CN109775993B - 一种ltcc基板及其制备方法 - Google Patents

一种ltcc基板及其制备方法 Download PDF

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CN109775993B
CN109775993B CN201910155188.XA CN201910155188A CN109775993B CN 109775993 B CN109775993 B CN 109775993B CN 201910155188 A CN201910155188 A CN 201910155188A CN 109775993 B CN109775993 B CN 109775993B
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glass
ltcc substrate
sio
ltcc
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陈涛
黄国洪
王岩
黄昆
沓世我
付振晓
刘芸
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Guangdong Fenghua Advanced Tech Holding Co Ltd
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Priority to PCT/CN2019/116357 priority patent/WO2020177368A1/zh
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Abstract

本发明涉及一种LTCC基板及其制备方法，尤其涉及一种介电常数可调的LTCC基板及其制备方法。本发明LTCC基板包括下述组分：玻璃、SiO2和Al2O3，所述SiO2在LTCC基板中的重量百分比为10％～25％。本发明通过在LTCC基板中添加SiO2，使LTCC基板的气孔率、介电常数和介电损耗有效降低，同时在一定程度上提高LTCC基板的弯曲强度。本发明通过调节玻璃、SiO2及Al2O3三者比例，所得LTCC基板介电常数可在4.3‑6.0之间调节，介电损耗低至0.2％；在满足LTCC基板低介电、低损耗特性的同时，保证了烧结基板的致密性及强度。

