Improvement of KFM performance by intermittent bias application method and by sampling detection of cantilever deflection

We have proposed an intermittent bias application method as well as a sampling detection method of cantilever deflection in Kelvin probe force microscopy (KFM) to improve its performances for surface potential measurements. In the former method, spiky biases, instead of the bias in a sinusoidal waveform normally used in KFM, are intermittently applied to generate electrostatic force at exact moments when the tip approaches the closest position to a sample surface. The latter one, on the other hand, realizes very sensitive detection of the electrostatic force, which is preferable in KFM. Both the dependence of the electrostatic force on the dc offset bias and the observed potential images clearly indicate that these two methods are very effective to improve the KFM performance.     

Imaging of optical disc using reflection-mode scattering-type scanning near-field optical microscopy

A phase-change optical disc was observed using a reflection-mode scattering-type scanning near-field optical microscope (RS-SNOM). In an a.c.-mode SNOM image, the 1.2 microm x 0.6 microm recording marks were successfully observed although the data were recorded on the groove. In contrast, no recording marks could be resolved in a d.c.-mode SNOM image. These results are in good agreement with those from a numerical simulation using the finite difference time domain method. The resolution was better than 100 nm with a.c.-mode SNOM operation and the results indicate that recording marks in phase-change optical media can be directly observed with the RS-SNOM.     

Environmental effects in Kelvin force microscopy of modified diamond surfaces

We have explored the effects of atmospheric environment on Kelvin force microscopy (KFM) measurements of potential difference between different regions of test polycrystalline diamond surfaces. The diamond films were deposited by microwave plasma-assisted chemical vapor deposition, which naturally produces hydrogen terminations on the surface of the films formed. Selected regions were patterned by electron-beam lithography and chemical terminations of oxygen or fluorine were created by exposure to an oxygen or fluorine plasma source. For KFM imaging, the samples were mounted in a hood with a constant flow of helium gas. Successive images were taken over a 5-h period showing the effect of the environment on KFM imaging. We conclude that the helium flow removes water molecules adsorbed on the surface of the samples, resulting in differences in surface potential between adjacent regions. The degree of water removal is different for surfaces with different terminations. The results highlight the importance of taking into account the atmospheric environment when carrying out KFM analysis.     

Imaging of optical disc using reflection-mode scattering-type scanning near-field optical microscopy

A phase-change optical disc was observed using a reflection-mode scattering-type scanning near-field optical microscope (RS-SNOM). In an a.c.-mode SNOM image, the 1.2 μm × 0.6 μm recording marks were successfully observed although the data were recorded on the groove. In contrast, no recording marks could be resolved in a d.c.-mode SNOM image. These results are in good agreement with those from a numerical simulation using the finite difference time domain method. The resolution was better than 100 nm with a.c.-mode SNOM operation and the results indicate that recording marks in phase-change optical media can be directly observed with the RS-SNOM.     

Friction property study of the surface of ZDDP and MoDTC antiwear additive films using AFM/LFM and force curve methods

The friction properties and material differences of the surface of ZDDP and MoDTC antiwear additive films, which give clear evidence of different friction coefficients in a pin-on-disc test, have been studied using atomic force microscopy (AFM)/lateral force microscopy (LFM) and force curve methods. The AFM/LFM observations show that the friction force on the surface of MoDTC additive films over the sliding area of a steel disc is lower and the friction force of ZDDP additive films is higher than that of afilmless area. Lateral force scope-trace evaluations reveal that the ratio of the friction forces on the surface of the ZDDP film, the filmless area, and the MoDTC film under the same normal force is approximately 1.5:1.0:0.7. Force curve measurements indicate that the surface materials of the ZDDP film, thefilmless area, and the MoDTC film differ according to their attractive forces, that is 29 nN for the ZDDP film, 22 nN for the filmless area, and 12 nN for the MoDTC film. These results correspond to the friction behaviour in the pin-on-disc test and also agree with the idea of the formation of solid MoS₂ lubricant from MoDTC additives on the surface of the antiwear film.     

