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1.
以水热法制备了纳米微粒MCM-41分子筛,通过离子交换法将Cd(II)交换到分子筛中,然后采用硫代乙酰胺作硫化氢前驱体对(MCM-41)-Cd进行硫化,制备出主-客体复合材料(MCM-41)-CdS.化学分析表明,客体成功地组装到分子筛中.粉末X射线衍射结果表明,组装过程并未破坏所制备的主-客体材料中分子筛的骨架,分子筛骨架完整且结晶度仍然很高.红外光谱表明所制备材料骨架保持完好.低温N2吸附-解吸附研究表明,相对于MCM-41分子筛主体所制备的复合材料孔体积、孔尺寸及比表面积降低,表明客体在分子筛孔道内组装成功.制备的主-客体复合材料固体扩散漫反射吸收光谱相对于CdS体相呈现某些蓝移,说明客体处于分子筛孔道内,也表明分子筛主体对纳米硫化镉客体表现出明显的立体限域效应.(纳米MCM-41)-CdS及(微米MCM-41)-CdS样品呈现明显发光.  相似文献   

2.
在室温下,以掺Yb3+的MCM-41作为主体,"热处理"后的Tb(aspirin)3phen作为发光客体,将其进行组装,通过XRD和N2-吸附脱附和IR对组装体的结构和物理性质进行了研究.利用激发和发射光谱分析了组装体的光致发光性能和主客体关系.采用了一种新型的掺杂方法"直接焙烧法",用以避免在试样合成中掺杂离子的损失.在Yb/MCM-41和Tb(aspirin)3phen-Yb/MCM-41的XRD谱图中同时在20=2.6时出现了(100)晶面衍射峰,表明试样为规则有序,六方结构的MCM-41材料.Tb(aspirin)3phen进入Yb/MCM-41孔道后,无机骨架的有序性进一步增加.相对于MCM-41,Yb/MCM-41在IR谱图中波数963cm-1的谱带减弱,表明Yb3+已经进入无机骨架.另外,波数1 384 cm-1的吸收谱带也能提供组装体Tb(as-pirin)3phen-MCM-41中成键的特征信息.PL测试结果表明,Tb(aspirin)3phen在240~375 nm区间的宽激发吸收分别归属于配体aspirin羰基n→π跃迁,苯环,π→π跃迁和phen的杂菲基团吸收.对客体Tb(aspirin)3phen进行热处理,能增强Tb(aspirin)3phen在MCM-41孔道中的发光效率,并且当基质MCM-41硅骨架掺杂Yb3+后,组装体的发光强度进一步增强,当Yb/Si=7.579×10-3时,发光强度最高.  相似文献   

3.
采用溶胶 凝胶法制备NiFe2 O4 纳米粉末 ,并经不同温度热处理 .测定了制备过程中各阶段的红外吸收光谱和不同温度处理样品的红外漫反射光谱 .结果表明 ,红外吸收光谱较好地反映了溶胶 凝胶法制备NiFe2 O4 纳米粉末过程中结构的变化 ,为确定热处理温度提供了实验依据 ,彻底消除有机物 ,热处理需在 40 0℃以上 ;红外漫反射谱可以较好地反映粉末的尺寸效应和形态效应 ,粉末粒径越小 ,漫反射函数 (K M)值越大 ;当粒径达到一定尺寸时 ,红外漫反射的尺寸效应消失  相似文献   

4.
将有机发光小分子8-羟基喹啉铝(Alq3)组装进介孔MCM-41中,采用XRD、IR、荧光光谱等测试方法对组装体Alq3-MCM-41进行表征。XRD表明,Alq3-MCM-41保持了有序的介孔骨架结构;IR谱图中,在波数1542 cm-1处出现的特征吸收谱带表明组装体中Alq3在孔道中与羟基成键;荧光光谱表明,组装体中MCM-41与Alq3分子间发生了能量转移,从而使Alq3-MCM-41具有优异的发光性能;荧光强度随组装量的增多而显著增强,这主要是由于在Alq3-MCM-41中,MCM-41有序孔道的微环境使Alq3分子分散性提高,减弱了Alq3分子间的聚集或缔合现象,从而有效地提高了其发光强度。  相似文献   

