CN113354409A - 微波介质陶瓷及其制备方法 - Google Patents

微波介质陶瓷及其制备方法 Download PDF

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CN113354409A
CN113354409A CN202110634264.2A CN202110634264A CN113354409A CN 113354409 A CN113354409 A CN 113354409A CN 202110634264 A CN202110634264 A CN 202110634264A CN 113354409 A CN113354409 A CN 113354409A
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microwave dielectric
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dielectric ceramic
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mass fraction
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宿金栋
蒋韶华
范宇
余亮
郭槐
梁宝龙
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Zhenjin New Materials Shenzhen Co ltd
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Abstract

本发明公开了一种微波介质陶瓷及其制备方法，所述微波介质陶瓷为RO掺杂镁钙钛体系陶瓷，其化学组成表达式为aMgTiO3‑bCaTiO3‑RO；其中，所述镁钙钛体系陶瓷为主料，其化学表达式为aMgTiO3‑bCaTiO3，a、b分别代表摩尔比，0.90≤a≤0.99，0.01≤b≤0.1，a+b＝1；所述RO为烧结助剂，包括MnO2、Fe2O3、ZnO、SiO2、Nb2O5、Cr2O3、La2O3、NiO、ZrO2及Nd2O3中至少一种。本发明的微波介质陶瓷，以作为烧结助剂的RO掺杂镁钙钛体系陶瓷形成微波介质陶瓷，具有优异的微波介电性能，品质因数高，介电常数适中，具备较好的温度稳定性且力学性能优异，具有广泛的应用前景，且制备工艺简单，操作方便重复性好。

