CN105461303B - 压电组合物、压电元件和溅射靶材 - Google Patents

压电组合物、压电元件和溅射靶材 Download PDF

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CN105461303B
CN105461303B CN201510617259.5A CN201510617259A CN105461303B CN 105461303 B CN105461303 B CN 105461303B CN 201510617259 A CN201510617259 A CN 201510617259A CN 105461303 B CN105461303 B CN 105461303B
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piezoelectric
formula
composition
composite oxides
piezoelectric composition
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CN105461303A (zh
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七尾胜
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TDK Corp
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Abstract

本发明的目的在于提供在‑40℃～85℃的温度区域中压电特性的温度变化率小的压电组合物以及具备它们的压电元件、或者溅射靶材。所述压电组合物以(K1‑x‑yNaxLiy)q(Nb1‑zTaz)O3…(1)(0.20≤x≤0.80，0.02≤y≤0.10，0.01≤z≤0.30，0.800≤q≤1.050)、SrZrO3…(2)、Ba(Nb1‑ wTaw)2O6…(3)(0.01≤w≤0.30)、(Bi0.5Na0.5)TiO3和/或(Bi0.5K0.5)TiO3…(4)、(1‑m‑n‑p)A+mB+nC+pD…(5)(A表示(1)所示的复合氧化物，B表示(2)所示的复合氧化物，C表示(3)所示的复合氧化物，D表示(4)所示的复合氧化物，0.04≤m≤0.07，0<n≤0.010，0.001≤p≤0.020)为主成分。

Description

压电组合物、压电元件和溅射靶材
技术领域
本发明涉及压电组合物和具备压电组合物的压电元件、或者溅射 靶材。
背景技术
利用了压电组合物的驱动器是利用了施加电场时会产生机械应变 和应力这样的压电现象而成的。该驱动器能够高精度地得到微小位移， 并且具有产生应力大等的特征，例如可以用于精密机床或光学装置的 定位。作为驱动器中使用的压电组合物，可以列举锆钛酸铅 (Pb(Zr,Ti)O3)。
然而，由于锆钛酸铅类压电组合物包含很多Pb，因此，最近存在 由酸雨导致的Pb溶出等对地球环境造成不良影响的问题。因此，期望 替代锆钛酸铅类压电组合物而开发不含有Pb的非铅类压电组合物。
例如，在专利文献1和2中，公开了居里温度高达350℃以上且机 电耦合系数kr也优异的由铌酸钠钾锂构成的非铅类压电组合物。
另外，在专利文献3和4中，作为表现比较大的位移量的非铅类 压电组合物，公开了铌酸钠钾锂类的压电组合物、以及含有钨青铜型 氧化物和钙钛矿型氧化物的压电组合物。
现有技术文献
专利文献
专利文献1：日本特开昭49-125900号公报
专利文献2：日本特公昭57-6713号公报
专利文献3：国际公开第2008/152851号
