• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The invention relates to a method for manufacturing a piezoelectric and / or pyroelectric device comprising a film (16) comprising polyvinylidene fluoride and / or at least one copolymer of polyvinylidene fluoride, the method comprising a step of forming a minus a portion (14) of a layer of a solution comprising a solvent and a compound comprising polyvinylidene fluoride and / or at least the polyvinylidene fluoride copolymer and a step of irradiating the portion with pulses of at least one ultraviolet radiation.
    公开号:FR3013510A1
    申请号:FR1361162
    申请日:2013-11-15
    公开日:2015-05-22
    发明作者:Abdelkader Aliane
    申请人:Commissariat a lEnergie Atomique CEA；Commissariat a lEnergie Atomique et aux Energies Alternatives CEA；
    IPC主号:
    专利说明:

    [0001] TECHNICAL FIELD This invention relates to a method of manufacturing a pyroelectric and / or piezoelectric device comprising a polyvinylidene fluoride (PVDF) film or a copolymer of the polyvinylidene fluoride. PVDF and a pyroelectric and / or piezoelectric device obtained by such a method. DESCRIPTION OF THE PRIOR ART Pyroelectric and / or piezoelectric devices can be used as sensors, for example as pressure sensors, as switches or as energy recovery devices. It is known to make a pyroelectric and / or piezoelectric device using a PVDF polymer film or a PVDF copolymer. The PVDF polymer and the PVDF copolymers are semi-crystalline polymers which, after the polymerization step, have a crystallinity generally of between 50% and 60%. The PVDF polymer or the PVDF copolymer may comprise crystalline phases of three types a, 13 and y. Phase 13 may have pyroelectric and piezoelectric properties while phase a does not.
    [0002] B12809 - DD14732E0 2 After the polymerization step, the crystalline phase obtained is generally in the majority phase a. An additional treatment must then generally be provided to transform at least part of phase a in phase 13. This treatment may comprise: thermal annealing, for example at a temperature of between 110 ° C. and 170 ° C. for a period varying from several minutes to several hours; the mechanical stretching of the polymer; the application to the film of an electric field of high intensity for several hours; and / or the ionization of the air around the PVDF film. It may be desirable to form the PVDF or PVDF copolymer film on a substrate of plastic material, for example polyethylene naphthalate (PEN) or polyethylene terephthalate (PET). It may further be desirable to form the PVDF film or a PVDF copolymer on a substrate on which or in which other electronic components, for example transistors, are also made.
    [0003] A disadvantage of the known processes for obtaining the crystalline phase 13 is that they may not be compatible with the use of a plastic substrate or with the formation of electronic components, in particular because of the high temperatures and / or the constraints applied mechanics.
    [0004] SUMMARY An embodiment aims to overcome the drawbacks of the methods of manufacturing the pyroelectric and / or piezoelectric devices described above. Another embodiment is directed to the manufacture of a pyroelectric and / or piezoelectric device comprising a PVDF film or a PVDF copolymer on a plastic substrate. Another embodiment relates to the manufacture of a pyroelectric and / or piezoelectric device comprising a PVDF film or a PVDF copolymer on a substrate on which B12809 - DD14732E0 3 or which are also formed other electronic components . Another embodiment aims to reduce the time of manufacture of a PVDF pyroelectric and / or piezoelectric film. Another embodiment aims at reducing or even eliminating the step of heating the substrate. Thus, an embodiment provides a method for manufacturing a piezoelectric and / or pyroelectric device comprising a film comprising polyvinylidene fluoride and / or at least one polyvinylidene fluoride copolymer, the process comprising the following steps: minus a portion of a layer of a solution comprising a solvent and a compound comprising polyvinylidene fluoride and / or at least the polyvinylidene fluoride copolymer; and irradiating at least the portion with pulses of at least one ultraviolet radiation. According to one embodiment, the compound comprises a polymer selected from the group consisting of polyvinylidene fluoride, poly (vinylidene trifluoroethylene polyfluoride), poly (vinylidene fluoride-tetrafluoroethylene) and a mixture of at least two of these polymers. According to one embodiment, the compound further comprises ceramic particles. According to one embodiment, the duration of each pulse is between 500 ps and 2 ms. According to one embodiment, the fluence of ultraviolet radiation is between 10 J / cm 2 and 25 J / cm 2. According to one embodiment, the solvent has an evaporation temperature of between 110 ° C and 140 ° C. According to one embodiment, the solution comprises from 80% to 95% by weight of the solvent and from 5% to 20% by weight of the compound.
