WO2012144895A1 - Mesure du profil spatio-temporel de température d'un objet - Google Patents

Mesure du profil spatio-temporel de température d'un objet Download PDF

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Publication number
WO2012144895A1
WO2012144895A1 PCT/NL2012/050257 NL2012050257W WO2012144895A1 WO 2012144895 A1 WO2012144895 A1 WO 2012144895A1 NL 2012050257 W NL2012050257 W NL 2012050257W WO 2012144895 A1 WO2012144895 A1 WO 2012144895A1
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WO
WIPO (PCT)
Prior art keywords
luminophores
luminescence
coating
temperature
microscopic method
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Application number
PCT/NL2012/050257
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English (en)
Inventor
Paulus Hubertus Maria VAN LOOSDRECHT
Maxim Stanislavovich PCHENITCHNIKOV
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Rijksuniversiteit Groningen
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Publication of WO2012144895A1 publication Critical patent/WO2012144895A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
    • G01K11/00—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00
    • G01K11/20—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00 using thermoluminescent materials

Definitions

  • the invention is directed to a microscopic method for measuring a spatio-temporal temperature profile of an object.
  • Thermal management in innovative technologies is a major problem to be solved, especially in novel electronic devices, such as further miniaturised microchips, memory devices, and interfaces between biological structures and semiconductor microstructures. Therefore, the semiconductor industry is highly interested in new thermal imaging technologies which allow high space (viz. nanometer scale) and time resolution.
  • Some previously reported techniques for measuring surface temperature profiles of objects include infrared thermal microscopy and photo emission microscopy in combination with Raman microscopy.
  • US-A-4 455 741 describes a method of measuring surface temperature profiles of a device by applying a thin film of material to the device, which material luminesces when irradiated with appropriate energy. This document does not teach using a different delay period for each pulse sequence.
  • Kolodner et al. (Appl. Phys. Lett. 1982, 40(9), 782-784) describe the measurement of surface temperature profiles by depositing a film whose fluorescence quantum yield depends on the temperature. At low temperatures, the film exhibits bright fluorescence under ultraviolet excitation, while the fluorescence intensity decreases with temperature due to
  • the spatial resolution of the method in this document is limited by the diffraction limit (i.e. it is inversely proportional to the wavelength of the emitted light). For fluorescent materials this, typically, leads to a spatial resolution in the range of from 500 to 1000 nm. In addition, the technique in this document does not allow a high temporal resolution.
  • US-A-4 819 658 describes a method of measuring surface temperature profiles by applying a thin luminescent film to a device, wherein the intensity of the luminescence is dependent upon the temperature of the material. This document further suggests applying heat pulses and
  • photo-excitation pulses to reduce the time resolution, such as down to about 10 ns or less.
  • EP-A-1 936 345 describes a method of measuring a temperature distribution with high spatial and temporal resolution.
  • the method uses a layer that contains molecules which exhibit a temperature dependent luminescence ratio at a first and second wavelength.
  • stimulated emission depletion microscopy In order to reduce the spatial resolution beyond the diffraction limit, it is suggested to apply stimulated emission depletion microscopy.
  • Motosuke et al. (Journal of Mechanical Science and Technology 2009, 23, 1821-1828) describe the measurement of the temperature of a fluid in a microfluidic device with high temporal and spatial resolution using laser-induced fluorescence. Temperature dependency is induced by employing a temperature dependent fluorophore. Despite these reported efforts, there remains a need for improving the visualisation of a spatio-temporal temperature distribution of an object with excellent spatial, thermal, and temporal resolution.
  • Objective of the invention is to provide a solution for this existing need in the art.
  • the invention is directed to a microscopic method for measuring a spatio-temporal temperature profile of an object, comprising:
  • step iii) repeating step iii) for a number of times wherein in each step iii) a
  • the method of the invention allows the measurement of dynamic spatio-temporal temperature profiles, such as in micro-electromechanical systems or any object on which the coating can be applied.
  • the temperature profiles are advantageously translated into one or more microscopic images with excellent thermal, spatial and temporal resolution.
