CL-20电子束的X射线光电子能谱-气体质谱原位同步分析技术研究

X射线光电子能谱仪是材料表面元素定性和半定量分析,尤其是元素化学态分析的重要手段之一. X射线光电子能谱仪的分析腔连接质谱仪进行分析,可有效获得样品表面元素变化及气体产物,实现原位同步分析. 基于炸药CL-20在光作用下存在着明显的分解现象,采用X射线光电子能谱-气体质谱同步分析方法(XPS-MS)获得CL-20在电子束作用下的表面元素及气体产物的变化. 试验结果表明,随着辐照时间增加,N、O元素峰峰强迅速下降,同时质谱仪可以有效获得气态产物峰,证实XPS-MS同步分析技术能够有效地实现对固态光降解反应的原位同步追踪.     

原位变温X射线衍射测试技术及其影响因素

在X射线衍射仪中引入加热台,可以实现原位变温X射线衍射分析.原位试验是研究材料在加热或冷却过程中材料动力学的有效手段.对变温X射线衍射测试样品的要求、测量方法的原理、布鲁克D8 advance衍射仪原位变温的测试步骤以及测试过程中样品的收缩问题、背底衍射峰干扰等常见影响因素进行了详细的说明,为变温X射线衍射测试提供了具体的试验指导.     

正负压一体式无空气X射线光电子能谱原位转移仓的开发及研制

针对空气敏感材料的表面分析,为了获得更加真实的表面组成与结构信息,需要提供一个可以保护样品从制备完成到分析表征过程中不接触大气环境的装置.通过使用O圈密封和单向密封柱,提出一种简便且有效的设计概念,自主研制了正负压一体式无空气X射线光电子能谱(XPS)原位转移仓,用于空气敏感材料的XPS测试,利用单向密封柱实现不同工作需求下正负压两种模式的任意切换.通过对空气敏感的金属Li片和CuCl粉末进行XPS分析表明,采用XPS原位转移仓正压和负压模式均可有效避免样品表面接触空气,保证测试结果准确可靠,而且采用正压密封方式转移样品可以提供更长的密封时效性.研制的原位转移仓具有设计小巧、操作简便、成本低、密封效果好的特点,适合给有需求的用户开放使用.     

润滑材料摩擦化学*

外界机械能能够引发的化学反应称为摩擦化学反应。当两个接触的表面进行相对运动时,在界面发生物理和化学变化或反应。润滑材料在服役过程中发生的摩擦化学反应对于其性能的具有正面或负面的影响。通过了解摩擦化学反应机理和反应产物结构及组成,对于理解润滑材料失效机制、性能调控原理具有指导意义。本文针对润滑材料的主要类型：润滑添加剂、纳米添加剂、离子液体、稀土、陶瓷、类金刚石薄膜、有机薄膜、聚合物,综述了近几十年来在相关润滑材料方面开展和取得的摩擦化学研究结果。     

镧－硼复合润滑添加剂的协合润滑机理

实验室和工业试验表明，含镧的润滑添加剂二烷基二硫代磷酸镧（ＬａＤＤＰ）和一种有机硼酸酯（ＯＢ）具有显著的协合润滑作用，将两种化合物复合加至润滑油中，可显著改善油品的抗磨减摩性能。采用俄歇电子能谱（ＡＥＳ）和Ｘ射线光电子能谱（ＸＰＳ）研究其协合润滑机理。结果表明，ＬａＤＤＰ和ＯＢ具有协合润滑作用的主要原因，除了在摩擦表面生成硫酸盐、磷酸盐、氧化镧和单质硼等表面膜起润滑作用外，更重要的是镧的存在对硼的摩擦扩散起到了“摩擦催渗”作用，使摩擦亚表面硼的含量增加，并形成Ｌａ－Ｂ摩擦共渗层，进一步提高材料表面硬度，从而改善耐磨性能     

模拟空间原子氧辐照下X射线光电子能谱仪的原位表征功能开发

对现有的X射线光电子能谱仪进行功能开发,在不改变仪器工作原理、不影响现有功能的前提下,将研制的空间交变温度原子氧辐照装置集成到其快速进样室,重点解决集群结构的匹配和性能兼容问题,实现模拟空间交变温度原子氧辐照环境下材料的原位表征功能.采用Kapton膜的质量损失方法测试空间交变温度原子氧辐照装置的原子氧通量密度,氧气流量、偏压和微波电流均对原子氧通量密度有较大影响.系统测试表明,原子氧辐照使WS 2薄膜表面发生了严重氧化,影响了薄膜的化学组成.不同温度原子氧辐照导致了不可忽略的化学组成与结构的差异.     

