EP3769302A1 - Porous acoustic phase mask - Google Patents
Porous acoustic phase maskInfo
- Publication number
- EP3769302A1 EP3769302A1 EP19712210.4A EP19712210A EP3769302A1 EP 3769302 A1 EP3769302 A1 EP 3769302A1 EP 19712210 A EP19712210 A EP 19712210A EP 3769302 A1 EP3769302 A1 EP 3769302A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- phase
- acoustic
- phase mask
- porosity
- mask
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 239000011148 porous material Substances 0.000 claims abstract description 91
- 239000011159 matrix material Substances 0.000 claims abstract description 26
- 239000011343 solid material Substances 0.000 claims abstract description 21
- 239000012071 phase Substances 0.000 claims description 164
- 239000000839 emulsion Substances 0.000 claims description 48
- 238000001035 drying Methods 0.000 claims description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 239000007791 liquid phase Substances 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 23
- 239000007789 gas Substances 0.000 claims description 22
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 18
- 239000000178 monomer Substances 0.000 claims description 18
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- 238000004132 cross linking Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 9
- 239000004094 surface-active agent Substances 0.000 claims description 8
- 238000000354 decomposition reaction Methods 0.000 claims description 6
- 230000005855 radiation Effects 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 239000007792 gaseous phase Substances 0.000 claims description 3
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 101100269850 Caenorhabditis elegans mask-1 gene Proteins 0.000 description 31
- 239000000463 material Substances 0.000 description 15
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 9
- 239000000203 mixture Substances 0.000 description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- 239000008346 aqueous phase Substances 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- 241001247482 Amsonia Species 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
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- 239000011780 sodium chloride Substances 0.000 description 3
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- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 2
- LEACJMVNYZDSKR-UHFFFAOYSA-N 2-octyldodecan-1-ol Chemical compound CCCCCCCCCCC(CO)CCCCCCCC LEACJMVNYZDSKR-UHFFFAOYSA-N 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 2
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- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 description 1
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 description 1
- 201000005488 Capillary Leak Syndrome Diseases 0.000 description 1
- 208000030984 MIRAGE syndrome Diseases 0.000 description 1
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 description 1
- 208000031932 Systemic capillary leak syndrome Diseases 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
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- 230000004048 modification Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 238000005373 pervaporation Methods 0.000 description 1
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- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 239000004626 polylactic acid Substances 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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- TVLSRXXIMLFWEO-UHFFFAOYSA-N prochloraz Chemical compound C1=CN=CN1C(=O)N(CCC)CCOC1=C(Cl)C=C(Cl)C=C1Cl TVLSRXXIMLFWEO-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- G—PHYSICS
- G10—MUSICAL INSTRUMENTS; ACOUSTICS
- G10K—SOUND-PRODUCING DEVICES; METHODS OR DEVICES FOR PROTECTING AGAINST, OR FOR DAMPING, NOISE OR OTHER ACOUSTIC WAVES IN GENERAL; ACOUSTICS NOT OTHERWISE PROVIDED FOR
- G10K11/00—Methods or devices for transmitting, conducting or directing sound in general; Methods or devices for protecting against, or for damping, noise or other acoustic waves in general
- G10K11/16—Methods or devices for protecting against, or for damping, noise or other acoustic waves in general
- G10K11/162—Selection of materials
- G10K11/165—Particles in a matrix
-
- G—PHYSICS
- G10—MUSICAL INSTRUMENTS; ACOUSTICS
- G10K—SOUND-PRODUCING DEVICES; METHODS OR DEVICES FOR PROTECTING AGAINST, OR FOR DAMPING, NOISE OR OTHER ACOUSTIC WAVES IN GENERAL; ACOUSTICS NOT OTHERWISE PROVIDED FOR
- G10K11/00—Methods or devices for transmitting, conducting or directing sound in general; Methods or devices for protecting against, or for damping, noise or other acoustic waves in general
- G10K11/18—Methods or devices for transmitting, conducting or directing sound
- G10K11/26—Sound-focusing or directing, e.g. scanning
- G10K11/30—Sound-focusing or directing, e.g. scanning using refraction, e.g. acoustic lenses
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0014—Use of organic additives
- C08J9/0023—Use of organic additives containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/40—Impregnation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/02—Foams characterised by the foaming process characterised by mechanical pre- or post-treatments
- C08J2201/032—Impregnation of a formed object with a gas
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/02—Foams characterised by the foaming process characterised by mechanical pre- or post-treatments
- C08J2201/036—Use of an organic, non-polymeric compound to impregnate, bind or coat a foam, e.g. fatty acid ester
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/08—Supercritical fluid
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/20—Ternary blends of expanding agents
- C08J2203/202—Ternary blends of expanding agents of physical blowing agents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2205/00—Foams characterised by their properties
- C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
- C08J2205/026—Aerogel, i.e. a supercritically dried gel
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2205/00—Foams characterised by their properties
- C08J2205/04—Foams characterised by their properties characterised by the foam pores
- C08J2205/048—Bimodal pore distribution, e.g. micropores and nanopores coexisting in the same foam
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2333/08—Homopolymers or copolymers of acrylic acid esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
Definitions
- the invention relates to an acoustic phase mask for the spatial manipulation of acoustic wave fronts, for example an acoustic lens for focusing an acoustic wave.
