CN110357629A - 一种钨青铜与钙钛矿结构氧化物形成的固溶体及制备方法 - Google Patents

一种钨青铜与钙钛矿结构氧化物形成的固溶体及制备方法 Download PDF

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CN110357629A
CN110357629A CN201910770398.XA CN201910770398A CN110357629A CN 110357629 A CN110357629 A CN 110357629A CN 201910770398 A CN201910770398 A CN 201910770398A CN 110357629 A CN110357629 A CN 110357629A
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solid solution
sbn
powder
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tungsten bronze
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张善涛
袁芯
李玲
陶纯玮
张骥
王瑞雪
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Abstract

本发明公开了一种基于异类材料钨青铜结构Sr0.75Ba0.25Nb2O6(SBN)与钙钛矿结构0.94Bi0.5Na0.5TiO3‑0.06BaTiO3(BNBT)形成的固溶体及其制备方法。将单相的SBN粉末和BNBT粉末混合均匀，在高温下烧结3h，得到(1‑x)SBN‑xBNBT固溶体。BNBT中的Bi3+、Na+、Ba2+和Ti4+在高温下扩散进入SBN钨青铜结构中占据晶格位置形成固溶体，此固溶体陶瓷具有很大的晶粒各向异性、大范围可调的电学性能以及优异的室温储能效率。与传统的基于同类材料的固溶体相比，本发明不仅提供了一种基于异类材料形成的固溶体，还提供了一种开发新型固溶体的新思路。