    [0005] According to one embodiment, the method further comprises the steps of: providing a substrate; depositing on the substrate a coating reflecting the ultraviolet radiation; and forming the film at least partially on the coating. According to one embodiment, the solvent is adapted to at least partially absorb the ultraviolet radiation. One embodiment provides a piezoelectric and / or pyroelectric device comprising a film comprising polyvinylidene fluoride and / or at least one copolymer of polyvinylidene fluoride and having two crystalline phases 13 having different orientations. According to one embodiment, the device comprises a substrate, on which the film is formed, of a polymer having a glass transition temperature of less than or equal to 130 ° C. BRIEF DESCRIPTION OF THE DRAWINGS These and other features and advantages will be set forth in detail in the following description of particular embodiments in a non-limitative manner with reference to the accompanying figures in which: FIGS. partial and schematic sections of the structures obtained at successive steps of an embodiment of a method for manufacturing a PVDF pyroelectric / piezoelectric device or a PVDF copolymer; FIG. 2 represents an X-ray diffraction diagram obtained for a film of a PVDF copolymer made according to a known manufacturing method and a film of a PVDF copolymer produced according to the embodiment described with reference to FIGS. LA to 1D; FIG. 3 represents evolution curves of the voltage obtained at the terminals of a pyroelectric device and / or piezoelectric B12809 - DD14732E0 as a function of the pressure applied for a device comprising a film of a copolymer of PVDF produced according to a method known manufacture and a device comprising a film of a PVDF copolymer made according to the embodiment described in relation to Figures LA to 1D; and FIG. 4 represents an evolution curve of the pyroelectric coefficient as a function of the temperature of a device comprising a film of a PVDF copolymer made according to the embodiment described in relation with FIGS. LA to 1D. DETAILED DESCRIPTION For the sake of clarity, the same elements have been designated with the same references in the various figures and, moreover, as is customary in the representation of the electronic circuits, the various figures are not drawn to scale. In addition, only the elements useful for understanding the present description have been shown and are described. In the rest of the description, unless otherwise indicated, the terms "substantially", "about" and "of the order of" mean "to within 10%". In the remainder of the description, the term "PVDF-based" element means an element comprising at least 70% by weight of the PVDF polymer and / or of at least one copolymer of PVDF. An embodiment of a method for manufacturing a pyroelectric and / or piezoelectric device comprising a PVDF-based film is intended in particular to form the crystalline phase 13 which has the desired piezoelectric and / or pyroelectric properties, by applying short pulses ultraviolet (UV) radiation on a liquid layer comprising a PVDF-based compound. This makes it possible to heat the liquid layer to promote the formation of the crystalline phase 13. This makes it possible to locally heat the liquid layer without heating the substrate on which the PVDF-based film is formed and / or without heating the electronic components adjacent to the film based on PVDF.
