• 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:
    Realization of a triboelectric generator element based on a given dielectric polymer material (15), having a rough surface having conical micro-tip shaped structures obtained by means of a thermal treatment of the polymeric material ( Figure 1C).
    公开号:FR3024303A1
    申请号:FR1457138
    申请日:2014-07-24
    公开日:2016-01-29
    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 AND PRIOR ART The present invention relates to the field of tribo-electric generators and their manufacture. BACKGROUND OF THE INVENTION It provides in particular for producing a triboelectric generator having at least one element comprising a layer of rough-surfaced dielectric polymer material, without necessarily having to use a mold to create or modify the roughness of the surface of this layer of dielectric material. The operation of a triboelectric generator is based on a contacting of a first material and a second material of different natures, a first material tending to give up electrons, the second material preferably having a tendency to capture electrons. By contacting materials of different triboelectric properties, a charge transfer between these two materials is created which can be translated as a potential difference or a current. The triboelectric effect can be increased by rubbing the materials against each other.
    [0002] To manufacture a tribo-electric generator, it is known to use a layer of polymer material which is structured to create a high surface roughness and thus increase the friction phenomenon. US 2013/0049531 A1 and "Transparent Triboelectric Nano-generators and Self-Powered Pressure Sensors Based on Micropatterned Plastic Films", Feng-Ru Fan et al., Nano Letters 2012, 12, 3109-3114 disclose a method for producing a triboelectric generator comprising a rough-surface polydimethylsiloxane (PDMS) layer, whose roughness is formed by creating patterns in the form of grooves, or cubes, or even pyramids, using a mold .
    [0003] Such a process requires a filling of the mold with PDMS, and especially a delicate step of removing the structured PDMS from the mold without damaging it. The withdrawal of the PDMS may also have the disadvantage of requiring the use of a surfactant.
    [0004] There is the problem of finding a novel method of making a triboelectric generator having at least one layer of rough polymeric material and which does not require the use of a mold. SUMMARY OF THE INVENTION According to one embodiment, the present invention firstly relates to a method of making an element of a triboelectric effect generator comprising the steps of: a) forming on a support a based on a material based on a given dielectric polymer, b) effecting at least one heat treatment on the given dielectric polymer material so as to crystallize the given dielectric polymer material and generate micro-tip shaped structures, particularly conical, on the surface of the given dielectric polymer material. The given dielectric polymer material may be selected to have a high dielectric constant, preferably such that Er> 30 (where er is the relative permittivity of the dielectric material). The given dielectric polymer material is advantageously a hydrophobic material. The given dielectric polymer material can thus be provided with a fluorinated group, for example a group of polyvinylidene fluoride (PVDF).
    [0005] Advantageously, the given dielectric polymer material may be a terpolymer such as P (VDF-TrFe-CFE) or P (VDF-TrFe-CTFE) or a mixture of P (VDF-TrFe-CFE) and P (VDF). -TrFe-CTFE). Other PVDF-based polymers such as P (VDF-TrFe) copolymers can be used.
    [0006] The polymeric material formed in step a) may be in the form of a polymer matrix having an additive selected to have a higher transition rate than the given dielectric polymer. By "transition" is meant a structural modification under the effect of the variation of an external parameter, here the temperature. The additive may be chosen so as to have a lower temperature of change of its structuring than that of the given polymer and so that, when the crystallization heat treatment is carried out, a structural modification (crystallization) of the polymer matrix causes a constraint of this additive. This mechanical stress brings out structures in the form of microtips, in particular of conical shape. The heat treatment step b) may be a photonic annealing comprising exposing the layer of polymer material to at least one UV radiation light pulse also called UV flash. Such a treatment has the particular advantage of being fast to achieve and allow to modify the dielectric polymer material mainly at the surface. The additive used in step a) can then be advantageously a compound absorbing UV radiation such as Pyrene. Such an additive may make it possible to promote the development of a rough surface on the dielectric polymer material during step b). According to one possible embodiment, the support may be a flexible support based on polymeric material. An embodiment of the present invention provides a method of manufacturing a triboelectric effect generator comprising a first member for contacting a second member to create electrical charges, the method comprising the steps of: - Perform a method as defined above to form the first element - form a layer based on graphene on a second support to achieve the second element.
