CN105948745B - 压电陶瓷材料、压电陶瓷烧结体及其压电陶瓷器件 - Google Patents
压电陶瓷材料、压电陶瓷烧结体及其压电陶瓷器件 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 16
- 239000000919 ceramic Substances 0.000 title claims description 48
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 8
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 15
- 238000003475 lamination Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 8
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- 239000000203 mixture Substances 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 5
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- 230000005684 electric field Effects 0.000 claims description 4
- 239000004014 plasticizer Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 239000011230 binding agent Substances 0.000 claims description 3
- 238000007766 curtain coating Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- 239000005416 organic matter Substances 0.000 claims description 3
- 230000010287 polarization Effects 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 2
- 229910010293 ceramic material Inorganic materials 0.000 claims description 2
- 238000003801 milling Methods 0.000 claims description 2
- 239000010946 fine silver Substances 0.000 abstract description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 abstract 1
- 238000000034 method Methods 0.000 description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 230000002706 hydrostatic effect Effects 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000009766 low-temperature sintering Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910000018 strontium carbonate Inorganic materials 0.000 description 2
- 238000010345 tape casting Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- PMTRSEDNJGMXLN-UHFFFAOYSA-N titanium zirconium Chemical compound [Ti].[Zr] PMTRSEDNJGMXLN-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明提供了一种压电陶瓷材料，所述压电陶瓷材料含有用化学通式:Pb1‑aSra(Zn1/ 3Nb2/3)1‑b‑cZrbTicO3+dwt％Sm2O3+ewt％Li2CO3，且满足如下关系的主要组分：0.01≤a≤0.1,0.2≤b≤0.6,0.3≤c≤0.7,0.2≤d≤0.6,0.1≤e≤0.5。本发明大幅降低了烧结温度，减少了PbO挥发对环境的危害，并使产品可以采用纯银电极，降低了大量材料成本。