  • the inventors found that the method of the invention allows a thermal resolution of better than 0.01 K, a spatial resolution of better than 20 nm, and a temporal resolution of better than 500 ps. The combination of these excellent resolutions is unique to the method of this invention.
  • the object of which the spatio-temporal temperature profile is to be determined can be an electronic device, including a micro-electromechanical system, a biological object, or combinations thereof.
  • the object is a solid state object, or at least comprises a solid state surface onto which the coating can suitably be applied.
  • step i) of the method the object is provided with a coating.
  • the coating may be applied onto the object using conventional techniques, including spin-coating, dip -coating, drop casting, doctor blading,
  • the coating can be applied to the surface of the object in the form of a thin film.
  • the coating can suitably have a thickness of 10 nm or more, such as 100 nm or more, or 500 nm or more. Normally, the coating will have a thickness of 10 ⁇ or less, preferably 5 ⁇ or less, such as 2 ⁇ or less. If the coating thickness is more than 10 ⁇ , then this will have an adverse effect on the spatial and thermal resolution. For example, if the heat capacity of the coating is relatively large, the layer itself will distort the observed temperature profile.
  • the coating may optionally be a multilayer.
  • the coating comprises a material which luminesces upon exposure to radiation.
  • materials upon exposure to ultraviolet radiation (having a wavelength ranging from 200 to 400 nm), may be excited, and upon de-excitation will emit ultraviolet, visible (wavelength ranging from 400 to 700 nm), or infrared (wavelength ranging from 700 to 1000 nm) radiation.
  • ultraviolet radiation having a wavelength ranging from 200 to 400 nm
  • infrared wavelength ranging from 700 to 1000 nm
  • such materials are generally referred to as luminophores.
  • the term "luminophore” as used in this application is meant to refer to a species that upon photoexcitation can emit light through fluorescence or phosphorescence.
  • the term "luminophore” in the context of this application is meant to includes a fluorophore, a chromophore, a phosphorescent compound, a quantum dot, a luminescent nanoparticle (that for instance comprise multiple luminescent molecules), and the like.
  • Nanoparticles in this respect can have an average particle size (defined as the diameter of an equivalent sphere having the same volume) in the range of 1-500 nm, such as 10-200 nm.
  • the equivalent spherical diameter of nanoparticles can be determined by dynamic light scattering or by high resolution imaging techniques such as electron microscopies or by coherent X-ray imaging.
  • luminescence as used in this application is meant to refer to the emission of electromagnetic radiation (light) from a material. In particular, this term is meant to include fluorescence and phosphorescence.
  • the luminophores In order to achieve the required thermal accuracy, the luminophores must emit with an intensity that is characteristic of the temperature of the underlying object. Therefore, it is required that the coating is in thermal contact with the surface of the object. In addition, the luminophore must have a temperature dependent luminescence quantum yield so that it is capable of translating the temperature of the surface of the object to a luminescence intensity that is correlated with said temperature.
  • the luminophores in the coating can for example comprise one or more rare earth metal chelate luminophores.
  • the rare earth metal is preferably europium or terbium.
  • the chelate can, for instance, comprise one or more selected from bidentate ligands, tridentate ligands, and tetradentate ligands.
  • Examples of luminophores that can be used for this purpose include, but are not limited to, europium thenoyltrifluoro-acetonate (EuTTA) and perdeutero(tris-6, 6, 7, 7, 7, 8, 8-heptafluoro-2, 2-dimethyl-3, 5-octanedionate) europium (EuFOD).
  • the luminophore can be incorporated into a polymer film which is applied onto a surface of the object.
  • the luminophore and polymer can, for example, be dissolved in an appropriate solvent, and the solution can be spinned onto the surface of the object.
  • the solution can be filtered prior to spinning in order to remove aggregates or crystallites. The solvent evaporates during the spinning step, leaving a thin film of polymer homogeneously doped with the luminophore.
  • polymers that can be used for incorporation of the luminophore include polystyrenes,
  • polymethylmethacrylates polycarbonates, polysilicones (such as
  • poly(dimethylsiloxane), and polyolefins such as polyethylene or
  • the polymer is optically transparent (i.e. the thin film of polymer without the luminophore is preferably optically transparent).
