微波法合成稀土氟化物纳米材料.doc

微波法合成稀土氟化物纳米材料18篇文献文摘目录1 侯远，董相廷，王进贤，刘桂霞稀土氟化物微纳米材料制备方法的研究进展中国稀土学报，2010，（05）：515524 中文摘要：稀土氟化物纳米材料由于其特殊的光、电、磁性质,在光学器件、显示、生物标记、光学晶体等领域有着广泛的应用,已成为材料科学领域的研究热点之一。目前研究者已用沉淀法、微乳液法、水热与溶剂热法、溶胶-凝胶法、微波法、超声波法、前驱体热解法、静电纺丝法等成功地制备出了纳米颗粒、纳米线、纳米膜、多面体纳米晶、复合结构纳米晶、核壳结构纳米材料等稀土氟化物纳米材料。本文总结了上述几种制备方法的研究进展,讨论了其优缺点,并结合课题组在稀土氟化物纳米材料制备方面的工作,对纳米稀土氟化物制备方法的发展方向做了展望。Rare earth fluorides nanometerials became one of the popular research subjects in recent years because they were extensively used in the fields of optical devices,display,biolabeling,opticalcrystals,etc.owingtotheiruniqueoptical,electricalandmagneticproperties.Recently,manymethods,suchasprecipitation,microemulsion,hydrothermalandsolvothermal,sol-gel,microwave,ultrasonic,precursorsthermaldecomposition,andelectrospinningtechniqueweresuccessfullyemployed to fabricate rare earth fluorides na2 闫景辉, 张鸣, 连洪州, 叶泽人, 石春山 .微乳液体系相图的研究及其在纳米氟化物制备中的应用 .高等学校化学学报 ,2 0 0 5 ,(06):10061009 中文摘要：绘制了十六烷基三甲基溴化铵(CTAB)/正丁醇(n2C4H9OH)/正辛烷(n2C8H18)/水 或NH4F 溶液、或Ba (NO3) 2 溶液、或KNO32M g (NO3) 2 混合溶液四组分微乳体系的拟三元相图. 观察了电导率随水(或盐溶液) 含量变化的规律, 很好地印证了微乳液体系相行为. 选取相图中微乳区点作为最佳条件, 制备了KM gF3 纳米粒子. 英文摘要：Pseudo-ternary phase diagrams in quaternary microemulsion systems of cetyltrimethyl ammonium bromide(CTAB), n-butanol, n-octane and wateror NH_4F solution, or Ba(NO_3)_2 solution, KNO_3-Mg(NO_3)_2 mixture solution are presented. Variation of the electrical conductivity with the change of water content(or solution) was observed, which supported the phase behavior of microemulsion systems. KMgF_3 nanoparticles were prepared with the optimal parameter of phase diagrams of microemulsions systems.3 马琳, 陈卫祥,李辉，徐铸德.微波合成PrF3 空心纳米粒子和氢氧化镨纳米棒.浙江大学学报( 工学版)，第42 卷第10 期 2008-10-036 18331837 中文摘要：用快速高效的微波辐射加热方法成功地合成了PrF3空心纳米粒子和氢氧化镨纳米棒,并以所制备的氢氧化镨纳米棒为前驱体通过热处理得到了氧化镨的纳米棒.对产物进行了X-射线衍射(XRD)、透射电镜(TEM)和电子能谱(EDX)的表征.结果表明,微波合成的PrF3为球形形貌的中空纳米粒子,并具有均匀的粒径大小.微波合成的氢氧化镨纳米棒具有高的结晶度和纯度.实验结果表明,较长的微波加热时间和较高的碱浓度有利于结晶度高的氢氧化镨纳米棒的形成.初步讨论了微波条件下合成氟化镨中空纳米粒子和氢氧化镨纳米棒的形成机理.PrF3 hollow nanoparticles and Pr(OH)3 nanorods were synthesized via a rapid microwave irradiation method and Pr6O11 nanorods were obtained by calcination of the as-prepared Pr(OH)3 nanorods as precursors.The products were characterized by X-ray powder diffraction(XRD),transmission electron microscope(TEM) and energy dispersive X-ray analysis(EDX).Results showed that the synthesized PrF3 nanoparticles by microwave irradiation were spherical-like hollow with uniform particle size.The synthesized Pr(OH)3 nanor.4 张秀凤，涂华民，张迈生，林木良.