WO2009125886A1 - Polymer measuring methods using microcantilever - Google Patents

Polymer measuring methods using microcantilever Download PDF

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Publication number
WO2009125886A1
WO2009125886A1 PCT/KR2008/002070 KR2008002070W WO2009125886A1 WO 2009125886 A1 WO2009125886 A1 WO 2009125886A1 KR 2008002070 W KR2008002070 W KR 2008002070W WO 2009125886 A1 WO2009125886 A1 WO 2009125886A1
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WO
WIPO (PCT)
Prior art keywords
microcantilever
polymer
temperature
cantilever
deflection
Prior art date
Application number
PCT/KR2008/002070
Other languages
French (fr)
Inventor
Sangmin Jeon
Namchul Jung
Hyejung Seo
Original Assignee
Postech Academy-Industry Foundation
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Publication date
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Publication of WO2009125886A1 publication Critical patent/WO2009125886A1/en

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00—Investigating or analyzing materials by the use of thermal means
    • G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
    • G01N25/12—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of critical point; of other phase change
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y35/00—Methods or apparatus for measurement or analysis of nanostructures
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/44—Resins; rubber; leather
    • G01N33/442—Resins, plastics

Definitions

  • the present invention relates to a method and an apparatus for detecting the phase transition of polymers. More particularly, the present invention relatesto an apparatus for detecting the phase transition temperatures of polymers using cantilevers with the polymers layered thereon which produce a deflection change with temperature, and a method for measuring the measuring phase transition temperatures of polymers using the same.
  • T g The glass transition temperature, accounting for an inherent property of a polymer, is usually measured by differential scanning calorimetry (DSC).
  • DSC is a thermoanalytical technique in which the difference in the amount of heat required to increase the temperature of a sample and a reference is measured as a function of temperature.
  • Heat sources divide DSC into power compensation DSC, heat flux DSC and a mixture thereof.
  • the present invention provides a method for measuring glass transition temperatures of polymers, comprising coating microcan- tilevers with respective polymers and monitoring a flexural property of the microcan- tilevers with changes in temperature.
  • the polymers are layered on upper or lower surfaces of the microcantilevers.
  • the layering of the polymers may be achieved by applying solutions of the polymers to the surfaces of the microcantilevers and drying them.
  • the term "the flexural property" accounts for a change in the deflection of the microcantilevers.
  • An embodiment of the present invention is accomplished by measuring the deflection of the microcantilevers with an optical means, an electrical means or a combination thereof.
  • the optical means may be a laser device, e.g., a He-Ne laser device that emits laser light to the cantilevers.
  • the electrical means is a piezoresistive cantilever which shows different resistances according to flexures of cantilevers.
  • the piezoresistive cantilever may be referred to Korean Patent Application No. 2006-115070 which is incorporated herein by reference in its entirety.
  • the microcantilevers preferably have micro-dimensions so that they can detect minute changes in, for example, glass transition temperature of polymers.
  • the microcantilevers are on the order of 0.1 to 10 microns in thickness and most preferably on the order of 0.5 to 5 microns in thickness. If cantilevers which are too thick are used, they cannot detect microscopic changes in the glass transition temperature. On the other hand, too small of a thickness makes it difficult to product the cantilevers commercially.
  • a glass transition temperature can be measured at a point where the deflection curvature of the cantilever changes on the heating and cooling curve after the enthalpic relaxation of the polymer.
  • the present invention provides an apparatus of measuring a glass transition temperature of a polymer, comprising at least one microcantilever with a polymer layered thereon; a heat controller for the micro- cantilever; and a detector for measuring the flexural property of the microcantilever.
  • the microcantilever is preferably plural in number so that it can measure a plurality of samples at the same time. More preferably, two or more microcantilevers are provided for the comparison of a sample and a reference. Most preferably, three or more microcantilevers are used to compare reference with a multiple number of samples.
  • the heat controller mounted on the cantilever comprises a heater and a thermocouple. Cooling may be accomplished in a natural manner or through a heat controller.
