LAMINAR STRUCTURE AS PART OF A PIEZOELECTRIC ULTRASONIC TRANSDUCER
20220120718 · 2022-04-21
Inventors
Cpc classification
G01N29/245
PHYSICS
International classification
B06B1/06
PERFORMING OPERATIONS; TRANSPORTING
Abstract
The present invention relates to a layered structure, the method for obtaining it and its use as part of a piezoelectric ultrasonic transducer to operate in broadband pulse-echo mode and with high sensitivity and axial resolution in the presence of a pressurised gas at a pressure between 14 bar and 103 bar. Furthermore, the present invention relates to the transducer comprising said layered or stratified structure. Therefore, the present invention can be framed in the area of materials with applications such as sensors in ultrasonic systems.
Claims
1. A layer structure comprising: a resonant adaptive polymer membrane with a thickness between 50 μm and 150 μm presenting; quarter-wave resonance conditions at a centre frequency greater than or equal to 1 MHz, between 1 MHz and 4 MHz, an acoustic impedance between 0.1 MRayl and 0.5 MRayl, a porosity greater than 70% and interconnected pores; a pressure-sensitive adhesive layer, less than 60 μm thick; located on the resonant layer and covering said layer completely; which has an acoustic impedance between 0.5 MRayl and 1.5 MRayl; a syntactic foam layer, with a thickness between 100 μm and 500 μm; located on the layer and covering said layer completely, which has an acoustic impedance between 0.5 MRayl and 2 MRayl; a polymer layer with a thickness between 100 μm and 500 μm; located on the layer and covering said layer completely, which has an acoustic impedance between 1.5 MRayl and 3.5 MRayl; a first conductive layer, with a thickness of between 20 nm and 100 nm, located on the layer and covering said layer completely; a piezoelectric layer comprising an internal face and an external face; with a thickness of between 0.5 and 2 mm, which is located on the conductive layer, wherein the external face is in direct contact with the conductive layer, and which is partially covering said conductive layer; a second conductive layer, with a thickness of between 20 nm and 100 nm, located on the internal face (i) of the piezoelectric layer and covering said layer completely; a block, with anechoic conical finish; with a thickness between 15 mm and 30 mm, located on the conductive layer and extending around the layers and until contacting the conductive layer, which has an acoustic impedance between 5 MRayl and 10 MRayl, and which is composed of an epoxy resin comprising particles with a diameter between 1 μm and 50 μm selected from among tungsten, zirconia, alumina and any of the combinations thereof; wherein the piezoelectric layer, the second conductive layer internal face, the second conductive layer external face, the block, the polymer layer, the syntactic foam layer, the pressure-sensitive adhesive layer and the resonant adaptive polymer membrane withstand hydrostatic pressures up to 262 bar, wherein the piezoelectric layer is polarised along the thickness thereof, and wherein the layers the polymer layer, the syntactic foam layer and the pressure-sensitive adhesive layer, form an assembly having quarter-wave resonance conditions at a centre frequency greater than or equal to 1 MHz, between 1 MHz and 4 MHz.
2. The structure according to claim 1, wherein the resonant adaptive polymer membrane is selected from polypropylene, cellulose nitrate, cellulose ester, polyethersulfone and nylon.
3. The structure according to claim 1, wherein the pressure-sensitive adhesive layer is selected from an acrylic layer or a polyurethane layer.
4. The structure according to claim 1, wherein the syntactic foam layer is composed of an epoxy resin with hollow spheres with a diameter between 1 μm and 20 μm.
5. The structure according to claim 1, wherein the polymer layer is an epoxy resin.
6. The structure according to claim 1, wherein the conductive layers internal face and external face are independently composed of a conductive material selected from Au, Ag, Cu, Sn and any of the combinations thereof.