纳米氟化铈()的微波固相氧化还原合成法。材料导报 ，2003（01):7880 中文摘要：首次在微波场作用下,采用直接法和间接法快速合成了氟化铈(),通过XRD、TG-DTG及场发射扫描电镜(FE-SEM)等方法对样品的组成、结构进行了分析表征,并讨论了两种合成方法以及微波合成条件对产物的影响。研究表明:采用本方法合成的CeF_3,晶型为类球形,平均粒径约为100nm。Nanostructure cenum() fluoride was synthesized by two ways in microwave radiation field.The samples were characterized by XRD,TG-DTA and FE-SEM.The effect of these two methods and reaction conditions in microwave radiation field were discussed.The results show that nanostructure cerium fluoride with a spherical morphology at a crystalline particle diameter of about 100nm was obtained.5王亚军; 刘前; 索全伶; 郝东升; 郭锋;稀土氟化物的沉淀方法及组成研究稀土,2000年 01期 16-20 中文摘要：本文研究了湿法制备稀土氟化物的工艺过程,考察了HF用量、稀土浓度、反应温度和添加大分子助沉剂对稀土收率和沉淀速率的影响。报道了一种快速沉淀稀土氟化物的新方法,并用透射电镜、X射线衍射、X射线荧光光谱和差热-热重等分析方法测定了氟化物的形貌、粒径和组成。The technological processes of rare earth fluoride prepared by hydrometallurgical methods have been studied.The effect of the fluohydric acid amount and rare earth concentration,reaction temperature and macromolecular precipitating aid agent on the yield of rare earth and precipitation rate was discussed.A new method of fast precipitating rare earth fluoride was reported.The component,appearance and grain size of the product were determined by TEM,XRD,X ray fluorescence,DTA and TG6 宋丽红.稀土掺杂氟化物及纳米复合发光材料的制备与光谱性质.长春理工大学 2007-06-06 中文摘要：本文采用十六烷基三甲基溴化铵正丁醇正辛烷水组成的微乳液体系制备了YF_3：Eu、YF_3：Tb、YF_3：Ce、YF_3：Er等一系列纳米微粒。运用XRD确认了制备所得样品为YF3斜方晶系；用ESEM观察YF_3：Eu、YF_3：Tb、YF_3：Ce和YF_3：Er纳米粒子，粒径大约为1340nm。 制备所得的YF_3：Eu纳米粒子的尖峰发射位于592nm，归属于Eu(3+)的5D_07F_1跃迁；YF_3；Tb尖峰发射位于544nm，属于Tb(3+)(5D_47F_5)的特征发射，是5D_4能级的绿色跃迁发射；而YF_3：Ce纳米粒子宽带发射峰的最大值位于340nm处，属于近紫外发光；YF_3：Er红外荧光光谱最大发射位于1547nm处，发生了红移现象，上转换发射为红光和绿光。 对YF_3：EuPMMA复合膜、YF_3：TbPMMA复合膜的制备及光谱性质进行了初步研究；荧光光谱研究表明，复合膜的激发和发射光谱与YF_3：Eu、YF_3：Tb纳米粒子相比，主要发射峰的位置没有发生变化，强度大大减弱。In the dissertation, nanoparticles of YF_3:Eu, YF_3:Tb, YF_3:Ce and YF_3:Er were prepared from the quaternary microemulsions of CTAB, n-butanol, n-octance and water based .The X-ray diffraction (XRD) patterns were indexed to a pure YF_3 orthorhombic phase. Envrionment scanning electron microscopy (ESEM) images showed spherical YF_3:Eu,YF_3:Tb,YF_3:Ce and YF_3:Er nanoparticles which were about 13-40 nm in diameter. The emission of YF_3: Eu nanoparticles peaked at 592 nm attributed to Eu(3+) 5D_07F_1 tr.7 马琳 .微波和水热合成稀土化合物、二硫化钼纳米材料及表征浙江大学 2008-10-07 中文摘要：无机纳米材料的形貌、尺寸及其微观结构对其物理和化学等性质和应用具有重要的影响。