X射线辐照合成金纳米颗粒及其原位表征

X射线辐照合成无机纳米粒子具有简单、清洁、高效等优点,是一种绿色合成方法.X射线技术,如X射线光电子能谱(XPS)、X射线吸收精细结构谱(XAFS)等,特别是同步辐射X射线技术的应用和发展,为人们探索纳米材料的结构信息提供了强大的工具.然而,利用X射线辐照合成金纳米颗粒及利用X射线技术原位探索金纳米颗粒的生长机理的综述...     

MeV碳离子及碳团簇C2+注入PC膜的光吸收谱研究

研究了MeV碳离子及碳团簇C2 注入的聚碳酸酯(Polycarbonate,PC)膜.光吸收谱研究结果表明,离子注入在聚合物近表面产生了断键及缺陷,改变了PC的光吸收性质,在可见光区域有较明显的吸收,并且吸收边与注入离子的种类、能量和注量密切相关.X射线光电子谱(X-ray photoelectron spectroscopy,XPS)对PC的近表面结构和成分配比进行了分析,证实了以上的结论.     

元素在长石、云母、角闪石表面吸附的XPS研究Ⅰ.铯、锶、铕、铈

用X射线光电子能谱(XPS)初步研究了Cs,Sr,Eu,Ce在长石、云母、角闪石表面的吸附行为。通过观察矿物中氧结合能谱的化学位移,对吸附机理进行了初步探讨。     

非晶Fe-Zr-B薄膜穆斯堡尔谱学研究

用X射线衍射分析、X射线光电子能谱(XPS)和穆斯堡尔谱学研究了直流磁控溅射法制备的Fe-Zr-B薄膜。X射线衍射分析结果表明制备态的薄膜是非晶的;X射线光电子能谱(XPS)结果表明样品表面氧化较明显,深层部分Fe, Zr, B结合占主导地位;穆斯堡尔谱学结果表明薄膜中Fe原子周围Zr、B原子的存在使Fe原子核内场值有所下降并导致超精细场分布P(H)出现双峰结构,薄膜中存在两种不同的局域微结构。     

双酚A型聚砜X射线致发降解的X射线光电子能谱研究

利用X射线光电子能谱(XPS)研究了双酚A型聚砜薄膜在超高真空下X射线辐照所引起的表面化学组成变化。结果表明:(1)聚砜在X射线辐照下,部分砜基团变成了硫化物。(2)硫化物的生成量取决于辐照时间。(3)在XPS的取样深度里,同一辐照时间下,X射线致发降解的程度基本上是均匀的。     

动态离子束混合技术制备氧化铬薄膜的X射线光电子能谱与俄歇电子能谱研究

本文介绍的动态离子束混合技术制备氧化铬薄膜系在不锈钢基体上进行1keV氩离子束溅射沉积铬(同时通入一定量的O),并用100 keV的氩离子束或氧离子束轰击该样品.对两种离子束轰击形成的氧化铬薄膜进行了X射线光电子能谱(X-ray photoelectron spectroscopy,XPS)和俄歇电子能谱(Auger electron spectroscopy,AES)的分析研究.发现Ar 离子束制备的氧化铬薄膜主要是Cr2O3化合物,而O 离子束制备的氧化铬薄膜含有其它价态的铬氧化物.Ar 离子束制备氧化铬薄膜的污染碳少于O 离子束制备.与O 离子束制备相比较,相同能量的Ar 离子束轰击更有利于提高沉积的Cr原子与周围O2的反应性;Ar 离子束制备的氧化铬薄膜过渡层的厚1/3左右,较厚的过渡层显示了制备的薄膜具有较好的附着力.     

团簇沉积C-N薄膜的研究

利用荷能团族沉积装置在高阻硅（111）衬底上沉积了碳氮薄膜。通过红外光谱、拉曼谱和X光电子能谱对薄膜的结构和化学组分进行了分析。结果表明,薄膜中存在N－sp^3(β－C3N4的键合方式）,但以N－^2C和C＝C双键的结合方式为主。     

Ti/Mo膜的X射线光电子能谱分析

利用X射线光电子谱仪(XPS)分析和Ar 刻蚀相结合的方法,分析了Ti膜表面的化学元素及相应原子的电子结合能.分析结果表明:Ti膜及膜材料样品表面有大量的C、O元素;膜表面存在从衬底扩散至Ti膜的Mo元素.对样品刻蚀后Ti 2p的XPS谱进行拟合表明:Ti膜表面的Ti由TiO2(约100%)和单质Ti组成,随刻蚀时间的增加,部分TiO2还原至低价Ti;薄的薄膜表面中的Mo由单质Mo和MoO3组成,而厚的薄膜以单质Mo为主;表面C由石墨态和结合能为288.2～288.9 eV的碳化物组成.     

