CN117164357A - Five-element high-power piezoelectric ceramic material and preparation method thereof - Google Patents
Five-element high-power piezoelectric ceramic material and preparation method thereof Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 239000011572 manganese Substances 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 27
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 claims abstract description 14
- JIYIUPFAJUGHNL-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] JIYIUPFAJUGHNL-UHFFFAOYSA-N 0.000 claims abstract description 14
- KOPBYBDAPCDYFK-UHFFFAOYSA-N caesium oxide Chemical compound [O-2].[Cs+].[Cs+] KOPBYBDAPCDYFK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910001942 caesium oxide Inorganic materials 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 11
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 84
- 239000000919 ceramic Substances 0.000 claims description 79
- 238000000498 ball milling Methods 0.000 claims description 42
- 238000002156 mixing Methods 0.000 claims description 35
- 239000002245 particle Substances 0.000 claims description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 239000002994 raw material Substances 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 24
- 238000005245 sintering Methods 0.000 claims description 21
- 238000005303 weighing Methods 0.000 claims description 21
- 239000011777 magnesium Substances 0.000 claims description 19
- 238000001354 calcination Methods 0.000 claims description 17
- 238000000227 grinding Methods 0.000 claims description 12
- FFQALBCXGPYQGT-UHFFFAOYSA-N 2,4-difluoro-5-(trifluoromethyl)aniline Chemical compound NC1=CC(C(F)(F)F)=C(F)C=C1F FFQALBCXGPYQGT-UHFFFAOYSA-N 0.000 claims description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- ZBSCCQXBYNSKPV-UHFFFAOYSA-N oxolead;oxomagnesium;2,4,5-trioxa-1$l^{5},3$l^{5}-diniobabicyclo[1.1.1]pentane 1,3-dioxide Chemical compound [Mg]=O.[Pb]=O.[Pb]=O.[Pb]=O.O1[Nb]2(=O)O[Nb]1(=O)O2 ZBSCCQXBYNSKPV-UHFFFAOYSA-N 0.000 claims description 9
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 claims description 8
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 239000003921 oil Substances 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 229910052709 silver Inorganic materials 0.000 claims description 6
- 239000004332 silver Substances 0.000 claims description 6
- ACNRWWUEFJNUDD-UHFFFAOYSA-N lead(2+);distiborate Chemical compound [Pb+2].[Pb+2].[Pb+2].[O-][Sb]([O-])([O-])=O.[O-][Sb]([O-])([O-])=O ACNRWWUEFJNUDD-UHFFFAOYSA-N 0.000 claims description 5
- 229910002056 binary alloy Inorganic materials 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000010955 niobium Substances 0.000 claims 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims 2
- 239000011787 zinc oxide Substances 0.000 claims 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims 1
- 229910052758 niobium Inorganic materials 0.000 claims 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 11
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- 238000010168 coupling process Methods 0.000 description 6
- 238000005859 coupling reaction Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 239000011701 zinc Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 1
- 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
- 230000000630 rising effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000026683 transduction Effects 0.000 description 1
- 238000010361 transduction Methods 0.000 description 1
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Abstract
The invention relates to a five-element high-power piezoelectric ceramic material and a preparation method thereof, wherein Pb is used as the piezoelectric ceramic material 1‑ x Sr x (Mn 1/3 Sb 2/3 ) y (Mg 1/3 Nb 2/3 )z(Nb 0.5 Sb 0.5 ) m1 Zr 0.5 Ti 0.5 O 3 The piezoelectric ceramic material is prepared by adding a manganese-zinc-doped ferrite material and cesium oxide as basic formulas, and the general chemical formula of the piezoelectric ceramic material is as follows: pb 1 x Sr x (Mn 1/3 Sb 2/3 ) y (Mg 1/3 Nb 2/3 ) Z (Nb 0.5 Sb 0.5 ) m1 Zr 0.5 Ti 0.5 O 3 +m2 manganese zinc ferrite material+m3 cesium oxide. The five-element high-power piezoelectric ceramic material has high quality factors (Qm), kp and d33, and the high Qm is not at the cost of reducing kp and d33.
Description
Technical Field
The invention relates to the technical field of piezoelectric ceramic materials, in particular to a five-element high-power piezoelectric ceramic material and a preparation method thereof.
Background
In recent years, high-power transducer devices and piezoelectric materials have taken an increasing importance in the industrial and scientific fields, and are widely used in sensors, drivers, transformers, various types of underwater acoustic, electroacoustic and ultrasonic transducers, and the like. In the age of rapid development of technology and industry in China at present, some key formulas and production process technologies for lead zirconate titanate-based piezoelectric ceramic materials which are applied on a large scale are still monopolized abroad, so that the cost for applying the piezoelectric ceramic materials in various fields in China is extremely high and is limited by people.
