CN107089832A - 一种基于铌锌、铌镍锆钛酸铅的压电陶瓷及其制备方法 - Google Patents
一种基于铌锌、铌镍锆钛酸铅的压电陶瓷及其制备方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 55
- VOLIIUVAEXIKFU-UHFFFAOYSA-N niobium zinc Chemical compound [Zn].[Zn].[Zn].[Nb] VOLIIUVAEXIKFU-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052451 lead zirconate titanate Inorganic materials 0.000 title claims abstract description 33
- HWHWBMBTCNLBGY-UHFFFAOYSA-N [Pb].[Ni].[Nb] Chemical compound [Pb].[Ni].[Nb] HWHWBMBTCNLBGY-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000010955 niobium Substances 0.000 claims abstract description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011701 zinc Substances 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 28
- 238000000498 ball milling Methods 0.000 claims description 21
- 238000007873 sieving Methods 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 12
- 238000005245 sintering Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 8
- 229910052709 silver Inorganic materials 0.000 claims description 8
- 239000004332 silver Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- 239000010431 corundum Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 230000005684 electric field Effects 0.000 claims description 7
- 239000012188 paraffin wax Substances 0.000 claims description 7
- 229920002545 silicone oil Polymers 0.000 claims description 7
- 229910052726 zirconium Inorganic materials 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 238000007650 screen-printing Methods 0.000 claims description 4
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- BEKPOVOEQGXHMA-UHFFFAOYSA-N [Zr].[Nb].[Ni] Chemical compound [Zr].[Nb].[Ni] BEKPOVOEQGXHMA-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- FEBJSGQWYJIENF-UHFFFAOYSA-N nickel niobium Chemical class [Ni].[Nb] FEBJSGQWYJIENF-UHFFFAOYSA-N 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract 1
