CN111348909B - 压电组合物和压电元件 - Google Patents
压电组合物和压电元件 Download PDFInfo
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- CN111348909B CN111348909B CN201911307070.0A CN201911307070A CN111348909B CN 111348909 B CN111348909 B CN 111348909B CN 201911307070 A CN201911307070 A CN 201911307070A CN 111348909 B CN111348909 B CN 111348909B
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2683—Other ferrites containing alkaline earth metals or lead
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/80—Constructional details
- H10N30/85—Piezoelectric or electrostrictive active materials
- H10N30/853—Ceramic compositions
- H10N30/8561—Bismuth-based oxides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
- C04B35/6262—Milling of calcined, sintered clinker or ceramics
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- C—CHEMISTRY; METALLURGY
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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Abstract
本发明提供一种压电组合物,其具有包含铋、钡、铁和钛的氧化物和银。氧化物具有钙钛矿结构。将氧化物的质量表示为MABO3,将银的质量表示为MAG。100×MAG/MABO3为0.01以上且10.00以下。
Description
技术领域
本发明涉及压电组合物和压电元件。
背景技术
当前实用化的大部分压电组合物是由锆酸铅(PbZrO3)和钛酸铅(PbTiO3)构成的固溶体(所谓的PZT类压电组合物)。PZT系压电组合物包含大量的氧化铅(PbO)作为主成分。由于氧化铅即使在低温下也极易挥发,因此,在压电组合物或使用其的压电元件的制造过程中,大量的氧化铅会扩散到大气中。因为铅是危害人体的环境污染物质,所以寻求不含铅的压电组合物。
不含铅的代表性的压电组合物是铁酸铋(BiFeO3)。例如,在下述专利文献1和非专利文献1中记载有由BiFeO3和钛酸钡(BaTiO3)构成的固溶体(BFO-BTO类压电组合物)。但是,目前的BFO-BTO类压电组合物由于电阻率小,在BFO-BTO类压电组合物中容易产生漏电流,因此,目前的BFO-BTO类压电组合物未必具有充分的压电性。例如,极化处理后的BFO-BTO类压电组合物的压电常数d33为135pC/N左右。下述专利文献2公开了由包含BiFeO3、Bi2Fe4O9和Bi25FeO39的粉体制造电介质陶瓷的方法。利用该制造方法,电介质陶瓷(压电组合物)的漏电流降低。但是,在下述专利文献2中,没有报告电介质陶瓷的具体的压电常数。
现有技术文献
专利文献
专利文献1:日本特开2009-298621号公报
专利文献2:日本专利第6146453号公报
非专利文献
非专利文献1:Wei et.al,Dielectric,Ferroelectric,and PiezoelectricProperties of BiFeO3-BaTiO3 Ceramics,J.Am.Ceram.Soc.,96[10](2013)3163-3168.
