NaGd（WO4）2:Yb3+,Tm3+纳米粉的制备与上转换发光性能

以聚乙二醇为络合剂,采用水热法成功制备了NaGd(WO4)2:Yb3+,Tm3+纳米粉。运用X射线粉末衍射、扫描电镜和光谱分析对制备的样品结构和发光性能进行了表征。结果表明,NaGd(WO4)2:Yb3+,Tm3+为四方晶系,晶粒尺寸约为50 nm。在980 nm半导体激光器激发下获得了发射光谱,有3个发射峰,发光中心位于455,476和650 nm,分别对应1D2→3F4,1G4→3H6,1G4→3F4的跃迁。讨论了Yb3+,Tm3+能量转换过程和机制。泵浦功率与发光强度关系表明,455,476和650 nm的3个发射均属于三光子过程。     

Li+掺杂对TeO2:Tm3+/Er3+/Yb3+纳米材料上转换发光的增强作用

采用水热法制备了发白光的Li+掺杂α-TeO2∶Tm3+/Er3+/Yb3+和β-TeO2∶Tm3+/Er3+/Yb3+纳米上转换发光材料。采用X射线衍射、透射电镜和上转换发光光谱对制备的TeO2∶Tm3+/Er3+/Yb3+/Li+纳米材料进行表征,结果显示:Li+的掺入基本不改变纳米材料的晶型和结构;在980 nm近红外光的激发下,纳米材料发射出中心波长476 nm的蓝光,525 nm及545 nm的绿光和659 nm及675nm的红光,分别对应于Tm3+的1G4→3H6能级跃迁,Er3+的2H11/2→4I15/2和4S3/2→4I15/2能级跃迁,Er3+的4F9/2→4I15/2能级跃迁和Tm3+的3F2→3H6能级跃迁;Li+的掺入能够增大白光体系的发光强度,基本不改变纳米材料的白光颜色。此外,探讨了纳米材料的上转换发光机理。     

Yb3+/Tm3+掺杂的NaY(WO4)2纳米晶的制备及发光特性

以聚乙二醇为配位剂,用水热法制备出纳米级上转换发光粉Yb3+和Tm3+共掺杂的NaY(WO4)2。研究了不同cYb/cTm对上转换发光强度的影响,实验表明当cYb/cTm=5∶1时,上转换发光强度最强。用XRD,SEM确定了Yb3+和Tm3+共掺杂的NaY(WO4)2是四方晶系,其粒径在25~35 nm范围,且分散均匀。用980 nm半导体激光器(LD)对其进行激发,在室温下观察到了365 nm附近紫外发射峰、456 nm,476 nm附近的蓝光发射峰和648 nm附近的红光发射峰,分别对应于Tm3+离子的1D2→3H6,1D2→3F4,1G4→3H6和1G4→3F4的跃迁。根据泵浦功率与发光强度的关系得出紫外发射峰、蓝光和红光发射均为双光子过程。     

一种上转换白光荧光粉的制备与发光性能研究

采用高温固相法制备了上转换白光荧光粉AlF3-YbF3:Er3+/Tm3+。通过XRD物相分析可知:上转换白光荧光粉AlF3-YbF3:Er3+/Tm3+是由三方AlF3相和正交YbF3相组成;利用发射光谱研究了该荧光粉的上转换发光性能,并且分析了当固定Er3+离子掺杂浓度时,Tm3+离子掺杂浓度对上转换白光荧光粉AlF3-YbF3:Er3+/Tm3+色度的影响,进而提出其上转换能量传递机制。结果表明:在980 nm激光激发下,波长为410 nm的紫光峰、550 nm的绿光峰和660 nm的红光峰分别对应于荧光粉中Er3+离子的2H9/2→4I15/2,4S3/2→4I15/2和4F9/2→4I15/2能级的跃迁,而波长为360 nm的紫外光峰、450 nm的蓝光峰、700 nm的红光峰,分别对应于荧光粉中Tm3+离子的1D2→3H6,1G4→3H6和1G4→3F4能级的跃迁,Er3+离子发出的光与Tm3+离子发出的光最终混合成色坐标为x=0.32,y=0.36的白光。此外,通过980 nm半导体激光器和EPM 2000 Dual-channel Joulemeter/Power meter测得该荧光粉最大上转换效率为6.90%。     

NaY(WO4)2:Eu3+/Tb3+/Tm3+白色荧光粉的制备与发光性能

采用溶剂热法合成了一种单一相白色荧光粉NaY(WO4)2:Eu3+,Tb3+,Tm3+.通过X射线衍射(XRD)、扫描电镜(SEM)、X射线能谱(EDS)及荧光光谱(PL)对制备的系列样品的物相、形貌和荧光性质进行了表征.结果表明:在荧光粉NaY(WO4)2:x％Eu3+,4％Tb3+,1％Tm3+(x=5,10,15,20)中,随着Eu3+掺入量的增加,发光从绿光区进入白光区.同时观察到Tb3+到Eu3+的有效能量传递.     

