CN115353387B - 一种微波介质材料ErVO4及其制备方法 - Google Patents

一种微波介质材料ErVO4及其制备方法 Download PDF

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CN115353387B
CN115353387B CN202210987202.4A CN202210987202A CN115353387B CN 115353387 B CN115353387 B CN 115353387B CN 202210987202 A CN202210987202 A CN 202210987202A CN 115353387 B CN115353387 B CN 115353387B
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李波
杨瑞佳
陈丽
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Abstract

本发明属于电子陶瓷及其制造领域，提供一种微波介质材料ErVO4及其制备方法。所述微波介质材料的化学式为ErVO4，晶相为ErVO4，晶体结构为四方锆石结构。在1100～1250℃烧结拥有优良的微波介电性能：介电常数εr为11.42～12.03、Q×f值20268～25549GHz、谐振频率温度系数τf为‑67.49～‑46.35ppm/℃。本发明微波介质材料ErVO4的制备工艺简单、生产成本低，有利于实现工业化生产。

Description

一种微波介质材料ErVO4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，涉及一种微波介质材料ErVO4及其制备方法。
背景技术
微波介质材料可用于制造滤波器、谐振器、介质天线等微波器件，被广泛应用于5G通信、GPS导航、雷达等领域。钒酸盐微波介质材料普遍具有较低的烧结温度、优良的微波介电性能，近年来受到人们的高度关注。在“Nanocrystalline ErVO4:synthesis,characterization,optical and photocatalytic properties,J.Mater.Sci.:Mater.Electron.28(2017)8446-8451”中，Abedini研究了ErVO4光催化性能，ErVO4在紫外光照射下对甲基橙进行了光催化降解。在“ErVO4 materials gas sensor for TEAdetection with fast response/recovery time,Mater.Lett.314(2022)131899”中，Yang等人研究了ErVO4作为气体传感器的快速响应/恢复时间。但是，在微波介质材料领域尚未有人对ErVO4进行研究和报道。
基于此，本发明提供一种微波介质材料ErVO4及其制备方法。
发明内容
本发明的目的在于提供了一种微波介质材料ErVO4及其制备方法。
为实现上述目的，本发明采用的技术方案如下：
一种微波介质材料，其特征在于，所述微波介质材料的化学式为ErVO4。
进一步的，所述微波介质材料的晶相为ErVO4，其晶体结构为四方锆石结构。
进一步的，所述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：按照ErVO4的摩尔比，以分析纯Er2O3、V2O5为原料进行配料；
步骤2：以去离子水和锆球为球磨介质，将混合料在尼龙罐中球磨6～7小时，球磨后出料置于110℃烘箱中干燥；
步骤3：对干燥料进行过筛，然后置于坩埚中在800℃预烧3～4小时，得到预烧料；
步骤4：以去离子水和锆球为球磨介质，将预烧料在尼龙罐中球磨4～6小时，球磨后出料置于110℃烘箱中干燥；
步骤5：将干燥料与聚乙烯醇(PVA)溶液混合、造粒，在10～20MPa干压得到生坯；
步骤6：将生坯在1100～1250℃烧结5～6小时，得到所述微波介质材料。
本发明的有益效果在于：
本发明提供一种微波介质材料ErVO4，在1100～1250℃烧结拥有优良的微波介电性能：介电常数εr为11.42～12.03、Q×f值20268～25549GHz、谐振频率温度系数τf为-67.49～-46.35ppm/℃。
本发明提供一种微波介质材料ErVO4，为单一晶相ErVO4，晶体结构为四方锆石结构；Q×f值与堆积分数和晶粒尺寸密切相关，在1150℃烧结的ErVO4晶粒尺寸均匀性好，堆积分数高，此时Q×f值最高；谐振频率温度系数τf与V-O键、Er-O键的键价密切相关，在1200℃烧结的ErVO4 V-O键、Er-O键的键价最大，此时τf最小，稳定性最佳。
附图说明
图1为实施例3制备的微波介质材料ErVO4的XRD图。
图2为实施例3制备的微波介质材料ErVO4的SEM图。
具体实施方案
下面结合附图和实施例对本发明做进一步详细说明。
本发明提供4个实施例，每个实施例的微波介质材料配方为ErVO4，烧结温度为1100～1250℃，均采用以下方法进行制备：
步骤1：按照ErVO4的摩尔比，以分析纯Er2O3、V2O5为原料进行配料；
步骤2：以去离子水和锆球为球磨介质，将混合料在尼龙罐中球磨6～7小时，球磨后出料置于110℃烘箱中干燥；
步骤3：对干燥料进行过筛，然后置于坩埚中在800℃预烧3～4小时，得到预烧料；
步骤4：以去离子水和锆球为球磨介质，将预烧料在尼龙罐中球磨4～6小时，球磨后出料置于110℃烘箱中干燥；
步骤5：将干燥料与聚乙烯醇(PVA)溶液混合、造粒，在10～20MPa干压得到生坯；
步骤6：将生坯在1100～1250℃烧结5～6小时，得到所述微波介质材料。
以上4个实施例的具体工艺参数及微波介电性能如下表所示：
编号 烧结温度(℃) 烧结时间(h) εr Q×f值(GHz) τf(ppm/℃)
实施例1 1100 5 11.42 21883 -67.49
实施例2 1150 5 12.03 25549 -52.89
实施例3 1200 5 11.54 24216 -46.35
实施例4 1250 5 11.61 20268 -50.35
由上表可见，本发明提供一种微波介质材料ErVO4，在1100～1250℃烧结拥有优良的微波介电性能：介电常数εr为11.42～12.03、Q×f值20268～25549GHz、谐振频率温度系数τf为-67.49～-46.35ppm/℃。
由图1可见，实施例2制备的微波介质材料ErVO4的XRD图，与四方锆石结构ErV O4的衍射花样完全匹配，表明是纯相ErVO4。如图2所示，实施例2制备的微波介质材料ErV O4的SEM图，在1150℃烧结时，晶粒排列致密，晶粒尺寸均匀，Q×f值最优。
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 (1)

1.一种微波陶瓷材料，其特征在于，所述微波陶瓷材料的化学式为ErVO4；所述微波陶瓷材料的晶相为ErVO4，属于四方锆石结构；所述微波陶瓷材料的介电常数εr值为11.42～12.03、Q×f值为20268～25549GHz、谐振频率温度系数τf为-67.49～-46.35ppm/℃；所述微波介质材料的制备方法，包括以下步骤：
步骤1：按照ErVO4的摩尔比，以分析纯Er2O3、V2O5为原料进行配料；
步骤2：以去离子水和锆球为球磨介质，将混合料在尼龙罐中球磨6～7小时，球磨后出料置于110℃的烘箱中干燥；
步骤3：对干燥料进行过筛，然后置于坩埚中在800℃预烧3～4小时，得到预烧料；
步骤4：以去离子水和锆球为球磨介质，将预烧料在尼龙罐中球磨4～6小时，球磨后出料置于110℃的烘箱中干燥；
步骤5：将干燥料与聚乙烯醇PVA溶液混合、造粒，在10～20MPa干压得到生坯；
步骤6：将生坯在1100～1250℃烧结5～6小时，得到所述微波介质材料。
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