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 6
- 239000011572 manganese Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 230000008901 benefit Effects 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(II,IV) oxide Inorganic materials O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- GNMQOUGYKPVJRR-UHFFFAOYSA-N nickel(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Ni+3].[Ni+3] GNMQOUGYKPVJRR-UHFFFAOYSA-N 0.000 description 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 2
- PZFKDUMHDHEBLD-UHFFFAOYSA-N oxo(oxonickeliooxy)nickel Chemical compound O=[Ni]O[Ni]=O PZFKDUMHDHEBLD-UHFFFAOYSA-N 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
本发明公开了一种基于铌锌、铌镍锆钛酸铅的压电陶瓷及其制备方法,按照摩尔百分比为Pb(Zn1/3Nb2/3)x(Ni1/3Nb2/3)y(Zr0.3Ti0.7)1‑x‑yO3+a Me,其中Me为四价元素,0<x<0.1、0.2<y<0.6。本发明制备的压电陶瓷具有介电、压电常数高、低损耗,性能稳定;且具有制备工艺简单,成本低,利于工业化生产,结构致密。与现有铌锌、铌镍系压电陶瓷相比,在1180℃所制备的陶瓷样品中。本发明的陶瓷有较高的电学性能,低介电损耗,介电损耗只有0.65%,压电常数达到600pC/N具有较好的综合性能。本发明的制备方法简单、可靠、成本低,便于工业化生产。
Description
技术领域
本发明属于压电陶瓷技术领域,尤其涉及一种基于铌锌、铌镍锆钛酸铅的压电陶瓷及其制备方法。
背景技术
压电陶瓷材料是一种功能陶瓷材料,能够把机械能与电能相互转换的功能,这种性能称为压电性能。压电陶瓷除具有压电性能外,还具有介电性能以及力学性能。由于压电陶瓷材料具有这些优异的综合性能,再加上其制备工艺简单、稳定、可靠,使其广泛应用于社会生活的各个方面,比如在电子材料领域。Pb(Ni1/3Nb2/3)系压电陶瓷材料自从被Smolenskii和Agranovskaya发现后,已经得到很多研究人员的关注和研究。Pb(Ni1/3Nb2/3)O3属于复合钙钛矿结构,符合ABO3型钙钛矿结构,具有典型的弛豫型铁电体的特征。PNN基的体系具有相对较低的烧结温度以及较高的介电常数。PZN基的压电陶瓷材料具有较高的电学性能。在此基础上,人们对于铌锌、铌镍系的压电陶瓷材料作了大量的研究。蔡晓峰等人研究发现铌锌、铌镍锆钛酸铅PZN-PNN-PZT压电陶瓷材料的具有较好的电学性能,通过掺杂Ca2+、Sr2+、Ba2+等元素对部分Pb的置换或者Li2CO3、Sb2O3等进入PZN-PNN-PZT压电陶瓷材料内部获得较优性能:相对介电常数εr~7000,压电应变常数d33=800pC/N,机电耦合系数kp=0.65。
综上所述,现有技术制备得到的高介电及压电常数的压电陶瓷材料;但因为PZN-PNN-PZT配方成分较为复杂,并且烧结温度区间较窄,导致所生产的压电陶瓷片电学性能的稳定性较低,不利于工业化生产。
发明内容