发明内容
发明要解决的技术问题
本发明的目的在于,提供具有高的电阻率和大的压电常数的压电组合物和具有该压电组合物的压电元件。
用于解决技术问题的技术方案。
本发明的一个方面涉及的压电组合物具有:包含铋、钡、铁和钛的氧化物和银,氧化物具有钙钛矿结构,将氧化物的质量表示为MABO3,将银的质量表示为MAG,100×MAG/MABO3为0.01以上且10.00以下。
本发明的一个方面涉及的压电组合物还包含选自钒、铌、钽、钼、钨和锰中的至少一种元素D。
本发明的一个方面涉及的压电组合物至少还包含铌作为元素D。
元素D的质量的总计值可以表示为MD,100×MD/MABO3可以为0.00以上5.00以下。
至少一部分的上述氧化物可以表示为x[BimFeO3]-y[BanTiO3],x可以为0.6以上且0.8以下,y可以为0.2以上且0.4以下,x+y可以为1,m可以为0.96以上且1.06以下,n可以为0.96以上且1.06以下。
本发明的一个方面涉及的压电元件具有上述的压电组合物。
发明的效果
根据本发明,提供具有高的电阻率和大的压电常数的压电组合物和具有该压电组合物的压电元件。
附图说明
图1是本发明的一个实施方式的压电组合物所含的氧化物的钙钛矿结构的晶胞的立体图。
图2是本发明的一个实施方式的压电元件的示意性立体图。
符号说明
2…基板、4…第一电极、6…压电体(压电组合物)、8…第二电极、uc…钙钛矿结构的晶胞。
具体实施方式
以下,参照附图对本发明的优选的实施方式进行说明。本发明不限定于下述实施方式。
本实施方式的压电组合物具有包含铋(Bi)、钡(Ba)、铁(Fe)和钛(Ti)的氧化物和银(Ag)。为了方便说明,将包含Bi、Ba、Fe和Ti的氧化物表示为“BFO-BTO”。BFO-BTO具有钙钛矿结构。BFO-BTO可以包含选自钙钛矿结构的正方晶(tetragonal crystal)、钙钛矿结构的立方晶(cubic crystal)和钙钛矿结构的菱面体晶(rhombohedral crystal)中的至少一种结晶。钙钛矿结构的晶胞的一例示于图1。晶胞uc也可以由位于A位点的元素A、位于B位点的元素B以及氧(O)构成。元素A可以为Bi或Ba。元素B可以为Fe或Ti。
将氧化物(BFO-BTO)的质量表示为MABO3。将Ag的质量表示为MAG。换言之MAG表示Ag的单质的质量。100×MAG/MABO3为0.01以上且10.00以下。通过使100×MAG/MABO3为0.01以上且10.00以下,压电组合物能够具有高的电阻率(ρ)和大的压电常数(d33)。其原因如以下。
构成BFO-BTO的钙钛矿结构的一部分氧容易缺失。即,在钙钛矿结构中,容易产生氧空位。构成钙钛矿结构的一部分氧的缺失例如由下述式1表示。随着产生一个氧空位(VO”),产生两个电子(e-)。因此,在压电组合物包含氧空位的情况下,在压电组合物中容易产生氧空位引起的漏电流。换言之,包含氧空位的压电组合物的电阻率低。其结果,难以对压电组合物施加高的电压,压电组合物没有被充分极化,压电组合物难以具有大的压电常数。但是,由于本实施方式的压电组合物包含Ag,因此,位于BFO-BTO的钙钛矿结构的A位点的Ba的一部分被Ag置换。Ba被Ag置换例如由下述式2表示。式2中的AgBA是代替Ba而位于钙钛矿结构的A位点的Ag。构成钙钛矿结构的Ba的价数为2,因为Ag的价数为1,所以随着Ba被Ag置换,产生空穴(h+)。而且,通过使100×MAG/MABO3为0.01以上且10.00以下,氧空位引起的电子和Ag引起的空穴容易平衡。即,Ag作为电子的受主起作用。其结果,压电组合物的电阻率比100×MAG/MABO3在上述范围外的压电组合物的电阻率高,压电组合物的漏电流被抑制。因此,能够对压电组合物施加高的电压,压电组合物被充分极化,压电组合物能够具有大的压电常数。例如,通过使100×MAG/MABO3在上述的范围内,压电组合物能够具有140pC/N以上的d33。在100×MAG/MABO3低于0.01的情况下,由于Ag引起的空穴而难以充分地抵消氧空位引起的电子。在100×MAG/MABO3大于10.00的情况下,在压电组合物中电荷也难以平衡,BFO-BTO的晶体结构(钙钛矿结构)由于过剩的Ag而容易损坏,压电组合物的压电常数容易减少。因为压电组合物容易具有高的电阻率和大的压电常数,所以100×MAG/MABO3可以优选为0.01以上且5.00以下,进一步优选为0.01以上且0.50以下。假如在压电组合物不包含Ag而包含价数为2的铜(Cu)的情况下,压电组合物难以具有高的电阻率,也难以具有大的压电常数。但压电组合物除Ag外也可以包含Cu。施加于压电组合物的电压也可以被称作电场。
