CN111606709A - 一种超低温烧结微波介质材料及其制备方法 - Google Patents

一种超低温烧结微波介质材料及其制备方法 Download PDF

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CN111606709A
CN111606709A CN202010528085.6A CN202010528085A CN111606709A CN 111606709 A CN111606709 A CN 111606709A CN 202010528085 A CN202010528085 A CN 202010528085A CN 111606709 A CN111606709 A CN 111606709A
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李波
邓亚平
姚朋玉
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University of Electronic Science and Technology of China
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Abstract

本发明属于电子陶瓷及其制造领域，具体提供一种超低温烧结微波介质陶瓷材料及其制备方法，用以克服目前微波陶瓷材料烧结温度普遍偏高的缺点，实现了低于670℃的超低温烧结。本发明陶瓷材料主晶相为Ba3V2O8，通过添加占主晶相质量百分比为6～12wt％的低熔点化合物Li2CO3，形成液相促进晶粒生长，大大降低烧结温度，实现650～670℃的超低温烧结，且具备优异的微波性能；同时，Li2CO3的添加能够调整陶瓷材料谐振频率温度系数，能够获得近零值，大大扩展材料的适用性；最后，本发明提供的超低温烧结微波介质材料制备工艺简单，所有原料成本低廉、来源丰富，有利于工业化生产，可广泛应用于低温共烧陶瓷体系、多层介质谐振器、滤波器等微波器件的制造。

Description

一种超低温烧结微波介质材料及其制备方法
技术领域
本发明属于电子陶瓷及其制造领域，涉及一种微波介质陶瓷材料，具体涉及超低温烧结微波介质陶瓷材料及其制备方法。
背景技术
微波介质陶瓷具有稳定的介电常数、较高的品质因数和近零的频率温度系数，可以制成介质稳频振荡器、介质谐振器、微波介质天线等，广泛应用于微波技术各个领域。低温烧结微波介质陶瓷是目前主要趋势，但很多微波介质陶瓷的烧结温度偏高，因此，如何降低烧结温度成为一个急需解决的问题；添加助烧剂是降低烧结温度的一个主要途径，助烧剂通常是低熔点的氧化物或玻璃来形成液相促进晶粒生长。近年出现了超低温共烧陶瓷(ULTCC)，具有节省能源和时间的优势。例如，Di Zhou等人在文献Microwave DielectricProperties of Li2WO4 Ceramic with Ultra-Low Sintering Temperature中在640℃制备的Li2WO4陶瓷具有较高的Q×f值，是适合于超低温烧结的微波介质陶瓷。
钒酸盐固有烧结温度低、微波性能优良，国内外学者对低温烧结钒酸盐陶瓷进行了研究。比如，Unnimaya等人在文献“Structure and microwave dielectric propertiesof 5BaO–2V2O5 binary ceramic system”中于1300℃的烧结温度下制备出Ba3V2O8微波介质陶瓷，其性能为εr＝12.3、Q×f＝52197GHz、τf＝41ppm/℃；同时，通过添加0.5wt％的B2O3到Ba3V2O8陶瓷，烧结温度降低至950℃，且微波性能较为优异：εr＝12.5，Q×f＝41,065GHz，τf＝38.8ppm/℃；但是，该Ba3V2O8微波介质陶瓷的烧结温度仍然偏高，远远达不到超低温烧结的要求。
基于此，本发明提供一种超低温烧结微波介质材料及其制备方法。
发明内容
本发明的目的在于提供一种超低温烧结微波介质陶瓷材料及其制备方法，用以克服目前微波陶瓷材料烧结温度普遍偏高的缺点，实现了低于670℃的超低温烧结。本发明陶瓷材料主晶相为Ba3V2O8，通过添加占主晶相质量百分比为6～12wt％的低熔点化合物Li2CO3，形成液相促进晶粒生长，以降低烧结温度，实现超低温烧结(烧结温度为650～670℃，介电常数为13～14，Q×f值为28000～34000GHz，谐振频率温度系数为-9～52ppm/℃)。
为实现上述目的，本发明所实施的技术方案为：
一种超低温烧结微波介质材料，其特征在于：所述微波介质材料包括：主晶相、以及占主晶相质量百分比为6～12wt％的添加剂；其中：
所述主晶相为：Ba3V2O8；
所述添加剂为：Li2CO3。
进一步的，所述微波介质材料的烧结温度为650～670℃，介电常数为13～14，Q×f值为28000～34000GHz，谐振频率温度系数为-9～52ppm/℃。
上述超低温烧结微波介质材料的制备方法，其特征在于，包括以下步骤：
步骤1.配料：以分析纯BaCO3、V2O5为原料，按化学式Ba3V2O8的摩尔比进行配料；
步骤2.一次球磨：以去离子水和锆球为介质，按照料：水：球为1:1.5:5(质量比)的比例在尼龙罐中湿磨混合原料6～8小时，球磨后出料置于烘箱中110℃烘干；
步骤3.过筛：用60目筛网过筛干燥料；
步骤4.预烧：将过筛料在空气中以750～800℃预烧3～4小时，得到主晶相为Ba3V2O8的预烧料；
步骤5.添加Li2CO3：将预烧料与占预烧料质量百分比为6～12wt％的Li2CO3粉末混合；
步骤6.二次球磨：以去离子水和锆球为介质，按照预烧料：球：水为1:5:1.5(质量比)的比例置于尼龙罐中湿磨混合7小时，球磨后出料置于烘箱中于110℃烘干；
步骤7.造粒成型：将干燥料与PVA溶液进行混合、造粒，然后在10～20MPa的压力下压制成生坯；
步骤8.烧结：将生坯在空气中以650～670℃的温度烧结5小时，得到所述的微波介质材料。
本发明的有益效果在于：
1.本发明提供超低温烧结微波介质材料，通过在主晶相Ba3V2O8中添加低熔点化合物Li2CO3，形成液相促进晶粒生长，大大降低烧结温度，实现650～670℃的超低温烧结，且具备优异的微波性能；为实现ULTCC技术提供了候选材料，具有节省能源和时间的优势；
2.本发明提供超低温烧结微波介质材料的主晶相为Ba3V2O8，通过添加低熔点化合物Li2CO3，调整其谐振频率温度系数，在添加10wt％的Li2CO3时获得近零值(τf＝4.7)；大大扩展材料的适用性；
3.本发明提供的超低温烧结微波介质材料制备工艺简单，所有原料成本低廉、来源丰富，有利于工业化生产，可广泛应用于低温共烧陶瓷体系、多层介质谐振器、滤波器等微波器件的制造。
附图说明
图1为实施例2制备得微波介质材料Ba3V2O8+8wt％Li2CO3的XRD图。
图2为实施例2制备得微波介质材料Ba3V2O8+8wt％Li2CO3的SEM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详细说明。
本发明共提供4个实施例，每个实施例提供的低温烧结微波陶瓷材料具有主晶相Ba3V2O8、属于六方晶系，以及占主晶相质量百分比为x wt％的Li2CO3，其中，x＝6、8、10、12。
上述低温烧结微波陶瓷材料的制备方法，包括以下步骤：
步骤1.配料：以分析纯BaCO3、V2O5为原料，按化学式Ba3V2O8的摩尔比进行配料；
步骤2.一次球磨：以去离子水和锆球为介质，按照料：水：球为1:1.5:5的比例在尼龙罐中湿磨混合原料6～8小时，球磨后出料置于烘箱中110℃烘干；
步骤3.过筛：用60目筛网过筛干燥料；
步骤4.预烧：将过筛料在空气中以750～800℃预烧3～4小时，得到主晶相为Ba3V2O8的预烧料；
步骤5.添加Li2CO3：将预烧后的Ba3V2O8粉末与x wt％的Li2CO3(x＝6，8，10，12)粉末混合；
步骤6.二次球磨：以去离子水和锆球为介质，按照预烧料：球：水为1:5:1.5的比例置于尼龙罐中湿磨混合7小时，球磨后出料置于烘箱中于110℃烘干；
步骤7.造粒成型：将干燥料与PVA溶液进行混合、造粒，然后在10～20MPa的压力下压制成生坯；
步骤8.烧结：将生坯在空气中以650～670℃的温度烧结5小时，得到所述的微波介质材料。
上述4个实施例的具体公开参数及制备得超低温烧结微波陶瓷材料微波介电性能如下表所示：
编号 组成 烧结温度 烧结时长 ε<sub>r</sub> Q×f值 τ<sub>f</sub>
实施例1 x＝6 670 5 13.66 28901 51.6
实施例2 x＝8 660 5 13.07 33129 13.3
实施例3 x＝10 650 5 13.62 31756 4.7
实施例4 x＝12 650 5 13.37 30262 -8.7
由上可见，实施例2中超低温烧结微波陶瓷材料Ba3V2O8+8wt％Li2CO3的XRD图如图1所示，由图可见，添加Li2CO3不会改变吸收峰的位置，Ba3V2O8晶相保持六方晶系不变；SEM图如图2所示，由图可见，由于Li2CO3熔点(618℃)低于烧结温度，因此烧结过程会形成大量液相聚集在晶界处，使晶界变得模糊。
以上所述，仅为本发明的具体实施方式，本说明书中所公开的任一特征，除非特别叙述，均可被其他等效或具有类似目的的替代特征加以替换；所公开的所有特征、或所有方法或过程中的步骤，除了互相排斥的特征和/或步骤以外，均可以任何方式组合。

