The extended surface forces apparatus. IV. Precision static pressure control

We report on design and performance of an extended surface forces apparatus (eSFA) built into a pressurized system. The aim of this instrument is to provide control over static pressure and temperature to facilitate direct surface force experiments in equilibrium with fluids at different loci of their phase diagram. We built an autoclave that can bear a miniature eSFA. To avoid mechanical or electrical feedtroughs the miniature apparatus uses an external surface coarse approach stage under ambient conditions. The surface separation is thus pre-adjusted to approximately ~3 μm before sliding the apparatus into the autoclave. Inside the autoclave, the surface separation can be further controlled with a magnetic drive at sub-?ngstrom precision over a 14 μm range. The autoclave pressure can then be set and maintained between 20 mbar and 170 bars with few mbar precision. The autoclave is connected to a specially designed pressurization system to precondition the fluids. The temperature can be controlled between -20 and 60 °C with few mK precision. We demonstrate the operation of the instrument in the case of gaseous or liquid carbon dioxide. Thanks to a consequent decoupling of the eSFA mechanical loop from the autoclave structure, the obtained measurement stability and reproducibility, at elevated pressures, is comparable to the one established for the conventional eSFA, operated under ambient conditions.     

What determines static friction and controls the transition to sliding?

We studied the shear response of a confined lubricant layer on approach of the transition to sliding with a surface force apparatus modified for oscillatory shear. In a given experiment, we found that the transition to sliding occurred always around the same deformation amplitude although the shear stress needed to initiate sliding varied up to a factor of two depending on sample history. This suggests the concept of deformation-controlled switching from rest to sliding. The elastic spring-constant, in the stick state, weakened with increasing deformation amplitude. This decrease can be described by a power law when plotted versus the distance to a critical deformation amplitude. The build-up of solid-like behavior after sliding stopped was also gradual and was consistent with a logarithmic time dependence. We suggest a model relating the gradual decrease of stiffness to weakening of the boundary layer, specifically to destruction of some elastic links between molecules or between molecules and the solid surfaces. Static friction (the force that must be overcome at the onset of kinetic motion) is proportional to the number of such links formed during the time of stick.     

单晶硅在氮离子注入前后的力学性能研究

以微机电系统常用的单晶硅材料和经氮离子注入单晶硅后形成的表面改性层为研究对象,在原位纳米力学测试系统上进行微压痕实验,对样品的表面纳米硬度进行了测试。同时,还通过该仪器的原子力成像功能对实验区域扫描成像,在纳米尺度下观察和分析形貌。结果表明:单晶硅在氮离子注入前后的纳米硬度值与载荷有很大关系。通过对微压痕和原子力图像的分析,表明单晶硅在氮离子注入后的纳米硬度值有所降低,其主要原因是氮离子注入后导致晶格抵抗变形的能力降低。     

异形内孔曲面的磨料流均匀加工方法研究

针对磨料流加工异形曲面一致性较差的问题,提出通过设置相似模芯结构以改善剪切应力分布的状态,从而实现均匀化加工异形曲面的方法。根据磨料流的剪切率与黏度的关系建立了幂律模型,通过COMSOL Multiphysics软件的 CFD模块计算得到置入模芯时磨料介质在加工表面的速度、剪切率和剪切应力的分布。仿真与实验表明:置入相似的模芯后可形成等宽的流道,各曲面受到的剪切应力趋向一致。工件内壁表面粗糙度Ra最大差值由无模芯时的0.376μm降为置入模芯后的0.017μm。     

泥水盾构接管用三通换向阀橡胶阀座密封研究

针对泥水盾构接管用三通换向阀密封结构易发生泄漏的问题,对三通换向阀橡胶阀座的密封特性进行研究,为提高其密封可靠性采用双道密封结构。建立双道密封结构二维有限元分析模型,对比分析橡胶双道密封在不同侧向介质压力、不同压缩量及不同倒角半径下的密封特性。结果表明:双道密封结构的von Mises应力与剪切应力与所受压缩量与侧向介质力呈线性关系;侧向介质力与倒角半径对第一道密封面的接触应力影响较大;密封面左侧的接触应力较高,第二道密封面的接触应力基本不变;当所受压缩量为2.0 mm,介质压力为1.5 MPa时,双道密封结构的综合密封性能最优。     

Study of thin surfactant films under shear using the tribological surface force apparatus

