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(12) United States Patent (10) Patent No.: US 8,177,422 B2 Kjoller Et Al

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(12) United States Patent (10) Patent No.: US 8,177,422 B2 Kjoller Et Al US008177422B2 (12) United States Patent (10) Patent No.: US 8,177,422 B2 Kjoller et al. (45) Date of Patent: May 15, 2012 (54) TRANSITION TEMPERATURE (56) References Cited MICROSCOPY U.S. PATENT DOCUMENTS (75) Inventors: Kevin Kjoller, Santa Barbara, CA (US); 6,185.992 B1* 2/2001 Daniels et al. ................ 25O?307 Khoren Sahagian, Burbank, CA (US); 6,200,022 B1* 3/2001 Hammiche et al. ............. 374/46 Doug Gotthard, Carpinteria, CA (US); gig3. R : S383 Airectalammiche et al. .............. (92.i Althy E" E. EcA 6,805,839 B2 * 10/2004 Cunningham et al. ... 422/82. 12 (US); Craig Prater, Santa Barbara, 7,448,798 B1 * 1 1/2008 Wang ..................... ... 374f183 (US); Roshan Shetty, Westlake Village, 2002/O126732 A1* 9, 2002 Shakouri et al. .............. 374,130 CA (US); Michael Reading, Norwich 2002/0196834 A1* 12/2002 Zaldivar et al. ................. 374,22 (GB) 2004/0026007 A1 2/2004 Hubert et al. ................... 156,64 2004/0202226 A1* 10, 2004 Gianchandani et al. ...... 374,185 2005/0105097 A1* 5/2005 Fang-Yen et al. ... 356,497 (73) Assignee: Anasys Instruments, Santa Barbara, CA 2006/0243034 A1 ck 11, 2006 Chand et al. T3/104 (US) 2007/0263696 A1* 11/2007 Kjoller et al. 374/31 2009 OO32706 A1* 2, 2009 Prater et al. 25O?307 (*) Notice: Subject to any disclaimer, the term of this 2009/0229020 A1* 9, 2009 Adams et al. ................... 850/33 patent is extended or adjusted under 35 SR A. 1939 CC. C. al . 3. U.S.C. 154(b) by 474 days. 2011/0078834 A1* 3/2011 King ................................. 850/9 (21) Appl. No.: 12/228,877 * cited by examiner (22) Filed: Aug. 15, 2008 Primary Examiner — Lisa Caputo Assistant Examiner — Mirellys Jagan (65) Prior Publication Data (74) Attorney, Agent, or Firm — Mark Rodgers US 201O/OO42356 A1 Feb. 18, 2010 (57) ABSTRACT (51) Int. Cl. A system and method for automatic analysis of temperature GOIN 25/00 (2006.01) transition data over an area of a sample surface. The system GOIK 3/00 (2006.01) relies on the use of a microfabricated probe, which can be GOIK 700 (2006.01) rapidly heated and cooled and has a sharp tip to provide high (52) U.S. Cl. .......... 374/16; 37.4/137; 374/164; 374/166; spatial resolution. The system also has fast X-y-Z positioners, 374/167 data collection, and algorithms that allow automatic analysis (58) Field of Classification Search .................... 374/16, of and visualization of temperature transition data. 374/137, 164, 166, 167 See application file for complete search history. 18 Claims, 8 Drawing Sheets Force feedback Nanothermal analysis curve 30 Cantilever motion Automatic Transition Detection 29 Temperature Nano 32 positioner / Thermal Controller 22 Transition temperature micrograph U.S. Patent May 15, 2012 Sheet 1 of 8 US 8,177,422 B2 OueN Jeuo???SOd 2Za NZII31H U.S. Patent May 15, 2012 Sheet 2 of 8 US 8,177,422 B2 U.S. Patent May 15, 2012 Sheet 3 of 8 US 8,177,422 B2 : w re: U.S. Patent May 15, 2012 Sheet 4 of 8 US 8,177,422 B2 †313 04 ZZ 9/ 8/ #8 U.S. Patent May 15, 2012 Sheet 6 of 8 US 8,177,422 B2 s U.S. Patent May 15, 2012 Sheet 7 of 8 US 8,177,422 B2 09 U.S. Patent May 15, 2012 Sheet 8 of 8 US 8,177,422 B2 US 8, 177,422 B2 1. 2 TRANSTION TEMPERATURE identify amorphousand crystalline regions, and identify dif MICROSCOPY ferent drug polymorphs, along with many other applications. BACKGROUND OF THE INVENTION BRIEF DESCRIPTION OF THE DRAWINGS This invention relates to a novel form of microscopy that The invention will be better understood by referring to the allows high resolution mapping of thermal transitions of following figures. materials. Measurement of thermal properties of materials is FIG. 1 is a simplified schematic diagram of an apparatus critical to the development of novel materials, including poly for transition temperature microscopy. mers and pharmaceuticals. Understanding the performance 10 FIG. 2 is a simplified schematic diagram of a nanothermal of materials at different temperatures is essential for applica analysis probe used for transition temperature microscopy. FIG.3 is an example of automated determination of a local tions like automotive components, construction materials, thermal transition temperature. food packaging, consumer electronics, drug delivery and FIG. 4 is a simplified Schematic diagram of a process flow many others. A key aspect of a materials thermal perfor 15 for transition temperature microscopy. mance is provided by its thermal transition temperatures, for FIG. 5 is an example transition temperature microscope example rubber/glassy transitions, and melting transitions. image of a blend of two polymer components. Many composite materials are manufactured with micro and FIG. 6 is an example transition temperature map of an nanoscale blends of different materials, for example plastic embedded epoxy sample. materials for stiffness and rubbery materials for energy FIG. 7 shows a simplified Schematic diagram of an appa