不同掺杂浓度Tm3+：LiLuF4单晶的1800 nm荧光发射

采用坩埚下降法生长了Tm3+掺杂浓度为0.45%,0.90%,1.63%与3.25%(摩尔分数,x)的LiLuF4单晶.测试了样品的电感耦合等离子体原子发射光谱(ICP-AES)、X射线衍射(XRD)谱、吸收光谱(1400-2000 nm),并且分析比较了808 nm半导体激光器(LD)激发下荧光光谱.结果表明:当Tm3+的浓度从0.45%变化到3.25%时,1800 nm处的荧光强度呈现了先增后减的趋势,当掺杂浓度约为0.90%时达到最大值,而位于1470 nm处的荧光强度则呈现了相反的趋势.Tm3+:3F4能级的荧光衰减寿命随着掺杂浓度的增加不断减小.1800 nm处的这种荧光强度变化归结于Tm3+离子间的交叉驰豫效应(3H6,3H4→3F4,3F4)和自身的浓度猝灭效应.同时计算得到了浓度为0.90%的样品在1890 nm处的最大发射截面为0.392×10-20cm2.并且根据Judd-Ofelt理论所得寿命和测定的荧光寿命计算得到了3F4→3H6的最大量子效率约为120%.     

不同掺杂浓度Tm3+∶LiLuF4单晶的1800 nm荧光发射

采用坩埚下降法生长了Tm3+掺杂浓度为0.45％,0.90％,1.63％与3.25％(摩尔分数,x)的LiLuF4单晶.测试了样品的电感耦合等离子体原子发射光谱(ICP-AES)、X射线衍射(XRD)谱、吸收光谱(1400-2000 nm),并且分析比较了808 nm半导体激光器(LD)激发下荧光光谱.结果表明:当Tm3+的浓度从0.45％变化到3.25％时,1800 nm处的荧光强度呈现了先增后减的趋势,当掺杂浓度约为0.90％时达到最大值,而位于1470 nm处的荧光强度则呈现了相反的趋势.Tm3+∶3F4能级的荧光衰减寿命随着掺杂浓度的增加不断减小.1800 nm处的这种荧光强度变化归结于Tm3+离子间的交叉驰豫效应(3H6,3H4→3F4,3F4)和自身的浓度猝灭效应.同时计算得到了浓度为0.90％的样品在1890 nm处的最大发射截面为0.392x 10-20 cm2.并且根据Judd-Ofelt理论所得寿命和测定的荧光寿命计算得到了3F→3H6的最大量子效率约为120％.     

LiMgPO_4:Tm,Tb磷光体的热释光特性

采用高温固相法合成了Li Mg PO4:Tm,Tb粉末样品,研究了热释光特性与发光机制,测量了热释光发光曲线、热释光三维光谱、X射线衍射谱和荧光光谱以及剂量响应曲线。热释光三维光谱显示其主发光峰的发光波长为455 nm,峰温为325℃。采用热释光一般级动力学方程对发光曲线进行拟合得到其陷阱深度为1.34 e V。Li Mg PO4:Tm,Tb主发光峰面积与Al2O3:C相近,在0.1~2000 Gy范围内具有良好的线性响应。对Li Mg PO4:Tm,Tb粉末样品反复测量的研究结果表明该样品具有良好的稳定性和可重复性。     

Yb3+/Tm3+共掺杂的钨酸镉纳米晶发光性能的研究

本文采用水热法制备了稀土离子Yb3+/Tm3+共掺杂的钨酸镉纳米晶。运用X-射线粉末衍射、场发射环境扫描电子显微镜和光谱分析对制备的样品的结构和发光性能进行了表征。根据XRD图谱可知,钨酸镉为单斜晶系,晶粒平均尺寸在28 nm左右。从ESEM图片可明显看出,钨酸镉呈纳米棒结构,直径在30 nm左右,长径比在5~8之间。利用980 nm半导体激光器激发钨酸镉纳米晶得到样品的发射光谱,存在一个较强的蓝光发射,发光峰位于481 nm,对应于Tm3+的1G4→3H6能级的跃迁,分析了Tm3+/Yb3+离子共掺体系的发光机制。讨论了发光强度随稀土离子浓度的变化,当Tm3+离子的掺杂浓度在2mol%,Yb3+/Tm3+物质的量浓度比cTm3+/cYb3+=10时钨酸镉纳米晶的发光强度最强。根据泵浦功率与发光强度之间的关系,可知处于481 nm的蓝光发射属于三光子过程,由发光强度与掺杂浓度之间的双对数衰减曲线可知,引起蓝光发射源于Tm3+的电偶极跃迁。     

