CN111499187B - 一种在20-60GHz高频频段内具有低损耗和低压电系数d33的玻璃材料 - Google Patents

一种在20-60GHz高频频段内具有低损耗和低压电系数d33的玻璃材料 Download PDF

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CN111499187B
CN111499187B CN202010351416.3A CN202010351416A CN111499187B CN 111499187 B CN111499187 B CN 111499187B CN 202010351416 A CN202010351416 A CN 202010351416A CN 111499187 B CN111499187 B CN 111499187B
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宋锡滨
艾辽东
张伟
奚洪亮
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Abstract

一种在20‑60GHz高频频段内具有低损耗和低压电系数d33的玻璃材料，其由如下质量百分比的组分制备而成：SiO210‑30wt％、B2O315‑35wt％、Al2O30‑10wt％、MgO 20‑40wt％、CaO 8‑30wt％、BaO 5‑15wt％、ZnO 0‑5wt％、Na2O 0‑6％、M2O3>0‑1％；其中，M为In、Yb、La或Y中的任意一种或几种。该玻璃材料制备得到的陶瓷片在高频段具有低介电常数和低介电损耗。

Description

一种在20-60GHz高频频段内具有低损耗和低压电系数d33的 玻璃材料
技术领域
本发明涉及电子陶瓷用玻璃材料技术领域，尤其是一种高频低损耗和低压电系数的玻璃材料及其制备方法。
背景技术
近年来，5G通信技术产生了对微波和毫米波频段的具有高频低损耗特性的电子元器件的巨大需求。低损耗和低介电常数的玻璃材料成为研究的热点，在高频频段具有非常大应用潜力。
玻璃/陶瓷体系和微晶玻璃体系是目前国内外广泛应用的LTCC基板材料。玻璃/陶瓷体系的物化性能主要由添加的陶瓷相决定，然而其基板的高频介电损耗大。微晶玻璃体系的介电性能和损耗性能由析出的晶体种类与数量控制，这类基板材料烧结后残余玻璃相极少，具有优良的高频性能，如CaO-B2O3-SiO2微晶玻璃的应用频率可达100GHz；但微晶玻璃体系的析晶行为对烧结工艺要求更高，产品性能稳定性差。
为了解决上述技术问题，提出了本发明的低损耗和低压电系数的玻璃材料及其制备方法。
发明内容
本发明针对高频频段(10-100GHz)天线模组设计对玻璃材料特定的应用需求，提出了一种在高频频段具有低损耗和低压电系数的玻璃材料，其在20-60GHz 频段内具有介电常数4-8，压电系数d33≤10C/N，介电损耗值0.002-0.005，满足对20-60GHz频段低损耗和低压电系数的技术要求。本发明还提出了上述玻璃材料的制备方法。
本发明提供了一种在20-60GHz高频频段内具有低损耗和低压电系数d33的玻璃材料，其由如下质量百分比的组分制备而成：
Figure BDA0002471951670000021
其中，M为In、Yb、La或Y中的任意一种或几种。
所述玻璃材料在20-60GHz频段内具有介电常数4-8，压电系数d33≤10C/N，介电损耗值0.002-0.005。
本发明的玻璃材料不含Pb、Bi、P、Sn等元素的氧化物，其在生产或应用期间保持环保和/或耐久性。
本发明还提供了制备上述玻璃材料的方法，包括如下步骤：根据配方称取各组分对应原料，混合均匀，熔融，保温，冷淬，将冷淬后的玻璃块球磨分散，并干燥过筛，得到玻璃粉。
其中，优选在1200-1400℃熔融，保温1-3h；更优选在1250-1350℃熔融，保温1.5-2.5h。
其中，优选干燥温度为120-150℃。
其中，所得到的玻璃粉的比表面积为0.2-10m2/g；优选0.2-2.0m2/g。
本发明还提供了由上述玻璃材料制备得到陶瓷片，该陶瓷片在20-60GHz频段内具有介电常数4-8，压电系数d33≤10C/N，介电损耗值0.002-0.005。
本发明还提供了上述陶瓷片的制备方法，包括向上述玻璃粉中，加入质量百分比1-2wt％的PVA，干压成型，然后在550-750℃烧结，保温1.5-2.5h，得到陶瓷片。
其中，烧结温度优选550-700℃。
对上述陶瓷片进行高频性能测试，测试完成以后，双面镀银进行压电性能测试。介电常数K的测试方法为该材料制备成表面平整的薄片，按照Q/0500SGC 企业标准测试方法(毫米波频段材料介电特性测试方法—开放式半球面电磁波谐振腔法)进行材料介电常数的测量。压电系数的测试采用ZJ-3型压电测试仪进行检测。
相比于现有技术，本发明具有以下优点：
稀土元素对玻璃陶瓷的介电常数和介电损耗产生影响，稀土元素的变价特性能够有效的改变玻璃陶瓷极化特性，介电常数和介电损耗随着稀土元素的种类和添加量的变化而变化。由于本发明在制备的LTCC配方粉材料体系中引入In2O3、 La2O3、Yb2O3中至少一种氧化物，这三种都是正三价元素，使得LTCC玻璃体系的玻璃网状结构参数发生变化，降低了极化偶极子和位移极化的数量，从而降低其软化点温度和介电常数。本发明的玻璃材料所制备得到的陶瓷片在高频段具有低介电常数和低介电损耗。
具体实施方式
以下结合实施例进一步说明本发明。
实施例1-10和对比例：
按照表1所示的各玻璃组分将原材料精确称量，干式混合均匀，将混合好的原材料加入白金坩埚，与1200-1400℃熔融2h后，将熔融后的玻璃倒入干式淬取机中进行快速降温淬取，将淬取得到的玻璃块，加入2倍玻璃质量的纯水和5 倍质量的氧化铝研磨球进行球磨分散，干燥过筛，得到实施例1-10和对比例的玻璃粉。
向实施例1-10和对比例的玻璃粉中，加入质量百分比1.5wt％的PVA，干压成型，然后在650℃烧结，保温2h，得到实施例1-10和对比例的陶瓷片。
对上述陶瓷片进行高频性能测试，测试完成以后，双面镀银进行压电性能测试。介电常数K的测试。测试前，首先将该材料制备成表面平整的薄片，然后采用经本公司长期研究开发的进阶型法布里-珀罗微扰法(简称AFPPM法)进行测试。进阶型法布里-珀罗微扰法：传统的法布里-珀罗微扰法在样品测试厚度上具有限制，无法满足市场上常见厚度的样品的测试，为解决此问题，根据电磁理论基础对法布里-珀罗微扰法进行改进，使其可以测试样品的厚度范围扩大，可应用到更多的市场上标准尺寸的基板材料，这种方法我们称之为进阶型法布里-珀罗微扰法(AdvancedFabry Perot Perturbation Methods)，简称AFPPM法。具体的测试过程详见企业标准Q/0500SGC 003.1-2020《毫米波频段材料介电性能测试方法第1部分：20-70GHz介电性能常温测试方法》。压电系数的测试采用ZJ-3型压电测试仪进行检测。
经测试，实施例1-10和对比例的玻璃材料所制备得到的陶瓷片在高频段具有低介电常数和低介电损耗。
Figure BDA0002471951670000051
Figure BDA0002471951670000061
显然，上述实施例仅仅是为清楚地说明所作的举例，而并非对实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引伸出的显而易见的变化或变动仍处于本发明创造的保护范围之中。

