碱土—稀土氟化物溶剂热合成中显微组织与发光性能的调控
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摘要
稀土掺杂纳米材料具有独特的发光和磁性质，在发光、颜色显示、防伪、生物大分子检测、生物荧光成像、生物分离和磁共振成像等方面应用前景广阔。寻找新的发光基质材料并研究其可控合成，得到满足各种应用需求的稀土掺杂纳米材料具有重要的学术价值和现实意义。碱土-稀土氟化物在高温下具有丰富的相组成，但对其低温相组成和纳米晶的可控合成还缺乏系统研究。本文以几种典型的碱土-稀土氟化物为研究对象，系统研究了在低温溶剂热合成时，稀土元素含量、反应条件对产物相结构、晶粒尺寸及形貌的影响，并对所获得的纳米晶的发光性能进行了研究。主要研究内容及结论如下:
1.低温溶剂热合成条件对SrF_2-LaF_3体系反应产物的相组成、晶粒尺寸及形貌的影响，纳米晶发光性能的调控。研究结果表明:采用低温溶剂热合成法制备的产物的相组成取决于SrF_2-LaF_3体系的成分，名义成分为Sr_(1-x)La_xF_(2+x)(原子百分数，at.%，以下相同)的产物，在0≤x<0.35、0.35≤x≤0.9和0.9 2.低温溶剂热合成条件对BaF_2-LuF_3体系反应产物的相组成、晶粒尺寸及形貌的影响，纳米晶发光性能的调控。研究结果表明：以NH_4F为氟源时，可得立方相的BaF2和Ba_(1-x)Lu_xF_(2+x)、单斜相的BaLu2F8和立方相NH_4Lu2F8，其中得到纯立方Ba_(1-x)Lu_xF_(2+x)相的体系成分范围很窄，在x＝0.40左右;当反应体系中加入NaOH后，反应产物包括立方相的BaF2和Ba_(1-x)Lu_xF_(2+x)、单斜相的BaLu4F14、六方相的Ba7F12Cl2和NaLuF4，其中获得纯立方相Ba_(1-x)Lu_xF_(2+x)的体系成分范围扩大，在0.30 3.低温溶剂热合成条件对SrF_2-LuF_3体系反应产物的相组成、晶粒尺寸及形貌的影响，纳米晶发光性能的调控及其表面改性。研究结果表明：以HF为氟源、不加NaOH时，名义组成为Sr_(1-x)La_xF_(2+x)的产物在0 4. BaF_2-GdF_3体系超细单分散碱土-稀土氟化物纳米晶的成核生长机制研究。研究结果表明：采用低温溶剂热合成法，可制备出名义为Ba_(1-x)Gd_xF_(2+x)的纳米晶，该纳米晶在0.5≤x≤0.8成分范围内具有纯立方相结构，并通过优化合成条件，其晶粒尺寸可以控制在10nm以下；由于在溶剂热反应体系中，GdF3的溶度积常数极低，导致含有Gd的Ba_(1-x)Gd_xF_(2+x)在结晶过程中更易均匀形核，同时，Ba_(1-x)Gd_xF_(2+x)固溶体中还存在大量缺陷能阻碍晶粒生长，因而Ba_(1-x)Gd_xF_(2+x)在溶剂热合成时更易获得超细单分散的纳米晶。
Due to their unique luminescent and magnetic properties, upercopnversionluminescent nanomaterials doped with rare-earth have a lot of potential applications inthe fileds of luminescence, laser anti-counterfeit, display, detection of biologicalmacromolecules, biological fluorescence imaging and bioseparation and magneticresonance imaging. Therefore, seeking new photoluminescent materials anddeveloping new ways to realize the controlled synthesis of the nanomaterial are veryimportant to meet various requirements of their applications. According to the phasediagram of alkaline earth-rare earth fluoride systems, there exisit aboundance phasesat high temperature in these systems. However, up to date, the systematic work on thephase consititions and the controlled synthesis of these systems at low temperature islacking. Therefore, in the thesis, several typical alkaline earth-rare earth fluorideswere synthesized using solvothermal method at low temperature. The influences of Lncontent and reaction conditons on the phase structure, grain size and morphology ofthe products were studied systematicly, and the upconversion emission properties ofthe synthesized ultra-fine monodisperse nanocrystals were also investigated. The maincontents and results are as follows:
1. The study on the effects of the reaction conditions on the phase consitutions,grain size and morphology of the reaction products in SrF_2-LaF_3system by usingsolvothermal method, and the multicolor upconversion emission behaviors of thenanosized SrF_2-LaF_3products. It is found that, the phase consititutions of the reactionproducts of Sr_(1-x)La_xF_(2+x)obtained by solvothermal method are strongly dependent onthe fluorides, the cubic phase, mixtures of cubic and hexagonal phases, and hexagonalphase can be obtained in Sr_(1-x)La_xF_(2+x)as its composition is in the range of0≤x<0.35,0.35≤x≤0.9, and0.9 2. The study on the effects of the reaction conditions on the phase consitutions,grain size and morphology of the reaction products in BaF_2-LuF_3system by usingsolvothermal method, the multicolor upconversion emission behaviors of thenanosized BaF_2-LuF_3products. By using NH_4F as fluorine source in the solvothermalreaction sytem of BaF_2-LuF_3, the products containing cubic BaF2and Ba_(1-x)Lu_xF_(2+x)phases, monoclinic BaLu2F8and cubic NH_4Lu2F8phases were succefully synthesized.However, to obtain the Ba_(1-x)Lu_xF_(2+x)with pure cubic structure, the compostion of theflorides should be controlled around x＝0.40. By addiing NaOH into the reactionsystems, the products containing cubic BaF2and