Most piezoelectric ceramics are difficult to realize practical application in the field of high-power transduction (P8 material series) devices, and are mainly expressed in the following aspects: first, the mechanical quality factor Qm (the mechanical quality factor Qm is as high as possible, usually more than 1300), the electromechanical coupling coefficient kp, the dielectric loss tan δ, and the piezoelectric constant d33 (the piezoelectric constant d33 is as high as possible, usually more than 300 pC/N), the fatigue resistance, and other key performance parameters are required, but it is sometimes difficult to achieve both high mechanical quality factor Qm and high piezoelectric constant d33 at the same time, for example, the high Qm is obtained at the cost of lowering kp and d33.
Disclosure of Invention
In order to overcome the above problems in the prior art, a first object of the present invention is to provide a five-membered high-power piezoelectric ceramic material, which uses Pb 1-x Sr x (Mn 1/3 Sb 2/3 ) y (Mg 1/3 Nb 2/3 )z(Nb 0.5 Sb 0.5 ) m1 Zr 0.5 Ti 0.5 O 3 The piezoelectric ceramic material is prepared by adding a manganese-zinc-doped ferrite material and cesium oxide as basic formulas, and the general chemical formula of the piezoelectric ceramic material is as follows: pb 1-x Sr x (Mn 1/3 Sb 2/3 ) y (Mg 1/3 Nb 2/3 ) Z (Nb 0.5 Sb 0.5 ) m1 Zr 0.5 Ti 0.5 O 3 A manganese zinc ferrite material +m2+m3 cesium oxide, wherein x=0.04-0.12, y=0.2, z=0.2, m1=0.02, m2=0.1-1.5%, m3=0.02-0.5%.
Compared with the prior art, the invention has the beneficial effects that: the five-element high-power piezoelectric ceramic material has good comprehensive performance parameters, and the quality factor (Qm) of the whole product is improved by introducing the Mn-Zn ferrite material, so that the quality factor of the material is improved. Meanwhile, the material improves the fatigue resistance of the product by introducing cesium oxide. In addition, the five-element high-power piezoelectric ceramic material has high quality factors (Qm), kp and d33, and the high Qm is not at the cost of reducing kp and d33.
The second aim of the invention is to provide a preparation method of a five-membered high-power piezoelectric ceramic material, which comprises the following steps:
s1, respectively weighing Pb according to stoichiometric ratio 3 O 4 、SrCO 3 、ZrO 2 、TiO 2 Mixing the above materials into a raw material mixture, ball-milling the mixture with alcohol or water as a medium for 6 hours to obtain a D50 particle size of 1-3 μm, drying wet powder, calcining at 1000-1100 ℃ for 2-4 hours, and repeating the ball-milling and drying to obtain Pb 1-x Sr x Zr 0.5 Ti 0.5 O 3 Piezoelectric ceramic powder of lead strontium zirconate titanate binary system;
s2, respectively weighing Pb according to stoichiometric ratio 3 O 4 、MnCO 3 、Sb 2 O 3 Mixing, preparing into raw material mixture, ball milling with alcohol or water as medium for 6 hr to obtain D50 particle size of 3-5 μm, drying wet powder, calcining at 800-900 deg.C for 2-4 hr, and repeating ball milling, mixing and drying to obtain Pb (Mn) 1/3 Sb 2/3 )O 3 Lead antimonite piezoelectric ceramic powder;
s3, respectively weighing Pb according to stoichiometric ratio 3 O 4 、MgO、Nb 2 O 5 Mixing, preparing into raw material mixture, ball milling with alcohol or water as medium to obtain D50 particle with particle size of 1-3 μm, drying wet powder, calcining at 1000-1060 deg.C for 2-4 hr, and repeating ball milling and drying to obtain Pb (Mg) 1/3 Nb 2/3 )O 3 Lead magnesium niobate piezoelectric ceramic powder;
s4, respectively weighing Pb according to stoichiometric ratio 3 O 4 、Sb 2 O 3 、Nb 2 O 5 Mixing, preparing into raw material mixture, ball milling with alcohol or water as medium to obtain D50 particle with particle size of 3-5 μm, drying wet powder, calcining at 800-900deg.C for 2-4 hr, and repeating ball milling and calcining to obtain Pb (Sb) 1/2 Nb 1/2 )O 3 Lead niobate piezoelectric ceramic powder;
