CN114591082A - 一种pzt-pnn-psn-pmn压电陶瓷及其制备方法 - Google Patents
一种pzt-pnn-psn-pmn压电陶瓷及其制备方法 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 75
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- 229910019653 Mg1/3Nb2/3 Inorganic materials 0.000 claims abstract description 12
- 238000000227 grinding Methods 0.000 claims description 25
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 21
- 229910052759 nickel Inorganic materials 0.000 claims description 21
- 239000011812 mixed powder Substances 0.000 claims description 16
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- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 10
- 238000007873 sieving Methods 0.000 claims description 9
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- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 claims description 5
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- 238000004364 calculation method Methods 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
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- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(II,IV) oxide Inorganic materials O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 description 4
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Abstract
本发明属于压电陶瓷技术领域,具体涉及一种PZT‑PNN‑PSN‑PMN压电陶瓷及其制备方法,其技术要点如下:陶瓷粉末的分子式为Pb0.92Sr0.08(Zr0.48Ti0.52)0.96‑x(Ni1/3Nb2/3)x(Sb1/2Nb1/2)0.03(Mg1/3Nb2/3)0.01O3,0.15<x<0.25。本发明提供的PZT‑PNN‑PSN‑PMN压电陶瓷及其制备方法,通过低熔沸点金属和高熔沸点金属的掺杂量对预烧结和烧结过程中的升温速率和保温时间进行精确计算和控制,在避免低熔沸点金属挥发逸出的情况下,保证了晶粒尺寸的均匀性,提高了由于Ni的掺杂降低的体积密度,有效提高三元压电陶瓷的介电常数和压电常数。
Description
技术领域
本发明属于压电陶瓷技术领域,具体涉及一种PZT-PNN-PSN-PMN压电陶瓷及其制备方法。