5.
铝阳极氧化多孔膜制备及Eu3+组装   总被引:1,自引:1,他引:0  
阳福  刘应亮 《发光学报》2005,26(2):233-236
在草酸体系中,采用二次阳极氧化法可制备大面积有序铝阳极氧化多孔膜(AAO),用X射线粉末衍射(XRD)仪进行物相分析,利用扫描电子显微镜(SEM)表征多孔膜的形貌。研究表明,低温条件下制备的多孔膜孔径大小分布均匀,有序性好。微孔在膜的表面沿二维空间规则排列,具有一定的六方对称准周期性。孔道相互平行且与铝基底垂直。低温条件下,草酸体系中电解获得的AAO膜以无定形结构存在,经过800℃高温退火后转化为γ-Al2O3。通过水热反应法,获得了Eu^3 的铝阳极氧化多孔膜组装体(AAO:Eu^3 ),研究了组装体系的光谱特性。结果表明,这种方法制备的发光材料具有非常高的组装浓度,其发光具有很高的色纯度。  相似文献   

6.
氧化锌纳米晶体的光谱分析   总被引:2,自引:5,他引:2  
采用沉淀法并通过控制前驱体的煅烧温度来制备粒径不同的氧化锌(ZnO)纳米晶体,对粒子的透射电镜照片进行分析,结果表明,制备出的纳米粒子分散性好、形貌一致、粒径分布集中.样品的X射线衍射光谱分析表明,随着前驱体煅烧温度增加,晶体粒径增大、结晶度提高;样品的紫外-可见吸收光谱的峰位随粒径减小而发生蓝移,这一实验结果表明ZnO纳米晶体呈现出较明显的量子限域效应;红外吸收光谱测量结果表明,用沉淀法制备的ZnO纳米晶体的表面会吸附一小部分残余的离子,对红外吸收光谱中的ZnO特征振动峰随粒径减小发生宽化和红移的现象进行了理论分析;光致发光光谱测量结果表明,ZnO纳米晶体在紫外区(360 nm)存在一较弱的发光峰,而在可见区(468 nm)存在一较强的发光峰,与理论计算结果进行比较后,认为锌空位点缺陷是导致ZnO纳米晶体可见区发光的主要原因.  相似文献   

7.
利用简单的液相合成方法,在室温下制备了KMnF3圆盘状产物,盘的直径约为300nm.通过X射线粉末衍射(XRD)、透射电镜以及选区电子衍射对它的结构成分和物相进行了表征,发现圆盘形貌是由KMnF3小颗粒自组装而形成的.同时对样品的发光性质进行了研究,在416和438nm处观测到特别强的光发射,并对发射峰的来源进行了指认分析.与XRD数据计算得到的晶格参数相比,发现利用样品发光数据和公式Eem=-16963+164R,可以达到方便快捷地估算Mn-F之间距离和样品晶格常数的目的.  相似文献   

8.
采用水热法,以溴化六甲双铵(HMBr2)为模板剂,硅溶胶、偏铝酸钠为硅铝源,以六水硝酸铈为铈源合成了稀土Ce-EU-1分子筛,并通过XRD、FTIR、紫外-可见漫反射光谱、热重分析(TG-DTG)和氮气吸附-脱附等测试手段对合成样品的孔道结构、物化性能及Ce的存在状态进行了表征。XRD结果表明,合成样品不仅具有很高的纯度和结晶度,为典型的立方有序排列的EU-1结构,而且部分Ce已取代Si或Al进入微孔分子筛的骨架。样品的FTIR图谱在980cm-1附近有明显的Si—O—Ce特征吸收峰,证明Ce存在于分子筛的骨架中。紫外-可见漫反射图谱显示,在253nm附近出现O—Ce之间的电子跃迁特征峰,进一步证明了Ce进入了分子筛骨架。氮气吸附-脱附结果表明了Ce的掺入对分子筛的物化性能和孔道结构产生了影响。同时考察了镧系其他金属离子(Ln:La、Nd、Sm和Gd)对EU-1分子筛的影响,发现随着镧系离子半径的减小,Ln-EU-1分子筛的相对结晶度逐渐降低,晶胞体积减小。  相似文献   