- the spatial manipulation of acoustic wave fronts, and particularly the focusing of acoustic waves, is typically performed using metamaterial devices, especially in a frequency range corresponding to the audible and / or ultrasonic frequencies.
- Martin et al. discloses a device comprising an anisotropic array of aluminum hollow cylinders arranged to form an acoustic index gradient n in the device. An incident sound acoustic wave, passing through the array of cylinders, is focused in predefined regions of space. The manufacture of such a device requires a precise and expensive mechanical assembly, limiting its industrial application.
- An object of the invention is to provide an acoustic phase mask that is easier to implement or to manufacture than the devices of the prior art.
- phase mask having a variation of the acoustic index n, characterized in that the phase mask comprises a body comprising:
- pores formed in the matrix the pores being predominantly filled with gas, the deformable solid material extending between the pores,
- the body having a porosity of less than or equal to 50%, and a controlled porosity gradient leading to a variation of the acoustic index n spatially in the body.
- the invention may be advantageously completed by the following characteristics, taken individually or in any of their technically possible combinations:
- the phase mask is an acoustic lens, the porosity gradient being such that the lens is able to focus an incident plane acoustic wave transmitted by the phase mask into at least one point of the space,
- the phase mask has two opposite planar faces extending parallel to a main plane and having at least one porosity gradient f oriented in a direction parallel to the main plane,
- the porosity is distributed in the body so as to correspond to an index n evolving linearly in the direction, in at least part of the phase mask,
- the porosity is distributed in the body so as to correspond to an index n evolving hyperbolic manner in the direction, in at least a part of the phase mask,
- the phase mask comprises a juxtaposition of layers comprising a matrix and pores, each layer having a constant porosity, the porosity of a layer being different from the porosity of a directly adjacent layer, the phase mask comprises a support having cavities, each cell containing a matrix, at least two matrices having different porosities,
- the two opposite planar faces are separated by a thickness d, the thickness d being between 100 ⁇ m and 10 mm. Indeed, this range of thicknesses d is suitable for the manipulation of acoustic waves having a wavelength of between 100 kHz and 10 MHz.
- Another aspect of the invention relates to a method for handling acoustic wave fronts, comprising a step of installing an acoustic phase mask previously described in the propagation space of an incident plane acoustic wave having a length wave l.
- the phase mask may advantageously have a thickness d according to a direction of propagation of the incident acoustic wave, the thickness d being strictly less than the wavelength ⁇ .
- Another aspect of the invention relates to a method of manufacturing a phase mask described above, the method comprising steps of:
- each emulsion having on the one hand a first liquid phase and, on the other hand, a second phase comprising monomers and at least one type of surfactant, so as to form drops of the first liquid phase in the second phase, at least two emulsions having respective fractions in first phase different,
- the invention may be advantageously completed by the following characteristics, taken individually or in any of their technically possible combinations:
- the drying step is a supercritical drying step of the first liquid phase
- the first liquid phase comprises, during the step of successively supercritical drying of water, a liquid chosen from ethanol and acetone, and carbon dioxide,
- the first liquid phase comprises a liquid compound adapted to decompose spontaneously at room temperature into a gas and a liquid, and in which, during the drying step, the decomposition of the liquid compound is expected so as to form a phase gas in the pores,
- the compound is hydrogen peroxide
- the crosslinking of the monomers is carried out by exposing the emulsions to ultraviolet radiation.