Description
【技术领域】
本发明涉及一种压电陶瓷材料、压电陶瓷烧结体及其压电陶瓷器件。
【背景技术】
目前采用向Pb(Zr,Ti)O3中加入第三组元并调节锆钛比来达到调整性能的目的，使用的陶瓷粉料需要在较高温度(＞1100℃)烧结，或者能在低温(＜960℃)烧结，但是性能达不到要求。
现有结构或者方法的失陷:需要较高的烧结温度(1100-1200℃)，在烧结过程中有大量的PbO挥发，会影响身体健康并污染环境；PbO的大量挥发会导致成分发生偏离，影响性能稳定性；另外，较高的烧结温度使得产品生产过程中必须使用含钯的银浆以避免烧结过程中电极挥发，成本较高。
【发明内容】
本发明的目的在于提供一种。
本发明的技术方案如下：提供一种压电陶瓷材料，所述压电陶瓷材料含有用化学通式:
Pb1-aSra(Zn1/3Nb2/3)1-b-cZrbTicO3+dwt％Sm2O3+ewt％Li2CO3表示且满足如下关系的主要组分：0.01≤a≤0.1,0.2≤b≤0.6,0.3≤c≤0.7,0.2≤d≤0.6,0.1≤e≤0.5。
提供一种压电陶瓷烧结体，所述压电陶瓷烧结体是通过烧制如上述所述的压电陶瓷材料而得到的烧结体。
提供一种压电陶瓷烧结体的制备方法，所述制备方法包括如下步骤：
配料：按Pb1-aSra(Zn1/3Nb2/3)1-b-cZrbTicO3+dwt％Sm2O3+ewt％Li2CO3化学式配比提供压电陶瓷材料的各组分并将所述组分制成粉末，其中0.01≤a≤0.1,0.2≤b≤0.6,0.3≤c≤0.7,0.2≤d≤0.6,0.1≤e≤0.5；
混料：将上述配置好的粉末加1：1质量的蒸馏水混合10小时后烘干；
煅烧：将上述烘干后的产物在750-850℃的环境中煅烧2小时以合成得到煅烧产物；
细磨：在上述煅烧产物中加入低温助剂后进行细磨并烘干；
制备浆料：向上述混合物中加入粘结剂、增塑剂、分散剂以及溶剂并混合以形成陶瓷浆料；
成型：将上述浆料除泡后流延形成陶瓷薄膜；
叠层：将陶瓷薄膜叠层形成多层产品；
排胶：将叠层后的产品置于排胶炉中在400-700℃的环境中脱去有机物；
烧结：在900-1000℃环境中保温3小时烧结得到陶瓷烧结体。
优选的，在配料步骤中，所述组分通过原料选择或球磨混合的方式制成粉末,所述粉末的颗粒度中位数控制在2μm以下。
优选的，在细磨步骤中，细磨后的混合物的粒度分布在中位数1μm以下。
提供一种压电陶瓷器件，所述压电陶瓷器件通过电极极化如上述所述的压电陶瓷烧结体形成的。
优选的，所述压电陶瓷器件在空气中以2-3kv/mm电场中极化5秒得到。
本发明的有益效果在于：改变加入Pb(Zr,Ti)O3中第三组元的种类，并采用SrCO3对其进行A位(Pb)置换，调整陶瓷性能使其满足产品需求；通过加入低温烧结助剂Sm2O3和Li2CO3降低烧结温度至银熔点(961℃)以下。大幅降低了烧结温度，减少了PbO挥发对环境的危害，并使产品可以采用纯银电极，降低了大量材料成本。
【附图说明】
图1为本发明优选实施例中煅烧后陶瓷粉料的X射线衍射图谱；
图2为本发明优选实施例中在950℃环境下烧结得到的陶瓷断面显微形貌图；
图3为本发明在不同烧结温度下的陶瓷性能对比图。
【具体实施方式】
下面结合附图和实施方式对本发明作进一步说明。
本发明提供本发明提供了一种压电陶瓷材料，所述压电陶瓷材料含有用化学通式:
Pb1-aSra(Zn1/3Nb2/3)1-b-cZrbTicO3+dwt％Sm2O3+ewt％Li2CO3表示且满足如下关系的主要组分：0.01≤a≤0.1,0.2≤b≤0.6,0.3≤c≤0.7,0.2≤d≤0.6,0.1≤e≤0.5。
本发明同时提供一种采用上述压电陶瓷材料加工形成压电陶瓷烧结体的制备方法，其通过控制原料和预烧后粉末的粒度，使用流延成型法制备所需压电陶瓷烧结体，然后在空气中以2-3kv/mm电场中极化5秒得到所需要的压电陶瓷器件，具体包括如下步骤：
配料：按Pb1-aSra(Zn1/3Nb2/3)1-b-cZrbTicO3+dwt％Sm2O3+ewt％Li2CO3化学式配比提供压电陶瓷材料的各组分并将所述组分制成粉末，其中0.01≤a≤0.1,0.2≤b≤0.6,0.3≤c≤0.7,0.2≤d≤0.6,0.1≤e≤0.5；粉末的粒度分布中位数均应小于2μm。
混料：将上述配置好的粉末加1：1质量的蒸馏水混合10小时后烘干。
煅烧：将上述烘干后的产物在750-850℃的环境中煅烧2小时以合成得到煅烧产物。图1为煅烧后陶瓷粉料的X射线衍射图谱。
细磨：在上述煅烧产物中加入低温助剂后进行细磨并烘干。
制备浆料：向上述混合物中加入粘结剂、增塑剂、分散剂以及溶剂并混合以形成陶瓷浆料；加入的粘接剂、增塑剂、分散剂以及溶剂如下表：
表1
成型：将上述浆料除泡后流延形成陶瓷薄膜。
叠层：将陶瓷薄膜叠层形成多层产品。