Yb:Er:Tm:LiTaO3的上转换发白光性能研究

980 nm脉冲激光激发下,首次通过高温固相法制备Yb(10%):Er(1%):Tm(1%):LiTaO3(摩尔分数)多晶粉并实现室温上转换白光.X射线粉末衍射测试结果表明,Yb:Er:Tm:LiTaO3中的掺杂离子并没有改变晶格结构,以取代的方式存在于钽酸锂晶格中.结合功率曲线测试结果和上转换机制研究发现,产生上转换蓝光的Tm3+离子1G4态的布居主要来自双光子同时吸收过程.而单光子上转换输出的红光,则由Tm3+和Er3+离子之间的交叉弛豫过程产生,即3F2/3(Tm3+)+4I15/2(Er3+)→3H6(Tm3+)+4I9/2(Er3+).上转换绿光来源于Yb/Er离子对的二次能量传递.     

Synthesis and properties of potassium 5,5'-azobis (1-nitraminotetrazolate): A green primary explosive with superior initiation power

Potassium 5,5'-azobis(1-nitraminotetrazolate), (K₂ABNAT), a new green primary explosive, was synthesized via a safe and convenient synthetic procedure based on methylcarbazate and cyanogen azide. The compound was characterized by single-crystal X-ray diffraction, IR spectroscopy, Raman spectroscopy, multinuclear NMR spectroscopy, elemental analysis, and differential scanning calorimetry (DSC). With the calculated (CBS-4M) heat of formation (617.0 kJ/mol) and the room temperature X-ray density (2.11 g/cm³), impressive values for the detonation parameters such as detonation velocity (8367 m/s) and pressure (31.5 GPa) were computed using the EXPLO5 program. The superior calculated energetic performance show it could serve as a green replacement for the widely used primary explosive, lead(II) azide, which contains toxic ingredient.     

Synthesis and Photoluminescence of Eu-doped ZnO Nanosheets

Eu-doped ZnO nanosheets were synthesized successfully by means of the hydrothermal method. The X-ray diffraction(XRD) pattern shows that the sample is a single phase with the ZnO-like wurtzite structure. And the X-ray photoelectron spectrum suggests that there are Eu3+ ions in the matrix of the sample. Eu3+-related red emissions resulted from energy transfer were observed for the nanosheets under UV laser excitation. The UV, green and yellow emissions were also seen in the photoluminescence spectra.     

阴离子对鼠尾草提取物中Ni盐前体绿色合成的NiO纳米粒子磁性和结构性能的影响

采用绿色合成方法,将鼠尾草提取物用作还原和封端剂合成氧化镍纳米颗粒(NiO NPs)。此外,使用各种前驱体合成了NiO NPs,并使用扫描电子显微镜对其形貌进行了分析。利用傅里叶变换红外光谱和粉末X射线衍射(PXRD)对NiO NPs的结构进行了表征,使用振动样品磁强计测量了它们的磁性。PXRD研究表明,所有合成的NiO NPs都表现出具有高结晶度的面心立方相,并且形成了具有高纯度相的NiO。磁化研究结果表明,3种镍盐(乙酸盐、氯化物和硫酸盐)前驱体合成的NiO NPs分别表现出超顺磁、软铁磁和顺磁行为。     

阴离子对鼠尾草提取物中Ni盐前体绿色合成的NiO纳米粒子磁性和结构性能的影响

采用绿色合成方法,将鼠尾草提取物用作还原和封端剂合成氧化镍纳米颗粒(NiO NPs)。此外,使用各种前驱体合成了NiO NPs,并使用扫描电子显微镜对其形貌进行了分析。利用傅里叶变换红外光谱和粉末X射线衍射(PXRD)对NiO NPs的结构进行了表征,使用振动样品磁强计测量了它们的磁性。PXRD研究表明,所有合成的NiO NPs都表现出具有高结晶度的面心立方相,并且形成了具有高纯度相的NiO。磁化研究结果表明,3种镍盐(乙酸盐、氯化物和硫酸盐)前驱体合成的NiO NPs分别表现出超顺磁、软铁磁和顺磁行为。     

Synthesis of highly stable silver nanoparticles by photoreduction and their size fractionation by phase transfer method

In this report we demonstrate a green chemical approach for the synthesis of stable silver nanoparticles in aqueous medium using tyrosine as an efficient photoreducing agent. A narrow size distribution of silver nanoparticles can be achieved by this simple photoirradiation method without using any additional stabilizing agents or surfactants. Two different irradiation sources have been explored resulting in a different particle size distribution pattern in each case. Further, we show that starting from a polydisperse tyrosine synthesized silver nanoparticles sample, it is also possible to fractionate them into different size ranges. The size fractionation was achieved by a 2 stage phase transfer method employing different organic solvents. The nanoparticles synthesized were characterized using UV-vis spectroscopy, Transmission electron microscopy (TEM) and X-ray diffraction (XRD) techniques.     

