CN107827453A - 一种低介电损耗钛酸锶陶瓷的制备方法 - Google Patents

一种低介电损耗钛酸锶陶瓷的制备方法 Download PDF

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CN107827453A
CN107827453A CN201710038502.7A CN201710038502A CN107827453A CN 107827453 A CN107827453 A CN 107827453A CN 201710038502 A CN201710038502 A CN 201710038502A CN 107827453 A CN107827453 A CN 107827453A
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strontium titanate
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李蔚
韩蕊
严嵩
刘会娇
彭华庆
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East China University of Science and Technology
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Abstract

本发明公开了一种低介电损耗钛酸锶陶瓷的制备方法。其制备过程如下：以高纯（99.9%）SrTiO3粉体为原料，以CaO、MgO、Al2O3、ZrO2、Nb2O5中的一种或多种作为添加剂，经湿法球磨与SrTiO3粉料混合，然后通过无压烧结制备钛酸锶陶瓷。据大量数据统计表明：掺杂一定量的添加剂得到的SrTiO3陶瓷样品，介电损耗低，介电性能得到了大幅度地提高。典型地，当添加2wt%Nb2O5时，其Q×f值可达6,281GHZ，大约是纯SrTiO3(1,145GHz)陶瓷样品的5.5倍。此外，本发明制备工艺简单，可控性强，具有良好的工业化前景。