专利文献4：日本专利第4513948号公报
发明内容
发明所要解决的技术问题
在民生、工业用电子设备所使用的驱动器或传感器等的用途中， 要求特别是-40℃～85℃的温度区域中压电特性的温度变化率小。
然而，在专利文献1～4的任一者中，尽管在非铅类压电组合物中 得到优异的压电特性，但是对于压电特性相对于温度的变化，都没有 进行研究。
本发明是鉴于上述的状况而完成的，其目的在于提供具有优异的 压电特性的环境友好型的压电组合物，并且在-40℃～85℃的温度区域 中压电特性的温度变化率小的压电组合物以及具有它们的压电元件或 者溅射靶材。
解决技术问题的手段
本发明人为了解决上述技术问题，进行具有优异的压电特性的环 境友好型的压电组合物，在-40℃～85℃的温度区域中压电特性的温度 变化率小的压电组合物的验证，发现了与现有的组成范围不同的压电 组合物。
即，压电组合物是以式(5)所示的组合物为主成分的压电组合物， 该式(5)所示的组合物包含下述式(1)所示的第1钙钛矿型氧化物、 下述式(2)所示的第2钙钛矿型氧化物、下述式(3)所示的钨青铜 型氧化物、以及下述式(4)所示的第3钙钛矿型氧化物。
(K1-x-yNaxLiy)q(Nb1-zTaz)O3···(1)
(其中，式中x为0.20≤x≤0.80，y为0.02≤y≤0.10，z为0.01 ≤z≤0.30，q为0.800≤q≤1.050)
SrZrO3···(2)
Ba(Nb1-wTaw)2O6···(3)
(其中，式中w为0.01≤w≤0.30)
(Bi0.5Na0.5)TiO3和/或(Bi0.5K0.5)TiO3···(4)
(1-m-n-p)A+mB+nC+pD···(5)
(其中，式中A表示上述式(1)所示的复合氧化物，B表示上述 式(2)所示的复合氧化物，C表示上述式(3)所示的复合氧化物，D 表示上述式(4)所示的复合氧化物，式中m为0.04≤m≤0.07，n为 0<n≤0.010，p为0.001≤p≤0.020)。
通过成为上述的组成范围，能够得到具有优异的压电特性的环境 友好型的压电组合物，并且在-40℃～85℃的温度区域中压电特性的温 度变化率小的压电组合物。
进一步，作为副成分，优选包含锰(Mn)和铜(Cu)中的至少一 种，并且在将所述副成分分别换算成氧化锰(MnO)、氧化铜(CuO) 时成为下述式(6)所示的压电组合物。由此，能够提高压电组合物的 电阻率，可以进行施加更高电场的极化处理，因此，能够得到更良好的压电特性。
(1-s)E+sF···(6)
(其中，式中E表示上述式(5)所示的主成分的复合氧化物，F 表示所述副成分，式中s为0＜s≤0.015)。
在主成分即复合氧化物的晶粒的晶界具有锰(Mn)和铜(Cu)中 的至少一种元素偏析的微细结构，由此可以提高压电组合物的电阻率， 能够得到偏差少的稳定的压电组合物。
另外，在本发明中，能够提供具备上述压电组合物并且具有优异 的压电特性的环境友好型的压电组合物中在-40℃～85℃的温度区域中 压电特性的温度变化率小的压电元件。进一步，利用使用上述压电组 合物而制作的溅射靶材，能够提供在所制作的压电元件中也具有优异 的压电特性且在环境友好型的压电组合物中在-40℃～85℃的温度区域中压电特性的温度变化率小的压电元件。
发明的效果
根据本发明，能够提供具有优异的压电特性的环境友好型的压电 组合物并且在-40℃～85℃的温度区域中压电特性的温度变化率小的压 电组合物、以及具备它们的压电元件或者溅射靶材。
附图说明
图1是表示使用了本发明的实施方式所涉及的压电组合物的压电 元件的结构图。
符号的说明：
1……压电基板
1a,1b……相对面
2,3……电极
具体实施方式
以下，根据需要参照附图，就本发明的优选的实施方式进行详细 地说明。
