CN112723880B - Preparation method of high-corrosion-resistant composite piezoelectric ceramic material - Google Patents
Preparation method of high-corrosion-resistant composite piezoelectric ceramic material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 38
- 238000005260 corrosion Methods 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000919 ceramic Substances 0.000 claims abstract description 55
- 238000000498 ball milling Methods 0.000 claims abstract description 26
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 21
- 239000011230 binding agent Substances 0.000 claims abstract description 13
- 230000010287 polarization Effects 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000005303 weighing Methods 0.000 claims abstract description 12
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001125 extrusion Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 229910052709 silver Inorganic materials 0.000 claims abstract description 9
- 239000004332 silver Substances 0.000 claims abstract description 9
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 8
- 238000005476 soldering Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 10
- 230000007797 corrosion Effects 0.000 claims description 9
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 7
- 239000003292 glue Substances 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 230000005684 electric field Effects 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000000853 adhesive Substances 0.000 claims description 4
- 230000001070 adhesive effect Effects 0.000 claims description 4
- 230000008878 coupling Effects 0.000 abstract description 16
- 238000010168 coupling process Methods 0.000 abstract description 16
- 238000005859 coupling reaction Methods 0.000 abstract description 16
- 230000008569 process Effects 0.000 abstract description 3
- 238000005469 granulation Methods 0.000 abstract 1
- 230000003179 granulation Effects 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 description 14
- 238000006467 substitution reaction Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 239000013078 crystal Substances 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
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- 239000003513 alkali Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
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- 238000005336 cracking Methods 0.000 description 1
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- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
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Abstract
The invention discloses a preparation method of a high-corrosion-resistant composite piezoelectric ceramic material, which comprises the following steps: weighing the following components: in stoichiometric ratio Ba 1‑x Mg x Ti 1‑2y Sb y In y O 3 Weighing; wherein x is 0.5-3 mol% and y is 0.2-3 mol%. (2) primary forming: mixing the raw materials of the components, and performing ball milling, drying, granulation, extrusion forming, binder removal, sintering and other processes to obtain piezoelectric ceramics; (3) polarization treatment: soldering and magnetron sputtering silver electrodes on the upper surface and the lower surface of the preliminarily formed piezoelectric ceramic respectively to finally obtain the high-corrosion-resistance composite piezoelectric ceramic material. The preparation method has simple steps, and the BT-based ceramic is doped in a soft and soft mode, so that the piezoelectric constant d is ensured 33 And the mechanical quality factor Qm and the electromechanical coupling coefficient Kp are improved.
Description
Technical Field
The invention relates to the field of piezoelectric ceramics, in particular to a preparation method of a high-corrosion-resistance composite piezoelectric ceramic material.
Background
With the continuous development of piezoceramic materials in China, the requirements of people on piezoceramics are higher and higher, for example, a lead zirconate titanate (PZT) ceramic system has a higher piezoelectric constant d 33 However, lead contained in PZT is apt to cause environmental pollution at the time of use or disposalTherefore, the development of lead-free piezoelectric ceramics has become a trend. And barium titanate (BaTiO) 3 BT) ceramic does not bring much pollution, but the piezoelectric constant of BT-based ceramic prepared by the traditional method is only about 200 pC/N. Due to BaTiO 3 The piezoelectric ceramic being ABO 3 The A site ions of the perovskite ferroelectric can be replaced by Ca, sr, la, Y and other elements, and the B site ions of the perovskite ferroelectric can be replaced by Zr, sn, nb, ce and other elements, most of the prior art carries out modification on BT-based ceramics by doping, but the modification brings about side effects, such as the reduction of the flatness factor caused by the increase of the dielectric coefficient and the electromechanical coupling coefficient, and the mechanical quality factor Qm is particularly important in devices such as a filter, a resonant transducer and the like, so that the demand for obtaining ceramic materials with excellent performances is urgent.