Studies on green synthesized silver nanoparticles using Abelmoschus esculentus (L.) pulp extract having anticancer (in vitro) and antimicrobial applications

Silver nanoparticles (Ag NPs) were successfully synthesized using AgNO₃ via an eco-friendly and simple green route using Abelmoschus esculentus (L.) pulp extract at room temperature. The phytochemicals present in A. esculentus (L.) pulp extract were used both as a reducing and a stabilizing agent for the synthesis of Ag NPs. The stabilization of Ag NPs with phytochemicals was justified using Fourier-transform infrared spectroscopy. The size of the as-synthesized Ag NPs was examined using dynamic light scattering and confirmed by transmission electron microscopy. The crystalline nature of Ag NPs had been identified using X-ray diffraction. The present study demonstrated the efficacy of Ag NPs against Jurkat cells in vitro. Our study also showed that the IC₅₀ dose of Ag NPs leads to the increase in intracellular reactive oxygen species and significantly diminished mitochondrial membrane potential, indicating the effective involvement of apoptosis in cell death. The synthesized Ag NPs also exhibited good antimicrobial activity against different gram class bacteria.     

SYNTHESIS OF CROSS-CONJUGATED （p-PHENYLENE）S-POLY（p- PHENYLENEVINYLENE）S HYBRIDS WITH LOW CONTENT OF STRUCTURAL DEFECTS

The novel shish-kebab-type liquid crystalline cross-conjugated （p-phenylene）s-poly（p-phenylenevinylene）s hybrid was synthesized through Gilch polymerization. Their structures and properties were characterized by NMR, GPC, DSC, X-ray diffraction and polarizing optical microscope （POM）. ^1H-NMR investigation of the polymers indicates that the shish-kebab-structure has a strong ability to suppress the structural defects in the polymers. The polymers are enantiotropic liquid crystals. The melting point （Tm） of the polymers decreases when the length of the alkoxy tails of the mesogenic units increases. The mesophase was identified by X-ray diffraction method. They showed not only a smectic LC phase, but also a strong green fluorescence in chloroform. The maximum absorption band of the ＂kebabs＂ of the two, 5-bis（4＇- alkoxyphenyl）benzene at 280 nm did not appear in absorption spectra of the polymers. The same phenomena were also observed in the fluorescence spectra. These results imply that the polymers have formed a cross-conjugated uniform structure and achieved an extended n-conjugation polymer.     

Four isomers of c(96) fullerene structurally proven as c(96) cl(22) and c(96) cl(24)

Direct proof of the cage connectivities of four isomers of C(96) , the highest isolable empty fullerene, has been achieved. C(96) fractions, which were isolated from fullerene soot by recycling HPLC, were chlorinated and the resulting single crystals of C(96) Cl(22) and C(96) Cl(24) were studied by X-ray diffraction using synchrotron radiation. D(2) -C(96) (183)Cl(24) (see structure; gray C, green Cl) was obtained in two crystalline modifications.     

Hexakis(2,4,6-triisopropylphenylsilsesquioxane)

Hexasilsesquioxanes bearing bulky Tip (2,4,6-triisopropylphenyl) groups were synthesized and the structure was determined. The X-ray crystal analysis revealed that the enantiomer pair originating from the restricted rotation of the bulky Tip groups was included in the single lattice. In solution, evidence for the rapid interconversion of both enantiomers was encountered in ¹H NMR. Thus, variable temperature NMR indicated peak broadeningupon warming the sample, with a coalescence temperature of 38 ° C. Kinetic parameters of the rotation were also calculated.     

界面聚合法合成聚邻苯二胺及其表征

邻苯二胺电聚合膜己广泛用于生物活性物质固定、电催化、腐蚀防护和电色材料研究,近期也用于制备分子印迹型化学/生物传感器[1,2]。人们已经研究了聚邻苯二胺的结构特性、性能及应用前景[3,4,5]。目前聚合物基纳米复合材料的制备方法主要有:分子自组装法、微乳液聚合法、电化学