SR-XRD和EXAFS研究Mn掺杂ZnO薄膜的微观结构

用射频磁控溅射技术在蓝宝石衬底上制备了一组不同衬底温度的Mn掺杂ZnO薄膜。质子激发X射线荧光(PIXE)测量表明,薄膜中仅有含量为5 at.%的Mn,未见其它磁性杂质元素(如Fe、Co、Ni等)。同步辐射X射线衍射(SR-XRD)表明,这些Mn掺杂ZnO薄膜具有纤锌矿ZnO结构。SR-XRD和扩展X射线吸收精细结构谱(EXAFS)分析显示,薄膜中未发现Mn团簇或MnO、MnO2、Mn2O3、Mn3O4等二次相,Mn原子是通过替代Zn原子而进入了ZnO晶格。     

北京同步辐射装置3B3光束线吸收谱测量及装置设计

介绍了在北京同步辐射装置(BSRF)3B3中能光束线(1.2～6.0keV)进行X射线吸收谱(XAS)的简易装置,并利用透射法对低原子序数元素(S、P、Cl、Ca、Al、Mg等)进行X射线吸收谱测量,分析结果表明在3B3中能X射线能区开展吸收谱学研究工作是可行的.根据计算X射线吸收谱信号的结果,设备设计满足测量要求,一套包含3种X射线吸收谱测量方式(透射法、荧光法和电子产额法)的精密设备正在建设,将有利于中等能区X射线谱学研究工作的广泛开展.     

Influence of N2 flow rate on structure and properties of TiBCN films prepared by multi-cathodic arc ion plating and studied with ion beam scattering spectroscopy

TiBCN films were deposited on Si(100) and cemented carbide substrates by using multi-cathodic arc ion plating in C_2H_2 and N_2atmosp~here. Their structure and mechanical properties were studied systematically under different N_2 flow rates. The results showed that the Ti BCN films were adhered well to the substrates. Rutherford backscattering sp~ectroscopy was employed to determine the relative concentration of Ti, B, C and N in the films.The chemical bonding states of the films were explored by X-ray photoelectron sp~ectroscopy, revealing the presence of bonds of Ti N, Ti(C,N), BN, pure B, sp~2C–C and sp~3C–C, which changed with the N_2 flow rate. Ti BCN films contain nanocrystals of Ti N/Ti CN and Ti B_2/Ti(B,C)embedded in an amorphous matrix consisting of amorphous BN and carbon at N_2 flow rate of up to 250 sccm.     

氢气流量对类金刚石薄膜结构与性能的影响

采用直流/射频耦合反应磁控溅射法在Si（100）衬底上成功制备出类金刚石（DLC）薄膜。利用表面轮廓仪、Raman光谱仪、X射线光电子能谱仪表征所制备薄膜在不同氢气流量下的沉积速率和化学结构,讨论了氢气流量对薄膜沉积速率和化学结构的影响;利用纳米压痕技术及曲率弯曲法表征薄膜的力学性能;利用扫描电镜和原子力显微镜表征薄膜的表面形貌与粗糙度。研究表明：随着氢气流量的增加,所制备薄膜的沉积速率逐渐减小,而薄膜中sp³键的含量逐渐增大。当氢气流量为25 mL/min时,薄膜中sp³键的含量为36.3%,薄膜的硬度和体弹性模量分别达到最大值17.5 GPa和137 GPa。同时,所制备薄膜的内应力均低于0.5 GPa,有望成功制备出低内应力的高质量DLC厚膜。随着氢气流量的增加,DLC薄膜的表面变得更致密光滑,且表面均方根粗糙度由5.40 nm降为1.46 nm。     

高质量类金刚石薄膜的制备与性能分析

采用直流/射频耦合磁控溅射法在Si(100)衬底上成功制备出类金刚石(DLC)薄膜。利用Raman光谱仪、X射线光电子能谱仪表征不同射频功率下所制备薄膜的化学结构,讨论射频功率对薄膜化学结构的影响。采用X射线小角反射法表征薄膜的质量密度,利用曲率弯曲法表征薄膜的残余内应力,采用扫描电镜和原子力显微镜表征所制备薄膜的表面形貌与粗糙度。研究表明:薄膜中sp3键的含量随着射频功率的增加而呈现出先增大后减小的趋势,且在射频功率为40 W时达到最大值45.6%。随着射频功率的增加,薄膜的表面粗糙度呈现出先减小后增大的趋势,当射频功率为40 W时薄膜的表面粗糙度最小,为1.6 nm。直流/射频耦合磁控溅射法在不同射频功率下制备出的薄膜,其内应力均低于1.0 GPa,薄膜质量密度的变化范围为2.26~2.44 g/cm~3,有望成功制备出内应力低、密度高的高质量DLC薄膜。     

Effect of Fe ion implantation on tribological properties and Raman spectra characteristics of diamond-like carbon film

1 Introduction It is well known that DLC (diamond-like carbon)prepared by physical vapor deposition, plasma en-hanced chemical vapor deposition (PECVD) and otherplasma processing is an amorphous carbon materialcontaining sp2 and sp3 bonded carbon atoms. DLCfilm possesses some interesting properties, such ashigh hardness and Young's modulus, chemical inert-ness and low friction coefficient. The property andstructure of DLC film can be modified by addingsome metals. Ion implantation…     

