CN110357627A - 低温烧结微波介质材料Ca5Ni4-xMgxV6O24及其制备方法 - Google Patents

低温烧结微波介质材料Ca5Ni4-xMgxV6O24及其制备方法 Download PDF

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CN110357627A
CN110357627A CN201910707189.0A CN201910707189A CN110357627A CN 110357627 A CN110357627 A CN 110357627A CN 201910707189 A CN201910707189 A CN 201910707189A CN 110357627 A CN110357627 A CN 110357627A
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李波
冷寒生
张树人
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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材料技术领域，提供低温烧结微波介质材料Ca5Ni4‑xMgxV6O24及其制备方法；所述低温烧结微波介质材料的化学通式为：Ca5Ni4‑xMgxV6O24，其中，0<x≤2；其晶相为A3B2V3O12立方石榴石相，其中，Ca占据A位，Ni、Mg共同占据B位。本发明微波介质材料有着低烧结温度和高Q×f值，具体为：烧结温度为845～900℃，介电常数为8～10，Q×f值为40000～61000GHz，谐振频率温度系数为‑85～‑50ppm/℃；同时，本发明微波介质材料制备工艺简单，原材料价格低廉、储量丰富，使得高性能的微波陶瓷基板实现低成本工业化生产成为可能。

Description

低温烧结微波介质材料Ca5Ni4-xMgxV6O24及其制备方法
技术领域
本发明属于电子陶瓷材料技术领域，具体涉及低温烧结微波介质材料Ca5Ni4- xMgxV6O24及其制备方法。
背景技术
随着微波通信技术的飞速发展，微波介质材料得到了广泛的应用，兼具低温烧结和高性能的微波介质陶瓷逐渐成为研究热点。近年来研究发现钒酸盐微波介质材料具有良好的微波性能同时有着固有烧结温度低的特性；如G.G.Yao等人于2013年在Journalof theAmerican Ceramic Society上发表的文章Novel Series of Low-Firing MicrowaveDielectric Ceramics:Ca5A4(VO4)6(A2+＝Mg,Zn)中报道了两种钒酸盐微波介质陶瓷Ca5Mg4(VO4)6和Ca5Zn4(VO4)6有着良好的微波性能：介电常数为9.2和11.7，Q×f值为53300GHz和49400GHz，谐振频率温度系数τf为-50ppm/℃和-83ppm/℃；于2017年在CeramicsInternational发表的文章Low temperature sintering and microwave dielectricproperties of Ca5Ni4(VO4)6ceramics中报道了Ca5Ni4(VO4)6在875℃下烧结微波性能表现良好：介电常数为9.5，Q×f值为54100GHz，τf为-60ppm/℃。在此基础上，本发明给出了低温烧结微波介质材料Ca5Ni4-xMgxV6O24及其制备方法。
发明内容
本发明目的在于提供一种低温烧结微波介质陶瓷Ca5Ni4-xMgxV6O24及其制备方法，其有着低烧结温度和较高的Q×f值。本发明中微波介质陶瓷化学式为Ca5Ni4-xMgxV6O24，其中0<x≤2，使其达到以下微波性能：烧结温度为845～900℃，介电常数为8～10，Q×f值为40000～61000GHz，谐振频率温度系数为-85～-50ppm/℃。
为实现上述目的，本发明所实施的技术方案为：
低温烧结微波介质材料Ca5Ni4-xMgxV6O24，其特征在于，所述微波介质材料的化学通式为：Ca5Ni4-xMgxV6O24，其中，0<x≤2；所述微波介质材料的晶相为A3B2V3O12立方石榴石相，其中，Ca占据A位，Ni、Mg共同占据B位。
进一步的，所述微波介质材料的烧结温度为845～900℃，介电常数为8～10，Q×f值为40000～61000GHz，谐振频率温度系数为-85～-50ppm/℃。
上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：
(1)配料：采用分析纯CaCO3、NiO、Mg(OH)2、V2O5粉末为原料，按化学组成式Ca5Ni4- xMgxV6O24的摩尔比进行配料，其中，0<x≤2；
(2)一次球磨：将原料混合后置于尼龙罐中，球磨7～9小时，以锆球为磨球，以去离子水为球磨介质，球磨后出料置于烘箱中100℃烘干；
(3)过筛：将干燥料过筛；
