CN114560689A - 一种新型四元系压电陶瓷及其制备方法 - Google Patents
一种新型四元系压电陶瓷及其制备方法 Download PDFInfo
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 18
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- 235000015895 biscuits Nutrition 0.000 claims description 6
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 6
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Abstract
本发明公开了一种新型四元系压电陶瓷及其制备方法，利用固相反应法制备了一种化学通式为(0.63‑x)BiFeO3‑0.32PbTiO3‑0.05BaZrO3‑xPb(Ni1/3Nb2/3)O3的四元系压电陶瓷，Pb(Ni1/ 3Nb2/3)O3含量x＝0和0.12，本申请中的0.63BiFeO3‑0.32PbTiO3‑0.05BaZrO3压电陶瓷随着Pb(Ni1/3Nb2/3)O3的掺杂量增高，相结构由四方转变为三方相，晶粒尺寸减小，当x＝0.12，BF‑PT‑BZ‑PNN压电陶瓷中三方和四方相共存，介电、铁电和压电性能达到最优，压电系数d33、压电电压常数g33和机电转换系数d33×g33分别为410pC/N、32×10‑3Vm/N和13045×10‑15m2/N，其中，d33×g33性能优于商用能量收集器材料PZT502(d33×g33＝11250×10‑15m2/N)，使铁酸铋‑钛酸铅‑锆酸钡基陶瓷在压电材料研究领域的应用化迈出了很大的一步。
Description
技术领域
本发明属于压电传感器、换能器等压电器件的功能材料制备技术领域，特别是涉及一种新型四元系压电陶瓷及其制备方法。
背景技术
作为重要的功能材料，压电材料在国民经济的多个领域都发挥着重要应用。随着现代工业的快速发展，特别是新能源、交通和国防工业的高速发展，在一些极端环境下对压电陶瓷的服役性能提出了新的挑战。例如工业上使用的超声加工、超声焊接等大功率超声换能器，核反应堆中使用的高温超声波定位探测器，内燃机中使用的燃油喷压电阀等，必须选用具有高居里点的压电材料，这样才能保证压电器件可在较宽温度范围内正常工作，在航空航天领域，高温压电加速度传感器也发挥着重要作用。
高温压电材料是高温压电器件最核心的敏感元件。然而性能优良、居里温度高的压电陶瓷材料以目前的情况，还是比较少。这就使得长期以来，特种高温压电器件不得不使用生产工艺复杂、成本高的压电单晶材料。因此，开发具有优异性能的高居里温度压电陶瓷材料已成为当务之急。目前，世界各地科学家正在为寻找能适用于高温环境下的压电陶瓷做出不懈努力。
发明内容
为了克服上述问题，本发明提供了一种新型四元系压电陶瓷及其制备方法。
本发明所采用的技术方案是：
一种新型四元系压电陶瓷，化学通式为：
(0.63-x)BiFeO3-0.32PbTiO3-0.05BaZrO3-xPb(Ni1/3Nb2/3)O3，Pb(Ni1/3Nb2/3)O3含量x＝0和0.12。
本发明还提供了一种新型四元系压电陶瓷的制备方法，包括以下步骤：
步骤一：合成BF-PT-BZ-PNN粉体：以分析纯的Bi2O3、Fe2O3、PbO、TiO2、BaCO3、ZrO2、Nb2O5和NiO为原料，按制备30g(0.63-x)BF-0.32PT-0.05BZ-xPNN所需化学计量比称取上述原料放入球磨罐中，加入24ml分析纯酒精和重量为60g、5mm直径大小的氧化锆小球进行球磨6h，将球磨后的浆料经过筛网滤出氧化锆小球，将浆料倒入陶瓷碗中，碗口覆盖铝箔，放入120℃烘箱中烘干，过120目网筛后放入坩埚中进行高温煅烧合成BF-PT-BZ-PNN粉体，煅烧完成后，将合成粉料研细，放入球磨罐中，进行第二次球磨，再进行上述相同的第二次煅烧和第三次球磨过程，第三次球磨后出料烘干，过120目筛，得到颗粒细小、均匀的BF-PT-BZ-PNN合成粉体；
步骤二：成型素坯：在制备好的合成粉体中滴加浓度为5％粘结剂PVA，进行造粒，在100MPa下干压成直径12mm、厚度1mm的圆片，随后进行200MPa等静压成型，等静压后进行排胶，最后获得BF-PT-BZ-PNN素胚；
步骤三：烧结陶瓷：将上述所得BF-PT-BZ-PNN素坯放在坩埚中密封烧结。