- FIG. 1 illustrates a phase mask according to one embodiment of the invention
- FIGS. 2a, 2b and 2c illustrate a method of manufacturing a porous material
- FIG. 3 illustrates a supercritical drying step
- FIGS. 4a, 4b and 4c are photomicrographs of porous materials
- FIG. 5 is a diagram illustrating the evolution of the porosity of a porous material as a function of the volume fraction in first dispersed phase after drying for different drying methods
- FIG. 6 illustrates the manipulation of a plane wave incident by a phase mask according to one embodiment of the invention
- FIG. 7 illustrates the evolution of the longitudinal velocity of an acoustic wave in a porous elastomeric material according to one embodiment of the invention as a function of the porosity of the porous elastomeric material
- FIGS. 8a, 8b, 8c, 8d, 8e and 8f illustrate a method of manufacturing a phase mask according to one embodiment of the invention
- FIGS. 9a, 9b, 9c and 9d illustrate a method of manufacturing a phase mask according to one embodiment of the invention
- FIGS. 10a and 10b illustrate the deflection of a plane wave incident at a predetermined angle, as well as the phase mask adapted for this deflection
- FIGS. 11a and 11b illustrate the focusing of an incident plane wave towards a predetermined focal point, as well as the phase mask adapted for this focusing
- FIGS. 12a, 12b and 12c illustrate experimental measurements enabling the deflection and focusing of acoustic waves produced by phase masks according to embodiments of the invention.
- the porosity of a porous material will be defined as the ratio between the pore volume of the porous material and the total volume of the porous material (i.e. sum of the pore volume of the porous material and the volume of solid material extending between the pores).
- Manipulation of an acoustic wave refers to any deliberate and controlled modification of said front (local phase, amplitude and / or polarization), for example the deflection or focusing of an acoustic wave. .
- phase mask denotes any device that locally modifies the phase of an incident wave passing through it.
- the phase mask is a planar device.
- emulsion denotes a mixture of two immiscible liquid substances, one of which is dispersed in the form of drops in the other in a homogeneous manner.
- FIG. 1 illustrates a section of an acoustic phase 1 mask.
- the phase mask 1 comprises a body 2.
- the body 2 allows a simplified use of the phase mask 1, with regard to other known devices, such as obstacle networks or transducer networks.
- the body 2 comprises at least one matrix 3, formed in a deformable solid material, and pores 4 formed in the matrix 3.
- the majority of the pores 4 are filled with gas, which allows the body 2 to be compressible (compressibility is between 10 9 Pa 1 for the body 2 non-porous to 10 6 Pa 1 for the body 2 having 40% pores filled with gas).
- the deformable solid material extends between the pores 4. This material has a shear modulus preferably less than 10 MPa.
- the pores 4 give the body 2 a local porosity.
- the body 2 has a porosity of less than 50%, that is to say that the local porosity at any point of the body 2 is less than 50%. In other words, the maximum porosity of the body 2 is less than 50%.
- the body 2 has a porosity gradient f. This porosity gradient in the body 2 is controlled and causes a spatial variation of the acoustic index n in the body 2.
- the variation of the acoustic index n, or the acoustic index gradient n makes it possible to cause a modulation incident wavefront during its passage through the phase mask 1, allowing for example to focus an incident wave, particularly an incident plane wave.
- FIG. 1 illustrates a phase-1 mask in section: the phase mask 1 has two opposite planar faces extending parallel to a main plane 7 and the body 2 of the phase-1 mask has a porosity gradient oriented in a parallel direction 7.
- the main plane 7 is parallel to the plane defined by the x and y axes, and the gradient is oriented along the x axis.
- the body 2 has a porosity f decreasing along the x axis.
- the body 2 is at least partly made of porous materials, that is to say a material comprising the matrix 3 of deformable solid material, and the pores 4, the deformable solid material of the matrix 3 extending between the pores 4
- the porous material is produced by polymerization of an aqueous emulsion in a polymerizable solvent, for example thermally or by irradiation under UV and then by drying.
- the deformable solid material comprises elastomeric polymers. These polymers have transition temperatures vitreous less than room temperature.
- the polymers of the deformable solid material have a glass transition temperature below -50 ° C., preferably below -80 ° C., and preferably below -100 ° C.
- the body 2 may have a higher compressibility than the known porous materials.
- a reference material i.e. water in the invention
- cre / 1500 ms 1
- the acoustic index n depends on the porosity.
- a porosity gradient of the porous material thus leads to an acoustic index gradient n in the body 2 of the phase 1 mask.
- the porosity of the porous material can be adjusted to have propagation speeds of typically between 10 ms -1 and 1000 ms 1 .
- the known devices do not make it possible to achieve variations in propagation speeds with such a high amplitude.