    [0006] B12809 - DD14732E0 Figures 1A to 1D illustrate an embodiment of a method of manufacturing a pyroelectric and / or piezoelectric device comprising a PVDF-based film. Figure LA is a partial and schematic sectional view of the structure obtained after forming a first electrode 12 on a substrate 10. The substrate 10 may be of an insulating or semiconductor material. For example, the substrate 10 is made of glass, silicon, or a plastic material. The substrate 10 may be made of a polymer, for example a polyimide, PEN or PET. For example, the thickness of the substrate 10 is between 25 gm and 200 pin. The substrate 10 may be flexible. The first electrode 12 is preferably an ultraviolet radiation reflective material, for example over a wavelength range between 200 nm and 400 nm. It may be a metal layer. For example, the material comprising layer 12 is selected from the group consisting of silver (Ag), aluminum (Al), gold (Au) or a mixture or alloy of two or more of two of these metals. The thickness of the layer 12 may be greater than or equal to 30 μm, preferably between 30 nm and 300 nm. The deposition of the first electrode 12 on the substrate 10 can be achieved by physical vapor deposition or by printing techniques, in particular by screen printing or by inkjet printing, or by spraying. FIG. 1B shows the structure obtained after having deposited a portion of a liquid layer 14, possibly viscous, on the first electrode 12. The liquid layer portion 14 comprises a solvent and a PVDF-based compound dissolved in the solvent. The thickness of the portion 14 is between 100 nm and 4 pin. The PVDF-based compound may comprise the single PVDF polymer, a single PVDF copolymer, a blend of two or more PVDF copolymers or a blend of the PVDF polymer B12809 - DD14732E0 7 and at least one PVDF copolymer . Preferably, the PVDF copolymer is poly (vinylidene trifluoroethylene fluoride) (P (VDF-TrFe)) or poly (vinylidene fluoride-tetrafluoroethylene), in particular P (VDFx-TrFeloo_x), where x is a actual number between 60 and 80. The PVDF-based compound may further comprise fillers. The fillers may correspond to ceramic particles, for example particles of barium titanate (BaPiO 3) or particles of lead zirconate titanate (PZT). The concentration by weight of fillers in the PVDF-based compound can vary from 5% to 25%. Preferably, the solvent is a polar solvent. This advantageously makes it possible to improve the dissolution of the PVDF-based polymer. Preferably, the solvent is adapted to absorb, at least partially, the UV radiation, for example over a wavelength range between 200 nm and 400 nm. According to one embodiment, the evaporation temperature of the solvent is between 110 ° C. and 140 ° C., preferably between 110 ° C. and 130 ° C., more preferably between 120 ° C. and 130 ° C. The solvent may be selected from the group consisting of cyclopentanone, dymethylsulphoxide (DMSO), dymethylformamide (DMF), dimethylacetamide (DMAc) or N-methyl-E-pyrrolidone (NMP). Preferably, the solvent is cyclopentanone. Portion 14 comprises from 1% to 30%, preferably from 1% to 20%, by weight of the PVDF-based compound and from 70% to 99%, preferably from 80% to 99%, by weight of the solvent. . Advantageously, the concentration by weight of the solvent is chosen to adjust the viscosity of the solution obtained to enable the implementation of printing techniques. The method of forming the liquid layer portion 14 may correspond to a so-called additive process, for example by directly printing the portion 14 at the desired locations, for example by ink jet printing, gravure printing, screen printing, flexography, coating by spraying (in B12809 - DD14732E0 8 English spray coating) or deposit drop-casting. The method of forming the liquid layer portion 14 may correspond to a so-called subtractive process, in which the liquid layer is deposited on the entire structure and in which the unused portions are then removed, for example by photolithography or laser ablation. . Depending on the material considered, the deposition on the entire structure may be carried out for example by liquid, sputtering or evaporation. This may include processes such as spin coating, spray coating, heliography, slot-die coating, blade-coating, flexography or screen printing. FIG. 1C illustrates a step of irradiating at least a portion of the portion 14, resulting in the formation of a PVDF-based film 16 having the desired pyroelectric and / or piezoelectric properties. The irradiation with UV rays is represented diagrammatically in FIG. 1C by the arrows 18. The irradiation is carried out by a succession of pulses of UV radiation, or ultraviolet flashes. By UV radiation is meant radiation whose wavelengths are, at least in part, between 200 nm and 400 nm. According to one embodiment, the duration of a UV pulse is between 500 ps and 2 ms. The duration between two successive UV pulses can be between 1 and 5 seconds. The fluence of the radiation (UV) can be between 10 J / cm 2 and 25 J / cm 2. The number of UV pulses depends in particular on the thickness of the portion 14. By way of example, for a thickness of the portion 14 of 100 nia, the number of UV pulses can be of the order of 1 to 2 with a fluence between 10 J / cm 2 and 15 J / cm 2 and for a thickness of the portion 14 of the order of 4 gm, the number of UV pulses can be of the order of 2 to 6 with a fluence between 17 J / cm2 and 21 J / cm2. Advantageously, during the irradiation of the portion 14, the first electrode 12 reflects a portion of the UV radiation having passed through the portion 14. This makes it possible to improve the amount of UV radiation received by the portion 14. The reflection of the UV rays is represented diagrammatically in FIG. 1C by the arrows 20.
