CN109133913A - 一种高介电常数锡钙酸钡钛及其制备方法和应用 - Google Patents

一种高介电常数锡钙酸钡钛及其制备方法和应用 Download PDF

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CN109133913A
CN109133913A CN201810842577.5A CN201810842577A CN109133913A CN 109133913 A CN109133913 A CN 109133913A CN 201810842577 A CN201810842577 A CN 201810842577A CN 109133913 A CN109133913 A CN 109133913A
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黄荣厦
宋海珠
彭聪斐
吴有亮
林华泰
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Guangdong University of Technology
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Abstract

本发明属于材料科学技术领域，公开了一种高介电常数锡钙酸钡钛及其制备方法和应用。该方法包括以下步骤：(1)将TiO2、CaCO3、BaCO3和SnO2混合，以酒精作为介质球磨24h；(2)将球磨后的浆料在烘箱内烘干，然后在1200℃下进行预烧2h；(3)预烧后的粉体造粒后压制成型，在650℃下排胶2h，然后再在1440℃温度下烧结；(4)将步骤(3)所得样品在1.5个大气压的氧气中进行退火处理，温度为1150℃，保温时间为2h；(5)将经过步骤(4)处理后的样品在空气中进行碳还原处理，温度为850℃,保温时间为2h，得到高介电常数锡钙酸钡钛。

Description

一种高介电常数锡钙酸钡钛及其制备方法和应用
技术领域
本发明属于材料科学技术领域，特别涉及一种高介电常数锡钙酸钡钛及其制备方法和应用。
背景技术
介电材料能够存储电能，可以更快地传递能量(即更短的充电或放电时间)，提高介电材料的介电常数对于应用在低电场区域下的能量储存设备至关重要，在混合电动汽车、便携式电子设备和功率脉冲器件中有非常广阔的应用前景。锡钙酸钡钛因具有很高的介电常数，因此在此领域被广泛使用。目前合成锡钙酸钡钛主要是通过传统固相烧结法来制成，通过BaCO3和TiO2以及掺杂元素的氧化物或碳酸盐按一定的比例配料、混合球磨，最后经髙温倍烧得到反应产物。例如Mahmoud E R,Afify A S,Mohamed A.The crossover of(Ba1-xCax)(Ti0.9Sn0.1)O3,piezoelectric ceramics from single-phase to compositewith studying the structural and dielectric properties[J].Journal ofMaterials Science Materials in Electronics,2017,28(16):11591-11602；Zhao C,Wang H,Xiong J,et al.Composition-driven phase boundary and electricalproperties in(Ba0.94Ca0.06)(Ti1-xMx)O3(M＝Sn,Hf,Zr)lead-free ceramics[J].DaltonTransactions,2016,45(15):6466-6480.从相关文献中可以得知，通过传统的固相烧结法制备的锡钙酸钡钛的介电常数最高可以达到25000左右，损耗可以达到0.03左右，为了适应工业发展对此类材料的要求，急需一种更高介电常数，并且有较低损耗的锡钙酸钡钛。
发明内容
为了解决现有技术中的缺点和不足之处，本发明的首要目的在于提供一种高介电常数锡钙酸钡钛的制备方法。
本发明的另一目的在于提供一种上述制备方法制备得到的高介电常数锡钙酸钡钛。
本发明的再一目的在于提供一种上述高介电常数锡钙酸钡钛的应用。
本发明目的通过以下技术方案实现：
一种高介电常数锡钙酸钡钛的制备方法，包括以下步骤：
(1)将TiO2、CaCO3、BaCO3和SnO2按照Ba、Ca、Sn、Ti和O元素的摩尔比0.94：0.06：0.14：0.86：3的比例进行混合，以酒精作为介质球磨24h；
(2)将球磨后的浆料在烘箱内烘干，然后在1200℃下进行预烧2h；
(3)预烧后的粉体造粒后压制成型，在650℃下排胶2h，然后再在1440℃下烧结2h；
(4)将步骤(3)所得样品在1.5个大气压的氧气中进行退火处理，温度为1150℃，保温时间为2h；
(5)将经过步骤(4)处理后的样品进行碳还原处理，温度为850℃，保温时间为2h，得到高介电常数锡钙酸钡钛。
步骤(2)所述预烧为固相烧结法；步骤(3)所述烧结为固相烧结法。
步骤(5)所述碳还原处理具体按照以下步骤：将经过步骤(4)处理后的样品用砂纸进行打磨抛光，以除去样品表面的杂质并形成光滑平整的表面，超声清洗并烘干后置于氧化铝板上，然后用事先表面打磨好的石墨块压在样品正上方，为了防止因石墨块太轻而导致热处理过程中无法保证与样品接触，在石墨块上再放置一个氧化锆柱子，之后放入烧结炉中进行热处理。
一种由上述的制备方法制备得到的高介电常数锡钙酸钡钛，所述高介电常数锡钙酸钡钛的介电常数为36332，介电损耗为0.024。
上述的高介电常数锡钙酸钡钛在制备低电场区域下的能量储存设备中的应用。
与现有技术相比，本发明具有以下优点及有益效果：本发明通过“空气中烧结+1150℃O2退火处理+850℃碳还原处理”这种制备方式，得到一种更高介电常数，更低介电损耗的锡钙酸钡钛。
附图说明
图1是高介电常数锡钙酸钡钛的制备方法流程图。
图2是碳还原处理示意图。
具体实施方法
下面结合实施例对本发明作进一步详细的描述，但本发明的实施方式不限于此。
实施例1：高介电常数锡钙酸钡钛的制备方法如下，流程如图1所示：
一种高介电常数锡钙酸钡钛的制备方法，包括以下步骤：
将TiO2、CaCO3、BaCO3和SnO2按照Ba、Ca、Sn、Ti和O元素的摩尔比0.94：0.06：0.14：0.86：3的比例进行混合，以酒精作为介质球磨24h；
(2)将球磨后的浆料在烘箱内烘干，然后在1200℃下进行预烧(固相烧结法)2h；
(3)预烧后的粉体造粒后压制成型，在650℃下排胶2h，然后再在1440℃下烧结(固相烧结法)2h；
(4)将步骤(3)所得样品在1.5个大气压的氧气中进行退火处理，温度为1150℃，保温时间为2h；
(5)将经过步骤(4)处理后的样品进行碳还原处理，即将样品用砂纸进行打磨抛光，以除去样品表面的杂质并形成光滑平整的表面，超声清洗并烘干后置于氧化铝板上，然后用事先表面打磨好的石墨块压在样品正上方，为了防止因石墨块太轻而导致热处理过程中无法保证与样品接触，在石墨块上再放置一个氧化锆柱子，如图2所示，之后放入烧结炉中进行热处理，温度为850℃，保温时间为2h，得到高介电常数锡钙酸钡钛。
本实施例最后所得高介电常数锡钙酸钡钛与现有技术采用空气中烧结方法获得的锡钙酸钡钛(即为本实施例步骤(3)烧结后所得样品)，介电常数和介电损耗如下表1所示：
表1本实施例高介电常数锡钙酸钡钛的性能
实验结果如表1所示，可以看出“空气中烧结+1150℃O2退火处理+850℃碳还原处理”这种制备方法，相对于传统的固相烧结法，介电常数的提高比率为53.5％，并且介电损耗也有所降低，可见本发明的所使用的方法可以得到相比于传统固相烧结法，更高介电常数的锡钙酸钡钛。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (5)

