PIIID复合强化处理轴承钢表面TiN膜层的XPS表征

用等离子体浸没离子注入与沉积(PIIID)复合强化新技术在AISI52100轴承钢基体表面成功合成了硬而耐磨的氮化钛薄膜。膜层表面的化学组成和相结构分别用X射线衍射(XRD)和X射线光电子能谱(XPS)表征;膜层表面的原子力显微镜(AFM)形貌显示出TiN膜结晶完整,结构致密均匀。XRD测试结果表明,TiN在(200)晶面衍射峰最强,具有择优取向。Ti(2p)的XPS谱峰泰勒拟合分析揭示出,Ti(2p_1/2)峰和Ti_2p3/2峰均有双峰出现,表明氮化物中的Ti至少存在不同的化学状态;N(1s)的XPS谱峰在396.51, 397.22和399.01 eV附近出现了三个分峰,分别对应于TiNO_y,TiN和N—N键中的氮原子。结合O(1s)的XPS结果,证实膜层中除生成有稳定的TiN相外,还有少量钛的氧化物和未参与反应的单质氮。整个膜层是由TiN,TiO₂,Ti—O—N化合物和少量单质氮组成的复合体系。     

傅里叶变换红外光谱在胃癌淋巴结转移诊断中的应用研究

观察傅里叶变换红外光谱技术无创、原位、快速诊断胃癌淋巴结转移的可行性。联合使用衰减全反射探头及傅里叶变换红外光谱仪测量新鲜离体胃周淋巴结红外光谱,发现每条光谱在吸收波长3 000～1 000 cm-1之间循序出现13条谱带,依据病理检测结果将淋巴结分为转移组及非转移组,比较两组淋巴结红外光谱的峰位和相对峰强等指标结果,最后进行标准统计学分析。36例胃癌患者,共检测淋巴结720枚,其中转移性淋巴结180枚,未转移540枚;与非转移淋巴结相比,转移淋巴结红外光谱有如下特征：(1)与核酸相关的峰强比I_{1 240}/I_{1 460}(p=0.015)和I_{1 080}/I_{1 460}(p=0.034)显著升高,提示转移淋巴结细胞的核酸含量增多;(2)与蛋白相关的I_{1 640}/I_{1 460}(p=0.001)和I_{1 546}/I_{1 460}(p=0.027)峰强比值升高,表明转移淋巴结组织的蛋白质含量明显升高;(3)与脂类相关的I_{2 855}/I_{1 460}和I_{1 740}/I_{1 460}显著降低(p＜0.001),提示癌组织脂类含量相对减少;(4)I_{1 160}/I_{1 460}(p=0.023)显著降低,表明恶性细胞糖类物质的减少。研究结果显示,傅里叶变换红外光谱分析技术有望成为术中原位、在体和快速诊断胃癌淋巴结转移的新方法。     

磁控溅射法制备金团簇纳米颗粒及性能表征

 采用磁控溅射法制备金团簇纳米颗粒，用透射电镜(TEM)、X射线衍射(XRD)、紫外可见光分光光度计(UV-Vis)和X射线光电子能谱(XPS)等分析手段对其表征，研究了金团簇纳米颗粒的形貌、颗粒度、结构、光吸收性质及物质成份。研究结果表明：制备的金团簇纳米颗粒呈球形，平均粒径在10 nm左右，粒径分布均匀，无团聚、氧化现象，颗粒的结构为面心立方。在519 nm处出现团簇颗粒的表面等离子共振吸收峰，测试得到Au(4f_7/2)和Au(4f_5/2)电子的结合能分别为83.3 eV和86.9 eV，并且没有出现金的氧化产物。     