  • optically transparent i.e. the thin film of polymer without the luminophore is preferably optically transparent.
  • the polymer is inert.
  • inert is meant to signify that such polymer is chemically inert, i.e. it neither undergoes chemical reactions with the fluorophore embedded in the polymer, nor with the sample.
  • the method of the invention is used to perform excellent temporal resolution (such as better than 1000 ps, smaller than 100 ps, or smaller than 10 ps) and temperature resolution (such as better than 1 K, better than 0.1 K, or better than 0.01 K) with good spatial resolution (such as better than 300 nm).
  • excellent temporal resolution such as better than 1000 ps, smaller than 100 ps, or smaller than 10 ps
  • temperature resolution such as better than 1 K, better than 0.1 K, or better than 0.01 K
  • good spatial resolution such as better than 300 nm.
  • the luminophores can have a temperature dependent quantum efficiency wherein preferably dl/dT is at least 1 % per degree K, more preferably at least 2 % per degree K, or even more preferably 5 % per degree K.
  • the coating can suitably have a
  • luminophore concentration in the range of 0.01-100 luminophores per 10 nm 3 of coating, such as in the range of 0.1-10 luminophores per 10 nm 3 of coating.
  • the luminophores are present in the coating at a
  • concentration in the range of from 20-50 mol% based on the total coating, preferably from 50-80 mol%.
  • the object is subjected to heat, after which multiple luminescence images are collected at variable delay time p in order to obtain the time development of the heat profile. Consequently, each of the luminescence images at a specific delay time can be converted into a temperature image using a calibrated relation between the luminescence intensity and temperature. This calibrated relation depends on the luminophore that is applied in the method of the invention and can be readily determined by the person skilled in the art.
  • step iii)a at least part of the coated object is subjected to heat.
  • the temporal behaviour of this heat defines a time to. This may be achieved, for instance, by applying a heat pulse (thereby defining a starting point), or by subjecting the object to a heat wave, which can define a time to using the wave phase.
  • the heat may be in pulsed or modulated mode.
  • the time scale of the induced transient heat variations may be in the range of 5 ps to 1 s.
  • the heat may, for example, be generated using a laser, a heater, an electronic element, or the like.
  • the coated object may be subjected to the heat as a whole, but also a part of the coated object can be subjected to the heat.
  • a delay time p is applied, after which at least part of the coated object is subjected to a photoexcitation pulse at time ti.
  • the photoexcitation pulse serves to photoexcite luminophores in the irradiated area. After photoexcitation, these photoexcited luminophores will return to their ground state while emitting light.
  • the photoexcitation pulse can, for example, be generated by means of a laser of diode.
  • the power of the source should be sufficient to excite at least part of the luminophores, such as at least 1 %, at least 10 %, or substantially all luminophores.
  • the photoexcitation pulse will be shorter than the time resolution that is intended.
  • the photoexitation pulse can last for 100 fs to 200 ps, such as 100 fs to 100 ps.
  • the photoexcitation pulse will normally be such that it
  • the wavelength of the photoexcitation pulse should be suitable for photoexcitation of the applied luminophores. Typically, the wavelength of the photoexcitation pulse will be in the ultraviolet (200-400 nm) or in the visible (400-700 nm) part of the spectrum.
  • the photoexcitation pulse can, for example, have a wavelength in the range of 250-700 nm, preferably in the range of 300-500 nm.
  • the lower limit of the delay time p is defined by the duration of the photoexcitation pulse, which can for instance be 10 ps, or preferably 5 ps.
  • the upper limit of the delay time p can, for example be in the range of 10 ps to 1 s and even longer, such as 10 ps, 1 ns, or 1 ⁇ . This delay time p is varied in step iv) of the method of the invention as will be discussed hereinafter.
  • step iii)d the luminescence image
  • the luminescence intensity can be collected as a function of the location.
  • a (x,y,I) image is obtained, wherein x is the location on the x-axis, y is the location on the y-axis, and I is the luminescence intensity.
  • the luminescence can be measured using a suitable detector, such as a charge coupled device (CCD) camera, or a photomultiplier. It is preferred to use a CCD camera.
  • CCD charge coupled device
  • each collected luminescence image in fact represents a difference luminescence image as a function of location ( ⁇ , ⁇ , ⁇ ). In this way, the temperature resolution of the method of the invention is improved.