s5, according to the stoichiometric ratio (the manganese zinc ferrite material is prepared from Fe 2 O 3 56～56.5％，Mn 3 O 4 41 to 42.5 percent and the balance of ZnO, and the total amount is 100 percent) respectively weighing Fe 2 O 3 、Mn 3 O 4 Mixing ZnO and alcohol to obtain mixed material, ball milling with alcohol or water as medium to obtain mixed material with D50 particle size of 1-2 microns, stoving wet powder, calcining at 900-1000 deg.c for 2-4 hr, and re-ball milling to obtain MnZnFe 2 O 4 Manganese zinc ferrite powder;
s6, respectively weighing Pb obtained in the step S1 according to stoichiometric ratio 1-x Sr x Zr 0.5 Ti 0.5 O 3 Lead strontium zirconate titanate piezoelectric ceramic powder and Pb (Mn) obtained in step S2 1/3 Sb 2/3 )O 3 Lead antimonate piezoelectric ceramic powder and Pb (Mg) obtained in step S3 1/ 3 Nb 2/3 )O 3 Lead magnesium niobate piezoelectric ceramic powder and Pb (Sb) obtained in step S4 1/2 Nb 1/2 )O 3 Lead niobate piezoelectric ceramic powder and MnZnFe obtained in step S5 2 O 4 Manganese zinc ferrite powder and cesium oxide are mixed to prepare a raw material mixture, then alcohol or water is used as a medium, ball milling and mixing are carried out for 12 hours, the D50 particle size of the mixture is 0.5-1.1 mu m, and the wet powder is baked at 1000-1060 ℃ and calcined for 2-4 hours, thus obtaining five-membered high-power piezoelectric ceramic powder;
s7, grinding the five-element high-power piezoelectric ceramic powder obtained in the step S6, then ball-milling for 10 hours by taking alcohol or water as a medium, grinding the powder to D90 with the particle size of 1.0-1.5 mu m, mixing the dried powder with a binder, granulating, and cold-pressing the powder under the pressure of 300-400MPa to form a wafer with the diameter of 10mm and the thickness of 0.6-1.0mm, thereby obtaining a ceramic blank; sintering the ceramic blank in a protective atmosphere by adopting a powder embedding method in air at normal pressure, wherein the sintering temperature is 1235 ℃, and the sintering time is 2 hours to obtain a piezoelectric ceramic sample;
and S8, coating silver electrodes on two ends of the piezoelectric ceramic sample prepared in the step S7 after polishing treatment, and then placing the piezoelectric ceramic sample in silicon oil at 110 ℃, and preserving heat and pressure for 30 minutes under a direct current field of 5kV/mm to obtain the quinary high-power piezoelectric ceramic.
Further, the temperature rising rate of the sintering temperature in the step S7 is 3-5 ℃/min. The slow heating rate of 3-5 ℃/min is beneficial to improving the quality factor of the material.
Compared with the prior art, the invention has the beneficial effects that:
the invention synthesizes Pb respectively 1-x Sr x Zr 0.5 Ti 0.5 O 3 Lead strontium zirconate titanate powder, pb (Mn) 1/3 Sb 2/3 )O 3 Lead antimonite powder, pb (Mg) 1/3 Nb 2/3 )O 3 Lead magnesium niobate powder, pb (Sb) 1/2 Nb 1/ 2)O 3 The lead niobate powder is further used to prepare five-element high-power piezoelectric ceramic material, and the lead niobate, the lead magnesium niobate and the lead antimonate are added into the binary system based on lead strontium zirconate titanate. This preparation method is relatively conventional in terms of Pb 3 O 4 、SrCO 3 、ZrO 2 、TiO 2 、MnCO 3 、Nb 2 O 5 And Sb (Sb) 2 O 3 The five-membered system substance is synthesized by mixing MgO and MgO, so that each component can be controlled more accurately, and no impurity phase is generated. The preparation method further ensures that the prepared five-element high-power piezoelectric ceramic material has high quality factors (Qm), kp and d33. In addition, the preparation method does not adopt high-cost modes such as hot-pressing sintering and the like, has low cost and is easier for mass production.
Detailed Description
The present invention will now be further described with reference to specific embodiments, it being apparent that some, but not all embodiments of the invention are described. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
A ferroelectric analyzer (TF 2000 analyzer, aixacct, aachen, ger many) is used for carrying out fatigue experiments and characterizing the electric hysteresis loop and field induced strain performance of a sample.
