CN112194468B - 一种低介低损Ca-Al-B基LTCC材料及其制备方法 - Google Patents

一种低介低损Ca-Al-B基LTCC材料及其制备方法 Download PDF

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CN112194468B
CN112194468B CN202011075136.0A CN202011075136A CN112194468B CN 112194468 B CN112194468 B CN 112194468B CN 202011075136 A CN202011075136 A CN 202011075136A CN 112194468 B CN112194468 B CN 112194468B
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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，涉及一种低介电常数、低介电损耗Ca‑Al‑B基微波介质LTCC材料及其制备方法。本发明将CaO‑Al2O3‑B2O3三元体系的典型代表CaAl2B2O7作为Ca‑Al‑B基微波介质陶瓷材料通过添加助剂使其可应用于LTCC领域，实现了850℃～900℃的低温致密烧结，介电常数5～6.2，损耗低至4.19×10‑4，频率温度系数‑30～‑20ppm/℃。CaAl2B2O7作为CaO‑Al2O3‑B2O3三元体系的典型代表，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LTCC材料提供了一种具有优异性能LTCC材料的新选择。

Description

一种低介低损Ca-Al-B基LTCC材料及其制备方法
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LTCC材料及其制备方法。
背景技术
随着5G通信技术、物联网和全球卫星通信系统的迅猛发展，人类进入了信息时代，通讯信息容量迅猛增加，无线通讯逐步趋向更高的微波频段，通信技术需要满足新兴行业超大数据吞吐量、高速传输能力等通讯需求，特别是由手持移动通讯系统从人工、自动阶段步入了蜂窝程序控制阶段，要求整个通讯系统高性能化、小型化。微波通信系统己成为当前通信技术发展的必然趋势，因此研发出能够应用于5G发展具有低温烧结、低介电常数、低介电损耗的微波介质陶瓷是支撑此项技术发展必不可少的基础材料。
同时，LTCC(低温共烧陶瓷)为便携式电子设备，提供了轻、高速，高集成度的电子元件和基片，成为了电子元器件制造工艺的主流趋势。LTCC的布线采用Cu、Ag、Au等金属，导体损耗小，高频电阻低。LTCC材料在800℃℃～900℃下烧结，形成高密度基板，且陶瓷的介电损耗比有机材料低。这使得LTCC特别适合高速数据通信所需的高频电路。LTCC材料在高频特性、热稳定性、无源器件集成能力等方面都具有优势，很适合集成基片和电子元件的高频应用。因此寻求具有低温烧结的低介电常数、低介电损耗材料是科研人员将微波介质陶瓷用于5G技术中不断探索的目标。
目前对于LTCC基板材料主要有微晶玻璃陶瓷材料、Al2O3系基板材料中加入低熔点玻璃等玻璃陶瓷和聚合物陶瓷，但是一般介电损耗较大。因此面对当前5G时代的到来，现有的低介低损LTCC材料在参数性能以及可选择面上或有不足。
发明内容
针对上述存在的问题和不足，为解决现有低介低损LTCC材料在参数性能以及可选择面上的不足问题，本发明提供了一种低介低损Ca-Al-B基LTCC材料及其制备方法，能够在低至850℃下烧结成瓷，并且保持良好的介电性能，使CaAl2B2O7微波陶瓷材料能够应用于LTCC领域。
一种低介低损Ca-Al-B基LTCC材料，其原料组成为CaCO3、Al2O3、B2O3、Li2CO3、Na2CO3和SiO2，化学通式为CaAl2B2O7-xM2CO3-yB2O3-zSiO2-mAl2O3，0＜x≤0.5mol，0＜y≤0.6mol，0＜z≤0.1mol，0＜m≤0.06mol；其中M为碱金属离子Li+和/或Na+。将原料按化学通式配料通过固相烧结法制得，实现了850℃～900℃的低温致密烧结，介电常数5～6.2，损耗低至4.19×10-4，频率温度系数-30～-20ppm/℃。
上述低介低损CaAl2B2O7基LTCC材料的制备方法如下：
步骤1：将原料CaCO3、Al2O3、B2O3、Li2CO3、Na2CO3和SiO2按照化学通式CaAl2B2O7-xM2CO3-yB2O3-zSiO2-mAl2O3，0＜x≤0.5mol，0＜y≤0.6mol，0＜z≤0.1mol，0＜m≤0.06mol，进行配料，其中M为碱金属离子Li+和/或Na+；
步骤2：将步骤1所配的原料粉体与锆球、去离子水以1:5:1.5～2.5置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，然后用40～60目筛网过筛后在大气气氛中以750℃～850℃预烧2～4小时；
步骤3：将步骤2得到的预烧后粉体再次与锆球、去离子水以1:5:1～2的比例混合置于球磨罐中球磨4～6小时。将球磨后的浆体于80℃～100℃烘干，然后把烘干后的粉体加入粘结剂与粉体混合均匀后，进行造粒。
步骤4：将步骤3制得产物压制成型，在400℃～500℃保温2小时排胶后在825℃～900℃大气气氛中烧结2～4小时，即可制成低介低损CaAl2B2O7基LTCC材料。
进一步的，所述步骤3中的粘结剂为占粉体质量5％-10％质量百分比的丙烯酸水溶液(丙烯酸和去离子水质量比＝1：1)。
综上所述，本发明使用固相法制得烧结温度低至850℃，具有低介电常数、低介电损耗的CaAl2B2O7基的低温烧结微波介质陶瓷材料。而CaAl2B2O7作为微波介质陶瓷具有低介电常数(εr＝4～6)、低介电损耗，但是其烧结温度在LTCC最高烧结温度附近，不利于其在LTCC中的应用；迄今为止，对CaAl2B2O7微波介质陶瓷的低温烧结性能及LTCC应用并未报道。
本发明将CaO-Al2O3-B2O3三元体系的典型代表CaAl2B2O7作为Ca-Al-B基微波介质陶瓷材料通过添加助剂使其可应用于LTCC领域，实现了850℃～900℃的低温致密烧结，介电常数5～6.2，损耗低至4.19×10-4，频率温度系数-30～-20ppm/℃。CaAl2B2O7作为CaO-Al2O3-B2O3三元体系的典型代表，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LTCC材料提供了一种具有优异性能LTCC材料的新选择。
附图说明
图1对应实施例2、5、6、7号的XRD衍射图谱。
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。
本发明按照化学通式CaAl2B2O7-xM2CO3-yB2O3-zSiO2-mAl2O3，x＝0～0.5mol，y＝0～0.6mol，z＝0～0.1mol，m＝0～0.06mol进行配料，其中M为碱金属离子Li+和/或Na+。原料为CaCO3、Al2O3、B2O3、Li2CO3、Na2CO3、SiO2。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 BDA0002716421540000031
Figure BDA0002716421540000032
Figure BDA0002716421540000041
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，最佳配方的CaAl2B2O7基微波陶瓷材料在825℃～900℃的烧结温度范围内，所有的样品微波介电性能优异，最佳烧结温度为850℃，能够在低于银电极熔点(961℃)的温度下烧结成瓷，说明该材料能够满足于LTCC工艺要求，可以应用于LTCC领域。
图1展示了本发明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、5、6和7号。从图1可以看出，主晶相为CaAl2B2O7(ICSD 01-089-5563)，次晶相为CaB2O4(ICSD 00-032-0155)。
以上实施例可见，本发明将CaO-Al2O3-B2O3三元体系的典型代表CaAl2B2O7作为Ca-Al-B基微波介质陶瓷材料通过添加助剂使其可应用于LTCC领域，实现了850℃～900℃的低温致密烧结，介电常数5～6.2，损耗低至4.19×10-4，频率温度系数-30～-20ppm/℃。为低介低损LTCC材料提供了一种具有优异性能LTCC材料的新选择。