  • the flexural property of the microcan- tilevers can be measured.
  • deflection can be measured with a He-Ne laser in combination with a PSD.
  • the microcantilevers are arrayed on a mobile stage, for example, a motorized transitional stage, so that their flexural property can be measured with one laser when the stage is operated.
  • the present invention provides the use of a cantilever as a sensor for detecting the phase transition of a polymer. Changes in the volume of the polymer layered on the cantilever in the process of temperature elevation and phase transition, although not yet defined theoretically, influence the deflection of the cantilever. Thus, the deflection can account for the phase transition.
  • the phase transition may be that of glass transition, melting, or heat decomposition.
  • the present invention provides a method for detecting a phase transition of a polymer, comprising forming a polymer film on a cantilever; modulating the temperature of the cantilever with the polymer film formed thereon; and analyzingthe flexural property of the cantilever.
  • the temperature may be selected from a group consisting of a glass transition temperature, a melting point, and a decomposition temperature.
  • the cantilever As concerns the detection of phase transition, it may be affected by the thickness of the cantilever.
  • the cantilever is on the order of 0.1 to 10 microns so that it can detect a minute change such as glass transition.
  • An embodiment of the present invention is accomplished by measuring the deflection of the microcantilever with an optical means, an electrical means or a combination thereof. Accordingly, the flexural property accounts for a change in the deflection of the cantilever.
  • the polymer film can be formed using various techniques including coating, deposition, spraying, etc.
  • the present invention provides a sensor for detecting a phase transition temperature, comprising a piezoelectric microcantilever and a circuit for converting temperature-dependent deflection into an electric signal.
  • the present invention provides a phase transition temperature chip and preferably a glass transition temperature chip based on the sensor.
  • the method and apparatus in accordance with the present invention can analyze even a trance amount of sample.
  • the temperature of the cantilever is easily controlled, thus allowing the precise detection of phase transition.
  • the apparatus can determine glass transition temperatures of multiple samples very rapidly compared to conventional DSC.
  • FIG. l is a schematic view showing an apparatus for determining phase transition temperatures of polymers, using microcantilevers.
  • FIG. 2 is of heating and cooling curves of polyvinylacetate as determined by the apparatus equipped with microcantilevers in accordance with the present invention.
  • FIG. 3 is of heating and cooling curves of polystyrene as determined by the apparatus equipped with microcantilevers in accordance with the present invention.
  • FIG. 4 is a curve for determining the glass transition temperature of polyvinylacetate as measured by the apparatus equipped with silicon microcantilevers in accordance with the present invention.
  • FIG. 5 is a curve resulting from determining the glass transition temperature of polystyrene as determined by the apparatus equipped with silicon microcantilevers in accordance with the present invention.
  • FIG. 6 is a graph in which the glass transition temperatures of polystyrene are plotted against the molecular weights thereof as determined by the cantilever and DSC.
  • FIG. 7 is a graph in which the glass transition temperatures of polystyrene are plotted against heating rates. Best Mode for Carrying out the Invention
  • an apparatus for determining the glass transition temperatures of polymers using microcantilevers.
  • an array of microcantilevers each 400 microns long, 100 microns wide and 1 micronthick, is mounted on a motorized translational stage with a heater and a thermocouple associated with a heater controller thereon.
  • This apparatus is also equipped with a He-Ne laser means and a PSD for measuring the deflection (V) of the cantilevers.
  • a polymer for example, polyvinyl acetate
  • the deflection (V) of the polymer e.g., polyvinyl acetate
  • the temperature of the cantilever changing within the range of from 15 to 70 0 C.
  • the measurements are plotted in FIG. 2.
  • An inflection point of the deflection curvatures indicates a Tg of 40.95 0 C as shown in FIG. 4.
  • a polystyrene solution may be applied to a cantilever and dried to form a polystyrene film which is then measured for deflection (V) while its temperature is modulated within a range of from 0 to 15O 0 C.
  • V deflection
  • the deflection is plotted against temperature as shown in FIG. 3. Curvatures on the deflection plot indicate that polystyrene has a Tg of 100.49 0 C as shown in FIG. 5.
  • Tg of a polystyrene film formed on the cantilever is measured at various heating rates and the results are depicted in FIG. 7.

