CN115215639A - 一种低温烧结微波介质陶瓷材料及其制备方法 - Google Patents

一种低温烧结微波介质陶瓷材料及其制备方法 Download PDF

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CN115215639A
CN115215639A CN202210895464.8A CN202210895464A CN115215639A CN 115215639 A CN115215639 A CN 115215639A CN 202210895464 A CN202210895464 A CN 202210895464A CN 115215639 A CN115215639 A CN 115215639A
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陈亚伟
周志斌
梁启新
简丽勇
付迎华
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Abstract

一种低温烧结微波介质陶瓷材料及其制备方法,本发明属于电子陶瓷及其制造领域，本发明材料为Ba2Si3O8基低温烧结微波介质陶瓷材料，其材料化学式为Ba2Si3O8‑x0.3BaCO3‑x0.45SiO2‑x0.2B2O3‑x0.05CuO（x=0‑0.6mol），通过固相反应法制备；烧结后的晶相为Ba2Si3O8相。本发明烧结温度830℃～900℃，介电常数6～9，损耗低至3.0×10‑4，该组分陶瓷品质因素高，能够应用在高频滤波器领域。本发明制备工艺简单，性能优异。

Description

一种低温烧结微波介质陶瓷材料及其制备方法
技术领域
本发明属于电子陶瓷及其制造领域，涉及一种低温烧结Ba2Si3O8基微波介质陶瓷材料及其制备方法。
背景技术
近几十年国内外通信行业不断发展，无线电移动通讯设备更新换代频繁，小型化、功能更强大、低成本成为其发展的趋势。微波介质陶瓷（MWDC）是无线电通信设备中微波元器件的关键基础材料，广泛用于介质谐振器、滤波器、介质基片、微带天线等，各国对它的研究也一直没有停止。
对于微波介质陶瓷来说，最重要的三个参数是相对介电常数ε r 、品质因数Q×f和谐振频率温度系数τ f 。其中，相对介电常数ε r 通常用于表征介质材料的极化性质和介电性质；品质因数Q×f表示一个储能器件（如电感线圈、电容等）、谐振电路中所储能量同每周期损耗能量之比的一种质量指标；谐振频率温度系数τ f 表示为谐振频率对温度变化的灵敏度。
低温共烧陶瓷（Low Temperature Co-fired Ceramic, LTCC）技术能够将多个不同类型、不同性能的无源元件集成在一个封装内，能够有效的降低各种通信射频器件的体积，是无源集成的主流技术。因为该技术要求与现今生产中所使用的Ag、Cu等电极进行共烧，所以LTCC材料要有较低的烧结温度（≤950℃）以及与电极良好的化学兼容性。
纯的Ba2Si3O8陶瓷有着优异的微波介电性能 ε r =8.2，Q×f=29800GHz，但是烧结温度高达1300℃，过高的烧结温度限制了其在LTCC领域的应用。但是迄今为止，关于Ba2Si3O8陶瓷的低温烧结及LTCC应用方面未见报道。
发明内容
针对以上问题，本发明提供了一种低温烧结Ba2Si3O8基微波介质陶瓷材料及其制备方法。
一种低温烧结Ba2Si3O8基微波介质陶瓷材料,原料的组分是BaCO3、SiO2、B2O3、CuO，按照Ba2Si3O8-x0.3BaCO3- x0.45SiO2-x0.2B2O3-x0.05CuO（x=0-0.6mol）化学通式进行配料，通过固相反应法合成。
其制备方法如下：
步骤1、将BaCO3、SiO2、B2O3、CuO的原始粉料按照Ba2Si3O8-x0.3BaCO3- x0.45SiO2-x0.2B2O3-x0.05CuO（x=0-0.6mol）化学通式进行配料；
步骤2、将步骤1准备的配料装入球磨罐，以锆球及去离子水作为研磨介质，按照粉体：锆球：去离子水=1:4～7:2～4（质量比）行星球磨5～7小时，然后在80～100℃烘干。烘干后的粉体以40～60目筛网过筛，随后在900～1050℃大气气氛中预烧2～4小时；
步骤3、对预烧后的粉料进行二次球磨，锆球：去离子水=1: 4～7:1～3（质量比）行星球磨2～6小时。球磨后的湿料取出烘干后，再用2～6wt%浓度的丙烯酸溶液作为粘接剂对粉料进行造粒；
步骤4、将步骤3造粒后的粉体放入模具中干压成型，将圆柱块体在400℃～600℃排胶后，在830℃～900℃空气气氛下烧结保温0.5～4小时，即可制得Ba2Si3O8基低温烧结微波介质陶瓷。
该电子陶瓷材料能在低温下（≤900℃）烧结致密，同时具有高的品质因数。其烧结后的晶相为Ba2Si3O8相，烧结温度可低至830℃，介电常数6～9，损耗低至3.0×10-4（10000GHz＜Q×f ≤ 30000 GHz），使其可以应用在LTCC领域，制备工艺简单，性能优异。
本发明通过调节BaCO3、SiO2、B2O3和CuO等低熔点的氧化物与BaCO3、SiO2主基料的比例，使其能够在较低烧结温度（≤900℃）下烧结致密，介电性能优异能够应用在高频滤波器领域，解决了Ba2Si3O8陶瓷在LTCC领域的应用。
本发明提供的制备方法为固相烧结法，工艺简单。
附图说明
图1为图1为实施例5的XRD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。
一种低温烧结Ba2Si3O8基微波介质陶瓷材料，采用如下方法制备：
步骤1、将BaCO3、SiO2、B2O3、CuO的原始粉料按照Ba2Si3O8-x0.3BaCO3- x0.45SiO2-x0.2B2O3-x0.05CuO（x=0-0.6mol）化学通式进行配料；
步骤2、将步骤1准备的配料装入球磨罐，以锆球及去离子水作为研磨介质，按照粉体：锆球：去离子水=1:5:2（质量比）行星球磨6小时，然后在100℃烘干。烘干后的粉体以60目筛网过筛，随后在1000℃大气气氛中预烧4小时；
步骤3、对预烧后的粉料进行二次球磨，锆球：去离子水=1:5:2（质量比）行星球磨2～6小时，湿料取出烘干后，再用3wt%浓度的丙烯酸溶液作为粘接剂对粉料进行造粒；
步骤4、将步骤3造粒后的粉体放入φ12的模具中干压成型，将圆柱块体在500℃排胶后，下列各表中的烧结温度的空气气氛下烧结保温1小时，即可制得Ba2Si3O8基低温烧结微波介质陶瓷。
图1为实施例5的XRD图。从图中可以看出，实施例表现为单一的Ba2Si3O8(JCPDS #00-027-1035)相。
采用上述的方法，调整各组分的用量（如下表所示），8个实施方式如下：
Figure 844586DEST_PATH_IMAGE002
Figure 292884DEST_PATH_IMAGE004
上述各个实施方式的微波介电性能如下表格：
Figure DEST_PATH_IMAGE005
从表中可以看出，在830℃至900℃保温1小时所有样品都表现出了优异的微波介电性能，说明在该温度内陶瓷成瓷状况良好，能够满足LTCC领域应用。
综合上述，本发明通过调节原料BaCO3、SiO2、B2O3和CuO的摩尔比例，最终得到了性能优异的低温烧结低介高品质因数的Ba2Si3O8基微波介质陶瓷体系，其制备方法简单，易于工业化生产。