其中，步骤一中煅烧曲线为：从室温5℃/min升温至450℃，保温2h，再5℃/min升温至750℃，保温4h，随炉冷却。
其中，步骤二中粘结剂PVA滴加量为粉体量的7％。
其中，步骤二中排胶曲线为：从室温720min升温至450℃，保温3h，再300min升温至600℃，保温3h，随炉冷却。
其中，步骤二中烧结曲线为：从室温5℃/min升温至1050℃，保温2h，随炉冷却。
本发明的优点如下：
1、本申请在BF-PT-BZ陶瓷中引入PNN形成固溶体，组分设置在准同型相界附近。现对于原组分，在保持较高的居里温度的同时，陶瓷的压电系数和单向电致应变量得到显著提升。
2、本申请所提供的BF-PT-BZ-PNN陶瓷是高绝缘性的压电材料，有望应用于下一代的压电器件。
附图说明
为了更清楚地说明本申请实施方式或现有技术中的技术方案，下面将对实施方式或现有技术描述中所需要使用的附图作简单介绍。显而易见地，下面描述中的附图仅用于示意本申请的一些实施方式，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图中未提及的技术特征、连接关系乃至方法步骤。
图1为本发明优选实施例(0.63-x)BiFeO3-0.32PbTiO3-0.05BaZrO3-xPb(Ni1/ 3Nb2/3)O3陶瓷样品x＝0.12和对比例x＝0的陶瓷样品的X射线衍射(XRD)对比图。
图2为本发明优选实施例(0.63-x)BiFeO3-0.32PbTiO3-0.05BaZrO3-xPb(Ni1/ 3Nb2/3)O3陶瓷样品x＝0.12和对比例x＝0的陶瓷样品的介电常数随温度变化图。
具体实施方式
为使本申请实施例的目的、技术方案和优点更加清楚，下面将结合本申请实施例中的附图，对本申请实施例中的技术方案进行清楚、完整的描述，显然，所描述的实施例是本申请一部分实施例，而不是全部的实施例。基于本申请中的实施例，本领域普通技术人员在没有做出创造。
本申请的目的是提供一种(0.63-x)BiFeO3-0.32PbTiO3-0.05BaZrO3-xPb(Ni1/ 3Nb2/3)O3压电陶瓷及其制备方法，具体如下：
在本实施例中，在0.63BiFeO3-0.32PbTiO3-0.05BaZrO3体系引入Pb(Ni1/3Nb2/3)O3形成化学式为(0.63-x)BiFeO3-0.32PbTiO3-0.05BaZrO3-xPb(Ni1/3Nb2/3)O3固溶体系的压电陶瓷材料。
在本实施例中，0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3压电陶瓷的制备方法，包括如下步骤：
步骤一：合成BF-PT-BZ-PNN粉体：以分析纯的Bi2O3、Fe2O3、PbO、TiO2、BaCO3、ZrO2、Nb2O5和NiO为原料，按制备30g(0.63-x)BF-0.32PT-0.05BZ-xPNN所需化学计量比称取上述原料放入球磨罐中，然后加入24ml分析纯酒精和重量为60g、5mm左右直径大小的氧化锆小球进行球磨6h。将球磨后的浆料经过筛网滤出氧化锆小球，然后将浆料倒入陶瓷碗中，碗口覆盖铝箔，放入120℃烘箱中烘干，然后过120目网筛后放入坩埚中进行高温煅烧合成BF-PT-BZ-PNN粉体，煅烧曲线为：从室温5℃/min升温至450℃，保温2h，再5℃/min升温至750℃，保温4h，随炉冷却。煅烧完成后，将合成粉料研细，放入球磨罐中，进行第二次球磨。之后，再进行上述相同的第二次煅烧和第三次球磨过程。第三次球磨后出料烘干，然后过120目筛，得到颗粒细小、均匀的BF-PT-BZ-PNN合成粉体。
步骤二：成型素坯：在制备好的合成粉体中滴加浓度为5％粘结剂PVA，进行造粒。滴加量为粉体量的7％。之后在100MPa下干压成型，随后进行200MPa等静压。等静压后进行排胶，最后获得BF-PT-BZ-PNN素胚，排胶曲线为：从室温720min升温至450℃，保温3h，再300min升温至600℃，保温3h，随炉冷却。
步骤三：烧结陶瓷：将上述所得BF-PT-BZ-PNN素坯放在坩埚中密封烧结，烧结曲线为：从室温5℃/min升温至10500℃，保温2h，随炉冷却。然后对样品的各项性能进行测试。
对比实验分析
对本申请所得(0.63-x)BiFeO3-0.32PbTiO3-0.05BaZrO3-xPb(Ni1/3Nb2/3)O3陶瓷和对比例0.63BiFeO3-0.32PbTiO3-0.05BaZrO3陶瓷进行表征及性能测试，包括如下实验分析：
1.X射线衍射仪(XRD)测试：