本实施方式的压电组合物是以式(5)所示的组合物为主成分的压 电组合物，该式(5)所示的组合物包含下述式(1)所示的第1钙钛 矿型氧化物、下述式(2)所示的第2钙钛矿型氧化物、下述式(3) 所示的钨青铜型氧化物、以及下述式(4)所示的第3钙钛矿型氧化物。另外，在本实施方式中，主成分是指包含压电组合物整体的98mol％以 上的成分。
(K1-x-yNaxLiy)q(Nb1-zTaz)O3···(1)
(其中，式中x为0.20≤x≤0.80，y为0.02≤y≤0.10，z为0.01 ≤z≤0.30，q为0.800≤q≤1.050)
SrZrO3···(2)
Ba(Nb1-wTaw)2O6···(3)
(其中，式中w为0.01≤w≤0.30)
(Bi0.5Na0.5)TiO3和/或(Bi0.5K0.5)TiO3···(4)
(1-m-n-p)A+mB+nC+pD···(5)
(式中，A表示上述式(1)所示的复合氧化物，B表示上述式(2) 所示的复合氧化物，C表示上述式(3)所示的复合氧化物，D表示上 述式(4)所示的复合氧化物，式中m为0.04≤m≤0.07，n为0<n≤0.010， p为0.001≤p≤0.020)。
上述式(1)中，钠(Na)的量即x为0.20≤x≤0.80。通过优选 满足0.40≤x≤0.70，能够成为在压电特性方面更优异的压电组合物。 如果x超过0.80，则压电特性降低；在小于0.20的情况下，钾(K) 的量相对较多，烧成时钾(K)的挥发剧烈，从而变得难以烧成。
上述式(1)中，锂(Li)的量即y为0.02≤y≤0.10。通过优选满 足0.03≤y≤0.08，能够成为压电特性更优异的压电组合物。如果y超 过0.10，则电阻率降低，无法在足够的电场下进行极化处理，因而压 电特性降低。另外，在小于0.02的情况下，也得不到高的压电特性。
上述式(1)和(3)中，钽(Ta)的量即z、w为0.01≤z、w≤0.30。 通过优选满足0.04≤z、w≤0.25、更优选满足0.05≤z、w≤0.15，能够 成为压电特性更优异的压电组合物。如果z、w超过0.30，则居里温度 降低，并且压电特性减小；在0的情况下得不到高的压电特性。
上述式(1)中的q即第1钙钛矿型氧化物的A位点与B位点之 比为0.800≤q≤1.050。通过优选满足0.850≤q≤1.030、更优选满足 0.900≤q≤1.000，能够成为压电特性更优异的压电组合物。如果q小 于0.800或者q超过1.050，则烧结性差且得不到高的压电特性。
上述式(5)中，锶(Sr)和锆(Zr)的量即m为0.04≤m≤0.07。 优选为0.04≤m≤0.06。通过满足其，能够抑制由温度变动所导致的压 电特性的降低。如果m超过0.07，则烧结变得困难，在小于0.04的情 况下不能得到高的压电特性。
上述式(5)中，钡(Ba)、铌(Nb)和钽(Ta)的量即n为0<n ≤0.010。通过优选满足0.001≤n≤0.008、更优选满足0.003≤n≤0.007， 能够成为压电特性更优异的压电组合物。在n为0的情况下和超过 0.010的情况下，不能得到高的压电特性。
上述式(5)中，铋(Bi)、钠(Na)或钾(K)、和钛(Ti)的量 即p为0.001≤p≤0.020。通过优选满足0.005≤p≤0.020、更优选满足 0.005≤p≤0.015，能够得到压电特性高且由温度所导致的变化小的压 电组合物。在p为0的情况下，压电特性的温度所导致的变化变大。另外，如果p超过0.020，则居里温度变低，并且不能得到高的压电特 性。
进一步，作为副成分，优选包含锰(Mn)和铜(Cu)中的至少一 种，并且在将所述副成分分别换算成氧化锰(MnO)、氧化铜(CuO) 时成为下述式(6)所示的压电组合物。由此，能够提高压电组合物的 电阻率，可以进行施加更高电场的极化处理，因而可以得到更良好的压电特性。
