CN112194466A - 一种低介低损Ca-Al-B基微波介质陶瓷材料 - Google Patents

一种低介低损Ca-Al-B基微波介质陶瓷材料 Download PDF

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CN112194466A
CN112194466A CN202011072559.7A CN202011072559A CN112194466A CN 112194466 A CN112194466 A CN 112194466A CN 202011072559 A CN202011072559 A CN 202011072559A CN 112194466 A CN112194466 A CN 112194466A
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李恩竹
温擎宇
杨鸿程
孙成礼
钟朝位
张树人
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Abstract

本发明属于电子陶瓷及其制造领域，涉及一种低介低损Ca‑Al‑B基微波介质陶瓷材料及其制备方法。本发明首次将CaO‑Al2O3‑B2O3三元体系的典型代表CaAl2B2O7作为低介低损Ca‑Al‑B基微波介质陶瓷材料应用，提供的低介低损Ca‑Al‑B基微波介质陶瓷材料，其原料组成为CaCO3、Al2O3和H3BO3，化学通式为CaAl2xB2O7(x＝0.25～1)，主晶相为CaAl2B2O7，利用固相烧结法制备，其预烧温度为750℃～900℃，烧结温度为930℃～1040℃，具有低介电常数(4～6)，损耗低至2.14×10‑4，频率温度系数‑20～‑30ppm/℃。本发明为低介低损介质陶瓷材料提供了一种新的选择。

Description

一种低介低损Ca-Al-B基微波介质陶瓷材料
技术领域
本发明属于电子陶瓷及其制造领域，涉及一种低介电常数、低介电损耗Ca-Al-B基微波介质陶瓷材料及其制备方法。
背景技术
5G是实现万物互联的基础，与4G相比5G的通信频率进入通信频率更高的微波频段，拥有极低的网络时延，更快的传输速率和更大的容量。在5G通信中需要能够实现高度集成化、低损耗和低延时的新型材料，因此，开发出能够满足5G高频高速传输要求的具有低介电常数低介电损耗的微波介质陶瓷具有重要的工业应用价值。
低介电常数基板材料一般有低熔点玻璃+陶瓷系、微晶玻璃系、聚合物陶瓷和单相陶瓷。低熔点玻璃+陶瓷系、微晶玻璃系和聚合物陶瓷能够实现很低的介电常数，但介电损耗较大，目前传输损耗最小的电路板就是陶瓷电路板，陶瓷基板拥有相比其他有机材料基板更高的导热度，和硅芯片的热膨胀系数也更为匹配，可以有效解决导热问题，在温度过高或是温差过大时，也不容易导致脱焊等问题。
目前，众多研究人员倾力探寻新型的微波介质陶瓷材料设计新型电子器件以促进通信技术行业的发展，在相对介电常数为3.8～1100的范围内已有许多商用多功能器件。对于相对介电常数临近5的材料体系，报道称可作为LTCC基板候选材料的有Li2WO4和Li2MoO4以及CaO-B2O3-SiO2玻璃陶瓷体系。迄今为止，低介硼酸盐的陶瓷体系的研究主要集中于研究ZnO-B2O3体系，因此面对当前5G时代的到来，现有的低介低损介质陶瓷材料在参数性能以及可选择面上或有不足。
发明内容
针对上述存在问题或不足，为解决现有低介低损介质陶瓷材料在参数性能以及可选择面上的不足问题，本发明了提供了一种低介低损Ca-Al-B基微波介质陶瓷材料，其预烧温度为750℃～900℃，烧结温度为930℃～1040℃，具有低介电常数(4～6)，损耗低至2.14×10-4，频率温度系数-20～-30ppm/℃。
具体技术方案如下：
一种低介低损Ca-Al-B基微波介质陶瓷材料，其原料组成为CaCO3、Al2O3和H3BO3，化学通式为CaAl2xB2O7，x＝0.25～1，主晶相为CaAl2B2O7，通过固相法制备。
上述低介低损Ca-Al-B基微波介质陶瓷材料的制备方法如下：
步骤1：将原料CaCO3、Al2O3和H3BO3按照化学式CaAl2xB2O7(x＝0.25～1)化学计量比进行配料；
步骤2：将步骤1所配的粉体与锆球、去离子水以1:5:1.5～2.5混合于球磨罐中进行球磨，行星球磨4～6小时，球磨后充分混合的粉体在烘箱中以80℃～110℃烘干，再用40～60目筛网过筛后在大气气氛中以750℃～900℃预烧2～4小时；
步骤3：将步骤2预烧后的粉体，再次以粉体：锆球：去离子水质量比为1:5:1～1:5:2进行球磨，行星球磨3～6小时，取出混合均匀的浆体在80℃～100℃的烘箱中烘干后，向得到的粉体中添加粘结剂造粒(如粘结剂：5％～10％质量比浓度50％的丙烯酸水溶液)；
步骤4：将步骤3制得粉体压制成型，在400℃～500℃排胶后于930℃～1040℃大气气氛中烧结2～4小时，即可制成低介低损Ca-Al-B基微波介质陶瓷材料。
综上所述，本发明首次将CaO-Al2O3-B2O3三元体系的典型代表CaAl2B2O7作为低介低损Ca-Al-B基微波介质陶瓷材料应用，提供的低介低损Ca-Al-B基微波介质陶瓷材料，其原料组成为CaCO3、Al2O3和H3BO3，化学通式为CaAl2xB2O7(x＝0.25～1)，主晶相为CaAl2B2O7，利用固相烧结法制备，其预烧温度为750℃～900℃，烧结温度为930℃-1040℃，具有低介电常数(4～6)，损耗低至2.14×10-4，频率温度系数-20～-30ppm/℃。CaAl2B2O7作为CaO-Al2O3-B2O3三元体系三元体系的典型代表，其研究仅限于发光性能以及晶体结构分析，在固相烧结中，其反应过程、物相组成以及微波介电性能与各个物相含量之间的关系均未具体研究。本发明为低介低损介质陶瓷材料提供了一种新的选择。
附图说明
图1对应实施例2、7、12、14号的XRD衍射图谱。
图2为图1在衍射角10°-50°范围内的局部放大。
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。
本发明按照化学式CaAl2xB2O7(x＝0.25～1)化学计量比进行配料，原料为CaCO3、Al2O3和H3BO3。由固相反应制备成本发明材料，具体制备步骤同上述步骤一致。
具体实施例的成分和微波介电性能如下
Figure BDA0002715604680000021
Figure BDA0002715604680000031
Figure BDA0002715604680000032
Figure BDA0002715604680000033
Figure BDA0002715604680000034
Figure BDA0002715604680000041
上表格数据囊括了在化学通式范围内的实施例配料结果及烧熟样品性能，从表中可以看出，Ca-Al-B基微波陶瓷材料介电性能优异，具有低介电常数，低介电损耗；随着Al非化学计量比减少，最佳烧结温度降低，当烧结温度能够在低于银电极熔点(961℃)的温度下烧结成瓷时，还可以应用于LTCC领域。
图1展示了本发明实施例陶瓷材料在最佳烧结温度下保温4小时后的XRD衍射图谱，分别对应实施例样品2、7、12和14号，图2为图1在衍射角10°-50°范围内的局部放大。从图1可以看出，主晶相为CaAl2B2O7(ICSD 01-089-5563)，从图2可以看出随着Al非化学计量比的减少，次相CaB2O4(ICSD 00-032-0155)衍射峰强度逐渐增强，Al2O3和Ca2B2O5杂相消失。