Static and dynamic behaviour of thin surfactant films in aqueous solution of hexadecyltrimethylammonium salicylate (C16TASal) were investigated using the tribological surface force apparatus. Normal force measurements show that 0.15 mM C16TASal builds up an innermost film of approximately 8–11 Å thickness at each mica surface, indicating that the surfactant adsorbs in a flat conformation. Furthermore, the height of the force barrier at approximately 60Å is low (ca 2 mN/m) indicating that the second adsorbed layer is easily pushed out. Addition of salicylate salt to 0.15 mM C16TASal give rise to a more close packed structure, with a total thickness of 62–65 Å, indicative of a micellar or bilayer arrangement at the surfaces. Furthermore, the frequency dependence of the shear modulus was investigated both at close separation at the innermost force barrier and at larger separations (up to 300–400 Å). The visco-elastic measurements show that the elasticity modulus, G′, dominates over the loss modulus, G″, for all studied cases, indicative of a more solid-like than liquid-like film. Finally, it is shown that shear at high contact pressures induces new aggregate structures at the surface.     

中间层液体的表面能对粘着行为中Pull-off力影响的实验研究

中间层液体膜存在的情况下,弯月面力(Cap illary Force)的作用使Pull-off力增加。中间层液体的表面能是影响弯月面力作用强度的重要因素之一。利用表面张力仪测量了1,2二氯丙烷、1,2乙二醇等5种液体的表面能,利用表面力仪测量了这5种液体作为中间层时Pull-off力的值。结果表明,在一定范围内,粘度相近液体量相同时,Pull-off力随表面能增加而增加;表面能相等时,Pull-off力随液体量增加而增加。     

Modification of Boundary Lubrication by Oil-Soluble Friction Modifier Additives

The molecular-level function of model and commercial friction modifier additives in lubricants of the type used at the wet clutch interface in automatic transmissions has been studied using a surface forces apparatus (SFA) modified for oscillatory shear. The nanorheological properties of tetradecane with and without a model friction modifier additive (1-hexadecylamine) were examined in the boundary lubrication regime and compared to a fully-formulated automatic transmission fluid (ATF). 1-Hexadecylamine adsorbed as a single layer on the sliding surfaces, reduced the static frictional force and the limiting shear stress, and eliminated the stick–slip transition that exists in pure tetradecane. The ATF, which contains commercial-grade friction modifiers, showed nanorheological properties similar to those observed for tetradecane containing 0.1–0.2 wt% 1-hexadecylamine.     

基于高精度位移传感器的新型减振平台

为了保证光学精密仪器工作基础的高稳定性,设计了一种新型的减振平台,该减振平台采用精度为0.1nm的位移传感器作为测量装置,通过位移传感器测量隔振平台支撑弹簧的长度变化,计算出支撑力的变化,然后调整电磁驱动器的电磁力,使光学精密仪器受力平衡,达到减振的目的。经过理论分析及仿真分析,采用这种减振方式能够到达减振要求,同时,这种减振方式有利于多级减振,每级减振装置之间是彼此相互独立的。     

Possibility of slip in hydrodynamic oil films under sliding contact conditions

In hydrodynamic lubrication theory, the oil film thickness build‐up increases with increasing sliding speed or oil viscosity, and the viscous resistance or shear stress also increases, both without limit. The entraining force forming the oil film is given by the moving surfaces, or by the adhesive force of the oil molecules on the rubbing surfaces and the interaction force between them. Therefore, the maximum friction force and maximum oil film thickness will be limited by the operating conditions, such as oil properties, rubbing materials, sliding speed, and load. In this study, friction tests were conducted using a plate‐on‐cylinder sliding contact apparatus. It was found that a critical shear stress existed, above which the friction force and oil thickness decreased from theoretical values. Slip in an oil film seems to occur when the theoretical shear stress exceeds the critical value of the oil, according to test conditions. The occurrence of slip in an oil film is responsible for the reduction in the oil film and friction force from theoretical values, leading to the lower‐viscosity components of the oil selectively passing through the conjunction zone.     

A rheo-optical apparatus for real time kinetic studies on shear-induced alignment of self-assembled soft matter with small sample volumes

In soft materials, self-assembled nanoscale structures can allow new functionalities but a general problem is to align such local structures aiming at monodomain overall order. In order to achieve shear alignment in a controlled manner, a novel type of rheo-optical apparatus has here been developed that allows small sample volumes and in situ monitoring of the alignment process during the shear. Both the amplitude and orientation angles of low level linear birefringence and dichroism are measured while the sample is subjected to large amplitude oscillatory shear flow. The apparatus is based on a commercial rheometer where we have constructed a flow cell that consists of two quartz teeth. The lower tooth can be set in oscillatory motion whereas the upper one is connected to the force transducers of the rheometer. A custom made cylindrical oven allows the operation of the flow cell at elevated temperatures up to 200 degrees C. Only a small sample volume is needed (from 9 to 25 mm(3)), which makes the apparatus suitable especially for studying new materials which are usually obtainable only in small quantities. Using this apparatus the flow alignment kinetics of a lamellar polystyrene-b-polyisoprene diblock copolymer is studied during shear under two different conditions which lead to parallel and perpendicular alignment of the lamellae. The open device geometry allows even combined optical/x-ray in situ characterization of the alignment process by combining small-angle x-ray scattering using concepts shown by Polushkin et al. [Macromolecules 36, 1421 (2003)].     

