CN112557516B - Bismuth scandate-lead titanate-bismuth ferrite ternary system piezoelectric ceramic and acoustic emission sensor thereof - Google Patents
Bismuth scandate-lead titanate-bismuth ferrite ternary system piezoelectric ceramic and acoustic emission sensor thereof Download PDFInfo
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Abstract
The invention discloses a high-temperature piezoelectric ceramic acoustic emission sensor which comprises a packaging shell, an acoustic transmission layer, conductive adhesive, a piezoelectric element, a lead connected with the positive electrode surface of the piezoelectric element, a back lining layer between the piezoelectric element and the packaging layer, a radio frequency connector and a radio frequency coaxial cable. The piezoelectric element used in the present invention is
Wherein x is more than or equal to 0.30 and less than or equal to 0.33, y is more than or equal to 0.05 and less than or equal to 0.10, a is more than or equal to 0.02 and less than or equal to 0.05, b is more than or equal to 0.01 and less than or equal to 0.03, and c is more than or equal to 0.01 and less than or equal to 0.03. The ceramic has a high Curie temperature ofT C =470 ℃ -500 ℃ and excellent piezoelectric property (C)d 33 >230 pC/N). The acoustic emission sensor prepared by the invention can stably work at the high temperature of 300 ℃, has the characteristics of high sensitivity, high signal-to-noise ratio, simple manufacturing process, convenient use and the like, and has important significance for applying the acoustic emission technology to online monitoring in the high-temperature field.
Description
Technical Field
The invention belongs to the technical field of high-temperature sensing, relates to an acoustic emission sensor, and particularly relates to bismuth scandate-lead titanate-bismuth ferrite ternary system piezoelectric ceramic and an acoustic emission sensor thereof.
Background
High-end equipment preparation in ChinaThe manufacturing enters the rapid development period, and as the basis and the core of intelligent manufacturing, the sensor can help the transformation and upgrading of high-end manufacturing in China. The piezoelectric material is a functional material capable of realizing interconversion between electric energy and mechanical energy, and a piezoelectric device prepared based on the piezoelectric material has urgent application requirements in the fields of national defense, aerospace, new energy, nuclear energy, oil well detection, automobile internal combustion engines and the like. With the rapid development of modern industry in recent years, the application of piezoelectric materials has shifted from conventional use to service in high-temperature extreme environments. This in turn places higher demands on the performance of the piezoelectric material and the piezoelectric device, i.e., stable performance without failure at high operating temperatures. At present, commercial PZT piezoelectric devices on the market suffer from the Curie temperature of PZT ceramicsT C ) Low (less than 350 ℃) limit, stable working temperature below 170 ℃ for a long time, and can not meet the application requirements under high-temperature extreme environment. Bismuth scandate-lead titanate (BiScO) 3 -PbTiO 3 ) Solid solutions have piezoelectric properties comparable to those of PZT piezoelectric solid solutions (d 33 =460 pC/N) and relatively highT C (450 ℃ C.). However, biScO 3 -PbTiO 3 The solid solution can not meet the high-temperature service environment of 300 ℃. And bismuth ferrite (BiFeO) 3 ) High temperature piezoelectric ceramic material having high Curie temperature: (T C =825 deg.C), but relatively small piezoelectric constant ((C)d 33 =27 pC/N) limits its applications.
The Acoustic Emission (AE) detection technology can accurately detect Acoustic Emission signals generated when the interior of a material is deformed or damaged, realizes nondestructive passive detection by only detecting fault Acoustic Emission waves emitted by an object, and has the characteristics of direct convenience, high sensitivity, real-time continuity and the like. The AE technology has wide market prospect in the field of high-temperature monitoring, such as online monitoring of cracking conditions of high-temperature parts of pipelines (300 ℃) and the like in the petroleum refining process, and health detection (280-325 ℃) of equipment such as pressure vessels, main pipelines, steam generators and the like of a pressurized water reactor nuclear power station in the service process, wherein the equipment needs to be assisted by an acoustic emission sensor working in a high-temperature environment.
Therefore, to obtain an acoustic emission sensor that operates stably at high temperatures, the following three requirements must be satisfied: (1) The piezoelectric performance of the core element piezoelectric material of the sensor has good temperature stability, and the problem of serious performance deterioration in a high-temperature environment is avoided. (2) The passive materials of the sensor, such as the matching layer, the back lining layer, the adhesive and the like, have high temperature resistance, and the failure phenomenon in a high-temperature environment is avoided. (3) The normal working temperature of the sensor is higher than the temperature of the contact area, and the sensor has the characteristics of high sensitivity, high signal-to-noise ratio and the like.