Description

一种LTCC基板及其制备方法
技术领域
本发明涉及一种LTCC基板及其制备方法，尤其涉及一种介电常数可调的LTCC基板及其制备方法。
背景技术
随着5G通讯及万物互联时代的到来，高频应用成为趋势，为减少信号传输损耗，加快信号传输速度，低介电常数LTCC瓷粉受到越来越多的关注。由于Al2O3介电常数偏高(9～11)，进一步的降低瓷粉介电常数较为困难，采用增加体系中玻璃比例的方法虽然可以有效降低介电常数，但玻璃的过多添加，导致烧结瓷体中存在较多的气孔，极大降低了基板的可靠性及强度。
发明内容
本发明的目的在于克服上述现有技术的不足之处而提供一种气孔率和介电常数均较低、且介电常数可调的LTCC基板及其制备方法。
为实现上述目的，本发明采取的技术方案为：一种LTCC基板，其包括下述组分：玻璃、SiO2和Al2O3，所述SiO2在LTCC基板中的重量百分比为10％～25％。
本发明的LTCC基板中添加了SiO2，SiO2的添加可在保证LTCC基板弯曲强度的同时，得到气孔率较低的致密基板。并且，通过调整配方，可以得到低介电常数且介电常数可调的LTCC基板。
研究表明，当SiO2在LTCC基板中的重量百分比为10％时，本发明LTCC基板的气孔率明显下降，且其介电损耗低，同时弯曲强度高。
作为本发明所述LTCC基板的优选实施方式，所述SiO2在LTCC基板中的重量百分比为20％～25％。随着LTCC基板中SiO2含量的增加，LTCC基板的气孔率、介电常数和介电损耗均会降低，当SiO2在LTCC基板中的重量百分比大于20wt％时，所得LTCC基板致密且无明显气孔，具体地，LTCC基板的孔率降低到约0.11％。
作为本发明所述LTCC基板的优选实施方式，所述SiO2在LTCC基板中的重量百分比为20％。若SiO2在LTCC基板中的含量太高，也会导致LTCC基板的弯曲强度降低，综合考虑LTCC基板的弯曲强度、气孔率、介电常数以及介电损耗，选择SiO2在LTCC基板中的重量百分比为20％。
作为本发明所述LTCC基板的优选实施方式，所述LTCC基板中，玻璃的重量百分比为50％-60％,Al2O3的重量百分比为25～40％。
作为本发明所述LTCC基板的优选实施方式，所述玻璃由下述重量百分比的组分组成：SiO2 45.8％，H3BO3 39.6％，K2CO3 3.3％，Na2CO3 3.6％，Li2CO3 0.7％，CaCO3 1.5％，SrCO3 1.1％，BaCO3 1.9％，Al2O3 1.2％，MgO 0.6％，TiO2 0.4％和ZnO 0.3％。
作为本发明所述LTCC基板的优选实施方式，所述玻璃为玻璃粉，所述玻璃粉的制备方法为：
(a)按比例称取玻璃中的各组分，球磨后烘干，然后在1250℃以上的温度下保温，使得玻璃液均化；
(b)将玻璃液取出，于水中淬火，再进行球磨，得到玻璃浆料，烘干玻璃浆料，得到所述玻璃粉。
上述玻璃粉熔制温度可低至1250℃(一般同行业熔制温度需要1500℃左右)，较低的玻璃熔制温度，可较大程度节省成本。
另外，本发明提供了上述LTCC基板的制备方法，其包括以下步骤：
(1)按比例称取玻璃、SiO2和Al2O3，进行球磨，使玻璃、SiO2和Al2O3混合均匀，然后烘干，得到LTCC瓷粉；
(2)向步骤(1)所得LTCC瓷粉中加入溶剂、分散剂、增塑剂、消泡剂及粘合剂，进行球磨，得到陶瓷浆料；
(3)将步骤(2)所得陶瓷浆料流延成膜片，叠层后进行等静压处理，然后切割成生片；
(4)烧结步骤(3)所得生片，冷却后得到所述LTCC基板。
作为本发明所述LTCC基板的制备方法的优选实施方式，所述步骤(3)中，膜片的厚度为60μm，等静压处理的压力为20MPa。
作为本发明所述LTCC基板的制备方法的优选实施方式，所述步骤(4)中，将步骤(3)所得生片于870℃烧结，保温30min，冷却后得到所述LTCC基板。
与现有技术相比，本发明的有益效果为：
(1)本发明通过在LTCC基板中添加SiO2，使LTCC基板的气孔率、介电常数和介电损耗有效降低，同时在一定程度上提高LTCC基板的弯曲强度。同时，由于SiO2介电常数低于Al2O3，通过调节玻璃、SiO2及Al2O3三者比例，所得LTCC基板介电常数在4.3-6.0较宽的范围内连续可调，介电损耗可低至0.2％，且提高了器件设计的灵活性；在满足LTCC基板低介电、低损耗特性的同时，保证了烧结基板的致密性及强度。本发明的LTCC基板适用于高频通讯领域及射频领域。
(2)本发明玻璃熔制温度可低至1250℃(一般同行业熔制温度需要1500℃左右)，较低的玻璃熔制温度，可较大程度节省成本。
附图说明
图1为本发明实施例3～5以及对比例1LTCC基板的SEM图。
具体实施方式
为更好地说明本发明的目的，技术方案和优点，下面将结合附图和具体实施例对本发明作进一步说明。
实施例1～5和对比例1LTCC基板
实施例1～5和对比例1LTCC基板的组成组分如表1所示。其中，所述玻璃为玻璃粉，所述玻璃由下述重量百分比的组分组成：SiO2 45.8％，H3BO3 39.6％，K2CO3 3.3％，Na2CO33.6％，Li2CO3 0.7％，CaCO3 1.5％，SrCO3 1.1％，BaCO3 1.9％，Al2O3 1.2％，MgO 0.6％，TiO2 0.4％和ZnO 0.3％。
所述玻璃的制备方法为：
(a)按比例称取玻璃中的各组分，采用玛瑙球磨罐，以去离子水为媒介，行星球磨4h，出料，100℃下烘干12h；
(b)将烘干原料粉装在铂金坩埚中，置于高温炉中，在1250℃下保温2h，使得玻璃液均化，将玻璃液高温取出，于去离子水中淬火；
(c)将上述淬火玻璃置于玛瑙球磨罐中，以氧化锆球为介质，去离子水为媒介，行星球磨12h,得到玻璃玻璃浆料，将玻璃浆料于100℃下烘干12h，得到干燥玻璃粉。
实施例1～5LTCC基板的制备方法为：
(1)按比称取玻璃粉、SiO2及Al2O3，于玛瑙球磨罐中，以去离子水为媒介，行星球磨2h，使得粉体混合均匀，再在100℃下烘干12h，得到LTCC瓷粉；
(2)将上述瓷粉添加适量溶剂、分散剂、增塑剂、消泡剂及粘合剂，置于卧式球磨罐中，球磨28h，得到均一稳定的陶瓷浆料；
(3)将上述陶瓷浆料流延成厚度～60μm膜片，叠层后以～20MPa压力等静压，切割成15mm*15mm方形生片；
(4)将上述生片于870℃烧结，保温30min，之后随炉冷却，得到表面平整LTCC基板。
对比例1LTCC基板的制备方法与实施例1～5LTCC基板的制备方法的区别仅在于：步骤(1)中，按比例称取玻璃粉及Al2O3于玛瑙球磨罐中。
测试实施例1～5和对比例1LTCC基板的气孔率、弯曲强度、介电常数和介电损耗，气孔率采用静水力学称重法，按照《中华人民共和国轻工业行业标准：QB/T 1642-2012》测试计算得到，弯曲强度采用三点弯曲法测试，1MHz下介电常数采用Agilent E4980A精密电桥测试仪测试，按照平行板电容器公式计算得出。10GHz下介电常数及损耗采用网络分析仪，以平行板反射法测试得到。实验结果如表1所示。同时采用SEM对实施例3～5和对比例1基板进行测定，结果如图1所示。图1中，(a)表示对比例1LTCC基板，(b)表示实施例3LTCC基板，(c)表示实施例4LTCC基板，(d)表示实施例5LTCC基板。
表1
Figure BDA0001982673400000051
SEM图表明，SiO2的添加可有效降低瓷体气孔率，SiO2含量为10wt％时，瓷体气孔率明显下降，SiO2含量大于20wt％时，瓷体中无明显气孔。结合表1数据可知，SiO2含量为10wt％时，瓷体气孔率低于0.26％，且弯曲强度高于169MPa，SiO2含量为20wt％时，气孔率降低到最低值0.11％，弯曲强度达到最大值186MPa。并且，在10GHz高频下，本发明LTCC基板可保持较低的介电损耗，最低可达到0.32％，在得到介电常数可调的性能同时，基板1MHz及高频下的损耗较低，同时兼具致密性及较高的弯曲强度。可应用于具有低延时传输要求的物联网、车联网及5G射频器件领域。
最后所应当说明的是，以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制，尽管参照较佳实施例对本发明作了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的实质和范围。