微纳米VO2膜层高温相变原位X射线衍射测试方法研究

通过设计、自制加热样品台结合商业X射线衍射仪的小角掠入射衍射模式,开发了微纳米膜层的原位高温相变测试方法,解决了样品表面微纳米膜层材料（厚度 < 10 μm）的高温相变难以原位测量的问题.研究了样品台与膜层表面的温度分布特征,验证了自制加热样品台的控温效果,原位测试了不同温度下二氧化钒（VO₂）膜层的X射线衍射图谱,揭示了VO₂膜层的高温相变行为.     

水凝胶微流控芯片的快速加工及在细胞培养检测中的应用

采用具有紫外光聚合性能的聚乙二醇(PEG)基水凝胶材料, 通过紫外光聚合作用快速加工双层水凝胶微流控芯片, 并验证了其对肿瘤细胞代谢液进行检测的可行性. 与传统微流控芯片材料相比, 该水凝胶芯片材料具有更好的生物相容性及可操控性, 可直接加工成形, 在生物学领域特别是细胞培养过程控制方面具有良好的应用前景. 实验结果表明, 该水凝胶微流控芯片可在微尺度空间有效模拟细胞生长环境, 并实现对细胞连续捕获后的原位培养. 将该芯片与卟啉可视阵列传感器系统结合, 经代谢特征分析可有效区分不同种类肿瘤细胞, 实现芯片细胞培养平台上的细胞代谢指纹快速可视化传感检测.     

高分子固液复合界面与液体黏附调控

受猪笼草口缘区润滑效应启发,将低表面能液体注入高分子微纳米多孔结构中可构筑高分子固液复合界面.与超疏水固体界面相比,固液复合界面展现出独特的浸润性和黏附性.界面黏附是高分子复合材料重要的性质之一,实现界面黏附的精准调控对促进这类材料的发展和应用具有至关重要的作用.本文重点从稳定性调控、方向性调控以及原位可逆调控3个方面综述提升固液复合界面黏附可控性的工作,通过在表面微米结构中组装纳米层状及异质纳米层状结构,提高界面黏附的稳定性;使用界面薄层定向冷冻干燥法、激光刻蚀法以及复型法等方法,构筑具有取向结构的高分子固液复合界面,实现界面黏附的方向性调控;通过在界面中引入快速响应的智能基元,设计智能响应高分子固液复合界面,实现界面黏附的原位可逆调控.最后,概述了这类材料目前存在的问题并展望了其未来发展的方向.     

摩擦化学的主要研究领域及其发展趋势

本文从摩擦过程中表面产生的化学效应、干摩擦及油润滑状态下的摩擦化学三个方面评述了摩擦化学的研究内容和进展; 介绍了摩擦化学在材料制备中的应用及摩擦化学的研究方法; 对摩擦化学研究中存在的问题及其发展趋势进行了讨论。     

A fully automated mass spectrometer for the analysis of organic solids

Automation of a mass spectrometer—computer system makes it possible to process up to 30 samples without attention after sample loading. An automatic sample changer introduces the samples successively into the ion source by means of a direct inlet probe. A process control unit determines the operation sequence. Computer programs are available for the hardware support, system supervision and evaluation of the spectrometer signals. The most essential precondition for automation — automatic evaporation of the sample material by electronic control of the total ion current — is confirmed to be satisfactory. The system operates routinely overnight in an industrial laboratory, so that day work can be devoted to difficult analytical problems. The cost of routine analyses is halved.     

