Position-resolved Surface Characterization and Nanofabrication Using an OpticalMicroscopeCombined with a Nanopipette/Quartz Tuning Fork Atomic Force Microscope

Quartz tuning fork (QTF) sensors offer an attractive alternative to traditional silicon microcantilevers for sensing applications in dynamic atomic force microscopy (DAFM). The QTF sensor consists of two identical, weakly-coupled tines with a sharp tip affixed to the distal end of one tine. The fundamental anti-phase mode of the QTF achieves a stable resonant frequency with a high Quality factor making it ideal for DAFM applications in which a small shift in the resonant frequency is linked to a tip-sample force. The addition of the tip-sample force also breaks the symmetry of the QTF leading to a classic eigenvalue veering scenario. The eigenvalue veering and accompanying mode localization phenomena violate the standard DAFM modeling assumptions which treat the addition of the tip-sample force as a small perturbation to a single-degree-of-freedom oscillator. We find that the eigenvalue veering can contribute a systematic error in force measurements on the order of 20%. Methodology for correcting the systematic error caused by eigenvalue veering is proposed.

Summary There are currently no technologies available to measure polymer solution viscosities at realistic downhole conditions in a well during enhanced oil recovery (EOR). In this paper, custom-made probes using quartz tuning fork (QTF) resonators are demonstrated for measurements of viscosity of polymer fluids in the laboratory. The electromechanical response of the resonators was calibrated in simple Newtonian fluids and in non-Newtonian polymer fluids at different concentrations. The responses were then used to measure field-collected samples of polymer injection fluids. In the polymer fluids, the measured viscosity values by tuning forks were lower than those measured by the conventional rheometer at 6.8 s−1, closer to the solvent viscosity values. However, the predicted rheometer viscosity vs. QTF-measured viscosity showed a distinct exponential correlation (R2=0.9997), allowing for an empirical calibration between the two viscometers for fluids having the same solvent and polymer compositions. The QTF sensors produced acceptable viscosity measurements of polymer fluids within the required polymer concentration ranges used in the field and predicted field sample viscosities with less than 1–2 cp (or 10–20%) error from the rheometer data. Results were validated based on separate independent tests where the devices were used to measure the viscosity of Newtonian fluids and non-Newtonian polymer fluids in a series of consecutive dip tests, simulating more realistic usage. These devices can be used to measure either the “relative” viscosity changes from a polymer solution prior and post-injection or to measure a “calibrated” viscosity via empirical exponential correlation. The compact QTF sensors developed in this study can be easily integrated into portable systems for laboratory or wellsite deployment as well as logging tools for downhole deployment. This work also demonstrates the ability of these QTF devices to make sensitive viscosity measurements at high-frequencies, opening opportunities for their use in high-frequency rheology studies of EOR fluids.

This paper presents oscillation control electronics for Frequency Modulation Atomic Force Microscope (FMAFM). It presents a Phase Locked Loop circuit performing the function of Frequency Control and its complete analysis.

The dissipative processes that occur with immersing a vibrating tuning fork in superfluid helium are investigated. The tuning forks resonance width Δf of frequencies from 32 to 97 kHz was measured in the temperature range from 0.2 to 2.5 K and He II pressure from SVP to 24.9 atm. Some of the tuning forks were in the original can (closed tuning fork), and for some tuning forks the can was either completely or partially removed (opened fork). We found that for the open tuning forks two dissipation mechanisms are clearly revealed in the temperature dependence of Δf, namely, acoustic radiation and scattering of ballistic thermal excitations at low temperatures, and viscous friction at high temperatures. At low temperatures (below ∼ 0.8 K) acoustic dissipation dominates, and the model of quadrupole oscillator for a tuning fork can be applied. We found that acoustic radiation for closed tuning forks is less effective and appears at lower temperatures. The first experimental data on dissipative processes in the quartz tuning fork–He II system at increased liquid pressures are obtained. It is shown that, for high frequency tuning forks the resonance bandwidth decreases with increasing pressure, i.e., with increasing wavelength of sound λ, according to the law λ−5. At low frequencies and low temperatures, with increasing mean free path of thermal excitations the resonance bandwidth is well described by the model of ballistic scattering.