Modifications to a fretting-fatigue testing apparatus based upon an analysis of contact stresses at complete and nearly complete contacts

An earlier form of fretting-fatigue test apparatus employs two collinear hydraulic actuators to impose bulk tension and shear. This apparatus employed a Hertzian contact to induce well-defined tractions. However, it is very difficult to make use of information culled from such tests in designing contacts which are either complete or almost complete in nature. A modified apparatus for investigating experimentally fretting fatigue under complete and nearly complete contact conditions is described. For these cases, any misalignment in the plane of the contact would alter the contact pressure distribution significantly leaving the results of the test questionable. Additionally, when applying a shearing force, it should be in the plane of the contact, eliminating the risk of a rocking moment which would otherwise have a similar effect. Here, we describe a testing apparatus that allows the above two issues to be addressed and resolved. The contact then sits in its “natural position” on the test specimen and the applied shearing force is in the plane containing the contact. Further implications for the development of the coefficient of friction are discussed.     

Dynamic modeling of oblique non-uniform piezoelectric MC in liquid with various percentages of glycerin in the presence of rough surface

One of the most useful applications of an AFM is imaging of biological particles in a liquid medium. The increase of the topography accuracy in a liquid medium requires accurate dynamic modeling of a Microcantilever (MC). This article investigates the accurate dynamic modeling of the non-uniform AFM piezoelectric MC with rectangular geometry in the amplitude mode in liquid medium for rough surfaces. To increase the accuracy of the modeling, the Modified couple stress (MCS) theory in the liquid medium according to the Timoshenko beam model has been used. Moreover, the differential quadrature (DQ) method has been used for solving equations, because in comparison with the other methods it has a high speed in solving equations and is accurate in the number of fewer elements. In addition, the accurate force modeling has been established by considering the shear forces caused by liquid on the sides of the piezoelectric MC by solving the Navier-Stokes equations, and by considering the hydrodynamic force, squeeze force and applied forces between the sample surface and the MC tip. The results illustrate that utilizing higher vibration modes affect the quality of rough surface topography with the step roughness in the liquid medium and increase the quality of surfaces topography in the tapping mode, especially in the second MC vibration mode. Moreover, it should be noted that the sensitivity of the MC vibration amplitude to the piezoelectric MC angle is higher in comparison with other investigated parameters.     

Creating a high temperature environment at high pressure in a gas piston cylinder apparatus

An internal heater capable of 1400 K has been developed for use with a gas piston cylinder apparatus capable of achieving in excess of 3 GPa with an argon pressure medium. The heated gas piston cylinder produces a truly hydrostatic environment for samples up to 3 mm in diameter and 8 mm in length. The apparatus can be used to study systems that are sensitive to stress or samples that cannot withstand shear tractions. The gas piston cylinder apparatus was developed in an effort to reduce experimental uncertainty in the pressure scale and has been used to improve understanding of the Bi I-II transition at 298 K. We estimate that the pressure during a high temperature soak in the gas piston cylinder can be known to within ±0.01 GPa.     

表面波度对液体椭圆孔端面密封上游泵送特性的影响

表面波度与端面几何型槽的耦合影响使得密封性能的变化规律更为复杂。基于粗糙和波度表面假设,建立空化效应下端面椭圆孔液体上游泵送密封的理论分析模型,对上游泵送端面密封的压力分布和泄漏率进行数值求解计算,分析周向表面波度幅值、数量等几何参数和转速、密封压力等操作参数对开启力和泄漏率的影响规律。结果显示：表面波度使得密封端面产生更高的流体动压效果,并减弱上游泵送效果,容易导致密封介质的泄漏;随着波高和周向波数的增加,开启力略有增加;泄漏率随着波高的增加呈现正向增强趋势,但波数对泄漏率没有明显影响;在空化效应和表面波度的影响下,速度剪切产生的密封端面开启力可增加50%以上,并形成流体的完全上游泵送;密封压力和膜厚的增加,使得流体的上游泵送性能和密封性下降。     