- the manufacture of a phase 1 mask, and in particular the porous material of one or more matrices 3 of the phase 1 mask comprises the steps of: a) forming a plurality of emulsions 12, each emulsion 12 having, on the one hand, a first liquid phase 13 and, on the other hand, a second phase 14 comprising monomers and at least one type of surfactant, in order to form drops of the first liquid phase in the second phase 14.
- At least two emulsions 12 have different first-phase respective fractions.
- the step of forming an emulsion is illustrated in FIG. 2a.
- the crosslinking step is illustrated in FIG. 2b.
- step c) drying the porous material obtained in step b) to remove the first liquid phase so as to fill most of the pores 4 gas.
- the drying step is illustrated by Fig. 2c.
- each inverse emulsion 12 is made between, on the one hand, a second phase 14 comprising monomers and a suitable surfactant, and on the other hand a first aqueous phase.
- a second phase 14 comprising monomers and a suitable surfactant
- a first aqueous phase comprising monomers and a suitable surfactant
- the emulsion 12 can be achieved using a shearing device (eg Rayneri, Ultraturrax, or any mechanical device allowing sufficient shear of the two phases).
- the emulsion can also be formed by exposing the first phase 13 and the second phase 14 to ultrasonic waves.
- the mother emulsion is emulsion 12 thus obtained.
- the volume fraction of the mother emulsion 12 in the first phase 13 can be between 0% and 90%.
- the choice of the surfactant is adapted to the monomers chosen in the second phase 14. In general, the surfactant has an HLB number of less than or equal to about 8.
- an inverse emulsion 12 that is, to say including drops of first phase
- the diameter of the first phase drops 13 formed in the second phase 14 is typically between 0.1 and 100 ⁇ m.
- the emulsions 12 are deposited in one or more containers. At least two emulsions 12 have different first-phase respective fractions. The fraction in first phase 13 can also vary in a controlled manner during the deposition of an emulsion 12 in a container, forming a plurality of emulsions 12 in a continuous manner.
- the container may be for example a mold or a cell. A wall of the container may be formed by an emulsion 12 already crosslinked.
- the monomers of the second phase 14 of the emulsion 12 are crosslinked so as to form a deformable solid material. Crosslinking of the monomers may be preferably carried out by exposure of the monomers to ultraviolet radiation or heating.
- one or more matrices 3 are obtained in deformable solid material. Pores 4 are formed by the matrix or matrices 3. These pores 4 are filled with first phase 1 3.
- step c) the matrix or matrices 3 are dried. This step makes it possible to replace, at least in majority and preferably completely, the first liquid phase 13 contained in the pores 14 by gas. Typically, the drying of the first phase 13 is carried out by pervaporation of the first liquid phase 13 through the polymer matrix 3.
- a drying front propagates in the matrix 3, and more particularly at the interface between the matrix 3 and the pores 4.
- This indicative value is greater than the typical shear moduli of the deformable solid material, elastomeric polymers.
- pore collapse is observed during the implementation of known drying methods, and the porosity of a porous material is thus limited because no gas replaces the disappearance of the first phase 1 3 in the pores 4.
- the drying step is a supercritical drying step of the porous material for removing the first liquid phase.
- the supercritical drying method is known for drying porous brittle materials, such as aerogels. She is by example described by Marre et al. (Marre, S., made Aymonier, C. (2016), Preparation of Nanomaterials in Flow and Supercritical Conditions from Coordination Complexes in Organometallic Flow Chemistry (pp. 177-211), Springer, Cham.).
- a liquid phase contained by the pores 4 is transformed into a gaseous phase, without phase transition, by imposing temperature and pressure conditions making it possible to bypass the critical point of the compound (s) contained in the pores.
- the absence of passage through a phase transition line makes it possible to avoid a drying front between a liquid phase and a gaseous phase.
- the drying pressure is decreased or equal to zero, and it is possible to avoid crushing the porous material on itself during drying.
- the drying fluid used for supercritical drying can be C0 2 .
- FIG. 3 illustrates the supercritical drying of the porous material using CO2.
- the pores 4 contain a first aqueous phase.
- the first phase 13 is first exchanged with liquid ethanol.
- the liquid contained in the pores 4 is miscible with the CO2.
- the exchange of the first phase 1 3 with a liquid phase of ethanol is carried out by immersing the porous material in an aqueous solution bath which is progressively enriched in ethanol by a system of pumps at ambient temperature and pressure. The exchange occurs gradually, on a time scale adapted to avoid imposing excessive mechanical stresses on the solid deformable material.
- the ethanol is then extracted with CO2.