(1-s)E+sF···(6)
(其中，式中E表示上述式(5)所示的主成分的复合氧化物，F 表示所述副成分，式中s为0＜s≤0.015)。
在主成分即复合氧化物的晶粒的晶界具有锰(Mn)和铜(Cu)中 的至少一种元素偏析的微细结构，由此可以提高压电组合物的电阻率， 能够得到偏差少的稳定的压电组合物。
至此所说明的压电组合物例如可以通过如下的方式进行制造。
首先，作为压电组合物的主成分和副成分的原料，分别准备例如 包含钠(Na)、钾(K)、锂(Li)、铌(Nb)、钽(Ta)、锶(Sr)、锆 (Zr)、钡(Ba)、铋(Bi)、钛(Ti)和锰(Mn)的化合物粉末。另外， 作为成为这些原料的化合物，可以使用各自的元素的氧化物或者复合 氧化物、或者通过加热成为氧化物的例如碳酸盐或草酸盐等化合物。 接着，使这些原料充分干燥之后，以最终组成为上述范围内那样的比 率称量。
接着，将这些材料使用球磨机或珠磨机等在有机溶剂中或水中进 行混合。
其后，将该混合物干燥，压制成型或者填充于陶瓷制容器等耐热 性容器等，在700℃～1100℃下预烧1～8小时。预烧的次数可以为1次， 或者也可以在将所得到的预烧物粉碎后，再次压制成型或者填充于耐 热性容器等反复预烧。
预烧后，例如将该预烧物通过球磨机或珠磨机等在有机溶剂中或 水中进行粉碎、干燥，由此得到压电组合物材料粉末。本发明的一个 实施方式所涉及的压电组合物通过将所述压电组合物材料粉末进行烧 结而得到。
例如，在压电组合物材料粉末中添加粘合剂进行造粒，使用单轴 压制成型机或冷等静压成型机(CIP：Cold Isostatic Pressing)等将该造 粒粉压制成型。成型后，例如对该成型物进行加热进行脱粘合剂，进 一步在950℃～1350℃下烧成2～8小时，由此得到压电组合物。
另外，该压电组合物可以包含Pb，但是其含量优选为1mol％以下， 如果不含有Pb则更优选。原因在于，能够将烧成时Pb的挥发、以及 在作为压电部件在市场流通并废弃后Pb向环境中的放出抑制到最小限 度，从而从低公害化、对环境性和生态学的立场来看更优选。该压电 组合物优选用作例如作为压电元件的驱动器等振动元件、发声器或传 感器等的材料。另外，也可以适用于溅射靶材或使用其的压电薄膜元 件。
图1表示使用了本实施方式所涉及的压电组合物的压电元件的一 个结构例。该压电元件具备由本实施方式的压电组合物构成的压电基 板1、以及分别设置于该压电基板的一对相对面1a,1b的一对电极2,3。 压电基板通过例如向厚度方向即电极2,3的相对方向极化，并且经由电 极2,3而施加电压，从而压电基板向厚度方向纵向振动和向径向拉伸振动。
电极2,3分别由例如银(Ag)、金(Au)等金属构成。在这些电极 2,3上经由导线等与外部电源电连接(没有图示)。
这样的压电元件可以通过例如根据需要对本实施方式的压电组合 物进行加工来形成压电基板1，设置电极2,3，并通过在加热后的硅油 中施加电场来进行极化处理，由此来进行制造。
以上，就本发明的优选的实施方式进行了说明，但是本发明并不 被限定于上述实施方式。例如，在上述实施方式中使用了固相反应法 作为压电组合物材料粉末的制造方法，但是也可以是使用水热合成法 或气相生长法等而制作的压电元件。
实施例
以下，基于实施例和比较例来更具体地说明本发明，但是本发明 并不被限定于以下的实施例。
(实施例1～5、26、27、比较例1～2)
首先，作为主成分和副成分的原料，准备碳酸钠(Na2CO3)粉末、 碳酸钾(K2CO3)粉末、碳酸锂(Li2CO3)粉末、氧化铌(Nb2O5)粉 末、氧化钽(Ta2O5)粉末、碳酸钡(BaCO3)、氧化锆(ZrO2)粉末、 碳酸锶(SrCO3)粉末、氧化铋(Bi2O3)粉末、氧化钛(TiO2)粉末、 以及碳酸锰(MnCO3)粉末或氧化铜(CuO)粉末。使这些原料充分 干燥后，以压电组合物的组成成为实施例1～5、26、27和比较例1～2 的组成、即p的值变化的方式称量各原料。