TRPO萃淋树脂从碱性氰化液中固相萃取Au(Ⅰ)机理研究

研究了TRPO-D3520萃淋树脂从碱性氰化液中固相萃取Au(CN)-₂的性能,并借助傅里叶变换红外光谱(FTIR)、X射线光电子能谱(XPS)和扫描电镜(SEM)等方法对固相萃取Au(Ⅰ)的机理进行了讨论。结果表明：阳离子表面活性剂CTMAB在固相萃取中起到了关键的作用,当待萃水相中加入的CTMAB与Au(CN)-₂的摩尔比达到1∶1时,TRPO-D3520萃淋树脂即对金具有良好的萃取性能;萃淋树脂负载金后,FTIR分析表明Au(CN)-₂中的C≡N伸缩振动吸收峰位于2 144 cm-1,TRPO中的PO伸缩振动峰由1 153 cm-1向低频移至1 150 cm-1;N(1s),Au(4f_7/2)和Au(4f_5/2)XPS谱揭示了树脂中金的价态和配位环境未发生变化,仍以Au(CN)-₂形态存在于萃淋树脂中;O(1s) XPS谱图表明,经固相萃取后,树脂中化学结合水的含量明显增加,化学结合水的峰面积由30.74%增加至42.34%;固相萃取后,P(2p)XPS谱图峰位由132.15 eV增加至132.45 eV,说明PO基团与水分子存在一定的氢键作用,生成P=O…H—O—H。综上可推测,TRPO-D3520树脂固相萃取Au(CN)-₂的过程为：离子对扩散至树脂孔内,被孔内的TRPO借助水分子为桥的氢键作用溶剂化而固相萃取。     

Cu2+掺杂ZnAl2 O4纳米颗粒的光学性能

采用水热法和热处理技术制备了不同掺杂比例的Zn_(1-x)Cu_xAl_2O_4(x=0,0.05,0.10,0.15,0.20)纳米颗粒,通过X射线衍射(XRD)、场发射透射电子显微镜(FETEM)、傅里叶红外光谱(FT-IR)、X射线光电子能谱(XPS)、光致发光光谱(PL)和紫外可见光谱(UV-Vis)对样品的晶体结构、形貌、元素分布、结合能和光学性能进行表征,并通过第一性原理计算得到了ZnAl_2O_4结构中存在的各种缺陷的能带结构。实验结果表明本方法制备的Zn_(1-x)Cu_xAl_2O_4纳米颗粒为尖晶石结构,XPS能谱说明Zn_(0.9)Cu_(0.10)Al_2O_4样品中Cu~(2+)全部占据了四面体位置,PL光谱显示Cu~(2+)掺杂的样品出现了猝灭现象,紫外光谱表明Cu~(2+)掺杂后样品出现了新的吸收峰。并结合第一性原理计算对样品的光学性质给出了合理解释。     

退火及溅射气氛对氮化硅薄膜光致发光的影响

利用射频磁控反应溅射方法制备富硅的氮化硅薄膜。衬底材料为抛光的硅片,靶材为硅靶,在Ar-N₂气环境下,通过改变两种气体的组分比来改变样品成分,并在高纯N₂气氛下对其进行高温退火处理。用X射线光电子能谱(XPS)和X射线衍射(XRD)对样品进行了表征,并测试了样品的光致发光谱 (PL)。实验结果表明：X射线光电子能谱中出现了Si—N键合结构,同时还有少量的Si—O键生成,通过计算得出Si/N比值约为1.51,制备出了富硅的氮化硅薄膜;薄膜未经退火前,在可见光区域没有观察到明显的光致发光峰,经过高温退火后,XRD中新出现的衍射峰证实了纳米硅团簇的生成,PL图谱中在可见光区域出现了光致发光峰的蓝移现象,结合XRD结果,用纳米晶的量子限域效应对上述现象进行了合理解释。     

基于MEH-PPV/ZnSe纳米复合器件的电致发光特性的研究

以巯基乙酸作为稳定剂在水相中制备了ZnSe纳米晶,用X射线粉末衍射(XRD)和X射线光电子能谱(XPS)对其进行了表征。用表面活性剂将ZnSe纳米晶从水相中转移到有机相中,使其与聚合物MEH-PPV复合作为发光层,制备了多层电致发光器件Glass/ITO/MEH-PPV∶ZnSe/BCP/Alq₃。对ZnSe纳米晶和MEH-PPV薄膜的光致发光谱及其吸收光谱的比较表明ZnSe纳米晶和MEH-PPV之间存在着能量传递,这是导致纳米复合薄膜的光致发光光谱和电致发光光谱存在差异的原因之一。文章对其在光激发和载流子注入条件下的不同发光机制进行了讨论。通过对器件的光电特性进行研究,发现ZnSe纳米晶发光的比例随着外加电压的增加而增加,而且器件的I-V特性基本上符合二极管的特性。     