Abstract

Provided is an apparatus for detecting the phase transition of polymer using a microcantilever. The apparatus comprises an array of microcantilevers with various polymers layered thereon. The microcantilevers are measured for deflection at various temperatures to detect the phase transition of the polymers. The apparatus based on the microcantilever array can detect the phase transitions of various polymer samples very sensitively at the same time even if they are present in trace amounts, and the microcantilevers can be miniaturized. It allows the observation of novel physical changes which cannot be detected with conventional ones.

Description

Description
POLYMER MEASURING METHODS USING MICRO- CANTILEVER
Technical Field
[1] The present invention relates to a method and an apparatus for detecting the phase transition of polymers. More particularly, the present invention relatesto an apparatus for detecting the phase transition temperatures of polymers using cantilevers with the polymers layered thereon which produce a deflection change with temperature, and a method for measuring the measuring phase transition temperatures of polymers using the same. Background Art
[2] The glass transition temperature, Tg, accounting for an inherent property of a polymer, is usually measured by differential scanning calorimetry (DSC). DSC is a thermoanalytical technique in which the difference in the amount of heat required to increase the temperature of a sample and a reference is measured as a function of temperature. Heat sources divide DSC into power compensation DSC, heat flux DSC and a mixture thereof.
[3] Operating in such a manner as to concurrently heat a sample and a reference, however, conventional DSC is problematic in that it cannot measure multiple samples at the same time. In addition, this conventional technique suffers from the disadvantages of requiring a relatively large quantity of sample and it being costly to measure expensive samples.
[4] Accordingly, there is a need for a technique that is an alternative to DSC.
Disclosure of Invention Technical Problem
[5] It is therefore an object of the present invention to provide a novel method for measuring the glass transitiontemperatures of polymers.
[6] It is another object of the present invention to provide a method for detecting a change in polymer properties upon phase transition.
[7] It is a further object of the present invention to provide a device for measuring glass transition temperatures of polymers.
[8] It is still a further object of the present invention to provide a device for measuring glass transition temperatures of multiple samples at the same time.
[9] It is still another object of the present invention to provide the use of a micro- cantilever in detecting the phase transition of a polymer. Technical Solution [10] In order to accomplish the above objects, the present invention provides a method for measuring glass transition temperatures of polymers, comprising coating microcan- tilevers with respective polymers and monitoring a flexural property of the microcan- tilevers with changes in temperature.
[11] In accordance with the present invention, the polymers are layered on upper or lower surfaces of the microcantilevers. In an embodiment of the present invention, the layering of the polymers may be achieved by applying solutions of the polymers to the surfaces of the microcantilevers and drying them.
[12] As used herein, the term "the flexural property "accounts for a change in the deflection of the microcantilevers. An embodiment of the present invention is accomplished by measuring the deflection of the microcantilevers with an optical means, an electrical means or a combination thereof. The optical means may be a laser device, e.g., a He-Ne laser device that emits laser light to the cantilevers. In another embodiment of the present invention, the electrical means is a piezoresistive cantilever which shows different resistances according to flexures of cantilevers. The piezoresistive cantilever may be referred to Korean Patent Application No. 2006-115070 which is incorporated herein by reference in its entirety.
