CN113788676A - 一种低温共烧改性NiTa2O6基微波介质陶瓷材料及其制备方法 - Google Patents
一种低温共烧改性NiTa2O6基微波介质陶瓷材料及其制备方法 Download PDFInfo
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Abstract
本发明属于电子陶瓷及其制造领域，涉及一种低温共烧改性NiTa2O6基微波介质陶瓷材料及其制备方法。本发明基于CuO与B2O3的低熔点特性，且Cu2+离子半径与Ni2+以及Ta5+离子相近，将本发明的化学通式设计为：xCuO‑(1‑x)NiO‑[7.42y+(xy/14.33)]B2O3‑Ta2O5，通过从原料调节各组分的摩尔含量，实现了在较低预烧温度下合成NiTa2O6主晶相的目的，从而直接一次合成了具有低温烧结特性且微波介电性能优异的NiTa2O6基陶瓷材料，拓宽了在LTCC领域中的应用范围。
Description
技术领域
本发明属于电子陶瓷及其制造领域，涉及一种低温共烧改性NiTa2O6基微波介质陶瓷材料及其制备方法。
背景技术
第五代移动通讯技术简称5G，随着5G技术的发展对应用于高频条件下，如毫米波段的电子元器件需求日益增加，如电子电路基板、介质天线与波导等。作为一种新型的三维集成封装互联技术，低温共烧陶瓷(LTCC)技术以其优异的电学、机械、热学及工艺特性，为制备内嵌电极的陶瓷模块或者整体电路提供了可靠的解决方案，因此开发应用于LTCC技术的陶瓷体系是当前研究的热点。
通常情况下陶瓷材料需在较高的烧结温度(>1000℃)条件下才能实现致密化以及良好的微波介电性能，但由于目前电子器件主要采用的电极材料如Ag、Au、Cu等的熔点一般低于1000℃，使其无法与LTCC技术中的Ag或Cu电极共烧(与Ag电极共烧需不超过950℃；与Cu电极共烧需不超过1000℃且在还原气氛下进行)。例如四方Tri-rutile结构NiTa2O6陶瓷在1400～1600℃烧结温度下经报道具有优异的微波介电性能：εr＝25～27，Q×f＝31200GHz，τf＝26～35ppm/℃。但该体系的烧结温度过高，限制了在LTCC领域中的进一步应用，目前亦未发现有降低该类陶瓷烧结温度的研究。因此，如何降低NiTa2O6陶瓷的烧结温度的同时使其继续保持低损耗的特性成为该领域研究的难点。
发明内容
针对上述存在的问题或不足，为解决现有NiTa2O6陶瓷因烧结温度过高限制其在LTCC领域中的进一步应用的问题，本发明提供了一种低温共烧改性NiTa2O6基微波介质陶瓷材料及其制备方法，在保持低介质损耗的同时有效降低了烧结温度，使其能够广泛应用于LTCC技术领域。
本发明采取的技术方案为：
一种低温共烧改性NiTa2O6基微波介质陶瓷材料，其化学通式为：
xCuO-(1-x)NiO-[7.42y+(xy/14.33)]B2O3-Ta2O5，其中0.02≤x≤0.2；0.02≤y≤0.08；经由固相法制备获得；物相组成为NiTa2O6结构；
该陶瓷材料的烧结温度为900～975℃，在大气气氛下采用850～900℃预烧温度；介电常数为16～23，品质因数Q×f值为12000～19000GHz，频率温度系数为20～27ppm/℃。
作为优选，当x＝0.1且y＝0.04时，在950℃烧结温度下材料的介电常数为22.4，品质因数Q×f值为18531GHz，频率温度系数为25.2ppm/℃，能够广泛应用于LTCC技术领域。
上述低温共烧改性NiTa2O6基微波介质陶瓷材料的制备方法，包括以下步骤：
步骤1：将CuO、NiO、B2O3和Ta2O5的原始粉料按照化学通式xCuO-(1-x)NiO-[7.42y+(xy/14.33)]B2O3-Ta2O5进行配料；其中0.02≤x≤0.2；0.02≤y≤0.08；
步骤2：将步骤1配好的粉体装入球磨罐，以氧化锆球和去离子水，按照粉料：氧化锆球：去离子水质的量比为1:4～6:3～5进行球磨，行星球磨6～8小时，取出后在80～120℃烘箱中烘干，以60～80目筛网过筛，后在850～900℃大气气氛中预烧3～5小时；
步骤3：将步骤2预烧后的粉体，再次按照粉体：锆球：去离子水质量比为1:4～6:1～3进行球磨，行星球磨混合3～6小时，取出烘干后，向得到的粉体中添加聚乙烯醇溶液进行造粒；
步骤4：将步骤3制得陶瓷生料压制成型，在600～650℃排胶后在900～975℃大气气氛中烧结4～6小时后，即可制得低温烧结的改性NiTa2O6微波介质陶瓷材料。
