CN105565808A - 一种低温共烧微波介质陶瓷材料及其制备方法 - Google Patents

一种低温共烧微波介质陶瓷材料及其制备方法 Download PDF

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CN105565808A
CN105565808A CN201510985097.0A CN201510985097A CN105565808A CN 105565808 A CN105565808 A CN 105565808A CN 201510985097 A CN201510985097 A CN 201510985097A CN 105565808 A CN105565808 A CN 105565808A
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陈鲁国
康建宏
李广新
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Dongguan Chuangxin Electronic Technology Co., Ltd.
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Abstract

本发明公开了一种非常适合LTCC工艺生产的低温共烧微波介质陶瓷材料及其制备工艺。所述低温共烧陶瓷材料由87～97wt%的Ba4(Nd1.0-XBix)9.33(Ti0.9Zr0.1)18O54、0～6wt%的粉末a和3～7wt%的粉末b组成，所述粉末a为预烧体，其组分为摩尔百分比1:1的Nd2O3与Al2O3，化学通式为NdAlO3；所述粉末b为预烧体，其组分为摩尔比为1∶？1：1的BaO、CuO与B2O3，其化学通式为BaCu（B2O5）。本发明的微波介质材料，不用熔制玻璃、制造成本低，烧结温度低于950℃，且能够与银匹配共烧，其相对介电常数55～70，Qf值3000～5000GHz，谐振频率温度系数可调。

Description

一种低温共烧微波介质陶瓷材料及其制备方法
技术领域
本发明涉及电子陶瓷材料领域，特别是涉及一种低温共烧微波介质陶瓷材料及其制备方法。
背景技术
随着移动通讯的迅猛发展，移动通信终端正向着小型化、轻量化、集成化方向发展，对以微波介质陶瓷为基础的微波电路元器件提出减小尺寸的要求，实现这一要求，有以下两种途径：一是寻找高介电常数的微波介质材料；二是借助于LTCC低温共烧技术。
低温共烧陶瓷技术(LowTemperatureCo-firedCeramic，LTCC)是近年来兴起的一种新型多学科交叉的整合组件技术，它在推动微波器件体积小型化和提高微波电路组装密度中都起到了巨大作用，成为电子器件模块化的关键技术之一。为了能与银(熔点为961℃)等高电导率的金属电极在空气中共烧，微波介质陶瓷的烧结温度要降到950℃以下。
BaO-Ln2O3-TiO2类陶瓷有较高的介电常数和Qf值，并可在较大范围内通过调整配方，得到不同特性的微波介电性能，但由于其烧结温度过高(>1200℃)，大大限制了其在LTCC领域的应用。为了实现与导体浆料的匹配共烧，大多采用掺入低熔点玻璃以降低陶瓷的烧结温度，但这种“陶瓷+玻璃”体系还存在很大的不足：①生产成本高，由于需要高温熔制玻璃，热处理时间长，耗能大，高温挥发易造成配方改变；②对设备要求高，玻璃熔融后，淬火对设备损耗大；③淬火后的玻璃渣硬度高，难以磨细。④玻璃相的存在，使得材料的损耗大幅增加。因此，如何在保证BaO-Ln2O3-TiO2类陶瓷优异的微波介电性能基础上，降低材料的烧结温度，实现与银电极的匹配共烧，成为该领域的一大难题。
发明内容
本发明的目的在于克服现有技术的不足，提供一种不用熔制玻璃、收缩一致性好、介电性能优良，非常适合LTCC流延工艺生产的低温共烧陶瓷材料及其原料与制备工艺。
本发明提供一种低温共烧微波介质陶瓷材料，由87～97wt%的微波介质陶瓷、0～6wt%的粉末a和3～7wt%的粉末b混合制成，所述粉末a为预烧体，其组分为摩尔百分比1:1的Nd2O3与Al2O3，化学通式为NdAlO3；所述粉末b为预烧体，其组分为摩尔比为1∶1：1的BaO、CuO与B2O3，化学通式为BaCu（B2O5）。
所述微波介质陶瓷，化学通式Ba4(Nd1.0-xBix)9.33(Ti0.9Zr0.1)18O54，在BaO-Ln2O3-TiO2系陶瓷中掺入Bi2O3取代Nd2O3，可以降低材料的烧结温度，并提高材料的介电常数，但随着Bi取代量的增加，品质因数呈直线下降的趋势。因此，需将Bi2O3取代量控制在一定的范围内，0.05≤x≤0.35，优选0.10≤x≤0.25。
本发明还提供了上述微波介质陶瓷材料的制备方法，包括以下步骤：
S1：将原材料BaCO3、Nd2O3、Bi2O3、ZrO2、TiO2粉体按化学通式Ba4(Nd1.0-XBix)9.33(Ti0.9Zr0.1)18O54配料,以无水乙醇为介质，行星球磨3～6小时，取出后烘干，过40目筛，然后在1100～1200℃大气气氛中预烧2～4小时，制成BNBTZ基料；
S2、将原材料Nd2O3与Al2O3按摩尔比1：1配料，以无水乙醇为介质，行星球磨3～6小时，取出后烘干，过40目筛，然后在1100～1200℃大气气氛中预烧2～4小时，制成粉末a预烧块；
S3、将原料BaO、CuO与B2O3按摩尔比为1：1：1配料，以无水乙醇为介质，行星球磨3～6小时，取出后烘干，过40目筛，然后在700～750℃大气气氛中预烧2～4小时，制成粉末b预烧块；
S4、在BNBTZ基料中加入占总质量百分比0～6wt%的粉末a和3～7wt%的粉末b，以无水乙醇为介质，行星球磨6～12小时，取出后烘干，过40目筛，加入PVA溶液造粒，压制成型，然后置于900～950℃的温度下烧结4～6小时，制成所述低温共烧陶瓷材料。
本发明中采用固相法，通过在Ba6-xLn8+2XTi18O54(x=2/3)陶瓷中掺杂ZrO2，大幅度提高材料的Qf值；同时引入负温度系数的NdAlO3，可得到趋于零的谐振频率温度系数；BaCu（B2O5）相的熔点大约为800℃，Qf值很高，因此，用它来做烧结助剂，可起到降低烧结温度，获得良好介电性能的作用。
本发明的有益效果是：区别于现有技术中Ba6-3xNd8+2xTi18O54陶瓷多采用熔制玻璃来降低烧结温度，致使Qf值偏低的缺点，本发明的微波介质陶瓷材料，烧结温度低于950℃，且能够与银匹配共烧，其相对介电常数50～65、Qf值3000～5000GHz、谐振频率温度系数可调。
具体实施方式
下面结合实施例，更具体地阐述本发明的内容。应当理解，本发明的实施并不局限于下面的实施例，对本发明所做的任何形式的变通或改变均在本发明保护范围。
实施例1～4
按化学通式Ba4(Nd1.0-XBix)9.33(Ti0.9Zr0.1)18O54称取BaCO3、Nd2O3、Bi2O3、ZrO2、TiO2原料,其中x按照表1取值，以无水乙醇为介质，行星球磨3小时，取出后烘干，在1100℃大气气氛中预烧2小时，制成BNBTZ基料；将原料BaO、CuO与B2O3按摩尔比为1：1：1配料，以无水乙醇为介质，行星球磨3小时，取出后烘干，在700℃大气气氛中预烧3小时，制成粉末b预烧块备用；在BNBTZ基料中加入占总质量百分比5wt%的粉末b，以无水乙醇为介质，行星球磨12小时，取出后烘干，加入PVA溶液造粒，压制成型，然后置于930℃的温度下烧结4小时，采用网络分析仪测量其介电性能指标，测试结果见表1。
表1
实施例5～9
按化学通式Ba4(Nd0.8Bi0.2)9.33(Ti0.9Zr0.1)18O54称取BaCO3、Nd2O3、Bi2O3、ZrO2、TiO2原料,以无水乙醇为介质，行星球磨3小时，取出后烘干，在1100℃大气气氛中预烧2小时，制成BNBTZ基料；将原材料Nd2O3与Al2O3按摩尔比1：1配料，以无水乙醇为介质，行星球磨3小时，取出后烘干，在1200℃大气气氛中预烧3小时，制成粉末a预烧块备用；将原料BaO、CuO与B2O3按摩尔比为1：1：1配料，以无水乙醇为介质，行星球磨3小时，取出后烘干，在700℃大气气氛中预烧3小时，制成粉末b预烧块备用；在BNBTZ基料中加入占总质量不同百分比的粉末a和粉末b，具体添加比例见表2，无水乙醇为介质，行星球磨12小时，取出后烘干，加入PVA溶液造粒，压制成型，然后置于900℃～950℃的温度下烧结4小时，采用网络分析仪测量其介电性能指标，测试结果见表2。
表2