7. The structure according to claim 1, wherein the composition of the piezoelectric layer is selected from a PZT-type ceramic of lead zirconate titanate PbZrO.sub.3—PbTiO.sub.3, a composite material of piezoelectric ceramic and resin with 1-3 type connectivity and with a volumetric concentration of ceramic between 25% and 80%, and a Pb (Mg.sub.1/3Nb.sub.2/3)OR.sub.3—PbTiO.sub.3-type piezoelectric single crystal.
8. A method for obtaining the structure according to claim 1, comprising the following steps: (a) joining the piezoelectric layer covered by the conductive layers internal face and external face to a sacrificial layer adhesive tape on a first face, (b) joining a metal housing or case to the sacrificial layer with adhesive tape, (c) filling the space formed between the piezoelectric layer and the metal housing or case with resin and curing said resin, (d) removing the sacrificial layer, (e) metallising the first face of the piezoelectric layer so that the conductive layer external face completely covers the piezoelectric element and the edge of the bushing, (f) depositing the polymer layer on the conductive layer external face, and curing and polishing, (g) affixing the syntactic foam layer to the polymer layer, (h) adhering the pressure-sensitive adhesive layer on the syntactic foam layer, (i) affixing the resonant adaptive polymer membrane to the pressure-sensitive adhesive layer, (j) fastening the assembly of the piezoelectric layer, the second conductive layer internal face, the second conductive layer external face, the block, the polymer layer, the syntactic foam layer, the pressure-sensitive adhesive layer and the resonant adaptive polymer membrane) and turning it over, and (k) filling the inner space of the metal housing or case with a conical mould to form a conical-shaped block.
9. The method according to claim 8, wherein step (e) is carried out by techniques selected from sputtering, vacuum metallisation, evaporation metallisation, screen-printed metallisation, dip coating or spin coating.
10. The method according to claim 8, wherein the deposition of step (f) is carried out by deposition techniques selected from dip coating, spin coating, or screen printing.
11. The method according to claim 8, wherein step (g) is carried out using an adhesive that has the same composition as the polymer layer.
12. A piezoelectric ultrasonic transducer to detect echoes generated by a solid body in the presence of a pressurised gas at a pressure between 14 bar and 103 bar, wherein the transducer comprises the structure according to claim 1.
13. The piezoelectric ultrasonic transducer according to claim 12, further comprising: the structure, wherein the resonant adaptive polymer membrane is configured to act as a quarter-wave resonant layer at the centre frequency of the transducer, wherein the assembly formed by the polymer layer, the syntactic foam layer and the pressure-sensitive adhesive layer is configured to act together as a single resonant layer of the centre frequency of the transducer and gradually reduce the acoustic impedance of the structure, wherein the first conductive layer external face and the second conductive layer internal face are configured to act as an electrode and enable the application/measurement of electric field in the piezoelectric layer, and wherein the block is configured to dampen the vibration of the piezoelectric layer, a metal housing or case comprising a coaxial connector with a ground connection and an internal connector of the rear cover of the metal housing or case and which is configured to house the structure and provide electromagnetic shielding, wherein the second conductive layer external face, the block, the polymer layer, the syntactic foam layer, the pressure-sensitive adhesive layer and the resonant adaptive polymer membrane are in contact with the walls of the housing or case; a coaxial connector that joins the internal connector of the rear cover of the metal housing or case to the second conductive layer internal face that is configured to apply a voltage to the piezoelectric element through the connector or to measure the voltage generated in the piezoelectric element; and a protective crown or rim configured to protect the resonant adaptive polymer membrane and the lateral edge of the resonant adaptive polymer membrane, the assembly formed by the polymer layer, the syntactic foam layer, the pressure-sensitive adhesive layer, the block, the first conductive layer external face and the second conductive layer internal face.
Description
BRIEF DESCRIPTION OF THE FIGURES
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EXAMPLES
[0127] The invention shall be illustrated below by way of assays carried out by the inventors, which shows the effectiveness of the product of the invention.
[0128] The following exemplary embodiment relates to a piezoelectric ultrasonic transducer with a circular cross section. The following table 1 lists and describes the elements that make up the transducer.
