CN1222489C - 压电陶瓷组合物和使用该压电陶瓷组合物的压电陶瓷器件 - Google Patents
压电陶瓷组合物和使用该压电陶瓷组合物的压电陶瓷器件 Download PDFInfo
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Abstract
本发明提供了具有下式的压电陶瓷组合物:{[Pb(1-15x)±(0~0.2)Lax][Ti(1-y-z)MnyCuz]O3},满足关系:0.02<x<0.14,0.01≤y<0.04和0.002≤z≤0.008。本发明的压电陶瓷组合物可以在标准大气压下稳定地烧结。即,不需要氧分压为80%或更高。此外,此组合物显示了优异的压电性能和热稳定性。因此,本发明的压电陶瓷组合物在厚度纵向三次谐振频率下具有优异的压电性能,能够产生15MHz或更高的高频,并且可以用作具有小电极面积的压电陶瓷器件的材料。
Description
技术领域
本发明涉及压电陶瓷组合物,更具体地说,涉及用其它成份代替传统的压电陶瓷成份的压电陶瓷组合物,此压电陶瓷组合物具有改进的耐热性和压电性能。
背景技术
随着近来信息工业的发展,几乎所有的电器和设备,例如硬盘驱动器(HDD)、手持电话(HHP)、光盘只读存储器(CD-ROM)、可擦写CD(CD-RW)、数字多能光盘(DVD)、可擦写DVD(DVD-RW)、无线键盘、光电鼠标等都配置有产生时钟频率的SMD型谐振器,作为数字时代的主要部件。随着数字产品性能的加强和微型化的发展,谐振器也向着更高频率和小、轻及更省电的方向发展。为了制造使用更高频率的越来越小的谐振器,需要具有优异的压电性能和热稳定性的压电陶瓷组合物。
近来主要使用Pb(Zr,Ti)O3基和PbTiO3基压电陶瓷组合物。厚度振动模式是这些压电陶瓷组合物中的具有代表性的振动模式。厚度振荡模式使用能阱振动并分为基本振动模式和更高的振动模式。
对于Pb(Zr,Ti)O3基组合物来说,与基本振动模式相比,在更高次振动模式的压电性能相当差。此外,对于高次振动模式来说,由于谐振频率常数非常小,因此难以得到高频。另一方面,PbTiO3基组合物具有低介电常数、小晶粒尺寸和高相转变温度的特性。此外,由于C轴方向大的晶格各向异性,因此难以俘获基本振动模式中的能量,但容易俘获更高次振动模式的能量,能够产生高频。基于这些事实,PbTiO3基组合物相对于Pb(Zr,Ti)O3基组合物具有优异的压电性能和热稳定性。因此,认为PbTiO3基组合物适用于高频带振荡器。
然而,由于PbTiO3基组合物具有大的结晶各向异性,因此冷却期间自然产生的相转变应力容易引起开裂,导致烧结性能变差。近来已经努力研究通过用其它成份代替A位和/或B位或者使用其它添加剂使冷却期间自然产生的相转变应力最小并且加强烧结性能。
作为代表例,日本专利公开文本No.7-206517(公开日:1995年8月8日,申请人:MATSUSHITA ELECTRIC IND CO LTD)公开了一种压电陶瓷组合物,包括(Pb,La)TiO3基主成份和CuO、ZrO2和MnO2作为添加剂。上述公开文本中的压电陶瓷组合物在谐振期间具有高的可用频率和大的D/R(能效比)。尽管有这些优点,但此压电陶瓷组合物必须在大于80%氧分压的气氛中烧结。使用此组合物作为15-18mm直径的压电陶瓷器件的材料;然而,此组合物不能用作最新的驱动硬盘的压电陶瓷器件的材料,驱动硬盘的压电陶瓷器件要具有2.5mm×2.0mm的电极面积并产生40MHz或更高的频率。当使此器件小型化时,出现一个问题是谐振期间D/R减小了,在三次谐波频率中出现乱真现象。
发明内容
因此,考虑到上述问题作出了本发明。本发明的目的是提供一种压电陶瓷组合物,用作具有小到2.5mm×2.0mm或更小的电极面积的压电陶瓷器件的材料。
本发明的另一个目的是提供一种压电陶瓷组合物,可以在标准大气压下烧结。
本发明的再一个目的是提供一种压电陶瓷组合物,具有优异的电性能(D/R=60以上)和在大约250℃或更高温度下回流的热性能。
本发明的再一个目的是提供一种压电陶瓷组合物,在厚度纵向振动三次谐波频率下显示了优异的压电性能。
本发明的另一个目的是提供一种微型压电陶瓷器件,它产生高频并能够在高温下以表面贴装的方式安装。
根据本发明,通过提供由下列通式表示的压电陶瓷组合物,可以实现上述和其它目的,此压电陶瓷组合物主要包括Pb、La、Ti、Mn和Cu:
式(1)
{[Pb(1-1.5x)±(0~0.2)Lax][Ti(1-y-z)MnyCuz]O3}
(其中,0.02<x<0.14,0.01<y<0.04并且0.002≤z≤0.008)。
根据本发明的另一方面,提供有一种微型压电陶瓷器件,此压电陶瓷器件产生高频,并能够在高温下以表面贴装的方式安装。所述压电陶瓷器件由压电陶瓷制成,其中所述压电陶瓷的组分为:
式(1)
{[Pb(1-1.5x)±(0~0.2)Lax][Ti(1-y-z)MnyCuz]O3}
其中,0.02<x<0.14,0.01≤y<0.04和0.002≤z≤0.008。
具体实施方式
由通式[Pb(1-1.5x)±(0~0.2)Lax][Ti(1-y-z)MnyCuz]O3表示本发明的压电组合物。此组合物是ABO3复合钙钛矿组合物,A位由PbO和La2O3构成,B位由TiO2、MnO2和CuO构成。与传统的组合物比较,锰(Mn)和铜(Cu)不是添加剂,而是代替钛(Ti)作为基体成份。结果,可以更稳定地调整晶粒和晶粒边界的电荷中性以及晶体结构和化学稳定性。
在上式中,A位成份镧(La)需要满足0.02<x<0.14。如果x值大于0.014,那么在由Pb占据的某些位形成空穴(cavities),这样保持电荷中性。结果,出现原子扩散以减小烧结期间由于晶体各向异性导致的内部应力,防止开裂的形成。然而,如果x值低于0.02,那么这种效果不能充分实现,如果超过0.14,那么振荡稳定性和热稳定性就会差。
在上式中,B位成份Mn和Cu少量存在,起到加强压电陶瓷组合物的电性能和热稳定性的作用。Mn需要满足0.01<y<0.04。如果y值大于0.04,那么由于Mn起电子受主的作用,存在的问题是烧结体的绝缘性能低,漏电流迅速增加,从而阻碍极化或降低压电特性。Cu需要满足0.002≤z≤0.008。在上述范围内,提供空穴,以便降低谐振电阻,这样控制漏电流量。如果z值在此范围外,压电性能低,热稳定性差。
本发明的压电陶瓷组合物烧结性能优异,这样即使在标准大气压下也能够稳定地烧结。因此,不需要在控制氧分压的气氛下烧结此组合物。此外,在高于250℃的回流下具有优异的电性能,并且即使在回流后也具有优异的稳定性。因此,它在厚度纵向振动三次谐波频率下显示了优异的压电性能,能够产生高频。而且,使用此组合物能够制造具有2.5mm×2.0mm或更小的电极面积的压电陶瓷器件。
为了实现优异的回流性能,回流必须在大约240-250℃进行,以便保持极化和大的D/R值,Tc值必须高于295℃。而且,如果D/R值低于60,电池消耗量即能量损耗大。因此,最好Tc值不仅高于295℃而且D/R值高于60。
实例
下面将参考下面的表1具体描述根据本发明的例子。
利用PbO、La2O3、TiO2、MnO2和CuO作为起始材料制备表1所示组合物。分别称取PbO、La2O3、TiO2、MnO2和CuO的重量并球磨混合。干燥混合好的浆料以便形成0.1-0.5μm粒径的粉末。注意在干燥过程中不要分层。如果出现分层,那么钙钛矿晶体形成两相,而不是单相,这对压电性能是致命的。如果粉末的平均粒径在上述范围之外,不能提供适于形成单相的能量,从而形成第二相或保留原材料粉末。
然后,在650-1,000℃煅烧粉末1-4小时。然而,如果没有形成单相,可以采用第二阶段煅烧方法。煅烧的粉末与少量的粘合剂混合,湿碎得到的产物,形成0.1-1.2μm平均粒径的粉末。然后,在1,000-1,350℃的烧结温度下在大气中烧结此粉末1-4小时,得到23mm×18mm的平板形式的烧结体。首先抛光得到的烧结体的两面,抛光到0.5mm的厚度,然后加工为其表面粗糙度优异、具有20MHz-60MHz的厚度纵向振动三次谐波频率模式的压电陶瓷。然后,在压电陶瓷的两面形成0.5-1.5mm直径的电极,制造成压电陶瓷样品。在100-250℃,在硅油中给样品施加3-10kVmm的电场,施加10-30分钟,从而极化该样品。
测量每个样品的下列参数:谐振频率(Fr)、反谐振频率(Fa)、谐振电阻(Zr)和反谐振电阻(Za);其中用阻抗分析仪(产品:HP4194A)在厚度纵向振动三次谐波频率的谐振频率下进行所有的测试。
在目前的试验中,得到了测得的D/R(能效比)、谐振频率系数(TCF)、相转变温度(Tc)和回流后在相转变温度(ΔFOSC)振荡频率的变化,而没有测量介电常数、机电耦合系数(Kt)和机械品质因数(Qm)。D/R是确定实际振荡器的振荡电路在工作期间的输出水平的因数,TCF对振荡稳定性是至关重要的。
D/R值是确定由下列等式表示的输出水平的因数。在例子中,利用厚度纵向振荡三次谐波频率模式在I.R.E.上测量D/R值。
利用下式根据在40-90℃测得的谐振频率(Fr)计算谐振频率(TCF)的温度系数:
表1示出了具有不同成分的每个压电陶瓷样品以及它们的压电性能和热性能。
表1
样品 | [Pb(1-1.5x)±(0~0.2)Lax][Ti(1-y-z)MnyCuz]O3 | D/R(dB) | TCF(ppm/℃) | Tc(℃) | ΔFosc(%) | 注释 | ||
x | y | z | ||||||
