超分子測試方法總結(jié)

1、 總 結(jié)超分子材料分析測試方法現(xiàn)代儀器分析方法組成分析結(jié)構(gòu)分析無機元素分析有機元素分析晶體材料分析有機材料分析 AAS ICP有機有機元素分析儀元素分析儀(CHNOS) XRD SCD 四大光譜四大光譜現(xiàn)代儀器分析方法形貌分析SEMTEMAFM 冷場SEM W燈絲、LaB6 SEMHRTEMSTEMFE-SEM 熱場SEMTEM選取電子衍射像（選取電子衍射像（SAEDSAED）高分辨像（晶格條文）高分辨像（晶格條文）形貌像（低倍，高倍）形貌像（低倍，高倍）EDSEDS二次電子像（低倍，高倍）二次電子像（低倍，高倍）背散射電子像（相貌、組成分析）背散射電子像（相貌、組成分析）EDSEDS（譜、點

2、掃、線掃及面掃）（譜、點掃、線掃及面掃）納米粒子成像納米粒子成像表面平整表面平整不需噴金不需噴金與XPS區(qū)別？X X射線光電子能譜射線光電子能譜（ XPSXPS ，全稱為，全稱為X-ray Photoelectron Spectroscopy）定義：是一種基于光電效應(yīng)的電子能譜，它是利用X射線光子激發(fā)出物質(zhì)表面原子的內(nèi)層電子，通過對這些電子進行能量分析而獲得的一種能譜。XPS的最大特色：在于能獲取豐富的化學信息,對樣品表面的損傷最輕微,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含有化學信息,它也通常被稱為化學分析電子能譜 （ ESCA，全稱為

3、Electron Spectroscopy for Chemical Analysis），XPS的更高級應(yīng)用可得到關(guān)于表面的化學組成和形成的更詳細的信息。XPS，EDS有哪些區(qū)別呢?項目EDSXPS入射源電子源X射線原理能量散射X射線譜是電子束和樣品作用，原子的電子發(fā)生躍遷，有能量差作為特征X射線放出。X光電子能譜是通過X射線的光子攜帶的能量給原子的電子能量電離，原子成為離子狀態(tài)。深度100nm5nm左右 表面分析內(nèi)容元素組成元素組成 價態(tài)變化范圍探測Z大于5的元素探測Z大于5的元素 分析除氫和氦以外的元素 Ag/ZnO heterostructure nanocatalysts with A

4、g 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 nanocatalyst is investigated by EDX mapping and XPS techni

5、ques. 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 on the dispersity of metallic Ag in Ag/ZnO nanocataly

6、st; 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 PropertyPhotocatalytic Activity of Ag/ZnO Heterostructur

7、e Nanocatalyst: Correlation between Structure and PropertyFigure 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 rectangular region of the as-synthesized samples in a-c. The

8、 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 nanocrystal373.2 eV367.2 eVbulk Ag Ag 3d5/2, 368.3 eVAg 3d3/2, 374.3 eVAg ZnOeThe shift of the binding energy of metall

9、ic Ag indicates that there is a strong interaction between metallic Ag and ZnO nanocrystalsAccording to the EDX mapping and XPS results, this phenomenon should be attributed to the highest dispersity of metallic Ag on the surface of ZnO nanocrystals for Ag/ZnO-DP sample.Figure 3. Ag 3d XPS spectra o

10、f 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 theas-synthesized Ag/ZnO heterostructure nanocrystals.The appearance of two kinds of characteristic absorption bandsalso confirms that the as-synthesized sampl

11、es are composed ofzerovalent 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 thephotograph of the as-synthesized samples dispersed in MO solution(the concentration of the catalysts is 1.25 mg/mL).TEM and HRTEM im

12、ages 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 atmosphere.Characterization of ZnO needle-shaped nanostructures grownon

13、NiO catalyst-coated Si substratesTEM 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 coating of ZnO nanorods by atomic layer depositionHRTEM image of a nanowire. T

14、he 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 interplanar separation of 0.30 nm corresponds to the 222 direction.SAED

15、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 nanocrystStructural characterization of ZnO/Er2O3 core/shell nanowiresControlled Growth and Characterization of Tungsten Oxide Nanowires Usin

16、g Thermal Evaporation of WO3 PowderSEM images of WO3 nanowires grown on tungsten substrate: (a, b) top views, (c) tilt view, and (d) EDX spectrum of the nanowire sampleFigure 3. (a) HRTEM image of WO3 nanowire. Insets (b, c) areenlargement HRTEMs from squares in (a). (d) Diffraction pattern oftungst

17、en oxide nanowires.It shows a single nanowire with a diameter of 70 nm that exhibitsa well-defined lattice fringe separation with 0.38 nm correspondingto 001 planes of a monoclinic WO3 crystal (JCPDS Card No. 75-2072).Figure 4. XRD profile of WO3 nanowires.The main peaks can be well indexed to be a

18、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 SAEDanalysis.Figure 5. XPS profiles of WO3 nanowires. (a)W4f peaks: the doublet 4f7/2 and 4f5/2, at binding energies of 35.5 and 37.5 eV, respe

19、ctively, 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 of the tungsten equal to +6 and the other peak at 532.2 eV corresponding to residual wa

20、ter bound in the nanowire structure or adsorbed on the surface.Figure 6. Evolution of W 4f spectra for thermal annealed WO3nanowires in the temperature range of 900-1100 C in a vacuum.The effects of the growth temperature on the oxidation states of the tungsten oxide nanowires were studied by XPS. T

21、he 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 corr

22、esponds 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 products.Raman measurements were performed since this technique is well-known to give the “fingerprint” of the WO3 chemical structure. It was found that the phonon activity may be grouped in a set of two ranges: high in the 600-900 cm-1region and low in the 200-400 cm-1 region (Figure 7). The four peaks obtained in the Raman spectrum of the WO3 nanowi