TABLE-US-00001 TABLE 1 Elements of the transducer with the description thereof Element Description Piezoelectric (1) PZT5A piezoelectric ceramic in epoxy resin layer matrix. Volumetric concentration of PZT5A piezoelectric ceramic 50%, Polarised in the direction of thickness. 1-3 connectivity (dice and fill, pixel: 200 μm) Shape: disc Diameter: 9.83 mm Thickness: 1.544 mm Conductive (2i) CuSn conductive layer layer and Thickness: 100 nm (2e) Block (3) Epoxy resin loaded with tungsten particles (diameter 20 μm). Acoustic impedance 4 MRayl. Thickness: 30 mm Polymer (4) Epoxy resin layer Impedance: 2.75 MRayl Shape: disc Diameter: 14 mm Thickness: 360 μm Syntactic (5) Epoxy resin loaded with hollow glass spheres foam layer (diameter 20 μm), Impedance: 0.7 MRayl. Shape: disc Diameter: 14 mm Thickness: 330 μm Pressure- (6) Impedance: 0.7 MRayl sensitive Shape: disc adhesive Thickness: 60 μm layer Diameter: 14 mm Resonant (7) Material: Polypropylene adaptive Impedance: 0.1 MRayl polymer Porosity 70% membrane Thickness: 90 μm Diameter: 14 mm Interconnected pores Metal housing (8) Aluminium tube or case Internal diameter: 11 mm External diameter: 13.3 mm Length: 28 mm Rear Cable or (9) Panel SMB-type connector. Connector It is a standard type of coaxial connector Front face (11) Aluminium protective External diameter: 15.2 mm crown Light: 11.0 mm Height: 5.1 mm * It is a composite material of piezoelectric ceramic and resin. The resin is the matrix and the ceramic comes in the form of a stack of pillars. This type of compound is referred to as 1-3, 1 because the ceramic is connected only in 1 direction, which are the pillars, and 3 because the resin is connected in the three directions of space, which is a matrix.
[0129] Dice and fill refers to the standard manufacturing method of this material: a ceramic disk is taken, a series of regularly spaced cuts are produced in two orthogonal directions that form the pillars, and the gaps are then filled with resin.
[0130] The materials used in the manufacturing are listed below:
[0131] Structural elements [(8), (9), (11)]: [0132] Conductive metal housing or case (cylinder with internal diameter 11 mm and wall thickness 1 mm). 25 mm in length. [0133] Flat rear cover with circular through hole in the centre for SMB connector. [0134] Metal front crown or rim for protection of the radiant face.
[0135] Housing or case, rear cover and front crown or rim according to
[0136] Other materials: [0137] SMB-type panel coaxial connector. [0138] Cable (0.2 mm) [(9)]. [0139] Disc of piezoelectric composite material [(1), (2i), (2e)], 1-3 connectivity, PZT5A ceramic and 50% epoxy resin. Manufactured by the dice and fill technique. Polarised in the thickness direction and metallised on both flat faces (100 nm thick CuSn coating). Disc with 9.83 mm diameter, 1.54 mm thickness. Resonance frequency: 1 MHz. [0140] Epoxy resin, density 1150 kg/m.sup.3, ultrasound speed 2450 m/s [(4)] [0141] Syntactic foam [(5)] (epoxy resin loaded with hollow spheres, diameter <20 μm (acoustic impedance of 0.7 MRayl and ultrasound velocity of 2100 m/s). [0142] Double-sided pressure-sensitive adhesive tape [(6)]. Without support, thickness: 60 microns, acoustic impedance 0.6 MRayl. [0143] Resonant polymer membrane [(7)] at the centre frequency of the transducer (1 MHz±10%). Material: Polypropylene; Impedance: 0.095 MRayl (±10%); Porosity: 70%, Porosity type: open (interconnected). Thickness: 90 μm Diameter: 14 mm.