- the extraction is carried out by placing the porous material bathed in pure ethanol in a high pressure reactor, in which the pressure and temperature conditions can be adjusted by means of injection pumps and a pressure regulator. output.
- the temperature of the reactor is first adjusted beyond the theoretical critical temperature of the CO 2 / ethanol mixture (ie between 45 and 50 ° C. for a 90/10 molar composition) while the reactor is slowly pressurized with CO2. up to a value greater than the critical pressure of the CO 2 / ethanol mixture (ie 1 10 bar).
- the C0 2 is then pumped continuously through the porous material at a constant flow rate (11 g / min), while the operating conditions are kept constant (the pressure is controlled by means of an outlet pressure controller).
- C0 2 mixes with ethanol and forms a supercritical monophasic mixture.
- the ethanol contained in the pores 4 is gradually replaced by a C 2 / ethanol supercritical mixture which progressively enriches with CO2.
- the fluid ethanol / CO 2 mixture is extracted from the reactor in order to maintain a constant internal volume of fluid.
- the pressure of the system is slowly reduced to 1 bar, for example in one hour, so as to bring the CO2 gas phase without ironing the liquid state.
- This pressure variation corresponds to the trajectory shown in dotted lines starting from point B and going to point I in FIG.
- the first liquid phase comprises a liquid compound adapted to decompose spontaneously at ambient temperature into a gas and a liquid.
- the kinetics of decomposition of the liquid into gas and liquid product can be fixed by the proportion of liquid capable of decomposing in the dispersed phase. This kinetics can be adjusted so that the characteristic gas bubble onset time is typically slower (i.e. typically greater than 30 minutes) than the time required for emulsification.
- the decomposition of the liquid compound is expected so as to form a gas phase in the pores 4.
- the compound 1 may be hydrogen peroxide H2O2. Hydrogen peroxide decomposes at constant ambient temperature and pressure into water (liquid) and gaseous oxygen.
- the proportion of H 2 O 2 in the first liquid phase may preferably be 1/3 in total mass of the first phase 13.
- the characteristic time of appearance of the gas bubbles is of the order of 30 minutes.
- This kinetics can be slowed down or accelerated by varying this proportion or by adding a controlled concentration catalyst in the dispersed phase (for example iodide ions I which are known to catalyze the reaction of decomposition of H2O2 into oxygen and water).
- a controlled concentration catalyst in the dispersed phase for example iodide ions I which are known to catalyze the reaction of decomposition of H2O2 into oxygen and water.
- This method does not require external control of the pressure and / or temperature imposed on the porous material.
- the use of the compound makes it possible to dry the porous material by using a simpler and less expensive material than during a supercritical drying.
- the drying by introduction of the compound is for example carried out by placing the porous material in an oven, in which the temperature is controlled at 40 ° C. under ambient atmosphere.
- Figures 4a, 4b and 4c are photomicrographs obtained by scanning electron microscopy, illustrating porous materials of the body 2, having different porosities.
- the porosity f of the porous material of the body 2 is substantially equal to 5%.
- the porosity f of the porous material of the body 2 is substantially equal to 10%.
- the porosity f of the porous material of the body 2 is substantially equal to 15%.
- FIG. 5 illustrates the evolution of the porosity of a porous material after a drying step carried out according to a known method (illustrated by curve (a)), a supercritical drying step (illustrated by curve (b)) and by a drying step by introducing a compound into the first phase 13 (illustrated by the curve (c)).
- the drying methods illustrated by curves (b) and (c) make it possible to obtain a porous material having a porosity f substantially equal to the volume fraction of the first phase 13 in the emulsion 12.
- the collapse of the matrix 3 on itself prevents an increase of the porosity above a threshold value (substantially 10%) and thus limits a possible acoustic index gradient n of the body 2.
- the second phase 14 comprises silicone oil Silcolease UV poly 200 from Bluestar Silicones, 4% by weight of catalyst Silcolease UV cata 21 1 from Bluestar Silicones, 0.4% by weight of surfactant (2-octyl-1-dodecanol) and 200 ppm of Rahn Genocure ITX.
- the first phase 13 comprises 1.5% by weight of sodium chloride.
- the amount of aqueous phase incorporated in the organic phase is dependent on the desired porosity for the porous material.
- the formation of an emulsion is carried out in a mortar by adding the first phase 13 dropwise during shear, and then it is refined, either using blade tools (Rayneri or Ultraturrax type), either by ultrasound.
- the crosslinking step is carried out by exposing the emulsion to ultraviolet radiation using the Dymax BlueWave 200 lamp.