使用球磨机在乙醇中将这些原料混合之后，在80～120℃的恒温槽 中使之充分干燥，进行压制成型，并在750～1050℃下预烧1～4小时。 将该预烧物使用球磨机在乙醇中进行粉碎后，再进行干燥来制作压电 组合物材料粉末。
接着，在压电组合物材料粉末中添加粘合剂(丙烯酸树脂)来进 行造粒。将该造粒粉通过单轴压制成型机在约25MPa的压力下成型为 直径17mm的圆板状小球(pellet)。
成型后，将该成型体在550℃下加热3小时进行脱粘合剂，进一步 在1050～1200℃下烧成2小时。其后，将该烧成体加工成厚度0.6mm 的圆板状制作压电基板1，在两面真空蒸镀银(Ag)从而形成电极2,3。 其后，在150℃的硅油中施加5MV/m的电场10～30分钟进行极化处理， 成为压电元件。
将所得到的压电元件放置24小时后，测定20℃下的相对介电常数 (εr)和机电耦合系数(kr)。在εr和kr的测定中使用阻抗分析仪4294A (Agilent Technologies Ltd.制造)，并且使用共振和反共振法，在εr的 测定中频率为1kHz。已知表示压电元件的位移量的压电应变常数d常 数与εr 1/2×kr成比例，作为压电特性，评价εr 1/2×kr。进一步，压电特性的由温度导致的变化以JISC60068-2-1和JISC60068-2-2标准为依据， 以20℃为基准评价在-40℃～85℃的温度区域中的εr 1/2×kr的变化率。
(评价结果)
将各实施例和比较例的压电组合物的组成、20℃下的相对介电常 数(εr)、机电耦合系数(kr)、εr 1/2×kr和以20℃为基准在-40℃～85℃的 温度区域中的εr 1/2×kr的变化率的绝对值的最大值表示在表1中。压电 特性优选高，因而，将εr 1/2×kr的值为12以上判定为优选并记为○，将 小于12的判定为不优选并记为×。温度变化率优选小，因而将εr 1/2×kr的温度变化率的绝对值的最大值为10％以下判定为更优选并记为◎， 将大于10％且20％以下判定为优选并记为○，将大于20％的情况判定 为不优选并记为×。
在组成分析中，使用ICP-AES装置ICPS-8100CL(岛津制作所制 造)和荧光X射线分析装置ZSZ-100e(Rigaku制造)，将锂(Li)通 过ICP-AES来进行分析，将其以外的元素通过荧光X射线分析来进行 分析。
对于实施例1～5、26、27和比较例1～2，将p的值以及εr、kr、压 电特性的温度变化率表示在表1中。根据表1可知，与p即铋(Bi)、 钠(Na)和/或钾(K)和钛(Ti)的量小于0.001的比较例1相比，0.001 以上且0.020以下的范围的实施例1～5和26、27的压电特性的温度变 化率小。另外，可知在p的值超过0.020的比较例2中，压电特性变低。
(实施例6～22、比较例3～14)
另外，除了称量各原料以使x、y、z、m、n、q的值变化以外，通 过与实施例1～5同样的方法，制作实施例6～22、比较例3～14的样品、 并进行评价，将其结果也表示在表1中。
在x即钠(Na)的量为0.20以上且0.80以下的情况，y即锂(Li) 的量为0.02以上且0.10以下的情况，z、w即钽(Ta)的量为0.01以 上且0.30以下的情况，m即锶(Sr)和锆(Zr)的量为0.04以上且0.07 以下的情况，n即钡(Ba)、铌(Nb)和钽(Ta)的量为0.010以下的 情况，q即钙钛矿结构氧化物的A位点与B位点之比为0.800以上且 1.050以下的情况下，如表1所示，可知压电特性高，且-40℃～85℃的 温度区域中的压电特性的温度变化率小。然而，如比较例3～14那样如 果在这些的范围外，则可知压电特性的温度变化率大或者压电特性低。