Claims (3)

1.一种超低温烧结微波介质材料，其特征在于：所述微波介质材料包括：主晶相、以及占主晶相质量百分比为6～12wt％的添加剂；其中：
所述主晶相为：Ba3V2O8；
所述添加剂为：Li2CO3。
2.按权利要求1所述超低温烧结微波介质材料，其特征在于，所述微波介质材料的烧结温度为650～670℃，介电常数为13～14，Q×f值为28000～34000GHz，谐振频率温度系数为-9～52ppm/℃。
3.按权利要求1所述超低温烧结微波介质材料的制备方法，其特征在于，，包括以下步骤：
步骤1.配料：以分析纯BaCO3、V2O5为原料，按化学式Ba3V2O8的摩尔比进行配料；
步骤2.一次球磨：以去离子水和锆球为介质，按照料：水：球为1:1.5:5的比例在尼龙罐中湿磨混合原料6～8小时，球磨后出料置于烘箱中110℃烘干；
步骤3.过筛：用60目筛网过筛干燥料；
步骤4.预烧：将过筛料在空气中以750～800℃预烧3～4小时，得到主晶相为Ba3V2O8的预烧料；
步骤5.添加Li2CO3：将预烧料与占预烧料质量百分比为6～12wt％的Li2CO3粉末混合；
步骤6.二次球磨：以去离子水和锆球为介质，按照预烧料：球：水为1:5:1.5的比例置于尼龙罐中湿磨混合7小时，球磨后出料置于烘箱中于110℃烘干；
步骤7.造粒成型：将干燥料与PVA溶液进行混合、造粒，然后在10～20MPa的压力下压制成生坯；
步骤8.烧结：将生坯在空气中以650～670℃的温度烧结5小时，得到所述的微波介质材料。
CN202010528085.6A 2020-06-11 2020-06-11 一种超低温烧结微波介质材料及其制备方法 Pending CN111606709A (zh)

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