ZnS基底沉积类金刚石薄膜研究

针对不能直接在红外光学材料ZnS基底上沉积类金钢石薄膜(下述简称DLC膜)的问题,介绍了在红外光学材料ZnS基底上沉积DLC膜的方法,指出了采用在ZnS基底表面镀制DLC膜的方法,来解决在ZnS基底表面上镀制高效增透膜后,其膜层耐磨强度不足以抵抗恶劣环境的缺点;同时,通过膜系优化设计,利用镀制组合膜层的方法来降低其单面反射率,可改善光学系统的成像质量。     

Al/Zr多层膜生长模型和数值计算

在17～19nm波段,利用直流磁控溅射技术将Al(1%wtSi)/Zr多层膜镀制在掺氟的二氧化硅基底上,基于原子力显微镜对不同膜对数(N=10,40,60,80)表面粗糙度的测量结果,将多层膜的生长模型应用于实际结果中,对表面均方根粗糙度随着膜对数的变化进行了深入的分析,并对Stearns粗糙度动态生长理论的适用条件作了补充性讨论。     

极紫外Mg/SiC、Mg/Co多层膜的稳定性

采用磁控溅射法在Si(100)基底上镀制了膜系结构分别为[Mg/Co]20、[Mg/SiC]20的两组多层膜,以研究Mg基多层膜的稳定性.对放置在室温和80％相对湿度环境下的样品进行显微镜、表面粗糙度和X射线掠入射反射率测试,对比研究了Mg/Co和Mg/SiC两种多层膜结构在相同环境中的损坏状况.对比结果显示:放置4天后,Mg/SiC损坏面积为26.34％,表面粗糙度为10 nm; Mg/Co的损坏面积为2.78％,表面粗糙度为5 nm.6天后,X射线掠入射反射率测量显示Mg/SiC多层膜一级反射峰完全消失,而Mg/Co多层膜的一级反射峰仍有47.63％的反射率.实验表明,Mg/Co多层膜的表面层和内部多层膜结构的损坏速度较Mg/SiC慢,具有较好的环境稳定性.另外,X射线光电子谱(XPS)测试Mg基多层膜损坏后的产物主要为MgCO3、Mg(OH)2和少量的MgO,且内层Mg(OH)2与MgCO3含量的比值显著高于表面层.分析认为,水汽是造成Mg基多层膜损坏的主要原因,今后Mg基多层膜保护层的研究可主要针对如何防止水汽进入膜层.     

软X射线多层膜设计中表面粗糙度对反射率的影响

给出了一种改进的软X射线波段的多层膜设计方法.在设计过程中,考虑了反射镜基底和各膜层之间的均方(RMS)粗糙度对反射率的影响 ;在Stearns提出的散射理论的基础上给出了粗糙界面的数学模型.文中以波长为λ=1.03nm的软X射线为例进行设计,设计结果表明 :要使波长为λ=1.03nm的多层膜的反射率大于10%,反射镜基底的均方粗糙度不应超过0.6nm.实验中选择几块表面粗糙度为 0.5nm(RMS)的熔石英平面镜作为基底来制作适用于该波长的、层对数超过70的多层膜.然后在的入射角下测量反射率,测得的值为10%,这与采用本设计方法得到的计算结果一致.该反射镜作为X射线谱仪的分光元件被应用于惯性约束聚变(ICF)的过程诊断中.     

应用SiC反射镜表面改性技术提高TMC光学系统信噪比

为了消除SiC反射镜的固有缺陷,提高反射式光学系统的信噪比,使用SiC表面改性技术对同轴三反射(TMC)光学系统的SiC反射镜进行了处理.首先,应用等离子体辅助沉积(PIAD)技术沉积了一层Si改性层,接着对改性层进行精密抛光,然后在反射镜表面镀制Ag膜和增强膜,最后获得了表面改性对TMC光学系统信噪比的影响.Wyko轮廓仪测试表明,SiC反射镜的粗糙度R_a由10.42 nm降低到了0.95 nm;镀制高反射膜后,主镜、次镜、三镜及折叠镜在0.5～0.8 μm可见光波段的反射率＞98%.计算结果表明,应用了表面改性技术后TMC反射式光学系统的信噪比提高了5%以上,说明SiC表面改性技术是一种提高TMC光学系统信噪比的有效方法.     

