SPM探针制备的新进展

扫描探针显微技术应用越来越广泛，其探针制备技术也不断得到开发。从探针结构的改进和探针功能的扩展等方面对近几年来探针制备技术的相关发展进行了阐述，探讨了SPM技术的拓展和新应用，同时也讨论各种制备方法的特点和适用条件。     

STM探针电化学腐蚀装置的设计及实验研究

本文根据扫描隧道显微镜(STM)探针电化学腐蚀方法的特点,在总结其它STM探针电化学腐蚀装置的基础上,自制了STM探针电化学腐蚀装置。并用此装置进行探针制备的实验研究,摸索出了此装置制备高质量钨探针的较佳工艺条件,同时给出了所制探针的STM成像结果。     

应用聚焦离子束/电子束技术的碳纳米管探针制备工艺研究

提出利用电子束诱导铂沉积和聚焦离子束铣削技术,实现碳纳米管原子力显微镜探针针尖的制备和结构优化研究。结合高分辨率扫描电子显微镜观测和纳米操纵仪,利用电子束诱导铂沉积实现碳纳米管固定到普通原子力显微镜探针末端,可实现直径小于10nm的纳米管探针制备。提出基于聚焦离子束铣削和照射技术实现对纳米管针尖的长度、角度的精确调控优化,纳米管探针的角度调控精度优于1°。     

SNOM/SFM结合的近场光学探针

介绍了近年来近场光学探针技术的进展，特别是可与扫描力显徽镜结合的探针制备技术。     

叶酸偶联的荧光聚合物纳米探针的制备及细胞成像

目的研究叶酸偶联的PFBT荧光聚合物纳米探针对U87细胞、H1299细胞及SKOV3细胞的细胞靶向效果。方法采用纳米共沉淀法制备PFBT聚合物纳米探针,采用EDC偶联试剂制备叶酸修饰的聚合物纳米探针,用共聚焦显微镜观察纳米探针在U87细胞、H1299细胞及SKOV3细胞的成像效果。结果 PFBT聚合物纳米探针与U87细胞、H1299细胞及SKOV3细胞共孵育12 h后,在细胞内仅检测到微弱的探针的荧光;而偶联叶酸后在相同条件下使细胞内的探针的荧光强度增加。结论叶酸偶联的PFBT聚合物纳米探针对U87细胞、H1299细胞及SKOV3细胞具有一定的靶向效果。     

亚微米级毛细管微探针的制作及其应用

设计了一种用热拉伸法制备毛细管微探针的新装置,可制作尖端内外径从亚微米量级至数十微米量级的毛细管微探针。介绍了微探针在细胞人工授精操作中的应用实例,并提出一种基于扫描隧道显微术与电化学技术,利用微探针进行集成电路微细加工的新方法。     

UV-LIGA技术制备微型柔性镍接触探针

对探针的制作方法、关键工艺环节等进行了分析与研究,给出了基于UV-LIGA技术制备微型柔性镍接触探针的工艺过程,分析了制备的技术关键,试验优选了关键制备环节的工艺参数,在此基础上,制作出微型柔性镍接触探针。试验结果表明:采用工艺条件优选的UV-LIGA技术,如前烘60 ℃,120 min,90 ℃,120 min;较大曝光剂量;后烘65 ℃,10 min,95 ℃,45 min;匀胶后静置、随炉冷却和超声辅助显影等辅助措施,所制备出的柔性接触探针(主体总长4 mm,宽80 μm,高100 μm;弹簧处高宽比为5(100 μm:20 μm))尺寸精度高;三角锥状针尖曲率半径小于5 μm;缺陷少,形貌质量高。     

激光辐照制备银纳米基底及其用于葡萄糖检测

通过激光辐照的方法制备银纳米条纹表面增强拉曼散射基底,该基底具有制备方法简单、均匀性好、重复性强的优点。用巯基吡啶(4-MPY)作为探针分子,葡萄糖和葡萄糖氧化酶产生的过氧化氢会改变银纳米条纹的形貌,进而影响探针分子的表面增强拉曼光谱强度,从而实现葡萄糖的间接检测。得到的探针分子的表面增强拉曼光谱的强度与葡萄糖溶液的浓度具有较好的线性关系。实验结果表明,该基底在葡萄糖的检测及定量分析方面具有良好的应用前景。     