Friction: the importance of accurately specifying the method of sample preparation and the test conditions

Buffing and splitting have both been used to prepare test pieces from products or thick sheets of rubber and it has been found that whereas the coefficients of friction against steel of buffed and split surfaces differ only slightly, the same parameters measured against PTFE can vary by as much as 2:1. Surprisingly, moulded sheets gave intermediate results on steel but very low results on PTFE, up to four times lower than split surfaces. The lubricating effect of water was more velocity-dependent against steel than against PTFE. A buffed rubber surface tested wet on PTFE gave results indistinguishable from a moulded rubber surface tested dry. A buffed leather surface tested wet on steel showed an increase in coefficient of friction compared with the corresponding dry material, but on PTFE there was little change.These experiments illustrated that results on one material could not be used to predict results on a different material and that test conditions must always be closely specified. The surfaces were examined by scanning electron microscopy but differences in structure were insufficient to account for differences in friction.     

油酸修饰CuS纳米颗粒的原位合成及其摩擦学性能

利用原位合成法室温下直接在基础油中成功制备了油酸修饰CuS 纳米颗粒, 将其长时间静置, 不会发生纳米颗粒的团聚. TEM 研究表明, 该方法制备的纳米颗粒粒径大约为30 nm. 红外光谱结果表明, 由于油酸的羧基与无机CuS纳米颗粒表面发生了化学吸附,使无机纳米颗粒的表面有一层有机修饰层, 从而增强了其油溶性.摩擦磨损试验结果表明,该添加剂在基础油中能起到抗磨减摩的效果.随着添加剂浓度的增大, 摩擦系数和磨斑直径都呈现下降趋势,当添加剂浓度为0.1%(w)时, 摩擦系数和磨斑直径都达到最小值,但是进一步增加添加剂浓度, 摩擦系数与磨斑直径又都开始增大. SEM 研究结果表明, 油酸修饰CuS 纳米颗粒能起到抗磨减摩作用的原因是因为其有利于在摩擦副表面形成牢固的润滑膜.     

Infrared Matrix-Assisted Laser Desorption Electrospray Ionization (IR-MALDESI) Imaging Source Coupled to a FT-ICR Mass Spectrometer

Mass spectrometry imaging (MSI) allows for the direct monitoring of the abundance and spatial distribution of chemical compounds over the surface of a tissue sample. This technology has opened the field of mass spectrometry to numerous innovative applications over the past 15 years. First used with SIMS and MALDI MS that operate under vacuum, interest has grown for mass spectrometry ionization sources that allow for effective imaging but where the analysis can be performed at ambient pressure with minimal or no sample preparation. We introduce here a versatile source for MALDESI imaging analysis coupled to a hybrid LTQ-FT-ICR mass spectrometer. The imaging source offers single shot or multi-shot capability per pixel with full control over the laser repetition rate and mass spectrometer scanning cycle. Scanning rates can be as fast as 1 pixel/second and a spatial resolution of 45 μm was achieved with oversampling.

An echelle polychromator for inductively coupled plasma optical emission spectroscopy with vacuum ultraviolet wavelength coverage and charge injection device detection

The development and evaluation of a simultaneous inductively coupled plasma optical emission spectrometer with vacuum ultraviolet (VUV) wavelength coverage and charge injection device (CID) detection are described. The spectrometer is an echelle polychromator with a magnesium fluoride prism as a cross-disperser. A thin coating of Lumogen, used as a wavelength conversion phosphor, is applied to the surface of the CID detector. The Lumogen coating increases sensitivity in the VUV region dramatically. Wavelengths between 130 and 800 nm can be measured by this spectrometer. A measured spectral bandwidth of 0.006 nm at 134.724 nm is achieved. The analytical performance in radial viewing mode is evaluated. The 3σ detection limit measured for Cl at 134.724 nm in aqueous solution is 100 ng ml⁻¹.     

