CN1064938C - 压电陶瓷及其制备方法 - Google Patents
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- 229910052719 titanium Inorganic materials 0.000 claims abstract description 6
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- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
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Abstract
一种机械品质因子Qm小,耐热性优良的压电陶瓷,例如群延迟时间特性平坦和相位失真小并可适用于表面安装的滤波元件中所用的压电陶瓷,以及稳定地制造这种压电陶瓷的方法。使氧化锰和氧化铅以高浓度(相对于压电陶瓷晶体内的晶粒中而言)共存于至少含有铅、锆和钛的复合氧化物的压电陶瓷的晶粒边界部分。其制造方法是将锰化合物和铅化合物粘附于压电陶瓷的表面,然后进行热处理,使金属氧化物扩散至该压电陶瓷的晶粒边界部分。
Description
本发明涉及特别要求耐热的、用于表面安装型压电元件的压电陶瓷及其制备方法。
作为陶瓷滤波器等器件中的压电陶瓷,过去广泛应用的是主要由锆钛酸铅(如Pb(TixZr1-x)O3或PZT)之类材料组成的压电陶瓷。
具有平坦的群延迟时间(GDT)特性和小的相位失真等优良特性的陶瓷滤波器中所用的材料,要求其机械品质因子Qm小。曾试验添加各种微量添加剂以改进其压电特性。已知的材料有加入了氧化铌,氧化锑,氧化钽之类添加剂的锆钛酸铅以及其中部分铅原子被稀土元素取代的锆钛酸铅。
但是,上述这些Qm小的压电陶瓷,即使其居里温度高,仍然具有缺点,即当形成在压电陶瓷两边的电极之间的间隙开路时,随着温度的上升,其电气机械耦合因子K下降而且其谐振和反谐振频率显著偏移(虽然在闭路时情况良好)。因此它们用作表面安装型滤波器时会有问题,就是在进行回流焊接(reflowsoldering)受到高温时(约250℃)其滤波特性会显著变坏。
日本专利公开平6-1655至1657号揭示,将锰化合物由Qm数值小、居里温度高的压电陶瓷的表面热扩散,使氧化锰不均匀分布在晶粒边界层,可降低晶粒边界部分的电阻率和提高耐热性,以解决上述问题。
但是在制造方面的问题是,当将锰化合物由压电陶瓷表面进行热扩散时,如果热扩散炉中的温度分布宽,或者在制造过程中由于蒸发等原因而使PZT系统压电陶瓷中的Pb数量波动,压电陶瓷的特性变化很大。而且晶粒边界部分的电阻率降低以及耐热性的提高也不足够。
因此,本发明的目的是提供一种压电陶瓷以解决上述问题,这种压电陶瓷的机械品质因子Qm小而且具有优良的耐热性,例如群延迟时间特性平坦和相位失真小并可适用于表面安装的滤波元件中所用的压电陶瓷,以及稳定地制造这种压电陶瓷的方法。
本发明的压电陶瓷的特征是,氧化锰和氧化铅以高浓度(与至少含有铅、锆和钛的复合氧化物的压电陶瓷晶体内的晶粒中相比)共存于这种压电陶瓷的晶粒边界部分。
本发明的压电陶瓷的制造方法的特征是,在至少含有铅、锆和钛的复合氧化物的压电陶瓷的表面粘附锰化合物和铅化合物,然后进行热处理,使金属氧化物扩散到压电陶瓷的晶粒边界部分。
由于氧化锰和氧化铅以高浓度(相对于压电陶瓷晶体内的晶粒中而言)共存于压电陶瓷晶粒的边界,就使压电陶瓷的电阻率下降,耐热性提高。
此外,在本发明的制造方法中,当将锰和铅的化合物粘附于压电陶瓷表面然后对其进行热处理时,在扩散温度下铅化合物熔化在压电陶瓷的表面(例如,氧化铅的熔点是890℃)。因此,锰化合物可容易地迁移到压电陶瓷的晶粒边界部分,所以它可在很宽的温度范围内均匀扩散。而且,即使压电陶瓷晶粒边界部分铅的数量较少,熔化在表面的铅化合物也可促进锰化合物扩散到晶粒边界。
参照下面的说明和附图,将可更清楚地看到本发明的上述优点和其它优点。
图1显示了电阻率ρ随扩散温度的变化;
图2显示了电气机械耦合因子K随扩散温度的变化。
以下通过实施例更具体地说明本发明。
首先,以可制得机械品质因子Qm小的压电陶瓷的组分PbO,SrCO3,La2O3,TiO2和ZrO2等的粉末作为原料。称量各种粉末,以便制得组成为(Pb0.95Sr0.03La0.02)(Zr0.51Ti0.49)O3的陶瓷,然后加入水,在球磨机中进行湿磨混合。
将这样得到的混合物干燥,然后在800-900℃煅烧2小时。再将煅烧后的材料用球磨机粉碎制得原料粉。
在原料粉中加入水或聚乙烯醇之类的结块剂,用压机模压以后,在1150-1250℃的温度下烧结2小时,得到20×30毫米和0.75毫米厚的矩形片状陶瓷。
同时,用清漆把MnCO3和PbO粉末揉捏在一起,得到一种糊料。