背景技术
压电陶瓷具有良好的机械能和电能转换能力,广泛应用于超声传感、压电致动器、压电变电器等各个领域。随着电子器件的微型化、智能化发展,对压电陶瓷的性能提出了越来越高的要求,如高压电常数、高介电常数和高机电耦合系数等。为了满足上述要求,压电制动器和压电泵等电器通常采用叠层结构,然而叠层对压电陶瓷的压电常数和介电常数的要求更高。
现有技术中通常采用三元甚至四元压电陶瓷,虽然提高了压电陶瓷的压电常数,但是过多种类的金属掺杂,容易造成晶体缺陷或体积密度下降等问题,严重制约了三元或四元压电陶瓷的推广和应用。
有鉴于上述现有压电陶瓷存在的缺陷,本发明人基于从事此类材料多年丰富经验及专业知识,配合理论分析,加以研究创新,开发出一种PZT-PNN-PSN-PMN压电陶瓷及其制备方法。
发明内容
本发明的第一个目的是提供一种PZT-PNN-PSN-PMN压电陶瓷,通过在B位引入Ni的掺杂,使钙钛矿结构中出现三方相,形成三方相和四方相在准同形相界共存,形成三方相和四方相的耦合,提高了准同形相界的极化率,进而大幅提高了三元压电陶瓷的压电常数和介电常数。
本发明的上述技术目的是通过以下技术方案得以实现的:
本发明提供的PZT-PNN-PSN-PMN压电陶瓷,陶瓷粉末的分子式为Pb0.92Sr0.08(Zr0.48Ti0.52)0.96-x(Ni1/3Nb2/3)x(Sb1/2Nb1/2)0.03(Mg1/3Nb2/3)0.01O3,0.15<x<0.25。
进一步的,陶瓷粉末的分子式为Pb0.92Sr0.08(Zr0.48Ti0.52)0.76(Ni1/3Nb2/3)0.2(Sb1/ 2Nb1/2)0.03(Mg1/3Nb2/3)0.01O3。陶瓷粉末的平均粒径为50μm。
本发明的第二个目的是提供一种PZT-PNN-PSN-PMN压电陶瓷的制备方法,具有同样的技术效果。
本发明提供的一种PZT-PNN-PSN-PMN压电陶瓷的制备方法,具体包括如下操作步骤:
具体包括如下操作步骤:
S1、将原料放入球磨机中球磨均匀得到混合粉末;
S2、将混合粉末压片后预烧结;
S3、对预烧结后的材料再次球磨;
S4、将再次球磨后的粉末与粘结剂搅拌均匀压片成型;
S5、排胶;
S6、烧结得到压电陶瓷。
进一步的,粘结剂是聚乙二醇。
进一步的,步骤S2中的预烧结温度为800~900℃。
进一步的,步骤S2中预烧结时间为180~300min。
进一步的,步骤S5中排胶的温度为500~600℃。
进一步的,步骤S6中的烧结温度为1200~1400℃。
进一步的,步骤S6中,烧结方式为先以5~7℃/min的升温速率,将烧结的温度升至1000℃;再以2℃/min的升温速率将烧结温度升至1200~1400℃;再以2℃/min的降温速率将温度降至1000℃,最后自然冷却。
进一步的,步骤S2中的预烧结的方式,先以V1的升温速率,将预烧结的温度升至800~900℃,保温时间为t1;再以V2的降温速率将温度降至400℃,最后自然冷却至室温;其中,V1的计算模型如下:
其中,V1为预烧结的升温速率,单位为℃/min;
T为预烧结的保温温度,单位为℃;
t1为保温时间,单位是min;
t为预烧结从升温到冷却至室温的总时长,单位是min;
a为常数,是所述压电陶瓷中Ni、Mg的掺杂量与PNN和PMN中Nb的掺杂量的比值。
由于Mg和Ni的熔沸点比其他金属更低,在预烧结过程中,若升温速率过快,会导致Ni和Mg在未与其他金属掺杂前就逸出,一方面造成晶格缺陷,另一方面导致Ni和Mg的掺杂量减小,压电陶瓷中的三方相较少,难以与四方相耦合,无法达到提高压电常数和介电常数的目的;若预烧结的升温速率过低,则会导致金属之间的掺杂性能差,造成晶粒尺寸不均匀,体积密度降低,同样影响压电陶瓷的电学性能。