Disclosure of Invention
The invention aims to provide a preparation method of a high-corrosion-resistance composite piezoelectric ceramic material, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: the preparation method of the high-corrosion-resistance composite piezoelectric ceramic material comprises the following steps:
(1) Weighing the following components: the raw material BaCO is mixed 3 、TiO 2 、MgO、Sb 2 O 5 And In 2 O 3 In stoichiometric ratio of Ba 1-x Mg x Ti 1- 2y Sb y In y O 3 Weighing; wherein x is 0.5-3 mol% and y is 0.2-3 mol%;
using Mg 2+ To Ba 2+ Equivalent replacement can improve the piezoelectric constant d of the BT-based ceramic 33 Using high valent ions Sb 5+ For Ti 4+ To be replaced by soft substituted, low valence ion In 3+ For Ti 4+ To make a hard substitution, equivalent to Sb 5+ And In 3+ Replacement of Ti 4+ The soft-hard implementation is realized, the mechanical quality factor Qm and the electromechanical coupling coefficient Kp are improved, and the piezoelectric constant d is not influenced 33 。
(2) Primary molding: mixing the raw materials of all the components, and then carrying out primary ball milling, drying and primary sintering to obtain pre-sintered piezoelectric ceramic powder; performing secondary ball milling and drying on the pre-sintered piezoelectric ceramic powder, adding a binder, grinding and granulating, performing extrusion forming, discharging glue, and performing secondary sintering to obtain piezoelectric ceramic;
(3) And (3) polarization treatment: soldering a layer of metallic tin on the upper surface and the lower surface of the preliminarily formed piezoelectric ceramic respectively, compacting, then performing magnetron sputtering on a layer of silver electrode, polarizing for 20-30 min in oil at the temperature of 75-85 ℃, and finally obtaining the high-corrosion-resistant composite piezoelectric ceramic material, wherein the polarizing electric field is 2500-4000V/mm.
The tin soldering layer of the metallic tin is used for effectively filling micro-pores on the surface of the preliminarily formed piezoelectric ceramic, so that the silver electrode subjected to magnetron sputtering is fully connected with the piezoelectric ceramic, and the contact resistance is reduced.
Preferably, x + y is 0.7 to 6 mol%.
Under the condition that the total doping amount is less than 0.7-6 mol%, the perovskite structure of BT ceramic is not changed, the simultaneously occurring lattice distortion increases the free energy, reduces the electric domain steering activation energy, and is more beneficial to the full deflection and retention of the electric domain during polarization treatment, thereby improving the piezoelectric constant d of the ceramic 33 Dielectric coefficient epsilon and electromechanical coupling coefficient Kp; if the doping amount is too large, grain boundary segregation occurs, and the crystal structure of the perovskite structure is changed, thereby affecting the piezoelectric performance of the ceramic.
Preferably, the time of the primary ball milling and the time of the secondary ball milling are respectively 12-14 h and 6-8 h, the rotating speed is 400-450 r/min, and the ball milling media are water and agate balls.
Preferably, the drying temperature is 70-80 ℃ and the drying time is 3-6 h.
Preferably, the primary sintering is carried out at the temperature rising rate of 80-90 ℃/h to 800-900 ℃ and the temperature is kept for 3-4 h.
Preferably, the binder is an aqueous solution of PVA at a concentration of 4 to 8 wt%.
Preferably, the pressure of the extrusion forming is 120-140 MPa.
Preferably, the temperature of the binder removal is increased to 450-500 ℃ at the heating rate of 40-50 ℃/h, and the temperature is kept for 50-60 min.
The binder removal is to remove the organic binder in the green body before the green body is fired so as to ensure the requirements of the shape, the size and the quality of the product; the heating rate should be controlled at 40-50 deg.C/h, and the slow heating rate is to ensure that the crystal structure is not damaged by deformation, cracks and other defects.
Preferably, the secondary sintering is carried out at the temperature rising rate of 105-115 ℃/h to 1200-1300 ℃, and the temperature is kept for 110-130 min.
