce~/(3+/)andNH/_4MgAlF/_6:Ce~/(3+/) are superior substrate of fluorescent material.

关 键 词： 复合氟化物 回流法 溶剂热法 荧光材料

领　　域： [一般工业技术]