Séverine Gomès

Amorphization and reduction of thermal conductivity in porous silicon by irradiation with swift heavy ions

In this article, we demonstrate that the thermal conductivity of nanostructured porous silicon is reduced by amorphization and also that this amorphous phase in porous silicon can be created by swift (high-energy) heavy ion irradiation. Porous silicon samples with 41%-75% porosity are irradiated with 110 MeV uranium ions at six different fluences. Structural characterisation by micro-Raman spectroscopy and SEM imaging show that swift heavy ion irradiation causes the creation of an amorphous phase in porous Si but without suppressing its porous structure. We demonstrate that the amorphization of porous silicon is caused by electronic-regime interactions, which is the first time such an effect is obtained in crystalline silicon with single-ion species. Furthermore, the impact on the thermal conductivity of porous silicon is studied by micro-Raman spectroscopy and scanning thermal microscopy. The creation of an amorphous phase in porous silicon leads to a reduction of its thermal conductivity, up to a factor of 3 compared to the non-irradiated sample. Therefore, this technique could be used to enhance the thermal insulation properties of porous Si. Finally, we show that this treatment can be combined with pre-oxidation at 300 °C, which is known to lower the thermal conductivity of porous Si, in order to obtain an even greater reduction.

Characterization of the thermal conductivity of insulating thin films by scanning thermal microscopy

This paper reports on the abilities of a Scanning Thermal Microscopy (SThM) method to characterize the thermal conductivity of insulating materials and thin films used in microelectronics and microsystems. It gives a review of the previous works on the subject and gives new results allowing showing the performance of a new method proposed for reducing the thermal conductivity of meso-porous silicon by swift heavy ion irradiation. Meso-porous silicon samples were prepared by anodisation of silicon wafers and underwent irradiation by 845MeV ^2^0^8Pb ions, with fluences of 4x10^1^1 and 7x10^1^1cm^-^2. Thermal measurements show that irradiation reduced thermal conductivity by a factor of up to 2.

Heat transfer at nanoscale contacts investigated with scanning thermal microscopy

This article investigates heat transfer at nanoscale contacts through scanning thermal microscopy (SThM) under vacuum conditions. Measurements were performed using two types of resistive SThM probes operating in active mode on germanium and silicon samples. The experiments measure the heat transfer through the nanoscale point contacts formed between the probe apex, platinum-rhodium alloy, or silicon nitride depending on the probe used, and the samples. The thermal resistance at the probe apex-sample interface becomes extremely important as the contact size becomes smaller or comparable to the phonon mean free path within the materials in contact. This resistance is derived from the measurements using a nanoconstriction model. Consistent to what is expected, the interfacial thermal resistance is found to be dependent on the tip and sample. Assuming perfect interfaces, the thermal boundary resistance Rb is determined for the different contacts. Results obtained for Rb range from 10−9 m2 K W−1 up to 14 × 10−...

Analysis of heat transfer in the water meniscus at the tip-sample contact in scanning thermal microscopy

Quantitative measurements of local nanometer-scale thermal measurements are difficult to achieve because heat flux may be transferred from the heated sensor to the cold sample through various elusive mixed thermal channels. This paper addresses one of these channels, the water meniscus at the nano-contact between a heated atomic force microscopy probe and a hydrophilic sample. This heat transfer mechanism is found to depend strongly on the probe temperature. The analysis of the pull-off forces as a function of temperature indicates that the water film almost vanishes above a probe mean temperature between 120 and 150 oC. In particular, a methodology that allows for correlating the thermal conductance of the water meniscus to the capillary forces is applied. In the case of the standard scanning thermal microscopy Wollaston probe, values of this thermal conductance show that the water meniscus mechanism is not dominant in the thermal interaction between the probe and the sample, regardless of probe temperature.

Temperature-dependent capillary forces at nano-contacts for estimating the heat conduction through a water meniscus

The temperature dependence of the capillary forces at nano-sized contacts is investigated. Two different resistive scanning thermal microscopy (SThM) nanoprobes are used in this study. Measurements of the capillary forces are reported as a function of the probe temperature on hydrophilic samples of different thermal properties. These forces appear to be largely reduced for probe temperatures larger than a threshold temperature, where the value depends on the sample thermal conductance. This could pave the way to an alternative solution to reduce the stiction in nano/ micro-electromechanical (NEMS/MEMS) devices. The dimensions of the water meniscus at the probe-sample contact were then estimated. Moreover, these results help the evaluation of thermal conductance through the water meniscus. It is found, through this work, that the values of the thermal conductance through the water meniscus can represent 6% of those of the contact thermal conductance in the case of the KNT probe (from Kelvin nanotechnology). These values can be equal to 4% of those of thermal conduction in the cantilever-sample air gap in the case of a doped-silicon probe.