具有特定形貌和微观结构的无机纳米材料(如：纳米线、纳米棒、中空纳米结构、纳米微米球等)的合成及其性能的表征对于新型无机功能材料的基础和应用研究都具有重要的意义。 稀土化合物，由于其离子的4f壳层内具有众多的跃迁模式，被广泛应用于高性能发光设备、磁性材料、催化剂以及其它功能材料。在纳米级的稀土化合物材料中，发光量子效率和显示分辨率都将得到进一步的提高。具有三明治层状结构的过渡金属硫化物二硫化钼(MoS_2)纳米材料，由于其在催化剂、储氢材料、镁离子和锂离子电池的电极材料以及固体润滑剂方面的潜在应用而得到人们的持续关注。本论文用快速的微波加热技术和温和的水热法合成不同形貌的多种稀土化合物纳米材料(如：氢氧化镨和氧化镨纳米棒、中空结构的氟化镨纳米粒子、稀土离子掺杂的氟化镧纳米粒子和磷酸镧纳米棒、不同形貌的氟化铈纳米结构、不同形貌的磷酸铈纳米棒聚集体、梭形的羟基碳酸铈和二氧化铈等)，对其结构和性能进行了表征，并讨论了相应的不同形貌的稀土化合物纳米材料的形成机理；用室温离子液体作为添加剂，水热法合成了由二硫化钼纳米片构成的微球。It is known that the size and shape of inorganic nanomaterials have great influence on their physical and chemical properties.Thus,the synthesis and propertycharacterization of inorganic nanomaterials with special morphologies andmicrostructures are of great importance for the basical and applied research of new inorganic functional materials. Rare earth compounds have been widely used in high performance luminescent devices,magnets,catalysts,and other functional materials owing to the numerous well-def.8涂华民; 张秀凤; 张迈生 轻稀土氟化物的微波固相快速合成法稀有金属 2004年 05期 875-879 中文摘要：在微波场作用下 ,采用轻稀土氧化物和氟化氨的固相反应快速合成了轻稀土氟化物、氟氧化物以及氟化物复盐 ,通过XRD及场发射扫描电镜 (FE SEM )等方法对样品的组成、结构进行了分析表征 ,并讨论了轻稀土氟化物的反应历程以及微波合成条件对产物的影响。研究表明 :在微波场作用下 ,采用NH4 F和轻稀土氧化物直接反应合成氟化稀土 ,具有方法简单 ,易于操作 ,高效节能等特点。The light rare earth fluorides, rare earth oxyfluorides, and the complex of rare earth fluoride with NH 4F were rapidly synthesized in a microwave radiation field by NH 4F reacted with rare earth oxides. XRD and FE-SEM were used to characterize the samples component and their crystal structure. The effect of these reaction conditions in a microwave radiation field was also discussed. The experimental results of XRD and FE-SEM show that REF 3 possess a spherical crystallite structure, in the micrometer9张秀凤 微波固相法快速合成稀土卤化物河北师范大学 2003-11-14稀土卤化物是一种应用范围非常广泛的物质，在石油化工、玻璃、冶金、纺织和养殖业等各个领域得到了应用，同时它在碳弧棒发光剂、钢铁和有色金属合金添加剂、制备单一稀土金属等方面也有重要的用途。近年来也成为制备新型电光源、氟化物光纤、红外区用荧光粉、永磁材料、储氢合金、磁光存储等新材料的重要原料。 在科研和生产实践中，无水氟化稀土常用的合成方法有：氢氟酸沉淀-真空脱水法、氟化氢气体氟化法和氟化氢铵氟化法三种方法。无水稀土氯化物的制备方法也有三种：结晶水合物稀土氯化物的减压(真空)脱水法；稀土氧化物直接氯化；稀土精矿高温加碳氯化。传统的合成无水氟化稀土和稀土氯化物方法常常用到具有毒性、腐蚀性的气体，如HF、HCl、Cl_2等，对人体造成很大危害，对环境造成严重污染。传统合成法具有反应时间长、过程繁琐、能耗大等缺点。 由于微波独特的加热方式，近几年微波技术已被广泛应用于各个化学领域。与传统加热方式相比，微波加热有其独特的优点：微波加热是材料在电磁场中由介质损耗而引起的体加热，使得被加热物质的温度在很短的时间内得以迅速升高。