磁控溅射沉积TiB_2/DLC纳米多层膜的结构及其机械性能研究

采用非平衡磁控溅射系统在P(100)硅片和304不锈钢基底上制备TiB_2/DLC纳米多层膜。利用FESEM、TEM、XRD和AFM观察多层膜的微观结构和表面形貌;利用纳米压痕仪、维氏硬度计和CSM球-盘摩擦磨损试验机考察TiB_2靶电流对多层膜的机械性能和摩擦学性能的影响。结果表明:TiB_2/DLC多层膜具有良好的多层调制结构,多层膜沿TiB_2(101)晶向择优生长;多层膜的表面粗糙度随着TiB_2靶电流增加而增加;多层膜中的大量异质界面能显著提高薄膜的硬度及韧性,而且当TiB_2靶电流为2.0 A时,多层膜的硬度约为单层DLC薄膜的两倍;多层膜中具有硬质TiB_2层和软质DLC层的交替结构,在摩擦过程中,硬层TiB_2起到良好的承载作用,软层DLC起到良好的润滑作用,使多层膜具有比单层DLC薄膜更低的摩擦因数。     

沉积温度对磁控溅射Ti/TiN多层膜光学和电学性能的影响

采用直流反应磁控溅射法于不同温度下在Si(111)基底上制备了Ti/TiN多层膜,采用X射线衍射仪和原子力显微镜对膜的物相和表面形貌进行了分析,研究了沉积温度对膜结构及其光学、电学性能的影响。结果表明:不同沉积温度下制备的Ti/TiN多层膜均由钛和TiN相组成,多层膜与单层TiN膜一样,其表面粗糙度随沉积温度的升高而减小,电阻率随沉积温度的升高显著降低;其表面形貌则比单层膜更加致密和均匀;多层膜红外反射率与其电阻率有关,当电阻率减小时,红外反射率增大。     

氮气反应溅射制备软X射线Co/Ti多层膜

针对"水窗"波段(280~540eV)对多层膜反射镜的应用需求,在Ti的L吸收边(452.5eV)附近,优化设计了Co/Ti多层膜的膜系结构。计算了不同界面粗糙度条件下的反射率,结果显示,界面粗糙度对多层膜反射率有较大影响。采用直流磁控溅射方法在超光滑硅基片上制备了Co/Ti多层膜,通过将氮气引入原有的溅射气体氩气中作为反应气体,明显减小了制备的多层膜的界面粗糙度。利用X射线掠入射反射实验和透射电子显微镜测试了多层膜结构,并在北京同步辐射装置(BSRF)3W1B实验站测量了不同氮气浓度下多层膜的反射率。结果显示,氮气含量为5%的溅射气体制备的多层膜样品反射率最高,即将纯氩气溅射制备得到的反射率9.5%提高到了12.0%。得到的结果表明,将氮气加入反应溅射气体可以有效改善Co/Ti多层膜的性能。     

离子辅助制备碳化硅改性薄膜

介绍了一种利用霍尔型离子源辅助电子束蒸发,在反应烧结碳化硅(RB-SiC)材料上制备硅改性薄膜的方法,研究了不同沉积速率下薄膜改性后的抛光效果.对样品进行了表面散射及反射的测量.通过样品的显微照片可知,硅膜层在沉积速率增大的条件下结构趋于疏松.在精细抛光镀制有硅改性薄膜的反应烧结碳化硅样品后,表面散射系数减小到1.46%,反射率接近抛光良好的微晶玻璃.温度冲击实验和表面拉力实验表明:硅膜无龟裂和脱落,性质稳定,与碳化硅基底结合良好.     