然后,用丝网印刷法将所得的糊料涂敷在陶瓷的表面,让它干燥,再在约850-1100℃热处理2小时,使锰化合物扩散。此后,将该陶瓷片抛光至厚度为0.5毫米厚,在其两边表面涂敷银电极并焙烧。然后在绝缘油中2-3千伏/毫米的电场下对它进行极化处理30分钟(温度:室温-100℃),以得到压电陶瓷。
另外,只用MnCO3粉而不用PbO粉和清漆揉合,涂敷在相同形状的压电陶瓷的表面上,制成样品进行测试,作为以MnCO3,PbO粉和清漆揉合而制得的样品的对比例。
将这些样品分别切成5×5毫米的方片形,测量其电阻率ρ和传播振动时的电气机械耦合因子K。
根据测量结果,图1显示了电阻率ρ随扩散温度的变化;图2显示了电气机械耦合因子K随扩散温度的变化。
从图1可见,使用含有锰化合物和铅化合物的糊料的实施例,与使用只含锰化合物而不含铅化合物的糊料的对比例相比,电阻率ρ在扩散温度的低温侧下降更多。
而由图2可见,使用含有锰化合物和铅化合物的糊料的实施例,与使用只含锰化合物而不含铅化合物的糊料的对比例相比,电气机械耦合因子K在扩散温度的大部分范围内都较大。
于是,根据本发明,锰和铅的氧化物以高浓度(与压电陶瓷晶体内的晶粒中相比)共存于至少包含铅、锆和钛的复合氧化物的压电陶瓷的晶粒边界部分的压电陶瓷,可在把锰化合物和铅化合物粘附在压电陶瓷表面以后,进行热处理,将金属氧化物扩散至该压电陶瓷的晶粒边界部分而制得。因而可在所述扩散温度范围内获得压电陶瓷所需的电阻率ρ低和电气机械耦合因子K大等特性。
应当说明,虽然以上实施例中糊料是用丝网印刷法涂敷在陶瓷表面的,但本发明中的涂敷方法并不仅限于该种方法,也可使用刷涂、喷涂等其他粘附方法。
另外,上面实施例中使用了组成为(Pb0.95Sr0.03La0.02)(Zr0.51Ti0.49)O3的陶瓷,但本发明并不仅限于这种陶瓷,它可以是具有其它成分的二组元或三组元系统PZT陶瓷,或是上述陶瓷中的一部分铅(即其中的主要物质)被Sr,Ba,Ca,La之类物质取代的材料。
在以上各实施例中,使用了碳酸锰和氧化铅,但本发明并不限于使用这些化合物。可以使用加热时会生成氧化物的其它锰和铅的化合物或其各种混合物。加热温度一般为约900-1100℃,但本发明并不限于这温度范围。加热较好是在920-1000℃进行。本发明中所用的锰化合物和清漆可在其中加入适当的铅化合物。存在于陶瓷内的锰化合物或氧化锰的数量,按MnO2计算,一般约为陶瓷重量的0.005-0.5%,较好约为0.005-0.3%。存在于陶瓷内的氧化铅的数量,一般等于或低于约5%(摩尔),较好等于或低于约3%(摩尔)。锰和铅的化合物粘附于压电陶瓷表面的方式也并无限制。
如上所述,不论在扩散炉的温度分布不匀或Pb数量波动的情况下,本发明都能使压电陶瓷的电阻率降低,使其耐热性提高,并使锰化合物在热扩散至PZT压电陶瓷时总能稳定地扩散。
因此,得到了一种机械品质因子Qm小、电阻率低而且具有优良的耐热性的压电陶瓷,例如群延迟时间特性平坦和相位失真小并可适用于表面安装的滤波元件中所用的压电陶瓷,并能稳定地制造这种压电陶瓷。
以上说明了较佳实施例,但本领域的技术人员可在下列权利要求所限定的本发明的范围内作各种改变。
Claims (19)
1.一种压电陶瓷,它是至少包含铅、锆和钛的复合氧化物,其特征在于在所述压电陶瓷的晶粒边界部位存在氧化锰和氧化铅,其浓度高于在该压电陶瓷晶体内晶粒中的浓度。
2.如权利要求1所述的压电陶瓷,其特征在于所述陶瓷是一种PZT陶瓷。
3.如权利要求1所述的压电陶瓷,其特征在于其中氧化锰的数量,按MnO2计算,为所述复合氧化物重量的约0.005-0.5%。
4.如权利要求2所述的压电陶瓷,其特征在于其中氧化锰的数量,按MnO2计算,为所述复合氧化物重量的约0.005-0.5%。
5.如权利要求4所述的压电陶瓷,其特征在于其中铅的数量等于或低于5%(摩尔)。
6.如权利要求5所述的压电陶瓷,其特征在于所述陶瓷是一种PZT陶瓷。
7.如权利要求3所述的压电陶瓷,其特征在于其中铅的数量等于或低于5%(摩尔)。
8.如权利要求1所述的压电陶瓷,其特征在于其中铅的数量等于或低于5%(摩尔)。
9.如权利要求8所述的压电陶瓷,其特征在于其中氧化锰的数量,按MnO2计算,为所述复合氧化物重量的约0.005-0.5%。
10.一种制备压电陶瓷的方法,其特征在于将表面粘有锰和铅的化合物的、包含至少是铅、锆和钛的复合氧化物的压电陶瓷,在足以使氧化锰和氧化铅扩散至其晶粒边界部位的温度下加热。
11.如权利要求10所述的制备压电陶瓷的方法,其特征在于所述的复合氧化物是由通式(Pb0.95Sr0.03La0.02)(Zr0.51Ti0.49)O3表示。
12.如权利要求10所述的制备压电陶瓷的方法,其特征在于所述粘附于表面的锰化合物是MnCO3。
13.如权利要求10所述的制备压电陶瓷的方法,其特征在于所述复合氧化物是在约900-1100℃的温度下加热。
14.如权利要求13所述的制备压电陶瓷的方法,其特征在于所述复合氧化物的加热处理时间为2小时。
15.如权利要求10所述的制备压电陶瓷的方法,其特征在于还包括把锰化合物和铅化合物粘附在复合氧化物表面的步骤。