本发明基于CuO与B2O3的低熔点特性，且Cu2+离子半径与Ni2+以及Ta5+离子相近，将化学通式设计为：xCuO-(1-x)NiO-[7.42y+(xy/14.33)]B2O3-Ta2O5，通过从原料调节各组分的摩尔含量，实现了在较低预烧温度下合成NiTa2O6主晶相的目的，从而直接一次合成了具有低温烧结特性且微波介电性能优异的NiTa2O6基陶瓷材料，拓宽了在LTCC领域中的应用范围。
附图说明
图1对应实施例样3的XRD衍射图谱；
图2对应实施例样3的SEM形貌图。
具体实施方式
下面结合附图和实施例对本发明做进一步的详细说明。
步骤1、将CuO、NiO、B2O3和Ta2O5的原始粉料按照化学通式xCuO-(1-x)NiO-[7.42y+(xy/14.33)]B2O3-Ta2O5(x＝0.1；y＝0.04)，采用摩尔比进行配料；
步骤2、将步骤1所得配料装入球磨罐，以锆球及去离子水作为研磨介质，按照配料：锆球：去离子水质量比1:6:4行星球磨6小时，然后在100℃烘干，以60目筛网过筛，最后在900℃大气气氛中预烧3小时；
步骤3、将预烧后的粉料、放入球磨罐中进行二次球磨，以粉体：锆球：去离子水质量比1:6:3，行星球磨4小时，再取出烘干后，向得到的粉料加入质量百分比为5％～8％的聚乙烯醇溶液进行造粒；
步骤4、将造粒好的粉体放入φ12的模具中在20MPa压力下干压成型(尺寸：12mm×6mm的圆柱块体)，然后将圆柱块体在650℃下保温2小时以除去粘结剂，然后升至900℃～975℃下保温4小时，最终制得低温烧结条件下的改性NiTa2O6基微波介质陶瓷材料，其化学式为：CuO-NiO-B2O3-Ta2O5(4.4:39.2:12.9:43.5mol％)。
按照上述步骤制作了4份实施例样品。图1为实施例样3的XRD衍射图谱，通过与标准卡片比对发现与NiTa2O6的标准卡片JCPDS card No.32-0702具有良好匹配性，X射线衍射峰的偏移说明了各离子固溶至阳离子格位，且体系中并未检测到第二相的存在，说明该类型陶瓷属于NiTa2O6结构的固溶体。
图2为实施例样3的SEM形貌图，样品的晶粒生长充分，晶界清晰可见，说明其低温烧结特性良好。
各实施例样的具体实施例的成分和微波介电性能如下：
表1为各实施例样的成分
表2为各实施例样的微波介电性能
从上述表格中可以看出，当x＝0.1，y＝0.4且烧结温度介于900～950℃范围内，改性NiTa2O6陶瓷材料的介电常数与品质因素Q×f值呈现出先增加后降低的趋势，并在烧结温度为950℃时取得最佳值：εr＝22.4，tanδ＝5.0×10-4，Q×f＝18531GHz，τf＝25.2ppm/℃，与现有文献报道相比烧结温度得到大幅降低，且此时微波介电性能仍相对较优异，能够广泛应用于LTCC技术领域。
Claims (3)
1.一种低温共烧改性NiTa2O6基微波介质陶瓷材料，其特征在于：所述低温共烧改性NiTa2O6基微波介质陶瓷材料的化学通式为：
xCuO-(1-x)NiO-[7.42y+(xy/14.33)]B2O3-Ta2O5，其中0.02≤x≤0.2；0.02≤y≤0.08；经由固相法制备获得；物相组成为NiTa2O6结构；
该陶瓷材料的烧结温度为900～975℃，在大气气氛下采用850～900℃预烧温度；介电常数为16～23，品质因数Q×f值为12000～19000GHz，频率温度系数为20～27ppm/℃。
2.根据权利要求1所述的一种低温共烧改性NiTa2O6基微波介质陶瓷材料，其特征在于：当x＝0.1且y＝0.04时，在950℃烧结温度下材料的介电常数为22.4，品质因数Q×f值为18531GHz，频率温度系数为25.2ppm/℃。
3.一种低温共烧改性NiTa2O6基微波介质陶瓷材料的制备方法，其特征在于：包括以下步骤：
步骤1：将CuO、NiO、B2O3和Ta2O5的原始粉料按照化学通式xCuO-(1-x)NiO-[7.42y+(xy/14.33)]B2O3-Ta2O5进行配料；其中0.02≤x≤0.2；0.02≤y≤0.08；
步骤2：将步骤1配好的粉体装入球磨罐，以氧化锆球和去离子水，按照粉料：氧化锆球：去离子水质的量比为1:4～6:3～5进行球磨，行星球磨6～8小时，取出后在80～120℃烘箱中烘干，以60～80目筛网过筛，后在850～900℃大气气氛中预烧3～5小时；
步骤3：将步骤2预烧后的粉体，再次按照粉体：锆球：去离子水质量比为1:4～6:1～3进行球磨，行星球磨混合3～6小时，取出烘干后，向得到的粉体中添加聚乙烯醇溶液进行造粒；
步骤4：将步骤3制得陶瓷生料压制成型，在600～650℃排胶后在900～975℃大气气氛中烧结4～6小时后，即可制得低温烧结的改性NiTa2O6微波介质陶瓷材料。
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