A force-matching method for quantitative hardness measurements by atomic force microscopy with diamond-tipped sapphire cantilevers

We present a new method to improve the accuracy of force application and hardness measurements in hard surfaces by using low-force (<50 μN) nanoindentation technique with a cube-corner diamond tip mounted on an atomic force microscopy (AFM) sapphire cantilever. A force calibration procedure based on the force-matching method, which explicitly includes the tip geometry and the tip-substrate deformation during calibration, is proposed. A computer algorithm to automate this calibration procedure is also made available. The proposed methodology is verified experimentally by conducting AFM nanoindentations on fused quartz, Si(1 0 0) and a 100-nm-thick film of gold deposited on Si(1 0 0). Comparison of experimental results with finite element simulations and literature data yields excellent agreement. In particular, hardness measurements using AFM nanoindentation in fused quartz show a systematic error less than 2% when applying the force-matching method, as opposed to 37% with the standard protocol. Furthermore, the residual impressions left in the different substrates are examined in detail using non-contact AFM imaging with the same diamond probe. The uncertainty of method to measure the projected area of contact at maximum force due to elastic recovery effects is also discussed.     

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.     

Subpixel edge location method proposed to improve the performance of optical fiber spherical coupling probe during dimensional measurement of micro-cavities with high aspect ratio

A subpixel edge location method based on orthogonal Jacobi–Fourier moments is proposed in this paper to improve the performance of optical fiber spherical coupling probe during dimensional measurement of micro-cavities with high aspect ratio. The effectiveness of the proposed method is proved through the performance test of a micro-hole measuring machine with optical spherical coupling probe. Test results indicate that a blind micro-hole of 400 μm in diameter can be experimentally measured at the depth of 2000 μm with a repeatability of 40 nm and an extremity resolution of 42 nm.     

An all-fiber Fabry-Pérot interferometer for pressure sensing in different gaseous environments

A gas pressure sensor based on an all-fiber Fabry-Pérot interferometer (FFPI) is reported. The sensing head consists of a small section of silica rod spliced with a large offset between two single-mode fibers. The silica rod is used only as mechanical support so that an air cavity can be formed between both SMF. It is shown that the FFPI sensor is sensitive to gas pressure variation and when submitted to different gaseous environments, namely carbon dioxide, nitrogen and oxygen – sensitivities of 6.2, 4.1 and 3.6 nm/MPa, respectively, were attained. The refractive index change on nitrogen environment by means of gas pressure variation was also determined and a sensitivity of 1526 nm/RIU was obtained. The response of the sensing device to temperature variations in air was also studied and a sensitivity of −14 pm/°C was attained.     

Mechanical and tribological properties of NiCr–Al2O3 composites at elevated temperatures

The effect of Al₂O₃ content on the mechanical and tribological properties of Ni–Cr alloy was investigated from room temperature to 1000 °C. The results indicated that NiCr–40 wt% Al₂O₃ composite exhibited good wear resistance and its compressive strength remained 540 MPa even at 1000 °C. The values obtained for flexural strength and fracture toughness at room temperature were 771 MPa, 15.2 MPa m^1/2, respectively. Between 800 °C and 1000 °C, the adhesive and plastic oxide layer on the worn surface of the composite was claimed to be responsible for low friction coefficient and wear rate.     

Characteristics of a dynamic atomic force microscopy based on a higher-order resonant silicon cantilever and experiments

