Quantitative nanoscale temperature mapping across the multi-quantum well of a light-emitting diode in operation using vacuum null-point scanning thermal microscopy to evaluate local energy conversion efficiency.

Electrical energy that is not converted into light in light emitting diodes (LEDs) is locally dissipated as heat in the active layers. Therefore, by measuring the temperature distribution with nanoscale resolution across the multi-quantum well (MQW) of an LED in operation, the effect of nanostructures inside the LED on the local energy conversion efficiency can be observed. In this study, we first demonstrated that vacuum null-point scanning thermal microscopy (VNP SThM) could be used to quantitatively map the two-dimensional temperature distribution across the MQW of an LED in operation with a sufficient signal-to-noise ratio. Subsequently, by increasing the injection current in four steps, we quantitatively mapped the temperature distribution across the MQW at each step and observed the shift in the temperature peak across the active layers due to the increase in injection current. The measurements of the temperature distribution around the MQW indicate that as the injection current increased, the overall temperature around the MQW increased significantly, and the temperature peak position shifted. These results show that the main cause of the dissipation of electrical energy into thermal energy inside an LED changes as the injection current increases, and the nanostructures inside an LED affect the dissipation of electrical energy into thermal energy. The high thermal sensitivity, nanoscale resolution, and convenience of VNP SThM may enable the direct observation of the effect of the nanostructures inside various types of nanophotonic devices on local energy conversion even under intense localized radiation.

Measuring the size dependence of thermal conductivity of suspended graphene disks using null-point scanning thermal microscopy.

Using null-point scanning thermal microscopy (NP SThM), we have measured and analyzed the size dependence of the thermal conductivity of graphene. To do so, we rigorously re-derived the principal equation of NP SThM in terms of thermal property measurements so as to explain how this technique can be effectively used to quantitatively measure the local thermal resistance with nanoscale spatial resolution. This technique has already been proven to resolve the major problems of conventional SThM, and to quantitatively measure the temperature profile. Using NP SThM, we measured the variation in the thermal resistance of suspended chemical vapor deposition (CVD)-grown graphene disks with radii of 50-3680 nm from the center to the edge with respect to the size. By thoroughly analyzing the size dependence of the thermal resistance, we show that, with increasing graphene size, the ballistic resistance becomes more dominant in the thermal resistance experienced by a heat source of finite size and that the thermal conductivity experienced by such a heat source can even decrease. The results of this study reveal that the thermal conductivity of graphene detected by a heat source depends on the size of the heat source relative to that of the suspended graphene and on how the heat source and graphene are connected. As demonstrated in this study, NP SThM will be very useful for quantitative thermal characterization of not only CVD-grown graphene but also various other nanomaterials and nanodevices.

Towards an Accurate Measurement of Thermal Contact Resistance at Chemical Vapor Deposition-Grown Graphene/SiO2 Interface Through Null Point Scanning Thermal Microscopy.

In the development of graphene-based electronic devices, it is crucial to characterize the thermal contact resistance between the graphene and the substrate precisely. In this study, we demonstrate that the thermal contact resistance between CVD-grown graphene and SiO2 substrate can be obtained by measuring the temperature drop occurring at the graphene/SiO2 interface with null point scanning thermal microscopy (NP SThM), which profiles the temperature distribution quantitatively with nanoscale spatial resolution (-50 nm) without the shortcomings of the conventional SThM. The thermal contact resistance between the CVD-grown graphene and SiO2 substrate is measured as (1.7 ± 0.27) x 10(-6) M2K/W. This abnormally large thermal contact resistance seems to be caused by extrinsic factors such as ripples and metal-based contamination, which inevitably form in CVD-grown graphene during the production and transfer processes.

Enabling low-noise null-point scanning thermal microscopy by the optimization of scanning thermal microscope probe through a rigorous theory of quantitative measurement.

The application of conventional scanning thermal microscopy (SThM) is severely limited by three major problems: (i) distortion of the measured signal due to heat transfer through the air, (ii) the unknown and variable value of the tip-sample thermal contact resistance, and (iii) perturbation of the sample temperature due to the heat flux through the tip-sample thermal contact. Recently, we proposed null-point scanning thermal microscopy (NP SThM) as a way of overcoming these problems in principle by tracking the thermal equilibrium between the end of the SThM tip and the sample surface. However, in order to obtain high spatial resolution, which is the primary motivation for SThM, NP SThM requires an extremely sensitive SThM probe that can trace the vanishingly small heat flux through the tip-sample nano-thermal contact. Herein, we derive a relation between the spatial resolution and the design parameters of a SThM probe, optimize the thermal and electrical design, and develop a batch-fabrication process. We also quantitatively demonstrate significantly improved sensitivity, lower measurement noise, and higher spatial resolution of the fabricated SThM probes. By utilizing the exceptional performance of these fabricated probes, we show that NP SThM can be used to obtain a quantitative temperature profile with nanoscale resolution independent of the changing tip-sample thermal contact resistance and without perturbation of the sample temperature or distortion due to the heat transfer through the air.