检测结果见图1，图1为本申请优选实施例x＝0.12和对比例x＝0的(0.63-x)BiFeO3-0.32PbTiO3-0.05BaZrO3-xPb(Ni1/3Nb2/3)O3陶瓷的X射线衍射(XRD)对比图。从图1中可以看出，当x＝0时，BF-PT-BZ陶瓷以四方相为主。引入PNN，三方相的含量增加，掺杂后的陶瓷同样是处于MPB区域的钙钛矿结构，三方相、四方相共存。
2.介电和压电性能测试：
检测结果见图2和下表1：
表1
表1为本申请优选实施例(0.63-x)BiFeO3-0.32PbTiO3-0.05BaZrO3-xPb(Ni1/ 3Nb2/3)O3陶瓷样品x＝0.12和对比例x＝0的陶瓷样品1kHz下的介电常数εr和介电损耗tanδ以及压电系数d33、压电电压常数g33和机电转换系数d33×g33。
图2为本申请优选实施例x＝0.12和对比例x＝0的(0.63-x)BiFeO3-0.32PbTiO3-0.05BaZrO3-xPb(Ni1/3Nb2/3)O3陶瓷在1kHz时介电温谱对比图。
掺PNN后相对于原组分介电常数增大近3倍，材料的绝缘性能大大提高。介电损耗增大，居里温度减小；压电常数也提高3倍，压电性能极大提升；同时机电转换系数也提高3倍，能量收集效率大幅度提升。因此BF-PT-BZ-PNN是一种潜力很大的压电陶瓷材料。
综合以上测试分析的结果表明：本申请优选实施例(0.63-x)BiFeO3-0.32PbTiO3-0.05BaZrO3-xPb(Ni1/3Nb2/3)O3压电陶瓷展示了优异的性能。本申请通过引入PNN弛豫体对0.63BF-0.32PT-0.05BZ压电陶瓷进行改性，制备出了三、四方相共存，在保持较高的居里温度的同时，介电常数增大，机电转换系数较大的0.365BiScO3-0.635Pb(Ti0.97Co0.03)O3陶瓷。这些结果表明引入PNN的BF-PT-BZ陶瓷有潜力应用于压电能量收集器领域的压电材料。
应当理解，在本申请实施例中使用的术语是仅仅出于描述特定实施例的目的，而非旨在限制本申请。在本申请实施例和所附权利要求书中所使用的单数形式的“一种”、“所述”和“该”也旨在包括多数形式，除非上下文清楚地表示其他含义，“多种”一般包含至少两种，但是不排除包含至少一种的情况。
还需要说明的是，术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含，从而使得包括一系列要素的商品或者系统不仅包括那些要素，而且还包括没有明确列出的其他要素，或者是还包括为这种商品或者系统所固有的要素。在没有更多限制的情况下，由语句“包括一个……”限定的要素，并不排除在包括所述要素的商品或者系统中还存在另外的相同要素。
最后应说明的是，本领域的普通技术人员可以理解，为了使读者更好地理解本申请，本申请的实施方式提出了许多技术细节。但是，即使没有这些技术细节和基于上述各实施方式的种种变化和修改，也可以基本实现本申请各权利要求所要求保护的技术方案。因此，在实际应用中，可以在形式上和细节上对上述实施方式作各种改变，而不偏离本申请的精神和范围。
Claims (6)
1.一种新型四元系压电陶瓷，其特征在于：四元系压电陶瓷的化学通式为：(0.63-x)BiFeO3-0.32PbTiO3-0.05BaZrO3-xPb(Ni1/3Nb2/3)O3，Pb(Ni1/3Nb2/3)O3含量x＝0和0.12。
2.一种新型四元系压电陶瓷的制备方法，其特征在于：包括以下步骤：
步骤一：合成BF-PT-BZ-PNN粉体：以分析纯的Bi2O3、Fe2O3、PbO、TiO2、BaCO3、ZrO2、Nb2O5和NiO为原料，按制备30g(0.63-x)BF-0.32PT-0.05BZ-xPNN所需化学计量比称取上述原料放入球磨罐中，加入24ml分析纯酒精和重量为60g、5mm直径大小的氧化锆小球进行球磨6h，将球磨后的浆料经过筛网滤出氧化锆小球，将浆料倒入陶瓷碗中，碗口覆盖铝箔，放入120℃烘箱中烘干，过120目网筛后放入坩埚中进行高温煅烧合成BF-PT-BZ-PNN粉体，煅烧完成后，将合成粉料研细，放入球磨罐中，进行第二次球磨，再进行上述相同的第二次煅烧和第三次球磨过程，第三次球磨后出料烘干，过120目筛，得到颗粒细小、均匀的BF-PT-BZ-PNN合成粉体；
步骤二：成型素坯：在制备好的合成粉体中滴加浓度为5％粘结剂PVA，进行造粒，在100MPa下干压成直径12mm、厚度1mm的圆片，随后进行200MPa等静压成型，等静压后进行排胶，最后获得BF-PT-BZ-PNN素胚；
步骤三：烧结陶瓷：将上述所得BF-PT-BZ-PNN素坯放在坩埚中密封烧结。