(4)预烧：将过筛料置于空气中，以775～800℃焙烧2～4小时，得到预烧料；
(5)二次球磨：将预烧料置于尼龙罐中，球磨7～9小时，球磨后出料置于烘箱中100℃烘干；
(6)造粒成型：将干燥料进行造粒，采用50wt％的丙烯酸溶液作为粘结剂，然后在20～30MPa的压力下压制成生坯；
(7)烧结：将生坯在空气中以845～900℃的温度进行烧结2～5小时，得到所述的微波介质材料。
本发明的有益效果在于：
(1)本发明提供低温烧结微波介质材料Ca5Ni4-xMgxV6O24，能够同时实现低烧结温度和高Q×f值，具体为：烧结温度为845～900℃，介电常数为8～10，Q×f值为40000～61000GHz，谐振频率温度系数为-85～-50ppm/℃；最优的：微波介质材料Ca5Ni2Mg2V6O24在875℃烧结，微波介电性能为：介电常数为8.01、Q×f＝60613GHz、谐振频率温度系数为-67ppm/℃。
(2)本发明涉及的微波介质材料烧结温度低，有利于节约能源；制备工艺简单且无需任何助烧剂，所形成相易于控制，同时使陶瓷保持了优良的微波性能；除此之外，原材料价格低廉、储量丰富，有利于实现高性能微波陶瓷基板的低成本工业化生产。
附图说明
图1为实施例1制备得微波介质材料Ca5Ni4-xMgxV6O24的XRD图。
图2为实施例1制备得微波介质材料Ca5Ni4-xMgxV6O24的SEM图。
具体实施方式
下面结合附图和实施例对本发明进行进一步详细说明。
实施例1～5
上述实施例提供的微波介质材料的化学式分别为：Ca5Ni3MgV6O24、Ca5Ni2.5Mg1.5V6O24Ca5Ni2Mg2V6O24、Ca5Ni2Mg2V6O24、Ca5Ni2Mg2V6O24，制备的具体步骤如下：
(1)配料：采用分析纯CaCO3、NiO、Mg(OH)2、V2O5粉末为原料，按化学组成式Ca5Ni4- xMgxV6O24的摩尔比进行配料，其中，0<x≤2；
(2)一次球磨：将原料混合后置于尼龙罐中，球磨8小时，球磨后出料置于烘箱中100℃烘干；
(3)过筛：将干燥料过60目筛；
(4)预烧：将过筛料置于空气中，以775℃焙烧3小时，得到预烧料；
(5)二次球磨：将预烧料置于尼龙罐中，球磨8小时，球磨后出料置于烘箱中100℃烘干；
(6)造粒成型：将干燥料进行造粒，采用50wt％的丙烯酸溶液作为粘结剂，然后在20MPa的压力下压制成生坯；
(7)烧结：将生坯在空气中以845～900℃的温度进行烧结5小时，得到所述的微波介质材料。
对上述实施例1～5制备得低温烧结微波介质材料进行测试，其微波性能如下表所示：
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.低温烧结微波介质材料Ca5Ni4-xMgxV6O24，其特征在于，所述微波介质材料的化学通式为：Ca5Ni4-xMgxV6O24，其中，0<x≤2；所述微波介质材料的晶相为A3B2V3O12立方石榴石相，其中，Ca占据A位，Ni、Mg共同占据B位。
2.按权利要求1所述低温烧结微波介质材料Ca5Ni4-xMgxV6O24，其特征在于，所述微波介质材料的烧结温度为845～900℃，介电常数为8～10，Q×f值为40000～61000GHz，谐振频率温度系数为-85～-50ppm/℃。
3.按权利要求1所述低温烧结微波介质材料Ca5Ni4-xMgxV6O24的制备方法，其特征在于，包括以下步骤：
(1)配料：采用分析纯CaCO3、NiO、Mg(OH)2、V2O5粉末为原料，按化学组成式Ca5Ni4- xMgxV6O24的摩尔比进行配料，其中，0<x≤2；
(2)一次球磨：将原料混合后置于尼龙罐中，球磨7～9小时，以锆球为磨球，以去离子水为球磨介质，球磨后出料置于烘箱中100℃烘干；
(3)过筛：将干燥料过筛；
(4)预烧：将过筛料置于空气中，以775～800℃焙烧2～4小时，得到预烧料；
(5)二次球磨：将预烧料置于尼龙罐中，球磨7～9小时，球磨后出料置于烘箱中100℃烘干；
(6)造粒成型：将干燥料进行造粒，采用50wt％的丙烯酸溶液作为粘结剂，然后在20～30MPa的压力下压制成生坯；
(7)烧结：将生坯在空气中以845～900℃的温度进行烧结2～5小时，得到所述的微波介质材料。
CN201910707189.0A 2019-08-01 2019-08-01 低温烧结微波介质材料Ca5Ni4-xMgxV6O24及其制备方法 Pending CN110357627A (zh)

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CN108358632A (zh) * 2018-05-24 2018-08-03 电子科技大学 一种超低温烧结高Q×f值微波介质材料及其制备方法
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Application publication date: 20191022