O→VO”+2e- (1)
Ag→AgBA+h+ (2)
压电组合物还可以包含选自钒(V)、铌(Nb)、钽(Ta)、钼(Mo)、钨(W)和锰(Mn)中的至少一种元素D。压电组合物可以包含多种元素D。元素D的价数为5或6。例如,钒、铌和钽各自的价数为5。钼、钨和锰各自的价数为6。通过压电组合物含有至少一种元素D,压电组合物的电阻率(ρ)容易提高,压电组合物的压电常数(d33)容易增加。其理由如下。但是,即使在压电组合物不含元素D的情况下,通过压电组合物含有Ag,压电组合物也能够具有高的电阻率和大的压电常数。
由于Bi容易挥发,因此,在压电组合物的制造过程中位于钙钛矿结构的A位点的一部分Bi有可能缺失。即,在钙钛矿结构中,有可能产生Bi的空位。构成钙钛矿结构的一部分Bi的缺失例如由下述式3表示。由于构成钙钛矿结构的Bi的价数为3,因此,随着产生一个Bi的空位(VBI”’),产生三个空穴(h+)。因此,在压电组合物包含Bi的空位的情况下,在压电组合物中容易产生由于空穴引起的漏电流。换言之,通过压电组合物包含Bi的空位,压电组合物的电阻率容易降低。其结果,难以对压电组合物施加高的电压,压电组合物难以被充分极化,压电组合物的压电常数难以增加。构成BFO-BTO的钙钛矿结构的Fe离子的价数为3。但是,在压电组合物的制造过程中,Fe离子的价数有可能减少。Fe离子的价数的减少例如由下述式4表示。由于构成钙钛矿结构的Fe的价数为3,因此,随着Fe的价数的减少,产生一个空穴(h+)。因此,随着Fe的价数的减少,在压电组合物中容易产生由于空穴引起的漏电流。换言之,随着Fe的价数的减少,压电组合物的电阻率容易降低。其结果,难以对压电组合物施加高的电压,压电组合物难以被充分极化,压电组合物的压电常数难以增加。另一方面,在压电组合物包含元素D的情况下,位于BFO-BTO的钙钛矿结构的B位点的元素的一部分被元素D置换。位于B位点的元素例如为Ti。在元素D的价数为5的情况下,Ti被元素D置换例如由下述式5表示。在元素D的离子的价数为6的情况下,Ti被元素D置换例如由下述式6表示。式4和式5中的DTI是代替Ti而位于钙钛矿结构的B位点的元素D。因为构成钙钛矿结构的Ti的价数为4,元素D的价数为5或6,所以随着Ti被元素D置换,产生电子(e-)。因此,由于Bi的空位引起的空穴、由于Fe的价数的减少引起的空穴和源自元素D的电子容易平衡。即,元素D作为电子的施主起作用。其结果,压电组合物的电阻率容易比不含元素D的压电组合物的电阻率高,且容易抑制压电组合物的漏电流。因此,容易对压电组合物施加高的电压,压电组合物容易被充分极化,压电组合物容易具有大的压电常数。
Bi→VBI”’+3h+ (3)
Fe3+→Fe2++h+ (4)
D→DTI+e- (5)
D→DTI+2e- (6)
压电组合物还可以至少包含铌作为元素D。包含铌的压电组合物与包含铌以外的元素D的压电组合物相比,容易具有高的电阻率。因此,包含铌的压电组合物与包含铌以外的元素D的压电组合物相比,容易具有大的压电常数。
可以将元素D的质量的总计值表示为MD,100×MD/MABO3可以为0.00以上且5.00以下。MD也可以称作元素D的单质的质量的总计值。通过使100×MD/MABO3为0.00以上且5.00以下,Bi的空位引起的空穴、Fe的价数的减少引起的空穴和源自元素D的电子容易平衡。其结果,压电组合物的电阻率容易比100×MD/MABO3在上述范围外的压电组合物的电阻率高,容易抑制压电组合物的漏电流。因此,对压电组合物容易施加高的电压,压电组合物容易被充分极化,压电组合物容易具有大的压电常数。例如,通过使100×MD/MABO3在上述的范围内,压电组合物能够具有150pC/N以上的d33。因为压电组合物容易具有高的电阻率和大的压电常数,所以100×MD/MABO3可以优选为0.01以上且1.00以下,进一步优选为0.01以上且0.10以下。