Pb used in the following examples of the invention 3 O 4 、SrCO 3 、ZrO 2 、TiO 2 、MnCO 3 、Sb 2 O 3 、MgO、Nb 2 O 5 、Fe 2 O 3 、Mn 3 O 4 The raw materials such as ZnO and the like are chemically pure or analytically pure. The piezoelectric ceramic provided by the embodiment of the invention is prepared according to the following method, and the difference is that x, y, z, m, m2 and m3 are different in value.
Five-element high-power piezoelectric ceramic material, which uses Pb 1-x Sr x (Mn 1/3 Sb 2/3 ) y (Mg 1/3 Nb 2/3 )z(Nb 0.5 Sb 0.5 ) m1 Zr 0.5 Ti 0.5 O 3 Is prepared by taking the basic formula, adding a doped Mn-Zn ferrite material and cesium oxideThe general chemical formula of the piezoelectric ceramic material is as follows: pb 1-x Sr x (Mn 1/3 Sb 2/3 ) y (Mg 1/3 Nb 2/3 ) Z (Nb 0.5 Sb 0.5 ) m1 Zr 0.5 Ti 0.5 O 3 A manganese zinc ferrite material +m2+m3 cesium oxide, wherein x=0.04-0.12, y=0.2, z=0.2, m1=0.02, m2=0.1-1.5%, m3=0.02-0.5%. The preparation method of the five-membered high-power piezoelectric ceramic material comprises the following steps:
s1, respectively weighing Pb according to stoichiometric ratio 3 O 4 、SrCO 3 、ZrO 2 、TiO 2 Mixing the above materials into a raw material mixture, ball-milling the mixture with alcohol or water as a medium for 6 hours to obtain a D50 particle size of 1-3 μm, drying wet powder, calcining at 1000-1100 ℃ for 2-4 hours, and repeating the ball-milling and drying to obtain Pb 1-x Sr x Zr 0.5 Ti 0.5 O 3 Piezoelectric ceramics of lead strontium zirconate titanate binary system;
s2, respectively weighing Pb according to stoichiometric ratio 3 O 4 、MnCO 3 、Sb 2 O 3 Mixing, preparing into raw material mixture, ball milling with alcohol or water as medium for 6 hr to obtain D50 particle size of 3-5 μm, drying wet powder, calcining at 800-900 deg.C for 2-4 hr, and repeating ball milling and drying to obtain Pb (Mn) 1/3 Sb 2/3 )O 3 Lead antimonate piezoelectric ceramics;
s3, respectively weighing Pb according to stoichiometric ratio 3 O 4 、MgO、Nb 2 O 5 Mixing, preparing into raw material mixture, ball milling with alcohol or water as medium to obtain D50 particle with particle size of 3-5 μm, drying wet powder, calcining at 1000-1060 deg.C for 2-4 hr, and repeating ball milling and drying to obtain Pb (Mg) 1/3 Nb 2/3 )O 3 Lead magnesium niobate piezoelectric ceramics;
s4, respectively weighing Pb according to stoichiometric ratio 3 O 4 、Sb 2 O 3 、Nb 2 O 5 Mixing, preparing into raw material mixture, using alcohol or water as medium,ball milling and mixing to obtain D50 particle size of 3-5 μm, drying wet powder, calcining at 800-900 deg.C for 2-4 hr, and repeating ball milling and mixing and drying to obtain Pb (Sb) 1/2 Nb 1/2 )O 3 Lead niobate piezoelectric ceramics;
s5, according to the stoichiometric ratio (the manganese zinc ferrite material is prepared from Fe 2 O 3 56～56.5％，Mn 3 O 4 41 to 42.5 percent and the balance of ZnO, and the total amount is 100 percent) respectively weighing Fe 2 O 3 、Mn 3 O 4 Mixing ZnO and alcohol to obtain mixed material, ball milling with alcohol or water as medium to obtain mixed material with D50 particle size of 1-2 microns, stoving wet powder, calcining at 900-1000 deg.c for 2-4 hr, ball milling, mixing and stoving to obtain MnZnFe 2 O 4 Manganese zinc ferrite;
