CN113735580A - 一种复相微波介质陶瓷及其冷烧结制备方法 - Google Patents

一种复相微波介质陶瓷及其冷烧结制备方法 Download PDF

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CN113735580A
CN113735580A CN202111020727.2A CN202111020727A CN113735580A CN 113735580 A CN113735580 A CN 113735580A CN 202111020727 A CN202111020727 A CN 202111020727A CN 113735580 A CN113735580 A CN 113735580A
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郑木鹏
李永强
侯育冬
朱满康
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Abstract

一种复相微波介质陶瓷及其冷烧结制备方法，属于电子陶瓷技术领域。易溶于水的Li2MoO4作为助烧剂，有机物PTFE作为正温度系数调节剂被引入(Ca0.65Bi0.35)(Mo0.65V0.35)O4体系，通过冷烧结方法在150℃和300MPa下，制备得到了一种复相微波介质陶瓷。该复相微波介质陶瓷具有低的介电常数和近零的谐振频率温度系数，在微波介质基板、谐振器等微波电子元器件中有广泛的应用前景。

Description

一种复相微波介质陶瓷及其冷烧结制备方法
技术领域
本发明属于电子陶瓷材料技术领域，具体涉及一种具有低介电常数和近零谐振频率温度系数的复相微波介质陶瓷及其冷烧结制备方法。
背景技术
在现代无线通讯系统飞速发展的今天，用于制造天线、谐振器、电容器和滤波器等电子元件的微波介质陶瓷受到了广泛关注。由于电子元器件要工作在不同的环境中，对其温度稳定性提出了更高的要求。谐振频率温度系数(τf)是评价微波介质陶瓷温度稳定性的关键参数，τf值越接近于零，其温度稳定性越好。目前，微波介质陶瓷的烧结工艺主要是能量密集型的常规高温烧结(>1000℃)，不能与低熔点电极(银、铝等)共烧结(<900℃)，更不能直接与聚合物集成(<200℃)。冷烧结技术(CSP)是一种新型超低温陶瓷烧结工艺，可以使许多陶瓷在极低的温度(<300℃)甚至室温下致密化。
对于陶瓷基复合材料要实现陶瓷与聚合物之间的复合需要经过两步处理，先烧成陶瓷骨架再与聚合物进行复合，这种方法存在有机材料易团聚、复合不均匀和工艺繁琐等缺点。通过冷烧结技术可以实现陶瓷与聚合物的均匀复合，在较低的温度下同时实现陶瓷和有机物的致密化，并且可以通过使用有机材料对陶瓷的介电性能进行调控。
(Ca0.65Bi0.35)(Mo0.65V0.35)O4(CBMVO)是一类具有高性能的微波介质陶瓷，但由于其粉体不溶于水，难以通过冷烧结技术制备。在本发明中，我们首次通过在CBMVO中添加Li2MoO4(LMO，极易溶于水)实现了CBMVO与有机材料聚四氟乙烯(PTFE)的冷烧结制备。基于冷烧结技术制备的新型CBMVO-LMO-PTFE复相陶瓷具有制备工艺简单、低成本、温度稳定性好等一系列优点。
发明内容
本发明提供了一种具有近零谐振频率温度系数的低介CBMVO-LMO-PTFE复相微波陶瓷及其冷烧结制备方法。
为实现上述目的，本发明采取以下技术方案：
一种具有近零谐振频率温度系数的低介CBMVO-LMO-PTFE复相微波陶瓷，其特征在于，该复相材料的化学组成为：(Ca0.65Bi0.35)(Mo0.65V0.35)O4-5wt.％Li2MoO4-xwt.％PTFE，其中0.5≤x≤20，进一步优选PTFE的添加量为3wt.％。
本发明上述具有近零谐振频率温度系数和低介电常数的复相微波材料的制备方法为冷烧结工艺。具体包括以下步骤：
(1)合成CBMVO-LMO陶瓷粉体即(Ca0.65Bi0.35)(Mo0.65V0.35)O4-5wt.％Li2MoO4陶瓷粉体，通过固相反应制备。首先，将原料CaCO3、MoO3、Bi2O3、V2O5、Li2CO3烘干，然后按照化学计量比称量，随后，以无水乙醇为介质通过行星式球磨机球磨10–12h，然后90℃条件下烘干。干燥的混合物在650℃保温4h煅烧，煅烧后的粉体再次球磨10–12h并烘干，以获得CBMVO-LMO粉体。
(2)将得到的CBMVO-LMO陶瓷粉体和PTFE粉体按化学计量比称量，以无水乙醇为介质通过行星球磨机球磨10–12h，然后80℃条件下烘干。
(3)称取适量粉体放入玛瑙研钵中，加入7wt.％的去离子水，研磨5min，将研磨粉体过80目筛，放入热压模具(直径11mm)在150℃的温度和300MPa的压力下成型，保温1h，然后将其在120℃下烘干12h，即得目标复相材料。
制备得到的复相材料经过砂纸打磨到厚度为5-6mm，对样品进行微波介电性能的测试。其中，最佳样品组成为：CBMVO-5wt.％LMO-3wt.％PTFE，其性能可达到：介电常数(εr)9.8，品质因数(Q×f)5120GHz，谐振频率温度系数(τf)-1.0ppm/℃，是潜在的应用于微波介质基板和高端微波元件的复相材料。
本发明易溶于水的Li2MoO4作为助烧剂，有机物PTFE作为正温度系数调节剂被引入(Ca0.65Bi0.35)(Mo0.65V0.35)O4体系，通过冷烧结方法在150℃和300MPa下，制备得到了一种复相微波介质陶瓷。该复相微波介质陶瓷具有低的介电常数和近零的谐振频率温度系数，在微波介质基板、谐振器等微波电子元器件中有广泛的应用前景。
附图说明
图1为CBMVO-LMO-PTFE复相陶瓷XRD图谱；
图2为CBMVO-LMO-PTFE复相陶瓷的微波介电性能。
具体实施方式
下面通过实施例进一步阐明本发明的实质性特点和显著优点。应该指出，本发明决非仅局限于所陈述的实施例。
实施例1：
(1)按化学式(Ca0.65Bi0.35)(Mo0.65V0.35)O4-5wt.％Li2MoO4-0.5wt.％PTFE称量CBMVO-LMO和PTFE，以无水乙醇为介质通过行星球磨机球磨10–12h，然后80℃条件下烘干。称取适量混合粉体放入玛瑙研钵中，加入7wt.％的去离子水，研磨5min，将研磨粉体过80目筛，放入热压模具(直径11mm)在150℃的温度和300MPa的压力下成型，保温1h，然后将其在120℃下烘干12h,即得目标复合材料。
实施例2：
按化学式(Ca0.65Bi0.35)(Mo0.65V0.35)O4-5wt.％Li2MoO4-1wt.％PTFE称量CBMVO-LMO和PTFE，其它同实施例1。
实施例3：
按化学式(Ca0.65Bi0.35)(Mo0.65V0.35)O4-5wt.％Li2MoO4-2wt.％PTFE称量CBMVO-LMO和PTFE，其它同实施例1。
实施例4：
按化学式(Ca0.65Bi0.35)(Mo0.65V0.35)O4-5wt.％Li2MoO4-3wt.％PTFE称量CBMVO-LMO和PTFE，其它同实施例1。
实施例5：
按化学式(Ca0.65Bi0.35)(Mo0.65V0.35)O4-5wt.％Li2MoO4-5wt.％PTFE称量CBMVO-LMO和PTFE，其它同实施例1。
实施例6：
按化学式(Ca0.65Bi0.35)(Mo0.65V0.35)O4-5wt.％Li2MoO4-10wt.％PTFE称量CBMVO-LMO和PTFE，其它同实施例1。
表1上述实施例性能对比表
Figure BDA0003241854160000041
Figure BDA0003241854160000051