(实施例23～25、比较例15)
另外，除了以作为添加物的氧化锰(MnO)的量变化的方式进行 称量以外，通过与实施例1～5同样的方法，制作实施例23～24、比较例 15的样品，并进行评价，将其结果也表示在表1中。另外，在实施例 25中，替代氧化锰(MnO)而称取并添加氧化铜(CuO)，以与实施例 1～4同样的方法制作样品，进行评价，并将其结果也表示在表1中。
如实施例23所示，可知在不添加氧化锰(MnO)、氧化铜(CuO) 的情况下，如果其它组成在规定的范围内，则压电特性优异，并且在 使用温度区域中由温度所导致的变化小。另外，如实施例24所示，可 知氧化锰(MnO)添加量s即使为s＝0.015，压电特性也优异并且在使 用温度区域中由温度导致的变化小。然而，如果氧化锰(MnO)添加 量s超过0.015且为0.020，则如比较例15所示压电特性下降。另外， 如实施例25所示，即使替代氧化锰(MnO)而添加氧化铜(CuO)也 可以得到与氧化锰(MnO)同样的效果。
上述如表1所示可知，如果在权利要求所记载的组成的范围内， 则压电特性高，且-40℃～85℃的温度区域中的压电特性的温度变化率 小。另一方面，可知如果组成为权利要求所记载的范围外，则压电特 性的温度变化率大，或者压电特性低。
以上，列举了实施方式和实施例来说明本发明，但是本发明并不 限定于实施方式和实施例，可以进行各种变形。
此外，在上述实施方式中，列举单板结构的压电元件为例进行了 说明，但是对于具有层叠结构等其它结构的压电元件，也同样能够应 用本发明。另外，尽管作为压电元件列举了驱动器等振动元件、发声 器和传感器为例，但是对于其它压电元件也可以应用本发明。另外， 也可以应用于溅射靶材或使用它而制作的压电元件。
产业上的可利用性
可以用于驱动器等振动元件、发声器和传感器等压电元件。

Claims (4)

1.一种压电组合物，其特征在于，
以式(5)所示的组合物为主成分，
所述式(5)所示的组合物包含下述式(1)所示的第1钙钛矿型氧化物、下述式(2)所示的第2钙钛矿型氧化物、下述式(3)所示的钨青铜型氧化物、以及下述式(4)所示的第3钙钛矿型氧化物，
(K1-x-yNaxLiy)q(Nb1-zTaz)O3…(1)
其中，式中x为0.20≤x≤0.80，y为0.02≤y≤0.10，z为0.01≤z≤0.30，q为0.800≤q≤1.050，
SrZrO3…(2)
Ba(Nb1-wTaw)2O6…(3)
其中，式中w为0.01≤w≤0.30，
(Bi0.5Na0.5)TiO3和/或(Bi0.5K0.5)TiO3…(4)
(1-m-n-p)A+mB+nC+pD…(5)
式中，A表示上述式(1)所示的复合氧化物，B表示上述式(2)所示的复合氧化物，C表示上述式(3)所示的复合氧化物，D表示上述式(4)所示的复合氧化物，式中m为0.04≤m≤0.07，n为0<n≤0.010，p为0.001≤p≤0.020。
2.根据权利要求1所述的压电组合物，其特征在于，
进一步包含锰(Mn)和铜(Cu)中的至少一种作为副成分，并且在将所述副成分分别换算成氧化锰(MnO)、氧化铜(CuO)时为下述式(6)所示的压电组合物，
(1-s)E+sF…(6)
其中，式中E表示上述式(5)所示的主成分的复合氧化物，F表示所述副成分，式中s为0＜s≤0.015。
3.一种压电元件，其特征在于，
在压电基板的表面形成有外部电极的压电元件中，该压电基板由权利要求1或2所述的压电组合物形成。
4.一种溅射靶材，其特征在于，
由权利要求1或2所述的压电组合物形成。
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