Description

微波介质陶瓷及其制备方法
技术领域
本发明涉及陶瓷材料技术领域，尤其涉及一种微波介质陶瓷及其制备方法。
背景技术
微波介质陶瓷作为一种新型功能陶瓷，具有介电常数大、介电损耗低、谐振频率温度系数小等特点，可制成滤波器、谐振器、振荡器、波导传输线、介质天线等元器件，在移动通信、卫星直播、无线电遥控、雷达、GPS等微波通信领域有广泛的应用，是当前通信技术的关键材料。目前业内微波介质陶瓷滤波器生产厂家都采用固相法高温烧结制备，工艺复杂，陶瓷力学性能差，长时间使用温度稳定性差、容易产生裂纹，无法正常工作，所以对其实际应用有极大限制。
发明内容
为解决上述技术问题，本发明的一个目的在于提供一种微波介质陶瓷，旨在解决现有技术中微波介质陶温度稳定性和力学性能差、工艺复杂的技术问题。
本发明的另一目的在于提供一种上述微波介质陶瓷的制备方法。
本发明解决其技术问题所采用的技术方案是：提供一种微波介质陶瓷，所述微波介质陶瓷为RO掺杂镁钙钛体系陶瓷，其化学组成表达式为aMgTiO3-bCaTiO3-RO；
其中，所述镁钙钛体系陶瓷为主料，其化学组成表达式为aMgTiO3-bCaTiO3，a、b分别代表摩尔比，0.90≤a≤0.99，0.01≤b≤0.1，a+b＝1；所述RO为烧结助剂，包括MnO2、Fe2O3、ZnO、SiO2、Nb2O5、Cr2O3、La2O3、NiO、ZrO2及Nd2O3中至少一种。
优选地，所述RO包括MnO2，其相对于主料的质量分数为0％-1％。
优选地，所述RO包括Fe2O3，其相对于主料的质量分数为0％-1％。
优选地，所述RO包括ZnO，其相对于主料的质量分数为0％-1％。
优选地，所述RO包括SiO2，其相对于主料的质量分数为0％-1％。
优选地，所述RO包括Nb2O5，其相对于主料的质量分数为0％-1％。
优选地，所述RO包括Cr2O3，其相对于主料的质量分数为0％-1％。
优选地，所述RO包括La2O3，其相对于主料的质量分数为0％-1％。
优选地，所述RO包括NiO，其相对于主料的质量分数为0％-1％。
优选地，所述RO包括ZrO2，其相对于主料的质量分数为0％-1％。
优选地，所述RO包括Nd2O3，其相对于主料的质量分数为0％-1％。
优选地，所述镁钙钛体系陶瓷的粉体粒径为1～10μm。
本发明还提供一种微波介质陶瓷的制备方法，包括以下步骤：
(1)以纯度在99％以上的MgO、TiO2、CaCO3为原料，球磨充分混合均匀，烘干、预烧，得到镁钙钛体系陶瓷，作为微波介质陶瓷的主料；
(2)以纯度在99.9％以上的烧结助剂进行掺杂：将主料和烧结助剂进行混合，然后充分球磨，再经过烘干、造粒和过筛，将过筛后的混合粉料压制成型，最后烧结得到微波介质陶瓷。
优选地，步骤(1)中，所述烘干的温度为200℃。
优选地，步骤(1)中，所述预烧的工艺参数为：预烧温度为1000℃～1200℃，预烧时间为2～6小时。
优选地，步骤(2)中，所述烧结的工艺参数为：烧结温度为1300℃～1360℃，烧结时间为3～6小时。
优选地，步骤(2)中，所述造粒是将烘干后的粉体与纯化水混合，然后制成微米级的球形颗粒。
优选地，步骤(2)中，过筛后的混合粉料被压制成直径为10mm、高度为8mm的圆柱体。
优选地，步骤(1)中的预烧以及步骤(2)中的烧结均是在空气氛围下进行。
本发明的有益效果：以作为烧结助剂的RO掺杂镁钙钛体系陶瓷形成微波介质陶瓷，具有优异的微波介电性能，品质因数高，介电常数适中，具备较好的温度稳定性且力学性能优异，具有广泛的应用前景，且制备工艺简单，操作方便重复性好。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅用以解释本发明，并不用于限定本发明。
本发明的微波介质陶瓷，为RO掺杂镁钙钛体系陶瓷，其化学组成表达式为aMgTiO3-bCaTiO3-RO。
其中，镁钙钛体系陶瓷为主料，其化学组成表达式为aMgTiO3-bCaTiO3，a、b分别代表摩尔比，0.90≤a≤0.99，0.01≤b≤0.1，a+b＝1。镁钙钛体系陶瓷的粉体粒径优选为1～10μm。
RO为烧结助剂，其可包括MnO2、Fe2O3、ZnO、SiO2、Nb2O5、Cr2O3、La2O3、NiO、ZrO2及Nd2O3中至少一种。在RO包括上述中任一种时，其相对于主料的质量分数为0％-1％；在RO包括上述中多种时，每一种相对于主料的质量分数为0％-1％。
本发明的微波介质陶瓷的制备方法，可包括以下步骤：
(1)以纯度在99％以上的MgO、TiO2、CaCO3为原料，按照组成表达式aMgTiO3-bCaTiO3中各元素的摩尔比进行配料，先溶解于去离子水，然后球磨充分混合均匀，烘干、预烧，得到镁钙钛体系陶瓷，作为微波介质陶瓷的主料。
其中，烘干的温度为200℃。预烧的工艺参数为：预烧温度为1000℃～1200℃，预烧时间为2～6小时。
(2)以纯度在99.9％以上的烧结助剂进行掺杂：相对于主料的质量，按照质量分数分别称取MnO2、Fe2O3、ZnO、SiO2、Nb2O5、Cr2O3、La2O3、NiO、ZrO2及Nd2O3中至少一种，然后将主料和烧结助剂进行混合，然后充分球磨，再经过烘干、造粒和过筛，将过筛后的混合粉料压制成型，最后烧结得到微波介质陶瓷。
其中，造粒是将烘干后的粉体与纯化水混合，然后制成微米级的球形颗粒。过筛后的混合粉料被压制成直径为10mm、高度为8mm的圆柱体。烧结的工艺参数为：烧结温度为1300℃～1360℃，烧结时间为3～6小时。