本发明的目的在于提供一种基于铌锌、铌镍锆钛酸铅的压电陶瓷及其制备方法,旨在解决现有技术制备得到的高介电及压电常数陶瓷材料,同时其介电损耗较高,此外其制备工艺复杂、不稳定及成本高,不利于工业化生产的问题。
本发明是这样实现的,一种基于铌锌、铌镍锆钛酸铅的压电陶瓷,所述基于铌锌、铌镍锆钛酸铅的压电陶瓷按照摩尔百分比为Pb(Zn1/3Nb2/3)x(Ni1/3Nb2/3)y(Zr0.3Ti0.7)1-x-yO3+aMe,其中Me为四价元素,0<x<0.1、0.2<y<0.6。
进一步,所述Me为Ce或Mn;
所述Me为Mn。
进一步,0<x<0.04,0.4<y<0.5。
本发明的另一目的在于提供一种所述基于铌锌、铌镍锆钛酸铅的压电陶瓷的制备方法,所述基于铌锌、铌镍锆钛酸铅的压电陶瓷的制备方法包括以下步骤:
步骤一,将原料按所述摩尔比混合,以酒精和锆球为球磨介质球磨,得粉料,将粉料放入烘箱中烘干,过40目筛子;
步骤二,将过筛后得到的粉料放入刚玉坩埚内,压实,加盖,在箱式电阻炉中预烧1-3h,然后随炉冷却;
步骤三,将预烧好的粉料二次球磨、烘干、过筛,加入5wt%-7wt%的石蜡进行造粒,之后将其过筛,然后压制成直径12mm,厚度为1.2mm的陶瓷圆片;
步骤四,将圆形陶瓷片放入坩埚中,密封,放入箱式电阻炉中进行烧结,然后随炉自然冷却至室温;
步骤五,将烧结好的陶瓷片进行清洁,在其上下表面印刷银浆,置于炉中,升温至800℃并保温30min,自然冷却至室温,然后将烧好的样品放置于硅油中加热到50-70℃,施加2kV/mm的直流电场,极化30min。
进一步,将原料按所述摩尔比混合,以酒精和锆球为球磨介质球磨16h,球磨转速为300r/min,得粉料,将粉料放入70℃的烘箱中烘干,过40目筛子;
将过筛后得到的粉料放入刚玉坩埚内,压实,加盖,在箱式电阻炉中在850℃-1000℃预烧2h,然后随炉冷却。
进一步,将预烧好的粉料二次球磨、烘干、过筛,加入5wt%-7wt%的石蜡进行造粒,之后将其过筛,在10Mpa的压强下压制成直径12mm,厚度为1.2mm的陶瓷圆片;
将圆形陶瓷片放入坩埚中,密封,放入箱式电阻炉中进行烧结,烧结温度为1100℃-1300℃,保温2h,然后随炉自然冷却至室温;
将烧结好的陶瓷片进行清洁,采用丝网印刷技术在其上下表面印刷银浆,置于炉中,升温至800℃并保温30min,自然冷却至室温,然后将烧好的样品放置于硅油中加热到50-70℃,施加2kV/mm的直流电场,极化30min;
所述预烧温度为850℃;烧结温度为1180℃。
本发明的另一目的在于提供一种利用所述基于铌锌、铌镍锆钛酸铅的压电陶瓷制备的电子元器件。
本发明的另一目的在于提供一种利用所述基于铌锌、铌镍锆钛酸铅的压电陶瓷制备的贾卡梳。
本发明的另一目的在于提供一种利用所述基于铌锌、铌镍锆钛酸铅的压电陶瓷制备的压电滤波器。
本发明提供的基于铌锌、铌镍锆钛酸铅的压电陶瓷及其制备方法,制备的压电陶瓷具有介电、压电常数高、低损耗,性能稳定的特点,制备工艺简单,可以通过传统的固相烧结法合成,且其烧结温度范围较宽(±30℃),适用于大批量工业生产;在其原材料中,各种金属氧化物价格成本也较低,并且均可采用化学纯原料,降低生产成本。经本发明制备的压电陶瓷具有高介电、压电常数、低介电损耗的优点,结构致密(如附图2)。与现有铌锌、铌镍系压电陶瓷相比,在1180℃所制备的陶瓷样品中,本发明的陶瓷的较高的电学性能,低介电损耗,,如表1所示,介电损耗只有0.65%,压电常数达到600pC/N具有较好的综合性能。本发明的制备方法简单、可靠、成本低,便于工业化生产。
附图说明
图1是本发明实施例提供的基于铌锌、铌镍锆钛酸铅的压电陶瓷的制备方法流程图。
图2是本发明实施例提供的掺杂氧化锰质量分数分别为0.0%、0.2%、0.4%、0.6%和0.8%的SEM示意图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
下面结合附图对本发明的应用原理作详细的描述。
本发明实施例提供的基于铌锌、铌镍锆钛酸铅的压电陶瓷按照摩尔百分比为Pb(Zn1/3Nb2/3)x(Ni1/3Nb2/3)y(Zr0.3Ti0.7)1-x-yO3+a Me,其中Me为四价元素,0<x<0.1、0.2<y<0.6。