本发明中,采用压电陶瓷中Ni和Mg的掺杂量与PNN和PMN中高熔沸点的Nb的掺杂量同时对升温速率进行控制,精确计算出最为合适的升温速率,使Ni和Mg在挥发前就与其他金属形成掺杂,进而牢牢锁住Ni和Mg,既保证了预烧结过程中金属掺杂的有效性,又避免了由于温度过高而导致的Ni和Mg的流失。
进一步的,V2的计算模型为:V1·a=V2。
本发明中,采用上述公式对降温速率进行控制,与自然冷却相比,给体系一个温度骤降的过程,进一步保证了晶粒的尺寸均匀,同时避免气孔率过高。
进一步的,在步骤S6中,烧结的保温时间为:
其中,S1为步骤S6中烧结的保温时间,单位为min;
S为步骤S6中烧结过程从升温直至降温至室温的时间总长度,单位为min;
T1为步骤S6中保温的温度,单位为℃;
V3为步骤S6中烧结温度升至1000℃的升温速率;b为常数,是压电陶瓷中Sr、Ni、Mg的总掺量与Nb的总掺量的比值。
在烧结过程中,过长的保温时间会导致Ni、Mg和Sr等低熔沸点的金属的挥发,进而导致钙钛矿结构的骨架坍塌,并导致三方相向四方相转化;而保温时间过短,则会导致物料的扩算系数降低,离子和空位无法得到充分的扩算,颗粒无法完成重排,降低了密度。
尤其是在本发明中,Ni的半径小于Zr和Ti,在烧结和掺杂过程中,会使陶瓷的晶粒尺寸减小,造成晶粒尺寸大小不均匀,出现不规则的气孔,虽然本发明中已经添加了Mg掺杂来改善晶粒尺寸,但是若保温时间过短,依然会导致体积密度降低。
因而,在本发明中,通过Sr、Mg、Ni与Nb的掺杂量对保温时间进行精确控制,既能够保证晶粒的尺寸均一,降低气孔率,同时还能够保证钙钛矿的晶体骨架不坍塌,保持良好的压电常数和介电常数。
进一步的,步骤S6中的烧结方式为振荡压力烧结。采用振荡烧结的技术,可以增加致密度,缩短烧结时间,从而提升压电材料的品质。
综上所述,本发明具有以下有益效果:
本发明提供的PZT-PNN-PSN-PMN压电陶瓷及其制备方法,通过低熔沸点金属和高熔沸点金属的掺杂量对预烧结和烧结过程中的升温速率和保温时间进行精确计算和控制,在避免低熔沸点金属挥发逸出的情况下,保证了晶粒尺寸的均匀性,提高了由于Ni的掺杂降低的体积密度,有效提高三元压电陶瓷的介电常数和压电常数。
附图说明:
图1为本发明实施例1~4压电陶瓷的XRD图;
图2为本发明实施例1~4的电学性能图。
具体实施方式
为更进一步阐述本发明为达成预定发明目的所采取的技术手段及功效,对依据本发明提出的一种PZT-PNN-PSN-PMN压电陶瓷及其制备方法,其具体实施方式、特征及其功效,详细说明如后。
下述实施例中,如无特殊说明,所使用的实验方法均为常规方法,所使用的材料等均可从化学试剂公司购买。
材料均从北京浩克科技有限公司购买,具体如下,纯度99.9%的Pb3O4、纯度99.9%的SrCO3、纯度99.99%的NiO、纯度99.9%的Nb2O5、纯度99.99%的Sb2O3、纯度99.9%的MgO、纯度99.9%的ZrO2和纯度99.9%的TiO2。
实施例1:一种PZT-PNN-PSN-PMN压电陶瓷及其制备方法
本实施例提供的压电陶瓷,分子式为Pb0.92Sr0.08(Zr0.48Ti0.52)0.76(Ni1/3Nb2/3)0.2(Sb1/2Nb1/2)0.03(Mg1/3Nb2/3)0.01O3。
其制备方法如下:
以Pb3O4、SrCO3、NiO、Nb2O5、Sb2O3、MgO、ZrO2和TiO2为原料,按照Pb0.92Sr0.08(Zr0.48Ti0.52)0.76(Ni1/3Nb2/3)0.2(Sb1/2Nb1/2)0.03(Mg1/3Nb2/3)0.01O3称量,具体包括如下操作步骤:
S1、将原料放入球磨机中,使用直径为5mm、10mm、15mm和20mm的氧化锆球作为研磨介质,以去离子水作为研磨分散剂,利用球磨机正、反交替运行,研磨28h得到混匀粉体;将粉体干燥过100目筛;