Claims (3)

1.一种低介低损Ca-Al-B基LTCC材料，其特征在于：
原料组成为CaCO3、Al2O3、B2O3、Li2CO3、Na2CO3和SiO2，化学通式为CaAl2B2O7-xM2CO3-yB2O3-zSiO2-mAl2O3，0＜x≤0.5mol，0＜y≤0.6mol，0＜z≤0.1mol，0＜m≤0.06mol，其中M为碱金属离子Li+和/或Na+；将原料按化学通式配料通过固相烧结法制得，烧结温度850℃ ～900℃ ，介电常数5～6.2，损耗低至4.19×10-4，频率温度系数-30～-20ppm/℃。
2.权利要求1所述低介低损Ca-Al-B基LTCC材料的制备方法，其特征在于：
步骤1：将原料CaCO3、Al2O3、B2O3、Li2CO3、Na2CO3和SiO2按照化学通式CaAl2B2O7-x M2CO3-yB2O3-zSiO2-mAl2O3，0＜x≤0.5mol，0＜y≤0.6mol，0＜z≤0.1mol，0＜m≤0.06mol，进行配料，其中M为碱金属离子Li+和/或Na+；
步骤2：将步骤1所配的原料粉体与锆球、去离子水以1:5:1.5~2.5置于球磨罐中进行球磨，行星球磨4~6小时，球磨后的粉体以80℃ ~110℃ 烘干，然后用40～60目筛网过筛后在大气气氛中以750℃ ~850℃ 预烧2~4小时；
步骤3：将步骤2得到的预烧后粉体再次与锆球、去离子水以1:5:1~2的比例混合置于球磨罐中球磨4~6小时；将球磨后的浆体于80℃ ~100℃ 烘干，然后把烘干后的粉体加入粘结剂与粉体混合均匀后，进行造粒；
步骤4：将步骤3制得产物压制成型，在400~500℃ 保温2小时排胶后在825℃ ~900℃大气气氛中烧结2~4小时，即可制成低介低损CaAl2B2O7基LTCC材料。
3.如权利要求2所述低介低损Ca-Al-B基LTCC材料的制备方法，其特征在于：所述步骤3中的粘结剂为占粉体质量5%-10%质量百分比的丙烯酸水溶液，丙烯酸和去离子水质量比=1：1。
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