The atomic force microscope (AFM) offers a rich observation window on the nanoscale, yet many dynamic phenomena are too fast and too weak for direct AFM detection. Integrated cavity-optomechanics is revolutionizing micromechanical sensing; however, it has not yet impacted AFM. Here, we make a groundbreaking advance by fabricating picogram-scale probes integrated with photonic resonators, to realize functional AFM detection that achieve high temporal resolution (< 10 ns) and picometer vertical displacement uncertainty, simultaneously. The ability to capture fast events with high precision is leveraged to measure the thermal conductivity (η), for the first time, concurrently with chemical composition at the nanoscale in photothermal induced resonance experiments. The intrinsic η of metal-organic-framework individual microcrystals, not measurable by macroscale techniques, is obtained with a small measurement uncertainty (8 %). The improved sensitivity (50×) increases the measurement throughput 2500-fold and enables chemical composition measurement of molecular-monolayer-thin samples. Our paradigm-shifting photonic readout for small probes breaks the common tradeoff between AFM measurement precision and ability to capture transient events, thus transforming the ability to observe nanoscale dynamics in materials.
Capillary condensation is the first-order vapor-to-liquid phase transition taking place in confined geometries. Such heterogeneous nucleation has been well described by thermodynamic laws such as the Kelvin equation, but the equation's applicability at the nanoscale is still unresolved. Here, we show that the Kelvin equation is valid down to approximately 0.5 nm radius of curvature when the curvature dependence of surface tension is taken into account. By the shear-mode atomic force microscopy, we have measured directly and accurately the critical tip-surface distance (d c) at which the water meniscus is capillary condensed in ambient condition; e.g., d c ≈ 1.2 nm at 10% relative humidity. In particular, we can determine the Tolman length, the unique characteristic of the curvature-dependent surface tension, as the single fitting parameter (δ ¼ 0.21 AE 0.05 nm). Our results that unify the validity of the Kelvin equation at molecular scale and the characterization of the curvature effect of surface tension may provide a better understanding of general nucleation phenomena in nature, including the role of nanometric aerosols in cloud formation.
We present the general stress tensor of the ubiquitous hydration water layer (HWL), based on the empirical hydration force, by combining the elasticity and hydrodynamics theories. The tapping and shear component of the tensor describe the elastic and damping properties of the HWL, respectively, in good agreement with experiments. In particular, a unified understanding of HWL dynamics provides the otherwise unavailable intrinsic parameters of the HWL, which offer additional but unexplored aspects to the supercooled liquidity of the confined HWL. Our results may allow deeper insight on systems where the HWL is critical.
We developed a nanoneedle transistor-based sensor (NTS) for the selective detection of calcium ions inside a living cell. In this work, a single-walled carbon nanotube-based field effect transistor (swCNT-FET) was first fabricated at the end of a glass nanopipette and functionalized with Fluo-4-AM probe dye. The selective binding of calcium ions onto the dye molecules altered the charge state of the dye molecules, resulting in the change of the source-drain current of the swCNT-FET as well as the fluorescence intensity from the dye. We demonstrated the electrical and fluorescence detection of the concentration change of intracellular calcium ions inside a HeLa cell using the NTS.
Titania, which exhibits superwetting under light illumination, has been widely used as an ideal material for environmental solution such as self-cleaning, water-air purification, and antifogging. There have been various studies to understand such superhydrophilic conversion. The origin of superwetting has not been clarified in a unified mechanism yet, which requires direct experimental investigation of the dynamic processes of water-layer growth. We report in situ measurements of the growth rate and height of the photo-adsorbed water layers by tip-based dynamic force microscopy. For nanocrystalline anatase and rutile TiO 2 we observe light-induced enhancement of the rate and height, which decrease after O 2 annealing. The results lead us to confirm that the long-range attraction between water molecules and TiO 2 , which is mediated by delocalized electrons in the shallow traps associated with O 2 vacancies, produces photo-adsorption of water on the surface. In addition, molecular dynamics simulations clearly show that such photo-adsorbed water is critical to the zero contact angle of a water droplet spreading on it. Therefore, we conclude that this "water wets water" mechanism acting on the photoadsorbed water layers is responsible for the light-induced superwetting of TiO 2 . Similar mechanism may be applied for better understanding of the hydrophilic conversion of doped TiO 2 or other photo-catalytic oxides.
We present experimental and computational investigations of tetramodal and pentamodal atomic force microscopy (AFM), respectively, whereby the first four or five flexural eigenmodes of the cantilever are simultaneously excited externally. This leads to six to eight additional observables in the form of amplitude and phase signals, with respect to the monomodal amplitude modulation method. We convert these additional observables into three or four dissipation and virial expressions, and show that these quantities can provide enhanced contrast that would otherwise remain hidden in the original observables. We also show that the complexity of the multimodal impact leads to significant energy transfer between the active eigenmodes, such that the dissipated power for individual eigenmodes may be positive or negative, while the total dissipated power remains positive. These results suggest that the contrast of individual eigenmodes in multifrequency AFM should be not be considered in isolation and that it may be possible to use different eigenfrequencies to probe sample properties that respond to different relaxation times.
The hydration water layer (HWL), a ubiquitous form of water on the hydrophilic surfaces, exhibits anomalous characteristics different from bulk water and plays an important role in interfacial interactions. Despite extensive studies on the mechanical properties of HWL, one still lacks holistic understanding of its energy dissipation, which is critical to characterization of viscoelastic materials as well as identification of nanoscale dissipation processes. Here we address energy dissipation of nanoconfined HWL between two atomically flat hydrophilic solid surfaces (area of ~120 nm2) by small amplitude-modulation, noncontact atomic force microscopy. Based on the viscoelastic hydration-force model, the average dissipation energy is ~1 eV at the tapping amplitude (~0.1 nm) of the tip. In particular, we determine the accurate HWL thickness of ~6 layers of water molecules, as similarly observed on biological surfaces. Such a long-range interaction of HWL should be considered in the nanoscale phenomena such as friction, collision and self-assembly.
When the surface of water is curved at nanoscale as a bubble, droplet and meniscus, its surface tension is expected to be smaller than that of planar interface, which still awaits experimental studies. Here, we report static and dynamic force spectroscopy that measures the capillary force of a single nanoscale water meniscus at constant curvature condition. Based on the Young-Laplace equation, the results are used to obtain the effective surface tension (ST) of the meniscus, which decreases to less than 20% of the bulk value at the radius-of-curvature (ROC) below 25 nm, while indicating the bulk behaviour above ~130 nm ROC. Interestingly, such a possibility provides a qualitative resolution of the unsettled discrepancies between experiments and theories in the thermodynamic activation processes for the mentioned three types of nano-curvatured water. Our results may not only lead to development of microscopic theories of ST as well as further experimental investigations, but also help better understanding of the ST-induced nanoscale dynamics such as cluster growth or protein folding, and the ST-controlled design of nano-biomaterials using the nano-meniscus.
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