absorption. Conventional techniques for imaging these mate ratus for determining the transition an alternative embodi rials includes TEM and Atomic Force Microscopy (AFM). In ment of transition temperature microscopy employing an AFM, phase imaging, as described in U.S. Pat. No. RE36,488 oscillatory heating profile. is commonly used to distinguish different materials in a mul FIG. 8 is a simplified diagram showing a method of deter ticomponent blend. While phase imaging has been very Suc 25 mining a transition temperature from the apparatus of FIG. 7. cessful for distinguishing some materials from each other, it is primarily sensitive to differences in mechanical properties, DETAILED DESCRIPTION OF THE INVENTION for example friction, adhesion, Viscolasticity and stiffness. In many cases, it is difficult to attribute the contrast to a quanti This invention provides high resolution microscope fiable physical property. And in Some cases little or no con 30 images of thermal transition temperatures. trast exists between materials, even when the materials have FIG. 1 is a simplified schematic diagram of an apparatus very different chemical and thermal properties. These mate for transition temperature microscopy. A probe 2 comprising rials may, however, have different thermal transition tempera a cantilever 4 and a heatable probe tip 6 is brought close to a tures. surface of sample 8. Thermal controller 22 supplies a control Bulk thermal analysis is a widely used technique. Tech 35 signal to a heater region 5 of the probe. A portion of the heat niques like differential scanning calorimetery (DSC) are from the probe flows from the probe tip 6 into the sample 8. widely used to measure thermal transitions. DSC, however, is The increase in Sample temperature causes a detectable probe performed on bulk samples and the transitions measured are data signal sensed by the probe. In one embodiment the not spatially differentiated. For this reason, extensive detected probe data signal is the motion of the cantilever. In research has been performed on local measurements of ther 40 this embodiment, the temperature rise of the sample may mal phase transitions using heated probe tips. Micro Thermal cause athermal expansion of the sample. This thermal expan Analysis employed Wollaston wire cantilever probes and sion may be detected by recording a change in the bend, measured thermal transitions on the scale of many microns. vertical position, and/or oscillation of the cantilever. One Nano Thermal Analysis (NanoTA) employs sharp probes simple method is to record the deflection of the cantilever 4 as typically microfabricated out of silicon based materials to 45 a function of the applied heater control signal 24. The canti measure transition temperatures over regions on Scales of less lever deflection can be measured in many ways, the most than 100 nm. Conventional micro and nanothermal analysis common being to use the optical lever deflection method. In measurements, however are measured manually at single this scheme a light beam 10 from a light source 12 is directed points or a handful of points without the ability to spatially to the backside of the cantilever 4 and the reflected beam 11 is resolve detailed variations in thermal transition temperatures. 50 directed toward a position sensitive detector 14. Analog and/ As such, no current technique provides high resolution or digital electronics 16 conditions the photodiode signal to images of transition temperatures. create a signal indicative of the cantilever deflection and/or oscillatory motion. BRIEF SUMMARY OF THE INVENTION The cantilever motion can also be measured using alterna 55 tive techniques to the optical lever arm, including but not Transition temperature microscopy allows high resolution limited to interferometric, thermal, piezoresistive, piezoelec measurements of the thermal phase transitions that occur in tric, capacitive, and/or inductive readout schemes. The non many materials. Based on probe microscopy and nanothermal optical techniques, especially piezoresistive and thermal sen analysis, transition temperature microscopy allows scientists sors can be directly integrated into the same probe 2 as the and engineers to reveal Surface structure of materials on 60 heater element. Demonstrations of the use of thermal detec scales from centimeters to nanometers by automatically mea tion of cantilever motion have been demonstrated by Prof. Suring and identifying temperatures at which thermal phase William King and coworkers. Any detection system that can transitions (e.g. glass transition temperatures and/or melting create a signal indicative of the cantilever motion on the scale points) occur. These thermal phase transition temperatures of 10s of nanometers may be sufficient. The probe data signal give critical information about material structure and compo 65 may also be due to the cantilever bend, cantilever oscillation, sition. Transition temperature microscopy can be used to including any combination of oscillation amplitude, phase, identify different material components in a composite blend, and/or frequency.
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