Jungchul Lee

Electrical, Thermal, and Mechanical Characterization of Silicon Microcantilever Heaters

Silicon atomic force microscope (AFM) cantilevers having integrated solid-state heaters were originally developed for application to data storage, but have since been applied to metrology, thermophysical property measurements, and nanoscale manufacturing. These applications beyond data storage have strict requirements for mechanical characterization and precise temperature calibration of the cantilever. This paper describes detailed mechanical, electrical, and thermal characterization and calibration of AFM cantilevers having integrated solid-state heaters. Analysis of the cantilever response to electrical excitation in both time and frequency domains aids in resolving heat transfer mechanisms in the cantilever. Raman spectroscopy provides local temperature measurement along the cantilever with resolution near 1 mum and 5degC and also provides local surface stress measurements. Observation of the cantilever mechanical thermal noise spectrum at room temperature and while heated provides insight into cantilever mechanical behavior and compares well with finite-element analysis. The characterization and calibration methodology reported here expands the use of heated AFM cantilevers, particularly the uses for nanomanufacturing and sensing

High efficiency organic multilayer photodetectors based on singlet exciton fission

We employ an exciton fission process that converts one singlet exciton into two triplet excitons to increase the quantum efficiency of an organic multilayer photodetector beyond 100%. The photodetector incorporates ultrathin alternating donor-acceptor layers of pentacene and C60, respectively. By comparing the quantum efficiency after separate pentacene and C60 photoexcitation we find that singlet exciton fission in pentacene enhances the quantum efficiency by (45±7)%. In quantitative agreement with this result, we also observe that the photocurrent generated from pentacene excitons is decreased by (2.7±0.2)% under an applied magnetic field of H=0.4 T, while the C60 photocurrent is relatively unchanged.

Toward attogram mass measurements in solution with suspended nanochannel resonators.

Using suspended nanochannel resonators (SNRs), we demonstrate measurements of mass in solution with a resolution of 27 ag in a 1 kHz bandwidth, which represents a 100-fold improvement over existing suspended microchannel resonators and, to our knowledge, is the most precise mass measurement in liquid today. The SNR consists of a cantilever that is 50 microm long, 10 microm wide, and 1.3 microm thick, with an embedded nanochannel that is 2 microm wide and 700 nm tall. The SNR has a resonance frequency near 630 kHz and exhibits a quality factor of approximately 8000 when dry and when filled with water. In addition, we introduce a new method that uses centrifugal force caused by vibration of the cantilever to trap particles at the free end. This approach eliminates the intrinsic position dependent error of the SNR and also improves the mass resolution by increasing the averaging time for each particle.

Differential Scanning Calorimeter Based on Suspended Membrane Single Crystal Silicon Microhotplate

This paper introduces an array of single crystal silicon microhotplates for differential scanning calorimetry. Heat transfer analysis considers the tradeoffs between heating and cooling rate, temperature uniformity, and measurement sensitivity, and determines the optimal design for a suspended membrane microhotplate with full backside release. Additionally, considering the requirements of routine sample loading, the size of the square heater (LH) is 100 or 200 mum, while the size of the backside membrane cavity is 400 mum. In the heater region, two interdigitated serpentine doped silicon resistors were designed such that several operational configurations were possible. The hotplates exhibited very high heating efficiency of 36.7 K/mW with LH = 100 mum and 18.3 K/mW with LH = 200 mum while also having time constants on the order of 1 ms. Paraffin wax was mounted on the sensor, and melting was observed when the heater temperature was 55degC with a voltage ramp of 0.2 V/s. With 8 V/s, the paraffin sample was completely consumed within 1 ms with 0.317 mJ of thermal energy extracted. Our design achieves a combination of time constant, temperature sensitivity, and heating efficiency that are comparable or superior to previously published microcalorimeters.

Topography imaging with a heated atomic force microscope cantilever in tapping mode

This article describes tapping mode atomic force microscopy (AFM) using a heated AFM cantilever. The electrical and thermal responses of the cantilever were investigated while the cantilever oscillated in free space or was in intermittent contact with a surface. The cantilever oscillates at its mechanical resonant frequency, 70.36 kHz, which is much faster than its thermal time constant of 300 micros, and so the cantilever operates in thermal steady state. The thermal impedance between the cantilever heater and the sample was measured through the cantilever temperature signal. Topographical imaging was performed on silicon calibration gratings of height 20 and 100 nm. The obtained topography sensitivity is as high as 200 microVnm and the resolution is as good as 0.5 nmHz(1/2), depending on the cantilever power. The cantilever heating power ranges 0-7 mW, which corresponds to a temperature range of 25-700 degrees C. The imaging was performed entirely using the cantilever thermal signal and no laser or other optics was required. As in conventional AFM, the tapping mode operation demonstrated here can suppress imaging artifacts and enable imaging of soft samples.