  • the time interval At can vary widely, from 100 ns to 1 s, such as 500 ns to 500 ⁇ , and strongly depends on the lifetime of the luminescent state.
  • the luminescence collection will normally be focussed on the field of interest.
  • the luminescence can have varying wavelengths, depending on the applied luminophores. This may comprise wavelengths in the ultraviolet, visible or infrared range of the spectrum.
  • a step iii)e) may be performed wherein steps iii)a)-iii)d) are repeated for a number of times to improve the signal to noise ratio.
  • Good results in respect of improved signal to noise ratio can already be achieved by repeating steps iii)a)-iii)d) for 4 times or more, such as 9 times or more, or 16 times or more.
  • the signal to noise ratio can be improved by multiple repetitions, of course this involves additional measuring time. Depending on the application and the intended purpose, the skilled person will be able to balance the signal to noise ratio to the measuring time.
  • the method of the invention comprises a step iv) wherein step iii) is repeated for a number of times with variable delay time p (i.e. using for each step iii) a different delay time p).
  • variable delay time p i.e. using for each step iii) a different delay time p.
  • Step iii) can, for example, be repeated for 5 times or more, preferably for 7 times or more, such as 10-20 times.
  • step vi) of the invention the (x,y,I) images, that contain spatially resolved information on the luminescence intensity at different delay times p, are converted into (x,y,T) images, that contain spatially resolved information on the temperature at different delay times p.
  • This can be achieved by using a calibrated relation between the luminescence intensity of the applied luminophore and temperature. Such relation may be known for the respective luminophore, or it may be pre-determined. This may, for instance, be done using the procedure as described by Otter et al. in
  • each luminescence image represents a difference luminescence image
  • the ( ⁇ , ⁇ , ⁇ ) images are converted into ( ⁇ , ⁇ . ⁇ ) images.
  • the method of the invention is used to perform excellent temporal resolution (such as better than 1000 ps, smaller than 100 ps, or smaller than 10 ps), temperature resolution (such as better than 1 K, better than 0.1 K, or better than 0.01 K) and spatial distance resolution (such as better than 20 nm).
  • excellent temporal resolution such as better than 1000 ps, smaller than 100 ps, or smaller than 10 ps
  • temperature resolution such as better than 1 K, better than 0.1 K, or better than 0.01 K
  • spatial distance resolution such as better than 20 nm.
  • the luminophores (like in the first embodiment described above) can have a temperature dependent quantum efficiency wherein preferably dl/dT is at least 1 % per degree K, more preferably at least 2 % per degree K, or even more preferably 5 % per degree K.
  • the coating has a very low concentration of luminophores in the coating, such as 1-10 luminophores per 1 ⁇ 2 of coating. It is preferred in this embodiment, that the luminophores are nanoparticles, such as nanoparticles comprising multiple luminescent molecules.
  • FIG. 1 An example of an instrumental setup for carrying out the first or second embodiment of the invention is shown in figure 1, wherein 1 is a the object of which the spatio-temporal temperature profile is to be determined, 2 is a coating with a temperature-dependent luminescence material applied to the object, 3 is a heat control unit, 4 is a source of photo-excitation radiation, 5 is an image detector, 6 is a collection lens, and 7 is a beam splitter.
  • Steps iii) and iv) in this second embodiment are the same as for the first embodiment, described hereinabove.
  • the collected luminescence images at each delay period p are fitted to two dimensional peaked intensity distributions at the positions of the luminophores prior to converting the collected luminescence image at each delay period p to a temperature image using integrated peak intensities of single luminophores.
  • the spatial resolution of the method will be improved.
  • the method of the invention is used to perform excellent temporal resolution (such as better than 1000 ps, smaller than 100 ps, or smaller than 10 ps), temperature resolution (such as better than 1 K, better than 0.1 K, or better than 0.01 K) and spatial resolution (such as better than 20 nm). Contrary to the second embodiment, however, this third embodiment does not require such low concentration of luminophores.
  • the luminophores are single molecules that can have a temperature dependent quantum efficiency wherein preferably dl/dT is at least 1 % per degree K, more preferably at least 2 % per degree K, or even more preferably 5 % per degree K.
  • the luminophores have an active state (in which they are capable of luminescence when exited at a specific wavelength) and an inactive state (in which they are incapable of luminescence when excited at the same wavelength).