Disclosure of Invention
Aiming at the requirement of a high-temperature environment on a monitoring sensor, the invention provides a piezoelectric acoustic emission sensor, wherein a core piezoelectric element adopts high-temperature piezoelectric ceramics, so that the aim of directly applying the acoustic emission sensor to the on-line monitoring of the high-temperature environment is fulfilled.
In order to achieve the purpose of the invention, the specific technical scheme of the invention is as follows:
an acoustic emission sensor comprises a packaging shell, an acoustic transmission layer, conductive adhesive, a piezoelectric element, a radio frequency connector and a radio frequency coaxial cable;
the sound-transmitting layer is arranged on the bottom opening of the packaging shell so as to arrange the piezoelectric element in the packaging shell;
the positive electrode on the upper surface of the piezoelectric element is connected with the radio frequency connector through a lead; the radio frequency connector is arranged on the packaging shell, and the other end of the radio frequency connector is connected with a radio frequency coaxial cable;
the lower electrode on the lower surface of the piezoelectric element is connected with the sound-transmitting layer through the conductive adhesive;
and a backing layer is filled between the piezoelectric element and the packaging shell.
Preferably, the packaging shell is a 316 stainless steel shell and has a cylindrical cavity; the sound-transmitting layer is Al 2 O 3 A ceramic; the backing layer is porous ZrO 2 (ii) a The lead is a mica cable wire, wherein the conductor is a twisted pure nickel wire, and the insulating material is high-temperature resistant yarn, glass fiber weaving or fluorophlogopite tape; the high-temperature conductive adhesive comprises high-temperature resistant silver powder conductive adhesive, graphite filling type conductive adhesive or high-temperature copper powder conductive adhesive; radio frequency linkThe connector is SiO 2 An insulated radio frequency connector; the radio frequency coaxial cable is SiO 2 An insulated radio frequency coaxial cable.
Preferably, the radio frequency connector is configured on a side surface of the package housing, and an end of the radio frequency connector inserted into the package housing is of a circular ring structure.
The outer diameter of the packaging shell of the acoustic emission sensor is 19mm, the inner diameter is 15mm, the wall thickness is 2mm, and the lower end and the side wall of the packaging shell are respectively provided with an opening.
The piezoelectric element of the acoustic emission sensor is wafer-shaped high-temperature piezoelectric ceramic, and the chemical formula is as follows:
wherein x is more than or equal to 0.30 and less than or equal to 0.33, y is more than or equal to 0.05 and less than or equal to 0.10, a is more than or equal to 0.02 and less than or equal to 0.05, b is more than or equal to 0.01 and less than or equal to 0.03, and c is more than or equal to 0.01 and less than or equal to 0.03.
The piezoelectric ceramic of the invention has a high Curie temperature (T C =470 ℃ -500 ℃ and excellent piezoelectric property (d 33 >230pC/N) 。
The preparation method of the piezoelectric ceramic comprises the following steps:
1) Weighing raw materials according to the stoichiometric ratio of chemical components, wherein the raw materials are oxides of Bi, sc, pb, ti, la, fe, ga and Mn, and uniformly mixing by wet ball milling.
2) And drying and presintering the ball-milled mixture.
3) And grinding and sieving the pre-sintered powder, adding an adhesive for granulation, performing compression molding, and performing degumming treatment to obtain the ceramic biscuit.
4) And sintering the ceramic biscuit at high temperature to obtain the ceramic wafer.
5) The ceramic sheet to be sintered is coated with silver.
6) And (4) performing electric polarization on the silver-coated ceramic chip.
In the step 1), ethanol with a certain proportion is added into the raw materials for wet ball milling, and the adding amount of the ethanol is 25mL/10g of the mixture. The ball milling time was 24 hours.
In the step 2), the drying temperature is 60-70 ℃, the presintering temperature is 800 ℃, and the presintering time is 2 hours.
In the step 3), the pre-sintered powder is ground and sieved by a 60-mesh sieve, the adhesive is 5% PVA water solution or paraffin, the degumming temperature is 500-600 ℃, the time is 2-4 hours, and the size of the formed biscuit is 10mm in diameter and 1.2mm in thickness.
In the step 4), the sintering temperature is 1050 ℃, and the sintering time is 2 hours.