Claims (3)

1.一种低温烧结Ba2Si3O8基微波介质陶瓷材料的制备方法，其特征在于：其制备方法如下：
步骤1、将BaCO3、SiO2、B2O3和CuO的原始粉料按照Ba2Si3O8-x0.3BaCO3- x0.45SiO2-x0.2B2O3-x0.05CuO化学通式进行配料，其中x=0-0.6mol；
步骤2、将步骤1准备的配料装入球磨罐，以锆球及去离子水作为研磨介质，按照粉体：锆球：去离子水的质量比为1:4～7:2～4行星球磨5～7小时，然后在80～100℃烘干，烘干后的粉体以40～60目筛网过筛，随后在900～1050℃大气气氛中预烧2～4小时；
步骤3、对预烧后的粉料进行二次球磨，锆球：去离子水的质量比为1: 4～7:1～3行星球磨2～6小时，球磨后的湿料取出烘干后，再用2～6wt%浓度的丙烯酸溶液作为粘接剂对粉料进行造粒；
步骤4、将步骤3造粒后的粉体放入模具中干压成型，将圆柱块体在400℃～600℃排胶后，在830℃～900℃空气气氛下烧结保温0.5～4小时，即可制得Ba2Si3O8基低温烧结微波介质陶瓷。
2.如权利要求1所述的低温烧结Ba2Si3O8基微波介质陶瓷材料的制备方法制备的陶瓷材料。
3.如权利要求2所述的陶瓷材料的应用，其特征在于，所述的陶瓷材料应用于LTCC领域。
CN202210895464.8A 2022-07-28 2022-07-28 一种低温烧结微波介质陶瓷材料及其制备方法 Pending CN115215639A (zh)

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