    [0007] Advantageously, the solvent of the liquid layer portion 14 absorbs at least part of the UV radiation. This makes it possible to improve the heating of the UV-based compound and to promote the formation of the crystalline phase 13. The evaporation temperature of the solvent is advantageously greater than 110 ° C. in order to avoid a too rapid evaporation of the solvent before the formation crystalline phase 13 which occurs between 120 ° C and 130 ° C. Preferably, the irradiation step causes an evaporation of more than 50% by weight, preferably more than 80% by weight, of the solvent of the liquid layer portion 14. FIG. 1D represents the structure obtained after having deposited a second electrode 22 on the film 16. The electrode 22 is, for example, a metal material selected from the group consisting of silver, copper or a mixture or an alloy of at least two of these materials. Depending on the material considered, the electrode 22 may be deposited by a physical vapor deposition (PVD) or by printing techniques, for example by inkjet printing or screen printing. In this case, an annealing step may then be provided, for example by irradiation of the UV-pulsed ink having a fluence of between 15 J / cm 2 and 25 J / cm 2. A subsequent step of applying an electric field to the structure may be provided. For example, the electric field can vary between 20 and 80 V / gm and can be applied at a temperature between 70 and 90 ° C for 5 to 10 minutes. The film 16 obtained by carrying out the above-described embodiment of the manufacturing method has pyroelectric and piezoelectric properties.
    [0008] B12809 - DD14732E0 Figure 2 shows two diffraction diagrams C1 and C2 respectively of first and second PVDF-based films. The first piezoelectric film associated with the curve C1 was obtained by forming a layer 2 microns thick by screen-printing a solution comprising 20% by weight of the copolymer P (VDF70-TrFe30) and 80% by weight of cyclopentanone. The solution was obtained by mixing 2 g of cyclopentanone and 0.4 g of P powder (VDF70-TrFe30) at a temperature between 40 and 45 ° C for several hours. The layer was heated on a hot plate for 5 minutes at 100 ° C and 3 minutes at 130 ° C. The second piezoelectric film associated with curve C2 was obtained by the embodiment of the manufacturing method described above in connection with FIGS. 1A-1D, in which liquid layer portion 14 had a thickness of 2 gm and was formed by serigraphically depositing a solution comprising 80% by weight of cyclopentanone and 20% by weight of the copolymer P (VDF70-TrFe30). The solution was obtained by mixing 0.4 g of P (VDF70-TrFe30) powder with 2 g of cyclopentanone at a temperature between 40 and 45 ° C for several hours. The layer was irradiated with 2 pulses of UV radiation provided by a UV lamp whose wavelength was between 240 nm of 1000 nm, with more than 75% of the energy between 240 nm and 400 nm. The duration of each pulse was 2 ms. The duration between two successive pulses was 1 second. The fluence of the UV radiation was 21 J / cm 2. The curve C1 comprises a peak P1 for an angle of 201 substantially equal to 20 °. This indicates the presence of a crystalline phase 13 in the first film, characteristic of pyroelectric / piezoelectric properties. Curve C2 also includes a peak P2 for the angle of 201. However, curve C2 further comprises a peak P2 at an angle 202 substantially equal to 32 °. This reflects the presence of another crystalline phase 1 in the second film which has a different orientation from the crystalline phase associated with the angel 201. The UV flash irradiation step allows the formation of minus two crystalline phases 13 in the second film. The inventors have demonstrated an improvement in the piezoelectric and / or pyroelectric activity of a film obtained by the embodiment of the manufacturing method described above in relation to FIGS. 1A-1B with respect to a piezoelectric film and / or pyroelectric obtained by heating. FIG. 3 shows evolution