1.一种高介电常数锡钙酸钡钛的制备方法，其特征在于包括以下步骤：
(1)将TiO2、CaCO3、BaCO3和SnO2按照Ba、Ca、Sn、Ti和O元素的摩尔比0.94：0.06：0.14：0.86：3的比例进行混合，以酒精作为介质球磨24h；
(2)将球磨后的浆料在烘箱内烘干，然后在1200℃下进行预烧2h；
(3)预烧后的粉体造粒后压制成型，在650℃下排胶2h，然后再在1440℃下烧结2h；
(4)将步骤(3)所得样品在1.5个大气压的氧气中进行退火处理，温度为1150℃，保温时间为2h；
(5)将经过步骤(4)处理后的样品进行碳还原处理，温度为850℃，保温时间为2h，得到高介电常数锡钙酸钡钛。
2.根据权利要求1所述的一种高介电常数锡钙酸钡钛的制备方法，其特征在于：步骤(2)所述预烧为固相烧结法；步骤(3)所述烧结为固相烧结法。
3.根据权利要求1所述的一种高介电常数锡钙酸钡钛的制备方法，其特征在于：步骤(5)所述碳还原处理具体按照以下步骤：将经过步骤(4)处理后的样品用砂纸进行打磨抛光，以除去样品表面的杂质并形成光滑平整的表面，超声清洗并烘干后置于氧化铝板上，然后用事先表面打磨好的石墨块压在样品正上方，在石墨块上再放置一个氧化锆柱子，之后放入烧结炉中进行热处理。
4.一种根据权利要求1所述的制备方法制备得到的高介电常数锡钙酸钡钛，其特征在于：所述高介电常数锡钙酸钡钛的介电常数为36332，介电损耗为0.024。
5.根据权利要求4所述的高介电常数锡钙酸钡钛在制备低电场区域下的能量储存设备中的应用。
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CN116143499A (zh) * 2022-12-08 2023-05-23 广东工业大学 一种用于固化锝的锝酸钡陶瓷固化体及其制备方法和应用

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