[13] In accordance with the present invention, the microcantilevers, as implied by the name thereof, preferably have micro-dimensions so that they can detect minute changes in, for example, glass transition temperature of polymers. In a preferred embodiment of the present invention, the microcantilevers are on the order of 0.1 to 10 microns in thickness and most preferably on the order of 0.5 to 5 microns in thickness. If cantilevers which are too thick are used, they cannot detect microscopic changes in the glass transition temperature. On the other hand, too small of a thickness makes it difficult to product the cantilevers commercially.
[14] For the determination of glass transition temperature, flexure changes with temperature are used. Changes in flexure with temperature elevation are preferred.
[15] Although not defined theoretically, a glass transition temperature can be measured at a point where the deflection curvature of the cantilever changes on the heating and cooling curve after the enthalpic relaxation of the polymer.
[16] In accordance with another aspect thereof, the present invention provides an apparatus of measuring a glass transition temperature of a polymer, comprising at least one microcantilever with a polymer layered thereon; a heat controller for the micro- cantilever; and a detector for measuring the flexural property of the microcantilever.
[17] In an embodiment of the present invention, the microcantilever is preferably plural in number so that it can measure a plurality of samples at the same time. More preferably, two or more microcantilevers are provided for the comparison of a sample and a reference. Most preferably, three or more microcantilevers are used to compare reference with a multiple number of samples.
[18] Provided for heating the cantilever in a controlled manner, the heat controller mounted on the cantilever comprises a heater and a thermocouple. Cooling may be accomplished in a natural manner or through a heat controller.
[19] Through a separately equipped laser system, the flexural property of the microcan- tilevers can be measured. In an embodiment of the present invention, deflection can be measured with a He-Ne laser in combination with a PSD. In accordance with the present invention, the microcantilevers are arrayed on a mobile stage, for example, a motorized transitional stage, so that their flexural property can be measured with one laser when the stage is operated.
[20] In accordance with a further aspect thereof, the present invention provides the use of a cantilever as a sensor for detecting the phase transition of a polymer. Changes in the volume of the polymer layered on the cantilever in the process of temperature elevation and phase transition, although not yet defined theoretically, influence the deflection of the cantilever. Thus, the deflection can account for the phase transition. In the practice of the present invention, the phase transition may be that of glass transition, melting, or heat decomposition.
[21] In accordance with still another aspect thereof, the present invention provides a method for detecting a phase transition of a polymer, comprising forming a polymer film on a cantilever; modulating the temperature of the cantilever with the polymer film formed thereon; and analyzingthe flexural property of the cantilever.
[22] In the present invention, the temperature may be selected from a group consisting of a glass transition temperature, a melting point, and a decomposition temperature.
[23] As concerns the detection of phase transition, it may be affected by the thickness of the cantilever. Preferably, the cantilever is on the order of 0.1 to 10 microns so that it can detect a minute change such as glass transition.
[24] An embodiment of the present invention is accomplished by measuring the deflection of the microcantilever with an optical means, an electrical means or a combination thereof. Accordingly, the flexural property accounts for a change in the deflection of the cantilever.
[25] The polymer film can be formed using various techniques including coating, deposition, spraying, etc.