s6, respectively weighing Pb obtained in the step S1 according to stoichiometric ratio 1-x Sr x Zr 0.5 Ti 0.5 O 3 Lead strontium zirconate titanate piezoelectric ceramic, pb (Mn) obtained in step S2 1/3 Sb 2/3 )O 3 Lead antimonate piezoelectric ceramic and Pb (Mg) obtained in step S3 1/3 Nb 2/3 )O 3 Lead magnesium niobate piezoelectric ceramic, and Pb (Sb) obtained in step S4 1/2 Nb 1/2 )O 3 Lead niobate piezoelectric ceramic and MnZnFe obtained in step S5 2 O 4 Mixing manganese zinc ferrite and cesium oxide to prepare a raw material mixture, ball-milling and mixing the raw material mixture for 12 hours by taking alcohol or water as a medium to ensure that the D50 particle size of the raw material mixture is 0.5-1.1 mu m, drying wet powder, and calcining the wet powder at 1000-1060 ℃ for 2-4 hours to obtain five-membered high-power piezoelectric ceramic powder;
s7, grinding the five-element high-power piezoelectric ceramic powder obtained in the step S6, then ball-milling for 10 hours by taking alcohol or water as a medium, grinding the powder to D90 with the particle size of 1.0-1.5 mu m, mixing the dried powder with a binder, granulating, and cold-pressing the powder into a wafer with the diameter of 10mm and the thickness of 0.6-1.0mm under the pressure of 300-400MPa to obtain a ceramic blank; sintering the ceramic blank in a protective atmosphere by adopting a powder embedding method in air at normal pressure, wherein the sintering temperature is 1235 ℃, the heating rate is 3-5 ℃/min, and the sintering time is 2 hours, so that a piezoelectric ceramic sample is obtained;
and S8, coating silver electrodes on two ends of the piezoelectric ceramic sample prepared in the step S7 after polishing treatment, and then placing the piezoelectric ceramic sample in silicon oil at 110 ℃, and preserving heat and pressure for 30 minutes under a direct current field of 5kV/mm to obtain the quinary high-power piezoelectric ceramic.
The preparation methods employed in comparative examples 1 to 3 are conventional preparation methods, which are specifically as follows:
comparative example 1:
s1, pb in the chemical formula 1-x Sr x (Mn 1/3 Sb 2/3 ) y (Mg 1/3 Nb 2/3 ) Z (Nb 0.5 Sb 0.5 ) m1 Zr 0.5 Ti 0.5 O 3 (where x=0.04, y=0.20, z=0.20, m1=0.02) accurate weighing, pb 3 O 4 、SrCO 3 、ZrO 2 、TiO 2、 MnCO 3 、Sb 2 O 3 、MgO、Nb 2 O 5 The raw materials are chemical pure or analytically pure, the raw materials are mixed to prepare raw material mixture, alcohol or water is used as medium, ball milling and mixing are carried out, D50 particle size is 3-5 mu m, wet powder is baked and calcined at 1000-1060 ℃ for 2-4 hours, pb is obtained 1-x Sr x (Mn 1/3 Sb 2/3 ) y (Mg 1/3 Nb 2/3 ) Z (Nb 0.5 Sb 0.5 ) m1 Zr 0.5 Ti 0.5 O 3 Piezoelectric ceramic powder;
s2, grinding the five-element high-power piezoelectric ceramic powder obtained in the step S1 of the comparative example 1, then ball-milling for 10 hours by taking alcohol or water as a medium, grinding the powder to obtain powder with the D90 particle size of 1.0-1.5 mu m, mixing the dried powder with a binder, granulating, and cold-pressing the powder into a wafer with the diameter of 10mm and the thickness of 0.6-1.0mm under the pressure of 300-400MPa to obtain a ceramic blank; sintering the ceramic blank in a protective atmosphere by adopting a powder embedding method in air at normal pressure, wherein the sintering temperature is 1235 ℃, the heating rate is 3-5 ℃/min, and the sintering time is 2 hours, so that a piezoelectric ceramic sample is obtained;
and S3, coating silver electrodes on two ends of the piezoelectric ceramic sample prepared in the step S2 of the comparative example 1 after polishing treatment, and then placing the piezoelectric ceramic sample in silicon oil at 110 ℃, and preserving heat and pressure for 30 minutes under a direct current electric field of 5kV/mm to obtain the five-membered high-power piezoelectric ceramic.