Description

一种钨青铜与钙钛矿结构氧化物形成的固溶体及制备方法
技术领域
本发明涉及一种钨青铜结构与钙钛矿结构氧化物形成的固溶体及制备方法。
背景技术
驰豫铁电体氧化物不仅是研究驰豫现象来源的基础，更由于其丰富的介电、铁电、压电等性质在信息、医疗、交通、生物等高新科技领域有着广泛应用。
近年来，随着人们环保意识的增强和社会可持续发展的需要，环境友好型无铅驰豫铁电体越来越成为研究的热点，其中以Sr1-xBaxNb2O6为代表的钨青铜结构氧化物和以Bi0.5Na0.5TiO3为代表的钙钛矿结构氧化物最为人们关注。一般而言，为了优化弛豫铁电体的电学性质，最有效可行的方法之一是形成固溶体，因为固溶体能够在纳米尺度上建立新的晶体结构和铁电畴结构。但目前报道的固溶体都为基于同类材料形成的固溶体，即钙钛矿-钙钛矿或钨青铜-钨青铜结构氧化物固溶体，这主要是因为同类材料具有相同的化学式和类似的晶格结构，更有利于形成固溶体。然而截止目前，基于同类材料形成固溶体的弛豫铁电性质仍然需要进一步优化以实现其实际应用。为此，发展形成固溶体的新方法仍然具有重要意义，而发展基于异类材料的固溶体是可能的方法之一。
一般情况下，异类材料由于化学式不同，很难提供成比例的晶格位置和离子来形成固溶体。因此，基于异类材料的固溶体鲜有报道。然而，以Sr1-xBaxNb2O6为代表的钨青铜结构氧化物中，Sr2+/Ba2+并未被占据全部的A位晶格位置，即Sr1-xBaxNb2O6是一种非完全占据的钨青铜结构氧化物。这意味着基于Sr1-xBaxNb2O6，引入以Bi0.5Na0.5TiO3为代表的钙钛矿氧化物，可能形成一种基于异类材料的新型固溶体。
发明内容
针对现有弛豫铁电固溶体都基于同类材料、而没有基于异类材料固溶体的现状，本发明提供一种基于异类材料钨青铜结构与钙钛矿结构氧化物形成的新型固溶体及其制备方法。
本发明固溶体采用的技术方案如下：
一种钨青铜与钙钛矿结构氧化物形成的固溶体，包括钨青铜结构Sr0.75Ba0.25Nb2O6和钙钛矿结构0.94Bi0.5Na0.5TiO3-0.06BaTiO3，分别用SBN和BNBT表示，所述固溶体的化学式为(1-x)SBN-xBNBT，其中，BNBT中的Ti4+离子取代SBN中的Nb5+离子，BNBT中的部分Bi3+、Na+和Ba2+离子取代SBN中的Sr2+和Ba2+离子，而其余部分Bi3+、Na+和Ba2+离子占据SBN中本来未被占据的晶格位置。
进一步地，x的取值为0.05、0.10、0.15或者0.20。
本发明一种钨青铜与钙钛矿结构氧化物形成的固溶体的制备方法，包括以下步骤：
(1)根据化学式(1-x)SBN-xBNBT称量经过干燥处理的单相SBN粉末和BNBT粉末；
(2)将步骤(1)称量的两种单相粉末通过球磨处理使其混合均匀，混合后的粉末经干燥处理后压制成薄圆片，并置于坩埚中，在1200-1300℃高温下烧结3h，获得致密性良好的(1-x)SBN-xBNBT混合式固溶体。
本发明的有益效果在于：
1、通过把不同摩尔比的钨青铜结构氧化物SBN和钙钛矿结构氧化物BNBT单相粉末混合并高温烧结，形成(1-x)SBN-xBNBT固溶体陶瓷。该固溶体陶瓷样品制备方法简便、效率高，期间无复杂工艺和昂贵的设备，成本较低。
2、与传统的基于同类材料的固溶体相比，本发明利用钨青铜结构SBN存在未被占据的晶格位置的特点，实现基于钨青铜-钙钛矿结构氧化物的新型固溶体陶瓷，可显著改变固溶体陶瓷的微观形貌并在大范围内可调控固溶体陶瓷的电学性质，并具有优异的室温储能性质，为设计新型固溶体提供了一种新思路。
附图说明
图1是实施例制备得到的系列(1-x)SBN-xBNBT陶瓷样品的X射线衍射谱。
图2是实施例制备得到的系列(1-x)SBN-xBNBT陶瓷样品的扫描电子显微镜图，(a)、(b)、(c)、(d)分别是实施例1、2、3、4制备得到的陶瓷样品的结构图。
图3是实施例制备得到的系列(1-x)SBN-xBNBT陶瓷样品的介电常数(上面一排图)和介电损耗谱(下面一排图)。
图4是实施例制备得到的系列(1-x)SBN-xBNBT陶瓷样品的室温电滞回线图。
图5是实施例制备得到的系列(1-x)SBN-xBNBT陶瓷样品的室温储能效率和储能密度图。
具体实施方式
实施例1：
称量5.8287克SBN粉末与0.1713克BNBT(x＝0.05)粉末，在两种粉末的混合物中加入适量酒精，然后球磨24小时使两种粉末混合均匀。所得的粉末进行干燥处理后，用15MPa的压力把适量的粉末压成直径约为10毫米，厚度约为2-3毫米的薄片。把适量的相应粉末放入Al2O3坩埚，再把薄片放入，并用相应的粉末覆盖薄片，最后用另一个坩埚倒扣到第一个坩埚上，使薄片处于密封状态。将密封有薄片的坩埚放入马弗炉中并升温，从室温到烧结温度(1200℃)的升温速率控制在3℃/分钟。在1300℃烧结3h后，以3℃/分钟的降温速率降温至600℃，然后自然降温。获得(1-x)SBN-xBNBT陶瓷；对上述样品进行微观结构，形貌和性能测试。
实施例2：
称量5.6496克SBN粉末与0.3504克BNBT(x＝0.10)粉末，在两种粉末的混合物中加入适量酒精，然后球磨24小时使两种粉末混合均匀。所得的粉末进行干燥处理后，用15MPa的压力把适量的粉末压成直径约为10毫米，厚度约为2-3毫米的薄片。把适量的相应粉末放入Al2O3坩埚，再把薄片放入，并用相应的粉末覆盖薄片，最后用另一个坩埚倒扣到第一个坩埚上，使薄片处于密封状态。将密封有薄片的坩埚放入马弗炉中并升温，从室温到烧结温度(1250℃)的升温速率控制在3℃/分钟。在1220℃烧结3h后，以3℃/分钟的降温速率降温至600℃，然后自然降温。获得(1-x)SBN-xBNBT陶瓷；对上述样品进行微观结构，形貌和性能测试。
实施例3：
称量5.4620克SBN粉末与0.5380克BNBT(x＝0.15)粉末，在两种粉末的混合物中加入适量酒精，然后球磨24小时使两种粉末混合均匀。所得的粉末进行干燥处理后，用15MPa的压力把适量的粉末压成直径约为10毫米，厚度约为2-3毫米的薄片。把适量的相应粉末放入Al2O3坩埚，再把薄片放入，并用相应的粉末覆盖薄片，最后用另一个坩埚倒扣到第一个坩埚上，使薄片处于密封状态。将密封有薄片的坩埚放入马弗炉中并升温，从室温到烧结温度(1200℃)的升温速率控制在3℃/分钟。在1200℃烧结3h后，以3℃/分钟的降温速率降温至600℃，然后自然降温。获得(1-x)SBN-xBNBT陶瓷；对上述样品进行微观结构，形貌和性能测试。
实施例4：
称量5.2652克SBN粉末与0.7348克BNBT(x＝0.20)粉末，在两种粉末的混合物中加入适量酒精，然后球磨24小时使两种粉末混合均匀。所得的粉末进行干燥处理后，用15MPa的压力把适量的粉末压成直径约为10毫米，厚度约为2-3毫米的薄片。把适量的相应粉末放入Al2O3坩埚，再把薄片放入，并用相应的粉末覆盖薄片，最后用另一个坩埚倒扣到第一个坩埚上，使薄片处于密封状态。将密封有薄片的坩埚放入马弗炉中并升温，从室温到烧结温度(1200℃)的升温速率控制在3℃/分钟。在1200℃烧结3h后，以3℃/分钟的降温速率降温至600℃，然后自然降温。获得(1-x)SBN-xBNBT陶瓷；对上述样品进行微观结构，形貌和性能测试。
测试结果：
图1是上述实施例制备得到的系列(1-x)SBN-xBNBT陶瓷样品的X射线衍射谱(XRD)，可以看出，样品均具有钨青铜结构。这说明钙钛矿BNBT中的Bi3+，Na+，Ba2+和Ti4+阳离子完全扩散进入钨青铜SBN中Sr2+、Ba2+和Ti4+离子占据的晶格位置和原本未被占据的晶格位置，形成固溶体。
图2是制备得到的系列(1-x)SBN-xBNBT陶瓷样品的扫描电子显微镜图(SEM)，可以看出，随着BNBT加入量的增加，柱状晶粒逐步增加且长径比逐渐增大，在x＝0.20时长径比急剧增大达到10.5。
图3是制备得到的系列(1-x)SBN-xBNBT陶瓷样品的介电常数和介电损耗谱，可以看出，铁电-顺电相变对应一个相对宽而平展的峰；与此同时，随着频率的增加，在介电常数实部峰值显著降低的同时，峰值对应的温度(Tm)明显向高温移动，也就是说存在频率色散现象，这也很好地证实了(1-x)SBN-xBNBT固溶体为驰豫铁电体，而驰豫现象的来源主要与成分起伏所引起的微观结构的无序有关。可以看出，固溶体的Tm显著依赖于其成分且在-61℃-43℃的大范围内可调。
图4是制备得到的系列(1-x)SBN-xBNBT陶瓷样品的电滞回线(P-E)图，可以看出，随着BNBT掺入量的增加，电滞回线首先变得细长然后再恢复，在x＝0.10时达到最细，这也与前所述的居里温度变化趋势是一致的。
图5是制备得到的系列(1-x)SBN-xBNBT陶瓷样品的储能性能图，可以看出，由于近乎理想的驰豫性质，本发明(1-x)SBN-xBNBT固溶体表现出良好的室温储能效率，在x＝0.10时达到最大93％。