压电组合物具有高的电阻率和大的压电常数的原因未必限定于上述的机制。
至少一部分氧化物(BFO-BTO)也可以由下述化学式A表示。下述化学式A等于化学式B。
x[BimFeO3]-y[BanTiO3] (A)
(BixmBayn)(FexTiy)O3 (B)
x+y为1。x可以为0.6以上且0.9以下、或0.6以上且0.8以下。y也可以为0.1以上且0.4以下、或0.2以上且0.4以下。m也可以为0.96以上且1.06以下。n也可以为0.96以上且1.06以下。在x为0.6以上且0.8以下,y为0.2以上且0.4以下的情况下,压电组合物容易具有高的电阻率,容易具有大的压电常数。
上述MABO3是基于假设压电组合物中所含的Bi、Fe、Ba和Ti的全部元素仅构成由化学式A表示的氧化物的x[BimFeO3]-y[BanTiO3]的质量的计算值。即,MABO3是用于规定100×MAG/MABO3的计算上的值。实际上,化学式A或化学式B中的一部分Ba或Bi也可以被Ag置换。化学式A或化学式B中的一部分Ti或Fe也可以被元素D置换。即,包含Bi、Ba、Fe和Ti的氧化物还可以包含Ag。包含Bi、Ba、Fe和Ti的氧化物还可以包含Ag和元素D双方。压电组合物可以仅由包含Bi、Fe、Ba、Ti、Ag和O的一种氧化物构成。压电组合物也可以仅由包含Bi、Fe、Ba、Ti、Ag、元素D和O的一种氧化物构成。压电组合物的一部分可以为由BimFeO3构成的相。压电组合物的一部分也可以为由BanTiO3构成的相。压电组合物也可以含有Bi、Fe、Ba、Ti、Ag、元素D和O以外的元素作为杂质或添加物。例如,压电组合物可以包含选自钠(Na)、钾(K)、镁(Mg)、铝(Al)、硫(S)、锆(Zr)、硅(Si)、磷(P)、铜(Cu)、锌(Zn)和铪(Hf)中的至少一种。本实施方式的压电组合物也可以不含Pb。但是,本实施方式的技术的范围内不一定排除包含Pb的压电组合物。
压电组合物整体的平均组成例如可以通过X射线荧光分析(XRF法)或电感耦合等离子体(ICP)发光光谱法分析。压电组合物的结构也可以通过X射线衍射(XRD)法鉴定。
如图2所示,本实施方式的压电元件10具有:基板2、重叠于基板2的表面的第一电极4、重叠于第一电极4的表面的压电体6、和重叠于压电体6的表面的第二电极8。压电体6包含本实施方式的上述压电组合物。压电体6可以为压电组合物的烧结体。压电体6除压电组合物外也可以包含其他成分。图2所示的压电体6为薄的长方体,但压电体6的形状及尺寸没有限定。基板2例如可以为金属、半导体、树脂、玻璃或陶瓷。只要第一电极4和第二电极8具有导电性,第一电极4和第二电极8各自的组成就没有限定。第一电极4和第二电极8分别可以为金属单质或合金。第一电极4和第二电极8分别也可以为具有导电性的金属氧化物。
本实施方式的压电元件的用途是多种多样的。压电元件例如可以为压电麦克风、压电变压器、收割机、振荡器、谐振器或声多层膜。压电元件例如也可以为压电促动器。压电促动器可以用于触觉反馈(haptics)。即,压电促动器可以用于寻求皮肤感觉(触觉)带来的反馈的各种器件。寻求皮肤感觉带来的反馈的装置例如可以是可穿戴式装置、触控屏、可视数据终端或游戏控制器。压电促动器可以用于磁头组件、磁头堆栈组件或硬盘驱动器。压电促动器也可以用于例如打印头、或喷墨打印装置。压电促动器也可以用于压电开关。压电元件例如可以为压电传感器。压电传感器可以用于例如陀螺仪传感器、压力传感器、脉搏传感器、超声波传感器或震动传感器。上述的各压电元件也可以为MEMS的一部分或全部。
本实施方式的压电组合物可以通过以下的制造方法制造。
在压电组合物的制造中,由起始原料制备原料粉末(原料颗粒)。通过原料颗粒的压制成型而形成成型体。通过烧制成型体而得到烧结体。通过对烧结体实施极化处理,得到压电体。本实施方式的压电组合物是指极化处理前的烧结体和极化处理后的烧结体这两者。以下,各工序的详细内容如下。