[0144] Materials for the backing [(3)]: [0145] Epoxy resin, density 1150 kg/m.sup.3, ultrasound speed 2450 m/s [0146] Rubber powder (particle size <120 microns). [0147] Tungsten powder (particle size: 12 microns).
[0148] Auxiliary materials: [0149] Low density polyurethane foam (100-300 kg/m.sup.3) for the manufacture of the conical mould for finishing the backing [(3)]. [0150] Demoulding agent. [0151] Plastic layer (200 um, polycarbonate). [0152] Tin and paste for soldering.
Manufacturing Method:
(1) Method for the Initial Verification of the Piezoelectric Disc by Measuring the Electrical Impedance and for Successive Verifications During the Manufacturing Process.
[0153] The integrity and suitability of the piezoelectric disc is checked by measuring the electrical impedance thereof in an impedance analyser or network analyser in the vicinity of the resonance frequency of the thickness mode provided by the manufacturer, in this case 1 MHz. To measure the electrical impedance of the disc, the metallised faces are connected to the output terminals of the impedance analyser. It is verified that the electrical resonance is at 1 MHz (tolerance 5%). This will be the centre frequency of the transducer to be manufactured. The integrity of the piezoelectric resonance is also verified by comparing the measured impedance curve with that which is provided by the manufacturer. Likewise, the almost negligible influence of radial modes of vibration is verified (lower frequency resonances and the harmonics thereof that can overlap with the resonance of the thickness mode located at 1 MHz).
[0154]
[0155] This same electrical impedance measurement taken at the terminals of the piezoelectric disc is repeated at each step of the process to verify the integrity of the piezoelectric response and the correct assembly and sizing of the layers and elements placed at each step by comparing the measured impedance curve with that which is calculated knowing the properties (thickness, impedance and damping) of each deposited layer.
(2) Fastening the Piezoelectric Disc to the Jousting or Case and Preparing Electrical Connections.
[0156] A piece of cable with a length approximately equal to twice the length of the housing or case (60 mm in this case) is taken and both ends are stripped to a length, approximately 3 mm). It is wound in the form of a solenoid (with an approximate diameter of ⅓ the internal diameter of the bushing, 4 mm in this case, and a similar length to that of the housing or case, 28.2 mm in this case) and one of the ends thereof is soldered to one of the faces of the piezoelectric disc using tin and paste for soldering. The other end of the cable is free. See
[0157] A demoulding agent is applied to the other face of the piezoelectric disc.
[0158] A plastic layer (polycarbonate 200 um, 30×30 mm) is taken and double-sided adhesive tape is affixed on a 40×40 mm surface. This will act as a support for fastening the piezoelectric disc to the housing or case. The piezoelectric disc is affixed to this layer on the face on which the demoulding agent was applied. See
[0159] The metal housing or case is affixed to the plastic film concentrically to the piezoelectric disc, ensuring the leak-tightness of the cavity formed by the bushing, piezoelectric disc and polycarbonate layer. See
[0160] The edge between the housing or case and the piezoelectric disc (width of 1 mm in the present example) is filled with epoxy resin loaded with tungsten powder and rubber powder, manufactured following the method explained in (3). See
[0161] The resin deposited between the housing or case and the piezoelectric disc is left to cure.
[0162] Once the resin has cured, the polycarbonate layer affixed to the piezoelectric disc and cylinder is removed. The external surface of the piezoelectric disc and the edge of the metal housing or case are cleaned of any remaining adhesive residue, preserving the metallisation of the piezoelectric disc. The end result in this step is that the piezoelectric disc is fastened to the housing or case by means of a resin ring loaded with tungsten powder See
[0163] The surface that has just been cleaned is metallised: piezoelectric disc+resin ring+edge of the housing or case. Any available technique can be used, either sputtering, evaporation or screen printing. See
[0164] Finally, the electrical conductivity between the surface that has just been metallised and the metal housing or case of the transducer is verified and the electrical impedance measurement is repeated to verify that the piezoelectric resonance remains unchanged except for the introduction of a slight damping due to the fastening from the piezoelectric disc to the housing or case. The result of the impedance measurement is shown in
(3) Manufacture of the Multilayer Material for Optimal Adaptation of Impedances to Gas/Air.