Claims (5)

1.一种LTCC基板，其特征在于，由下述重量百分比的组分组成：玻璃50％、SiO2 20％和Al2O3 30％；其中，所述玻璃由下述重量百分比的组分组成：SiO245.8％，H3BO3 39.6％，K2CO3 3.3％，Na2CO3 3.6％，Li2CO3 0.7％，CaCO3 1.5％，SrCO3 1.1％，BaCO3 1.9％，Al2O31.2％，MgO 0.6％，TiO2 0.4％和ZnO 0.3％。
2.如权利要求1所述的LTCC基板，其特征在于，所述玻璃为玻璃粉，所述玻璃粉的制备方法为：
(a)按比例称取玻璃中的各组分，球磨后烘干，然后在1250℃以上的温度下保温，使得玻璃液均化；
(b)将玻璃液取出，于水中淬火，再进行球磨，得到玻璃浆料，烘干玻璃浆料，得到所述玻璃粉。
3.如权利要求1或2所述LTCC基板的制备方法，其特征在于，包括以下步骤：
(1)按比例称取玻璃、SiO2和Al2O3，进行球磨，使玻璃、SiO2和Al2O3混合均匀，然后烘干，得到LTCC瓷粉；
(2)向步骤(1)所得LTCC瓷粉中加入溶剂、分散剂、增塑剂、消泡剂及粘合剂，进行球磨，得到陶瓷浆料；
(3)将步骤(2)所得陶瓷浆料流延成膜片，叠层后进行等静压处理，然后切割成生片；
(4)烧结步骤(3)所得生片，冷却后得到所述LTCC基板。
4.如权利要求3所述LTCC基板的制备方法，其特征在于，所述步骤(3)中，膜片的厚度为60μm，等静压处理的压力为20MPa。
5.如权利要求3所述LTCC基板的制备方法，其特征在于，所述步骤(4)中，将步骤(3)所得生片于870℃烧结，保温30min，冷却后得到所述LTCC基板。
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