S2、将混合粉末压片后预烧结,预烧结温度是880℃,升温速率为15℃/min;
S3、对预烧结后的材料再次球磨,同样使用直径为5mm、10mm、15mm和20mm的氧化锆球作为研磨介质,以去离子水作为研磨分散剂,利用球磨机正、反交替运行,研磨28h得到混匀粉体;将粉体干燥过100目筛;
S4、将再次球磨后的粉末与聚乙二醇搅拌均匀,压片成型,聚乙二醇的加入量为粉体质量的6%;
S5、排胶,排胶温度为580℃,排胶时间为4h;
S6、烧结:在马弗炉中以6℃/min升温至1000℃,然后以2℃/min升温至1280℃保温2h,再以2℃/min降温至1000℃,最后随炉冷却。
实施例2:一种PZT-PNN-PSN-PMN压电陶瓷及其制备方法
本实施例提供的压电陶瓷,分子式为Pb0.92Sr0.08(Zr0.48Ti0.52)0.76(Ni1/3Nb2/3)0.2(Sb1/2Nb1/2)0.03(Mg1/3Nb2/3)0.01O3。
其制备方法如下:
以Pb3O4、SrCO3、NiO、Nb2O5、Sb2O3、MgO、ZrO2和TiO2为原料,按照Pb0.92Sr0.08(Zr0.48Ti0.52)0.76(Ni1/3Nb2/3)0.2(Sb1/2Nb1/2)0.03(Mg1/3Nb2/3)0.01O3称量,具体包括如下操作步骤:
S1、将原料放入球磨机中,使用直径为5mm、10mm、15mm和20mm的氧化锆球作为研磨介质,以去离子水作为研磨分散剂,利用球磨机正、反交替运行,研磨28h得到混匀粉体;将粉体干燥过100目筛;
S2、将混合粉末压片后预烧结,预烧结温度是880℃,预烧结时长为300min,升温速率为V1,保温60min后,以V2的降温速率将温度降至400℃,随炉冷却至室温;
S3、对预烧结后的材料再次球磨,同样使用直径为5mm、10mm、15mm和20mm的氧化锆球作为研磨介质,以去离子水作为研磨分散剂,利用球磨机正、反交替运行,研磨28h得到混匀粉体;将粉体干燥过100目筛;
S4、将再次球磨后的粉末与聚乙二醇搅拌均匀,压片成型,聚乙二醇的加入量为粉体质量的6%;
S5、排胶,排胶温度为580℃,排胶时间为4h;
S6、烧结:在马弗炉中以6℃/min升温至1000℃,然后以2℃/min升温至1280℃保温2h,再以2℃/min降温至1000℃,最后随炉冷却。
其中,V1为预烧结的升温速率,单位为℃/min;
T为预烧结的保温温度,单位为℃;
t1为保温时间,单位是min;
t为预烧结从升温到冷却至室温的总时长,单位是min;
a为常数,是压电陶瓷中Ni、Mg的掺杂量与PNN和PMN中Nb的掺杂量的比值;
V2为预烧结的降温速率,单位为℃/min。
计算可知,V1=3.76℃/min,V2=3.57℃/min。
实施例3:一种PZT-PNN-PSN-PMN压电陶瓷及其制备方法
本实施例提供的压电陶瓷,分子式为Pb0.92Sr0.08(Zr0.48Ti0.52)0.71(Ni1/3Nb2/3)0.25(Sb1/2Nb1/2)0.03(Mg1/3Nb2/3)0.01O3。
其制备方法如下:
以Pb3O4、SrCO3、NiO、Nb2O5、Sb2O3、MgO、ZrO2和TiO2为原料,按照Pb0.92Sr0.08(Zr0.48Ti0.52)0.76(Ni1/3Nb2/3)0.2(Sb1/2Nb1/2)0.03(Mg1/2Nb1/2)0.01O3称量,具体包括如下操作步骤:
S1、将原料放入球磨机中,使用直径为5mm、10mm、15mm和20mm的氧化锆球作为研磨介质,以去离子水作为研磨分散剂,利用球磨机正、反交替运行,研磨28h得到混匀粉体;将粉体干燥过100目筛;
S2、将混合粉末压片后预烧结,预烧结温度是880℃,预烧结时长为300min,升温速率为V1,保温60min后,以V2的降温速率将温度降至400℃,随炉冷却至室温;