多光束干涉光纤FP探针脉动微压传感研究

本文提出一种面向脉动微压传感的多光束干涉光纤法布里-珀罗(FP)探针。建立探针多光束干涉波长漂移与微压传感模型,分析其在气、液相环境中微压灵敏度差异。采用化学腐蚀、放电熔接、精密切割技术制备光纤探针器件。利用医用注射器、透明柔性软管、石英插芯构建微压测试环境,通过有限元仿真分析测试环境内部压强分布情况,在气相环境压强范围14.41～85.22 kPa、液相环境压强范围4.50～26.02 kPa的测试条件下,对3支光纤探针微压传感特性进行分析。实验结果表明,气、液相环境中,探针波长均随压强增大发生红移现象,反之,发生蓝移现象;气相环境探针平均微压灵敏度可达8.210 pm·kPa^-1,液相环境探针平均微压灵敏度可达66.720 pm·kPa^-1,高于气相环境,与理论模型相符。选取气、液相环境中微压灵敏度最高的光纤探针进行液相脉动微压传感特性研究。实验结果表明,5个脉动周期内探针波长响应良好,且重复性误差较小。本文提出的光纤探针结构紧凑,易于制备,灵敏度高,可实现1 Hz频率范围内的脉动微压传感,为液相环境脉动微压传感提供了重要的参考价值。     

溶胶-凝胶固定纳米光纤探针上生物活性分子的研究

为提高纳米光纤生物传感器的性能,研究了以溶胶-凝胶法将生物活性分子固定于纳米光纤探针上。首先以正硅酸乙酯(TEOS)为前驱体,制备了以葡萄糖氧化酶(GOD)为生物活性分子的溶胶,然后利用提拉法将GOD凝胶固定于纳米光纤探针上;讨论了固定化GOD活性及凝胶膜在纳米光纤探针上成膜的条件;最后通过扫描电子显微镜检测到薄膜均匀连续,生物探针尺寸小于1μm,并利用电子探针验证了GOD被固定于纳米光纤探针上。     

Using defined structures on very thin foils for characterizing AFM tips

Knowledge of tip geometry is necessary for reproducible atomic force microscope (AFM) measurements. This is particularly important for measurements in contact mode, in which a certain wear of the tip will always occur. For small or flat structures or for structures of larger dimensions, knowledge of the tip radius and the entire tip geometry is important. Additionally, the tilt of the tip in relation to the sample is of importance. Normally, very complicated lithographically manufactured structures for tip characterization are used. In contrast, the structures shown in this work are very simple. For measuring the tip geometry very thin foils patterned by focused ion beam (FIB) were used. In this work we demonstrate the possibility of determining the AFM tip geometry and the tilt based on several different large structures. A proven algorithm was developed for the reconstruction of the tips. The shape of FIB-structured foils was determined by electron microscopy prior to AFM measurements. This new method for determining tip shape is also presented as it compares to other current methods. In this case a discussion on the stability and advantages of the new method is presented.     

用有限元方法计算X光源场发射阴极电流

针对场致发射阵列建立了有效的三维有限元模型来分析单个尖锥的发射电流.考虑到场致发射阵列的周期性和尖锥的轴对称性,仅对一个尖锥单元的1/4进行分析.对模型的表面施加电压边界条件,计算得到尖锥表面电场强度分布,电场强度在尖锥顶点最强,场发射电流在此处也最强.由Fowler-Nordheim函数可得到尖锥表面的场致发射电流密度分布,对整个尖锥表面进行积分后得到了单个尖锥的场致发射电流约为7μA.计算了在100V门电压下不同顶端半径的场致发射电流.结果显示,场发射对顶端半径有很强的依赖性.计算了100个顶端半径为8nm的尖锥在不同门电压下的总场致发射电流,发射电流与开启电压与实际测量值符合得很好.     

Arrangement and stability of atoms at the apex of a scanning tip

A field ion microscope was used to examine the stability of the atomic arrangement at tip apexes. Although a single W atom at the top layer of a [111]-orientated tip apex protrudes from the underneath layer by only 0·91 Å, the present study suggests that the (111)-orientated W tip is the most desirable tip for scanning tunnelling microscopes because a large activation energy for surface diffusion on the (111) plane immobilizes the apex atom while the tip scans over a specimen surface and the tip apex can be resharpened by simply heating the tip.     

Tip bluntness transition measured with atomic force microscopy and the effect on hardness variation with depth in silicon dioxide nanoindentation

Depth-sensing indentation measurements of surfaces and structures with indentation depths less than 100 nm necessitate the use of accurate area functions for correct property evaluation. Here, the effect of a blunt nanoindenter tip geometry is characterized using atomic force microscopy to measure the direct tip geometry and modeled by a power law profile shape. Direct measurement of tip geometry is a method to observe changes in the tip curvature and transition from the blunt tip region to an ideal tip geometry. The tip shape, curvature, and transition to ideal geometry is found to correspond with the increase in hardness observed experimentally in SiO2 using a self-similar contact model. For a Berkovich indenter, tip bluntness was found to have a power law degree of 1.5 near the tip apex with a continuously varying degree of bluntness until an ideal pyramidal shape was reached at a depth of 160 nm.     