Description

一种低介电损耗钛酸锶陶瓷的制备方法
技术领域
本发明涉及一种低介电损耗钛酸锶陶瓷材料，属于环境友好型的微波介电陶瓷领域，可用于微波通讯等领域。
背景技术
近年来，随着信息处理技术和电子信息数字化技术的快速发展，微波通讯技术占据着越来越重要的地位，这就要求微波介质材料具有高的介电常数（εr）,高的Q×f值和近零频率温度系数(τ f )。SrTiO3陶瓷，室温下具有很高的介电常数εr(~230)和很大的正温度系数τf≈+1100ppm/℃，可与低介电常数，负温度系数的材料复合，获得一些性能优良的微波介质材料。例如Yuan-Bin Chen 等指出在0.55La(Mg1/2Ti1/2) O3-0.45SrTiO3陶瓷体系中加入0.25wt% B2O3，得到的样品介电常数为46.32,Q×f值为34,000(GHz), 温度系数τ f 为-0.12ppm/℃。Cheng-Shing 等人的研究表明，掺杂0.25wt% CuO于0.5LaAlO3-0.5SrTiO3体系中，样品的介电性能良好：εr =35.2，Q×f= 24,000GHz，τ f =-13.5ppm/℃。Won Woo等报道了把2wt% 的 B2O3掺杂到0.96MgTiO3-0.036SrTiO3陶瓷体系中，样品的介电性能为：εr=19，Q×f=75,300GHz，τ f =-8.9ppm/℃。但是由于晶格中各阶非谐振振荡，衰减的存在，以及材料内部缺陷，杂质以及气孔的影响，SrTiO3陶瓷介电损耗较大，Q×f值并不高（~1000GHz），这将影响所形成的复合材料的性能。因此降低钛酸锶材料的介电损耗，从而进一步提高复合材料的Q×f值是一项紧迫且有重大意义的课题。
钙钛矿（ABO3）结构对外来离子有着较强的相容能力，只要满足电中性和离子配合半径的要求，A位和B位均可被外来离子占据而变成复合钙钛矿结构，并由此引发各种新的性能。因此，在这里我们可以通过掺杂来降低材料的介电损耗，进而提高钛酸锶材料的微波介电性能。
发明内容
本发明目的在于提供一种低介电损耗钛酸锶陶瓷材料，解决现有技术中钛酸锶材料介电损耗（tanδ）较高、Q ×f值较低的问题。
为了实现上述发明目的，本发明采用的技术方案如下：首先以SrTiO3作为原料，选用CaO、MgO、Al2O3、 ZrO2、Nb2O5中的一种或多种作为掺杂物，湿法球磨（为了有助于干粉的成型，可在球磨过程中加入少许粘结剂）干燥后，经研磨、过筛得到混合干粉。
优选的，上述氧化物的掺杂量为0.5~5wt%；其中，当掺杂量为0时，即钛酸锶陶瓷粉体材料中未掺杂氧化物，最后所得的SrTiO3陶瓷样品Q ×f值为1,145GHz；当Nb2O5的掺杂量为2wt%时，最后所得的SrTiO3陶瓷材料的Q ×f值达到最高为6,281GHz，大约是纯钛酸锶陶瓷材料的5.5倍，介电性能得到了很大的改善。
优选的，球磨时间为24h，球磨介质为去离子水。
前述的一种低介电损耗钛酸锶陶瓷的制备方法，将前述的混合干粉在50~200MPa的压强下干压成型，压制成直径约16mm，高度约12mm的柱形样品，然后将样品放置于马弗炉中升温至1300~1500℃烧结2~6h, 得到致密的SrTiO3陶瓷样品。
优选的，干压成型的压强为100MPa，样品的烧结温度为1450℃，保温时间为4h。
本发明的有益效果：本发明选用氧化物掺杂来调节SrTiO3陶瓷样品的介电性能，降低其介电损耗，其操作方法简单，生产流程短，所需要的工艺设备也很简单。另外，在本发明中，成型方法为普通干压成型，所需的成型压力为50~200MPa，在很短的时间内加压就可获得介电性能良好的SrTiO3陶瓷样品，可大量节约时间成本。此外，由于本发明采用价格低廉易于供应的CaO、MgO、Al2O3、 ZrO2、Nb2O5中的一种或多种用为掺杂物，大大节约了生产成本，适合规模化生产。在本发明中，掺杂量适中的SrTiO3陶瓷样品，介电损耗大大降低，介电性能得到了大幅度地改善，其Q×f值大约是纯SrTiO3陶瓷样品的5~6倍。
附图说明
图1 是本发明优选实施例1 ~实施例4中95瓷样品的配方以及Q × f 值。
下面结合图表和具体实施方式对本发明作进一步的说明。
具体实施方式
实施例1：一种低介电损耗钛酸锶陶瓷，它是通过以下方法制备而成的：取高纯钛酸锶粉体20g，放置于球磨罐中，以去离子水为研磨介质（为了助于干粉的成型，可在研磨过程中加入少许粘结剂），球磨24h后在80℃的烘箱中干燥。然后将干燥后的块体进行研磨，过筛，最后在100MPa的压强下将粉末干压成直径约16mm、高度约12mm的柱行样品，置于马弗炉中1450℃下保温4h。
将烧制好的样品放置若干小时后，进行介电性能测试，结果显示：所得的纯钛酸锶陶瓷样品介电常数为295，Q ×f值为1,145GHz。
实施例2：一种低介电损耗钛酸锶陶瓷，它是通过以下方法制备而成的：取6份高纯SrTiO3粉末，每份20g，放置于6个球磨罐中，选用ZrO2作为掺杂物，其掺杂含量为0.5~5wt%，随后将混合料进行湿法球磨，以去离子水作为研磨介质。球磨24h后在80℃的烘箱中干燥。然后将干燥后的块体进行研磨、过筛，最后在100MPa的压强下将粉末干压成直径约16mm、高度约12mm的柱行样品，置于马弗炉中1450℃下保温4h。
将烧制好的样品放置若干小时后，进行介电性能测试，结果显示如图1所示：当ZrO2的掺杂量达到2wt%时，其Q ×f值达到最高，为6,170GHz，介电常数为278。
实施例3：一种低介电损耗钛酸锶陶瓷，它是通过以下方法制备而成的：取6份高纯SrTiO3粉末，每份20g，放置于6个球磨罐中，Nb2O5的掺杂量为0.5~5wt%，随后将混合料进行湿法球磨，以去离子水作为研磨介质，球磨24h后在80℃的烘箱中干燥。然后将干燥后的块体进行研磨，过筛，最后在100MPa的压强下将粉末干压成直径约16mm、高度约12mm的柱行样品，置于马弗炉中1450℃下保温4h。
将烧制好的样品放置若干小时后，进行介电性能测试，结果显示：当Nb2O5的掺杂量达到2wt%时，其Q ×f值最高为6,281GHz，介电常数为286。
实施例4：一种低介电损耗钛酸锶陶瓷，它是通过以下方法制备而成的：取6份高纯SrTiO3粉末，每份20g，放置于6个球磨罐中，选用Al2O3、Nb2O5作为掺杂剂，总的掺杂含量为0.5~5wt%，随后将混合料进行湿法球磨，以去离子水作为研磨介质，球磨24h后在80℃的烘箱中干燥。然后将干燥后的块体进行研磨，过筛，最后在100MPa的压强下将粉末干压成直径约16mm、高度约12mm的柱行样品，置于马弗炉中1450℃下保温4h。
将烧制好的样品放置若干小时后，进行介电性能测试，结果显示：当Al2O3和Nb2O5的掺杂量各为1wt%，其Q ×f值最高为5,781GHz，介电常数为283。
实施例5：一种低介电损耗钛酸锶陶瓷，它是通过以下方法制备而成的：取6份高纯SrTiO3粉末，每份20g，放置于6个球磨罐中，CaO、ZrO2、Nb2O5作为掺杂物，总的掺杂含量为0.5~5wt%，随后将混合料进行湿法球磨，以去离子水作为研磨介质，球磨24h后在80℃的烘箱中干燥。然后将干燥后的块体进行研磨，过筛，最后在100MPa的压强下将粉末干压成直径约16mm、高度约12mm的柱行样品，置于马弗炉中1450℃下保温4h。
将烧制好的样品放置若干小时后，进行介电性能测试，结果显示：当CaO、ZrO2、Nb2O5的掺杂量分别为0.4wt%、1wt%、0.6wt%时，其Q ×f值最高为5,821GHz，介电常数为279。
实施例6：一种低介电损耗钛酸锶陶瓷，它是通过以下方法制备而成的：取6份高纯SrTiO3粉末，每份20g，放置于6个球磨罐中，选用MgO、Al2O3、ZrO2、Nb2O5作为掺杂物，总的掺杂含量为0.5~5wt%，随后将混合料进行湿法球磨，以去离子水作为研磨介质，球磨24h后于80℃的烘箱中干燥。然后将干燥后的块体进行研磨，过筛，最后在100MPa的压强下将粉末干压成直径约16mm、高度约12mm的柱行样品，置于马弗炉中1450℃下保温4h。
将烧制好的样品放置若干小时后，进行介电性能测试，结果显示：当MgO、Al2O3、ZrO2、Nb2O5的掺杂量分别为0.2wt%、0.2wt%、1wt%、0.6wt%时，其Q ×f值最高为5,636GHz，介电常数为280。