Temperature Study of Sub-Micrometric ICs by Scanning Thermal Microscopy

Surface temperature measurements were performed with a scanning thermal microscope mounted with a thermoresistive wire probe of micrometric size. A CMOS device was designed with arrays of resistive lines 0.35 mum in width. The array periods are 0.8 mum and 10 mum to study the spatial resolution of the SThM. Integrated circuits (ICs) with passivation layers of micrometric and nanometric thicknesses were tested. To enhance signal-to-noise ratio, the resistive lines were heated with an ac current. The passivation layer of nanometric thickness allows us to distinguish the lines when the array period is 10 mum. The results raise the difficulties of the SThM measurement due to the design and the topography of ICs on one hand and the size of the thermal probe on the other hand.

Heat transfer mechanisms quantified at submicron scales in scanning thermal microscopy

This work investigates the heat transfer between scanning thermal microscopy (SThM) probes and samples. It presents a detailed study of the heat transfer mechanisms that operate between the probe and the sample. Two SThM resistive probes of different sizes were used in active mode. Depending on the experimental conditions, the heat transferred to the sample through water meniscus, solid-solid contact and air is quantified. The methodology established to estimate the heat conduction through water meniscus shows that this mechanism is not dominant in the tip-sample heat exchange. Based on experimental results of measurements performed under vacuum conditions, the thermal boundary resistance at different contacts is estimated and in accordance with literature values. Through measurements performed under ambient conditions, the heat conduction through air appears to be strongly dependent on the sample thermal conductivity.

Investigation of the thermal properties of thin solid materials at different temperature levels using a set of microresistors

The measurement of thermal properties of solid materials at different temperatures above ambient is investigated using a set of microresistors. Samples consisted of suspended films with sets of long, parallel resistive wires deposited on their surfaces. One resistive wire was heated by an alternating current. Surface temperature changes in DC and AC regimes were then detected by measuring the change in electrical resistance of the other wires deposited on the surface. The length of wires was chosen so that they may be assumed isothermal and such that heat diffusion acts perpendicularly to their axes. By measuring the dependence of the surface alternating temperature oscillation on the modulation frequency f and on the separation between the heating wire and the probing wires, the thermal diffusivity of the sample was determined. Through adjustment of the alternating current amplitude in the source wire, the temperature at which the thermal diffusivity of the sample was evaluated was finely controlled. For the validation of the method, pure silicon samples were first studied. An experimental bench was set up and resistive source and probes were experimentally characterized. Results obtained from ambient temperature to 500 K for pure silicon are in accordance with reference data found in the scientific literature.

Analysis of the Microstructure of Polymers With Regard to Their Thermomechanical History: STHM and DSC Measurements

The variation of the microstructure within the thickness of moulding plates of two semicrystalline polymers, an isotactic Poly-Propylene and a Poly-Butylene Terephtalate, was observed by optical microscopy technique. These observations allowed specifying the different zones of iso-microstructure within the plate thickness, commonly called “skin zone”, “shear zone”, “post filling zone ”and“ core zone”in terms of crystallite size and zone thickness. The variation of the melting temperature was then analysed by using a local thermal analysis method based on the scanning thermal microscopy technique in each of these zones. Our results show the expected link between the local microstructure and the polymer melting temperature. They also highlight a strong coupling between the microstructure, the material and its processing conditions.Copyright

Microfabricated sensor platform with through-glass vias for bidirectional 3-omega thermal characterization of solid and liquid samples

Abstract A novel microfabricated, all-electrical measurement platform is presented for a direct, accurate and rapid determination of the thermal conductivity and diffusivity of liquid and solid materials. The measurement approach is based on the bidirectional 3-omega method. The platform is composed of glass substrates on which sensor structures and a very thin dielectric nanolaminate passivation layer are fabricated. Using through-glass vias for contacting the sensors from the chip back side leaves the top side of the platform free for deposition, manipulation and optical inspection of the sample during 3-omega measurements. The thin passivation layer, which is deposited by atomic layer deposition on the platform surface, provides superior chemical resistance and allows for the measurement of electrically conductive samples, while maintaining the conditions for a simple thermal analysis. We demonstrate the measurement of thermal conductivities of borosilicate glass, pure water, glycerol, 2-propanol, PDMS, cured epoxy, and heat-sink compounds. The results compare well with both literature values and values obtained with the steady-state divided bar method. Small sample volumes (∼0.02 mm³) suffice for accurate measurements using the platform, allowing rapid temperature-dependent measurements of thermal properties, which can be useful for the development, optimization and quality testing of many materials, such as liquids, gels, pastes and solids.