CN105712711A - 一种高性能微波介质陶瓷材料及其制备方法 - Google Patents

一种高性能微波介质陶瓷材料及其制备方法 Download PDF

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CN105712711A
CN105712711A CN201610039081.5A CN201610039081A CN105712711A CN 105712711 A CN105712711 A CN 105712711A CN 201610039081 A CN201610039081 A CN 201610039081A CN 105712711 A CN105712711 A CN 105712711A
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龙梅
苗峰
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Southwest Minzu University
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Abstract

本发明公开了一种高性能微波介质陶瓷材料及其制备方法，该陶瓷材料由以下重量份的原料制备而成：ZrO2 2030份、BaCO3 2535份、Nb2O5 13份、无机纳米粒子3035份、导热填料1020份、红外反射二氧化钛0.55.5份、光稳定剂0.21.0份、金属纳米级添加剂15份、耐化学品改性剂0.55份、其他助剂0.52.0份；所述耐化学品改性剂为含氟类添加剂，分子量为100010000，可以为液体或固体形态存在。本发明制备工艺简单，制备所得的材料稳定性好，具有优良的耐候性，介电常数大，Qf值高，谐振频率温度系数近零可调，成本低，且易于大批量生产。

Description

一种高性能微波介质陶瓷材料及其制备方法
技术领域
本发明涉及微波材料领域，具体涉及一种高性能微波介质陶瓷材料及其制备方法。
背景技术
随着移动通信的发展，微波元器件的小型化、集成化、高频率化和低成本化已成为发展趋势。微波介质陶瓷材料由于具有较高的介电常数、低介电损耗和稳定的谐振频率温度系数而成为微波元器件发展的关键材料之一。理论及实验均证明，以微波介质陶瓷制作的各种微波器件，如介质谐振器、滤波器及微波介质天线等广泛应用于微波技术的各个领域。
介质谐振器通常具有无载品质因数高、频率温度系数小且可调、体积不大等特点，因而受到越来越广泛的应用。相应的微波介质陶瓷材料必须同时具有(1)较高的介电常数(30-60)、(2)高的品质因数(Qf≥40000GHz)、(3)近零可调的谐振频率温度系数。
虽然介质的介电常数越高，谐振器和滤波器的尺寸可以越小。但是这种情况下介质的介电常数过大，介质谐振器中电磁场集中于介质内，导致谐振器的耦合太弱而使滤波器的带宽变小。而且介质材料的Qf值与介电常数成反比，通常介电常数大于60且谐振频率温度系数近零的介质材料其Qf值不超过30000GHz。
目前现代通信行业的发展趋势对介质材料提出的要求是在满足介电常数较大与谐振频率温度系数近零可调的同时，要尽可能的提高Qf值，同时要降低成本，提高产品性能的稳定性和重复性。
发明内容
本发明的目的在于针对上述现有技术存在的问题，提供一种高性能微波介质陶瓷材料及其制备方法，制备工艺简单，制备所得的材料稳定性好，具有优良的耐候性，介电常数大，Qf值高，谐振频率温度系数近零可调，成本低，且易于大批量生产。
为实现上述目的，本发明采取的技术方案是：
一种高性能微波介质陶瓷材料，由以下重量份的原料制备而成：
ZrO2 20-30份、BaCO3 25-35份、Nb2O5 1-3份、无机纳米粒子30-35份、导热填料10-20份、红外反射二氧化钛0.5-5.5份、光稳定剂0.2-1.0份、金属纳米级添加剂1-5份、耐化学品改性剂0.5-5份、其他助剂0.5-2.0份；