3.根据权利要求2所述的一种新型四元系压电陶瓷的制备方法，其特征在于：所述的步骤一中煅烧曲线为：从室温5℃/min升温至450℃，保温2h，再5℃/min升温至750℃，保温4h，随炉冷却。
4.根据权利要求2所述的一种新型四元系压电陶瓷的制备方法，其特征在于：所述的步骤二中粘结剂PVA滴加量为粉体量的7％。
5.根据权利要求2所述的一种新型四元系压电陶瓷的制备方法，其特征在于：所述的步骤二中排胶曲线为：从室温720min升温至450℃，保温3h，再300min升温至600℃，保温3h，随炉冷却。
6.根据权利要求2所述的一种新型四元系压电陶瓷的制备方法，其特征在于：所述的步骤二中烧结曲线为：从室温5℃/min升温至1050℃，保温2h，随炉冷却。
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20160149119A1 (en) * | 2014-11-21 | 2016-05-26 | Samsung Electro-Mechanics Co., Ltd. | Piezoelectric ceramic composition, piezoelectric element, and method for the same |
| CN106810235A (zh) * | 2017-01-23 | 2017-06-09 | 上海大学 | 铁酸铋‑钛酸铅‑钛酸钡三元体系高温压电陶瓷及其制备方法 |
| CN108238795A (zh) * | 2016-12-27 | 2018-07-03 | 中国科学院福建物质结构研究所 | 一种具有高居里温度的新型三元铁电陶瓷系统及其制备方法和应用 |
| CN113149639A (zh) * | 2021-05-10 | 2021-07-23 | 上海大学 | 一种二元系压电陶瓷及其制备方法 |
| CN113307619A (zh) * | 2021-05-15 | 2021-08-27 | 西安外事学院 | 一种铁酸铋-钛酸铅-铌镁酸铋三元体系高温压电陶瓷的制备方法 |
-
2022
- 2022-02-22 CN CN202210162927.XA patent/CN114560689A/zh active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20160149119A1 (en) * | 2014-11-21 | 2016-05-26 | Samsung Electro-Mechanics Co., Ltd. | Piezoelectric ceramic composition, piezoelectric element, and method for the same |
| CN108238795A (zh) * | 2016-12-27 | 2018-07-03 | 中国科学院福建物质结构研究所 | 一种具有高居里温度的新型三元铁电陶瓷系统及其制备方法和应用 |
| CN106810235A (zh) * | 2017-01-23 | 2017-06-09 | 上海大学 | 铁酸铋‑钛酸铅‑钛酸钡三元体系高温压电陶瓷及其制备方法 |
| CN113149639A (zh) * | 2021-05-10 | 2021-07-23 | 上海大学 | 一种二元系压电陶瓷及其制备方法 |
| CN113307619A (zh) * | 2021-05-15 | 2021-08-27 | 西安外事学院 | 一种铁酸铋-钛酸铅-铌镁酸铋三元体系高温压电陶瓷的制备方法 |
Non-Patent Citations (2)
| Title |
|---|
| QIANG LI等: "Enhanced dielectric and piezoelectric properties in BaZrO3 modified BiFeO3–PbTiO3 high temperature ceramics", 《JOURNAL OF MATERIALS SCIENCE-MATERIALS IN ELETRONICS》 * |
| ZHENRONG LI等: "Dielectric，pyroelectric and piezoelectric properties of (1-x)Pb(Ni1/3Nb2/3)O3-x PbTiO3 system", 《JOURNAL OF MATERIALS SCIENCE LETTERS》 * |
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