在造粒工序中,秤量压电组合物的起始原料。可以使用多种起始原料。起始原料包含Bi、Fe、Ba、Ti和Ag。起始原料还可以包含元素D。起始原料可以为各元素的单质(金属)或化合物。化合物例如也可以为氧化物、碳酸盐、氢氧化物、草酸盐或硝酸盐等。各起始原料可以为固体(例如粉末)。通过秤量各起始原料,起始原料整体的Bi、Fe、Ba和Ti的摩尔比可以调整为上述化学式A中的Bi、Fe、Ba和Ti的摩尔比。起始原料整体的Ag的质量可以调整为100×MAG/MABO3为0.01以上且10.00以下。起始原料整体的元素D的质量的总计值可以调整为100×MD/MABO3为0.00以上且5.00以下。
铋化合物(Bi化合物)可以为氧化铋(Bi2O3)、硝酸铋(Bi(NO3)3)等。铁化合物(Fe化合物)可以为氧化铁(Fe2O3)、氯化铁(FeCl3)或硝酸铁(Fe(NO3)3)等。钡化合物(Ba化合物)可以为氧化钡(BaO)、碳酸钡(BaCO3)、草酸钡(BaC2O4)、醋酸钡((CH3COO)2Ba)、硝酸钡(Ba(NO3)2)、硫酸钡(BaSO4)或钛酸钡(BaTiO3)等。钛化合物(Ti化合物)可以为氧化钛(TiO2)等。Ag的化合物可以为Ag2O(氧化银)。元素D的化合物可以为元素D的氧化物。元素D的氧化物例如可以为选自氧化钒(V2O5)、氧化铌(Nb2O5)、氧化钽(Ta2O5)、氧化钼(MoO3)、氧化钨(WO3)和氧化锰(MnO3)中的至少一种。
在造粒工序中,由上述的起始原料制备原料颗粒。也可以制备组成不同的多种原料颗粒。原料颗粒的制备方法例如可以如下。
可以通过混合起始原料和溶剂而制备浆料。可以通过使用了球磨机等的浆料的湿式混合,粉碎浆料中的起始原料。浆料的制备中使用的溶剂例如可以为水。溶剂也可以为乙醇等醇。溶剂也可以为水和乙醇的混合物。湿式混合后的起始原料可以通过喷雾干燥机等进行干燥。
通过将粉碎后的起始原料的混合物成型,形成预成型体。通过将预成型体在氧化的气氛中进行加热(煅烧,calcine),得到预烧结体。氧化的气氛例如可以为大气。预烧温度可以为700℃以上且1050℃以下。预烧的时间可以为1~3小时左右。通过粉碎预烧结体,得到原料颗粒。可以混合原料颗粒和溶剂而制备浆料。可以通过使用球磨机等湿式混合浆料,粉碎浆料中的原料颗粒。可以通过该湿式混合,调整原料颗粒的一次粒径的平均值。原料颗粒的一次粒径的平均值例如可以为0.01μm以上且20μm以下。湿式混合后的原料颗粒可以通过喷雾干燥机等进行干燥。
通过原料颗粒和粘合剂的混合物的压制成型,得到成型体。粘合剂可以为聚乙烯醇或乙基纤维素等有机粘合剂。分散剂可以添加到粘合剂中。
通过将成型体在氧化的气氛中进行烧制(烧结,sinter),得到烧结体。也可以在成型体烧制前进行成型体的脱粘合剂处理。即,可以通过加热成型体,分解成型体中的粘合剂。脱粘合剂处理和烧制也可以连续进行。脱粘合剂处理和烧制也可以分别进行。烧制温度可以为900℃以上且1250℃以下。烧制时间可以为1小时以上且8小时以下。
可以在后述的极化处理之前,通过切断烧结体而形成由烧结体构成的薄板。可以对烧结体的薄板的表面实施研磨机研磨。烧结体的切断可以使用刀具、切片机或切割锯等切断机。在研磨机研磨后,在烧结体的对置的一对表面上分别形成极化处理用的预电极。预电极可以通过真空蒸镀法或溅射形成。预电极通过使用氯化铁溶液等的蚀刻处理而容易除去。
在极化处理中,在夹着烧结体的一对预电极之间施加极化电场。在极化处理中,可以加热烧结体。极化处理中的烧结体的温度可以为80℃以上且300℃以下。施加极化电场的时间可以为1分钟以上且30分钟以下。极化电场可以为烧结体的矫顽电场的0.9倍以上。
在极化处理后从烧结体除去预电极。可以通过加工烧结体,形成具有期望的形状的压电组合物(压电体)。
以上,对本发明的优选的实施方式进行了说明,但本发明并一定限定于上述的实施方式。例如,本发明的压电组合物也可以为压电薄膜。
[实施例]
以下,通过实施例和比较例详细说明本发明。但是,本发明不限定于以下的实施例。
(实施例1)