所述耐化学品改性剂为含氟类添加剂，分子量为1000-10000，可以为液体或固体形态存在。
优选地，所述无机纳米粒子为纳米二氧化硅。
优选地，所述含氟类添加剂为含有全氟烷基的丙烯酸系添加剂。
优选地，所述导热填料由为氧化镁、氧化锌、氢氧化铝、氮化硼按质量比1∶2∶3∶1混合所得，所述导热填料的粒径在0.5um-2.0um，纯度大于96％。
优选地，所述光稳定剂为水杨酸酯、苯并三唑类的UV吸收剂、受阻胺类自由基捕捉剂中的一种或两种混合物。
优选地，所述金属纳米级添加剂Zn、Zr、Mn、Mg、Ni或Co中的一种或多种；其中Zn为1.5-2.5wt/％，Zr为0-2.5wt/％，Mn为0-2wt/％，Mg为0-1.5wt/％，Ni为0-1wt/％，Co为0-1.5wt/％。
优选地，其他助剂选偶联剂、抗氧剂、阻燃剂和润滑剂中的至少两种的混合物。
为解决上述问题，本发明还提供了一种高性能微波介质陶瓷材料的制备方法，包括如下步骤：
S1、按上述一种高性能微波介质陶瓷材料的配方分别称取各组分；
S2、将S1步骤中称取的ZrO2、BaCO3、Nb2O5、在球磨机中球磨成料浆；
S3、将无机纳米粒子通过超声波振荡设备分散于纯净水中形成无机纳米粒子分散液与步骤S1所得的料浆混合后，在120℃下烘干，得混合物A；；
S3、将步骤S2得到的混合物与称取的导热填料、红外反射二氧化钛、光稳定剂、耐化学品改性剂和其他助剂，置于高速搅拌机中搅拌5-30min后，出料得到混合物B；；
S4、将所得的混合物B过30-40目筛，并在1100-1300℃下煅烧3-5小时后冷却得到陶瓷粉体；
S5、将所得陶瓷粉体中加入金属纳米级添加剂再倒入球磨机中，加入水和锆球，球磨成料浆后，100-120℃喷雾干燥后，过80-250目过筛，添加聚乙烯醇溶液后经过双螺杆挤出机挤出造粒，挤出机的温度为180-220℃，严格真空度大于0.09Mpa，螺杆转速为180-200转/分；
S6、将造粒后的粉料装入模具在110-120MPa的压力下干压成型；然后将成型后的陶瓷生坯除去粘结剂，最后以5-10℃/min的升温速率在1400-1550℃下烧结2-12小时后，随炉冷却得到烧结好的高性能微波介质陶瓷材料。
优选地，去除粘结剂是800-1000℃下以升温速率为5-10℃/min加热2小时去除。
本发明具有以下有益效果：
制备工艺简单，制备所得的材料稳定性好，具有优良的耐候性，介电常数大，Qf值高，谐振频率温度系数近零可调，成本低，且易于大批量生产，所得材料可作为微波移动通讯用滤波器、谐振器、振荡器和电容器等电子元器件的关键核心材料，广泛应用于卫星通信、移动通信、全球卫星定位系统、蓝牙技术以及无线局域网等现代通信行业，具有重要的工业应用价值。
具体实施方式
为使本发明要解决的技术问题、技术方案和优点更加清楚，下面将结合具体实施例进行详细描述。
以下实施例中所使用的导热填料由为氧化镁、氧化锌、氢氧化铝、氮化硼按质量比1∶2∶3∶1混合所得，所述导热填料的粒径在0.5um-2.0um，纯度大于96％。所使用的光稳定剂为水杨酸酯、苯并三唑类的UV吸收剂、受阻胺类自由基捕捉剂中的一种或两种混合物。所使用的金属纳米级添加剂Zn、Zr、Mn、Mg、Ni或Co中的一种或多种；其中Zn为1.5-2.5wt/％，Zr为0-2.5wt/％，Mn为0-2wt/％，Mg为0-1.5wt/％，Ni为0-1wt/％，Co为0-1.5wt/％。所使用的其他助剂选偶联剂、抗氧剂、阻燃剂和润滑剂中的至少两种的混合物。
实施例1
S1、称取ZrO2 20份、BaCO3 25份、Nb2O5 1份、纳米二氧化硅30份、导热填料10份、红外反射二氧化钛0.5份、光稳定剂0.2份、金属纳米级添加剂1份、全氟烷基的丙烯酸系添加剂0.5份、其他助剂0.5份；
S2、将S1步骤中称取的ZrO2、BaCO3、Nb2O5、在球磨机中球磨成料浆；