The excessive high temperature rise rate is not beneficial to the elimination of pores during the sintering of the ceramic, and further the compactness is influenced, and the slow temperature rise rate of 80-90 ℃/h can effectively avoid the cracking problem and the breakdown problem caused by the polarization treatment in the sintering process.
The invention also provides the high-corrosion-resistance composite piezoelectric ceramic material prepared by the method.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention adopts Mg 2+ For Ba 2+ Equivalent replacement is carried out to improve the piezoelectric constant d of BT-based ceramic 33 While using the same amount of Sb 5+ And In 3+ Replacement of Ti 4+ Realizes the combination of hardness and hardness, and ensures the piezoelectric constant d 33 Can not be excessively reduced, the mechanical quality factor Qm and the electromechanical coupling coefficient Kp of the composite piezoelectric ceramic are improved, and the mechanical quality factor Qm low caused by doping high-valence ions and the piezoelectric constant d caused by doping low-valence ions in the prior art are improved 33 Low and poor aging stability.
(2) In the prior art, the electrode prepared by a magnetron sputtering method alone can only be deposited on the surface of ceramic but cannot go deep into micropores, the problem of point contact or surface contact among silver particles is caused by a conductive silver paste coating method, and both the silver particles and the piezoelectric ceramic generate contact resistance.
(3) According to the invention, the piezoelectric ceramic is prepared by two-step slow heating mode of glue discharging and secondary sintering, so that organic matters and air holes can be effectively removed, and the density of the piezoelectric ceramic is improved. Meanwhile, the high hardness and the hydrophobicity of the piezoelectric ceramic are improved due to the compact combination of the multi-component raw materials, and the corrosion problem caused by the absorption of acid and alkali liquor is avoided.
(4) BaCO used in the invention 3 、TiO 2 The materials such as MgO and the like have wide sources and are economical, the preparation method of the invention is simple and mild, and the prepared composite piezoelectric ceramic material has uniform performance.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
The invention provides a preparation method of a high-corrosion-resistance composite piezoelectric ceramic material, which comprises the following steps:
(1) Weighing the following components: mixing the raw material BaCO 3 、TiO 2 、MgO、Sb 2 O 5 And In 2 O 3 In stoichiometric ratio of Ba 1-x Mg x Ti 1- 2y Sb y In y O 3 Weighing; wherein x is 0.5 mol% and y is 0.2 mol%;
(2) Primary molding: mixing the raw materials of all the components, and then carrying out primary ball milling, drying and primary sintering to obtain pre-sintered piezoelectric ceramic powder; performing secondary ball milling and drying on the pre-sintered piezoelectric ceramic powder, adding a binder, grinding and granulating, performing extrusion forming, discharging glue, and performing secondary sintering to obtain piezoelectric ceramic;
(3) And (3) polarization treatment: soldering a layer of metallic tin on the upper surface and the lower surface of the preliminarily formed piezoelectric ceramic respectively, compacting, performing magnetron sputtering on a layer of silver electrode, polarizing in oil at 75 ℃ for 20 min, wherein the polarization electric field is 2500V/mm, and finally obtaining the high-corrosion-resistance composite piezoelectric ceramic material.
Wherein said x + y is 0.7 mol%; the time of the primary ball milling and the time of the secondary ball milling are respectively 12 hours and 6 hours, the rotating speed is 400 r/min, and the ball milling media are water and agate balls; the drying temperature is 70 ℃, and the drying time is 3 hours; the primary sintering is carried out by heating to 800 ℃ at a heating rate of 80 ℃/h and preserving heat for 3 h; the adhesive is PVA aqueous solution with the concentration of 4 wt%; the pressure intensity of the extrusion forming is 120 Mpa; the temperature of the binder removal is increased to 450 ℃ at the heating rate of 40 ℃/h, and the temperature is kept for 50 min; the secondary sintering is carried out by heating to 1200 ℃ at a heating rate of 105 ℃/h and keeping the temperature for 110 min.
The invention also provides the high-corrosion-resistance composite piezoelectric ceramic material prepared by the method.
