超分子测试方法总结.ppt

1、总 结,超分子材料分析测试方法,现代仪器分析方法,组成分析,结构分析,无机元素分析,有机元素分析,晶体材料分析,有机材料分析,AAS,ICP,有机元素分析仪(CHNOS),XRD,SCD,四大光谱,现代仪器分析方法,形貌分析,SEM,TEM,AFM,冷场SEM,W灯丝、LaB6 SEM,HRTEM,STEM,FE-SEM,热场SEM,TEM,选取电子衍射像（SAED） 高分辨像（晶格条文） 形貌像（低倍，高倍） EDS,二次电子像（低倍，高倍） 背散射电子像（相貌、组成分析） EDS（谱、点扫、线扫及面扫）,纳米粒子成像 表面平整 不需喷金,与XPS区别？,X射线光电子能谱 （ XPS ，全称

2、为X-ray Photoelectron Spectroscopy）,定义： 是一种基于光电效应的电子能谱，它是利用X射线光子激发出物质表面原子的内层电子，通过对这些电子进行能量分析而获得的一种能谱。,XPS的最大特色： 在于能获取丰富的化学信息,对样品表面的损伤最轻微,表面的最基本XPS分析可提供表面存在的所有元素(除H和He外)的定性和定量信息。,正是由于XPS含有化学信息,它也通常被称为化学分析电子能谱 （ ESCA，全称为Electron Spectroscopy for Chemical Analysis），XPS的更高级应用可得到关于表面的化学组成和形成的更详细的信息。,XPS，E

3、DS有哪些区别呢?,Ag/ZnO heterostructure nanocatalysts with Ag content of 1 wt % are successfully prepared through three different simple methods, where chemical reduction and photolysis reaction are adopted to fabricate the heterostructure. The dispersity of Ag clusters and/or nanoparticles in Ag/ZnO nanoc

4、atalyst is investigated by EDX mapping and XPS techniques. The experimental results show that deposition-precipitation is an efficient method to synthesize Ag/ZnO nanocatalyst with highly dispersed Ag clusters and/or nanoparticles; the photocatalytic activity of Ag/ZnO photocatalysts mainly depends

5、on the dispersity of metallic Ag in Ag/ZnO nanocatalyst; the higher the dispersity of metallic Ag in Ag/ZnO nanocatalyst is, the higher the photocatalytic activity of Ag/ZnO photocatalyst should be.,Photocatalytic Activity of Ag/ZnO Heterostructure Nanocatalyst: Correlation between Structure and Pro

6、perty,Photocatalytic Activity of Ag/ZnO Heterostructure Nanocatalyst: Correlation between Structure and Property,Figure 2. Low-magnification SEM images and EDX mapping of the as-synthesized samples: (a) Ag/ZnO-DP, (b) Ag/ZnO-CP and (c) Ag/ZnOST; (d) EDXS spectra recorded from the corresponding recta

7、ngular region of the as-synthesized samples in a-c. The coverage of blue color in a-c reflects Ag distributions in the as-synthesized samples, and the inset in a and c is the corresponding HRTEM image of a single Ag/ZnO heterostructure nanocrystal,373.2 eV,367.2 eV,bulk Ag Ag 3d5/2, 368.3 eV Ag 3d3/

8、2, 374.3 eV,The shift of the binding energy of metallic Ag indicates that there is a strong interaction between metallic Ag and ZnO nanocrystals,According to the EDX mapping and XPS results, this phenomenon should be attributed to the highest dispersity of metallic Ag on the surface of ZnO nanocryst

9、als for Ag/ZnO-DP sample.,Figure 3. Ag 3d XPS spectra of the as-synthesized samples: (a) Ag/ ZnO-DP, (b) Ag/ZnO-CP, and (c) Ag/ZnO-ST.,Figure 4. (a) UV-vis diffuse-reflectance and (b) PL spectra of the as-synthesized Ag/ZnO heterostructure nanocrystals.,The appearance of two kinds of characteristic