The quartz tuning fork has recently become a popular experimental tool for investigations of both classical and quantum turbulence in cryogenic helium. Its increased use in low-temperature experiments and a number of puzzling results obtained in the past have led to many questions concerning the interaction of multiple tuning forks or the interaction of tuning forks with other oscillators. We report measurements performed in He II at low temperatures around 360 mK, on the mutual interaction of tuning forks placed in the same volume of fluid, and examine the responsible mechanisms in an effort to discriminate between acoustic coupling and interaction via quantized vortices. To this end, the interaction of two tuning forks is investigated by analyzing their recorded resonance curves, looking for any nonelectrical crosstalk. Further, the force-velocity characteristics of a detector tuning fork are measured for different operating velocities of a generator tuning fork. As a complementary measurement, the intensity of sound waves is recorded using a set of miniature receivers. We confirm the current knowledge on acoustic emission by tuning forks in He II and verify properties of their radiation patterns. We conclude that in our experiment the interaction is almost entirely mediated by sound waves.

A theoretical-experimental framework for the analysis of the dynamic response of a QEPAS tuning fork device immersed in a fluid medium

This paper reports the first demonstration of hydrogel conical tip attachment onto quartz tuning fork (QTF) by using an elastomeric tip mold that is soft-lithographically replicated from an electrochemically etched tungsten wire. The tungsten tip of 10–100 nm radius obtained by time-controlled electrochemical etching is replicated with h-polydimethylsiloxane (h-PDMS) to make negative conical tip molds large enough to be used for QTFs. By approaching a QTF to the negative h-PDMS tip mold filled with polyethylene glycol-diacrylate (PEGDA), a PEGDA tip is attached to the QTF without using an adhesive. Then, the PEGDA tip attached QTF is employed for shear force microscopy for calibration grating and atomic layers of hexagonal silicon carbide and also compared with a silicon tip attached QTF. Exclusively for the PEGDA tip attached QTF, we demonstrate that the imaging tip could be regenerated multiple times to address issues associated with tip wear. In a stark contrast with conventional QTF probes in attachment of electrochemically etched metallic wires or microfabricated AFM cantilevers, photocuring of liquid phase prepolymer within a tip mold demonstrated herein allows adhesive-free and exclusive attachment of the imaging tip onto a QTF. The relatively large PEGDA tip enables facile operation during approach and engagement. Moreover, the organic and inorganic combination of imaging tip and resonating body offers regeneration of the imaging tip upon its degradation.

In this paper, we investigate the potential of using quartz tuning fork (QTF) sensing system for detection of specific metal ions in aqueous solutions with sample volume of $1~\mu \text{L}$ . Functionalized self-assembled monolayers (SAMs) of L-glutathione (LG) on gold-coated QTFs were used to sense specific analytes of CaCl2 and HgCl2, whereas functionalized L-cysteine based SAMs used to sense PbCl2. The resonance frequency undergoes a shift in response to the interaction between functionalized QTF and target analyte. X-ray photoelectron spectroscopy was used to study the interaction of thiol groups between the functionalized SAM and gold coated on QTF surface. Our analysis revealed that active QTFs functionalized with LG are more sensitive to detection of CaCl2 compared with HgCl2. The SAM-based QTF sensors were found to be capable of detecting low concentrations ( $10^{- {12}}$ M) of divalent analyte solutes with high sensitivity.

We report here a chemical sensor based on detecting the mechanical response of a thin (approximately 10-microm) polymer wire stretched across the two prongs of a wristwatch quartz tuning fork (QTF). When the fork is set to oscillate, the wire is stretched and compressed by the two prongs. The stretching/compression force changes upon adsorption of analyte molecules onto/into the polymer wire, which is detected by the QTF with pico-Newton force sensitivity. An array of such sensors with different polymer wires is used for simultaneous detection of several analytes and for improvement of pattern recognition. The low cost (approximately 10 cent) of the QTF, together with that an array of QTFs can be driven to oscillate simultaneously and their resonance frequencies detected with the same circuit, promises a high performance, low cost, and portable sensor for detecting various chemical vapors. We demonstrate here detection of parts-per-billion-level water, ethylnitrobenzene, and ethanol vapors using the QTF arrays.

