CN110357628A - 一种Ca5Mg4-xCox(VO4)6低温烧结微波陶瓷材料及其制备方法 - Google Patents

一种Ca5Mg4-xCox(VO4)6低温烧结微波陶瓷材料及其制备方法 Download PDF

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CN110357628A
CN110357628A CN201910707555.2A CN201910707555A CN110357628A CN 110357628 A CN110357628 A CN 110357628A CN 201910707555 A CN201910707555 A CN 201910707555A CN 110357628 A CN110357628 A CN 110357628A
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李波
刘伟
张树人
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University of Electronic Science and Technology of China
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Abstract

本发明属于功能陶瓷领域，具体提供一种Ca5Mg4‑xCox(VO4)6低温烧结微波陶瓷材料及其制备方法；本发明所述微波陶瓷材料的化学式为Ca5Mg4‑xCox(VO4)6，其中，0<x≤2，主晶相为Ca5Mg4(VO4)6，能在775℃～800℃烧结。本发明有效解决了微波陶瓷材料烧结温度普遍过高的问题，并通过一定量的Co离子替代Mg离子，与Mg离子共占B位，微观上提高了原子堆积率和阳离子有序度，宏观上提高了该微波陶瓷材料微波介电性能，尤其提高了材料的Q×f值，特别是x＝1时，获得了如下性能：εr＝9.65、Q×f＝54685GHz、τf＝‑55.3ppm/℃，同时，本发明制备方法简易，原材料成本低，具有较高的实际应用价值。

Description

一种Ca5Mg4-xCox(VO4)6低温烧结微波陶瓷材料及其制备方法
技术领域
本发明属于功能陶瓷领域，具体涉及一种Ca5Mg4-xCox(VO4)6低温烧结微波陶瓷材料及其制备方法。
技术背景
微波陶瓷材料在现代通信中扮演着重要的角色，已被用移动电话、卫星、雷达等许多领域。实际应用中的微波陶瓷通常需要具有良好的微波介电性能、尽量低的烧结温度，为满足后者，国内外研究常采用助烧剂降烧的方法，但此方法会带来更为繁琐的制备工艺以及更为高昂的成本。因此，开发微波介电性能良好且本征烧结温度低的微波陶瓷材料的重要性越为明显。
石榴石型钒酸盐的发现满足了以上需要，Guo-guang Yao等人采用传统固相法在875℃的烧结温度下制备出Ca5Mn4(VO4)6微波陶瓷，并得到如下微波介电性能：εr＝11.2，Q×f＝33800GHz，τf＝-70ppm/℃(J Mater Sci:Mater Electron 27:7292-7296(2016))；进一步的，G uo-guang Yao等人在800℃的烧结温度下制备出Ca5Mg4(VO4)6微波陶瓷，其性能为εr＝9.2、Q×f＝53300GHz、τf＝-50ppm/℃(J.Am.Ceram.Soc.,96[6]:1691–1693(2013))；上述材料因其较低的烧结温度而具有很高的研究价值，但在实际制备过程中，由于V2O5的熔点较低，易在预烧以及烧结过程中挥发，并形成难以控制的钒缺位和气孔，影响了材料的微波介电性能，尤其是降低了品质因数Q×f。
基于上述背景，本发明提供一种Ca5Mg4-xCox(VO4)6低温烧结微波陶瓷材料及其制备方法。
发明内容
本发明目的在于提供一种Ca5Mg4-xCox(VO4)6低温烧结微波陶瓷材料及其制备方法，用以解决微波陶瓷材料烧结温度普遍过高的问题，并通过一定量的Co离子替代Mg离子，与Mg离子共占B位，改善了材料的原子堆积率，提高了阳离子有序度，获得了明显的性能提升。
为实现以上目的，本发明采用的技术方案为：
一种Ca5Mg4-xCox(VO4)6低温烧结微波陶瓷材料，其特征在于，所述微波陶瓷材料的化学式为：Ca5Mg4-xCox(VO4)6，其中，0<x≤2。
进一步的，所述微波陶瓷材料的主晶相为Ca5Mg4(VO4)6；晶体结构为A3B2V3O12型立方石榴石结构，其中，Ca占A位，Mg、Co共占B位。
所述微波陶瓷材料烧结温度为750℃～800℃，介电常数约为9.5～10.5，Q×f值为47000～55000GHz，谐振频率温度系数为-60ppm/℃～-50ppm/℃。
上述低温烧结微波陶瓷材料的制备方法，其特征在于，包括步骤如下：
(1)按照化学式Ca5Mg4-xCox(VO4)6的摩尔配比，以CaCO3、Mg(OH)2、CoO、V2O5为原料进行配料，得到混合料；
(2)以锆球为磨球、以去离子水为球磨介质，将混合料球磨6～8小时，后将浆料烘干、研磨、过筛，得到干燥粉体；
(3)将干燥粉体置于700℃的条件下预烧2～4小时，得到预烧料；
(4)将预烧料在相同条件下进行二次球磨并烘干，得到二次球磨料；
(5)将二次球磨料与聚乙烯醇溶液混合进行造粒，并在20MPa下干压成型，得到生坯；
(6)将生坯置于750℃～800℃空气中烧结6～8小时，得到所述低温烧结微波陶瓷材料。
本发明的有益效果在于：
(1)本发明提供的微波陶瓷材料主晶相为Ca5Mg4(VO4)6，相较于B位由单一离子占位的A3B2V3O12型钒酸盐体系微波陶瓷，本发明中用一定量的Co离子取代Mg离子，与Mg离子共占B位，微观上提高了原子堆积率和阳离子有序度，宏观上提高了该微波陶瓷材料的微波介电性能，尤其当x＝1时，获得了如下性能：εr＝9.65、Q×f＝54685GHz、τf＝-55.3ppm/℃；
(2)本发明不使用任何降烧方法，成相稳定，本征烧结温度为775℃～800℃，实现了低温烧结；
(3)本发明提供的微波陶瓷材料制备工艺简单，一定程度上简化了工业化生产流程、降低了生产成本。
附图说明
图1为本发明实施例2制备得的Ca5Mg4-xCox(VO4)6低温烧结微波陶瓷材料的SEM图。
图2为本发明实施例2制备得的Ca5Mg4-xCox(VO4)6低温烧结微波陶瓷材料的XRD图。
具体实施方式
下面结合附图和实施例对本发明进一步详细说明。
实施例1
依据微波陶瓷材料Ca5Mg4-xCox(VO4)6(x＝0.5)的化学计量配比，称取CaCO3、Mg(OH)2、CoO、V2O5共30g，与30g去离子水、150g锆球一同置于球磨罐中球磨7h；将球磨所得浆料放入温度为100℃的烘箱中烘干，后研磨、过筛；将所得均匀分散的粉体置于烧结炉中，在700℃下预烧3h；将所得预烧料再次球磨7h，后烘干、造粒，所用粘结剂为质量浓度为5％的聚乙烯醇溶液，并经干压成型后得生坯；将生坯置于800℃下烧结7h，制备得低温烧结微波陶瓷材料，测试得其微波介电性能如下：εr＝9.73、Q×f＝47751GHz、τf＝-55.9ppm/℃。
实施例2
依据微波陶瓷材料Ca5Mg4-xCox(VO4)6(x＝1)的化学计量配比，称取CaCO3、Mg(OH)2、CoO、V2O5共30g，与30g去离子水、150g锆球一同置于球磨罐中球磨7h；将球磨所得浆料放入温度为100℃的烘箱中烘干，后研磨、过筛；将所得均匀分散的粉体置于烧结炉中，在700℃下预烧3h；将所得预烧料再次球磨7h，后烘干、造粒，所用粘结剂为质量浓度为5％的聚乙烯醇溶液，并经干压成型后得生坯；将生坯置于800℃下烧结7h，制备得低温烧结微波陶瓷材料，测试得其微波介电性能如下：εr＝9.65、Q×f＝54685GHz、τf＝-55.3ppm/℃。
实施例3
依据微波陶瓷材料Ca5Mg4-xCox(VO4)6(x＝1.5)的化学计量配比，称取CaCO3、Mg(OH)2、CoO、V2O5共30g，与30g去离子水、150g锆球一同置于球磨罐中球磨7h；将球磨所得浆料放入温度为100℃的烘箱中烘干，后研磨、过筛；将所得均匀分散的粉体置于烧结炉中，在700℃下预烧3h；将所得预烧料再次球磨7h，后烘干、造粒，所用粘结剂为质量浓度为5％的聚乙烯醇溶液，并经干压成型后得生坯；将生坯置于775℃下烧结7h，制备得低温烧结微波陶瓷材料，测试得其微波介电性能如下：εr＝10.05、Q×f＝47534GHz、τf＝-55.9ppm/℃。
实施例4
依据微波陶瓷材料Ca5Mg4-xCox(VO4)6(x＝2)的化学计量配比，称取CaCO3、Mg(OH)2、CoO、V2O5共30g，与30g去离子水、150g锆球一同置于球磨罐中球磨7h；将球磨所得浆料放入温度为100℃的烘箱中烘干，后研磨、过筛；将所得均匀分散的粉体置于烧结炉中，在700℃下预烧3h；将所得预烧料再次球磨7h，后烘干、造粒，所用粘结剂为质量浓度为5％的聚乙烯醇溶液，并经干压成型后得生坯；将生坯置于775℃下烧结7h，制备得低温烧结微波陶瓷材料，测试得其微波介电性能如下：εr＝10.26、Q×f＝47874GHz、τf＝-55.2ppm/℃。
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 (4)