curves C 3 and C 4 of the voltage applied between the piezoelectric sensor terminals comprising respectively third and fourth PVDF-based films. The third piezoelectric film associated with curve C3 was obtained by forming a 2 μm thick layer by screen printing a solution comprising 80% by weight of cyclopentanone and 20% by weight of copolymer P (VDF70-TrFe30). The solution was obtained by mixing 0.4 g of P (VDF70-TrFe30) powder with 2 g of cyclopentanone at a temperature between 40 and 45 ° C for several hours. The layer was heated for 30 minutes at 130 ° C after deposition. The fourth piezoelectric film associated with the curve C4 was obtained by the embodiment of the manufacturing method described above in connection with Figures LA to 1D, in which the liquid layer portion 14 had a thickness of 2 lm and was formed by serigraphically depositing a solution comprising 80% by weight of cyclopentanone and 20% by weight of the copolymer P (VDF70-TrFe30). The solution was obtained by mixing 0.4 g of P powder (VDF70-TrFe30) with 2 g of cyclopentanone at a temperature between 40 and 45 ° C for several hours. The layer was irradiated with 4 pulses of UV radiation provided by a UV lamp whose wavelength was between 240 nm and 1000 nm, with B12809 - DD14732E0 12 more than 75% of the energy between 240 nia and 400 nia. The duration of each pulse was 1.5 ms. The duration between two successive pulses was 1 second. The fluence of UV radiation was 17.5 J / cm 2.
    [0009] Curve C4 is located above curve C3. This means that the piezoelectric activity of the sensor comprising the fourth PVDF-based film is greater than the piezoelectric activity of the sensor comprising the third PVDF-based film.
    [0010] FIG. 4 represents an evolution curve C5 of the pyroelectric coefficient Coeff of a pyroelectric sensor comprising the fourth film based on PVDF. Curve C5 illustrates the pyroelectric activity of the PVDF-based film manufactured according to the embodiment of the manufacturing method described above according to FIGS. LA to 1D. An advantage of the embodiment of the pyroelectric / piezoelectric device manufacturing method is that it has a short duration, in particular less than 1 minute. In addition, it does not include a step of heating the entire substrate on which the PVDF-based film is formed at a temperature above 130 ° C. This allows the use of a plastic substrate. This makes it possible, in addition, to produce other electronic components in and / or on the substrate.
    [0011] An advantage of the embodiment of the method for manufacturing the pyroelectric / piezoelectric device is that the treatment for forming the crystalline phase comprising a thermal annealing, the application of mechanical stresses and / or the application of a magnetic field, may not to be present.
    [0012] Particular embodiments have been described. Various variations and modifications will be apparent to those skilled in the art.
    权利要求:
    Claims (11)
    [0001]
    REVENDICATIONS1. A method of manufacturing a piezoelectric and / or pyroelectric device comprising a film (16) comprising polyvinylidene fluoride and / or at least one polyvinylidene fluoride copolymer, the process comprising the steps of: forming at least one portion (14) a layer of a solution comprising a solvent and a compound comprising polyvinylidene fluoride and / or at least the polyvinylidene fluoride copolymer; and irradiating at least the portion with pulses of at least one ultraviolet radiation.
    [0002]
    The process according to claim 1, wherein the compound comprises a polymer selected from the group consisting of polyvinylidene fluoride, poly (vinylidene trifluoroethylene polyfluoride), polyvinylidene-tetrafluoroethylene polyfluoride and a mixing at least two of these polymers.
    [0003]
    The method of claim 1 or 2, wherein the compound further comprises ceramic particles.
    [0004]
    The method of any one of claims 1 to 3, wherein the duration of each pulse is between 500 ps and 2 ms.