In order to improve the sensitivity and scanning speed of the dynamic AFM, a surface scanning method using higher-order resonant cantilever is adopted and investigated based on the higher-order resonance characteristics of the silicon cantilever, and the theoretical analysis and experimental verification on the higher-order resonance characteristics of the corresponding dynamic AFM cantilever are given. In this method, the cantilever is excited to oscillate near to its higher-order resonant frequency which is several times higher than that of the fundamental mode. Then the characteristic changes a lot compared with the first-order resonant cantilever. Because of the changes of the quality factor, amplitude and the mode shape of the cantilever, the higher-order resonant AFM gets higher sensitivity and scanning speed. Based on the home-built tapping-mode AFM experiment system, the resolution and the response time of the first and second order resonance measured by experiment are respectively: 0.83 nm, 0.42 nm; 1265 μs, 573 μs. The higher-order resonance cantilever has higher sensitivity and the dynamic measurement performance of the cantilever is significantly improved from the experimental results. This can be a useful method to develop AFM with high speed and high sensitivity. Besides above, the surface profile of a grating sample and its three-dimensional topography are obtained by the higher-order resonant mode AFM.     

Simultaneous interferometric measurement of the absolute thickness and surface shape of a transparent plate using wavelength tuning Fourier analysis and phase shifting

The absolute optical thickness and surface shape of optical devices are considered as the fundamental characteristics when designing optical equipment. The thickness and surface shape should be measured simultaneously to reduce cost. In this research, the absolute optical thickness and surface shape of a 6–mm-thick fused silica transparent plate of diameter 100 mm was measured simultaneously by a three-surface Fizeau interferometer. A measurement method combining the wavelength tuning Fourier and phase shifting technique was proposed. The absolute optical thickness that corresponds to the group refractive index was determined by wavelength tuning Fourier analysis. At the beginning and end of the wavelength tuning, the fractional phases of the interference fringes were measured by the phase shifting technique and optical thickness deviations with respect to the ordinary refractive index and surface shape were determined. These two kinds of optical thicknesses were synthesized using the Sellmeier equation for the refractive index of fused silica glass, and the least square fitting method was used to determine the final absolute optical thickness distribution. The experimental results indicate that the all the measurement uncertainties for the absolute optical thickness and surface shape were approximately 3 nm and 35 nm, respectively.     

Digital filtering methodology used to reduce scale of measurement effects in roughness parameters for magnetic storage supersmooth hard disks

Roughness of disk media influences the tribological interaction of head-disk interfaces, especially when the intended flying-height is below 5 nm that is required to achieve extremely high-density recording (EHDR). Roughness parameters such as the root-mean-square (RMS) amplitude, however, are influenced by the scale of measurement, such as the scan size. Effects related to scale of measurement such as varying the scan size were investigated and means to reduce such effects were proposed by establishing an “ad hoc” digital filtering procedure. Two types of magnetic disks intended for EHDR were measured by an atomic force microscope (AFM) at various scan dimensions ranging from 0.5 μm × 0.5 μm to 112 μm × 112 μm. The proposed filtering method used the RMS values as a filter design parameter for choosing the appropriate high-pass cutoff wavelength for each scan size. The study revealed the existence of a unique cutoff wavelength that would identify different wavelength regimes and the associated critical scan size in each disk. To substantiate the effectiveness of the proposed filtering method in reducing the scale of measurement effects related to the scan size, other roughness parameters were also calculated subsequent to the filtering procedure. It was found that the proposed filtering scheme effectively reduced the scale of measurement effects in the amplitude parameters (e.g., RMS and the ten-point height variation) and the functional parameters (e.g., material and core void volumes). These parameters exhibited steady-state trends with respect to increasing scan size, indicating reduced scale of measurement effects.     

Friction and wear durability studies on the 3D negative fingerprint and honeycomb textured SU-8 surfaces