- the porous material is then dried by supercritical drying or by introducing a compound as described above.
- the second phase 14 comprises 64% by weight of ethylhexyl acrylate, 5.5% by weight of styrene, 10.5% by weight of divinylbenzene and 20% by weight of SPAN 80 surfactant.
- sodium chloride 25.10 3 mol / L and potassium peroxodisulfate 5.10 3 mol / L.
- the amount of first phase 13 incorporated into the organic phase is dependent on the desired porosity for the final material.
- the formation of an emulsion is carried out using a Rayneri type blade tool by adding the first phase 13 dropwise during shearing.
- the crosslinking of the monomers is carried out by heating at a temperature of 60 ° C.
- the porous material is then dried by supercritical drying or by introduction of a compound, as described above.
- a deformable silicone-based solid material (denoted SiVi / SiH) can be obtained by thermal polymerization of the PDMS via a hydrosilylation reaction.
- the second phase 14 comprises 8.8 g of PDMS-vinyl (BLUESIL FLD 621 V1500), 1.8 g of PDMS-silane (BLUESIL FLD 626V30H2.5) and 0.352 g of platinum catalyst (SCLS CATA1 1091 M), (BlueStar Silicones Company).
- SCLS CATA1 1091 M platinum catalyst
- 4.4 mg of polymerization retarder (1-ethynyl-1-cyclohexanol, ECH of Sigma Aldrich) are added.
- 2-octyl-1-dodecanol or Silube J208-812 can be used.
- the emulsions 12 are prepared by introducing a first aqueous phase comprising 1.5% by weight of NaCl with stirring. The emulsion is then poured into a Teflon mold and then heated at 60 ° C for 24 hours. The porous material is then dried by supercritical drying or by introducing a compound as described above.
- a porosity gradient leading to a spatial variation of the acoustic index n in the body 2 it is possible to locally control the celerity of the acoustic waves and thus to bend the acoustic rays by mirage effect (version 3D of the gradient medium) or to control delays / phase advances at wave fronts (2D version of these media, for example a phase 1 mask).
- mirage effect version 3D of the gradient medium
- delays / phase advances at wave fronts 2D version of these media, for example a phase 1 mask.
- the term "manipulation" of the acoustic wavefront is understood to mean at least one of the effects previously described on a plane incident acoustic wave.
- the phase mask 1 may have a subwavelength thickness.
- the phase mask 1 has two opposite planar faces extending parallel to the main plane 7 and has at least one porosity gradient f oriented in the direction 8 parallel to the plane principal 7.
- the thickness d denotes the distance between the two opposite planar faces.
- the manipulation of an incident plane acoustic wave front plane 6, of length l can be implemented with a phase mask 1 of a thickness d strictly less than the wavelength 1.
- the incident wavelengths 6 are between 100 kHz and 10 MHz, in particular for water as a surrounding medium.
- the thickness d of the phase mask is preferably between 100 ⁇ m and 10 mm.
- FIG. 6 illustrates an incident plane acoustic wave 6 presenting a simple physical wavefront (uniform / flat for example) at the input of the phase 1 mask.
- the transmitted wave 19 or target wave 19 has a wavefront different from that of the incident plane wave 6 at the output of the phase mask 1.
- the output wavefront results in a "target" volume acoustic field (a converging field, for example, for focusing).
- FIG. 6 also illustrates a method using a phase 1 mask for generating a sound pressure target field p c (at non-planar phase fronts) from an incident plane wave 6 or an excitation plane front ( by an ultrasonic transmitter for example).
- the target pressure field may, for example, be a harmonic field of pulsation w.
- the target pressure can be written is the pressure amplitude, O c the target phase, and t the time.
- U is possible to consider that the phase mask 1 presents an acoustic index n variable in the xy plane and constant in its thickness d, supposed small compared to 1, that is to say to consider that n depends on x and y.
- the phase mask locally shifts the field m (x, y) k Q d
- the spatial distribution of the acoustic index n of the phase mask 1 must verify the formula: to be adapted to generate the target field P c .
- the distribution of the porosity in the phase mask 1 is thus chosen so as to produce a phase 1 mask having an acoustic index n satisfying the formula (2).
- FIG. 7 illustrates the evolution of the celerity of an acoustic wave in the phase 1 mask with the porosity of the body 2.
- the measured celerities correspond to an acoustic index n of between approximately 1.5 and 40.
- the phase mask 1 is, in general, adapted to have an acoustic index between 1, 5 and 40.
