CN112898021A - 一种低温烧结微波介质材料Mg2-xCoxV2O7及其制备方法 - Google Patents

一种低温烧结微波介质材料Mg2-xCoxV2O7及其制备方法 Download PDF

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CN112898021A
CN112898021A CN202110333559.6A CN202110333559A CN112898021A CN 112898021 A CN112898021 A CN 112898021A CN 202110333559 A CN202110333559 A CN 202110333559A CN 112898021 A CN112898021 A CN 112898021A
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李波
曹慧敏
韩如意
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Abstract

本发明属于电子陶瓷及其制造领域，提供一种低温烧结微波介质材料及其制备方法；所述低温烧结微波介质材料为：Mg2‑xCoxV2O7(0.5≤x≤1.0)，其晶相为：Mg2V2O7，晶体结构为：单斜晶体结构、钴离子和镁离子共同占据A位。本发明中，钴离子的加入使微波介质的晶相Mg2V2O7从三斜结构转变为单斜结构，且晶粒长大、原子堆积率提高，从而获得了Q×f值的极大提升；同时，实现了860～870℃的低温烧结，解决了微波介质材料烧结温度偏高的问题。本发明提供低温烧结微波介质材料在860～870℃烧结温度下拥有优良的微波介电性能：介电常数为8～9、Q×f值为66000～72000GHz、谐振频率温度系数为‑30～‑26ppm/℃；并且，该低温烧结微波介质材料制备工艺简单、生产成本低，有利于实现工业化生产。