  • the transition of the active state to the inactive state may be reversible or irreversible. It can, for instance, be a photoisomerisation process, wherein one photoisomer represents the active state, while the other photoisomer represents the inactive state.
  • the luminophores are photoisomerising luminescent molecules.
  • the molecules can be rare earth metal chelates wherein the ligand can photoisomerise thereby allowing a transition from an active (luminescent) state to an inactive (non-luminescent) state of the molecule.
  • FIG. 2 An example of an instrumental setup for carrying out the third embodiment of the invention is shown in figure 2, wherein 1 is a the object of which the spatio-temporal temperature profile is to be determined, 2 is a coating with a temperature-dependent luminescence material applied to the object, 3 is a heat control unit, 4 is a source of photo-excitation radiation, 5 is an image detector, 6 is a collection lens, 7 and 8 are a beam splitters, and 9 is a source of activation/inactivation radiation.
  • the coating in accordance with this third embodiment, can suitably have a luminophore concentration in the range of 0.01-1 luminophores per 10 nm 3 of coating, such as in the range of 0.05-0.5 luminophores per 10 nm 3 of coating, or 0.1-0.5 luminophores per 10 nm 3 .
  • the luminophore concentration in the range of 0.01-1 luminophores per 10 nm 3 of coating, such as in the range of 0.05-0.5 luminophores per 10 nm 3 of coating, or 0.1-0.5 luminophores per 10 nm 3 .
  • luminophores are present in the coating at a concentration in the range of from 20-50 mol% based on the total coating, preferably from 50-80 mol%.
  • step iii) at least part of the coated object is subjected to an activation or inactivation radiation pulse, wherein part of the luminophores are at least temporarily activated or inactivated.
  • part of the luminophores are at least temporarily activated or inactivated.
  • 1-10 % of the luminophores (more preferably 1-5 % of the luminophores) in the area of interest should become or remain active after being subjected to the activation or inactivation radiation pulse, respectively.
  • this inactivation radiation pulse can have the effect that at least 90 % of the luminophores that are subjected to the inactivation radiation pulse is inactivated, preferably at least 95 %, such as at least 98 %.
  • this activation radiation pulse can have the effect that at most 10 %, of the luminophores that are subjected to the activation radiation pulse are activated, preferably at most 5 %, such as at most 2 %.
  • This activation or inactivation radiation pulse may typically be generated by a laser having a wavelength in the ultraviolet, visible or (near) infrared range of the spectrum.
  • the activation or inactivation radiation pulse can, for example, have a wavelength in the range of 250-1000 nm, preferably 350-800 nm Suitable lasers include, for instance, dye lasers, solid-state lasers or gas lasers.
  • the pulse can, for example, have a duration in the range of from 10 ps to 1 ms, such as in the range of from 100 ps to 100 ⁇ . Normally, the entire area of interest will be irradiated.
  • the exact timing of this activation or inactivation radiation pulse is not critical, as long as it is performed prior to step iii) of the method of the invention.
  • the concentration of luminophores can be at a reasonably high level, and in any case significantly higher than in the second embodiment.
  • Steps iii) and iv) in this third embodiment are the same as for the first and second embodiments, described hereinabove.
  • the third embodiment of the method of the invention further comprises a step v), after step iv), wherein previously activated luminophores are inactivated and/or destroyed, or wherein previously inactivated
  • This step may be performed by application of a laser pulse, such as an ultraviolet, visible or (near) infrared laser pulse.
  • the duration of the pulse may be from 10 ps to 1 ms, such as from 100 ps to 10 ⁇ , or from 1 ns to 1 ⁇ .
  • this step involves a back transition of previously converted photoisomers to their original state (before the activation or inactivation radiation pulse). Normally, this step will involve irradiation of the whole field of interest.
  • the collected luminescence images at each delay period p can be fitted to two dimensional peaked intensity distributions at the positions of the luminophores prior to converting the collected luminescence image at each delay period p to a temperature image using integrated peak intensities of single luminophores.
  • the spatial resolution of the method will be improved.
  • steps ii) to v) are repeated for a number of times in order to increase the spatial resolution.
  • the steps ii) to v) can be repeated for 2-50 times, such as 5-30 times, or 10-25 times.
  • the images at each specified delay time p from the repeated cycles are then combined to arrive at the desired spatio-temporal temperature profile of the object.