上述步骤(1)中的预烧以及步骤(2)中的烧结均是在空气氛围下进行。
以下结合具体实施例对本发明进行详细说明。
实施例1
微波介质陶瓷0.955MgTiO3-0.045CaTiO3-MnO2-SiO2，为烧结助剂MnO2和SiO2掺杂的镁钙钛陶瓷，其中MnO2相对于主料0.955MgTiO3-0.045CaTiO3的质量分数为0.21％；SiO2相对于主料的0.955MgTiO3-0.045CaTiO3质量分数为0.13％。
上述微波介质陶瓷的制备方法，包括以下步骤：
(1)以纯度在99％以上的MgO、TiO2、CaCO3为原料，溶解于去离子水中，然后球磨充分混合均匀，配制形成的混合溶液置于200℃的烘箱中烘干，粉碎，过筛；将过筛获得的粉体进行预烧，预烧温度为1000℃，预烧时间为2小时，得到主料镁钙钛陶瓷粉体；
(2)向镁钙钛陶瓷粉体中加入烧结助剂MnO2和SiO2、分散剂、脱模剂、粘结剂进行喷雾造粒和压制成型；将成型坯料在马弗炉中进行烧结，烧结温度为1360℃，烧结时间为4小时，即得微波介质陶瓷。
实施例2
微波介质陶瓷0.955MgTiO3-0.045CaTiO3-SiO2-ZrO2-Fe2O3，为烧结助剂SiO2、ZrO2和Fe2O3掺杂的镁钙钛陶瓷，其中SiO2相对于主料0.955MgTiO3-0.045CaTiO3的质量分数为0.15％；ZrO2相对于主料的0.955MgTiO3-0.045CaTiO3质量分数为0.91％；Fe2O3相对于主料的0.955MgTiO3-0.045CaTiO3质量分数为0.18％。
上述微波介质陶瓷的制备方法，包括以下步骤：
(1)以纯度在99％以上的MgO、TiO2、CaCO3为原料，溶解于去离子水中，然后球磨充分混合均匀；将配制形成的混合溶液置于200℃的烘箱中烘干，粉碎，过筛；将过筛获得的粉体进行预烧，预烧温度为1050℃，预烧时间为2小时，得到主料镁钙钛陶瓷粉体；
(2)向镁钙钛陶瓷粉体中加入烧结助剂SiO2、ZrO2和Fe2O3、分散剂、脱模剂、粘结剂进行喷雾造粒和压制成型；将成型坯料在马弗炉中进行烧结，烧结温度为1340℃，烧结时间为3小时，即得微波介质陶瓷。
实施例3
微波介质陶瓷0.955MgTiO3-0.045CaTiO3-Cr2O3-ZrO2-Fe2O3-Nd2O3，烧结助剂Cr2O3、ZrO2、Fe2O3、Nd2O3掺杂的镁钙钛陶瓷，其中Cr2O3相对于主料的0.955MgTiO3-0.045CaTiO3质量分数为0.05％；ZrO2相对于主料的0.955MgTiO3-0.045CaTiO3质量分数为0.15％；Fe2O3相对于主料的0.955MgTiO3-0.045CaTiO3质量分数为0.23％；Nd2O3相对于主料0.955MgTiO3-0.045CaTiO3的质量分数为0.18％。
上述微波介质陶瓷的制备方法，包括以下步骤：
(1)以纯度在99％以上的MgO、TiO2、CaCO3为原料，溶解于去离子水中，然后球磨充分混合均匀；将配制形成的混合溶液置于200℃的烘箱中烘干，粉碎，过筛；将过筛获得的粉体进行预烧，预烧温度为1100℃，预烧时间为3小时，得到主料镁钙钛陶瓷粉体；
(2)向镁钙钛陶瓷粉体中加入烧结助剂Cr2O3、ZrO2、Fe2O3和Nd2O3、分散剂、脱模剂、粘结剂进行喷雾造粒和压制成型；将步成型坯料在马弗炉中进行烧结，烧结温度为1360℃，烧结时间为3.5小时，即得微波介质陶瓷。
实施例4
微波介质陶瓷0.955MgTiO3-0.045CaTiO3-MnO2-Nb2O5-NiO-La2O3，烧结助剂MnO2、Nb2O5、NiO、La2O3掺杂的镁钙钛陶瓷，其中MnO2相对于主料0.955MgTiO3-0.045CaTiO3的质量分数为0.16％；Nb2O5相对于主料的0.955MgTiO3-0.045CaTiO3质量分数为0.2％；NiO相对于主料的0.955MgTiO3-0.045CaTiO3质量分数为0.12％；La2O3相对于主料的0.955MgTiO3-0.045CaTiO3质量分数为0.75％。
上述微波介质陶瓷的制备方法，包括以下步骤：
(1)以纯度在99％以上的MgO、TiO2、CaCO3为原料，溶解于去离子水中，然后球磨充分混合均匀；将配制形成的混合溶液置于200℃的烘箱中烘干，粉碎，过筛；将过筛获得的粉体进行预烧，预烧温度为1000℃，预烧时间为2小时，得到主料镁钙钛陶瓷粉体；
(2)向镁钙钛陶瓷粉体中加入烧结助剂MnO2、Nb2O5、NiO和La2O3、分散剂、脱模剂、粘结剂进行喷雾造粒和压制成型；将成型坯料在马弗炉中进行烧结，烧结温度为1340℃，烧结时间为5小时，即得微波介质陶瓷。
对实施例1～4制备得到的微波介质陶瓷样品进行性能检测，包括相对介电常数εr、品质因数(Q×f)和谐振频率温度系数τf以及力学性能，结果见表1。
表1
Figure BDA0003104771450000071
由表1检测结果可以看出，本发明实施例1～4制备的微波介质陶瓷具有很高品质因数、近零谐振频率温度系数以及合适的相对介电常数，且力学性能优异，可靠性好，长期使用不会产生裂纹，提高了使用寿命，降低成本，具有优异的微波介电性能且制备工艺简单，操作方便重复性好。
以上所述仅为本发明的实施例，并非因此限制本发明的专利范围，凡是利用本发明说明书内容所作的等效结构或等效流程变换，或直接或间接运用在其他相关的技术领域，均同理包括在本发明的专利保护范围内。