- the body 2 of the phase mask 1 can be manufactured by stacking layers 9, each layer 9 comprising a matrix 3 and pores 4 and having a constant porosity f , the porosity of a layer 9 being different from the porosity of a layer 9 directly adjacent.
- a first emulsion 12 is deposited in a mold 19 comprising a support of polytetrafluoroethylene (PTFE) and two transparent side walls.
- PTFE polytetrafluoroethylene
- the monomers of emulsion 12 are crosslinked by exposing emulsion 12 to UV radiation. This exposure is possible thanks to the transparent walls 20. Thermal crosslinking of the emulsion 12 is also possible.
- the thickness d of the mold (distance between the two walls 20) can be between 0.5 mm and 5 mm when the crosslinking is carried out by UV. The thickness may be greater when the crosslinking is carried out by heating.
- a first phase volume fraction emulsion 12 different from that of the emulsion 12 described in FIG. 8a, for example greater, is deposited in the mold 19 on the crosslinked layer 9 described in FIG. 8b.
- the monomers of the emulsion 12 described in FIG. 8c are crosslinked so as to form two juxtaposed layers 9.
- the different layers 9 can be dried before each deposit of a new emulsion.
- the various layers 9 can be extracted from the mold 19.
- the different juxtaposed layers 9 thus form the body 2 of a phase 1 mask.
- FIG. 8f is a front view photograph of a phase 1 mask manufactured according to the method described in FIGS. 8a to 8e.
- the phase mask 1 thus has a porosity gradient, the porosity being maximum in the middle of the phase 1 and minimum mask at the low and high ends of the phase 1 mask.
- the dotted lines correspond to the boundaries between the different layers 9.
- the layers 9 deposited have a height h smaller than the wavelength 1 of the incident acoustic wave 6. For example, for a frequency of 100 kHz, the wavelength 1 of an incident plane acoustic wave 6 is 15 mm.
- the layers 9 have a height equal to 8 mm (ie about 1/2), which is sufficient for the acoustic index gradient n is actually perceived as continuous for the incident plane wave 6. It is obviously possible to reduce the width of the strips, for example up to about 1 mm.
- the body 2 may comprise a support 10 having cells 1 1, each cell 1 1 containing a matrix 3, at least two of the matrices 3 having different porosities.
- the support 10 may for example be manufactured by 3D printing.
- the parameters of the 3D printing are chosen so as to manufacture a support 10 in which cells 1 1 are delimited by thin thicknesses (typically about 100 micrometers) of polylactic acid (PLA), polyamide (PA) or any other printable polymer.
- PVA polylactic acid
- PA polyamide
- the emulsions 12 of different volume fractions in the first phase 1 3 are introduced into the cells 1 1.
- the monomers of all the emulsions 12 may be crosslinked simultaneously, for example by exposure to UV through a wall 20.
- the phase mask 1 may comprise the support 10.
- the thickness of the support 10 may be typically 0.1 mm, and considered negligible compared to the acoustic wavelengths. The acoustic experiments carried out show that the presence of such a support 10, not filled with material, introduces no change in the acoustic field.
- the phase mask 1 comprises the body 2, the body 2 comprising a succession of strips or layers 9 and the support 10.
- the body 2 has a porosity gradient due to the formation of the different matrices 3 of different porosities.
- the phase mask 1 may comprise a succession of strips or layers 9, as described above.
- the phase mask 1 may make it possible to modify the propagation angle ⁇ between the propagation direction of an incident plane acoustic wave 6 and that of a transmitted wave 19, ie an angle of deflection Q with respect to the main plane 7.
- incident incident plane wave 6 of incident field P in is nsi have transformed into plane wave transmitted or deflected 19 of target field
- the gradient is preferably constant, which corresponds to a linear evolution of the porosity of the body 2 in space. In this case, it is equal to sin 9 / d and oriented along the x axis.
- the phase mask 1 can be used to focus an incident plane acoustic wave 6.
- the target field is expressed in the form
- acoustic n evolves hyperbolic way in a part of the body 2.
- Phase 1 masks with a thickness equal to 2 mm are deposited on the surface of an ultrasonic transducer (supplied by the company Imasonic) emitting at a center frequency of 1 50 kHz and having side dimensions of 150 mm ⁇ 40 mm in the plane defined by the x and y axes.
- the whole is immersed in a tank filled with water allowing measurements in immersion, as performed in underwater acoustics.
- the ultrasonic transducer is positioned in the upper part of the tank and its active face is oriented towards the bottom so as to generate an incident plane wave propagating from top to bottom along the z axis.