9.
以甘氨酸为燃料,采用溶液燃烧法制备了Y2O3:Eu3 (3%)纳米粉末,并研究了制备过程中前驱溶液的pH值对Y2O3:Eu3 发光性质的影响.从XRD和SEM分析得到,随着溶液pH值的增大,样品颗粒逐渐变大,并且多孔粉末变得越来越致密.通过对样品发光性质的测量得到,随着pH值的增大,样品发光逐渐增强,但寿命逐渐变短.激发谱显示,基质吸收和电荷迁移带的相对强度比随着pH值的增大逐渐减小.  相似文献   

10.
方容川  杨嘉玲 《发光学报》1992,13(4):275-280
用电化学腐蚀法制备出多孔硅系列样品.室温下具有明亮可见的光致发光.增大电解电流或延长腐蚀时间,发光光谱明显地“蓝移”;提高样品测量温度,发光光谱也明显地“蓝移”。红外吸收光谱表明多孔硅中除了硅丝骨架以外,还含有H、F及O等元素,随着腐蚀时间的增加,F和O原子的相对含量增加.实验结果表明,多孔硅在可见光区的发光现象是一种量子尺寸效应.  相似文献   

11.
The enthalpies of solution of pure silver halides AgCl and AgI and a composite material with molar composition 0.5 AgCl-0.5 AgI were measured at 298 K in a mixture of Na2S2O3 (1 M) and NH4OH (1 M). X-ray diffraction patterns showed that the composite material contained the metastable γ-AgI phase; different mechanisms for its stabilization were discussed. The phase transition enthalpies of AgI modifications and the enthalpy of formation of the composite material were deduced from the measurements. The latter could be related to a change of interfacial enthalpies.  相似文献   

12.
We report here the structural and magnetic behaviors of nickel-silver (Ni-Ag) and nickel-iron (Ni-Fe) nanoclusters stabilized with polymer (polypyrrole). High resolution transmission electron microscopy (HRTEM) indicates Ni-Ag nanoclusters to stabilize in core-shell configuration while that of Ni-Fe nanoclusters in a mixed type of geometry. Structural characterizations by X-ray diffraction (XRD) reveal the possibility of alloying in such bimetallic nanoclusters to some extent even at temperatures much lower than that of bulk alloying. Electron paramagnetic resonance (EPR) spectra clearly reveal two different absorption behaviors: one is ascribed to non-isolated Ni2+ clusters surrounded by either silver or iron giving rise to a broad signal, other (very narrow signal) being due to the isolated superparamagnetic Ni2+ clusters or bimetallic alloy nanoclusters. Results obtained for Ni-Ag and Ni-Fe nanoclusters have been further compared with the behavior exhibited by pure Ni nanoclusters in polypyrrole host. Temperature dependent studies (at 300 and 77 K) of EPR parameters, e.g. linewidth, g-value, line shape and signal intensity indicating the significant influence of surrounding paramagnetic silver or ferromagnetic iron within polymer host on the EPR spectra have been presented.  相似文献   

13.
在分析复杂混合物方面原位薄层色谱-红外光谱联用有巨大潜力,二者联用能够相互取长补短,极大地提高对复杂混合物的解析能力。但因固定相自身的红外吸收能够对样品的检测造成干扰,使该方法进展缓慢。实验应用对中红外光透明的碘化银纳米微粒作为固定相制备薄层层析板,并对碘化银薄层板的层析效果及原位红外光谱检测的可行性进行了初步的研究。通过正交设计实验法优化反应条件,制备出粒径为100nm左右的碘化银颗粒;应用沉降-挥发法制备薄层层析板,实验表明该薄层板具备分离混合物的能力,且原位红外光谱检测结果表明碘化银作为固定相不干扰样品检测。  相似文献   

14.
采用传统熔融-淬冷法制备了一系列新型(100-x) (4GeSe2-In2Se3) -xAgI(x=20,30,40 mol%)硫系玻璃样品.利用X射线衍射分析、差热分析、可见-近红外吸收光谱、红外透过光谱、喇曼分析等技术手段研究了该玻璃系统的组成、结构、热稳定性和光学特性等.利用Tauc方程计算出了样品的间接带隙;测试了部分样品在不同升温速率下的差示扫描量热曲线,并采用Kissinger法计算了玻璃样品的析晶活化能.X射线衍射数据表明,该玻璃体系在较宽的组分范围内有良好的非晶特性,成玻范围较宽;差热分析和析晶动力学研究表明,玻璃样品70(4GeSe2-In2Se3)-30AgI具有较好的热稳定性(ΔT=114℃)和较高的活化能(Ea=320.4 kJ/mol).随着AgI含量的增加,玻璃的短波吸收限蓝移,并且光学带隙有增大的趋势.此外,红外透过光谱分析表明该玻璃体系具有良好的红外透过性能,其红外截止波长不会随着AgI含量的增加而发生明显变化,皆为16μm左右.  相似文献   