Abstract

La présente invention concerne un procédé microscopique permettant de mesurer un profil spatio-temporel de température d'un objet. Le procédé microscopique de l'invention comprend : i) l'application d'un revêtement sur l'objet, le revêtement contenant au moins un luminophore possédant un rendement quantique de luminescence dépendant de la température et étant en contact thermique avec la surface de l'objet ; iii) l'exécution de la séquence suivante : a) soumettre au moins une partie de l'objet revêtu à de la chaleur, ladite chaleur définissant un temps, t0 ; b) attendre pendant une période d'attente p ; c) soumettre au moins une partie de l'objet revêtu à une impulsion de photoexcitation à un temps t1 après t0, pour ainsi soumettre à une photoexcitation au moins une partie des luminophores, où t1 = t0 + p ; d) collecter une image de luminescence à partir des luminophores photoexcités pendant un intervalle de temps ?t, à partir d'un temps t2, à ou après t1 ; et e) répéter éventuellement les étapes a) à d) un certain nombre de fois pour améliorer le rapport signal sur bruit ; iv) la répétition de l'étape iii) un certain nombre de fois, la période d'attente p étant différente dans chaque étape iii) ; et vi) la conversion de l'image de luminescence collectée à chaque période d'attente p en image de température au moyen d'une relation étalonnée prédéterminée entre l'intensité de la luminescence et la température.
PCT/NL2012/050257 2011-04-20 2012-04-19 Mesure du profil spatio-temporel de température d'un objet WO2012144895A1 (fr)

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EP11163209.7 2011-04-20
EP11163209 2011-04-20
US201161481740P 2011-05-03 2011-05-03
US61/481,740 2011-05-03

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105890795B (zh) * 2016-04-09 2018-06-29 南昌航空大学 单光谱检测温度场的方法
CN109425624A (zh) * 2017-09-05 2019-03-05 株式会社岛津制作所 X射线成像装置
US20210364370A1 (en) * 2017-03-27 2021-11-25 The University Of Memphis Light Weight Flexible Temperature Sensor Kit

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US4455741A (en) 1982-02-11 1984-06-26 At&T Bell Laboratories Fabrication of solid state electronic devices using fluorescent imaging of surface temperature profiles
US4819658A (en) 1982-02-11 1989-04-11 American Telephone And Telegraph Company, At&T Bell Laboratories Method and apparatus for measuring the temperature profile of a surface
EP1936345A1 (fr) 2006-12-22 2008-06-25 Sony Deutschland Gmbh Détection haute résolution de la température et de la répartition de la température dans des dispositifs électroniques microscopiques et des objets biologiques

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US4455741A (en) 1982-02-11 1984-06-26 At&T Bell Laboratories Fabrication of solid state electronic devices using fluorescent imaging of surface temperature profiles
US4819658A (en) 1982-02-11 1989-04-11 American Telephone And Telegraph Company, At&T Bell Laboratories Method and apparatus for measuring the temperature profile of a surface
EP1936345A1 (fr) 2006-12-22 2008-06-25 Sony Deutschland Gmbh Détection haute résolution de la température et de la répartition de la température dans des dispositifs électroniques microscopiques et des objets biologiques

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105890795B (zh) * 2016-04-09 2018-06-29 南昌航空大学 单光谱检测温度场的方法
US20210364370A1 (en) * 2017-03-27 2021-11-25 The University Of Memphis Light Weight Flexible Temperature Sensor Kit
CN109425624A (zh) * 2017-09-05 2019-03-05 株式会社岛津制作所 X射线成像装置

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