Characteristics of fracture during the approach process and wear mechanism of a silicon AFM tip

The wear of an atomic force microscope (AFM) tip is one of the crucial issues in AFM as well as in other probe-based applications. In this work, wear tests under extremely low normal load using an AFM were conducted. Also, in order to understand the nature of silicon tip wear, the wear characteristics of crystal silicon and amorphous silicon oxide layer were investigated by a high-resolution transmission electron microscope (HRTEM). It was found that fracture of the tip readily occurred due to impact during the approach process. Experimental results showed that the impact should be below 0.1 nNs to avoid significant fracture of the tip. Also, it was observed that wear of the amorphous layer, formed at the end of the tip, occurred at the initial stage of the silicon tip damage process. Based on Archard's wear law, the wear coefficient of the amorphous layer was in the range of 0.009-0.014. As for the wear characteristics of the silicon tip, it was shown that wear occurred gradually under light normal load and the wear rate decreased with increase in the sliding distance. As for the wear mechanism of the silicon tip, oxidation wear was identified to be the most significant. It was shown that the degree of oxidation was higher under high normal load and in a nitrogen environment, oxidation of the silicon tip was reduced.     

V形切口尖端裂纹起裂方向的主应力判别准则及其验证

围绕V形切口尖端裂纹起裂方向,分析了V形切口尖端裂纹应力场、位移场、应力强度因子,提出了裂纹起裂方向的主应力判别准则。首先,详细给出了V形切口尖端应力应变场的求解方法,通过裂纹尖端场本征值的三次线性拟合及误差分析,确定了V形切口尖端裂纹位移场;然后,建立了V形切口尖端的数值分析模型,运用数值计算方法确定了应力强度因子和切口强度因子,提出了V形切口尖端裂纹起裂方向的主应力判断准则,给出了外推法求解分析过程;最后,以LY8为试验材料,在张角2β＝60°的V形切口情况下,对提出的V形切口尖端裂纹起裂方向计算方法与判别准则进行了试验验证。     

Effects of Atomic Force Microscope Silicon Tip Geometry on Large-Scale Nanomechanical Modification of the Polymer Surface

The shape of an atomic force microscope (AFM) silicon tip has a significant effect on the mechanical modification of the polymer surface, especially for a longer sliding distance of from several to several hundreds of millimeters. In this work, a pyramidal silicon tip was used to cut into the polymethyl methacrylate (PMMA) surface, forming nanogrooves with a linear sliding distance of about 80 mm and wear box structures with a total tip sliding distance of 1,024 mm. The effects of the tip edges and the tip radius on the form of the wear debris chips, wear depth, and debris transferred to the tip were investigated. The experimental results showed that four sides of the tip influenced the morphology of the removed material. Adhesion appeared to play a role in the tip wear mechanism by successive removal of SiO₂ layers during transfer of adhered PMMA from the tip to the surface. The tip radius generally increased with sliding distance. Simultaneously, adhesion of the removed materials to the tip induced a larger tip radius and a sharper tip was revealed as dropping off of the materials during the test from time to time. Thus, with the same normal load the worn tip may induce failure of the machining process. The results presented in this study provide insight into long-term nanoscratch/wear and nanomechanical machining of glassy polymer surfaces with a silicon AFM tip.     

裂纹尖端滑移系选择的探讨

本文利用断裂力学知识和张量分析方法得到了外加应力在裂尖滑移系沿滑方向的分解剪切应力,并定义了裂纹尖端Schmid因子。本文还讨论了裂尖应力场对裂尖滑移系开动的影响。当裂纹尖端向外发射位错时,裂尖滑移系的选择由裂尖Schmid因子支配,并且在裂尖附近区域内位错源开动或螺位错交滑移时滑移系的选择也由裂尖Schmid因子支配。     

In situ metal tip sharpening of scanning probe microscopes

This article demonstrated a new approach for fabrication and sharpening of metal tips of scanning probe microscopes. Experimentally, a metal tip was heated and melted by a focused laser light. The tip was then sharpened by a strong electric field and consolidated as the laser was turned off. With a low‐vacuum and a high‐voltage source, a 25‐µm indium‐coated platinum wire was sharpened to a tip with diameters below 50 nm. The minimal tip radius by this method is estimated to be below 1 nm. With this technique, in situ tip sharpening for SPM would be possible. SCANNING 34: 76–79, 2012. © 2011 Wiley Periodicals, Inc.     

水平轴风力机的转矩性能及叶尖损失对其的影响

分析了叶尖损失机理,根据PRANDTL 和GLAUERT叶尖损失修正因子及叶素-动量理论,推导出考虑叶尖损失的叶片弦长公式,然后沿叶片展向积分,推导出与风力机尖速比和翼型升阻比关联的风力机转矩系数解析表达式,并得到风力机在任何稳定运行状态转矩系数的最高参数值,可作为风力机转矩系数的设计参考值。研究表明,叶尖损失对弦长的影响集中在叶尖部位,当升阻比为无穷大且尖速比从常见范围10变化到4时,叶尖损失导致转矩性能损失约4%~10%,且损失的数值随升阻比的变化极小。