S3、对预烧结后的材料再次球磨,同样使用直径为5mm、10mm、15mm和20mm的氧化锆球作为研磨介质,以去离子水作为研磨分散剂,利用球磨机正、反交替运行,研磨28h得到混匀粉体;将粉体干燥过100目筛;
S4、将再次球磨后的粉末与聚乙二醇搅拌均匀,压片成型,聚乙二醇的加入量为粉体质量的6%;
S5、排胶,排胶温度为580℃,排胶时间为4h;
S6、烧结:在马弗炉中以6℃升温至1000℃,然后以2℃/min升温至1280℃保温时间为S1,再以2℃/min降温至1000℃,最后随炉冷却,烧结总时长为600min。
其中,V1为预烧结的升温速率,单位为℃/min;
T为预烧结的保温温度,单位为℃;
t1为保温时间,单位是min;
t为预烧结从升温到冷却至室温的总时长,单位是min;
a为常数,是压电陶瓷中Sr、Ni、Mg的掺杂量与PNN和PMN中Nb的掺杂量和Zr的掺杂量的比值;
V2为预烧结的降温速率,单位为℃/min;
在步骤S6中,烧结的保温时间为:
其中,S1为步骤S6中烧结的保温时间,单位为min;
S为步骤S6中烧结过程从升温直至降温至室温的时间总长度,单位为min;
T1为步骤S6中保温的温度,单位为℃;
V3为步骤S6中烧结温度升至1000℃的升温速率;b为常数,是压电陶瓷中Sr、Ni、Mg的总掺量与Nb的总掺量的比值。
计算可知,V1=3.76℃/min,V2=3.57℃/min;S1=169min。
实施例4:一种PZT-PNN-PSN-PMN压电陶瓷及其制备方法
本实施例提供的压电陶瓷,分子式为Pb0.92Sr0.08(Zr0.48Ti0.52)0.71(Ni1/3Nb2/3)0.25(Sb1/2Nb1/2)0.03(Mg1/3Nb2/3)0.01O3。
其制备方法如下:
以Pb3O4、SrCO3、NiO、Nb2O5、Sb2O3、MgO、ZrO2和TiO2为原料,按照Pb0.92Sr0.08(Zr0.48Ti0.52)0.71(Ni1/3Nb2/3)0.25(Sb1/2Nb1/2)0.03(Mg1/3Nb2/3)0.01O3称量,具体包括如下操作步骤:
S1、将原料放入球磨机中,使用直径为5mm、10mm、15mm和20mm的氧化锆球作为研磨介质,以去离子水作为研磨分散剂,利用球磨机正、反交替运行,研磨28h得到混匀粉体;将粉体干燥过100目筛;
S2、将混合粉末压片后预烧结,预烧结温度是880℃,预烧结时长为300min,升温速率为V1,保温60min后,以V2的降温速率将温度降至400℃,随炉冷却至室温;
S3、对预烧结后的材料再次球磨,同样使用直径为5mm、10mm、15mm和20mm的氧化锆球作为研磨介质,以去离子水作为研磨分散剂,利用球磨机正、反交替运行,研磨28h得到混匀粉体;将粉体干燥过100目筛;
S4、将再次球磨后的粉末与聚乙二醇搅拌均匀,压片成型,聚乙二醇的加入量为粉体质量的6%;
S5、排胶,排胶温度为580℃,排胶时间为4h;
S6、烧结:在马弗炉中以6℃升温至1000℃,然后以2℃/min升温至1280℃保温时间为S1,再以2℃/min降温至1000℃,最后随炉冷却,烧结总时长为600min。
其中,V1为预烧结的升温速率,单位为℃/min;
T为预烧结的保温温度,单位为℃;
t1为保温时间,单位是min;
t为预烧结从升温到冷却至室温的总时长,单位是min;
a为常数,是压电陶瓷中Ni、Mg的掺杂量与PNN和PMN中Nb的掺杂量的比值;
V2为预烧结的降温速率,单位为℃/min;
在步骤S6中,烧结的保温时间为:
其中,S1为步骤S6中烧结的保温时间,单位为min;
S为步骤S6中烧结过程从升温直至降温至室温的时间总长度,单位为min;
T1为步骤S6中保温的温度,单位为℃;