Comparative example 2:
s1, pb in the chemical formula 1-x Sr x (Mn 1/3 Sb 2/3 ) y (Mg 1/3 Nb 2/3 ) Z (Nb 0.5 Sb 0.5 ) m1 Zr 0.5 Ti 0.5 O 3 (where x=0.08, y=0.20, z=0.20, m1=0.02) accurate weighing, pb 3 O 4 、SrCO 3 、ZrO 2 、TiO 2 、MnCO 3 、Sb 2 O 3 、MgO、Nb 2 O 5 The raw materials are chemical pure or analytically pure, the raw materials are mixed to prepare raw material mixture, alcohol or water is used as medium, ball milling and mixing are carried out, D50 particle size is 3-5 mu m, wet powder is baked and calcined at 1000-1060 ℃ for 2-4 hours, pb is obtained 1-x Sr x (Mn 1/3 Sb 2/3 ) y (Mg 1/3 Nb 2/3 ) Z (Nb 0.5 Sb 0.5 ) m1 Zr 0.5 Ti 0.5 O 3 Piezoelectric ceramic powder;
s2, grinding the five-element high-power piezoelectric ceramic powder obtained in the step S1 of the comparative example 2, then ball-milling for 10 hours by taking alcohol or water as a medium, grinding the powder to obtain powder with the D90 particle size of 1.0-1.5 mu m, mixing the dried powder with a binder, granulating, and cold-pressing the powder into a wafer with the diameter of 10mm and the thickness of 0.6-1.0mm under the pressure of 300-400MPa to obtain a ceramic blank; sintering the ceramic blank in a protective atmosphere by adopting a powder embedding method in air at normal pressure, wherein the sintering temperature is 1235 ℃, the heating rate is 3-5 ℃/min, and the sintering time is 2 hours, so that a piezoelectric ceramic sample is obtained;
and S3, coating silver electrodes on two ends of the piezoelectric ceramic sample prepared in the step S2 of the comparative example 2 after polishing treatment, and then placing the piezoelectric ceramic sample in silicon oil at 110 ℃, and preserving heat and pressure for 30 minutes under a direct current electric field of 5kV/mm to obtain the five-membered high-power piezoelectric ceramic.
Comparative example 3:
s1, pb in the chemical formula 1-x Sr x (Mn 1/3 Sb 2/3 ) y (Mg 1/3 Nb 2/3 ) Z (Nb 0.5 Sb 0.5 ) m1 Zr 0.5 Ti 0.5 O 3 (where x=0.12, y=0.20, z=0.20, m1=0.02) accurate weighing, pb 3 O 4 、SrCO 3 、ZrO 2 、TiO 2 、MnCO 3 、Sb 2 O 3 、MgO、Nb 2 O 5 The raw materials are chemical pure or analytically pure, the raw materials are mixed to prepare raw material mixture, alcohol or water is used as medium, ball milling and mixing are carried out, D50 particle size is 3-5 mu m, wet powder is baked and calcined at 1000-1060 ℃ for 2-4 hours, pb is obtained 1-x Sr x (Mn 1/3 Sb 2/3 ) y (Mg 1/3 Nb 2/3 ) Z (Nb 0.5 Sb 0.5 ) m1 Zr 0.5 Ti 0.5 O 3 Piezoelectric ceramic powder;
s2, grinding the five-element high-power piezoelectric ceramic powder obtained in the step S1 of the comparative example 3, then ball-milling for 10 hours by taking alcohol or water as a medium, grinding the powder to obtain powder with the D90 particle size of 1.0-1.5 mu m, mixing the dried powder with a binder, granulating, and cold-pressing the powder into a wafer with the diameter of 10mm and the thickness of 0.6-1.0mm under the pressure of 300-400MPa to obtain a ceramic blank; sintering the ceramic blank in a protective atmosphere by adopting a powder embedding method in air at normal pressure, wherein the sintering temperature is 1235 ℃, the heating rate is 3-5 ℃/min, and the sintering time is 2 hours, so that a piezoelectric ceramic sample is obtained;
and S3, coating silver electrodes on two ends of the piezoelectric ceramic sample prepared in the step S2 of the comparative example 3 after polishing treatment, and then placing the piezoelectric ceramic sample in silicon oil at 110 ℃, and preserving heat and pressure for 30 minutes under a direct current electric field of 5kV/mm to obtain the five-membered high-power piezoelectric ceramic.
Examples, comparative examples and corresponding test data
As can be seen from comparison of the test data of examples 1-3, that is, when x is in the range of (0.04-0.12), the dielectric constant, the electromechanical coupling coefficient kp, d33 (pC/N) and the Q value all show increasing trend as x increases. When x=0.08, the dielectric constant, the electromechanical coupling coefficient kp, d33 (pC/N) reach the maximum value, and the performance is optimal. When x exceeds 0.08, the dielectric constant, the electromechanical coupling coefficient kp and the d33 (pC/N) Q value all show a decreasing trend as x increases.
As can be seen from comparison of the test data of examples 4-6, the Mn-Zn ferrite material doped with m2 can greatly improve the Q value. That is, M2 has a tendency that the Q value increases and decreases with an increase in M2 in the range of (m2=0.1 to 1.5%). Equivalent m2=0.8%, reaches maximum value, Q value reaches 1350, and performance is optimal.