Nano-pulsed laser irradiation scanning system for phase-change materials

Recently, the demand of a laser irradiation tester is increasing for phase change random access memory (PRAM) as well as conventional optical storage media. In this study, a nano-pulsed laser irradiation system is developed to characterize the optical property and writing performance of phase-change materials, based on a commercially available digital versatile disk (DVD) optical pick-up. The precisely controlled focusing and scanning on the material's surface are implemented using the auto-focusing mechanism and a voice coil motor (VCM) of the commercial DVD pick-up. The laser irradiation system provides various writing and reading functions such as adjustable laser power, pulse duration, recording pattern (spot, line and area), and writing/reading repetition, phase transition, and in situ reflectivity measurement before/after irradiation. Measurements of power time effect (PTE) diagram and reflectivity map of Ge(2)Sb(2)Te(5) samples show that the proposed laser irradiation system provides the powerful scanning tool to quantify the optical characteristics of phase-change materials.     

Note: Quantitative (artifact-free) surface potential measurements using Kelvin force microscopy

The measurement of local surface potentials by Kelvin force microscopy (KFM) can be sensitive to external perturbations which lead to artifacts such as strong dependences of experimental results (typically in a ～1 V range) with KFM internal parameters (cantilever excitation frequency and/or the projection phase of the KFM feedback-loop). We analyze and demonstrate a correction of such effects on a KFM implementation in ambient air. Artifact-free KFM measurements, i.e., truly quantitative surface potential measurements, are obtained with a ～30 mV accuracy.     

Resistance measurement of isolated single-walled carbon nanotubes

Conductive atomic force microscopy (CAFM) and Kelvin force microscopy (KFM) were used to measure the resistance of isolated single-walled carbon nanotubes (SWNTs). By analyzing the current map and surface potential obtained from CAFM and KFM methods respectively, the intrinsic resistance of SWNTs could be calculated. The results calculated by these two methods are the same for the same batch of SWNTs, which is on the order of 10⁷–10⁸ Ω.     

Tip-to-sample distance dependence of an electrostatic force in KFM measurements

In most scanning probe methods like an atomic force microscopy, a cantilever is mechanically vibrated in order to obtain topographies. Therefore, a tip-to-sample distance periodically changes during the scanning. Since the electrostatic force, which is a long-range force, is used for potential feedback in Kelvin probe force microscopy (KFM), such mechanical vibration leads to the fluctuation of the electrostatic force between the tip and the sample. In this study, firstly, we performed two-dimensional simulations of the electric fields between surfaces of the tip and the sample and evaluated the tip-to-sample distance dependence of the electrostatic force. Secondly, we experimentally confirmed the existence of the fluctuation of the electrostatic force and the tip-to-sample distance dependence of the electrostatic force was evaluated. Both the simulations and the experiments on the tip-to-sample distance dependence showed the importance of considering the tip sidewall effect in the KFM potential determination.     

相变薄膜热物性对电子设备热控的影响

相变热控技术是被动热控的重要方法之一。文中对利用柔性相变薄膜材料进行电子设备热控进行了实验研究和数值模拟,获得了相变材料热物性参数和结构参数对热控性能的影响规律。研究结果表明,相变材料的比热容和相变潜热对热控性能的影响较小,材料的热导率、厚度以及来自芯片的热流密度和热源面积因子对热控有较大影响;当系统达到热平衡时,热源中心温度与相变材料热导率、厚度以及热源面积因子成负相关,与热流密度成正相关。     

Rapid and accurate measurement for phase-change optical recording bits

Conducting atomic force microscopy (CAFM) and scanning surface potential microscopy (SSPM) have been used to image the phase-change optical recording bits. Commercially available digital versatile discs (DVD) + rewritable (RW) with initialization process were measured in experiments. Comparing the measurement results of both, the measurement resolution of CAFM is far superior to that of SSPM. With the DVD + RW disc rotating at a linear speed of 3.5 m/s, appropriate writing laser power range, may be precisely identified by CAFM as 10-15 mW. This is sufficient to verify the high-resolution recording bits research method. This new method may also be applied to the development of new types of phase-change recording materials.     