Claims (5)

1.一种复相微波介质陶瓷材料，其特征在于，该复合材料的化学组成为：(Ca0.65Bi0.35)(Mo0.65V0.35)O4-5wt.％Li2MoO4-xwt.％PTFE，其中0.5≤x≤20，进一步优选x的数值为3。
2.按照权利要求1所述的一种复相微波介质陶瓷材料，其特征在于，复相材料的谐振频率温度系数由负到正，根据需要具有可调节性。
3.按照权利要求1所述的一种复相微波介质陶瓷材料，其特征在于，x＝3时的化学组成为：(Ca0.65Bi0.35)(Mo0.65V0.35)O4-5wt.％Li2MoO4-3wt.％PTFE，其性能可达到：介电常数9.8，品质因数5120GHz，谐振频率温度系数-1.0ppm/℃。
4.制备权利要求1-3所述的一种复相微波介质陶瓷材料的方法，其特征在于，首先通过固相反应制备(Ca0.65Bi0.35)(Mo0.65V0.35)O4-5wt.％Li2MoO4陶瓷粉体，引入PTFE至上述合成的粉体中，通过冷烧结方法制备，具体包括以下步骤：
(1)将原料CaCO3、MoO3、Bi2O3、V2O5、Li2CO3烘干，然后按照化学计量比称量，随后，以无水乙醇为介质通过行星式球磨机球磨10-12h，然后90℃条件下烘干；干燥的混合物在650℃保温4h煅烧，煅烧后的粉体再次球磨10–12h并烘干，以获得(Ca0.65Bi0.35)(Mo0.65V0.35)O4-5wt.％Li2MoO4粉体；
(2)将得到的(Ca0.65Bi0.35)(Mo0.65V0.35)O4-5wt.％Li2MoO4陶瓷粉体和PTFE粉体按化学计量比称量，以无水乙醇为介质通过行星球磨机球磨10–12h，然后80℃条件下烘干；
(3)称取适量粉体放入玛瑙研钵中，加入7wt.％的去离子水，研磨5min，将研磨粉体过80目筛后放入热压模具，在150℃的温度和300MPa的压力下成型，保温1h，然后将其在120℃下烘干12h，即得目标复合材料。
5.权利要求1-3任一项所述的一种复相微波介质陶瓷材料的应用，用于微波介质基板或微波电子元件。
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CN115196945A (zh) * 2022-08-12 2022-10-18 佛山科学技术学院 一种基于冷烧结辅助低温致密化制备微波陶瓷块体的方法
CN115872740A (zh) * 2022-12-28 2023-03-31 北京工业大学 一种超低温烧结的低介微波介质陶瓷及其制备方法

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