壳聚糖亚胺环钯化合物的合成与表征

用水杨醛接枝改性后的壳聚糖亚胺与Li₂PdCl₄甲醇溶液反应得到壳聚糖环钯化合物。壳聚糖、壳聚糖席夫碱及其钯化合物用红外光谱(IR)、X射线衍射光谱(XRD)、热分析(DTA-TG)、荧光光谱以及X射线光电子能谱(XPS)等分析手段进行了表征分析。根据表征结果提出了席夫碱及壳聚糖亚胺环钯化合物的结构。     

开关式氧化锌量子点荧光探针制备及其特异性检测Cu2+应用

采用溶胶凝胶法制备出一种荧光性能稳定的氧化锌量子点(ZnO-NH2 QDs),并对其进行紫外-可见光谱(UV-Vis)、傅里叶变换红外光谱(FTIR)、X射线衍射(XRD)、透射电子显微镜(TEM)、X射线光电子能谱(XPS)、荧光(PL)表征.基于Cu2+对ZnO-NH2 QDs动态荧光猝灭且Cu2+可与邻苯二胺(O...     

纳米TiO2的表面能态及光生电子-空穴对复合过程的研究

以液相法制备了水溶态纳米TiO2,并通过X射线衍射(XRD)、X射线光电子能谱(XPS)和傅里叶红外光谱仪(FTIR)对纳米TiO2的结构和组成作了细致分析.并对其紫外-可见光谱(UY-Vis spectrum)和荧光发光光谱(PL spectrum)进行了分析.结果发现纳米TiO2呈现较好的锐钛矿型,平均粒径为5 nm.水溶态纳米TiO2由于吸附而在表面形成了Ti-OH和Ti-H2O的表面态,其能级位于其价带以上约0.6和0.54eV;500℃热处理后样品的表面吸附水基本消失,但OH-仍然存在,同时在纳米TiO2晶格中出现了氧空位,其能级位于价带以上3.13 eV.对于水溶态纳米TiO2,表面复合是电子-空穴对的主要复合过程;热处理后的样品,由于表面态遭到破坏,粒子半径变大,直接复合成为电子-空穴对的主要复合过程,同时还伴随有通过氧空位的间接复合和通过Ti-OH的表面复合.     

Solvothermal preparation of nano-β-HgS from a precursor,bis(dibenzyldithiocarbamato)mercury(II)

A simple solvothermal method for the selective synthesis of β-HgS (meta cinnabar) nanoparticles in aqueous solutions is reported with bis(dibenzyldithiocarbamato)mercury(II) as the precursor. Crystal structure, size, morphology and composition of the products are characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX) analysis, high-resolution transmission electron microscopy (HRTEM), SAED and X-ray photoelectron spectroscopy (XPS). PXRD shows (111), (220), (200), (311), (222), (400), (331), (420) reflections characteristic of β-HgS. SEM micrographs display the spherical nature of the nano-β-HgS. EDX analysis showed the presence of Hg and S. HRTEM images indicate the spherical nature of the nanoparticles with their size in the range of 10–15 nm and the FFT pattern shows the crystalline nature of the spherical particles. The results are in agreement with those estimated from the XRD pattern. XPS signals observed at 162.6 and 162.8 eV are due to S2p _3/2 and S2p _1/2 electrons and the S2s was observed at 222.3 eV. The band gap of nano-β-HgS has been found to be 3.6 eV from the UV–visible spectral measurement. The blue-shifted band gap compared to the bulk HgS is a consequence of “size quantization” effect. A comprehensive characterization of the precursor by IR and single crystal X-ray crystallography shows the presence of HgS₄ coordination environment, with a distinct Hg–S bond asymmetry.     

Preparation of indium sulfide thin films by spray pyrolysis using a new precursor indium nitrate

Indium nitrate and thiourea were used as the precursor solutions for preparing indium sulfide thin films using Chemical Spray Pyrolysis (CSP) technique. Films having various In/S ratios were characterized using X-Ray Diffraction (XRD), Energy Dispersive X-ray Analysis (EDX), Scanning Electron Microscopy (SEM), X-ray Photoelectron Spectroscopy (XPS), optical absorption, transmission and photosensitivity measurements. Sample having In/S ratio 2/3 showed better crystallinity with band gap 2.66 eV. Depth profile of the sample also indicated the formation of indium sulfide. It was also observed that In/S ratio in the initial precursor solution determined the composition as well as electrical properties of the films. Maximum photosensitivity was observed for the sample prepared using solution having In/S ratio 2/4.     