- the ultrasonic transducer is powered via a function generator (provided by Agilent) to generate in the water an ultrasonic wave train (30 cycles) centered at 150 kHz.
- the sound pressure emitted is then mapped in the central zone of the field near this transducer by means of a needle hydrophone having a diameter of 1 mm (supplied by Accuracy Acoustics) in the XZ plane (60 mm x 100 mm).
- the pitch in x and z between each measurement is 2 mm, that is to say 5 times smaller than the wavelength of the ultrasound used.
- the time signals were recorded by means of an acquisition card (provided by Alazartech) with a sampling frequency of 1 MHz over a duration of 300 ps for each measurement position.
- the transducer is not covered by a phase 1 mask.
- the wave fronts are planar, parallel and horizontal, and are characteristic of a plane wave propagating vertically from top to bottom of the tank as expected along the z axis.
- the transducer is covered with a phase 1 mask.
- the phase mask 1 comprises a body having a constant gradient of acoustic index (ie a variation of n linear acoustic index).
- the plane, parallel and inclined wavefronts show a deflection of the ultrasonic waves related to the presence of the phase mask 1 at the surface of the ultrasonic transducer.
- the deflection angle ⁇ of the ultrasonic beam is connected to the index gradient and the thickness of the porous material by 2 mm, and is substantially equal to 5 °.
- the transducer is covered with a phase 1 mask.
- the phase mask 1 comprises a body having a variation of n hyperbolic acoustic index.
- the mapping of the diffracted acoustic field in FIG. 12c illustrates the existence of a small central zone whose width is slightly smaller than the wavelength (ie approximately 10 mm) in which the energy of the acoustic beam is concentrated.
- the convergent (and divergent) curved wave fronts respectively visible above and below this focal task underline the focusing effect of the phase 1 mask.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- Multimedia (AREA)
- Acoustics & Sound (AREA)
- Physics & Mathematics (AREA)
- Emergency Medicine (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Respiratory Apparatuses And Protective Means (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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FR1852569A FR3079340B1 (en) | 2018-03-23 | 2018-03-23 | POROUS ACOUSTIC PHASE MASK |
PCT/EP2019/057427 WO2019180270A1 (en) | 2018-03-23 | 2019-03-25 | Porous acoustic phase mask |
Publications (1)
Publication Number | Publication Date |
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EP3769302A1 true EP3769302A1 (en) | 2021-01-27 |
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Family Applications (1)
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EP19712210.4A Withdrawn EP3769302A1 (en) | 2018-03-23 | 2019-03-25 | Porous acoustic phase mask |
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US (1) | US20210142778A1 (en) |
EP (1) | EP3769302A1 (en) |
FR (1) | FR3079340B1 (en) |
WO (1) | WO2019180270A1 (en) |
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FR2860730B1 (en) * | 2003-10-14 | 2006-02-03 | Ecole Polytech | PROCESS FOR MANUFACTURING POROUS ELEMENT AND APPLICATIONS |
KR101782624B1 (en) * | 2010-02-12 | 2017-09-28 | 삼성전자주식회사 | Aerogel and method of making the aerogel |
KR101660316B1 (en) * | 2010-03-30 | 2016-09-28 | 삼성전자 주식회사 | Organic aerogel and composition for the organic aerogel |
KR20110049572A (en) * | 2009-11-05 | 2011-05-12 | 삼성전자주식회사 | Organic aerogel, composition for the organic aerogel and method of manufacturing the organic aerogel |
KR20120026279A (en) * | 2010-09-09 | 2012-03-19 | 삼성전자주식회사 | Aerogel composite and method of manufacturing the same |
FR3035737B1 (en) * | 2015-04-29 | 2018-08-10 | Centre National De La Recherche Scientifique | ACOUSTIC METAMATERIAL FOR INSULATION AND METHOD OF MANUFACTURING THE SAME |
-
2018
- 2018-03-23 FR FR1852569A patent/FR3079340B1/en not_active Expired - Fee Related
-
2019
- 2019-03-25 EP EP19712210.4A patent/EP3769302A1/en not_active Withdrawn
- 2019-03-25 US US17/040,662 patent/US20210142778A1/en not_active Abandoned
- 2019-03-25 WO PCT/EP2019/057427 patent/WO2019180270A1/en active Application Filing
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US20210142778A1 (en) | 2021-05-13 |
FR3079340B1 (en) | 2020-03-20 |
WO2019180270A1 (en) | 2019-09-26 |
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