Description

一种低温烧结微波介质材料Mg2-xCoxV2O7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，涉及微波介质陶瓷Mg2V2O7的掺杂改性，具体涉及一种低温烧结微波介质材料Mg2-xCoxV2O7及其制备方法。
背景技术
低温共烧陶瓷(LTCC)技术已被广泛应用于微波器件制备领域，如移动电话、卫星广播、雷达等。应用于实际的微波介质材料需要具备低介电损耗，适当的介电常数及近零谐振频率温度系数。MgO-V2O5系钒酸盐以其固有烧结温度低、微波性能优良等优点而被广泛关注， Joung等人在期刊Journal of the American Ceramic Society中发表了文章“Formation and Microwave Dielectric Properties of the Mg2V2O7 Ceramics”。文中采用固相反应法在950℃的烧结温度下制得Mg2V2O7微波介质陶瓷，其微波介电性能为εr＝10.5、Q×f＝58275GHz、τf＝-26.9ppm/℃，其烧结温度依然较高，且微波介电性能有待提升。
基于此，本发明提供一种低温烧结微波介质材料Mg2-xCoxV2O7及其制备方法。
发明内容
本发明的目的在于提供了一种低温烧结微波介质材料Mg2-xCoxV2O7及其制备方法，基于微波介质陶瓷Mg2V2O7进行掺杂改性，进而降低烧结温度、提升微波介电性能。
为实现上述目的，本发明采用的技术方案如下：
一种低温烧结微波介质材料，其特征在于，所述微波介质材料的化学式为：Mg2- xCoxV2 O7，其中，0.5≤x≤1.0。
进一步的，所述微波介质材料的晶相为Mg2V2O7；所述微波介质材料的晶体结构为：单斜晶体结构，其中，镁离子与钴离子共同占据A位。
进一步的，所述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：按照Mg2-xCoxV2O7(0.5≤x≤1.0)的摩尔比，以分析纯CoO、MgCO3、V2O5为原料进行配料；
步骤2：以酒精和锆球为球磨介质，将混合料在尼龙罐中球磨4～6小时，球磨后出料置于70℃烘箱中干燥；
步骤3：对干燥料进行过筛，然后置于坩埚中在700～750℃下预烧3～4小时，得到预烧料；
步骤4：以酒精和锆球为球磨介质，将预烧料在尼龙罐中球磨4～6小时，球磨后出料置于70℃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860～870℃的温度烧结5～6小时，得到所述微波陶瓷材料。
本发明的有益效果在于：
1.本发明提供一种低温烧结微波介质材料Mg2-xCoxV2O7(0.5≤x≤1.0)，其晶相为：Mg2V2O7，晶体结构为：单斜晶体结构，钴离子和镁离子共同占据A位；钴离子的加入使该微波介质的晶相Mg2V2O7从三斜结构转变为单斜结构，且晶粒长大，原子堆积率提高，从而获得了Q×f值的极大提升，为实现低温共烧陶瓷(LTCC)技术提供了候选材料；
2.Mg2V2O7和Co2V2O7的晶格类型相同，钴与镁的离子键价相差不大、且离子半径接近，故在该微波介质材料中钴离子与镁离子共同占据A位而形成了固溶体，从而实现了860～870℃的低温烧结，解决了微波介质材料烧结温度偏高的问题。
综上所述，本发明提供低温烧结微波介质材料Mg2-xCoxV2O7(0.5≤x≤1.0)，其在860～870℃烧结温度下拥有优良的微波介电性能：介电常数为8～9、Q×f值66000～72000GHz、谐振频率温度系数为-30～-26ppm/℃，尤其在x＝0.5时，所述低温烧结微波介质材料在870℃烧结温度下微波介电性能为：εr＝8.3、Q×f＝72639GHz、τf＝-29ppm/℃；同时，该低温烧结微波介质材料制备工艺简单、生产成本低，有利于实现工业化生产
附图说明
图1为实施例3制备得微波介质材料Mg2-xCoxV2O7(x＝0.5)的XRD图。
图2为实施例3制备得微波介质材料Mg2-xCoxV2O7(x＝0.5)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3个实施例，每个实施例提供的低温烧结微波介质材料配方为：Mg2- xCox V2O7，其中，x＝0.5、0.75、1.0；所述低温烧结微波陶瓷材料均采用如下方法进行制备：
步骤1：按照Mg2-xCoxV2O7(0.5≤x≤1.0)的摩尔比，以分析纯CoO、MgCO3、V2O5为原料进行配料；
步骤2：以酒精和锆球为球磨介质，将混合料在尼龙罐中球磨4～6小时，球磨后出料置于70℃烘箱中干燥；
步骤3：对干燥料进行过筛，然后置于坩埚中在700～750℃下预烧3～4小时，得到预烧料；
步骤4：以酒精和锆球为球磨介质，将预烧料在尼龙罐中球磨4～6小时，球磨后出料置于70℃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860～870℃的温度烧结5～6小时，得到所述微波陶瓷材料。
以上3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 组成 烧结温度(℃) 烧结时长(h) ε<sub>r</sub> Q×f值(GHz) τ<sub>f</sub>(ppm/℃)
实施例1 x＝0.5 870 5 8.31 72639 -29.6
实施例2 x＝0.75 860 5 8.99 69731 -30.4
实施例3 x＝1.0 870 5 9.21 66463 -26.4
由上表可见，本发明提供低温烧结微波介质材料Mg2-xCoxV2O7(0.5≤x≤1.0)，其在860 ～870℃烧结温度下拥有优良的微波介电性能：介电常数为8～9、Q×f值为66000～72000GHz、谐振频率温度系数为-30～-26ppm/℃。实施例1制备得微波介质材料Mg2-xCoxV2O7(x＝0.5)的X RD图、SEM图分别如图1、图2所示。由图可见，实施例1制备得微波介质材料Mg2-xCox V2O7(x＝0.5)的XRD衍射图样与单斜结构的Mg2V2O7完全匹配，表明了晶相Mg2V2O7从三斜结构向单斜结构的转变；SEM微观形貌显示陶瓷晶粒排列致密，晶粒尺寸明显增大，在低温870℃烧结的基础上，获得了Q×f值的极大提升。
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)

1.一种低温烧结微波介质材料，其特征在于，所述微波介质材料的化学式为：Mg2- xCoxV2O7，其中，0.5≤x≤1.0。
2.按权利要求1所述低温烧结微波介质材料，其特征在于，所述微波介质材料的晶相为Mg2V2O7；所述微波介质材料的晶体结构为：单斜晶体结构，其中镁离子与钴离子共同占据A位。
3.按权利要求1所述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：按照Mg2-xCoxV2O7(0.5≤x≤1.0)的摩尔比，以分析纯CoO、MgCO3、V2O5为原料进行配料；
步骤2：以酒精和锆球为球磨介质，将混合料在尼龙罐中球磨4～6小时，球磨后出料置于70℃烘箱中干燥；
步骤3：对干燥料进行过筛，然后置于坩埚中在700～750℃下预烧3～4小时，得到预烧料；
步骤4：以酒精和锆球为球磨介质，将预烧料在尼龙罐中球磨4～6小时，球磨后出料置于70℃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860～870℃的温度烧结5～6小时，得到所述微波陶瓷材料。
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