Nanoparticles of nickel oxide: growth and organization on zinc-substituted anionic clay matrix by one-pot route at room temperature

A room temperature nanocarving strategy is developed for the fabrication of nanoparticles of nickel oxide on zinc-substituted anionic clay matrix (Ni/ZnLDH). It is based on the growth and organization of nanoparticles of nickel oxide which occur during the structural reconstruction of the layered structure of the anionic clay in NiSO₄ aqueous solution. No organic compounds are used during the fabrication. The described material was characterized by X-ray diffraction (XRD), IR spectroscopy (FTIR), transmission electron microscopy (TEM), field-emission scanning electron microscopy (FESEM), energy dispersive X-ray (EDX) spectroscopy, and X-ray photoelectron spectroscopy (XPS). Results show that the nickel-clay nanoarchitecture consists of small nanoparticles of nickel oxide (average size 7 nm) deposited on the larger nanoparticles (average size 90 nm) of zinc-substituted clay. The optical properties of the new nickel-zinc formulation are studied by UV–Vis.     

NH_3-Ar气氛下制备的Zn_3N_2薄膜的结构和光学性能(英文)

Zn3N2是一种宽带隙半导体材料,在温度高于400°C氧化可生成p型ZnO:N,p型ZnO:N在电子学和光电子学领域有广泛的应用.在NH3-Ar气氛下,用RF磁控溅射金属Zn靶在玻璃衬底上室温制备了Zn3N2薄膜.用紫外-可见分光光度计、X射线衍射仪、X射线光电子谱分析仪、荧光分光光度计对Zn3N2薄膜的光学透过、光学吸收、结构、化学键态和光致发光进行了测量,研究了NH3分压对Zn3N2薄膜的结构和光学特性的影响.XRD分析表明Zn3N2薄膜呈现多晶结构,具有(321)择优取向,Zn3N2(321)衍射峰强度随NH3分压增加而增强.在NH3分压5%～10%制备的Zn3N2薄膜有较低透过率,透过率随NH3分压增加而提高.Zn3N2薄膜是间接带隙半导体,当NH3分压从5%变化到25%时,光学带隙从2.33eV升高到2.70eV.XPS分析表明Zn3N2薄膜在潮湿空气中容易水解.室温下Zn3N2薄膜在437nm和459nm波长出现了发光峰.     

Hydrothermal synthesis of chalcopyrite CuInS2, CuInSe2 and CuInTe2 nanocubes and their characterization

CuInS₂, CuInSe₂ and CuInTe₂ nanocubes of chalcopyrite structure have been successfully synthesized by hydrothermal process using deionized water as solvent at 180 °C for 20 h. The crystallinity, compositional, morphological and optical properties of the synthesized samples were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray (EDX), Raman and photoluminescence (PL) spectra analyses. The Raman spectra of the synthesized CuInS₂, CuInSe₂ and CuInTe₂ samples show the dominant A₁ modes at 293, 172 and 121 cm⁻¹ respectively. The possible chemical reaction and mechanism of nanocubes formation were discussed. The emission wavelength of as synthesized CuInS₂, CuInSe₂ and CuInTe₂ samples were blue shifted at 746 nm (1.66 eV), 863 nm (1.43 eV) and 859 nm (1.44 eV) respectively.     

Synthesis and photoelectric characterization of semiconductor CdSe microrod array by a simple electrochemical synthesis method

It is reported here that the microrod array of CdSe on indium doped tin oxide coated conducting glass (ITO) substrate has been developed by a simple electrochemical synthesis method. The electrodeposition of CdSe was also investigated by cyclic voltammetric technique. The sample was characterized by XRD, EDX, FESEM and UV-vis spectroscopic. The X-ray diffraction investigation demonstrates that the CdSe microrod is a uniform hexagonal CdSe crystal. EDX shows that the high purity CdSe is obtained. Field emission scanning electron microscope (FESEM) results show that the microrods’ length, diameter, and direction of growth are nearly uniform and perpendicular to the ITO substrate. UV-vis absorption spectrum study shows the presence of direct transition with the band gap energy 2.13 eV. Photoelectrochemical solar cells are constructed using CdSe microrod array as the photocathode in polysulphide electrolyte and their power output characteristics are studied.     