The effects of two different textures (a 3D negative fingerprint texture and a honeycomb texture) on the tribological performance of SU-8 polymer surface have been investigated with a ball-on-disc tribometer. Friction and wear behaviors of the textured surfaces are conducted against a 4 mm diameter silicon nitride (Si₃N₄) ball counterface. The coefficient of friction for the negative fingerprint textured surface (μ=∼0.08) is much lower than that of the untextured surface (∼0.2) and the honeycomb textured surface (∼0.41) under a normal load of 100 mN and a rotational speed of 2 rpm. The coefficients of friction of the textured surfaces decrease with increasing normal loads between 100 mN and 300 mN. Above the normal load of 300 mN, the coefficient of friction of the negative fingerprint textured surface increases due to the occurrence of plastic deformation. The honeycomb textured surface has shown the highest coefficient of friction. The wear durability tests are also conducted at a normal load of 100 mN and a rotational speed of 500 rpm on the untextured/textured surfaces on SU-8 in the presence of an overcoat of a nano-lubricant, perfluoropolyether(PFPE). Six samples i.e. the untextured surface (Si/SU-8 and Si/SU-8/PFPE), the 3D negative fingerprint textured surface (Si/SU-8/FP and Si/SU-8/FP/PFPE) and the honeycomb textured surface (Si/SU-8/HC and Si/SU-8/HC/PFPE), each with and without PFPE nano-lubricant, have been investigated for their tribological behaviours. The negative fingerprint pattern on SU-8 with PFPE coating has shown the highest wear life of 60,000 cycles under a normal load of 100 mN. The reasons for excellent tribological performance of 3D fingerprinted SU-8 surface are analyzed using the Hertzian contact area calculation.     

A novel method for micro-gap control in electrogenerated chemical polishing

In the electrogenerated chemical polishing (EGCP), material removal rate (MRR) is inversely proportional to the processing gap. To polish a workpiece with a large area, high and uniform MRR is necessary, which prefers a small and uniform processing gap. Based on the principle of the hydrostatic support, a novel micro-gap control method is proposed. The method uniformly controls the gap between the electrode and workpiece to a micro level over a large area. A relationship between the gap size and the inlet pressure is derived theoretically and verified experimentally. The proposed method is successfully applied to the polishing of a Cu surface with a diameter of 50 mm. Promising results are obtained that surface roughness and flatness are reduced from average roughness (Ra) 82 nm and peak-to-valley (PV) value 290 nm to Ra 4 nm and PV 120 nm, respectively.     

Tribological performance of silicone composite coatings filled with wax-containing microcapsules

The effect of wax-containing microcapsules incorporated in silicone composite coatings deposited on aluminum (Al) alloy substrates on the tribological performance of the coatings was systematically investigated. The wax-containing microcapsules were prepared via in situ polymerization. The tribological behavior of the composite coatings was evaluated using ball-on-disk tribological test. It was found that the increase in microcapsule concentration in the composite coatings apparently reduced the friction coefficient of the coatings because the lubricant released from the broken microcapsules during the tribological test of the coatings lubricated the rubbing surfaces. The results showed that the silicone composite coatings rubbed by a smaller Cr6 steel ball (3 mm diameter) under a lower normal load (100 mN) produced higher friction coefficients via reduced complication of their underlying strong substrates compared to the same coatings tested against a larger Cr6 steel ball (6 mm diameter) under a higher normal load (1 N).     

Study of TiAlSiN coatings post-treated with N and C + N ion implantations. Part 2: The tribological analysis