Shear force distance control in near-field optical microscopy: experimental evidence of the frictional probe-sample interaction

The properties of the probe-surface contact for a near-field optical microscope driven in the shear force mode have been studied applying lateral amplitudes of the probing fiber tip larger than 15 nm. Electric current measurements between a conductive tip and a conductive sample reveal a pulsed current behavior at the very beginning of the approach curve. In the upper part of the approach curve it turns to the quasiconstant current. From this observation a conclusion is drawn about the presence of permanent mechanical contact between the probe and the surface in the shear force mode. A shift of the approach curve along the z-axis as a function of dither amplitude was discovered. These results are in contradiction to the established conception of possible physical mechanisms of shear force interaction. To settle this issue the friction model is proposed according to which the damping of the probe vibrations is caused by the friction between the tip and the surface.     

Research on unbounded abrasive polishing process with assisted ultrasonic vibration of workpiece

Ultrasonic-assisted machining was an effective method to improve the material removal quality especially to difficult-to-cut metal materials. The ultrasonic vibration was usually superimposed on the machining tool but seldom on the workpiece, although the ultrasonic vibration of workpiece could improve the processability of material more effectively. In this paper, a rectangle hexahedron ultrasonic sonotrode with optimized slots was developed as a platform to realize the assisted ultrasonic vibration of workpiece and the ultrasonic-assisted polishing process of austenitic stainless steel was also studied. The unbounded abrasive was selected as polishing medium, and the path compensation strategy of soft polishing tool was carried out for getting uniform polishing force. The orthogonal experiments were designed to study the optimization of ultrasonic polishing parameters and the relation between different types of ultrasonic polishing path and polishing quality. The results appear that the horizontal ultrasonic vibration of workpiece can reduce polishing force and improve polished surface roughness, which can also reinforce the proportion of plastic shear effect in the material removal process. The ultrasonic polishing path keeping consistent with workpiece vibration direction can get more uniform polishing force and better surface roughness. And the 45° oblique crossing ultrasonic path can get the maximum average polishing force reduction by 75.2 %.     

Specialized scanning ion-conductance microscope for imaging of living cells

A specialized scanning ion conductance microscope (SICM) for imaging living cells has been developed from a conventional patch-clamp apparatus, which uses a glass micropipette as the sensitive probe. In contrast with other types of scanning probe microscope, the SICM probe has significant advantages for imaging living cells: it is most suitable for imaging samples immersed in water solutions; and since the probe senses ion current and does not need physical contact with the sample during the scan, any preliminary preparation of cells (fixation or adherence to a substrate) is unnecessary. We have successfully imaged murine melanocytes in growth medium. The microscope images the highly convoluted surface structures without damaging or deforming them, and reveals the true, three-dimensional relief of the cells. This instrument has considerable ability to operate, potentially simultaneously, in applications as diverse as real-time microscopy, electrophysiology, micromanipulation and drug delivery.     

An alternative method for the measurement of the mechanical impulse of a vertically directed blast

An alternative method for the measurement of the total mechanical impulse of a vertically directed blast due to an explosive charge is presented. The method differs from apparatus that employ a vertically displaced mass (similar in principle to the ballistic pendulum) in that a relatively compact spring-damper system is employed to constrain the movement of the mass. The mechanical impulse is determined by integrating, with respect to time, the net force applied to the spring-damper system. The details of an explosive impulse measuring instrument rated to 12 kN s are presented.     

Shear-induced dilation of confined liquid films

We demonstrate that sheared molecularly-thin fluid films dilate at the point of stick-to-slip (which is the transition from static to kinetic friction), indicating that density decreases when sliding occurs. This contrasts with incompressibility characteristic of bulk fluids when they are deformed. The magnitude of dilation was less than the size of the molecule and was larger in a polymer system (large molecules) than for small-molecule fluids. The experiments employed a surface forces apparatus modified to measure, using piezoelectric methods, sub-angstrom variations of film thickness during dynamic shear excitations that were performed at rates too rapid to allow fluid to enter and exit the zone of shear contact during the period of shear excitation. To demonstrate generality of the dilation effect, the specific systems studied included nonpolar fluids whose complexity was varied (a globular-shaped molecule, OMCTS; a branched alkane, squalane; a tethered diblock copolymer, polyvinylpyridine–polybutadiene) and also an aqueous electrolyte, MgCl₂ dissolved in water. Extensive analysis is also presented of the piezoelectric methods that were employed to detect volume changes too small to observe by the methods of multiple beam interferometry that are traditional for thickness measurement in a surface forces apparatus.