CN110066169B - 一种氧化硅基低介电常数微波介质陶瓷及制备方法 - Google Patents
一种氧化硅基低介电常数微波介质陶瓷及制备方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 59
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
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- 238000000498 ball milling Methods 0.000 claims description 28
- 238000005245 sintering Methods 0.000 claims description 27
- 229910052681 coesite Inorganic materials 0.000 claims description 15
- 229910052906 cristobalite Inorganic materials 0.000 claims description 15
- 229910052682 stishovite Inorganic materials 0.000 claims description 15
- 229910052905 tridymite Inorganic materials 0.000 claims description 15
- 239000011230 binding agent Substances 0.000 claims description 11
- 238000005303 weighing Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 6
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- 238000004891 communication Methods 0.000 abstract description 3
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- 239000013078 crystal Substances 0.000 description 7
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
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- 229910002367 SrTiO Inorganic materials 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种氧化硅基低介电常数微波介质陶瓷及制备方法，其化学组成的表达式为xZnO‑yAl2O3‑mSiO2‑nSrTiO3，其中38mol％≤x≤64mol％，6mol％≤y≤9mol％，26mol％≤m≤50mol％，0≤n≤7mol％，x+y+m+n＝1。其制备方法包括以下步骤：(1)陶瓷中间体粉料的制备；(2)xZnO‑yAl2O3‑mSiO2‑nSrTiO3陶瓷的制备。本发明的微波介质陶瓷的介电常数为6.4～8.2，品质因数大于9,346GHz，谐振频率温度系数较小。本发明的微波介质陶瓷在与微波通讯领域相关的工业生产活动中具有巨大应用价值。
Description
技术领域
本发明涉及微波介质陶瓷材料，特别涉及一种低介电常数微波介质陶瓷及制备方法。
背景技术
近年来，第五代移动通讯技术(5G)、自动驾驶技术等均要求设备工作在较高频段以提供更宽的带宽，因此对于高频下高性能材料产生大量需求。微波介质陶瓷是指在微波频段(频率范围300MHz～300GHz，波长10-3m～1m)的电路中作为介质基板、填充材料等的陶瓷。它可应用在移动电话、电视卫星、射频电子标签(RFID)和军事雷达等通讯设备中。在微波设备中，降低基板介电常数可以提高信号传输速率，降低基板介电损耗可以降低微波电路的损耗，降低基板谐振频率温度系数可以使设备在变化的环境中正常工作，将基板材料的介电常数做成系列化可满足不同高频设备对尺寸的不同要求。微波介质陶瓷在介电常数稳定性和介电损耗方面的性能远优于商业化的高分子材料。因此，开发高性能微波介质陶瓷是提高微波设备性能的最佳途径之一。
目前市场上使用的微波介质陶瓷基板材料主要是Al2O3陶瓷，Al2O3陶瓷材料具有很高的品质因数，但是其介电常数相对较高(εr＝10)，烧结温度也较高(1500℃～1800℃)。