由于微波加热速率快，避免了材料合成过程中晶粒的异常长大，所以采用微波加热合.Rare earth halides. are widely used in many fields, such as in petroleum company, glass, metallurgy, breed aquatics industry and so on . Meanwhile, it is very useful in carbon arc stick luminescence, iron, addiction in colored metals and manufacture of rare earth metals, etc. In recent years, rare earth halides are of very importance in preparation of new electron-resource material, fluoride. IR fluorescent powder, etc. When it comes to the preparation of rare earth halides, there are three conventional .10 张迈生; 祁家雄; 杨燕生 Sol-Gel法和微波辐射法合成亚纳米级Zn_2SiO_4Mn(2+),Er(3+)高效绿色荧光体，发光学报,1999年 03期 258-261用法和微波法合成了亚纳米级 ， 高效绿色荧光体， 考察了 单掺和 敏化的荧光体的发光， 探讨了掺杂浓度对发光性质的影响， 发现 可有效敏化 的发光 表明 ， 的粒度约为 In this paper, Sol Gel method and microwave radiation method were used to synthesize the phosphors of silicate oxyapatites doped with Mn 2+ , or codoped with Mn 2+ and Er 3+ . The high efficient, green color, subnanometer phosphors of Zn 2SiO 4Mn 2+ , Er 3+ , with 150350nm were obtained by means of these two methods11 张先如; 徐政 微波技术在材料化学中的原理及其应用进展辐射研究与辐射工艺学报 2005年 04期 196-200微波作为一种新的技术手段,已广泛应用于材料的各个领域。综述了微波化学的原理、实验设备及其在材料化学中的应用进展,并对微波在有机合成、高分子化学及加工、无机合成等方面的最新应用情况进行了综述。As a new technical method, microwave has been used in every aspect of materials. This paper summarizes the principle of microwave chemistry, experimental equipments and application in material chemistry. At the same time we introduce progresses in organic synthesis, macromolecule chemistry and inorganic synthesis with microwave technique.12 梁政勇; 章亚东;微波技术在氟化反应中的应用进展 .辐射研究与辐射工艺学报,2010年 02期 69-74绿色有机合成技术作为一门新兴合成技术,已逐渐引起人们的广泛关注与重视,在酯化、缩合、氧化、还原等许多有机单元反应中都有着广泛的应用。微波独特、高效的加热效果使得微波有机反应具有反应速度快、选择性好等优点,甚至可使一些在常规加热条件下无法进行的反应顺利进行。本文综述了近年来微波有机合成技术在氟化反应中的应用新进展,并对微波技术工业化推广中存在的问题进行了评述。Microwave-assisted organic synthesis,as a novel green synthesis technology,has been given more and more attention. It has been widely applied in many unit reactions,such as esterification,condensation,oxidation and reduction reaction etc. The unique and high efficiency heating effect of microwave,in many cases,could increase the reaction rate and product selectivity. Even some reactions could be taken place successfully in microwave while it was almost impossible in conventional heating. In this paper,rec.13梁政勇; 吕春绪; 李斌栋;微波作用下卤素交换氟化制备氟代苯甲醛及二苯甲酮类化合物 化学通报, 2006年 11期 836-840在微波作用下,采用高效催化剂体系,于中等极性非质子溶剂中经卤素交换氟化高效制备了系列含氟芳香醛(酮)类化合物,产品收率533%926%,反应时间较常规加热最多可缩短80%以上。采用中等极性反应溶剂,还可突出表现出微波对反应促进的“非热效应”,从而大大拓宽了氟化反应溶剂的选择范围。