15.
AgI molecules were dilutely adsorbed into nano-cages of Na+, K+ and Cs+ type FAU zeolites in order to understand the interaction between host zeolite and guest AgI. This interaction was investigated using optical absorption spectroscopy and extended X-ray absorption fine structure (EXAFS). The optical spectra strongly depend on the type of the alkali cations. Compared with the lowest absorption band of AgI molecules in gas phase, the spectra of AgI molecules adsorbed in the zeolite cages shifts to higher energy in the order of Cs+, K+, and Na+. On the contrary, Ag-I bond lengths of adsorbed AgI molecules obtained from EXAFS were independent of the type of the alkali-cations. The bond length was very close to gas phase AgI molecules. Therefore, the interaction between AgI molecules and the zeolite, whose magnitude is Na+ > K+ > Cs+, is important in the photo-excited electronic state.  相似文献   

16.
The pseudopotential calculations of Cohen and Bergstresser on the zinc-blende structures of Sn, InSb and CdTe, are extended to the I–VII compound, AgI. The resulting bandstructure for the metastable phase with the zinc-blende structure, denoted γ-AgI, is found to be in good agreement with that derived by a previous tight-binding calculation.The same pseudopotential form factors are used to calculate the bandstructure for β-AgI which is the stable low temperature phase having the wurtzite structure. This bandstructure is shown to be consistent with the predictions of the earlier tight-binding analysis.Taken together, these bandstructures and pseudopotential form factors provide a suitable basis for calculating the electronic properties of these two silver iodide polytypes.  相似文献   

17.

We report about recent X-ray absorption spectroscopy (XAS) measurements on solid and liquid AgI under high pressure. The structural behaviour of AgI has been investigated to pressures P~4.3 GPa at room temperature and to P~1.8 GPa at 1100 K. The high temperature/high pressure conditions have been obtained by means of a large-volume press of the Paris-Edinburgh type, coupled with a 10 mm boron/epoxy biconical gasket. The absorption spectra have been collected in transmission mode, both at the K-edge of Ag and I, and the samples have been characterized in situ by energy scanning X-ray diffraction at fixed angles. Our XAS results for solid AgI are compatible with previous X-ray diffraction measurements. For liquid AgI, we observe a slight change in the intensity and a shift in the frequency of the XAS oscillations with respect to what obtained in the case of the ambient pressure liquid.  相似文献   

18.
Hollow spheres of AgI with an average radius of 100-200 nm have been prepared by a simple reaction between AgBr suspension and KI in the presence of gelatin. Gelatin played a decisive role as an inhibitor of the direct attack of I ions to AgBr surfaces and coagulation of the growing AgI in producing the spherical AgI particles. The products were characterized by X-ray powder diffraction, transmission electron microscopy, UV-vis absorption spectroscopy and X-ray photoelectron spectra techniques. The band gaps are estimated to be 2.95 eV according to the results of optical measurements of the hollow spheres of AgI.  相似文献   

19.
CdS clusters were synthesized in A type zeolite by reaction in alkaline aqueous solution at temperatures from 30 to 70 °C. The optical properties of the samples were studied by diffuse reflectance and photoluminescence spectroscopy. Their crystalline structure and morphology were studied by X-ray diffraction and by transmission and scanning electron microscopy. We found that at lower temperatures the CdS clusters are encapsulated in the zeolite cages. We compared the properties of these clusters with those encapsulated in the cages of zeolites X and Y, prepared by similar methods. CdS clusters smaller than the CdS exciton diameter are also formed outside the cages in the zeolite matrix. The size of these clusters increases with temperature producing a red-shift of the absorption edge in the optical absorption spectra.  相似文献   

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