    [0007] The advantage of Graphene is that it is a rough conductive material that is conducive to generating friction and whose electrical conductivity increases with temperature, this being likely to increase when friction increases. According to another aspect, the invention relates to a triboelectric generator 5 implemented using a method as defined above. The invention thus also relates to a triboelectric generator for creating electrical charges by contacting a first element and a second element, the first element comprising a conductive layer coated with a rough polymeric dielectric material comprising micro-shaped tips. conical. The given dielectric polymer material may be a high dielectric constant dielectric material, in particular such that Er> 30 (Er is the relative permittivity of the dielectric material). A dielectric material with a high dielectric constant makes it possible to generate a larger triboelectric current, particularly in the case where the friction (temperature generation at the interfaces) increases its dielectric constant. The given dielectric polymer material may advantageously be a hydrophobic material. By providing a hydrophobic polymeric material, moisture is reduced at the rough surface of this material coming into contact with another element to generate electrical charges. This avoids reducing the friction at the level of the rough contact surface which allows to have a better production of electrical energy. The given dielectric polymer material may comprise a terpolymer, in particular based on PVDF such as P (VDF-TrFe-CFE) or P (VDF-TrFe-CTFE) or a mixture of P (VDF-TrFe-CFE). and P (VDF-TrFe-CTFE). It is also possible to use a copolymer based on PVDF such as P (VDF-TrFe). The second element may advantageously be coated with graphene. An embodiment of the invention also provides a humidity sensor comprising a triboelectric generator as defined above.
    [0008] BRIEF DESCRIPTION OF THE DRAWINGS The present invention will be better understood on reading the description of exemplary embodiments given, purely by way of indication and in no way limiting, with reference to the appended drawings in which: FIGS. 1A-1C illustrate an example of a method according to one embodiment of the invention for implementing an element of a triboelectric generator, this element comprising a dielectric polymer material on which a rough surface is created in the form of conical microtips by modifying by treatment thermal structure of the dielectric material of the polymer; FIG. 2 illustrates an embodiment of another triboelectric generator element intended to be brought into contact with an element as illustrated for example in FIGS. 1A-1C; FIG. 3 illustrates a rough surface provided with conical micro-tips on a dielectric polymer material as implemented in a triboelectric generator according to the invention; FIG. 4 illustrates an exemplary device according to the invention comprising a triboelectric generator associated with a circuit for recovering and storing electrical energy produced by the generator; FIGS. 5A-5C illustrate an electrical test of a triboelectric generator; FIG. 6 illustrates a variant of a triboelectric generator provided with a layer of graphene intended to be put in contact with a rough dielectric polymer material in order to improve the generation of the electric charges; Identical, similar or equivalent parts of the different figures bear the same numerical references so as to facilitate the passage from one figure to another. The different parts shown in the figures are not necessarily in a uniform scale, to make the figures more readable.
    [0009] DETAILED DESCRIPTION OF PARTICULAR EMBODIMENTS An exemplary method of producing a triboelectric generator element will now be given in conjunction with FIGS. 1A-1C. The starting material of this process may be a support 11 whose composition and thickness are provided so as to make it flexible. The support 11 may be formed of a layer of polymeric material, for example such as ethylene polynaphthalate (PEN) or polyethylene terephthalate (PET), or polyimide (PI), or polyether-ether -Ketone (PEEK), or a cellulose paper substrate and having a thickness which may be for example between 5 iim and 10 200 iim, for example of the order of 25 iim. On the support 11, a conductive layer 12 (FIG. 1A) is first deposited, intended to form a first electrode. The conductive layer may be formed for example by physical vapor deposition (PVD) or by ink jet, or by screen printing, or ultrasonic spray coating ("ultrasonic spray coating" in the English terminology). The conductive layer 12 may for example be based on a metallic material such as silver (Ag), platinum (Pt), aluminum (Al), copper (Cu), gold (Au), titanium (Ti), indium tin oxide (ITO), or nano-son, for example based on silver, and may have a thickness of, for example, between 10 nm and 1 μm. In a particular embodiment, the metal layer 12 is a 30 nm thick gold-based layer. Next, a layer 14 of a dielectric polymer material 15 (FIG. 1B) is formed on the metal layer 12. The layer of dielectric polymer material 15 has a thickness which may be, for example, between 100 nm and 20 μm. The dielectric polymer material 15 is preferably selected to have a high