1*2*3*4*5*6*789*10*11121314*15*1617*18*19*20*21*22*23*24*25* | 0000.010.020.020.030.070.070.070.110.110.110.110.110.130.140.140.140.140.140.140.160.180.20 | 00.010.10.010.10.010.010.020.040.0010.010.020.030.040.10.010.010.020.030.040.060.080.010.060.08 | 000.010.0020.0110.0020.0030.0050.0110.10.0020.0050.0080.010.0150.0060.0020.0050.0080.010.020.100.0020.0150.10 | 27515061635525606672534860536356504844604854 | 12151314172825263230303331364240404352464852 | 390354350349345342345300300295290291296270264260260257251255241240 | 0.010.020.020.010.010.070.090.070.110.130.140.450.151.451.381.340.91.00.82.160.90.9 | 不可烧结不可烧结不可烧结 |
26*27*28*29*30*31* | 0.200.200.200.200.200.20 | 0.010.020.040.060.080.10 | 0.0020.0050.0080.0150.0150.10 | 606058534851 | 565250505358 | 227226224223221220 | 0.70.90.80.80.70.9 |
(比较例用星号(*)表示)
从表1可以看出,满足0.02<x<0.14,0.01≤y<0.04和0.002≤z≤0.008,可以在标准大气压下烧结本发明的压电陶瓷成分,并且可以用作具有小到2.5mm×2.0mm电极面积的压电器件的材料。而且,在x、y和z的预定范围内,保持D/R值高于60dB,每种组合物的相转变温度(Tc)高于295℃。除此以外,此组合物显示了回流后在每种组合物的相转变温度下振荡频率的变化(ΔFOSC)为±1%和谐振频率(TCF)的温度系数低于60ppm/℃的特性。
可以稳定地烧结压电陶瓷组合物,并且在厚度纵向振动三次谐波频率显示了优异地压电性能。能够产生高于15MHz的高频。
镧能够减小内部应力,因此防止在2-14摩尔%范围内开裂的形成。如果镧的含量超过2摩尔%,那么烧结性能会加强并且D/R增加,而如果超过14摩尔%,那么谐振频率(TCF)的温度系数在高于60ppm/℃的范围外,而且减小了相转变温度。
需要锰的含量为1-4摩尔%。在此范围内,谐振电阻低,确保改进的压电性能,并且增强了耐热性,确保热稳定性。如果锰含量低于1摩尔%,其效果不明显,如果超过4摩尔%,由于绝缘电阻,漏电流量迅速增加,从而阻碍压电的形成。
组合物中的铜成分是四价金属元素。它提供了晶体结构中的空穴,从而降低了谐振电阻,控制了漏电流量。当它的含量增加时,谐振频率的温度系数趋于稍稍降低。如果铜含量低于0.2摩尔%,其效果不明显,而如果含量超过0.8摩尔%,则压电性能差。
为了说明尽管已经公开了本发明的最佳实施例,但本领域技术人员应理解,在不离开如附加的权利要求所公开的本发明的范围和精神的情况下,各种修改、添加和置换都是可能的。
如上所述,本发明的压电陶瓷组合物可以在标准大气压下稳定地烧结。即,不需要氧分压为80%或更高。此外,此组合物在250℃或更高的回流温度下不仅显示了高达60db或更高的电性能,而且具有优异的热稳定性。可以得到回流后振荡频率变化为±1、谐振频率的温度系数高达30ppm/℃这样优异的压电陶瓷组合物。
因此,本发明的压电陶瓷组合物在厚度纵向三次谐振频率具有优异的压电性能,能够产生15MHz或更高的高频,并且可以用作具有小电极面积的压电陶瓷器件的材料。
Claims (2)
1.一种压电陶瓷组合物,具有式(1):
式(1)
{[Pb(1-1.5x)±(0~0.2)Lax][Ti(1-y-z)MnyCuz]O3}
其中,0.02<x<0.14,0.01≤y<0.04和0.002≤z≤0.008。
2.一种压电陶瓷器件,所述压电陶瓷器件由压电陶瓷制成,其中所述压电陶瓷的组分为:
式(1)
{[Pb(1-1.5x)±(0~0.2)Lax][Ti(1-y-z)MnyCuz]O3}
其中,0.02<x<0.14,0.01≤y<0.04和0.002≤z≤0.008。
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