Claims (3)

1.一种低介低损Ca-Al-B基微波介质陶瓷材料，其特征在于：
原料组成为CaCO3、Al2O3和H3BO3，化学通式为CaAl2xB2O7，x＝0.25～1，主晶相为CaAl2B2O7，通过固相法制备；其预烧温度为750℃～900℃，烧结温度为930℃～1040℃，介电常数4-6，损耗低至2.14×10-4，频率温度系数-20～-30ppm/℃。
2.如权利要求1所述低介低损Ca-Al-B基微波介质陶瓷材料，其制备方法如下：
步骤1：将原料CaCO3、Al2O3和H3BO3按照化学式CaAl2xB2O7，x＝0.25～1，化学计量比进行配料；
步骤2：将步骤1所配的粉体与锆球、去离子水以1:5:1.5～2.5混合于球磨罐中进行球磨，行星球磨4～6小时，球磨后充分混合的粉体在烘箱中以80℃～110℃烘干，再用40～60目筛网过筛后在大气气氛中以750℃～900℃预烧2～4小时；
步骤3：将步骤2预烧后的粉体，再次以粉体：锆球：去离子水质量比为1:5:1～1:5:2进行球磨，行星球磨3～6小时，取出混合均匀的浆体在80℃～100℃的烘箱中烘干后，向得到的粉体中加入丙烯酸水溶液作为粘结剂造粒；
步骤4：将步骤3制得粉体压制成型，在400℃～500℃排胶后于930℃～1040℃大气气氛中烧结2～4小时，即可制成低介低损Ca-Al-B基微波介质陶瓷材料。
3.如权利要求2所述低介低损Ca-Al-B基微波介质陶瓷材料的制备方法如下，其特征在于：所述步骤4中粘结剂为5％～10％质量比浓度50％的丙烯酸水溶液。
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JPH04275944A (ja) * 1991-02-26 1992-10-01 Nippon Electric Glass Co Ltd 封着材料
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JPH04275944A (ja) * 1991-02-26 1992-10-01 Nippon Electric Glass Co Ltd 封着材料
CN101230485A (zh) * 2007-01-26 2008-07-30 中国科学院理化技术研究所 一种去除紫外吸收的含铝光学晶体的生长方法
CN104402438A (zh) * 2014-11-21 2015-03-11 桂林理工大学 温度稳定型超低介电常数微波介电陶瓷Ca2LaBO5

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