S3、将无机纳米粒子通过超声波振荡设备分散于纯净水中形成无机纳米粒子分散液与步骤S1所得的料浆混合后，在120℃下烘干，得混合物A；；
S3、将步骤S2得到的混合物与称取的导热填料、红外反射二氧化钛、光稳定剂、耐化学品改性剂和其他助剂，置于高速搅拌机中搅拌5min后，出料得到混合物B；；
S4、将所得的混合物B过30目筛，并在1100℃下煅烧3小时后冷却得到陶瓷粉体；
S5、将所得陶瓷粉体中加入金属纳米级添加剂再倒入球磨机中，加入水和锆球，球磨成料浆后，100℃喷雾干燥后，过80目过筛，添加聚乙烯醇溶液后经过双螺杆挤出机挤出造粒，挤出机的温度为180℃，严格真空度大于0.09Mpa，螺杆转速为180转/分；
S6、将造粒后的粉料装入模具在110MPa的压力下干压成型；然后将成型后的陶瓷生坯除去粘结剂，最后以5℃/min的升温速率在1400℃下烧结12小时后，随炉冷却得到烧结好的高性能微波介质陶瓷材料。
实施例2
S1、称取ZrO2 30份、BaCO3 35份、Nb2O5 3份、纳米二氧化硅35份、导热填料20份、红外反射二氧化钛5.5份、光稳定剂1.0份、金属纳米级添加剂5份、全氟烷基的丙烯酸系添加剂5份、其他助剂2.0份；
S2、将S1步骤中称取的ZrO2、BaCO3、Nb2O5、在球磨机中球磨成料浆；
S3、将无机纳米粒子通过超声波振荡设备分散于纯净水中形成无机纳米粒子分散液与步骤S1所得的料浆混合后，在120℃下烘干，得混合物A；；
S3、将步骤S2得到的混合物与称取的导热填料、红外反射二氧化钛、光稳定剂、耐化学品改性剂和其他助剂，置于高速搅拌机中搅拌30min后，出料得到混合物B；；
S4、将所得的混合物B过40目筛，并在1300℃下煅烧5小时后冷却得到陶瓷粉体；
S5、将所得陶瓷粉体中加入金属纳米级添加剂再倒入球磨机中，加入水和锆球，球磨成料浆后，120℃喷雾干燥后，过250目过筛，添加聚乙烯醇溶液后经过双螺杆挤出机挤出造粒，挤出机的温度为220℃，严格真空度大于0.09Mpa，螺杆转速为200转/分；
S6、将造粒后的粉料装入模具在120MPa的压力下干压成型；然后将成型后的陶瓷生坯除去粘结剂，最后以10℃/min的升温速率在1550℃下烧结2小时后，随炉冷却得到烧结好的高性能微波介质陶瓷材料。
实施例3
S1、称取ZrO2 25份、BaCO3 30份、Nb2O5 2份、纳米二氧化硅32.5份、导热填料15份、红外反射二氧化钛6份、光稳定剂0.6份、金属纳米级添加剂3份、全氟烷基的丙烯酸系添加剂2.75份、其他助剂1.25份；
S2、将S1步骤中称取的ZrO2、BaCO3、Nb2O5、在球磨机中球磨成料浆；
S3、将无机纳米粒子通过超声波振荡设备分散于纯净水中形成无机纳米粒子分散液与步骤S1所得的料浆混合后，在120℃下烘干，得混合物A；；
S3、将步骤S2得到的混合物与称取的导热填料、红外反射二氧化钛、光稳定剂、耐化学品改性剂和其他助剂，置于高速搅拌机中搅拌17.5min后，出料得到混合物B；；
S4、将所得的混合物B过35目筛，并在1200℃下煅烧4小时后冷却得到陶瓷粉体；
S5、将所得陶瓷粉体中加入金属纳米级添加剂再倒入球磨机中，加入水和锆球，球磨成料浆后，110℃喷雾干燥后，过165目过筛，添加聚乙烯醇溶液后经过双螺杆挤出机挤出造粒，挤出机的温度为200℃，严格真空度大于0.09Mpa，螺杆转速为190转/分；
S6、将造粒后的粉料装入模具在115MPa的压力下干压成型；然后将成型后的陶瓷生坯除去粘结剂，最后以7.5℃/min的升温速率在1475℃下烧结7小时后，随炉冷却得到烧结好的高性能微波介质陶瓷材料。
以上所述是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明所述原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (9)