In the step 5), the sintering temperature of the silver is 560 ℃ and the time is 0.5h.
In the step 6), electric polarization is carried out in silicone oil, the polarization field strength is 4.5-5kV/mm, the polarization temperature is 80 ℃, and the polarization time is 0.5h.
Advantageous effects
The invention constructs the ternary system solid solution of bismuth scandate-lead titanate-bismuth ferrite and realizes high Curie temperatureT C =470 ℃ -500 ℃ and excellent piezoelectric constantd 33 >230pC/N, and an acoustic emission sensor is prepared based on the solid solution ceramic, the sensor can stably work under the high temperature condition of 300 ℃, the noise is less than 30dB, and the signal is more than 90dB.
Drawings
Fig. 1 is a schematic structural diagram of an acoustic emission sensor according to the present invention.
FIG. 2 shows 0.33Bi 0.991 La 0.009 ScO 3 -0.62PbTiO 3 -0.05Bi 0.999 La 0.001 Fe 0.95 Ga 0.05 O 3 -1mol% Mn XRD pattern.
FIG. 3 shows 0.33Bi 0.991 La 0.009 ScO 3 -0.62PbTiO 3 -0.05Bi 0.999 La 0.001 Fe 0.95 Ga 0.05 O 3 -1mol% mn dielectric thermogram;
fig. 4 is a time domain characteristic diagram of the sensor in embodiment 1 of the present invention.
FIG. 5 is a high temperature impact acoustic emission test experiment of the sensor in example 1 of the present invention.
In the figure, 1, a package housing; 2. an acoustically transparent layer; 3. a conductive adhesive; 4. a lower electrode; 5. a piezoelectric element; 6. an upper electrode; 7. a lead wire connected to the positive electrode surface of the piezoelectric element; 8. a backing layer between the piezoelectric element and the encapsulation layer; 9. a radio frequency connector; 10. a radio frequency coaxial cable.
Detailed Description
The invention is further illustrated by the following figures and specific examples, which are provided for the purpose of illustrating the advantages and solutions of the present invention, and are not to be construed as limiting the scope thereof.
Fig. 1 shows a schematic structural view of an acoustic emission sensor according to the invention. As shown, comprises a package housing 1; an acoustically transparent layer 2; a conductive adhesive 3; a lower electrode 4; a piezoelectric element 5; an upper electrode 6; a lead 7 connected to the positive electrode surface of the piezoelectric element; a backing layer 8 between the piezoelectric element and the package housing; a radio frequency connector 9; a radio frequency coaxial cable 10.
The sound-transmitting layer 2 is arranged on the bottom opening of the package housing 1 to arrange the piezoelectric element in the package housing 1;
the positive electrode 6 on the upper surface of the piezoelectric element 5 is connected with the radio frequency connector 9 through a lead 7; the radio frequency connector 9 is arranged on the side surface of the packaging shell 1, the end of the radio frequency connector inserted into the packaging shell is of a circular ring structure, and the other end of the radio frequency connector is connected with a radio frequency coaxial cable 10;
the lower electrode 4 on the lower surface of the piezoelectric element 5 is connected with the sound-transmitting layer 2 through the conductive adhesive 3;
and a backing layer 8 is filled between the piezoelectric element 5 and the packaging layer.
The packaging shell is a high-temperature 316 stainless steel shell and structurally adopts a cylindrical cavity; the sound-transmitting layer is Al 2 O 3 A ceramic; the back lining layer is porous ZrO 2 (ii) a The lead is a mica cable wire, wherein the conductor is a twisted pure nickel wire, and the insulating material is high-temperature resistant yarn, glass fiber weaving or fluorophlogopite tape; the high-temperature conductive adhesive comprises high-temperature resistant silver powder conductive adhesive, graphite filled conductive adhesive or high-temperature copper powder conductive adhesive; the radio frequency connector is SiO 2 An insulated radio frequency connector; the radio frequency coaxial cable is SiO 2 An insulated radio frequency coaxial cable. As shown in fig. 1, the piezoelectric element 5 is a core element of the sensor, and functions to receive an acoustic wave; the conductive adhesive 3 is connected with the negative electrode surface of the piezoelectric crystalThe function of the packaging shell; the sound-transmitting layer 2 is used for reducing sound loss in the sound transmission process and improving the monitoring effect; the backing layer 8 acts as ZrO 2 The porous structure of (a) helps to absorb the backward acoustic radiation energy, thereby reducing the impact on forward acoustic transmission.