dielectric constant, in particular such as Er> 30, and preferably capable of varying depending on the temperature at which this material is placed. The dielectric polymer material may also be selected to have hydrophobic properties. To meet these criteria, the chosen dielectric polymer material 30 may for example be based on a terpolymer comprising a fluorinated group, in particular based on polyvinylidene fluoride (PVDF). According to particular embodiments, the dielectric polymer material may be P (VDF-TrFe-CFE), or P (VDF-TrFe-CTFE), or a P-based compound (VDF-TrFe-CFE). and P (VDF-TrFe-CTFE). According to another example, the dielectric polymer material may be a PVDF-based copolymer such as for example P (VDF-TrFe). Prior to its deposition, the dielectric polymer material may be prepared in the form of a mixture of a first solution based on a terpolymer such as P (VDF-TrFe-CFE), or P (VDF-TrFe). -CTFE), or mixed P (VDF-TrFe-CFE), or P (VDF-TrFe) and P (VDF-TrFe-CTFE), and a second solution comprising an additive having a transition temperature, in particular of crystallization lower than that of the given polymer. The additive chosen may for example be Pyrene (CH-ho). The first solution can be carried out by introducing a powder based on P (VDF-TrFe-CFE) and / or P (VDF-TrFe-CTFE) which is dissolved in a solvent such as, for example, cyclopentanone. dimethylformamide or dimethylacetamide. The proportion of terpolymer in its solvent may vary by weight for example from 1% to 20%. The second solution can be carried out by introducing solid grains of pyrene which is dissolved in a solvent such as for example acetone so as to have a proportion by weight of pyrene which can be for example between 5% and 40%. The proportion of terpolymer in the mixture conditions in particular the viscosity of the deposition solution, which can be adapted according to the type of deposition technique that it is desired to use. For example, when it is desired to perform a screen printing deposit, it is possible to use a solution having a high viscosity, by providing a large concentration of terpolymer in its solvent. In another example, when it is desired to make a spin coating deposit ("spin coating" in the English terminology), a solution of lower viscosity and therefore having a lower terpolymer concentration is used.
    [0010] The deposition solution can be composed, in the end, of 3% to 40% by weight of the second solution in the first solution. The final mixture is stirred at a temperature which may be, for example, between 30 ° C and 45 ° C. The deposition of the terpolymer solution is then followed by at least one so-called "crystallization" thermal annealing step, in order to modify the structure of the polymer material and increase the roughness of its surface. Thermal annealing or annealing successions at a temperature above the crystallization temperature of the polymer material can be achieved. For example, a first annealing may be carried out at a temperature which may be, for example, between 90 and 100 ° C. and in a duration which may be for example between 5 and 30 min. A particular example of implementation provides for performing the first thermal annealing at a temperature of about 100 ° C for a period of 5 minutes. Then, a second annealing is carried out at a temperature which may be for example between 110 and 130 ° C and in a time for example between 5 and 30 min. This second annealing may make it possible to improve the crystallization of the polymer. A particular example of implementation provides for carrying out the second thermal annealing at a temperature of the order of 115 ° C. for a period of 30 minutes. During the annealing (s), because of the higher crystallization speed of the polymer matrix, the structure of the additive chosen, for example pyrene, is structurally modified on the surface because of the mechanical stresses exerted by the crystallization. dielectric polymer material. The inventors have found that, surprisingly, this stressing resulted in the appearance of microstructures or microtips 17 in the form of a cone of revolution. The heat treatment of the polymeric material thus makes it possible to promote the formation of a large roughness on the layer 12 (FIG. 1C). The appearance of the conical microtips is conditioned in particular by the choice in terms of respective rates of crystallization and the appearance of mechanical stresses on the surface of the terpolymer and of the additive, and the conditions (time, temperature) of thermal annealing. A crystallization rate of the terpolymer or the appropriate copolymer makes it possible to mechanically constrain the additive at the surface and creates microstructures in the form of tips. The size of the micro-tips 17 is in turn conditioned in particular by the proportion of terpolymer material in the deposition solution.
    [0011] The micro-tips 17 obtained can have a base of diameter D1 (measured in a direction parallel to the plane [0; x; y] of the orthogonal reference [0; x; y; z] in FIG. 1C) included for example between 2 μm and 10 μm, of the order of several micrometers and a height H1 (measured in a direction orthogonal to the plane [0; x; y] in Figure 1C), for example between 200 nm and 5 μm.
