Systems and methods for analyzing viscoelastic properties of...

Data processing: measuring – calibrating – or testing – Measurement system in a specific environment – Chemical analysis

Reexamination Certificate

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C702S022000, C324S071100, C324S715000, C436S002000, C073S023200, C374S010000

Reexamination Certificate

active

06671631

ABSTRACT:

BACKGROUND OF THE INVENTION
The present invention relates generally to systems and methods for analyzing the viscoelastic properties of combinatorial libraries of materials. More specifically, the present invention relates to systems and methods for analyzing the thermal properties of libraries of polymers and polymer films using an array of full bridge devices. The systems and methods of the present invention may also be used to analyze such properties as vapor sorption, chemical resistance, weatherability, and oxidative stability.
Typically, the viscoelastic properties of materials, such as polymers and polymer films, have been analyzed using devices such as acoustic wave devices, micro-hotplates, micromechanical calorimetric sensors, and shear/stress sensors. For example, acoustic wave devices have been used to measure the glass transition temperature and melting temperature of materials. Micro-hotplates have been used as micron-scale differential scanning calorimeters on a chip. Micromechanical calorimetric sensors have been used to detect thermal changes in test samples containing biomolecules undergoing chemical and biochemical reactions. Other sensor devices have been arranged in a standard combinatorial array configuration.
U.S. Pat. No. 4,312,228 discloses an acoustic wave sensor and methods for monitoring predetermined parameters of polymers including generating a surface acoustic wave in a piezoelectric material element and contacting a thin layer of the polymer with the surface through which the acoustic wave travels. The thin polymer layer is subjected to variations in environment thereby modifying the predetermined parameter of the polymer and changing the velocity of acoustic waves in and/or a dielectric property of the polymer, thus altering the frequency, amplitude, and/or phase of the surface acoustic wave. These alterations may be measured and related to glass transition temperature, the rate of solvent evaporation from the polymer, the photo-crosslinking characteristics of the polymer, and the crystalline transition characteristics of the polymer.
U.S. Pat. No. 6,079,873 discloses a differential scanning microcalorimeter produced on a silicon chip that enables microscopic scanning calorimetry measurements of small material samples and thin films. The microcalorimeter includes a reference zone and a sample zone. An integrated polysilicon heater provides heat to each zone and a thermopile including a succession of thermocouple junctions generates a voltage representing the temperature difference between the reference zone and the sample zone. Temperature differences between the zones provide information about the chemical reactions and phase transitions which occur in a sample placed in the sample zone.
U.S. Pat. No. 5,451,371 discloses a non-scanning, constant temperature microcalorimeter device. The device is built on a silicon base which is etched, leaving a frame of silicon supporting two polysilicon platforms. A catalyst is disposed on one platform to sense the presence of hydrocarbons. Platinum resistors on each platform serve as heaters and thermometers.
U.S. Pat. No. 6,096,559 discloses a calorimeter sensor apparatus using microcantilevered spring elements for detecting thermodynamic changes within a material sample containing biomolecules that undergo chemical and biochemical reactions. The spring elements each include a bimaterial layer of chemicals disposed on a coated region of at least one surface of the microcantilever. The chemicals generate a differential thermal stress across the surface upon reaction of the chemicals with an analyte or biomolecules within the sample due to the heat of the resulting reactions. The thermal stress experienced by the spring element creates a mechanical bending of the microcantilever. Deflections of the microcantilever may be detected by a variety of detection techniques.
U.S. Pat. No. 5,719,324 discloses a piezoelectric transducer that is fabricated with a cantilever having a spring element which is treated with a chemical having an affinity for a specific vapor phase chemical. An oscillator means maintains a resonant vibrational frequency during the detection of the chemical, with changes in resonant vibrational frequency indicating amounts of the targeted chemical present in the monitored atmosphere.
U.S. Pat. No. 5,445,008 discloses a mass microsensor that is also fabricated with a microcantilever having a material which absorbs a targeted chemical from the monitored atmosphere. Oscillation is induced using a piezoelectric transducer and the resonant frequency of the microcantilever is analyzed to detect amounts of the targeted chemical present in the monitored atmosphere. U.S. Pat. No. 5,475,318 discloses a microprobe including a microcantilever, a base, a probe tip projecting from the base, and a heating element that may be used to probe the material to be investigated.
U.S. Pat. No. 4,963,815 discloses a device and a method for determining an analyte by measuring a redox potential-modulated photoinducing electrical signal from an electrically conducting layer of a semiconductor device.
U.S. Pat. No. 6,106,149 discloses a mass and heat flow measurement sensor including a microresonator, such as a quartz crystal microbalance (QCM), a heat flow sensor, such as an isothermal heat conduction calorimeter, and a heat sink thermally coupled to the heat flow sensor. The microresonator may be used to measure changes in mass of a material sample at its surface and the heat flow sensor, which is thermally coupled to the microresonator, may be used to measure heat flow from the material sample to the heat sink.
U.S. Pat. No. 6,157,009 discloses a reactive screening tool, such as a calorimeter apparatus, having a low test cell-to-test sample thermal mass ratio so as to minimize heat sink effects on the test sample during chemical reaction. A heater control algorithm includes a calibration stage during which the heater is set to the predetermined test conditions and a test stage during which the heater controls the test conditions in a ramping mode and in an adiabatic mode. The reactive screening tool may also include a foam detector for detecting the presence of foam in the test sample.
U.S. Pat. No. 5,563,341 discloses a vapor pressure sensor including a substrate having a body with first and second parallel planar surfaces. A hole is formed in the body and extends through and between the first and second surfaces. A beam disposed within the hole in the body is formed as a cantilever. A vapor absorbing polyimide coating of substantially uniform thickness is disposed on the surface of the beam in full shear restraint. A strain measuring device forms a portion of a bridge carried by the substrate and measures shear forces exerted on the beam by the vapor absorbing coating.
U.S. Pat. No. 4,969,359 discloses a silicon accelerometer responsive to three (3) orthogonal force components. Three rectangular beams or cantilevers are formed, each having vertical sidewalls lying in crystalline planes orthogonal to one another.
U.S. Pat. No. 6,126,311 discloses a dew point sensor using micro-electromechanical systems (MEMS) including a microcantilevered beam formed on a substrate. A cooling device and a temperature sensor are in thermal communication with the microcantilevered beam and a control circuit operable for controlling and monitoring its resonance. The dew point is determined by identifying the temperature of the microcantilevered beam when its resonance or vibratory mode changes due to a change in mass caused by the formation of dew on the microcantilevered beam.
U.S. Pat. No. 6,016,686 discloses a micromechanical microcantilever potentiometric sensor used for detecting and measuring predetermined physical and chemical parameters in a material sample. A spring element includes a region coated with at least one chemical coating that accumulates a surface charge in response to hydrogen ions, redox potential, or ion concentrations in the material sample being monitored. Differing surface charges on opposing surfaces create a

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