10、absorption bands also confirms that the as-synthesized samples are composed of zerovalent Ag and ZnO.,Figure 5. Photodegradation of MO by the as-synthesized samples: (a) Ag/ZnO-DP, (b) Ag/ZnO-CP, and (c) Ag/ZnO-ST. The inset is the photograph of the as-synthesized samples dispersed in MO solution (t

11、he concentration of the catalysts is 1.25 mg/mL).,TEM and HRTEM images for the grown ZnO nano-needle.,FE-SEM images for the nanostructures grown on silicon substrate. ZnO grown for: (a) 30 min, (b) 60 min, (c) 180 min, and (d) ZnO nano-needles after annealing for 180 min at 500 C only under N2 atmos

12、phere.,Characterization of ZnO needle-shaped nanostructures grown on NiO catalyst-coated Si substrates,TEM image of an Al2O3-deposited ZnO nanorod. The central part (A) is the ZnO nanorod and the outer part (B) is the deposited Al2O3 layer.,HRTEM image of an Al2O3-deposited ZnO nanorod.,Al2O3 coatin

13、g of ZnO nanorods by atomic layer deposition,HRTEM image of a nanowire. The left part presents interplanar separation of 0.52 nm and consists of a single ZnO crystal. The crystal growth direction 001 is perpendicular to the planes. The small inclusions on the right consist of Er2O3 nanocrystals. The

14、 interplanar separation of 0.30 nm corresponds to the 222 direction.,SAED pattern obtained at the surface of a nanowire. The rectangular pattern is due to the 210 direction in ZnO. The rings are due to different orientations of Er2O3 nanocryst,Structural characterization of ZnO/Er2O3 core/shell nano

15、wires,Controlled Growth and Characterization of Tungsten Oxide Nanowires Using Thermal Evaporation of WO3 Powder,SEM images of WO3 nanowires grown on tungsten substrate: (a, b) top views, (c) tilt view, and (d) EDX spectrum of the nanowire sample,Figure 3. (a) HRTEM image of WO3 nanowire. Insets (b,

16、 c) are enlargement HRTEMs from squares in (a). (d) Diffraction pattern of tungsten oxide nanowires.,It shows a single nanowire with a diameter of 70 nm that exhibits a well-defined lattice fringe separation with 0.38 nm corresponding to 001 planes of a monoclinic WO3 crystal (JCPDS Card No. 75-2072

17、).,Figure 4. XRD profile of WO3 nanowires.,The main peaks can be well indexed to be a monoclinic WO3 phase (JCPDS Card No. 75-2072; a ) 7.274, b ) 7.501, c ) 3.824, and ) 89.930; space group P21/a), which is in good agreement with our TEM and SAED analysis.,Figure 5. XPS profiles of WO3 nanowires. (

18、a)W4f peaks: the doublet 4f7/2 and 4f5/2, at binding energies of 35.5 and 37.5 eV, respectively, and the two fitted doublets representing the different oxidation states of W (green line, W6+; blue line, W5+) for specimen grown at 1000C. (b) O 1s peaks: a peak at 530.5 eV corresponding to the valence

19、 of the tungsten equal to +6 and the other peak at 532.2 eV corresponding to residual water bound in the nanowire structure or adsorbed on the surface.,Figure 6. Evolution of W 4f spectra for thermal annealed WO3 nanowires in the temperature range of 900-1100 C in a vacuum.,The effects of the growth

20、 temperature on the oxidation states of the tungsten oxide nanowires were studied by XPS. The shape of the W 4f peaks changes at different temperatures (Figure 6). The W 4f peak of samples annealed at 1000-1100 C shows a stoichiometric feature of WO3. However, for samples annealed at 900 C, the peak becomes broader and a shoulder forms at the higher binding energy side. This shoulder corresponds to lower oxidation state of 2 in the x of WOx structure. These results indicate that, at high growth temperatures, WO2 readily transforms into WO3.,Figure 7. Raman spectrum of as-synthesized produc