V3为步骤S6中烧结温度升至1000℃的升温速率;b为常数,是压电陶瓷中Sr、Ni、Mg的总掺量与Nb的总掺量的比值。
计算可知,V1=3.66℃/min,V2=1.83℃/min;S1=144min。
性能测试:
对实施例1~4得到的压电陶瓷进行压电常数、介电常数进行测试,测试结果如下:
表一
根据实施例1和实施例2的XRD图对比可知,本发明中,采用压电陶瓷中Ni和Mg的掺杂量与PNN和PMN中高熔沸点的Nb的掺杂量同时对升温速率进行控制,精确计算出最为合适的升温速率,使Ni和Mg在挥发前就与其他金属形成掺杂,进而牢牢锁住Ni和Mg,既保证了预烧结过程中金属掺杂的有效性,又避免了由于温度过高而导致的Ni和Mg的流失。
根据实施例2和实施例3的XRD图和电学性能图对比可知,本发明通过Sr、Mg、Ni与Nb的掺杂量对保温时间进行精确控制,既能够保证晶粒的尺寸均一,降低气孔率,同时还能够保证钙钛矿的晶体骨架不坍塌,保持良好的压电常数和介电常数。
以上所述,仅是本发明的较佳实施例而已,并非对本发明作任何形式上的限制,虽然本发明已以较佳实施例展示如上,但并非用以限定本发明,任何熟悉本专业的技术人员,在不脱离本发明技术方案范围内,当可利用上述揭示的技术内容做出些许更动或修饰为等同变化的等效实施例,但凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰,均仍属于本发明技术方案的范围内。
Claims (10)
1.一种PZT-PNN-PSN-PMN压电陶瓷,其特征在于,所述陶瓷粉末的分子式为Pb0.92Sr0.08(Zr0.48Ti0.52)0.96-x(Ni1/3Nb2/3)x(Sb1/2Nb1/2)0.03(Mg1/3Nb2/3)0.01O3,0.15<x<0.25。
2.前述的PZT-PNN-PSN-PMN压电陶瓷的制备方法,其特征在于,以Pb3O4、SrCO3、NiO、Nb2O5、Sb2O3、MgO、ZrO2和TiO2为原料,通过球磨工艺研磨混匀粉体,过筛后烧结得到,其中各组分配比按照Pb0.92Sr0.08(Zr0.48Ti0.52)0.96-x(Ni1/3Nb2/3)x(Sb1/2Nb1/2)0.03(Mg1/3Nb2/3)0.01O3,0.15<x<0.25称量。
3.根据权利要求2所述的一种PZT-PNN-PSN-PMN压电陶瓷的制备方法,其特征在于,具体包括如下操作步骤:
S1、将原料放入球磨机中球磨均匀得到混合粉末;
S2、将混合粉末压片后预烧结;
S3、对预烧结后的材料再次球磨;
S4、将再次球磨后的粉末与粘结剂搅拌均匀压片成型;
S5、排胶;
S6、烧结得到所述压电陶瓷。
4.根据权利要求3所述的一种PZT-PNN-PSN-PMN压电陶瓷的制备方法,其特征在于,所述步骤S2中的预烧结温度为800~900℃。
5.根据权利要求4所述的一种PZT-PNN-PSN-PMN压电陶瓷的制备方法,其特征在于,所述步骤S2中预烧结时间为180~300min。
6.根据权利要求3所述的一种PZT-PNN-PSN-PMN压电陶瓷的制备方法,其特征在于,所述步骤S6中的烧结温度为1200~1400℃。
7.根据权利要求3所述的一种PZT-PNN-PSN-PMN压电陶瓷的制备方法,其特征在于,所述步骤S6中,烧结方式为先以5~7℃/min的升温速率,将烧结的温度升至1000℃;再以2℃/min的升温速率将烧结温度升至1200~1400℃;再以2℃/min的降温速率将温度降至1000℃,最后自然冷却。
9.根据权利要求8所述的一种PZT-PNN-PSN-PMN压电陶瓷的制备方法,其特征在于,所述V2的计算模型为:V1·a=V2。
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