16.如权利要求15所述的制备压电陶瓷的方法,其特征在于所粘附的锰化合物的数量,按MnO2计算,为0.005-0.5%(重量),所粘附的铅的数量等于或低于5%(摩尔)。
17.如权利要求16所述的制备压电陶瓷的方法,其特征在于所述复合氧化物是在约850-1100℃的温度下加热。
18.如权利要求17所述的制备压电陶瓷的方法,其特征在于所述粘附于表面的锰化合物是MnCO3。
19.如权利要求18所述的制备压电陶瓷的方法,其特征在于所述的复合氧化物是由通式(Pb0.95Sr0.03La0.02)(Zr0.51Ti0.49)O3表示。
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JP260228/1995 | 1995-10-06 | ||
JP26022895A JP3119138B2 (ja) | 1995-10-06 | 1995-10-06 | 圧電磁器及びその製造方法 |
JP260228/95 | 1995-10-06 |
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CN1153756A CN1153756A (zh) | 1997-07-09 |
CN1064938C true CN1064938C (zh) | 2001-04-25 |
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US (1) | US5766502A (zh) |
EP (1) | EP0767151B1 (zh) |
JP (1) | JP3119138B2 (zh) |
KR (1) | KR100200180B1 (zh) |
CN (1) | CN1064938C (zh) |
DE (1) | DE69613927T2 (zh) |
TW (1) | TW365679B (zh) |
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TW516251B (en) * | 2000-01-31 | 2003-01-01 | Murata Manufacturing Co | Piezoelectric ceramic and manufacturing method therefor |
JP3827915B2 (ja) * | 2000-05-11 | 2006-09-27 | 株式会社日本自動車部品総合研究所 | 圧電材料およびその製造方法 |
CN100407468C (zh) * | 2003-09-25 | 2008-07-30 | 松下电器产业株式会社 | 压电元件及备有该压电元件的喷墨头以及它们的制造方法 |
DE10345499A1 (de) * | 2003-09-30 | 2005-04-28 | Epcos Ag | Piezoelektrisches Keramikmaterial, Vielschichtbauelement und Verfahren zur Herstellung des Keramikmaterials |
JP5004797B2 (ja) * | 2005-06-29 | 2012-08-22 | 日本碍子株式会社 | 圧電/電歪膜型素子 |
CN101215168B (zh) * | 2008-01-16 | 2010-06-02 | 武汉理工大学 | 镁钽酸锆钛酸铅陶瓷的掺杂改性方法 |
CN102260079B (zh) * | 2010-05-31 | 2013-10-02 | 中国科学院上海硅酸盐研究所 | 一种“收/发”两用型PZT-Pb(Sb2/3Mn1/3)三元系压电陶瓷材料及其制备方法 |
WO2012086740A1 (ja) * | 2010-12-22 | 2012-06-28 | 京セラ株式会社 | 誘電体セラミックスおよびこれを備える誘電体フィルタ |
CN103086715A (zh) * | 2013-01-05 | 2013-05-08 | 广东工业大学 | 一种制备钛锆酸铅压电陶瓷粉体的方法 |
US10105940B2 (en) * | 2016-04-18 | 2018-10-23 | The Boeing Company | Formation of composite laminates having one or more divergent flanges |
JP7078037B2 (ja) * | 2017-03-28 | 2022-05-31 | Tdk株式会社 | 圧電組成物および圧電素子 |
AT18002U1 (de) | 2017-08-30 | 2023-10-15 | Blum Gmbh Julius | Schubladenausziehführung |