Claims (5)

1.一种钨青铜与钙钛矿结构氧化物形成的固溶体，包括钨青铜结构Sr0.75Ba0.25Nb2O6和钙钛矿结构0.94Bi0.5Na0.5TiO3-0.06BaTiO3，分别用SBN和BNBT表示，其特征在于，所述固溶体的化学式为(1-x)SBN-xBNBT，其中，BNBT中的Ti4+离子取代SBN中的Nb5+离子晶格位置，BNBT中的部分Bi3+、Na+和Ba2+离子取代结构SBN中的Sr2+和Ba2+离子晶格位置，而其余部分Bi3+、Na+和Ba2+离子占据SBN中本来未被占据的晶格位置。
2.根据权利要求1所述的一种钨青铜与钙钛矿结构氧化物形成的固溶体，其特征在于，x的取值为0.05、0.10、0.15或者0.20。
3.根据权利要求1所述一种钨青铜与钙钛矿结构氧化物形成的固溶体的制备方法，其特征在于，包括以下步骤：
(1)根据化学式(1-x)SBN-xBNBT称量经过干燥处理的单相SBN粉末和BNBT粉末；
(2)将步骤(1)称量的两种单相粉末通过球磨处理使其混合均匀，混合后的粉末经干燥处理后压制成薄片，并置于坩埚中，在高温下烧结，获得致密性良好的(1-x)SBN-xBNBT混合式固溶体。
4.根据权利要求3所述的制备方法，其特征在于，所述步骤(2)中，将混合后的粉末压制成薄圆片。
5.根据权利要求3所述的制备方法，其特征在于，所述步骤(2)中，将薄片在1200-1300℃高温烧结3h。
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