成型陶瓷薄膜的方法主要有四种；轧膜成型、流延成型、干压成型和静水压成型。轧膜成型适用于薄片元件；流延成型适合于更薄的元件，膜厚可以小于10μm；干压成型适合于块状元件；静水压成型适合于异形或块状元件。除了静水压成型外，其他成型方法都需要有粘合剂，粘合剂一般占原料重量的3％左右。成型以后需要排胶。粘合剂的作用只是利于成型，但它是一种还原性强的物质，成型后应将其排出以免影响烧结质量。
排胶：将叠层后的产品置于排胶炉中在400-700℃的环境中脱去有机物。
烧结：在900-1000℃环境中保温3小时烧结得到陶瓷烧结体。
作为本发明的一种具体实施方式，表2为在950℃环境下烧结得到的陶瓷烧结体的性能：
表2
图2为通过上述制备方法制成的实施例配方的压电陶瓷在950℃环境下烧结得到的陶瓷断面的显微形貌图。图3为不同烧结温度得到的陶瓷烧结件的性能对比图。
本发明还提供了一种压电陶瓷器件，所述压电陶瓷器件通过电极极化如上所述的压电陶瓷烧结体形成的。该压电陶瓷器件在空气中以2-3kv/mm电场中极化5秒得到。
改变加入Pb(Zr,Ti)O3中第三组元的种类，并采用SrCO3对其进行A位(Pb)置换，调整陶瓷性能使其满足产品需求；通过加入低温烧结助剂Sm2O3和Li2CO3降低烧结温度至银熔点(961℃)以下。大幅降低了烧结温度，减少了PbO挥发对环境的危害，并使产品可以采用纯银电极，降低了大量材料成本。
以上所述的仅是本发明的实施方式，在此应当指出，对于本领域的普通技术人员来说，在不脱离本发明创造构思的前提下，还可以做出改进，但这些均属于本发明的保护范围。
Claims (5)
1.一种压电陶瓷烧结体的制备方法，其特征在于，所述制备方法包括如下步骤：
配料：按Pb1-aSra(Zn1/3Nb2/3)1-b-cZrbTicO3+dwt％Sm2O3+ewt％Li2CO3化学式配比提供压电陶瓷材料的各组分并将所述组分制成粉末，其中0.01≤a≤0.1,0.2≤b≤0.6,0.3≤c≤0.7,0.2≤d≤0.6,0.1≤e≤0.5；
混料：将上述配置好的粉末加1：1质量的蒸馏水混合10小时后烘干；
煅烧：将上述烘干后的产物在750-850℃的环境中煅烧2小时以合成得到煅烧产物；
细磨：在上述煅烧产物中加入低温助剂后进行细磨并烘干；
制备浆料：向上述混合物中加入粘结剂、增塑剂、分散剂以及溶剂并混合以形成陶瓷浆料；
成型：将上述浆料除泡后流延形成陶瓷薄膜；
叠层：将陶瓷薄膜叠层形成多层产品；
排胶：将叠层后的产品置于排胶炉中在400-700℃的环境中脱去有机物；
烧结：在900-1000℃环境中保温3小时烧结得到陶瓷烧结体。
2.根据权利要求1所述的制备方法，其特征在于，在配料步骤中，所述组分通过原料选择或球磨混合的方式制成粉末,所述粉末的颗粒度中位数控制在2μm以下。
3.根据权利要求1所述的制备方法，其特征在于，在细磨步骤中，细磨后的混合物的粒度分布在中位数1μm以下。
4.一种压电陶瓷器件，其特征在于，所述压电陶瓷器件通过电极极化如权利要求1至3任意一项所述的制备方法制得的压电陶瓷烧结体形成的。
5.根据权利要求4所述的压电陶瓷器件，其特征在于，所述压电陶瓷器件在空气中以2-3kv/mm电场中极化5秒得到。
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| WO2006067924A1 (ja) * | 2004-12-22 | 2006-06-29 | Murata Manufacturing Co., Ltd | 圧電磁器組成物および圧電アクチュエータ |
| CN101020608A (zh) * | 2006-12-11 | 2007-08-22 | 中国科学院上海硅酸盐研究所 | 一种钛酸铋钠－钛酸钡无铅压电陶瓷及其制备方法 |
| CN101024573A (zh) * | 2007-01-30 | 2007-08-29 | 合肥工业大学 | 多元铌酸钾钠系无铅压电陶瓷及其制备方法 |
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| WO2006067924A1 (ja) * | 2004-12-22 | 2006-06-29 | Murata Manufacturing Co., Ltd | 圧電磁器組成物および圧電アクチュエータ |
| CN101188270A (zh) * | 2006-11-21 | 2008-05-28 | Tdk株式会社 | 层叠型压电元件 |
| CN101020608A (zh) * | 2006-12-11 | 2007-08-22 | 中国科学院上海硅酸盐研究所 | 一种钛酸铋钠－钛酸钡无铅压电陶瓷及其制备方法 |
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