Ion implantation has found to be an effective approach to modify surface properties of materials. The present research investigates the effect of (1) nitrogen (N), and (2) carbon subsequently with nitrogen (C + N) implantations on the mechanical and tribological properties of the titanium–aluminium–silicon–nitride (Ti–Al–Si–N) coatings. Superhard TiAlSiN coatings produced by magnetron sputtering, of approximately 2.5 μm thickness, were post-treated by implantations of N or C + N at an energy level of 50 keV. The dose range was between 5 × 10¹⁶ and 1 × 10¹⁸ ions cm^?2. After implantation, the tribological performance of the coatings was investigated by a ball-on-disk tribometer against WC–6 wt.%Co ball under dry condition in ambient air. The wear performance of the samples was examined by a variety of characterization techniques, such as secondary electron microscopy (SEM), 3D profilometry, atomic force microscopy (AFM), and micro-Raman. The results showed that the wear performance of the samples depended strongly on the implanted elements and doses. There was slight improvement on the samples implanted with N whereas significant improvement was found on the C + N implantations. Particularly, the friction coefficient of the sample with 5 × 10¹⁷ C⁺ cm^?2 and 5 × 10¹⁷ N⁺ cm^?2 could reach 0.1. In addition, the specific wear rate of the sample was extremely low (0.85 × 10^?7 mm³/Nm), which was nearly two orders of magnitude below that of the un-implanted coating. The speculation of the mechanical and tribological analyses of the samples indicates that the improvement of the N implanted and C + N implanted TiAlSiN samples could be due to a combined effect of improved hardness, plus enhanced adhesive and cohesive strength. In addition, the improved performance of the C + N implanted samples could be explained by the formation of lubricating implanted-layer, which existed mostly in sp² C–C and C–N forms. The formation of such implanted layer could lead to a change of wear mode from strong abrasive wear to mostly adhesive wear, and result in a drop of friction coefficient and wear rate.     

Atomic force microscope probe calibration by use of a commercial precision balance

In this paper, we investigate the characteristics of a piezoresistive AFM cantilever in the range of 0–1.6 μN by using nano force calibrator (NFC), which consists of a high precision balance with resolution of 1 nN and 1-D fine positioning stage. Brief modeling of the cantilever is presented and then, the calibration results are shown. Tests revealed a linear relationship between the probing force and sensor output (resistance change), but the force vs. deflection is not as linear as the force vs. sensor output curve. The force constant of the cantilever was measured to 0.26 N/m with a standard deviation of 0.01 N/m. It shows that there is big difference between measured and nominal spring constant of 1 N/m provided by the manufacturer’s specifications.     

Characterization and tribological investigation of sol–gel ceramic films on Ti–6Al–4V

SiO₂, TiO₂, and hydroxyapatite (HA) thin films with good biocompatibility were grown on Ti–6Al–4V (coded as TC4) substrate by sol–gel and dip-coating processes from specially formulated sols, followed by annealing at 500 °C The chemical states of some typical elements in the target films were detected by means of X-ray photoelectron spectroscopy (XPS). Atomic force microscopy (AFM) and high-resolution scanning electron microscopy (SEM) are applied to characterize the original unworn films. The tribological properties of thin films sliding against an AISI52100 steel ball were evaluated on a reciprocating friction and wear tester. As the result, the target films composed of nano-particles ranging from 30 nm to 100 nm around were obtained. All the sol–gel ceramic films are superior in resisting wear compared with the TC4 substrate. Among all, HA film shows the best resistance while SiO₂ film shows the worst wear resistance both under higher (3 N) and lower load (1 N). TiO₂ shows good wear resistance under lower load (1 N). SEM observation of the morphologies of worn surfaces indicates that the wear of TC4 is characteristic of abrasive wear. Differently, abrasion, plastic deformation and micro-fracture dominate the wear of ceramic films. The superior friction reduction and wear resistance of HA film is greatly due to the slight plastic deformation of the film. It is supposed that the deformation of the HA film is closely related to the special arrangement of the nano-particles and microstructure. HA film is recommended for clinical application from the point of wear resistance view.     

Nanowire cutting by an ultrasonically vibrating micro tool

Cutting of a nanoscale workpiece is useful in nano testing and fabrication, and novel cutting methods with little gasification of cut nano samples and simple device structures are needed for practical applications. In this paper, an ultrasonic nanowire cutting strategy is demonstrated, in which the linear and elliptical vibration of the tip of a micro cutting tool and the adhesion force between a substrate and nanowire are employed to cut and fix the nanowire, respectively. With this strategy, cutting of individual silver nanowires with a diameter from 50 nm to 400 nm is implemented, in which the vibration velocity amplitude of the micro cutting tool’s root is from 18 to 220 mm/s, and the working frequency is about 96.9 kHz and 45.2 kHz, respectively. The dependency of the minimum cutting velocity and optimum cutting velocity range’s lower limit on the AgNW diameter is experimentally clarified. Also, the cutting principle is analyzed, which can well explain the incision morphology and cutting characteristics.     