Claims (10)

1.一种微波介质陶瓷，其特征在于，所述微波介质陶瓷为RO掺杂镁钙钛体系陶瓷，其化学组成表达式为aMgTiO3-bCaTiO3-RO；
其中，所述镁钙钛体系陶瓷为主料，其化学组成表达式为aMgTiO3-bCaTiO3，a、b分别代表摩尔比，0.90≤a≤0.99，0.01≤b≤0.1，a+b＝1；所述RO为烧结助剂，包括MnO2、Fe2O3、ZnO、SiO2、Nb2O5、Cr2O3、La2O3、NiO、ZrO2及Nd2O3中至少一种。
2.如权利要求1所述的微波介质陶瓷，其特征在于，所述RO包括MnO2，其相对于主料的质量分数为0%-1%；或，
所述RO包括Fe2O3，其相对于主料的质量分数为0%-1%；或，
所述RO包括ZnO，其相对于主料的质量分数为0%-1%；或，
所述RO包括SiO2，其相对于主料的质量分数为0%-1%；或，
所述RO包括Nb2O5，其相对于主料的质量分数为0%-1%；或，
所述RO包括Cr2O3，其相对于主料的质量分数为0%-1%；或，
所述RO包括La2O3，其相对于主料的质量分数为0%-1%；或，
所述RO包括NiO，其相对于主料的质量分数为0%-1%；或，
所述RO包括ZrO2，其相对于主料的质量分数为0%-1%；或，
所述RO包括Nd2O3，其相对于主料的质量分数为0%-1%。
3.如权利要求1或2所述的微波介质陶瓷，其特征在于，所述镁钙钛体系陶瓷的粉体粒径为1～10μm。
4.一种权利要求1～3任一项所述的微波介质陶瓷的制备方法，其特征在于，包括以下步骤：
（1）以纯度在99%以上的MgO、TiO2、CaCO3为原料，球磨充分混合均匀，烘干、预烧，得到镁钙钛体系陶瓷，作为微波介质陶瓷的主料；
（2）以纯度在99.9%以上的烧结助剂进行掺杂：将主料和烧结助剂进行混合，然后充分球磨，再经过烘干、造粒和过筛，将过筛后的混合粉料压制成型，最后烧结得到微波介质陶瓷。
5.如权利要求4所述的微波介质陶瓷的制备方法，其特征在于，步骤（1）中，所述烘干的温度为200℃。
6.如权利要求4所述的微波介质陶瓷的制备方法，其特征在于，步骤（1）中，所述预烧的工艺参数为：预烧温度为1000℃～1200℃，预烧时间为2～6小时。
7.如权利要求4所述的微波介质陶瓷的制备方法，其特征在于，步骤（2）中，所述烧结的工艺参数为：烧结温度为1300℃～1360℃，烧结时间为3～6小时。
8.如权利要求4所述的微波介质陶瓷的制备方法，其特征在于，步骤（2）中，所述造粒是将烘干后的粉体与纯化水混合，然后制成微米级的球形颗粒。
9.如权利要求4所述的微波介质陶瓷的制备方法，其特征在于，步骤（2）中，过筛后的混合粉料被压制成直径为10mm、高度为8mm的圆柱体。
10.如权利要求4所述的微波介质陶瓷的制备方法，其特征在于，步骤（1）中的预烧以及步骤（2）中的烧结均是在空气氛围下进行。
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CN115611625A (zh) * 2022-11-15 2023-01-17 南京国睿微波器件有限公司 一种钛酸镁基微波介质陶瓷及其制备工艺

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