A new high luminosity UHV orange type magnetic spectrometer used for depth selective Mössbauer spectroscopy

A new magnetic spectrometer of the orange type has been built for energies up to 45 keV. Its features are: ·?Transmission: 20% of 4π ·?Relative momentum resolution: 0.1 to 1%, ·?Energy band width: ΔE/E = ± 4% For Auger Electron Spectroscopy (AES) a combination with an electrostatic retardation field around the sample will provide an even higher resolution. For depth selective conversion electron Mössbauer spectroscopy (DCEMS) the exceptional high effective luminosity of the ultrahigh vacuum (UHV) orange spectrometer allows the analysis of non-enriched samples in reasonable time without loss in depth resolution. The UHV was realized by a differentially evacuated double chamber system made of an aluminium alloy using Viton gaskets. The inner part can be heated to 150°?C.     

The application of surface analytical techniques to silicon technology

Summary Most modern semiconductor device engineering takes place in the top micron of the host wafer and involves the creation of regions whose composition varies over lateral dimensions which may be less than 0.5 m. Normal to the wafer surface, large changes in matrix and impurity composition may occur in the space of a single atomic plane. In future, the fabrication of quantum dots and wires will result in active device features a few nm in extent. Such material developments need to be supported by parallel development in surface analytical techniques with high spatial resolution. There are, however, fundamental limitations to what can be achieved directly. For a destructive technique such as secondary ion mass spectrometry (SIMS), the analytical sensitivity and spatial resolution are determined by the analyte volume which needs to be consumed to achieve the necessary statistical precision. Moreover, the type of information obtained depends on the details of the interaction between the primary probe and the sample surface. In order to combine high spatial resolution with high sensitivity, special sample structures and modified instruments are required. Techniques need to be developed for accurately compensating for the effects on the analysis of large localized changes in conductivity in the materials. A multi-technique approach to semiconductor analysis is required both to investigate the limitations of the techniques themselves, and to fully describe the material properties.     

On-line monitoring of a frontal chromatographic separation using inductively coupled plasma atomic emission spectroscopy

A test array is described employing a destructive analytical technique for the long-term monitoring of an industrial-scale separation process. As an example, we chose frontal chromatography as the separation and ICP/AES as the analytical method. The feed solution of the process was conveyed by a process pump via the separation unit to a sample station, where a small portion was diverted and transported by a roller pump into the spectrometer. We equipped our array with different loops for operating the process, calibrating the instrument and verifying the calibration. We obtained identical results for the different loops by absorbing the pulsation of the process pump and arranging for identical suction lines of the spectrometer pump. Based on the results, we redesigned the sample station for a technical application using only commercially available parts.     

一种新型在线近红外光谱分析仪的研制

研制了一种新型的电荷耦合器件(CCD)在线近红外光谱分析仪，它由光谱仪系统、电源电路与控制系统、光纤及其附件与流通池系统、防爆系统、样品前处理系统、模型界外样品抓样系统、实时光谱测量和化学计量学软件等部分组成。在兰州炼油厂联合重整装置上连续5个月的工业实验表明，该仪表测定汽油辛烷值的准确性为0．3个辛烷值单位，重复性为0．2个辛烷值单位，具有准确性高、稳定性好、测量速度快、安全性强、自动化程度高和分析测试项目扩展性宽等特点。该仪表可与APC技术或其它自动化系统联用，对石化等大型生产装置的技术进步将产生积极的推动作用。     

双电离源(辉光放电/激光溅射电离)四极杆质谱仪的研制

本研究将辉光电离源与激光溅射电离源巧妙地结合在同一台仪器中,使固体样品在离子源腔体中既能辉光电离,也能激光电离;并且使用同一质量分析器,两种离子源的结果可以相互比对,进而得到更为准确的分析结果.此仪器主要由真空系统、离子源、离子传输系统、四极杆质量分析器及检测与数据采集系统等组成.实验中分别用两种离子源测试了标准样品SRM 1262b,并获得了半定量结果.结果表明,仪器具有定性能力强,分析速度快,检测灵敏度高等优点,对固体样品元素分析的检出限可达μg/g量级.实验表明,激光溅射电离质谱的性能优于辉光放电质谱.