    [0005]
    The method of any of claims 1 to 4, wherein the fluence of ultraviolet radiation is between 10 J / cm 2 and 25 J / cm 2.
    [0006]
    The process according to any of claims 1 to 5, wherein the solvent has an evaporation temperature of between 110 ° C and 140 ° C.
    [0007]
    7. A process according to any one of claims 1 to 6, wherein the solution comprises from 80% to 95% by weight of the solvent and from 5% to 20% by weight of the compound.
    [0008]
    The method of any one of claims 1 to 7, further comprising the steps of: providing a substrate (10); depositing on the substrate a coating (12) reflecting ultraviolet radiation; and forming the film (16) at least partially on the coating.
    [0009]
    9. Process according to any one of claims 1 to 8, wherein the solvent is adapted to at least partially absorb ultraviolet radiation.
    [0010]
    A piezoelectric and / or pyroelectric device comprising a film (16) comprising polyvinylidene fluoride and / or at least one copolymer of polyvinylidene fluoride and having two crystalline phases 13 having different orientations.
    [0011]
    The device of claim 10, comprising a substrate (10), on which the film (16) is formed, of a polymer having a glass transition temperature of less than or equal to 130 ° C.
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    引用文献:
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    WO2005064653A1|2003-12-22|2005-07-14|Koninklijke Philips Electronics N.V.|Method for patterning a ferroelectric polymer layer|
    US20090306264A1|2006-02-01|2009-12-10|Meiten Koh|Highly dielectric film|
    KR20090030825A|2007-09-21|2009-03-25|경희대학교 산학협력단|METHOD FOR PRODUCING POLY FILM WITH HIGH beta-TYPE CRYSTAL STRUCTURE|
    KR20100046641A|2008-10-28|2010-05-07|한국과학기술연구원|Method of forming a pattern array of ferroelectric pvdf thin film by using a polymer binder|FR3044409A1|2015-11-30|2017-06-02|Commissariat Energie Atomique|THERMAL PATTERN SENSOR COMPRISING A HIGH PYROELECTRIC PORTION WITH HIGH THERMAL CONDUCTIVITY|CN106575575B|2014-06-09|2018-12-28|沙特基础全球技术有限公司|The organic ferroelectric material of film is handled using pulsed electromagnetic radiation|FR3019381B1|2014-03-31|2017-08-25|Commissariat Energie Atomique|ELECTROACTIVE ACTUATOR AND METHOD OF MAKING|
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    FR3074576B1|2017-12-04|2020-01-03|Commissariat A L'energie Atomique Et Aux Energies Alternatives|THERMAL PATTERN SENSOR WITH PYROELECTRIC CAPACITY COMPRISING A SOL-GEL MATRIX AND METAL OXIDE PARTICLES|
    FR3074574B1|2017-12-04|2020-01-03|Commissariat A L'energie Atomique Et Aux Energies Alternatives|THERMAL PATTERN SENSOR WITH PYROELECTRIC CAPACITY|
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    法律状态:
    2015-11-25| PLFP| Fee payment|Year of fee payment: 3 |
    2016-11-30| PLFP| Fee payment|Year of fee payment: 4 |
    2017-11-30| PLFP| Fee payment|Year of fee payment: 5 |
    2019-11-29| PLFP| Fee payment|Year of fee payment: 7 |
    2021-08-06| ST| Notification of lapse|Effective date: 20210705 |
    优先权:
    申请号 | 申请日 | 专利标题
    FR1361162A|FR3013510B1|2013-11-15|2013-11-15|METHOD FOR MANUFACTURING A PYROELECTRIC AND / OR PIEZOELECTRIC DEVICE|FR1361162A| FR3013510B1|2013-11-15|2013-11-15|METHOD FOR MANUFACTURING A PYROELECTRIC AND / OR PIEZOELECTRIC DEVICE|
    US15/033,892| US10593857B2|2013-11-15|2014-10-27|Process for manufacturing a pyroelectric and/or piezoelectric drive|
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