Example 1
Adopts high-temperature piezoelectric ceramic pieces as piezoelectric elements and contains Al 2 O 3 99% of Al with a diameter of 18mm and a thickness of 1mm 2 O 3 Ceramic as sound-transmitting layer, silver powder as high-temp. conducting adhesive and adhesive, pt as upper and lower electrode layers, and porous ZrO 2 Is a sound absorbing material.
Wherein the ceramic is 0.33Bi 0.991 La 0.009 ScO 3 -0.62PbTiO 3 -0.05Bi 0.999 La 0.001 Fe 0.95 Ga 0.05 O 3 -1mol% of Mn. With analytically pure starting material Bi 2 O 3 、Sc 2 O 3 、PbO、TiO 2 、La 2 O 3 、Fe 2 O 3 、Ga 2 O 3 、MnO 2 Proportioning according to a stoichiometric ratio, adding ethanol, wherein the adding amount of the ethanol is 25mL/10g of the mixture, and putting the mixture into a ball milling tank for ball milling for 24 hours to be uniformly mixed; after being uniformly mixed, the mixture is put into a drying oven and dried at 60 ℃; grinding the dried mixture and sieving the ground mixture by a 60-mesh sieve; presintering for 2 hours at the temperature of 800 ℃; and adding 0.5ml of PVA solution into the pre-sintered material, grinding and sieving by a 100-mesh sieve to complete granulation. Pressing the granulated pre-sintered material into a round sheet with the diameter of 10mm and the width of 1mm by using a tablet press, and carrying out glue discharging at the temperature of 600 ℃ to obtain a ceramic biscuit, wherein the glue discharging time is 2 hours; then sintering the biscuit at 1050 ℃ for 2h to obtain a ceramic wafer; polishing two surfaces of the sintered ceramic wafer, and burning silver by an Ag electrode; applying a direct current electric field of 4.5kV/mm in the silicone oil at 80 ℃ and keeping for 0.5h to obtain 0.33Bi 0.991 La 0.009 ScO 3 -0.62PbTiO 3 -0.05Bi 0.999 La 0.001 Fe 0.95 Ga 0.05 O 3 -1mol% mn of a finished piezoelectric ceramic product; the properties of the ceramics are as follows:T C =500℃，d 33 =270pC/N。
figure 3 is a time domain plot of the sensor,
FIG. 4 shows the high temperature impact acoustic emission test experiment of the sensor at 300 deg.C, with noise less than 30dB and signal greater than 90dB.
Example 2
Adopts high-temperature piezoelectric ceramic pieces as piezoelectric elements and contains Al 2 O 3 99% of Al with a diameter of 18mm and a thickness of 1mm 2 O 3 Ceramic as sound-transmitting layer, silver powder as high-temp. conducting adhesive and adhesive, pt as metal layer as upper and lower electrode layers, and porous ZrO 2 Is a high temperature sound absorbing material.
Wherein the ceramic is 0.3Bi 0.992 La 0.008 ScO 3 -0.6PbTiO 3 -0.1Bi 0.998 La 0.002 Fe 0.95 Ga 0.05 O 3 -1mol% of Mn. With analytically pure starting material Bi 2 O 3 、Sc 2 O 3 、PbO、TiO 2 、La 2 O 3 、Fe 2 O 3 、Ga 2 O 3 Proportioning according to a stoichiometric ratio, adding ethanol, wherein the adding amount of the ethanol is 25mL/10g of the mixture, and putting the mixture into a ball milling tank for ball milling for 24 hours to be uniformly mixed; after being uniformly mixed, the mixture is put into a drying oven and dried at 60 ℃; grinding the dried mixture and sieving the ground mixture by a 60-mesh sieve; presintering for 2h at the temperature of 800 ℃; and adding 0.5ml of VA solution into the pre-sintered material, grinding and sieving by a 100-mesh sieve to complete granulation. Pressing the granulated pre-sintered material into a round sheet with the diameter of 10mm and the width of 1mm by using a tablet press, and carrying out glue discharging at the temperature of 600 ℃ to obtain a ceramic biscuit, wherein the glue discharging time is 2 hours; then sintering the biscuit at 1050 ℃ for 2h to obtain a ceramic wafer; polishing two surfaces of the sintered ceramic wafer, and burning silver by an Ag electrode; applying a direct current electric field of 4.5kV/mm in the silicone oil at the temperature of 80 ℃ and keeping for 0.5h to obtain 0.3Bi 0.992 La 0.008 ScO 3 -0.6PbTiO 3 -0.1Bi 0.998 La 0.002 Fe 0.95 Ga 0.05 O 3 -1mol% of mn; the properties of the ceramics are as follows:T C =470℃，d 33 =238pC/N。
Claims (9)