Al、Sn掺杂对于ZnO薄膜微结构及光学特性的影响

采用真空电子束蒸发金属薄膜及后续热氧化技术在石英衬底上分别制备出了ZnO、Al∶ZnO以及Sn∶ZnO薄膜。通过X射线衍射仪(XRD),紫外-可见分光光度计和原子力显微镜(AFM)等分析仪器对比研究了Al、Sn掺杂对ZnO薄膜结晶质量、光学性质及表面形貌的影响。测试结果表明,Al、Sn掺杂可以使薄膜结晶质量得到提高,薄膜应力部分释放,薄膜表面的粗糙度也相应增加,掺杂对薄膜光学带隙的影响在一定程度取决于金属薄膜的氧化程度,氧化充分可以使光学带隙变宽,反之则变窄。     

Mechanical Property Investigation of Soft Materials by Cantilever‐Based Optical Interfacial Force Microscopy

Cantilever‐based optical interfacial force microscopy (COIFM) was applied to the investigation of the mechanical properties of soft materials to avoid the double‐spring effect and snap‐to‐contact problem associated with atomic force microscopy (AFM). When a force was measured as a function of distance between an oxidized silicon probe and the surface of a soft hydrocarbon film, it increases nonlinearly in the lower force region below ∼10 nN, following the Herzian model with the elastic modulus of ∼50 MPa. Above ∼10 nN, it increases linearly with a small oscillatory sawtooth pattern with amplitude 1–2 nN. The pattern suggests the possible existence of the layered structure within the film. When its internal part of the film was exposed to the probe, the force depends on the distance linearly with an adhesive force of −20 nN. This linear dependence suggests that the adhesive internal material behaved like a linear spring with a spring constant of ∼1 N/m. Constant‐force images taken in the repulsive and attractive contact regimes revealed additional features that were not observed in the images taken in the noncontact regime. At some locations, however, contrast inversions were observed between the two contact regimes while the average roughness remained constant. The result suggests that some embedded materials had spring constants different from those of the surrounding material. This study demonstrated that the COIFM is capable of imaging mechanical properties of local structures such as small impurities and domains at the nanometer scale, which is a formidable challenge with conventional AFM methods. SCANNING 35:59‐67, 2013. © 2012 Wiley Periodicals, Inc.     

Current and potential characterization on InAs nanowires by contact-mode atomic force microscopy and Kelvin probe force microscopy

We fabricated InAs nanowires on GaAs giant step structures, and studied their surfaces by two methods; one was current detection by contact-mode atomic force microscopy, and the other was surface potential measurement by Kelvin probe force microscopy (KFM). In the current detection method, the regions where the large current flowed were distributed along the step edges, and these regions agreed well with the expected distribution of InAs. This result confirms that the InAs nanowires were formed along the GaAs giant step edges. The KFM measurements showed that the potential value became more negative along each step edge, where the InAs nanowire was expected to be formed. The surface potential of the InAs nanowires is more negative than that of the surrounding GaAs, which may result from the electron accumulation in the InAs nanowires.     

纳米压痕硬度尺寸效应分析及其试验研究

针对材料纳米压痕硬度的压痕尺寸效应(Indentation size effect,ISE),利用纳米压痕技术测得单晶铝和单晶硅的载荷-压深曲线,获得最大载荷和最大压深,并结合原子力显微镜,获得压痕的三维形貌,计算出压痕的真实残余面积。根据最大压深和残余面积提出了一个新的模型——残余面积最大压深模型,此模型能更好地理解和描述材料硬度的压痕尺寸效应,并与其他几种典型的理论和模型进行了比较和分析。     

Scanning probe microscopy for industrial applications: Selected examples

Some examples are selected to demonstrate the variety of possible scanning probe microscopy application in industry. Magnetic and magneto-optical storage media can be investigated by magnetic force microscopy, whereas a conventional scanning force microscope is used to examine surface features of many different materials, such as technical glasses, photosensitive materials, new superconductors, and biomolecules. Some other examples include the modification as well as the observation of liquid crystal devices, and the impact that scanning probe microscopy has on other techniques such as high precision stepping motors and high quality electron beam sources.     