Claims (5)

1.一种低温共烧微波介质陶瓷材料，由87wt%～97wt%的微波介质陶瓷、0～6wt%的粉末a和3～7wt%的粉末b混合制成，其特征在于，所述微波介质陶瓷由BaCO3、Nd2O3、Bi2O3、ZrO2与TiO2组成，所述粉末a为预烧体，由Nd2O3与Al2O3的混合粉末煅烧而成；所述粉末b为预烧体，由BaO、CuO、B2O3的混合粉末煅烧而成。
2.根据权利要求1所述的低温烧结微波介质陶瓷材料，其特征在于，所述BaCO3、Nd2O3、Bi2O3、ZrO2与TiO2的摩尔百分比按照化学通式Ba4(Nd1.0-XBix)9.33(Ti0.9Zr0.1)18O54确定，其中0.05≤x≤0.35。
3.根据权利要求1所述的低温共烧微波介质陶瓷材料，其特征在于，所述粉末a，Nd2O3与Al2O3的摩尔比为1∶1。
4.根据权利要求1所述的低温共烧微波介质陶瓷材料，其特征在于，所述粉末b，BaO、CuO与B2O3的摩尔比为1∶1：1。
5.一种制备低温共烧微波介质陶瓷材料的方法，其特征在于，按照以下步骤进行：S1：将原材料BaCO3、Nd2O3、Bi2O3、ZrO2、TiO2粉体按化学通式Ba4(Nd1.0-XBix)9.33(Ti0.9Zr0.1)18O54配料,以无水乙醇为介质，行星球磨3～6小时，取出后烘干，过40目筛，然后在1100℃～1200℃大气气氛中预烧2～4小时，制成BNBTZ基料；S2、将原材料Nd2O3与Al2O3按摩尔比1：1配料，以无水乙醇为介质，行星球磨3～6小时，取出后烘干，过40目筛，然后在1100℃～1200℃大气气氛中预烧2～4小时，制成粉末a预烧块；S3、将原料BaO、CuO与B2O3按摩尔比为1：1：1配料，以无水乙醇为介质，行星球磨3～6小时，取出后烘干，过40目筛，然后在700℃～750℃大气气氛中预烧2～4小时，制成粉末b预烧块；S4、在BNBTZ基料中加入占总质量百分比0～6wt%的粉末a和3～7wt%的粉末b，以无水乙醇为介质，行星球磨6～12小时，取出后烘干，过40目筛，加入PVA溶液造粒，压制成型，然后置于900～950℃下烧结4～6小时，制成所述低温共烧微波介质材料。
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