Ba_(1-x)Lu_xF_(2+x)phases, monoclinicBaLu4F14phase, and hexagonal Ba7F12Cl2and NaLuF4phase can be obtained, and thecompostion of the fluorides to obtain pure cubic Ba_(1-x)Lu_xF_(2+x)phase is expended to bein the range of0.30 3. The study on the effects of the reaction conditions on the phase consitutions,grain size and morphology of the reaction products in SrF_2-LuF_3system by usingsolvothermal method, the multicolor upconversion emission behaviors of thenanosized SrF_2-LuF_3products, and surface modifaction of the products. By usingsolvothermal method under low temperature in the SrF_2-LuF_3reaction systemswithout NaOH containing, the products of Sr_(1-x)Lu_xF_(2+x)contain the mixtures of cubicSrF2and Sr_(1-x)Lu_xF_(2+x)phases, the pure cubic Sr_(1-x)Lu_xF_(2+x)phase, and the mixtures ofcubic Sr_(1-x)Lu_xF_(2+x)and orthogonal LuF3phase as its composition is in the range of0 4. The study on the nucleation and growth mechanism of the ultrasmllmonodisperse alkaline earth-rare earth fluoride nanocrystals in BaF_2-GdF_3system. Byusing solvothermal method, the products of Ba_(1-x)Gd_xF_(2+x)with pure cubic structure canbe synthesized at190C as its composition is in the range of0.5≤x≤0.8, and the grain size of the products is less than10nm. Under the same conditions, the Ba_(1-x)Gd_xF_(2+x)products with the composiotn in the range of0.5≤x≤0.8show a grain size far smallerthan that of pure phase BaF2and GdF3. It is found that GdF3has an extremely lowsolubility product constant in H2O solution in comparison with BaF2and there exist alarge amount of defects in cubic Ba_(1-x)Gd_xF_(2+x)non-stoichiometric phase, which may beresponsible for the ultrafine grain size of Ba_(1-x)Gd_xF_(2+x).
1.低温溶剂热合成条件对SrF_2-LaF_3体系反应产物的相组成、晶粒尺寸及形貌的影响，纳米晶发光性能的调控。研究结果表明:采用低温溶剂热合成法制备的产物的相组成取决于SrF_2-LaF_3体系的成分，名义成分为Sr_(1-x)La_xF_(2+x)(原子百分数，at.%，以下相同)的产物，在0≤x<0.35、0.35≤x≤0.9和0.9
Due to their unique luminescent and magnetic properties, upercopnversionluminescent nanomaterials doped with rare-earth have a lot of potential applications inthe fileds of luminescence, laser anti-counterfeit, display, detection of biologicalmacromolecules, biological fluorescence imaging and bioseparation and magneticresonance imaging. Therefore, seeking new photoluminescent materials anddeveloping new ways to realize the controlled synthesis of the nanomaterial are veryimportant to meet various requirements of their applications. According to the phasediagram of alkaline earth-rare earth fluoride systems, there exisit aboundance phasesat high temperature in these systems. However, up to date, the systematic work on thephase consititions and the controlled synthesis of these systems at low temperature islacking. Therefore, in the thesis, several typical alkaline earth-rare earth fluorideswere synthesized using solvothermal method at low temperature. The influences of Lncontent and reaction conditons on the phase structure, grain size and morphology ofthe products were studied systematicly, and the upconversion emission properties ofthe synthesized ultra-fine monodisperse nanocrystals were also investigated. The maincontents and results are as follows:
1. The study on the effects of the reaction conditions on the phase consitutions,grain size and morphology of the reaction products in SrF_2-LaF_3system by usingsolvothermal method, and the multicolor upconversion emission behaviors of thenanosized SrF_2-LaF_3products. It is found that, the phase consititutions of the reactionproducts of Sr_(1-x)La_xF_(2+x)obtained by solvothermal method are strongly dependent onthe fluorides, the cubic phase, mixtures of cubic and hexagonal phases, and hexagonalphase can be obtained in Sr_(1-x)La_xF_(2+x)as its composition is in the range of0≤x<0.35,0.35≤x≤0.9, and0.9
引文
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