密封环圆台型织构化粗糙表面对润滑性能的影响

针对密封环接触面之间的润滑问题,基于Reynolds方程,考虑粗糙度的影响,建立在流体动压润滑状态下圆台型表面织构的数学模型,对密封环接触表面在不同织构参数、不同粗糙度参数下润滑膜压力大小及分布情况进行研究。采用有限差分法、牛顿迭代法研究不同润滑介质下,圆台型微凹坑的几何参数及粗糙度参数对润滑膜平均压力的影响,并与理论数值结果进行对比验证。结果表明:密封环端面的平均膜压随圆台型织构间距、小径的增大而减小,随织构大径的增大而增大;存在最佳织构深度使平均膜压最大;润滑介质黏度越大,密封环端面平均膜压越大;粗糙峰峰高越大,端面平均膜压越小,而粗糙峰波长对端面平均膜压的影响较小,因此粗糙峰应尽可能小;存在织构参数、粗糙度参数的最优组合使润滑膜平均压力值达到最大。     

氧化石墨烯添加剂对基础油成膜特性的影响

为了探究氧化石墨烯(GO)添加剂在不同润滑状态下对基础油成膜特性的影响,利用原子力显微镜(AFM)和傅里叶变换红外光谱仪(FTIR)分别对GO的厚度、层数和表面官能团进行表征,选用聚α-烯烃(PAO10)和聚醚(PAG)为基础油,利用球-盘点接触光干涉油膜厚度测量试验台,研究GO添加剂在弹流润滑和混合润滑状态下对不同基础油润滑成膜性能的影响。结果表明：在全膜润滑状态下,GO对PAO10和PAG基础油的成膜能力影响很小,添加GO前后基础油的最小膜厚相差并不大;在混合润滑状态下,GO可有效地提高PAO10基础油的最小膜厚,减缓接触区内的乏油状况,而对PAG基础油成膜性能的影响很小。     

Single-molecule near-field optical energy transfer microscopy with dielectric tips

The fluorescence lifetime and the fluorescence rate of single molecules are recorded as a function of the position of a Si₃N₄ atomic force microscopy tip with respect to the molecule. We observe a decrease of the excited state lifetime and the fluorescence rate when the tip apex is in close proximity to the molecule. These effects are attributed to the fact that the dielectric tip converts non‐propagating near‐fields to propagating fields within the dielectric tip effectively quenching the fluorescence. The spatial extension of the quenching area is of subwavelength dimensions. The results are discussed in terms of molecular fluorescence in a system of stratified media. The experiment provides surprising new insights into the interactions between a fluorescent molecule and a dielectric tip. The methodology holds promise for applications in ultra high‐resolution near‐field optical imaging at the level of single fluorophores.     

Atomic force microscopy of protein films and crystals

A customized atomic force microscopy (AFM) instrument optimized for imaging protein crystals in solution is described. The device was tested on crystals and Langmuir-Blodgett (LB) films of two proteins with quite different molecular weights. This approach enables the periodicity and morphology of crystals to be studied in their mother liquid, thereby preserving the native periodic protein crystal structure, which is typically destroyed by drying. Moreover, the instrument appears to distinguish protein crystals from salt crystals, which under the optical microscope are frequently quite similar, the difference between them often being revealed only during x-ray analysis. AFM estimates of the packing, order, and morphology of the given single proteins appear quite similar in the LB thin film and in the crystals, which means that routine crystal measurements can be performed at high resolution. The AFM consists of a custom-built measuring head and a homemade flexible SPM controller which can drive the head for contact, noncontact and spectroscopy modes, thus providing the user with a high degree of customization for crystal measurement.