An effective co_catalyst was used in halogen-exchange fluorination of chlorobenzaldehydes and chlorinated diphenyl ketones under the irradiation of microwave. The yield of products was in the range of 53.3%92.6%, and the reaction time can be shortened by more than 80% at most in comparison with that of common heating. In addition, “non-thermal effect can be showed obviously when the reaction was carried in medium polar aprotic solvents. So, more kinds of solvents can be used in halogen-exchange fluorinati.14 陶萍芳; 覃利琴; 庞起; 方岳平;稀土掺杂氟化物的水热合成及其发光性能的研究玉林师范学院学报 2010年 02期 36-39本文在不需要任何辅助剂,反应温度为140,恒温12h的简易水热条件下,成功地合成了掺杂不同稀土离子(如:Eu3+、Ce3+、Tb3+等)的玉米穗状氟化物(如YF3:Eu3+;YF3:Ce3+;YF3:Tb3+等),所得的产物用X-射线衍射仪(XRD)、扫描电子显微镜(SEM)和时间分辨荧光光谱仪等手段对其结构和形貌以及发光性能进行表征.XRD结果表明产物各衍射峰归属为纯相YF3,SEM结果表明产物为由纳米颗粒自组装成的玉米穗.PL结果表明YF3:Eu3+,YF3:Ce3+,YF3:Tb3+主发光峰位置各不相同.In this paper,rare earth ions(Eu3+、Ce3+、Tb3+) doped corn-like YF3 have been successfully synthesized via simple hydrothermal process,at 140 by 12h without any assistant agent.The structure and morphology of the obtained products were characterized by XRD,SEM and photoluminescence.The X-ray diffraction analysis revealed the obtained products were pure phase YF3,and the SEM showed that the products are microcorn-like self-assembled by nanoparticles.PL proved that the main peak of different rare earth ions(Eu.15 张瑞锐; 高源; 唐波;稀土掺杂氟化物纳米材料的上转换发光特征及其生物应用分析科学学报 2010年 03期 353-357稀土掺杂氟化物纳米材料由于具有低的声子能,可以获得较高的上转换发光效率,使其在太阳能电池、生物医学、光电子学、信息等领域有着广泛而重要的应用前景。本文就当前稀土氟化物上转换纳米材料的改性、光性能研究,以及在生物检测,生物成像标记,免疫分析,疾病治疗方面的最新研究进展做一综述,并对上转换纳米颗粒在生物应用过程中存在的主要问题进行了讨论。Lanthanide-doped fluoride nanoparticles have low phonon energies,which leads to a great contribution to the luminescence intensity,and thus have huge promise in solar cells,biomedicine,optoelectronics,and telecommunications,etc.The preparation,properties enhanced of lanthanide-doped fluoride nanoparticls and their application in life sciences are intrigued many scientists.Recent research progress in the application of lanthanide-doped fluoride nanoparticles in bioanalysis,label and image,immunological assa.16 郭琦; 缪建军; 耿珺; 朱俊杰 微波热解法制备Cu/Cu_2O纳米材料应用化学 2010年 12期 1438-1443在二乙二醇溶剂体系中利用微波介电加热分解醋酸铜前体,进一步还原得到Cu2O和Cu纳米粒子以及Cu/Cu2O核壳结构。采用X射线衍射、透射电子显微镜、扫描电子显微镜和紫外吸收光谱测试技术对产物的形貌、结构和组成进行了研究,结果表明,得到的Cu/Cu2O核壳结构直径为500nm左右。对比实验研究了不同聚合度乙二醇系列溶剂、反应时间以及表面活性剂或配位剂对产物形貌、组成的影响,表明低聚合度乙二醇和长的反应时间有利于醋酸铜还原形成铜。Copper acetate was decomposed by microwave heating to form Cu2O and Cu nanoparticles and Cu/Cu2O core