13.9nm和19.6nm正入射Mo/Si多层膜反射镜反射率的测量

根据理论模拟计算并设计了分别工作在13.9nm类镍银和19.6nm类氖锗两种X射线激光的Mo/Si多层膜,将自行设计的小型反射率计安装在Mcpherson247单色仪出射狭缝附近,组成以铜靶激光等离子体辐射源作为极紫外光源的反射率测量装置,对研制的Mo/Si多层膜反射镜的反射率进行了测量。实验结果显示,中心波长分别是13.91nm和19.60nm,相应反射率分别是41.9%和22.6%,半宽度分别是0.56nm和1.70nm,中心波长和半宽度与理论值基本一致。为了全面了解多层膜的性能,用WYKO测量多层膜的表面粗糙度,13.9nm和19.6nmMo/Si多层膜的表面粗糙度分别是0.52nm和0.55nm。     

Suppression of spurious vibration of cantilever in atomic force microscopy by enhancement of bending rigidity of cantilever chip substrate

To improve the precision of dynamic atomic force microscopy (AFM) using cantilever vibration spectra, a simple but effective method for suppressing spurious response (SR) was developed. The dominant origin of SR was identified to be the bending vibration of the cantilever substrate, by the analysis of the frequency of SR. Although a rigid cover pressing the whole surface of the substrate suppressed SR, the utility was insufficient. Then, a method of enhancing the bending rigidity of the substrate by gluing a rigid plate (clamping plate, CP) to the substrate was developed. This chip can be used with an ordinary cantilever holder, so that the reproducibility of SR suppression when attaching and detaching the cantilever chip to the holder was improved. To verify its utility, the evaluation of a microdevice electrode was performed by ultrasonic atomic force microscopy. The delamination at a submicron depth was visualized and the detailed variation of the delamination was evaluated for the first time using clear resonance spectra. The CP method will particularly contribute to improving dynamic-mode AFM, in which resonance spectra with a low quality factor are used, such as noncontact mode AFM in liquid or contact resonance mode AFM. The effect of the CP can be achieved by fabricating a substrate with a thick plate beforehand.     

极紫外光刻机多层膜反射镜表面碳污染的清洗

针对极紫外(EUV)光刻机工作过程中,多层膜反射镜表面沉积碳污染造成的反射率下降问题展开研究,讨论了多层膜反射镜表面碳污染清洗方法。首先描述了在EUV曝光过程中多层膜表面的碳污染形成过程,简单阐述了碳污染对多层膜反射镜的危害。然后从清洗机理、速率以及效果等方面详细描述了多种EUV多层膜表面碳污染清洗方法,分析对比了各清洗技术在清洗速率和效果等方面的优缺点。分析表明:离子体氧和活化氧清洗速率相差不多,可达到2nm/min,但清洗过程中容易造成表面氧化;等离子体氢和原子氢的清洗速率相对较慢,一般在0.37nm/min左右,但清洗过程中不易产生氧化。最后针对不同方法应用于在线清洗EUV多层膜反射镜过程中将遇到的问题和难点进行了讨论。     

Investigation of the Tribological Behaviors of Polymer Molecular Deposition Films by Tribometer Based on Interferometer

The polymer molecular deposition films including polyelectrolyte molecular deposition (PEMD) film and nanoparticles composite molecular deposition (NPs/MD) film have been prepared using the molecular deposition method and the in situ synthesize method. The polymer molecular deposition films were characterized by atomic force microscope (AFM) and X-ray photoelectron spectroscopy (XPS). The tribological behaviors of the substrate and polymer molecular deposition films were investigated by a tribometer based on interferometer. It is found that the NPs/MD film has a lower friction force and a better anti-wear property than the PEMD film under the dry friction. The poly alpha olefin (PAO2) and water films confined between samples and steel ball surfaces have been investigated using thin film interferometry. The friction force of substrate was lower than the polymer molecular deposition films under PAO2 lubrication. The friction forces alteration of PEMD film and NPs/MD film were similar and consistent, and lower than that for substrate under water lubrication.     