[26] In accordance with yet another aspect thereof, the present invention provides a sensor for detecting a phase transition temperature, comprising a piezoelectric microcantilever and a circuit for converting temperature-dependent deflection into an electric signal.
[27] In accordance with yet a further aspect thereof, the present invention provides a phase transition temperature chip and preferably a glass transition temperature chip based on the sensor. Advantageous Effects
[28] Based on a novel mechanism in which the flexural properties of cantilevers are associated with temperature changes of polymers, a method and an apparatus are provided for determining the glass transition temperatures of polymers.
[29] Equipped with cantilevers in micron dimensions, the method and apparatus in accordance with the present invention can analyze even a trance amount of sample. In addition to being small in size, the temperature of the cantilever is easily controlled, thus allowing the precise detection of phase transition.
[30] Having multiple microcantilevers, the apparatus can determine glass transition temperatures of multiple samples very rapidly compared to conventional DSC. Brief Description of Drawings
[31] FIG. lis a schematic view showing an apparatus for determining phase transition temperatures of polymers, using microcantilevers.
[32] FIG. 2is of heating and cooling curves of polyvinylacetate as determined by the apparatus equipped with microcantilevers in accordance with the present invention.
[33] FIG. 3is of heating and cooling curves of polystyrene as determined by the apparatus equipped with microcantilevers in accordance with the present invention.
[34] FIG. 4 is a curve for determining the glass transition temperature of polyvinylacetate as measured by the apparatus equipped with silicon microcantilevers in accordance with the present invention.
[35] FIG. 5 is a curve resulting from determining the glass transition temperature of polystyrene as determined by the apparatus equipped with silicon microcantilevers in accordance with the present invention.
[36] FIG. 6 is a graph in which the glass transition temperatures of polystyrene are plotted against the molecular weights thereof as determined by the cantilever and DSC.
[37] FIG. 7 is a graph in which the glass transition temperatures of polystyrene are plotted against heating rates. Best Mode for Carrying out the Invention
[38] With reference to FIG. 1, an apparatus is providedfor determining the glass transition temperatures of polymers using microcantilevers. As seen in this figure, an array of microcantilevers, each 400 microns long, 100 microns wide and 1 micronthick, is mounted on a motorized translational stage with a heater and a thermocouple associated with a heater controller thereon. This apparatus is also equipped with a He-Ne laser means and a PSD for measuring the deflection (V) of the cantilevers.
[39] A polymer, for example, polyvinyl acetate, may be layered on the cantilever by applying a polymer solution to the cantilever and drying it. Using the He-Ne laser means and the PSD, the deflection (V) of the polymer, e.g., polyvinyl acetate, is measured with the temperature of the cantilever changing within the range of from 15 to 700C. The measurements are plotted in FIG. 2. An inflection point of the deflection curvatures indicates a Tg of 40.950C as shown in FIG. 4.
[40] Likewise, a polystyrene solution may be applied to a cantilever and dried to form a polystyrene film which is then measured for deflection (V) while its temperature is modulated within a range of from 0 to 15O0C. The deflection is plotted against temperature as shown in FIG. 3. Curvatures on the deflection plot indicate that polystyrene has a Tg of 100.490C as shown in FIG. 5.
[41] Polystyrene of various molecular weights was applied to cantilevers and measured for Tgs. The measurements are plotted in FIG. 6 and compared with those measured with DSC.
[42] Additionally, Tg of a polystyrene film formed on the cantilever is measured at various heating rates and the results are depicted in FIG. 7.