Quantitative thermopower profiling across a silicon p-n junction with nanometer resolution.

Thermopower (S) profiling with nanometer resolution is essential for enhancing the thermoelectric figure of merit, ZT, through the nanostructuring of materials and for carrier density profiling in nanoelectronic devices. However, only qualitative and impractical methods or techniques with low resolutions have been reported thus far. Herein, we develop a quantitative S profiling method with nanometer resolution, scanning Seebeck microscopy (SSM), and batch-fabricate diamond thermocouple probes to apply SSM to silicon, which requires a contact stress higher than 10 GPa for stable electrical contact. The distance between the positive and negative peaks of the S profile across the silicon p-n junction measured by SSM is 4 nm, while the theoretical distance is 2 nm. Because of its extremely high spatial resolution, quantitative measurement, and ease of use, SSM could be a crucial tool not only for the characterization of nano-thermoelectric materials and nanoelectronic devices but also for the analysis of nanoscale thermal and electrical phenomena in general.

Quantitative measurement with scanning thermal microscope by preventing the distortion due to the heat transfer through the air.

Because of its high spatial resolution, scanning thermal microscopy (SThM) has been developed quite actively and applied in such diverse areas as microelectronics, optoelectronics, polymers, and carbon nanotubes for more than a decade since the 1990s. However, despite its long history and diverse areas of application, surprisingly, no quantitative profiling method has been established yet. This is mostly due to the nonlocal nature of measurement by conventional SThM: the signal measured by SThM is induced not only from the local heat flux through the tip-sample thermal contact but also (and mostly) from the heat flux through the air gap between the sample and the SThM probe. In this study, a rigorous but simple and practical theory for quantitative SThM for local measurement is established and verified experimentally using high-performance SThM probes. The development of quantitative SThM will make possible new breakthroughs in diverse fields of nanothermal science and engineering.

Quantitative temperature measurement of an electrically heated carbon nanotube using the null-point method.

Previously, we introduced the double scan technique, which enables quantitative temperature profiling with a scanning thermal microscope (SThM) without distortion arising from heat transfer through the air. However, if the tip-sample thermal conductance is disturbed due to the extremely small size of the sample, such as carbon nanotubes, or an abrupt change in the topography, then quantitative measurement becomes difficult even with the double scan technique. Here, we developed the null-point method by which one can quantitatively measure the temperature of a sample without disturbances arising from the tip-sample thermal conductance, based on the principle of the double scan technique. We first checked the effectiveness and accuracy of the null-point method using 5 µm and 400 nm wide aluminum lines. Then, we quantitatively measured the temperature of electrically heated multiwall carbon nanotubes using the null-point method. Since the null-point method has an extremely high spatial resolution of SThM and is free from disturbance due to the tip-sample thermal contact resistance, and distortion due to heat transfer through the air, the method is expected to be widely applicable for the thermal characterization of many nanomaterials and nanodevices.

Nanoscale range finding of subsurface structures by measuring the absolute phase lag of thermal wave.

The need for a subsurface imaging technique to locate and characterize subsurface defects in multidimensional micro- and nanoengineered devices has been growing rapidly. We show that a subsurface heater can be located accurately using the phase lag of a thermal wave. We deduce that the absolute phase lag is composed of four components. Among the four components, we isolate the component directly related to the position and the structure of the periodic heat source. We demonstrate that the position of the heater can be estimated accurately from the isolated phase lag component.

Transient thermal conductivity and colloidal stability measurements of nanofluids by using the 3omega method.

Nanofluid is a mixture of nanoscale particles of metal, metal oxide or carbon nanotube and heat transfer fluids such as water and ethylene glycol. This work presents the application of the 3-omega (3omega) method for measuring the colloidal stability and the transient thermal conductivity of multi-wall carbon nanotube (MWCNT), Al2O3 and TiO2 nanoparticles suspended in water or ethylene glycol. The microfabricated 3omega device is verified by comparing the measured thermal conductivities of pure fluids with the table values. After the validation, the transient thermal responses of the nanofluids are measured to evaluate the colloidal stability. All of Al2O3 nanofluid samples show a clear sign of sedimentation while the acid-treated MWCNT (tMWCNT) nanofluid and a couple of TiO2 nanofluids with pH control or surfactant addition are found to have excellent colloidal stability. The thermal conductivities of tMWCNT nanofluids in the de-ionized water and ethylene glycol are measured, which are found to be in good agreement with previous data.