CN113149639A - 一种二元系压电陶瓷及其制备方法 - Google Patents

一种二元系压电陶瓷及其制备方法 Download PDF

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CN113149639A
CN113149639A CN202110505074.0A CN202110505074A CN113149639A CN 113149639 A CN113149639 A CN 113149639A CN 202110505074 A CN202110505074 A CN 202110505074A CN 113149639 A CN113149639 A CN 113149639A
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程晋荣
徐周上
陈建国
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Abstract

本申请涉及一种新型二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0.365BiScO3‑0.635Pb(Ti(1‑x)Cox)O3的二元系压电陶瓷，Co含量x＝0、0.03。本申请中的压电陶瓷相对于未掺Co的0.365BiScO3‑0.635PbTiO3陶瓷，四方相衍射峰强度增大，在保持较高的居里温度的同时，介电损耗有所降低，kp、kt减小，Qm显著增大。1kHz时，x＝0、0.03的介电常数分别为1715、1107；介电损耗tanδ分别为5.1％、3.0％；其居里温度Tc分别为421℃、449℃；其kp分别为0.55、0.41；kt分别为0.53、0.47；Qm分别是23、151。本申请通过引入Co离子对BS‑PT陶瓷进行改性，制备出了具有较高居里温度，介电损耗较小，Qm较大的的0.365BiScO3‑0.635Pb(Ti(1‑x)Cox)O3压电陶瓷，使钪酸铋‑钛酸铅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

一种二元系压电陶瓷及其制备方法
技术领域
本申请涉及一种新型压电陶瓷，特别涉及一种二元系压电陶瓷及其制备方法，应用于压电传感器、换能器等压电器件的功能材料制备技术领域。
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。
目前广泛商业化应用的锆钛酸铅(PZT)体系压电陶瓷在MPB区域附近表现出卓越的压电响应和机电性能，是目前广泛较为广泛的大功率压电材料。虽然PZT压电陶瓷有着压电系数高、性能稳定、机械强度大等优点，但其居里温度Tc约为360℃，由于热激活老化过程，PZT陶瓷安全使用温度仅在180℃以下，这限制了它在特殊环境中的使用。
经研究发现新型铋基钙钛矿二元固溶体xBiScO3-(1-x)PbTiO3(BS-PT)在准同型相界MPB(x～0.64)附近四方相和三方相共存，具有较高的居里温度(Tc～450℃)和优良的压电性能(d33～450pC/N)，是压电陶瓷高温应用的理想材料。尽管xBiScO3-(1-x)PbTiO3压电陶瓷相对于PZT压电陶瓷具有较高的居里温度和相当的压电性能，但其介电损耗较大以及机械品质因子较小的问题限制了其广泛使用。
发明内容
鉴于以上所述现有技术的缺点，本申请提供了一种新型二元系压电陶瓷，其化学通式为：0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3，其中Co含量x＝0、0.03。这一二元系压电陶瓷可以通过以下方法制备而成：
粉料合成：采用固相反应法在0.365BiScO3-0.635PbTiO3陶瓷中引入Co离子，形成0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3压电陶瓷粉体；
素坯成型：在合成粉体中加入PVA进行造粒，得到粉料颗粒；将所述粉料颗粒装入模具中，加压成型后进行排胶，获得0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3素胚；
陶瓷烧结：将所述素坯放在坩埚中密封烧结，得到化学式为0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3的压电陶瓷。
可选地，在所述粉料合成步骤中，以分析纯的Bi2O3、Sc2O3、PbO、TiO2、Co2O3为原料进行研磨，煅烧，从而合成所述陶瓷粉体。具体地，可以采用球磨的方式获得粉料，并将所获得的粉料煅烧合成所述陶瓷粉体。
可选地，在所述粉料合成步骤的煅烧步骤包括如下子步骤：升温至750℃，保温4h；随炉冷却至室温。
可选地，所述素坯成型步骤的排胶步骤包括：升温至600℃，保温3h；随炉冷却至室温。
可选地，在所述陶瓷烧结步骤中，烧结温度为1080℃，保温时间为2h。
本申请与现有技术相比较，具有以下优点：
1.本申请在0.365BiScO3-0.635PbTiO3陶瓷中引入Co离子，形成掺Co的固溶体，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，介电损耗显著降低，Qm有所增大。
2.本申请所提供的0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3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为本申请优选实施例0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3陶瓷样品x＝0.03和对比例x＝0的陶瓷样品的X射线衍射(XRD)对比图。
图2为本申请优选实施例0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3陶瓷样品x＝0.03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性劳动前提下所获得的所有其他实施例，都应当属于本申请保护的范围。
本申请的目的是提供一种0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3压电陶瓷及其制备方法，具体如下：
在本实施例中，在0.365BiScO3-0.635PbTiO3体系引入Co离子形成0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3固溶体系，形成的化学式为0.365BiScO3-0.635Pb(Ti0.97Co0.03)O3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：
a.粉料合成：采用固相反应法制备0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3陶瓷体系，即以分析纯的Bi2O3、Sc2O3、PbO、TiO2和Co2O3为原料，以设定的陶瓷化学式的x值分别为0、0.03，按照所需化学计量比称取上述原料球磨。将充分球磨后的浆料烘干，再进行高温煅烧合成0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3粉体，煅烧过程是将粉体升温至750℃，保温4h，随炉冷却至室温获得0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3陶瓷粉体。
b.素坯成型：在合成粉体中加入适当浓度的粘结剂PVA进行造粒。取合适质量造粒完的粉料装入模具中，在120MPa压力下干压成所需圆片。成型后进行排胶，最后获得0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3素胚，排胶程序是24h升温至600℃，保温3h，最后随炉冷却至室温。
c.陶瓷烧结：将上述所得0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3素坯放在坩埚中密封烧结，烧结温度为1080℃，保温2h，随炉冷却后，最终分别得到化学式为0.365BiScO3-0.635PbTiO3、0.365BiScO3-0.635Pb(Ti0.97Co0.03)O3的压电陶瓷材料。
对比实验分析
对本申请所得0.365BiScO3-0.635Pb(Ti0.97Co0.03)O3陶瓷和对比例0.365BiScO3-0.635PbTiO3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＝0.03和对比例x＝0的0.365BiScO3-0.635Pb(Ti(1-x)Cox)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，BS-PT陶瓷以三方相为主。引入Co元素后，四方相的含量增加，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、压电性能测试：
检测结果见图2和下表1：
Figure BDA0003058042810000041
表1
表1为本申请优选实施例0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3陶瓷样品x＝0.03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以及机电耦合系数kp、kt和机械品质因子Qm值。
图2为本申请优选实施例x＝0.03和对比例x＝0的0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3陶瓷在1kHz时介电温谱对比图。x＝0、0.03的居里温度Tc分别为421℃、449℃，相对于原组分的居里温度421℃，添加Co后的陶瓷样品的居里温度都有所增加。表1为本申请优选实施例x＝0.03和对比例x＝0的0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3陶瓷在1kHz时其介电常数εr和介电损耗tanδ值以及kp、kt和Qm值。掺Co后相对于原组分介电常数减小，介电损耗减小。x＝0、0.03的陶瓷在1kHz时，介电常数分别为1715、1107，介电损耗tanδ分别为5.1％、3.0％，掺Co后kp、kt减小，kp分别为0.55、0.41；kt分别为0.53、0.47；Qm增大，分别是23、151。掺Co的陶瓷样品在工作时内摩擦会更小，产生的热也更少，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0.365BiScO3-0.635Pb(Ti0.97Co0.03)O3压电陶瓷展示了优异的电学性能。本申请通过引入变价金属元素Co对0.365BiScO3-0.635PbTiO3压电陶瓷进行改性，制备出了四方相含量较多，在保持较高的居里温度的同时，介电损耗较低，Qm较大的0.365BiScO3-0.635Pb(Ti0.97Co0.03)O3陶瓷。这些结果表明引入Co离子的BS-PT陶瓷有潜力应用于压电换能器领域的压电材料。
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 (8)