As can be seen from comparison of the test data of examples 7-9, cesium oxide doped, the fatigue resistance (strain attenuation) is improved; as m3 increases, fatigue (strain decay) is resisted. When m3=0.3%, the fatigue resistance (strain attenuation) reaches a maximum value, and when the strain attenuation is further increased, the fatigue resistance is reduced.
As can be seen from the above examples and comparison of test data: the dielectric constant, the electromechanical coupling coefficient kp and the d33 (pC/N) compressive strength tan delta (%) all show parabolic trend change, and then the dielectric constant, the electromechanical coupling coefficient kp, the d33 (pC/N), the Qm and the fatigue resistance of the piezoelectric ceramic are improved by matching with the Mn-Zn ferrite material and cesium oxide, so that the stability of the product quality is finally improved.
The foregoing is a further detailed description of the invention in connection with the preferred embodiments, and it is not intended that the invention be limited to the specific embodiments described. It will be apparent to those skilled in the art that several simple deductions or substitutions may be made without departing from the spirit of the invention, and these should be considered to be within the scope of the invention.
Claims (6)
1. A five-element high-power piezoelectric ceramic material is characterized in that Pb is used as the piezoelectric ceramic material 1-x Sr x (Mn 1/ 3 Sb 2/3 ) y (Mg 1/3 Nb 2/3 )z(Nb 0.5 Sb 0.5 ) m1 Zr 0.5 Ti 0.5 O 3 The piezoelectric ceramic material is prepared by adding a manganese-zinc-doped ferrite material and cesium oxide as basic formulas, and the general chemical formula of the piezoelectric ceramic material is as follows: pb 1-x Sr x (Mn 1/3 Sb 2/3 ) y (Mg 1/3 Nb 2/3 ) Z (Nb 0.5 Sb 0.5 ) m1 Zr 0.5 Ti 0.5 O 3 A manganese zinc ferrite material +m2+m3 cesium oxide, wherein x=0.04-0.12, y=0.2, z=0.2, m1=0.02, m2=0.1-1.5%, m3=0.02-0.5%.
2. The five-membered high-power piezoelectric ceramic material according to claim 1, wherein: the five-membered high-power piezoelectric ceramic material comprises the following components: lead strontium zirconate titanate piezoelectric ceramic, lead manganese antimonate piezoelectric ceramic, lead magnesium niobate piezoelectric ceramic, lead niobium antimonate piezoelectric ceramic, manganese zinc ferrite and cesium oxide.
3. The five-membered high-power piezoelectric ceramic material according to claim 2, wherein: the manganese zinc ferrite comprises: iron oxide, manganese oxide and zinc oxide.
4. A method for preparing the five-membered high-power piezoelectric ceramic material according to claim 1, comprising the steps of:
s1, respectively weighing Pb according to stoichiometric ratio 3 O 4 、SrCO 3 、ZrO 2 、TiO 2 Mixing the above materials into a raw material mixture, ball-milling the mixture with alcohol or water as a medium for 6 hours to obtain a D50 particle size of 1-3 μm, drying wet powder, calcining at 1000-1100 ℃ for 2-4 hours, and repeating the ball-milling the mixture and drying to obtain Pb 1-x Sr x Zr 0.5 Ti 0.5 O 3 Piezoelectric ceramic powder of lead strontium zirconate titanate binary system;
s2, respectively weighing Pb according to stoichiometric ratio 3 O 4 、MnCO 3 、Sb 2 O 3 Mixing, preparing into raw material mixture, ball milling with alcohol or water as medium for 6 hr to obtain D50 particle size of 3-5 μm, drying wet powder, calcining at 800-900 deg.C for 2-4 hr, and repeating ball milling, mixing and drying to obtain Pb (Mn) 1/3 Sb 2/3 )O 3 Lead antimonite piezoelectric ceramic powder;
s3, respectively weighing Pb according to stoichiometric ratio 3 O 4 、MgO、Nb 2 O 5 Mixing, preparing into raw material mixture, ball milling with alcohol or water as medium to obtain D50 particle with particle size of 1-3 μm, drying wet powder, calcining at 1000-1060 deg.C for 2-4 hr, and repeating ball milling and drying to obtain Pb (Mg) 1/3 Nb 2/3 )O 3 Lead magnesium niobate piezoelectric ceramic powder;
s4, respectively weighing Pb according to stoichiometric ratio 3 O 4 、Sb 2 O 3 、Nb 2 O 5 Mixing, preparing into raw material mixture, ball milling with alcohol or water as medium to obtain D50 particle with particle size of 3-5 μm, drying wet powder, calcining at 800-900deg.C for 2-4 hr, and repeating ball milling and drying to obtain Pb (Sb) 1/2 Nb 1/2 )O 3 Lead niobate piezoelectric ceramic powder;