[0165] Deposition of a 300-350 micron resin layer, using a screen printing, deep coating or any similar technique on the external surface of the piezoelectric disc. For this purpose, both components of the resin are mixed, the trapped air is removed using a vacuum hood and deposited, while in a liquid state, on the metallised surface, covering it completely. It is not necessary for the deposited layer to lie flat or parallel. The amount of resin deposited, equivalent to a 300-350 micron layer, is controlled by means of weighing on a precision scale. The final result can be seen in
[0166] The resin thus deposited is left to cure following the resin manufacturer's instructions.
[0167] Once cured, its external surface is polished using an automatic polisher to leave a flat finish normal to the axis of the bushing. The final thickness of this layer should be 260 μm, roughness <5 μm. The result after this step can be seen in
[0168] At this point, the electrical impedance measurement of the transducer is repeated to verify the correct deposition of the resin layer, as explained in (1). For this, the free end of the cable and the bushing are connected to the terminals of the impedance analyser. The result is shown in
[0169] A 1 mm thick layer, with a side >25 mm, is cut from a block of syntactic foam.
[0170] The thickness of the previous layer is lowered, either by means of a numerical control lathe or by using a polisher, to a thickness of 330 μm, guaranteeing the flat parallelism of both faces of the layer. A disc is cut from this layer with the same diameter as the external diameter of the housing or case of the transducer (13.3 mm in this case). Said operation can be performed using a punch.
[0171] The syntactic foam layer is affixed to the surface of the transducer using the same epoxy resin that was deposited on the surface of the piezoelectric element. The added thickness of epoxy resin to achieve this bond must be 100 μm. The amount of resin added is controlled by weighing on a precision scale. See
[0172] Once the previous layer has cured and therefore the syntactic foam layer has been affixed, the electrical impedance measurement is repeated by connecting the free end of the cable and the housing or case to the terminals of the impedance analyser to verify the correct placement of this layer as explained in (1). The result is shown in
[0173] Once verified, a layer of pressure-sensitive double-sided adhesive tape (thickness 60 μm) is placed on the external surface of the syntactic foam layer. The adaptive and resonant polymer membrane is placed on this layer of adhesive tape. See
[0174] Once this cycle is finished and the transducer has cooled down, the electrical impedance measurement is repeated by connecting the free end of the cable and the bushing to the terminals of the impedance analyser to verify the correct placement of this layer as explained in (1). The result is shown in
(4) Front Crown or Rim.
[0175] Once the last layer of the stack of layers has been deposited, both the front face and the side face are protected by placing the front protection ring, which can be simply fitted or fitted and affixed onto the housing or case. See
(5) Placement of the Backing.
[0176] Once the front protection crown or rim is placed, the transducer is placed in a vertical position, resting on the front crown. The cavity formed by the housing or case and the surface of the piezoelectric disc is filled with the mixture of epoxy resin, tungsten and rubber powder before the mixture begins to cure, up to a height of ⅔ of the total height of the bushing, ensuring that the free end of the cable soldered to the piezoelectric disc is free. The mixture is left to cure. See
[0177] Manufacture of the mould for the conical finish of the backing. A disc is cut from the low-density polyurethane foam (100-300 kg/m.sup.3), with a diameter equal to the internal diameter of the metal bushing and a thickness equal to the radius. A conical surface with a generatrix at 45 degrees from the axis is carved on one of the faces of this disc. A small hole (<1 mm diameter) is made at the vertex.