Claims

Claims
[I] A method for measuring a glass transition temperature of a polymer, comprising coating a microcantilever with the polymer and monitoring a flexural property of the microcantilever with a change in temperature.
[2] The method according to claim 1, wherein the polymer is applied to one surface of the microcantilever. [3] The method according to claim 1, wherein the flexural property takes into account deflection of the microcantilever. [4] The method according to claim 3, wherein the deflection is measured using one selected from a group consisting of an optical means, an electric means and a combination thereof. [5] The method according to claim 1 or 2, wherein the microcantilever ranges in thickness from 0.1 to 10 microns. [6] The method according to claim 1, wherein the temperature is changed at different rates to measure glass transition temperatures with regard to heating rates. [7] The method according to claim 4, wherein the optical means is a laser device.
[8] The method according to claim 4, wherein the electric means utilizes a piezoelectric effect. [9] The method according to claim lor 2, wherein the temperature is modulated by heating, cooling or a combination thereof. [10] The method according to claim 1 or 2, wherein the glass transition temperature is determined from deflection curvatures on a heating and cooling curve.
[I I] An apparatus of measuring a glass transition temperature of a polymer, comprising: at least one microcantilever with a polymer layered thereon; a heat controller for the microcantilever; and a detector for measuring a flexural property of the microcantilever.
[12] The apparatus according to claim 11, wherein the polymer is applied to a surface of the microcantilever.
[13] The apparatus according to claim 11, wherein the heat controller is able to heat or cool the microcantilever.
[14] The apparatus according to one of claims 11 to 13, wherein the flexural property takes into account defection of the microcantilever. (— wherein the defection of the microcantilever causes the flexural property? — )
[15] The apparatus according to claim 14, wherein the microcantilever is a piezoelectric device.
[16] The apparatus accordingto claim 11 or 12, wherein the glass transition tern- perature is measured at a point where the deflection curvature of the cantilever changes on a heating and cooling curve of the polymer after the polymer undergoes enthalpic relaxation. [17] Use of acantilever as a sensor for measuring a phase transition property of a polymer. [18] The use according to claim 17, wherein the phase transition property is selected from a group consisting of glass transition, melting and thermal decomposition. [19] A method for detecting phase transition of a polymer, comprising: forming a polymer film on a cantilever; m odulating a temperature of the cantilever with the polymer film formed thereon; and analyzing a flexural property of the cantilever. [20] The method according to claim 19, wherein a temperatureof the phase transition to be detected is selected from a group consisting of a glass transition temperature, a melting point, and a thermal decomposition temperature. [21] The method according to claim 19, wherein the cantilever ranges in thickness from 0.1 to 10 microns. [22] The method according to claim 19or 20, wherein the flexural property of the cantilever is measured using one selected from a group consisting of an optical means, an electric means and a combination thereof. [23] The method according to claim 19 or 20, wherein the flexural property accounts for a deflection curvature with regard to temperatures. [24] The method according to claim 19 or 20, wherein the temperature is modulated by heating or cooling. [25] The method according to claim 19 or 20, wherein the polymer film is formed using a coating technique or a deposition technique. [26] Asensor for detecting a phase transition temperature, comprising a piezoelectric microcantilever and a circuit for converting temperature-dependent deflection into an electric signal. [27] A chip for detecting a phase transition temperature, comprising a piezoelectric microcantilever and a circuit for converting temperature-dependent deflection into an electric signal.
PCT/KR2008/002070 2008-04-08 2008-04-11 Polymer measuring methods using microcantilever WO2009125886A1 (en)

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KR10-2008-0032892 2008-04-08
KR1020080032892A KR20090107390A (en) 2008-04-08 2008-04-08 Polymer measuring methods using microcantilever

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Citations (3)

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US20050121615A1 (en) * 2000-10-30 2005-06-09 Craig Prater Cantilever array sensor system
US6935165B2 (en) * 2002-03-20 2005-08-30 Purdue Research Foundation Microscale sensor element and related device and method of use
JP2006329955A (en) * 2005-05-30 2006-12-07 Rikogaku Shinkokai Heat characteristic measuring instrument and heat characteristic measuring method

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Publication number Priority date Publication date Assignee Title
US20050121615A1 (en) * 2000-10-30 2005-06-09 Craig Prater Cantilever array sensor system
US6935165B2 (en) * 2002-03-20 2005-08-30 Purdue Research Foundation Microscale sensor element and related device and method of use
JP2006329955A (en) * 2005-05-30 2006-12-07 Rikogaku Shinkokai Heat characteristic measuring instrument and heat characteristic measuring method

Non-Patent Citations (2)

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Title
BOHME, THOMAS: "EVIDENCE FOR SIZE DEPENDENT MECHANICAL PROPERTIES FROM SIMULATIONS OF NANOSCOPIC POLYMERIC STRUCTURES", JOURNAL OF CHEMICAL PHYSICS, vol. 116, no. 22, 2002, WISCONSIN, pages 9950 - 9951 *
BOWLES, ANITA: "STRESS EVOLUTION IN THIN FILMS OF A POLYMER", 2006, HARVARD UNIVERSITY, pages: 16, - 27-29,79 *

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