Example two
The invention provides a preparation method of a high-corrosion-resistant composite piezoelectric ceramic material, which comprises the following steps:
(1) Weighing the components: mixing the raw material BaCO 3 、TiO 2 、MgO、Sb 2 O 5 And In 2 O 3 In stoichiometric ratio of Ba 1-x Mg x Ti 1- 2y Sb y In y O 3 Weighing; wherein x is 3 mol% and y is 3 mol%;
(2) Primary molding: mixing the raw materials of all the components, and then carrying out primary ball milling, drying and primary sintering to obtain pre-sintered piezoelectric ceramic powder; carrying out secondary ball milling and drying on the pre-sintered piezoelectric ceramic powder, adding a binder, grinding and granulating, carrying out extrusion forming, discharging the glue, and carrying out secondary sintering to obtain piezoelectric ceramic;
(3) And (3) polarization treatment: soldering a layer of metallic tin on the upper surface and the lower surface of the preliminarily formed piezoelectric ceramic respectively, compacting, carrying out magnetron sputtering on a layer of silver electrode, and polarizing in oil at 85 ℃ for 30 min, wherein the polarizing electric field is 4000V/mm, thereby finally obtaining the high-corrosion-resistance composite piezoelectric ceramic material.
Wherein said x + y is 6 mol%; the time of the primary ball milling and the time of the secondary ball milling are respectively 14h and 8h, the rotating speed is 450r/min, and the ball milling media are water and agate balls; the drying temperature is 80 ℃ and the drying time is 6 hours; the primary sintering is carried out by heating to 900 ℃ at the heating rate of 90 ℃/h and preserving heat for 4 h; the adhesive is PVA aqueous solution with the concentration of 8 wt%; the pressure intensity of the extrusion forming is 140 Mpa; the temperature of the binder removal is raised to 500 ℃ at the heating rate of 50 ℃/h, and the temperature is kept for 60 min; the secondary sintering is carried out by heating to 1300 ℃ at the heating rate of 115 ℃/h and preserving the heat for 130 min.
The invention also provides the composite piezoelectric ceramic material with high corrosion resistance, which is prepared by the method.
EXAMPLE III
The invention provides a preparation method of a high-corrosion-resistance composite piezoelectric ceramic material, which comprises the following steps:
(1) Weighing the following components: the raw material BaCO is mixed 3 、TiO 2 、MgO、Sb 2 O 5 And In 2 O 3 In stoichiometric ratio Ba 1-x Mg x Ti 1- 2y Sb y In y O 3 Weighing; wherein x is 2 mol% and y is 1 mol%;
(2) Primary molding: mixing the raw materials of all the components, and then carrying out primary ball milling, drying and primary sintering to obtain pre-sintered piezoelectric ceramic powder; performing secondary ball milling and drying on the pre-sintered piezoelectric ceramic powder, adding a binder, grinding and granulating, performing extrusion forming, discharging glue, and performing secondary sintering to obtain piezoelectric ceramic;
(3) And (3) polarization treatment: soldering a layer of metallic tin on the upper surface and the lower surface of the preliminarily formed piezoelectric ceramic respectively, compacting, carrying out magnetron sputtering on a layer of silver electrode, polarizing for 25 min in oil at 80 ℃, and obtaining the high-corrosion-resistance composite piezoelectric ceramic material with a polarizing electric field of 3000V/mm.
Wherein said x + y is 3 mol%; the time of the primary ball milling and the time of the secondary ball milling are respectively 13 h and 7 h, the rotating speed is 420 r/min, and the ball milling media are water and agate balls; the drying temperature is 75 ℃, and the drying time is 4 hours; the primary sintering is carried out at the temperature rise rate of 85 ℃/h to 850 ℃, and the temperature is kept for 3.5 h; the adhesive is a PVA aqueous solution with the concentration of 6 wt%; the pressure intensity of the extrusion forming is 130 Mpa; the temperature of the discharged glue is increased to 480 ℃ at the heating rate of 45 ℃/h, and the heat is preserved for 55 min; the secondary sintering is carried out by heating to 1250 ℃ at the heating rate of 110 ℃/h and preserving the heat for 120 min.
