Abstract: A sample and a scanning probe microscope system are used as the detector for an infrared spectrometer to circumvent the diffraction limit of conventional infrared microscopy, and to provide spectroscopic images with a greatly improved spatial resolution, potentially as low as a few tens of nanometers. The beam from an infrared spectrometer is directed at the sample. The sample is heated to the extent that it absorbs infrared radiation. Thus the resulting temperature rise of an individual region depends upon the particular molecular species present, as well as the range of wavelengths of the infrared beam. These individual temperature differences are detected by a miniature thermal probe. The thermal probe is mounted in a scanning thermal microscope. The scanning thermal microscope is then operated used to produce multiple surface and sub-surface images of the sample, such that the image contrast corresponds to variations in either thermal diffusivity, surface topography or chemical composition.

Abstract: A system and method for performing localized mechanothermal analysis with scanning probe microscopy (“MASM”) is disclosed. In a preferred embodiment an image of the surface or subsurface of a sample is created. A localized region of the sample is selected from the image. Using a scanning microscope, an active or passive thermal probe is positioned at the selected region. A temperature ramp is applied to the localized region. In addition, a dynamic or modulated stress or strain is applied to the localized region. Force data resulting from the applied temperature and stress or strain is collected and processed to produce a graph or fingerprint of the dynamic mechanical and/or calorimetric properties of the selected localized region.

Abstract: A platinum/Rhodium resistance thermal probe is used as an active device which acts both as a highly localized heat source and as a detector to perform localized differential calorimetry, by thermally inducing and detecting events such as glass transitions, meltings, recystallizations and thermal decomposition within volumes of material estimated at a few .mu.m.sup.3. Furthermore, the probe is used to image variations in thermal conductivity and diffusivity, to perform depth profiling and sub-surface imaging. The maximum depth of the sample that is imaged is controlled by generating and detecting evanescent temperature waves in the sample.

Abstract: A modulated differential scanning calorimeter ("MDSC") wherein the temperature of the sample and/or the reference is modulated by modulating the characteristics of a gas in thermal contact with the sample and or a reference. In a first embodiment, the major heat flow path between the sample/reference and the furnace is the purge gas in the furnace chamber. The composition of the purge gas in the furnace chamber of the DSC cell is modulated by alternately purging the DSC cell with a high thermal conductivity gas (e.g., helium) and with a low thermal conductivity gas (e.g., nitrogen), thus modulating the flow of heat to and from the cell. In a second embodiment, the sample and reference are heated (or cooled) by a temperature-controlling gas flowing around the sample and reference holders. The gas is heated by being passed through a furnace before it flows around the sample and the reference.

Abstract: The interpretation of dynamic differential calorimetry ("DDSC") data is enhanced by parsing the data according to whether it is obtained while the sample is being heated, cooled, or re-heated. Each DDSC scan is split up into three separate components, depending upon whether the sample is undergoing heating, cooling or reheating. Each component can then be analyzed separately to investigate the sample response to temperature change as the sample is being heated, cooled, or re-heated. Each file is deconvoluted separately, using a deconvolution routine that first removes the effect of the phase lag due to the instrument's finite response time.

Abstract: The present invention is a modulated differential thermal analysis technique for determining the composition, phase, structure, identification, or other properties of a material that undergoes a transition as function of temperature or other driving variable. As applied to differential scanning calorimetric analysis (DSC), the preferred embodiment comprises (1) heating a sample of the material with a linear temperature ramp that is modulated with a sinusoidal heating rate oscillation; (2) simultaneously heating a reference at the same linear temperature ramp; (3) measuring the differential temperature of the sample and reference; and (4) deconvoluting the resultant heat flow signal into rapidly and non-rapidly reversible components.

Abstract: The present invention relates to differential analytical techniques for determining the composition, phase, structure, identification or other properties of a material that undergoes a transition as function of a driving variable. As applied to differential scanning calorimetric analysis (DSC), the preferred embodiment comprises: (1) heating a sample of the material with a linear temperature ramp that is modulated with a sinusoidal heating rate oscillation; and (2) deconvoluting the resultant heat flow signal into rapidly reversible and non-rapidly reversible components.

Abstract: A method and apparatus for measuring the thermal conductivity of materials using modulated differential scanning calorimetry (MDSC). Two MDSC heat capacity measurements are made consecutively. One measurement is made under conditions which ensure obtaining a fairly accurate value for the heat capacity of the material ("quasi-ideal conditions"). Another measurement is made under conditions such that the measured effective heat capacity differs from the accurate value of the heat capacity due to thermal conductivity effects. Generally, the non-ideal conditions differ from the ideal conditions by one parameter, such as the size of the sample, the modulation frequency used to measure the heat capacity, or, for thin films, the presence or absence of a specimen on the thin film. The thermal conductivity of the material is then calculated from the difference between the heat capacity measured under quasi-ideal conditions and the effective heat capacity measured under non-ideal conditions.

Abstract: The present invention is a spatially-resolved differential analysis technique. A modulated differential analysis technique is applied using a proximal probe to obtain a spatially resolved characterization of a heterogeneous sample comprising at least two phases. As applied to spatially-resolved modulated differential scanning calorimetry, the present invention comprises a thermocouple probe that is scanned over the sample surface. The differential temperature of the area of the sample just beneath the thermocouple probe is obtained with respect to the temperature of a reference. The temperature of the sample and the reference is modulated above and below a transition temperature for one phase of the sample. The signal from the thermocouple probe is deconvoluted to obtain an image of the sample delineating the regions of the sample having that phase.

Abstract: The present invention relates to differential analytical techniques for determining the composition, phase, structure, identification or other properties of a material that undergoes a transition as function of a driving variable. As applied to differential scanning calorimetric analysis (DSC), the preferred embodiment comprises: (1) heating a sample of the material with a linear temperature ramp that is modulated with a sinusoidal heating rate oscillation; and (2) deconvoluting the resultant heat flow signal into rapidly reversible and non-rapidly reversible components.