1.一种Ca5Mg4-xCox(VO4)6低温烧结微波陶瓷材料，其特征在于，所述微波陶瓷材料的化学式为：Ca5Mg4-xCox(VO4)6，其中，0<x≤2。
2.按权利要求1所述Ca5Mg4-xCox(VO4)6低温烧结微波陶瓷材料，其特征在于，所述微波陶瓷材料的主晶相为Ca5Mg4(VO4)6；晶体结构为A3B2V3O12型立方石榴石结构，其中，Ca占A位，Mg、Co共占B位。
3.按权利要求1所述Ca5Mg4-xCox(VO4)6低温烧结微波陶瓷材料，其特征在于，所述微波陶瓷材料烧结温度为750℃～800℃，介电常数约为9.5～10.5，Q×f值为47000～55000GHz，谐振频率温度系数为-60ppm/℃～-50ppm/℃。
4.按权利要求1所述Ca5Mg4-xCox(VO4)6低温烧结微波陶瓷材料的制备方法，其特征在于，包括步骤如下：
(1)按照化学式Ca5Mg4-xCox(VO4)6的摩尔配比，以CaCO3、Mg(OH)2、CoO、V2O5为原料进行配料，得到混合料；
(2)以锆球为磨球、以去离子水为球磨介质，将混合料球磨6～8小时，后将浆料烘干、研磨、过筛，得到干燥粉体；
(3)将干燥粉体置于700℃的条件下预烧2～4小时，得到预烧料；
(4)将预烧料在相同条件下进行二次球磨并烘干，得到二次球磨料；
(5)将二次球磨料与聚乙烯醇溶液混合进行造粒，并在20MPa下干压成型，得到生坯；
(6)将生坯置于750℃～800℃空气中烧结6～8小时，得到所述低温烧结微波陶瓷材料。
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