Synthesis of nanocrystalline CdS thin film by SILAR and their characterization

Cadmium sulphide (CdS) thin film was prepared by successive ion layer adsorption and reaction (SILAR) technique using ammonium sulphide as anionic precursor. Characterization techniques of XRD, SEM, TEM, FTIR and EDX were utilized to study the microstructure of the films. Structural characterization by x-ray diffraction reveals the polycrystalline nature of the films. Cubic structure is revealed from X-ray diffraction and selected area diffraction (SAD) patterns. The particle size estimated using X-ray line broadening method is approximately 7 nm. Instrumental broadening was taken into account while particle size estimation. TEM shows CdS nanoparticles in the range 5–15 nm. Elemental mapping using EFTEM reveals good stoichiometric composition of CdS. Characteristic stretching vibration mode of CdS was observed in the absorption band of FTIR spectrum. Optical absorption study exhibits a distinct blue shift in band gap energy value of about 2.56 eV which confirms the size quantization.     

Effect of RF power and sputtering pressure on the structural and optical properties of TiO2 thin films prepared by RF magnetron sputtering

TiO₂ thin films were deposited onto quartz substrates by RF magnetron sputtering. The samples deposited at various RF powers and sputtering pressures and post annealed at 873 K, were characterized using X-ray diffraction (XRD), micro Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), UV-vis spectroscopy and photoluminescence (PL) spectroscopy. XRD spectrum indicates that the films are amorphous-like in nature. But micro-Raman analysis shows the presence of anatase phase in all the samples. At low sputtering pressure, increase in RF power favors the formation of rutile phase. Presence of oxygen defects, which can contribute to PL emission is evident in the XPS studies. Surface morphology is much affected by changes in sputtering pressure which is evident in the SEM images. A decrease in optical band gap from 3.65 to 3.58 eV is observed with increase in RF power whereas increase in sputtering pressure results in an increase in optical band gap from 3.58 to 3.75 eV. The blue shift of absorption edge in all the samples compared to that of solid anatase is attributed to quantum size effect. The very low value of extinction coefficient in the range 0.0544-0.1049 indicates the excellent optical quality of the samples. PL spectra of the films showed emissions in the UV and visible regions.     

纳米Zn_2SiO_4∶Mn包覆SiO_2颗粒的制备及表征

采用水热合成方法添加KOH在SiO2颗粒表面包覆Mn2+掺杂纳米Zn2SiO4,通过X射线衍射(XRD)仪、扫描电子显微镜(SEM)、能谱、光致发光(PL)光谱仪对产物的晶体结构、形貌及光学性能进行表征,并对Zn2SiO4晶体在水热反应过程中的反应机制进行了讨论。XRD测试结果表明:220℃水热条件下,添加少量KOH,反应不同时间后,可在石英砂表面生成一层Zn2SiO4;SEM照片显示所生成的Zn2SiO4为六棱柱形,并且不同反应条件下Zn2SiO4的包覆程度不同。反应产物经光致发光性能研究表明:Mn2+掺杂纳米Zn2SiO4包覆SiO2样品中显示两套光致发光谱,一套为250nm左右激发产生的522nm绿色发光带,另一套为340～410nm宽带激发的440nm蓝色发光带,前者为典型的Mn2+离子发光,后者440nm发光带则有可能来源于基体SiO2的氧空位缺陷。     

六硝基菧的紫外光解

采用紫外-可见光谱、X-射线光电子能谱、电子自旋共振谱及质谱等实验手段研究了固态含能材料六硝基菧（HNS）在365 nm紫外光照下的光解机理。HNS的乙腈溶液被紫外光照射后,在310 nm和350 nm处出现了两个新的吸收峰。X-射线光电子能谱实验中,N元素和O元素的窄谱图分别在401 eV和528 eV处出现了新峰。质谱分析则显示在质荷比403和329处出现了两个新的特征离子峰。实验结果表明:CNO2键断裂、分子中NO2基团异构化为亚硝基,以及随后的NO消去等过程均可能发生在六硝基菧的紫外光解反应过程中。