1.一种二元系压电陶瓷，其特征在于，所述二元系压电陶瓷的化学通式为：0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3，其中Co含量x＝0、0.03。
2.一种二元系压电陶瓷的制备方法，其特征在于，包括如下步骤：
粉料合成：采用固相反应法在0.365BiScO3-0.635PbTiCoO3陶瓷中引入Co离子，形成0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3压电陶瓷粉体；
素坯成型：在合成粉体中加入PVA进行造粒，得到粉料颗粒；将所述粉料颗粒装入模具中，加压成型后进行排胶，获得0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3素胚；
陶瓷烧结：将所述素坯放在坩埚中密封烧结，得到化学式为0.365BiScO3-0.635Pb(Ti(1-x)Cox)O3的压电陶瓷。
3.根据权利要求2所述的方法，其特征在于：在所述粉料合成步骤中，以分析纯的Bi2O3、Sc2O3、PbO、TiO2、Co2O3为原料进行研磨，煅烧，从而合成所述陶瓷粉体。
4.根据权利要求3所述的方法，其特征在于：所述研磨和煅烧的步骤，是采用球磨的方式获得粉料，并将所获得的粉料煅烧合成所述陶瓷粉体。
5.根据权利要求3所述的方法，其特征在于：在所述粉料合成步骤的煅烧步骤包括：升温至750℃，保温4h；随炉冷却至室温。
6.根据权利要求2所述的方法，其特征在于：所述素坯成型步骤的排胶步骤包括：升温至600℃，保温3h；随炉冷却至室温。
7.根据权利要求2所述的方法，其特征在于：在所述陶瓷烧结步骤中，烧结温度为1080℃，保温时间为2h。
8.一种二元系压电陶瓷，其特征在于，所述压电陶瓷经由权利要求2至7中任意一项所述的方法制备而成。
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