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JPS601656A (ja) * | 1983-06-17 | 1985-01-07 | Fujitsu Ltd | 磁気記録再生装置 |
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JPS61657A (ja) * | 1984-06-12 | 1986-01-06 | 帝人株式会社 | 乾式不織布用ポリエステルバインダ |
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JPH0624841A (ja) * | 1990-09-20 | 1994-02-01 | Mitsubishi Kasei Corp | アクチュエータ用圧電セラミック組成物 |
JP3214055B2 (ja) * | 1991-06-26 | 2001-10-02 | 三菱化学株式会社 | アクチュエータ用圧電セラミック組成物 |
DE69318071T2 (de) * | 1992-06-23 | 1998-12-03 | Murata Mfg. Co., Ltd., Nagaokakyo, Kyoto | Piezoelektrische Keramiken |
JP3221145B2 (ja) * | 1993-02-26 | 2001-10-22 | 株式会社村田製作所 | 圧電磁器 |
JP3384044B2 (ja) * | 1993-07-19 | 2003-03-10 | 株式会社村田製作所 | 圧電磁器 |
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1995
- 1995-10-06 JP JP26022895A patent/JP3119138B2/ja not_active Expired - Fee Related
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1996
- 1996-10-05 KR KR1019960044089A patent/KR100200180B1/ko not_active IP Right Cessation
- 1996-10-07 CN CN961134356A patent/CN1064938C/zh not_active Expired - Fee Related
- 1996-10-07 DE DE69613927T patent/DE69613927T2/de not_active Expired - Lifetime
- 1996-10-07 EP EP19960116023 patent/EP0767151B1/en not_active Expired - Lifetime
- 1996-10-07 US US08/729,733 patent/US5766502A/en not_active Expired - Lifetime
- 1996-10-07 TW TW085112224A patent/TW365679B/zh not_active IP Right Cessation
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JPS601656A (ja) * | 1983-06-17 | 1985-01-07 | Fujitsu Ltd | 磁気記録再生装置 |
JPS61657A (ja) * | 1984-06-12 | 1986-01-06 | 帝人株式会社 | 乾式不織布用ポリエステルバインダ |
JPS61655A (ja) * | 1984-06-13 | 1986-01-06 | チコピー | 孔あき不織布の製造方法 |
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KR970021025A (ko) | 1997-05-28 |
JPH09100159A (ja) | 1997-04-15 |
TW365679B (en) | 1999-08-01 |
CN1153756A (zh) | 1997-07-09 |
DE69613927T2 (de) | 2002-01-17 |
US5766502A (en) | 1998-06-16 |
JP3119138B2 (ja) | 2000-12-18 |
EP0767151A1 (en) | 1997-04-09 |
KR100200180B1 (ko) | 1999-06-15 |
DE69613927D1 (de) | 2001-08-23 |
EP0767151B1 (en) | 2001-07-18 |
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