    [0012] In lieu of thermal annealing, photonic annealing can be performed to crystallize the polymeric material and to expose micro-tips 17 on its surface. Photonic annealing may include a very short exposure, i.e. between several us and several ms, to UV radiation. A UV pulse 15 also called a UV flash with a duration of, for example, between 1 ms and 2 ms, and with a fluence of, for example, between 15 J / cm 2 and 50 J / cm 2 may be used to carry out this photonic annealing. A particular example provides for exposure to UV pulsed radiation with a pulse duration (also known as "pulse") of 2 ms and a fluence of 20 17 J / cm 2 when the layer of polymeric material has a thickness of the order of 2 um. FIG. 3 gives an image obtained by scanning electron microscope of the upper face of a polymer layer formed from a mixture of PVDF and Pyrene after a heat treatment as described above and leading to the formation of microtips 17 conical.
    [0013] In order to be able to generate electrostatic charges, the layer 14 of rough-surfaced and microtip-coated dielectric polymer material 15 is intended to be brought into contact with another element having an electrode. An exemplary embodiment of this other element is given in FIG. 2 and comprises a second support 21 intended to be brought into contact with the layer of dielectric polymer material 15 with a rough surface. The second support 21 is formed from a given material having triboelectric characteristics different from those of the dielectric polymer material 15 resting on the first support 11. The second support 21 may for example be based on a dielectric material 25 which may be polymeric and similar to the material of the first support 11.
    [0014] The dielectric material 25 of the second support 21 can thus be, for example, ethylene polynaphthalate (PEN) or polyethylene terephthalate (PET), or polyimide (PI), or polyether-ether-ketone (PEEK). ), or cellulose paper and have a thickness which may be for example between 5 um and 200 um, for example of the order of 25 um. Thus, the second support 21 may also have a composition and thickness provided so as to make it flexible. On the second support 21, a conductive layer 22, which may be metallic, forms a second electrode. The conductive layer 22 may advantageously be made at the same time as that formed on the first support 11. FIG. 4 illustrates the triboelectric generator previously produced 15 associated with an electric energy recovery circuit. Operation of the triboelectric generator may be effected by exerting pressure on the first support 11 and / or the second support 21, so as to contact the rough surface of the layer 14 of dielectric polymer material 15 having microtips 17 The roughness of the dielectric polymer material 15 by means of the conically shaped micro-tips makes it possible to obtain a good coefficient of friction with the dielectric material 25. At the moment of the friction between Since the materials 15 and 25 have different triboelectric properties, and in particular different abilities to give up or accept electrons, a local heating due to friction varies the dielectric constant and therefore the electrical capacitance of the system and consequently the electrical signal generated. by triboelectric effect by the generator. The electrical energy recovery circuit is connected to the conductive layers 12, 22 charge collectors and may include a rectifier means 31 for rectifying an electrical signal produced by the generator, as well as a means 32 for storing electrical charges, by example in the form of a capacity output of the rectifier means 31 31 for storing the electrical energy produced by the generator. The rectifier 31 is for example formed of a bridge of 4 diodes. FIGS. 5A-5C illustrate a previously described test of the triboelectric generator in which the polymeric dielectric layer 15 is contacted with the dielectric material 25 of the carrier 21 by applying a finger to the first carrier 11 (FIG. 5A). The contacting is such that the contact area between the materials 15 and 25 may for example be of the order of 2.5 cm * 2.5 cm. The pressure exerted on the first support 11 is then released and an electric signal (FIG. 5B) generated by the triboelectric effect at the output of the generator is displayed, for example using an oscilloscope having an input impedance, for example of the order of 1 Mn. FIG. 5C gives an example of an electrical signal generated across the capacitor 32 at the output of the rectifier bridge 31. According to an alternative embodiment of the triboelectric generator, the porous dielectric material 15 comprising conical micro-structures 17, can be contacted directly with an electrode to generate electrostatic charges. FIG. 6 illustrates a particular exemplary embodiment of such an alternative in which the rough dielectric porous material is intended to be contacted with a conductive electrode layer formed of a rough conductive material 42. This material rough conductor 42 is a material whose electrical resistivity decreases when the temperature increases such as for example graphene. When the generator is operated so as to friction the graphene-based rough conductive layer 42 and the rough dielectric porous material having tribo-electric properties different from those of graphene, the electrical conductivity of the graphene is increased. which makes it possible to increase the electric signal generated by tribo-electric effect. A particular application of a triboelectric generator according to one or the other of the examples previously described concerns the measurement of humidity. It is thus possible to integrate the triboelectric generator into a humidity sensor.