使用Bi2O3的粉末、Fe2O3的粉末、BaCO3的粉末、TiO2的粉末和Ag(金属单质)的粉末作为起始原料。以起始原料整体中的Bi、Fe、Ba和Ti的摩尔比与下述化学式A1的Bi、Fe、Ba和Ti的摩尔比一致的方式秤量BaCO3、TiO2、Bi2O3和Fe2O3。在实施例1的情况下,化学式A1中的x和y的值为下述表1所示的值。以100×MAG/MABO3为5.2的方式秤量Ag。MAG为起始原料中所含的Ag的质量。MABO3是基于起始原料中所含的Bi、Fe、Ba和Ti的全部元素仅构成由下述化学式A1表示的氧化物的假设的x[BiFeO3]-y[BaTiO3]的质量的计算值。以下,将100×MAG/MABO3表示为α。
x[BiFeO3]-y[BaTiO3](A1)
全部的起始原料和纯水通过球磨机混合10小时。将混合后的起始原料干燥后,通过起始原料的压制成型,得到预成型体。通过将预成型体以800℃进行加热,得到预烧制体。预烧制体通过球磨机进行粉碎。通过将粉碎的预烧结体干燥,得到原料颗粒。通过原料颗粒和粘合剂(聚乙烯醇)的混合物的压制成型,得到成型体。通过加热成型体,除去粘合剂。通过在脱粘合剂处理后,将成型体在1000℃的大气中烧制4小时,得到烧结体。烧结体相当于极化处理前的压电组合物。
通过使用双面研磨盘及切割锯加工烧结体,形成由烧结体构成的板。加工后的烧结体的尺寸为长16mm×宽16mm×厚0.5mm。
使用真空蒸镀装置,由Ag构成的电极分别形成于烧结体的两面。各电极的厚度为1.5μm。各电极的尺寸为15mm×15mm。
通过对被一对电极夹着的压电组合物施加直流电场,测定压电组合物的电阻率ρ(单位:Ω·cm)。直流电场为0.1kV/cm。直流电场施加到压电组合物的时间为40秒。实施例1的ρ示于表1。
通过对被一对电极夹着的烧结体施加电场,使烧结体极化。施加到烧结体的电场的强度为矫顽电场的1.5~2倍。电场向烧结体施加15分钟。上述极化处理在温度为120℃的硅油槽中实施。在极化处理后,再次测定压电组合物的电阻率ρ。极化处理后的实施例1的压电组合物的电阻率ρ为1×1012Ω·cm以上。在后述的实施例2~28情况下,极化处理后的压电组合物的电阻率ρ也为1×1012Ω·cm以上。
通过以上的方法,得到实施例1的压电组合物。基于X射线荧光分析法的分析结果是,压电组合物中的Bi、Fe、Ba和Ti的摩尔比与上述化学式A1中的Bi、Fe、Ba和Ti的摩尔比一致。化学式A1中的x和y的值与下述表1中所示的值一致。压电组合物中的Ag的质量的比例α与下述表1中所示的值一致。通过X射线衍射图谱,确认了压电组合物具有钙钛矿结构。
使用d33测量仪,测定实施例1的压电组合物的压电常数d33(单位:pC/N)。d33测量仪是用于通过基于JIS(Japanese Industrial Standards,日本工业标准)R 1696的Berlincourt法测定d33的装置。在Berlincourt法中,利用对压电组合物赋予振动时的压电正效应测定d33。因此,在Berlincourt法中,与利用对压电组合物施加电场时的压电逆效应的测定方法不同,没有电致伸缩的影响,得到压电组合物的本来的d33。实施例1的d33是下述表1中所示的值。
(实施例2~28)
通过秤量起始原料,将实施例2~28各自的x、y和α调整为下述表1~3中所示的值。
在实施例3~28中,可以使用元素D的氧化物作为起始原料。实施例3~28各自的元素D示于下述表1~3。在实施例3~28任一例的情况下,通过秤量元素D的氧化物,将100×MD/MABO3调整为规定的值。MD为起始原料中所含的元素D的质量的总计值。以下,100×MD/MABO3表示为β。实施例3~28各自的β示于下述表1~3。因为在实施例2中没有使用元素D,所以实施例2的β为零。
除了上述事项以外,通过与实施例1同样的方法,制作实施例2~28各自的压电组合物。
通过与实施例1同样的方法分析实施例2~28各自的压电组合物。在实施例2~28中任一例的情况下,压电组合物中的Bi、Fe、Ba和Ti的摩尔比都与上述化学式A1中的Bi、Fe、Ba和Ti的摩尔比一致。在实施例2~28中任一例的情况下,化学式A1中的x和y的值与下述表1~3中所示的值一致。在实施例2~28中任一例的情况下,压电组合物中的Ag的质量的比例α都与下述表1~3中所示的值一致。在实施例2~28中任一例的情况下,压电组合物中的元素D的质量的比例β都与下述表1~3中所示的值一致。在实施例2~28中任一例的情况下,都确认了压电组合物具有钙钛矿结构。