A theoretical model describing the acoustic coupling between two resonator tubes in spectrophones exploiting custom-made quartz tuning forks (QTFs) is proposed. The model is based on an open-end correction to predict the optimal tube length. A calculation of the sound field distribution from one tube exit allowed for the estimation of the optimal radius as a function of the QTF prong spacing and the sound wavelength. The theoretical predictions have been confirmed using experimental studies employing a custom QTF with a fundamental flexural mode resonance frequency of 15.8 kHz and a quality factor of 15,000 at atmospheric pressure. The spacing between the two prongs was 1.5 mm. Spectrophones mounting this QTF were implemented for the quartz-enhanced photoacoustic detection of water vapor in air in the mid-infrared spectral range.

Pilot line manufactured custom quartz tuning forks (QTFs) with a resonance frequency of 28 kHz and a Q value of >30, 000 in a vacuum and ∼ 7500 in the air, were designed and produced for trace gas sensing based on quartz enhanced photoacoustic spectroscopy (QEPAS). The pilot line was able to produce hundreds of low-frequency custom QTFs with small frequency shift < 10 ppm, benefiting the detecting of molecules with slow vibrational-translational (V-T) relaxation rates. An Au film with a thickness of 600 nm were deposited on both sides of QTF to enhance the piezoelectric charge collection efficiency and reduce the environmental electromagnetic noise. The laser focus position and modulation depth were optimized. With an integration time of 84 s, a normalized noise equivalent absorption (NNEA) coefficient of 1.7 × 10−8 cm-1∙W∙Hz-1/2 was achieved which is ∼10 times higher than a commercially available QTF with a resonance frequency of 32 kHz.

We report a sub-terahertz scattering-type scanning near-field microscope (sub-THz s-SNOM) which uses a 6 mm long metallic tip driven by a quartz tuning fork as the near-field probe. Under continuous-wave illumination by a 94 GHz Gunn diode oscillator, terahertz near-field images are obtained by demodulating the scattered wave at both the fundamental and the second harmonic of the tuning fork oscillation frequency together with the atomic-force-microscope (AFM) image. The terahertz near-field image of a gold grating with a period of 2.3 µm obtained at the fundamental modulation frequency agrees well with the AFM image. The experimental relationship between the signal demodulated at the fundamental frequency and the tip-sample distance is well fitted with the coupled dipole model indicating that the scattered signal from the long probe is mainly contributed by the near-field interaction between the tip and the sample. This near-filed probe scheme using quartz tuning fork can adjust the tip length flexibly to match the wavelength over the entire terahertz frequency range and allows for operation in cryogenic environment.

A quartz tuning fork was used instead of cantilever as a force sensor for the atomic force microscope. A tungsten tip was made by electrochemical etching from a wire of 50 µm diameter. In order to have mechanical stability of the tuning fork, it was attached on an alumina plate. The tungsten tip was attached on the inside end of a prong of a tuning fork. The phase shift was used as a feedback signal to control the distance between the tip and sample, and the amplitude was kept constant using a lock-in amplifier and a homemade automatic gain controller. Due to the mechanical stability, the sensor shows a high quality factor (∼10(3)), and the image quality obtained with this sensor was equivalent to that of the cantilever-based AFM.

Chaos control in AFM systems using nonlinear delayed feedback via sliding mode control

We report on experimental investigations of acoustic emission by quartz tuning forks resonating at frequencies 32 kHz, 38 kHz, 77 kHz and 100 kHz immersed in cold gaseous 4He and its normal and superfluid liquid phases. Frequency dependence of the observed low-drive-linewidth at 350 mK together with the temperature and pressure dependences (1.3 K < T < 4.2 K, 0 < p < 25 bar) of the observed damping of the high frequency (77 and 100 kHz) resonators measured in normal liquid 4He and its superfluid phase provide strong and direct evidence of the importance of sound emission by these tuning forks. Three analytical models of acoustic emission by vibrating tuning forks are developed and compared with the experimental results. We also discuss the importance of sound emission for experiments with the commonly used 32 kHz tuning forks as well as other oscillating structures—spheres, wires, grids and various micromachined sensors. We compare the relative importance of dissipative losses due to laminar viscous/ballistic drag and acoustic emission in liquid and superfluid 4He.