CN105399413A公开了一种低介电常数、低损耗的微波介质陶瓷及制备方法，陶瓷主晶向结构为：xZnO-yMgO-zB2O3，其中1≤x≤3,0.2≤y≤1,1≤z≤3；烧结助剂为5～20wt％的SiO2，1～4wt％的TiO2，5～15wt％的Al2O3。当主晶向为2ZnO-MgO-2B2O3，并添加了15wt％SiO2、2wt％TiO2、5wt％Al2O3后，其微波性能为：介电常数εr＝6.2，介电损耗tanδ＝0.0001，谐振频率温度系数τf＝3ppm/℃。
SiO2是目前已知的介电常数最低的陶瓷材料(εr≈3.8)，但是SiO2存在多种高低温晶型，高温晶型向低温晶型转变时会伴随着较大的体积变化，导致难以制备成无裂纹的致密陶瓷，向SiO2中直接添加烧结助剂会引起介电常数大幅提升。虽然高纯致密的SiO2陶瓷难以制备，但是具有一定比例SiO2的性能良好的SiO2基微波介质陶瓷材料在一定条件可以制备出来。在微波介质陶瓷材料中，铝酸盐系的ZnAl2O4陶瓷微波介电性能：εr＝8.5，Q×f＝56,319GHz，τf＝-79ppm/℃，硅酸盐系的Zn2SiO4的介电常数微波介电性能：εr＝6.6，Q×f＝219,000GHz，τf＝-61ppm/℃。二者均具备良好的微波介电性能。在相图中ZnAl2O4-Zn2SiO4-SiO2的最低共熔点为1305℃，有望抑制SiO2晶型转变，实现陶瓷的致密烧结。
发明内容
为了克服现有技术的上述缺点与不足，本发明的目的在于提供一种低介电常数微波介质陶瓷的制备方法，制备工艺简单。
本发明的另一目的在于提供一种低介电常数微波介质陶瓷，具有介电常数低，品质因数高，谐振频率温度系数较小的特性。
本发明的目的通过以下技术方案实现。
一种氧化硅基低介电常数微波介质陶瓷，其化学组成的表达式为xZnO-yAl2O3-mSiO2-nSrTiO3，其中38mol％≤x≤64mol％，6mol％≤y≤9mol％，26mol％≤m≤50mol％，0≤n≤7mol％，x+y+m+n＝1。
本发明还提供了一种如上所述氧化硅基低介电常数微波介质陶瓷的制备方法，包括如下步骤：
(1)按化学组成的表达式xZnO-yAl2O3-mSiO2的化学计量比称取ZnO、Al2O3、SiO2，混合，球磨，烘干，预烧后得xZnO-yAl2O3-mSiO2陶瓷中间体粉料；
(2)按所述陶瓷的化学组成的表达式xZnO-yAl2O3-mSiO2-nSrTiO3的化学计量比称取xZnO-yAl2O3-mSiO2陶瓷中间体粉料和SrTiO3粉料，混合，球磨，烘干，添加粘结剂造粒，模压成型，烧结，得所述微波介质陶瓷。
优选地，步骤(1)所述的ZnO、Al2O3、SiO2的纯度为99％以上。
优选地，步骤(1)所述的球磨为湿式球磨，球磨时间为30～120分钟。
优选地，步骤(1)中的预烧温度为1100～1200℃，预烧的气氛为空气，预烧的时间为1～6小时。
优选地，步骤(2)中所述的球磨为湿式球磨，球磨时间为30～120分钟。
优选地，步骤(2)中添加的粘结剂的量为xZnO-yAl2O3-mSiO2陶瓷中间体粉料质量的5～10％。
优选地，所述粘结剂为质量浓度5～10％的聚乙烯醇溶液。
优选地，步骤(2)中烧结的温度为1140～1400℃，烧结的气氛为空气气氛，烧结的时间为1～6小时。
优选地，步骤(1)和步骤(2)中所述的球磨采用的是行星球磨仪。
与现有技术相比，本发明具有以下优点和有益效果：
(1)本发明的微波介质陶瓷，具有低介电常数(6.4～8.2)，高品质因数(>9,346GHz)，较小谐振频率温度系数；
(2)本发明的微波介质陶瓷，可在1140～1400℃烧结；
(3)本发明制备的低介电常数微波介质陶瓷使用清洁无污染的常见元素，不含昂贵的稀土元素，原材料价格低廉。
附图说明
图1为0.64ZnO-0.09Al2O3-0.27SiO2的XRD图；
图2为0.62ZnO-0.09Al2O3-0.27SiO2-0.02SrTiO3的XRD图。
具体实施方式
下面结合实施例，对本发明作进一步地详细说明，但本发明的实施方式不限于此实施例。
表3为化学组成表达式xZnO-yAl2O3-mSiO2-nSrTiO3的介质陶瓷的微波介电性能表，式中x、y、m、n分别表示ZnO、Al2O3、SiO2、SrTiO3的摩尔数比，各实施例中的x、y、m、n取值见表3。
(1)按化学组成的表达式xZnO-yAl2O3-mSiO2的化学计量比称取纯度为99.9％的ZnO、Al2O3、SiO2原料粉末，行星球磨(溶剂为酒精，转速为300转/分钟)，烘干后在空气气氛中预烧，得xZnO-yAl2O3-mSiO2陶瓷中间体粉末，其物相如图1(以实施例1制得的0.64ZnO-0.09Al2O3-0.27SiO2为例)所示。其中，行星球磨是在球磨罐中球磨，球磨罐材质为聚四氟乙烯，球磨介质为1mm二氧化锆小球，溶剂为酒精，其中球磨介质、原料粉末和酒精的质量比为1:1:1。其中各实施例的球磨时间，预烧温度，预烧时间见表1