软X射线磁性圆二色光束线的调试和实验

合肥国家同步辐射实验室二期工程建立了基于软X射线吸收的光束线和实验站。光束线采用了平面变线距光栅单色器,可以提供100—1000eV的单色光,在1000eV处当分辨本领为1000时,光子通量可以超过108s-1。光束线的焦点尺寸是3mm×1mm。在该设备上已经获得软X射线磁性圆二色吸收谱和C、N、O的K吸收边的近边吸收谱。     

Surface chemistry analysis of lithium conditioned NSTX graphite tiles correlated to plasma performance

Lithium wall conditioning in NSTX has resulted in reduced divertor recycling, improved energy confinement, and reduced frequency of edge-localized modes (ELMs), up to the point of complete ELM suppression. NSTX tiles were removed from the vessel following the 2008 campaign and subsequently analyzed using X-ray photoelectron spectroscopy as well as nuclear reaction ion beam analysis. In this paper we relate surface chemistry to deuterium retention/recycling, develop methods for cleaning of passivated NSTX tiles, and explore a method to effectively extract bound deuterium from lithiated graphite. Li–O–D and Li–C–D complexes characteristic of deuterium retention that form during NSTX operations are revealed by sputter cleaning and heating. Heating to ～850 °C desorbed all deuterium complexes observed in the O 1s and C 1s photoelectron energy ranges. Tile locations within approximately ±2.5 cm of the lower vertical/horizontal divertor corner appear to have unused LiO bonds that are not saturated with deuterium, whereas locations immediately outboard of this region indicate high deuterium recycling. X-ray photo electron spectra of a specific NSTX tile with wide ranging lithium coverage indicate that a minimum lithium dose, 100–500 nm equivalent thickness, is required for effective deuterium retention. This threshold is suspected to be highly sensitive to surface morphology. The present analysis may explain why plasma discharges in NSTX continue to benefit from lithium coating thickness beyond the divertor deuterium ion implantation depth, which is nominally <10 nm.     

铀铌合金在O_2气氛中氧化初期的XPS研究

采用X射线光电子能谱 (XPS)分析研究了 2 98K时铀铌合金的清洁表面在O2 气氛中的原位氧化过程。通过分析反应各阶段U4f ,Nb3d和O1s谱峰的变化 ,揭示了O2 在铀铌合金表面吸附解离后 ,优先与表面Nb原子和U原子结合生成NbO、UO2 -x和UO2 ,然后NbO进一步氧化为NbO2 和Nb2 O5,在氧化的不同阶段U和Nb分别向表面偏析     

Synthesis and Characteristics of Diamond-like Carbon Films Deposited on Quartz Substrate

Diamond-like carbon (DLC) fihns are deposited on quartz substrate using pure CH4 in the surface wave plasma equipment. A direct current negative bias up to -90 V is applied to the substrate to investigate the bias effect on the film characteristics. Deposited films are characterized by Raman spectroscopy, infrared (IR) and ultraviolet-visible absorption techniques. There are two broad Raman peaks around 1340 cm^-1 and 1600 cm^-1 and the first one has a greater sp^3 component with an increased bias. Infrared spectroscopy has three sp^3 C-H modes at 2852 cm^-1, 2926 cm^-1 and 2962 cm^-1, respectively and also shows an intensity increase with the negative bias. Optical band gap is calculated from the ultraviolet-visible absorption spectroscopy and the increased values with negative bias and deposition time are obtained. After a thermal anneal at about 500℃ for an hour to the film deposited under the bias of-90 V, we get an almost unchanged Raman spectrum and a peak intensity-reduced IR signal, which indicates a reduced H-content in the film. Meanwhile the optical band gap changed from 0.85 eV to 1.5 eV.     

类金刚石碳剥离膜的制备及其性能研究

采用磁过滤阴极真空弧(FCVA)技术制备了质量厚度为5~7μg/cm2的类金刚石碳(DLC)剥离膜。用XP2U型精密电子天平测试分析了100mm范围内的DLC剥离膜均匀性,结果显示其最大不均匀性小于10%。通过扫描电子显微镜(SEM)、原子力显微镜(AFM)、万能摩擦磨损试验机和X光电子谱(XPS)测试分析了DLC剥离膜的表面形貌、耐磨损特性和结构,结果显示采用双90°FCVA技术沉积的DLC剥离膜表面光滑致密、耐磨,几乎没有大颗粒的污染,表征金刚石特性的sp3键含量超过70%。在北京HI-13串列加速器上使用107 Ag-、70 Ge-、48 Ti-、28Si-、197 Au-和127I-六种典型质量的离子束对质量厚度为5~7μg/cm2的DLC剥离膜和碳剥离膜寿命进行测试比较,结果显示DLC剥离膜寿命比碳剥离膜的高2.6~10倍。