A long-stroke 3D contact scanning probe for micro/nano coordinate measuring machine

This paper presents a long-stroke contact scanning probe with high precision and low stiffness for micro/nano coordinate measuring machines (micro/nano CMMs). The displacements of the probe tip in 3D are detected by two plane mirrors supported by an elastic mechanism, which is comprised of a tungsten stylus, a floating plate and two orthogonal Z-shaped leaf springs fixed to the outer case. A Michelson interferometer is used to detect the vertical displacement of the mirror mounted on the center of the floating plate. An autocollimator based two dimensional angle sensor is used to detect the tilt of the other plane mirror located at the end of the arm of the floating plate. The stiffness and the dynamic properties are investigated by simulation. The optimal structural parameters of the probe are obtained based on the force-motion model and the constrained conditions of stiffness, measurement range and horizontal size. The results of the performance tests show that the probe has a contact force gradient within 0.5 mN/μm, a measuring range of (±20 μm), (±20 μm), and 20 μm, respectively, in X, Y and Z directions, and a measurement standard deviation of 30 nm. The feasibility of the probe has preliminarily been verified by testing the curved surface of a convex lens.     

Formation and tribological properties of hollow sphere-like nano-MoS2 precipitated in TiO2 particles

MoS₂ hollow spheres with an average diameter of 165 nm were prepared from Na₂MoO₄ and CH₃CSNH₂ at 82 °C. A simple method was used to obtain smaller hollow spheres (70 nm) without any complicated step, except for the addition of TiO₂. The tribological properties of MoS₂/TiO₂ in rapeseed oil were studied using a four-ball tribometer under 350 N at 0.383 m/s. The effects of load and sliding velocity were also investigated. Wear was significantly alleviated by the produced lubricating film as lubricated with MoS₂/TiO₂, which was composed of MoO₃, Fe₂O_3, Fe₂(SO₄)₃, TiO₂ (trace), and carbon-containing compounds. The tribological properties were also improved because of the decrease in the size of MoS₂ and the synergistic effect between MoS₂ and TiO₂.     

Uncertainty analysis of slot die coater gap width measurement by using a shear mode micro-probing system

A shear mode micro-probing system was constructed for gap measurement of a precision slot die coater with a nominal gap width of 90 μm and a length of 200 mm. A glass micro-stylus with a nominal tip ball diameter of 52.6 μm was oscillated by a tuning fork quartz crystal resonator with its oscillation direction parallel to the measurement surfaces. An on-line qualification setup was established to compensate for the influences of the uncertainty sources, including the water layers on the measurement surfaces. The measurement uncertainty of the measured gap width was estimated to be less than 100 nm.     

Micro-scale hole profile measurement using rotating wire probe and acoustic emission contact detection

The development of a new probing method to inspect the inner diameter of micro-scale holes is presented in this paper. This was accomplished by contact detection using acoustic emission with a Ø170 μm rotating wire probe tip. Contact is detected when the rotating probe approaches and impacts the hole’s inner surface. The effective diameter of the rotating probe is calibrated by using a high precision grade 0 Mitutoyo gauge block. The wire rotating probe used was fabricated with micro stainless steel wire and micro tubes. The probe’s effective diameter was compensated for in the measurement of the hole. The probe was used to measure the diameter and the roundness of micro-scale holes. Probes used in previous publications have different geometry than the probe in this paper and are used almost exclusively for external dimensions. Micro-scale holes of less than 1.0 mm in diameter and 10 mm in depth are successfully measured and the 3D profile is created accordingly. Also, the out-of-roundness values of each level spacing, 50 μm apart in height, are calculated.