s5, respectively weighing Fe according to stoichiometric ratio 2 O 3 、Mn 3 O 4 Mixing ZnO and alcohol to obtain mixed material, ball milling with alcohol or water as medium to obtain mixed material with D50 particle size of 1-2 microns, stoving wet powder, calcining at 900-1000 deg.c for 2-4 hr, ball milling, mixing and stoving to obtain MnZnFe 2 O 4 Manganese zinc ferrite powder;
s6, respectively weighing Pb obtained in the step S1 according to stoichiometric ratio 1-x Sr x Zr 0.5 Ti 0.5 O 3 Lead strontium zirconate titanate piezoelectric ceramic powder and Pb (Mn) obtained in step S2 1/3 Sb 2/3 )O 3 Lead antimonate piezoelectric ceramic powder and Pb (Mg) obtained in step S3 1/3 Nb 2/3 )O 3 Lead magnesium niobate piezoelectric ceramic powder and Pb (Sb) obtained in step S4 1/2 Nb 1/2 )O 3 Lead niobate piezoelectric ceramic powder and MnZnFe obtained in step S5 2 O 4 Manganese zinc ferrite powder and cesium oxide are mixed to prepare a raw material mixture, then alcohol or water is used as a medium, ball milling and mixing are carried out for 12 hours, the D50 particle size of the mixture is 0.5-1.1 mu m, and the wet powder is baked at 1000-1060 ℃ and calcined for 2-4 hours, thus obtaining five-membered high-power piezoelectric ceramic powder;
s7, grinding the five-element high-power piezoelectric ceramic powder obtained in the step S6, then ball-milling for 10 hours by taking alcohol or water as a medium, grinding the powder to D90 with the particle size of 1.0-1.5 mu m, mixing the dried powder with a binder, granulating, and cold-pressing to form a wafer under the pressure of 300-400MPa to obtain a required ceramic blank; sintering the ceramic blank in a protective atmosphere by adopting a powder embedding method in air at normal pressure, wherein the sintering temperature is 1235 ℃, and the sintering time is 2 hours to obtain a piezoelectric ceramic sample;
and S8, coating silver electrodes on two ends of the piezoelectric ceramic sample prepared in the step S7 after polishing treatment, and then placing the piezoelectric ceramic sample in silicon oil at 110 ℃, and preserving heat and pressure for 30 minutes under a direct current field of 5kV/mm to obtain the quinary high-power piezoelectric ceramic.
5. The method for preparing a five-membered high-power piezoelectric ceramic material according to claim 2, wherein the diameter of the wafer in the step S7 is 10mm and the thickness thereof is 0.6-1.0mm.
6. The method for producing a five-membered high-power piezoelectric ceramic material according to claim 2, wherein the temperature rise rate of the sintering temperature in step S7 is 3 to 5 ℃/min.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6311521A (en) * | 1986-07-02 | 1988-01-19 | Natl Inst For Res In Inorg Mater | Production of ceramics powder capable of easily sintering for producing dielectric porcelain having high density |
| CN1803708A (en) * | 2006-01-19 | 2006-07-19 | 湖北大学 | Low temperature sintered PMMSN titanic acid piezoelectric ceramic material and preparation method thereof |
| JP2010177571A (en) * | 2009-01-30 | 2010-08-12 | Tokai Rubber Ind Ltd | Method of manufacturing dielectric material and dielectric film manufactured therefrom |
| JP2012009800A (en) * | 2010-05-24 | 2012-01-12 | Mitsubishi Materials Corp | Ferroelectric thin film and thin film capacitor using the same |
| IN2014DN00101A (en) * | 2011-06-06 | 2015-05-15 | Starpharma Pty Ltd |
-
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6311521A (en) * | 1986-07-02 | 1988-01-19 | Natl Inst For Res In Inorg Mater | Production of ceramics powder capable of easily sintering for producing dielectric porcelain having high density |
| CN1803708A (en) * | 2006-01-19 | 2006-07-19 | 湖北大学 | Low temperature sintered PMMSN titanic acid piezoelectric ceramic material and preparation method thereof |
| JP2010177571A (en) * | 2009-01-30 | 2010-08-12 | Tokai Rubber Ind Ltd | Method of manufacturing dielectric material and dielectric film manufactured therefrom |
| JP2012009800A (en) * | 2010-05-24 | 2012-01-12 | Mitsubishi Materials Corp | Ferroelectric thin film and thin film capacitor using the same |
| IN2014DN00101A (en) * | 2011-06-06 | 2015-05-15 | Starpharma Pty Ltd |
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