An In Situ Method for Simultaneous Friction Measurements and Imaging of Interfacial Tribochemical Film Growth in Lubricated Contacts

Tribological investigations of macroscopic lubricated sliding contacts are critical for a wide range of industrial applications including automotive engines, gears, bearings, and any other contacting surfaces in relative motion. However, the inability of existing techniques to access buried sliding interfaces with high spatial resolution inhibits the development of fundamental insights into the tribological processes at play. Here we demonstrate a novel and general in situ method, based on atomic force microscopy (AFM), in which micrometer-scale spherical probes are attached to a standard microfabricated AFM cantilever which is then slid over a substrate while immersed in a liquid lubricant. In this case, steel colloidal probes and steel substrates were used, and the contact was immersed in a commercial polyalphaolefin oil with zinc dialkyl dithiophosphate (ZDDP) additive at both room temperature and 100 °C, but the method can be used for a broad range of material combinations, lubricants, and temperatures. We demonstrate that the in situ measurements of friction force and the morphological evolution of the tribochemical films on the substrate can be simultaneously achieved with nanometer-level spatial resolution. In addition, we demonstrate that the sliding zone is readily accessible for further characterization with higher spatial resolution using standard AFM probes with nanometer-scale tip radii. Ex situ characterization of the micrometer-scale probe and the sample is also feasible, which is demonstrated by acquiring high-resolution AFM topographic imaging of the final state of the probe.     

Torsional Fretting Wear Behavior of Bonded MoS2 Solid Lubricant Coatings

The effects of applying a bonded MoS₂ solid lubricant to a 1050 steel substrate were investigated using a torsional fretting wear apparatus. Tests were conducted under a normal load of 50 N with angular displacement amplitudes ranging from 0.1 to 5°. Wear scars were examined using scanning electron microscopy, energy-dispersive X-ray spectrometry, optical microscopy, and surface profilometry. The MoS₂ coating exhibited different torsional fretting regimes than those of the substrate. Fretting regimes of the coating were primarily in the partial slip regime (PSR) and the slip regime (SR) with no mixed fretting regime. The width of the PSR narrowed. Due to the lubricating effects of the coating, the friction torque was consistently lower than that of the substrate. The damage to the coating in the PSR was very slight, and its granular structure remained even after 1,000 cycles. The damage mechanism to the SR coating was a combination of abrasive wear, oxidative wear, and delamination. The MoS₂ coating had potential to alleviate torsional fretting wear.     

Thin film thickness measurements in two phase annular flows using ultrasonic pulse echo techniques

The electric power generation and oil/gas production industries have a strong interest in the physical characterization of conducting and non-conducting liquid films that are formed during the flow of liquids in pipes. Conducting and non-conducting liquid films do not lend themselves to the same characterization techniques due to the different requirements originating from their electrical properties. Techniques based on the use of ultrasound are extremely attractive for that purpose as they do not depend on the electrical properties of the liquid and are also non-invasive. This paper presents the application of ultrasonic techniques for measuring the thickness of wavy thin liquid films (<6 mm) in vertical pipes. Initial benchtop experiments were performed, and different signal processing methods were implemented in order to identify the most suitable depending on the film thickness. For a film thickness >0.5 mm a time of flight method was utilized whereas for a film thicknesses <0.5 mm a frequency method and time domain method were utilized. These methods were validated using a theoretical volume measurement on a static system. The studied methods were then tested on downward and upward vertical flow experimental rigs with pipe diameters of 127 mm and 34.5 mm respectively. The results of the experiments using ultrasonic methods showed good agreement with the measurements obtained using a multi pin film sensor and a concentric conductance probe, highlighting the potential that ultrasound offers in thin film measurements.     