The invention also provides the composite piezoelectric ceramic material with high corrosion resistance, which is prepared by the method.
In order to detect the performance of each composite piezoelectric ceramic material, the invention respectively tests the piezoelectric constant d of each composite piezoelectric ceramic material 33 Dielectric coefficient epsilon, electromechanical coupling coefficient Kp and mechanical quality factor Qm. Cutting the prepared composite piezoelectric ceramic material into a rectangle with the size of 10 mm multiplied by 2 mm multiplied by 1 mm, determining the frequency dependence of the impedance of the ceramic sample by using an impedance analyzer, and calculating the piezoelectric constant d according to the observed resonance frequency and the antiresonance frequency 33 Dielectric coefficient epsilon, and mechanical quality factor Qm. Piezoelectric constant d 33 The larger the piezoelectric performance, the larger the mechanical quality factor Qm, and the smaller the loss of the ceramic at the time of resonance vibration. The composite piezoelectric ceramic is cut into a wafer with the diameter of 10 mm and the thickness of 2 mm, and then a dielectric temperature spectrometer is used for automatically measuring the dielectric coefficient epsilon of the material.
Through comparative experiments on the three groups of examples, the composite piezoelectric ceramic material with excellent performance and high corrosion resistance can be prepared by each group of examples. Wherein, the piezoelectric constant d of the composite piezoelectric ceramic material with high corrosion resistance prepared in the first embodiment 33 389 pC/N, dielectric coefficient epsilon 2487, electromechanical coupling coefficient Kp 41%, mechanical quality factor Qm 334; piezoelectric constant d of the high corrosion resistant composite piezoelectric ceramic material prepared in example two 33 393 pC/N, a dielectric coefficient ε of 2271, an electromechanical coupling coefficient Kp of 39%, and a mechanical quality factor Qm of 312; piezoelectric constant d of the high corrosion resistant composite piezoelectric ceramic material prepared in example three 33 410 pC/N, a dielectric coefficient ε of 2418, an electromechanical coupling coefficient Kp of 38%, and a mechanical quality factor Qm of 326. It can be seen that the piezoelectric constant d of the high corrosion resistant composite piezoelectric ceramic material prepared by the invention 33 HoldingThe mechanical quality factor Qm can reach 310 at the same time of over 380 pC/N, wherein the three effects of the embodiment are the best.
Comparative example 1: the difference from the third embodiment is that only Mg is doped 2+ To Ba 2+ Equivalent replacement is carried out to obtain the piezoelectric constant d of the composite piezoelectric ceramic material 33 381 pC/N, a dielectric coefficient ε of 1893, an electromechanical coupling coefficient Kp of 32%, and a mechanical quality factor Qm of 117. The piezoelectric constant d of the BT-based ceramic can be further improved by only carrying out small-amount doping of equivalent ions 33 However, the ceramic crystal structure lacking soft or hard substitution is almost unchanged, and the compactness of the ceramic basically keeps the characteristics of the original BT-based ceramic, so that the mechanical quality factor Qm is lower.
Comparative example 2: the difference from the third example is the absence of the higher valence ions Sb 5+ For Ti 4+ Soft substitution of (2), and the piezoelectric constant d of the obtained composite piezoelectric ceramic material 33 235 pC/N, a dielectric coefficient ε of 1698, an electromechanical coupling coefficient Kp of 31%, and a mechanical quality factor Qm of 337. The lack of high valence ion pairs Ti can be seen 4+ The replaced composite piezoelectric ceramic material contains Mg 2+ Doping to raise the piezoelectric constant d 33 But a piezoelectric constant d after soft substitution by high valence ions 33 And again decreases, only increasing the mechanical quality factor Qm.