Claims (5)

1.一种低介电损耗钛酸锶陶瓷的制备方法，其特征在于该方法的具体步骤为：(1) 以高纯SrTiO3粉体为原料，放置于球磨罐中，然后分别加入CaO、MgO、Al2O3、 ZrO2、Nb2O5 等掺杂物中的一种或多种，湿法球磨干燥后经研磨，过筛得到混合干粉；(2)将步骤 (1) 得到的混合干粉压制成型，烧制，即可得到不同掺杂的钛酸锶陶瓷样品。
2.根据权利要求1所述一种低介电损耗钛酸锶陶瓷制备方法，其特征在于：步骤 (1)中，所述掺杂物的含量为0.5~5wt%；所述的球磨时间为12~24h，所述的球磨介质为去离子水。
3.根据权利要求1所述一种低介电损耗钛酸锶陶瓷制备方法，其特征在于：步骤 (2)中，所述样品的烧结温度为1300~1500 ℃，保温时间为2~6h，升温速度为2~5 ℃/min。
4.根据权利要求3所述的一种低介电损耗钛酸锶陶瓷的制备方法，其特征在于，取权利要求1步骤 (1) 所述的混合干粉，将粉末干压成直径约16mm，高度约12mm的柱形样品，然后将样品放置于马弗炉中升温至1450 ℃烧结4h，得到致密的钛酸锶陶瓷样品。
5.烧结过程中，炉子的升温速度为2 ℃/min。
CN201710038502.7A 2017-01-19 2017-01-19 一种低介电损耗钛酸锶陶瓷的制备方法 Pending CN107827453A (zh)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112876229A (zh) * 2021-03-22 2021-06-01 南宁国人射频通信有限公司 一种微波陶瓷及其制备方法
CN114644519A (zh) * 2022-02-28 2022-06-21 华南理工大学 一种介电陶瓷材料及其制备方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112876229A (zh) * 2021-03-22 2021-06-01 南宁国人射频通信有限公司 一种微波陶瓷及其制备方法
CN114644519A (zh) * 2022-02-28 2022-06-21 华南理工大学 一种介电陶瓷材料及其制备方法

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