Weighing nanoparticles in solution at the attogram scale

Significance Naturally occurring and engineered nanoparticles (e.g., exosomes, viruses, protein aggregates, and self-assembled nanostructures) have size- and concentration-dependent functionality, yet existing characterization methods in solution are limited for diameters below ∼50 nm. In this study, we developed a nanomechanical resonator that can directly measure the mass of individual nanoparticles down to 10 nm with single-attogram (10−18 g) precision, enabling access to previously difficult-to-characterize natural and synthetic nanoparticles. Physical characterization of nanoparticles is required for a wide range of applications. Nanomechanical resonators can quantify the mass of individual particles with detection limits down to a single atom in vacuum. However, applications are limited because performance is severely degraded in solution. Suspended micro- and nanochannel resonators have opened up the possibility of achieving vacuum-level precision for samples in the aqueous environment and a noise equivalent mass resolution of 27 attograms in 1-kHz bandwidth was previously achieved by Lee et al. [(2010) Nano Lett 10(7):2537–2542]. Here, we report on a series of advancements that have improved the resolution by more than 30-fold, to 0.85 attograms in the same bandwidth, approaching the thermomechanical noise limit and enabling precise quantification of particles down to 10 nm with a throughput of more than 18,000 particles per hour. We demonstrate the potential of this capability by comparing the mass distributions of exosomes produced by different cell types and by characterizing the yield of self-assembled DNA nanoparticle structures.

Frequency-Dependent Electrical and Thermal Response of Heated Atomic Force Microscope Cantilevers

This paper investigates the electrical and thermal response of the heated atomic force microscope (AFM) cantilevers in the frequency range from 10 Hz to 1 MHz. Spectrum analysis of the cantilever voltage response to periodic heating distinguishes different thermal behaviors of the cantilever in the frequency domain: the cantilever voltage at low frequencies is modulated by higher-order harmonics, and at high frequencies it oscillates with 1-omega only. A simple model facilitates the understanding of complicated electrical and thermal behaviors in the cantilever, thus, it is possible to determine the cantilever temperature. The calculation predicts that temperature oscillation is restricted to the heater region when the cantilever is operated at about 10 kHz, suggesting that the periodic-heating operation of the cantilever may be employed for highly sensitive thermal metrology

Reducing recombination losses in planar organic photovoltaic cells using multiple step charge separation

We enhance the efficiency of heterojunction organic solar cells by introducing a thin interfacial layer between the acceptor and donor layers. The interfacial layer energy levels are chosen to provide a gradient for charges crossing the interface, approximating a conventional p-n junction with three organic semiconductors. Devices with interfacial layers exhibit increased open circuit voltage (VOC) and increased short circuit current (JSC). The increase in VOC is due to a reduction in dark current and charge recombination. The increase in JSC is correlated with an increase in the conversion efficiency of excitons originating in the donor or acceptor layers. The interfacial layer destabilizes charge transfer states at the donor-acceptor interface, yielding reduced exciton recombination. The introduction of thin interfacial layers may prove to be an important probe of the physics of exciton separation in organic photovoltaic cells.

Rapid thermal lysis of cells using silicon–diamond microcantilever heaters

This paper presents the design and application of microcantilever heaters for biochemical applications. Thermal lysis of biological cells was demonstrated as a specific example. The microcantilever heaters, fabricated from selectively doped single crystal silicon, provide local resistive heating with highly uniform temperature distribution across the cantilevers. Very importantly, the microcantilever heaters were coated with a layer of 100 nm thick electrically insulating ultrananocrystalline diamond (UNCD) layer used for cell immobilization on the cantilever surface. Fibroblast cells or bacterial cells were immobilized on the UNCD/cantilever surfaces and thermal lysis was demonstrated via optical fluorescence microscopy. Upon electrical heating of the cantilever structures to 93 degrees C for 30 seconds, fibroblast cell and nuclear membrane were compromised and the cells were lysed. Over 90% of viable bacteria were also lysed after 15 seconds of heating at 93 degrees C. This work demonstrates the utility of silicon-UNCD heated microcantilevers for rapid cell lysis and forms the basis for other rapid and localized temperature-regulated microbiological experiments in cantilever-based lab on chip applications.

Microcantilever actuation via periodic internal heating

This paper reports electrothermal actuation of silicon microcantilevers having integrated resistive heaters. Periodic electrical excitation induced periodic resistive heating in the cantilever, while the cantilever deflection was monitored with a photodetector. Excitation was either at the cantilever resonant frequency, f(0), f(0)/2, or f(0)/3. When the time averaged maximum cantilever temperature was 174 degrees C, the cantilever out-of-plane actuation amplitude was 484 nm near the cantilever resonance frequency of 24.9 kHz. This actuation was sufficiently large to operate the cantilever in intermittent contact mode and scan a calibration grating of height of 20 nm.