1.一种高性能微波介质陶瓷材料，其特征在于，由以下重量份的原料制备而成：
ZrO220-30份、BaCO325-35份、Nb2O51-3份、无机纳米粒子30-35份、导热填料10-20份、红外反射二氧化钛0.5-5.5份、光稳定剂0.2-1.0份、金属纳米级添加剂1-5份、耐化学品改性剂0.5-5份、其他助剂0.5-2.0份；
所述耐化学品改性剂为含氟类添加剂，分子量为1000-10000，可以为液体或固体形态存在。
2.根据权利要求1所述的一种高性能微波介质陶瓷材料，其特征在于，所述无机纳米粒子为纳米二氧化硅。
3.根据权利要求1所述的一种高性能微波介质陶瓷材料，其特征在于，所述含氟类添加剂为含有全氟烷基的丙烯酸系添加剂。
4.根据权利要求1所述的一种高性能微波介质陶瓷材料，其特征在于，所述导热填料由为氧化镁、氧化锌、氢氧化铝、氮化硼按质量比1∶2∶3∶1混合所得，所述导热填料的粒径在0.5um-2.0um，纯度大于96％。
5.根据权利要求1所述的一种高性能微波介质陶瓷材料，其特征在于，所述光稳定剂为水杨酸酯、苯并三唑类的UV吸收剂、受阻胺类自由基捕捉剂中的一种或两种混合物。
6.根据权利要求1所述的一种高性能微波介质陶瓷材料，其特征在于，所述金属纳米级添加剂Zn、Zr、Mn、Mg、Ni或Co中的一种或多种；其中Zn为1.5-2.5wt/％，Zr为0-2.5wt/％，Mn为0-2wt/％，Mg为0-1.5wt/％，Ni为0-1wt/％，Co为0-1.5wt/％。
7.根据权利要求1所述的一种高性能微波介质陶瓷材料，其特征在于，其他助剂选偶联剂、抗氧剂、阻燃剂和润滑剂中的至少两种的混合物。
8.一种高性能微波介质陶瓷材料的制备方法，其特征在于，包括如下步骤：
S1、按照权利要求1-7所述一种高性能微波介质陶瓷材料的配方分别称取各组分；
S2、将S1步骤中称取的ZrO2、BaCO3、Nb2O5、在球磨机中球磨成料浆；
S3、将无机纳米粒子通过超声波振荡设备分散于纯净水中形成无机纳米粒子分散液与步骤S1所得的料浆混合后，在120℃下烘干，得混合物A；；
S3、将步骤S2得到的混合物与称取的导热填料、红外反射二氧化钛、光稳定剂、耐化学品改性剂和其他助剂，置于高速搅拌机中搅拌5-30min后，出料得到混合物B；；
S4、将所得的混合物B过30-40目筛，并在1100-1300℃下煅烧3-5小时后冷却得到陶瓷粉体；
S5、将所得陶瓷粉体中加入金属纳米级添加剂再倒入球磨机中，加入水和锆球，球磨成料浆后，100-120℃喷雾干燥后，过80-250目过筛，添加聚乙烯醇溶液后经过双螺杆挤出机挤出造粒，挤出机的温度为180-220℃，严格真空度大于0.09Mpa，螺杆转速为180-200转/分；
S6、将造粒后的粉料装入模具在110-120MPa的压力下干压成型；然后将成型后的陶瓷生坯除去粘结剂，最后以5-10℃/min的升温速率在1400-1550℃下烧结2-12小时后，随炉冷却得到烧结好的高性能微波介质陶瓷材料。
9.根据权利要求8所述的一种高性能微波介质陶瓷材料的制备方法，其特征在于，去除粘结剂是800-1000℃下以升温速率为5-10℃/min加热2小时去除。
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1179405A (zh) * 1997-11-04 1998-04-22 胡勇波 锆镁质钢化瓷
CN1634800A (zh) * 2003-12-30 2005-07-06 广东风华高新科技集团有限公司 超低温烧结的陶瓷介质材料、其制备方法及所得的电容器
US20070106043A1 (en) * 2004-03-24 2007-05-10 Masayoshi Horiuchi Method of producing acrylic copolymer
CN103304226A (zh) * 2013-05-15 2013-09-18 江苏中电联瑞玛节能技术有限公司 蓄热陶瓷材料及其制备方法
CN104341144A (zh) * 2013-08-01 2015-02-11 北京元六鸿远电子技术有限公司 低温烧结c0g特性微波介质材料及其制备方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1179405A (zh) * 1997-11-04 1998-04-22 胡勇波 锆镁质钢化瓷
CN1634800A (zh) * 2003-12-30 2005-07-06 广东风华高新科技集团有限公司 超低温烧结的陶瓷介质材料、其制备方法及所得的电容器
US20070106043A1 (en) * 2004-03-24 2007-05-10 Masayoshi Horiuchi Method of producing acrylic copolymer
CN103304226A (zh) * 2013-05-15 2013-09-18 江苏中电联瑞玛节能技术有限公司 蓄热陶瓷材料及其制备方法
CN104341144A (zh) * 2013-08-01 2015-02-11 北京元六鸿远电子技术有限公司 低温烧结c0g特性微波介质材料及其制备方法

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