    [0015] The moisture within the sensor is capable of varying the friction between the layer 14 of rough dielectric material with conical micro-tips and another layer having different triboelectric properties. Thus, depending on the humidity of the medium in which the sensor is located, it is possible to obtain at the output of the generator, for the same actuating force making it possible to bring its elements into contact, different signal levels at the output of the generator. tribo-electric effect.
    权利要求:
    Claims (14)
    [0001]
    REVENDICATIONS1. A method of producing a triboelectric generator element comprising a rough dielectric polymer material for generating electric charges to be contacted with another material having triboelectric properties different from those of the dielectric polymer material, the method comprising steps of: a) forming on a support (11) a layer (14) based on a material formed of a given dielectric polymer (15), b) performing at least heat treatment so as to crystallize the material given dielectric polymer and forming micro-tip shaped structures at the surface of the given dielectric polymer material.
    [0002]
    The method of claim 1, wherein the given dielectric polymer material comprises a PVDF-based terpolymer or copolymer.
    [0003]
    3. The method of claim 1 or 2, wherein the given dielectric polymer material is hydrophobic.
    [0004]
    4. Method according to claim 2 or 3, wherein the given dielectric polymer material is based on polyvinylidene fluoride (PVDF), in particular based on P (VDF-TrFe-CFE) and / or P (VDF). -TrFe-CTFE) or P (VDF-TrFe).
    [0005]
    5. Method according to one of claims 1 to 4, wherein the polymer material formed in step a) is mixed with an additive so that the crystallization of the dielectric polymer material leads to the exercise of mechanical stresses on the surface. additive and promotes the appearance of structures in the form of micro-tips on the surface. 3024303 14
    [0006]
    6. Method according to one of claims 5, wherein the additive is a compound absorbing UV radiation such as Pyrene.
    [0007]
    7. Method according to one of claims 1 to 6, wherein the step 5 b) heat treatment comprises photonic annealing by exposing the layer of polymeric material to at least one light pulse of UV radiation.
    [0008]
    8. Method according to one of claims 1 to 7 wherein the support is a flexible support based on polymeric material. 10
    [0009]
    9. A method of manufacturing a triboelectric effect generator comprising a first element intended to be brought into contact with a second element to create electric charges, the method comprising the steps of: - carrying out method according to one of claims 1 to 7 to form the first element; - to form a graphene-based layer on a second support (21) to make the second element.
    [0010]
    10. Triboelectric generator comprising a first element and a second element, the generator being able to create electrical charges by tribo-electric effect by contacting the first element and the second element, the first element comprising a conductive layer coated with a rough polymeric dielectric material having conical micro-tips. 25
    [0011]
    The triboelectric generator of claim 10, wherein the given dielectric polymer material has a relative permittivity Er> 30.
    [0012]
    The triboelectric generator of claim 10 or 11, wherein the given dielectric polymer material is hydrophobic. 3024303 15
    [0013]
    13. Triboelectric generator according to one of claims 11 or 12, wherein the given dielectric polymer material is based on a terpolymer such as P (VDF-TrFe-CFE) and / or P (VDF-TrFe-CTFE). ), or a copolymer such as P (VDF-TrFe).
    [0014]
    14. Moisture sensor comprising a triboelectric generator according to one of claims 10 to 13.
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    优先权:
    申请号 | 申请日 | 专利标题
    FR1457138A|FR3024303B1|2014-07-24|2014-07-24|IMPROVED METHOD FOR MAKING A TRIBOELECTRIC GENERATOR WITH ROUGH DIELECTRIC POLYMER|FR1457138A| FR3024303B1|2014-07-24|2014-07-24|IMPROVED METHOD FOR MAKING A TRIBOELECTRIC GENERATOR WITH ROUGH DIELECTRIC POLYMER|
    US14/803,429| US10498259B2|2014-07-24|2015-07-20|Method of producing a triboelectric generator with rough dielectric polymer|
    EP15177468.4A| EP2978123B1|2014-07-24|2015-07-20|Method for manufacturing a triboelectric generator with rough dielectric polymer|
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