Comparative example 3: the difference from the third example is the lack of In as low-valent ion 3+ For Ti 4+ Hard substitution of (A), the piezoelectric constant d of the obtained composite piezoelectric ceramic material 33 414 pC/N, a dielectric coefficient ε of 2474, an electromechanical coupling coefficient Kp of 38%, and a mechanical quality factor Qm of 109. The doping of equivalent ions and high valence ions can influence the piezoelectric constant d of the composite piezoelectric ceramic 33 But the mechanical quality factor Qm of the ceramic material after softening is reduced, and the improvement effect is not substantial.
Comparative example 4: the difference from example three is that x + y is 20 mol%, and the piezoelectric constant d of the resulting composite piezoelectric ceramic material 33 186 pC/N, dielectric coefficient ε 934, electromechanical coupling coefficient Kp 26%, and mechanical quality factor Qm 53. Appropriate amount of equivalent ion extractionThe substitution, soft substitution or hard substitution can be modified on the basis of not changing the perovskite crystal structure, and once the impurity-excessive crystal structure is damaged, the piezoelectric performance of the BT-based ceramic is reduced or even disappears.
Comparative example 5: the difference from the third embodiment lies in that the piezoelectric constant d of the composite piezoelectric ceramic material prepared by using the conductive silver paste coating mode to prepare the electrode 33 402 pC/N, a dielectric coefficient ε of 2359, an electromechanical coupling coefficient Kp of 32%, and a mechanical quality factor Qm of 287. Since insufficient connection between the electrode and the composite piezoelectric ceramic results in excessive contact resistance, insufficient polarization in a partial region during polarization treatment, and reduced polarization uniformity, the electromechanical coupling coefficient Kp and the mechanical quality factor Qm are both reduced.
Comparative example 6: the difference from the third embodiment is that the temperature rise rate of the secondary sintering is 200 ℃/h, and the piezoelectric constant d of the prepared composite piezoelectric ceramic material 33 376 pC/N, a dielectric coefficient ε of 2127, an electromechanical coupling coefficient Kp of 33%, and a mechanical quality factor Qm of 265. Because the temperature rise rate is too fast, pores in the ceramic in the sintering process cannot be effectively eliminated, the compactness is greatly reduced, and the mechanical quality factor is reduced.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (1)
1. A preparation method of a high corrosion resistant composite piezoelectric ceramic material is characterized by comprising the following steps: the method comprises the following steps:
(1) Weighing the following components: mixing the raw material BaCO 3 、TiO 2 、MgO、Sb 2 O 5 And In 2 O 3， In stoichiometric ratio Ba 1-x MgxTi 1- 2y Sb y In y O 3 Weighing; wherein x is 3 mol% and y is 3 mol%;
(2) Primary molding: mixing the raw materials of all the components, and then carrying out primary ball milling, drying and primary sintering to obtain pre-sintered piezoelectric ceramic powder; carrying out secondary ball milling and drying on the pre-sintered piezoelectric ceramic powder, adding a binder, grinding and granulating, carrying out extrusion forming, discharging the glue, and carrying out secondary sintering to obtain piezoelectric ceramic;
(3) And (3) polarization treatment: soldering a layer of metallic tin on the upper surface and the lower surface of the preliminarily formed piezoelectric ceramic respectively, compacting, performing magnetron sputtering on a layer of silver electrode, polarizing in oil at 85 ℃ for 30 min, wherein the polarization electric field is 4000V/mm, and finally obtaining the high-corrosion-resistance composite piezoelectric ceramic material;
the time of the primary ball milling and the time of the secondary ball milling are 14h and 8h respectively, the rotating speed is 450r/min, and the ball milling media are water and agate balls; the drying temperature is 80 ℃ and the drying time is 6 hours; the primary sintering is carried out by heating to 900 ℃ at the heating rate of 90 ℃/h and preserving heat for 4 h; the adhesive is PVA aqueous solution with the concentration of 8 wt%; the pressure intensity of the extrusion forming is 140 MPa; the temperature of the binder removal is increased to 500 ℃ at the heating rate of 50 ℃/h, and the temperature is kept for 60 min; the secondary sintering is carried out by heating to 1300 ℃ at the heating rate of 115 ℃/h and keeping the temperature for 130 min.
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