1. an acoustic emission sensor, characterized by: the piezoelectric acoustic transducer comprises a packaging shell (1), an acoustic transmission layer (2), conductive adhesive (3), a piezoelectric element (5), a lead (7) connected with the positive electrode surface of the piezoelectric element, a backing layer (8) between the piezoelectric element and the packaging layer, a radio frequency connector (9) and a radio frequency coaxial cable (10);
the sound-transmitting layer (2) is arranged on the bottom opening of the package housing (1) to arrange the piezoelectric element in the package housing (1);
the positive electrode (6) on the upper surface of the piezoelectric element (5) is connected with the radio frequency connector (9) through a lead (7); the radio frequency connector (9) is arranged on the packaging shell (1), and the other end of the radio frequency connector is connected with a radio frequency coaxial cable (10);
the lower electrode (4) on the lower surface of the piezoelectric element (5) is connected with the sound-transmitting layer (2) through the conductive adhesive (3);
a back lining layer (8) is filled between the piezoelectric element (5) and the packaging layer;
the piezoelectric element is high-temperature piezoelectric ceramic and has a chemical formula as follows:
2. The acoustic emission sensor of claim 1, wherein the package housing is a 316 stainless steel housing configured as a cylindrical cavity; the sound-transmitting layer is Al 2 O 3 A ceramic; the backing layer is porous ZrO 2 (ii) a The lead is a mica cable wire, wherein the conductor is a twisted pure nickel wire, and the insulating material is high-temperature resistant yarn, glass fiber weaving or fluorophlogopite tape; the high-temperature conductive adhesive comprises high-temperature resistant silver powder conductive adhesive, graphite filled conductive adhesive or high-temperature copper powder conductive adhesive; the radio frequency connector is SiO 2 An insulated radio frequency connector; the radio frequency coaxial cable is SiO 2 An insulated radio frequency coaxial cable.
3. The acoustic emission sensor according to claim 2, wherein the rf connector (9) is disposed on a side surface of the package housing (1), and an end of the rf connector inserted into the package housing is a ring-shaped structure.
4. The acoustic emission sensor of claim 1, wherein the piezoelectric ceramic is prepared by a method comprising the steps of:
1) Weighing raw materials according to the stoichiometric ratio of chemical components, wherein the raw materials are oxides of Bi, sc, pb, ti, la, fe, ga and Mn, and uniformly mixing by wet ball milling;
2) Drying and pre-sintering the ball-milled mixture;
3) Grinding and sieving the pre-sintered powder, adding an adhesive for granulation, performing compression molding, and performing degumming treatment to obtain a ceramic biscuit;
4) Sintering the ceramic biscuit at high temperature to obtain a ceramic wafer;
5) Coating silver on the sintered ceramic wafer;
6) And (4) performing electric polarization on the silver-coated ceramic chip.
5. The acoustic emission sensor of claim 4, wherein in step 1), ethanol is added to the raw materials for wet ball milling, the addition amount is 25mL/10g of the mixture, and the ball milling time is 24 hours.
6. The acoustic emission sensor of claim 4, wherein in step 2), the drying temperature is 60-70 ℃, the pre-sintering temperature is 800 ℃, and the pre-sintering time is 2 hours.
7. The acoustic emission sensor according to claim 4, wherein in step 3), the pre-sintered powder is ground and sieved with a 60-mesh sieve, the binder is PVA aqueous solution or paraffin with the content of 5%, the degumming temperature is 500-600 ℃, the time is 2-4h, and the size of the formed biscuit is 10mm in diameter and 1.2mm in thickness.
8. The acoustic emission sensor according to claim 4, characterized in that in step 4), the sintering temperature is 1050 ℃ and the sintering time is 2h.
9. The acoustic emission sensor of claim 4, wherein in step 5), the silver sintering temperature is 560 ℃ and the time is 0.5h; in the step 6), electric polarization is carried out in silicone oil, the polarization field strength is 4.5-5kV/mm, the polarization temperature is 80 ℃, and the polarization time is 0.5h.
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