Effect on crystalline structure of AISI M2 steel using tungsten–thorium electrode through MRR,EWR, and surface finish

To investigate on the crystalline structure of AISI M2 steel by using tungsten–thorium electrode in electrical discharge machining (EDM) process was studied. Furthermore, the investigation were carried out for finding the value of material removal rate (MRR), electrode wear rate (EWR) and surface roughness (SR) of tool steel material depending upon three variable input process parameters. On the basis of weight loss, the value of MRR and EWR were calculated at optimized process parameter. Subsequently, surface topography of the processed material were examined through different characterization techniques like scanning electron microscopy (SEM), Optical surface profiler (OSP) and Atomic force microscopy (AFM), respectively. In XRD study, broadening of the peak was observed which confirmed the change in material properties due to the homogeneous dispersion of the particles inside the matrix. Lowest surface roughness and MRR of 0.001208 mg/min was obtained. Minimum surface roughness was obtained 1.12 μm and 2.18427 nm by OSP and AFM study, respectively. Also, minimum EWR was found as 0.013986 mg/min.     

Study of thermal and acoustic noise interferences in low stiffness atomic force microscope cantilevers and characterization of their dynamic properties

The atomic force microscope (AFM) is a powerful tool for the measurement of forces at the micro/nano scale when calibrated cantilevers are used. Besides many existing calibration techniques, the thermal calibration is one of the simplest and fastest methods for the dynamic characterization of an AFM cantilever. This method is efficient provided that the Brownian motion (thermal noise) is the most important source of excitation during the calibration process. Otherwise, the value of spring constant is underestimated. This paper investigates noise interference ranges in low stiffness AFM cantilevers taking into account thermal fluctuations and acoustic pressures as two main sources of noise. As a result, a preliminary knowledge about the conditions in which thermal fluctuations and acoustic pressures have closely the same effect on the AFM cantilever (noise interference) is provided with both theoretical and experimental arguments. Consequently, beyond the noise interference range, commercial low stiffness AFM cantilevers are calibrated in two ways: using the thermal noise (in a wide temperature range) and acoustic pressures generated by a loudspeaker. We then demonstrate that acoustic noises can also be used for an efficient characterization and calibration of low stiffness AFM cantilevers. The accuracy of the acoustic characterization is evaluated by comparison with results from the thermal calibration.     

Camphor sulfonic acid (CSA) doped polypyrrole (PPy) films: Measurement of microstructural and optoelectronic properties

In this paper, camphor sulfonic acid doped polypyrrole have been successfully prepared using different weight percentages of camphor sulfonic acid (10–50%) dispersed in polypyrrole by solid state synthesis method. Films of CSA doped PPy were prepared by spin coating technique on a glass substrate. The effect of varying concentrations of CSA on the structure, morphology, optical and electrical properties of polypyrrole was explored using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM) atomic force microscopy (AFM), UV–visible spectroscopy and two probe technique respectively. The presence of CSA in PPy matrix and their interaction was confirmed by using XRD and FTIR techniques. The dramatic change in the surface morphology has been observed with increasing content of CSA in PPy matrix. The AFM study shows porous uniform globular morphology. The UV–vis spectra of CSA doped PPy film was found to shift to a lower wavelength side as compared to those of observed in PPy, indicating synergetic interaction between dopant CSA and PPy. CSA doped PPy not only can maintain a good solubility but also enhance the electrical conductivity. The results of dc electrical conductivity shows that, increase in electrical conductivity of PPy with increasing content of CSA (10–50%) in PPy matrix.     

电解锰阴极板超声波清洗机的声场研究

本文结合电解锰行业目前的状况,研发了一种针对电解锰阴极板的超声波清洗机。分析了超声波清洗的工作原理,并利用ANSYS有限元分析软件对不同频率下的超声波做了声场压力分布分析,有效的指导了超声波清洗机研发过程当中的频率选择问题。