[0178] The mould thus manufactured is placed on the backing deposited in the housing or case by passing the free end of the cable soldered to the piezoelectric disc through the hole made at the vertex of the conical surface. See
[0179] The conical space between the mould and the backing is filled with the same mixture of resin, tungsten and rubber powder with which the backing was manufactured. It is left to cure. See
[0180] Once the backing is placed, the correct operation is verified again by measuring the electrical impedance of the transducer. The result is shown in
(6) Placement of the Connector and Rear Cover.
[0181] The panel SMB coaxial connector is fastened to the rear cover. The grounded connector is connected to the rear cover. The free end of the cable is soldered to the internal pin of the coaxial connector (SMB). See
[0182] The rear cover is fastened to the housing or case ensuring the electrical connectivity between the rear cover and the body of the housing or case and between the internal pin of the connector and the cable of the transducer. See
(7) Manufacture of the Material to Make the Backing of the Transducer and of the Material to Fasten the Piezoelectric Disc to the Bushing. Both Materials are Identical.
[0183] The material is made up of epoxy resin, tungsten powder (12 microns) and rubber powder (<120 microns). Weight ratio: Resin: 22%, Tungsten powder: 72%, rubber powder: 6%
[0184] The additives (tungsten powder and rubber powder) are added to component A of the resin.
[0185] The three components are mixed well.
[0186] Resin hardener (part B) is added.
[0187] The mixture is placed in a vacuum to remove trapped gas.
[0188] The mixture is deposited in its final location. The mixture is again degassed in a vacuum hood.
[0189] It is subjected to hydrostatic pressure to remove the smallest bubbles (30 min, 6 bar).
[0190] The resin is cured following the manufacturer's instructions.
(8) Verification of the Properties of the Membrane: Resonance Frequency and Impedance.
[0191] To verify the correct selection of the membrane, the characterisation technique described in the following references is applied [0192] [1] T. Gómez Álvarez-Arenas, “Air-coupled ultrasonic spectroscopy for the study of membrane filters,” J. Memb. Sci., vol. 213, no. 1-2, p. 195-207, March 2003. [0193] [2] T. E. Gómez Alvarez-Arenas, “A non-destructive integrity test for membrane filters based on air-coupled ultrasonic spectroscopy.” IEEE Trans. Ultrason. Ferroelectr. Freq. Control, vol. 50, no. 6, p. 676-85, June 2003. [0194] [3] T. E. Gómez Álvarez-Arenas. Device for the characterisation of ultrasonic materials with gas coupling (air) and the application thereof to carry out a non-destructive test to verify the integrity of porous membranes. Patent ES 223950061, 2003
which consists of the measurement of the transmission coefficient of the membrane to the ultrasounds using normal incidence and air as a coupling medium in a frequency range where the membrane thickness resonance appears. Under these conditions, said resonance appears at the frequency wherein the wavelength is equal to twice the thickness (that is, resonance λ/2). This frequency has to be twice the centre frequency of the transducer, since when the membrane is deposited on the transducer its resonance will be λ/4. That is, a membrane is needed the resonance frequency of which is 2.0 MHz, the tolerance for this criterion is 5%.
[0195] In addition, based on the theoretical analysis of the magnitude and phase of the transmission coefficient, it is also possible to determine the impedance of the material [4]. [0196] [4] T. E. Gómez Alvarez-Arenas, “Simultaneous determination of the ultrasound velocity and the thickness of solid plates from the analysis of thickness resonances using air-coupled ultrasound.” Ultrasonics, vol. 50, no. 2, p. 104-9, February 2010.
[0197] The spectrum of the transmission coefficient of the selected membrane (magnitude and phase) and the theoretical adjustment that enables the determination of the impedance are shown in
[0198]
[0199] To measure the impulse response and the sensitivity band at ambient pressure and with an air overpressure of 5 bar, of the manufactured transducer, an Olympus transmitter-receiver (5072) is used, a 90 V amplitude excitation pulse, and the received signal is taken directly to the oscilloscope, without any extra amplification. A 22 uH inductance is placed in parallel with the terminals of the transducer. The reflector was a steel block located at 7 mm.
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