Claims (9)

1.一种在20-60GHz高频频段内具有低损耗和低压电系数d33的玻璃材料，其由如下质量百分比的组分制备而成：
Figure FDA0003508397520000011
其中，M为In、Yb、La或Y中的任意一种或几种；
所述玻璃材料为玻璃粉。
2.如权利要求1所述的玻璃材料，其中，所述玻璃材料不含Pb、Bi、P、Sn元素的氧化物。
3.如权利要求1所述的玻璃材料，其中，所述玻璃材料为比表面积为0.2-10m2/g的玻璃粉。
4.一种如权利要求1-3任一所述的玻璃材料的制备方法，包括如下步骤：根据配方称取各组分对应原料，混合均匀，熔融，保温，冷淬，将冷淬后的玻璃块球磨分散，并干燥过筛，得到玻璃粉。
5.如权利要求4所述的玻璃材料的制备方法，其中，在1200-1400℃熔融，保温1-3h。
6.如权利要求4-5任一所述的玻璃材料的制备方法，其中，干燥温度为120-150℃。
7.一种由权利要求1-3任一所述的玻璃材料制备得到的陶瓷片，所述陶瓷片在20-43.5GHz频段内具有介电常数4-8，压电系数d33≤10C/N，介电损耗值0.002-0.005。
8.如权利要求7所述的陶瓷片的制备方法，包括向所述玻璃粉中，加入质量百分比1-2％的PVA，干压成型，然后在550-750℃烧结，保温1.5-2.5h，得到陶瓷片。
9.如权利要求8所述的陶瓷片的制备方法，其中，烧结温度为550-700℃。
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