所述Me为Ce或Mn。
所述Me为Mn。
所述0<x<0.04,0.4<y<0.5。
所述原料为Pb3O4、ZrO2、TiO2、Ni2O3、Nb2O5及ZnO、MnO2。
如图1所示,本发明实施例提供的基于铌锌、铌镍锆钛酸铅的压电陶瓷的制备方法包括以下步骤:
S101:将所述原料按所述摩尔比混合,以酒精和锆球为球磨介质球磨,得粉料,将粉料放入烘箱中烘干,过40目筛子;
S102:将过筛后得到的粉料放入刚玉坩埚内,压实,加盖,在箱式电阻炉中预烧1-3h,然后随炉冷却;
S103:将预烧好的粉料二次球磨、烘干、过筛,加入5wt%-7wt%的石蜡进行造粒,之后将其过筛,然后压制成直径12mm,厚度为1.2mm的陶瓷圆片;
S104:将圆形陶瓷片放入坩埚中,密封,放入箱式电阻炉中进行烧结,然后随炉自然冷却至室温;
S105:将烧结好的陶瓷片进行清洁,在其上下表面印刷银浆,置于炉中,升温至800℃并保温30min,自然冷却至室温,然后将烧好的样品放置于硅油中加热到50-70℃,施加2kV/mm的直流电场,极化30min。
将所述原料按所述摩尔比混合,以酒精和锆球为球磨介质球磨16h,球磨转速为300r/min,得粉料,将粉料放入70℃的烘箱中烘干,过40目筛子;
将过筛后得到的粉料放入刚玉坩埚内,压实,加盖,在箱式电阻炉中在850℃-1000℃预烧2h,然后随炉冷却;
将预烧好的粉料二次球磨、烘干、过筛,加入5wt%-7wt%的石蜡进行造粒,之后将其过筛,在10Mpa的压强下压制成直径12mm,厚度为1.2mm的陶瓷圆片;
将圆形陶瓷片放入坩埚中,密封,放入箱式电阻炉中进行烧结,烧结温度为1100℃-1300℃,保温2h,然后随炉自然冷却至室温;
将烧结好的陶瓷片进行清洁,采用丝网印刷技术在其上下表面印刷银浆,置于炉中,升温至800℃并保温30min,自然冷却至室温,然后将烧好的样品放置于硅油中加热到50-70℃,施加2kV/mm的直流电场,极化30min。
所述预烧温度为850℃;烧结温度为1180℃。
本发明实施例制备的基于铌锌、铌镍锆钛酸铅四价掺杂的压电陶瓷在电子元器件领域中的应用。
下面结合具体实施例对本发明的应用原理作进一步的描述。
实施例1:
本发明实施例提供的基于铌锌、铌镍锆钛酸铅四价掺杂的压电陶瓷,其组成及摩尔百分比为Pb(Zn1/3Nb2/3)x(Ni1/3Nb2/3)y(Zr0.3Ti0.7)1-x-yO3+a Me,其中Me是Mn的四价元素;
所述原料为Pb3O4、ZrO2、TiO2、Ni2O3、Nb2O5及ZnO、MnO2。
配方参数:x=0.02,y=0.49,a=0.0%、0.2%、0.4%、0.6%及0.8%。
所述制备方法包括如下步骤:
(1)配料
将所述原料按所述摩尔比混合,以酒精和锆球为球磨介质球磨16h,球磨转速为300r/min,得粉料,将粉料放入80℃的烘箱中烘干,过40目筛子;
(2)预烧
将步骤(1)过筛后得到的粉料放入刚玉坩埚内,压实,加盖,在箱式电阻炉中在900℃预烧2h,然后随炉冷却;
(3)压片
将步骤(2)中预烧好的粉料二次球磨、烘干、过筛,加入5wt%-7wt%的石蜡进行造粒,之后将其过筛,在10Mpa的压强下压制成直径12mm,厚度为1.2mm的陶瓷圆片;
(4)烧结
将步骤(3)的圆形陶瓷片放入坩埚中,密封,放入箱式电阻炉中进行烧结,烧结温度为1200℃,保温2h,然后随炉自然冷却至室温;
(5)刷银、极化
将步骤(4)烧结好的陶瓷片进行清洁,采用丝网印刷技术在其上下表面印刷银浆,置于炉中,升温至800℃并保温30min,自然冷却至室温,然后将烧好的样品放置于硅油中加热到50-70℃,施加2kV/mm的直流电场,极化30min。
(6)测试电学性能
取经本发明实施例制备的陶瓷片和现有技术制备的陶瓷片,放置在室温下,24h后测量样品的各项电学性能,并记录在表1中。
表1在1180℃烧结下,不同掺杂含量样品的电学性能参数
其中压电常数通过准静态d33测试仪方法ZJ-3A China,介电损耗tanδ通过TH2826-LCRMeter来测量,采用精密阻抗分析仪(Agilent HP4294A)分析材料的介电常数εr,机电耦合系数kp,通过测定谐振频率fs和反谐振频率fp,并根据下式计算:
从表1可以看出,本发明通过在铌锌、铌镍锆钛酸铅陶瓷原料中添加适量的四价MnO2,掺杂含量a=0.4%,并调整基础配方摩尔比x=0.02,y=0.49,选用合适的烧结温度1180℃来制备得到压电陶瓷,使该铌锌、铌镍系压电陶瓷的介电损耗降低了近3倍多,该体系的压电陶瓷材料能够广泛的应用于电子元器件领域,比如贾卡梳、压电滤波器等。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (9)
1.一种基于铌锌、铌镍锆钛酸铅的压电陶瓷,其特征在于,所述基于铌锌、铌镍锆钛酸铅的压电陶瓷按照摩尔百分比为Pb(Zn1/3Nb2/3)x(Ni1/3Nb2/3)y(Zr0.3Ti0.7)1-x-yO3+aMe,其中Me为四价元素,0<x<0.1、0.2<y<0.6。
2.如权利要求1所述的基于铌锌、铌镍锆钛酸铅的压电陶瓷,其特征在于,所述Me为Ce或Mn;
所述Me为Mn。
3.如权利要求1所述的基于铌锌、铌镍锆钛酸铅的压电陶瓷,其特征在于,0<x<0.04,0.4<y<0.5。
4.一种如权利要求1所述基于铌锌、铌镍锆钛酸铅的压电陶瓷的制备方法,其特征在于,所述基于铌锌、铌镍锆钛酸铅的压电陶瓷的制备方法包括以下步骤:
步骤一,将原料按所述摩尔比混合,以酒精和锆球为球磨介质球磨,得粉料,将粉料放入烘箱中烘干,过40目筛子;
步骤二,将过筛后得到的粉料放入刚玉坩埚内,压实,加盖,在箱式电阻炉中预烧1-3h,然后随炉冷却;
步骤三,将预烧好的粉料二次球磨、烘干、过筛,加入5wt%-7wt%的石蜡进行造粒,之后将其过筛,然后压制成直径12mm,厚度为1.2mm的陶瓷圆片;
步骤四,将圆形陶瓷片放入坩埚中,密封,放入箱式电阻炉中进行烧结,然后随炉自然冷却至室温;
步骤五,将烧结好的陶瓷片进行清洁,在其上下表面印刷银浆,置于炉中,升温至800℃并保温30min,自然冷却至室温,然后将烧好的样品放置于硅油中加热到50-70℃,施加2kV/mm的直流电场,极化30min。
5.如权利要求4所述的基于铌锌、铌镍锆钛酸铅的压电陶瓷的制备方法,其特征在于,将原料按所述摩尔比混合,以酒精和锆球为球磨介质球磨16h,球磨转速为300r/min,得粉料,将粉料放入70℃的烘箱中烘干,过40目筛子;
将过筛后得到的粉料放入刚玉坩埚内,压实,加盖,在箱式电阻炉中850℃-1000℃预烧2h,然后随炉冷却。
6.如权利要求4所述的基于铌锌、铌镍锆钛酸铅的压电陶瓷的制备方法,其特征在于,将预烧好的粉料二次球磨、烘干、过筛,加入5wt%-7wt%的石蜡进行造粒,之后将其过筛,在10Mpa的压强下压制成直径12mm,厚度为1.2mm的陶瓷圆片;
将圆形陶瓷片放入坩埚中,密封,放入箱式电阻炉中进行烧结,烧结温度为1100℃-1300℃,保温2h,然后随炉自然冷却至室温;
将烧结好的陶瓷片进行清洁,采用丝网印刷技术在其上下表面印刷银浆,置于炉中,升温至800℃并保温30min,自然冷却至室温,然后将烧好的样品放置于硅油中加热到50-70℃,施加2kV/mm的直流电场,极化30min;
所述预烧温度为850℃;烧结温度为1180℃。
7.一种利用权利要求1~3任意一项所述基于铌锌、铌镍锆钛酸铅的压电陶瓷制备的电子元器件。
8.一种利用权利要求1~3任意一项所述基于铌锌、铌镍锆钛酸铅的压电陶瓷制备的贾卡梳。
9.一种利用权利要求1~3任意一项所述基于铌锌、铌镍锆钛酸铅的压电陶瓷制备的压电滤波器。
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CN114890789A (zh) * | 2022-04-06 | 2022-08-12 | 山东国瓷功能材料股份有限公司 | 匹配银内电极共烧铌锰-锆钛酸铅压电陶瓷、其制备方法及其制品 |
CN115710123A (zh) * | 2022-11-23 | 2023-02-24 | 西安交通大学 | 一种无铅铁电材料及其制备方法和应用 |
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