通过与实施例1同样的方法测定实施例2~28各自的压电组合物的电阻率ρ。实施例2~28各自的极化处理前的ρ示于表1~3。通过与实施例1同样的方法,测定实施例2~28各自的压电组合物的压电常数d33。实施例2~28各自的d33示于下述表1~3。
(比较例1~8)
在比较例1~8中任一例的情况下,都不使用Ag作为起始原料。在比较例1~8各自的起始原料的秤量中,将x、y和β调整成下述表4中所示的值。因为在比较例1中没有使用元素D的氧化物,所以比较例1的β为零。
除了上述的事项以外,通过与实施例1同样的方法制作比较例1~8各自的压电组合物。
通过与实施例1同样的方法,分析比较例1~8各自的压电组合物。在比较例1~8中任一例的情况下,压电组合物中的Bi、Fe、Ba和Ti的摩尔比都与上述化学式A1中的Bi、Fe、Ba和Ti的摩尔比一致。在比较例1~8中任一例的情况下,化学式A1中的x和y的值都与下述表4中所示的值一致。在比较例1~8中任一例的情况下,压电组合物中的Ag的质量的比例α都为零。在比较例1~8中任一例的情况下,压电组合物中的元素D的质量的比例β都与下述表4中所示的值一致。在比较例1~8中任一例的情况下,都确认了压电组合物具有钙钛矿结构。
通过与实施例1同样的方法,测定比较例1~8各自的压电组合物的电阻率ρ。比较例1~8各自的极化处理前的ρ示于表4。通过与实施例1同样的方法,测定比较例1~8各自的压电组合物的压电常数d33。比较例1~8各自的d33示于下述表4。
下述表1~4的判定的栏中记载的A、B、C和D如以下定义。A是指ρ为1.0×1012Ω·cm以上(1E+12Ω·cm以上),d33为160pC/N以上。B是指ρ为1.0×1012Ω·cm以上,d33为150pC/N以上且低于160pC/N。C是指ρ为1.0×1012Ω·cm以上,d33为140pC/N以上且低于150pC/N。D是指ρ低于1.0×1012Ω·cm,d33低于140pC/N。
[表1]
[表2]
[表3]
[表4]
产业上的可利用性
本发明的压电组合物例如用于压电促动器。
Claims (6)
1.一种压电组合物,其特征在于:
具有包含铋、钡、铁、钛和银的氧化物,
所述氧化物具有钙钛矿结构,
MABO3是基于假设所述压电组合物中所含的铋、钡、铁和钛的全部元素仅构成x[BimFeO3]-y[BanTiO3]的、x[BimFeO3]-y[BanTiO3]的质量的计算值,
x为0.6以上且0.9以下,
y为0.1以上且0.4以下,
x+y为1,
m为0.96以上且1.06以下,
n为0.96以上且1.06以下,
将所述银的质量表示为MAG,
100×MAG/MABO3为0.01以上且10.00以下,
至少一部分所述氧化物表示为x[BimFeO3]-y[BanTiO3],
表示所述氧化物的x[BimFeO3]-y[BanTiO3]中的Bi及Ba中的至少一元素的一部分被Ag置换。
2.根据权利要求1所述的压电组合物,其特征在于:
还包含选自钒、铌、钽、钼、钨和锰中的至少一种元素D,
所述元素D的价数为5或6,
表示所述氧化物的x[BimFeO3]-y[BanTiO3]中的Fe及Ti中的至少一元素的一部分被所述元素D置换。
3.根据权利要求1所述的压电组合物,其特征在于:
至少还包含铌作为元素D,
铌的价数为5,
表示所述氧化物的x[BimFeO3]-y[BanTiO3]中的Fe及Ti中的至少一元素的一部分被Nb置换。
4.根据权利要求2所述的压电组合物,其特征在于:
将所述元素D的质量的总计值表示为MD,
100×MD/MABO3为0.01以上且5.00以下。
5.根据权利要求1所述的压电组合物,其特征在于:
x为0.6以上且0.8以下,
y为0.2以上且0.4以下。
6.一种压电元件,其特征在于:
具有权利要求1所述的压电组合物。
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