表1
(2)按陶瓷的化学组成的表达式为xZnO-yAl2O3-mSiO2-nSrTiO3的化学计量比称取xZnO-yAl2O3-mSiO2陶瓷中间体粉料和纯度为99.5％的SrTiO3粉料，其中x、y、m、n的取值按照表3。将xZnO-yAl2O3-mSiO2陶瓷中间体粉料和SrTiO3粉料混合后，得粉料，将粉料进行行星球磨(溶剂为酒精，其中球磨介质、粉料和酒精的质量比为1:1:1，转速为300转/分钟)。向烘干过筛后的粉料，添加粘结剂造粒，通过单轴加压制成直径8mm，厚度4mm的圆柱状生坯，最后的空气气氛中烧结，烧结后陶瓷的物相如图2所示(以实施例2制得的0.62ZnO-0.09Al2O3-0.27SiO2-0.02SrTiO3为例)，上述的粘结剂采用质量浓度p为5～10％的聚乙烯醇溶液，使用剂量w占称取的xZnO-yAl2O3-mSiO2陶瓷中间体粉料质量的5～10％。其中步骤(2)中相应的球磨时间，烧结温度，烧结时间和聚乙烯醇溶液的质量浓度和使用剂量见表2。
表2
所获得的微波电介质陶瓷，用网络分析仪E8363B进行性能测试，方法为圆柱介质谐振腔法，获得的介电性能如表3。
表3
本发明的微波介质陶瓷体系介电常数较低且可系列化、品质因数高、谐振频率温度系数可调到近零。本发明所用原料清洁绿色、不含稀土元素，价格低廉环境友好。所获微波介质陶瓷，可应用于毫米波通讯系统中的介质谐振器、滤波器、震荡器、介质波导、微带天线等微波元器件中。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受所述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。
Claims (6)
1.一种氧化硅基低介电常数微波介质陶瓷，其特征在于，其化学组成的表达式为xZnO-yAl2O3-mSiO2-nSrTiO3，其中38mol%≤x≤54mol%，6mol%≤y≤8mol%，36mol%≤m≤50mol%，0＜n≤7mol%，x+y+m+n=1；
所述氧化硅基低介电常数微波介质陶瓷的制备方法包括如下步骤：
（1）按化学组成的表达式xZnO-yAl2O3-mSiO2的化学计量比称取ZnO、Al2O3、SiO2，混合，球磨，烘干，预烧后得xZnO-yAl2O3-mSiO2陶瓷中间体粉料；
（2）按所述微波介质陶瓷的化学组成的表达式xZnO-yAl2O3-mSiO2-nSrTiO3的化学计量比称取xZnO-yAl2O3-mSiO2陶瓷中间体粉料和SrTiO3粉料，混合，球磨，烘干，添加粘结剂造粒，模压成型，烧结，得所述微波介质陶瓷；
步骤（1）中的预烧温度为1100~1200℃，预烧的气氛为空气，预烧的时间为1~6小时；
步骤（2）中烧结的温度为1180~1300℃，烧结的气氛为空气气氛，烧结的时间为1~6小时；
步骤（2）中添加的粘结剂的量为xZnO-yAl2O3-mSiO2陶瓷中间体粉料质量的5～10％；
所述粘结剂为质量浓度5～10％的聚乙烯醇溶液。
2.一种如权利要求1所述氧化硅基低介电常数微波介质陶瓷的制备方法，其特征在于，包括如下步骤：
（1）按化学组成的表达式xZnO-yAl2O3-mSiO2的化学计量比称取ZnO、Al2O3、SiO2，混合，球磨，烘干，预烧后得xZnO-yAl2O3-mSiO2陶瓷中间体粉料；
（2）按所述微波介质陶瓷的化学组成的表达式xZnO-yAl2O3-mSiO2-nSrTiO3的化学计量比称取xZnO-yAl2O3-mSiO2陶瓷中间体粉料和SrTiO3粉料，混合，球磨，烘干，添加粘结剂造粒，模压成型，烧结，得所述微波介质陶瓷；
步骤（1）中的预烧温度为1100~1200℃，预烧的气氛为空气，预烧的时间为1~6小时；
步骤（2）中烧结的温度为1180~1300℃，烧结的气氛为空气气氛，烧结的时间为1~6小时；
步骤（2）中添加的粘结剂的量为xZnO-yAl2O3-mSiO2陶瓷中间体粉料质量的5～10％；
所述粘结剂为质量浓度5～10％的聚乙烯醇溶液。
3.根据权利要求2所述的氧化硅基低介电常数微波介质陶瓷的制备方法，其特征在于，步骤（1）所述的ZnO、Al2O3、SiO2的纯度为99％以上。
4.根据权利要求2所述的氧化硅基低介电常数微波介质陶瓷的制备方法，其特征在于，步骤（1）所述的球磨为湿式球磨，球磨时间为30~120分钟。
5.根据权利要求2所述的氧化硅基低介电常数微波介质陶瓷的制备方法，其特征在于，步骤（2）中所述的球磨为湿式球磨，球磨时间为30~120分钟。
6.根据权利要求2所述的氧化硅基低介电常数微波介质陶瓷的制备方法，其特征在于，步骤（1）和步骤（2）中所述的球磨采用的是行星球磨仪。
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