CN110092655A - 一种钡钐钛系低损耗微波介质陶瓷及其制备方法 - Google Patents
一种钡钐钛系低损耗微波介质陶瓷及其制备方法 Download PDFInfo
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- 239000010936 titanium Substances 0.000 title claims abstract description 62
- 239000000919 ceramic Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 229910052788 barium Inorganic materials 0.000 title claims abstract description 29
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 title claims abstract description 29
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 28
- 239000004615 ingredient Substances 0.000 claims abstract description 61
- 239000000463 material Substances 0.000 claims abstract description 29
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 20
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 10
- 238000000498 ball milling Methods 0.000 claims description 22
- 238000007873 sieving Methods 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 17
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- 238000005245 sintering Methods 0.000 claims description 12
- 239000010431 corundum Substances 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000005469 granulation Methods 0.000 claims description 7
- 230000003179 granulation Effects 0.000 claims description 7
- 239000011812 mixed powder Substances 0.000 claims description 7
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims description 7
- 239000008187 granular material Substances 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000009702 powder compression Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims 1
- 231100000252 nontoxic Toxicity 0.000 abstract description 4
- 230000003000 nontoxic effect Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 4
- LYLNLPRRNKLKSP-UHFFFAOYSA-N [Ti].[Sm].[Ba] Chemical compound [Ti].[Sm].[Ba] LYLNLPRRNKLKSP-UHFFFAOYSA-N 0.000 description 3
- 238000004891 communication Methods 0.000 description 3
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- 238000010295 mobile communication Methods 0.000 description 2
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 210000000540 fraction c Anatomy 0.000 description 1
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- BYUJNNSZGXHGPB-UHFFFAOYSA-N samarium titanium Chemical compound [Ti][Sm] BYUJNNSZGXHGPB-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种钡钐钛系低损耗微波介质陶瓷,该微波介质陶瓷是由主料和辅料复合而成,主料的组成表达式为Ba7‑xSm(8+2x/3)Ti30O79,其中,0.01≤x≤0.06,所述辅料为Cu‑ZnO、Al2O3和MnO2,其中,Cu‑ZnO相对于主料的质量分数为a,1%≤a≤5%,Al2O3相对于主料的质量分数为b,0%≤b≤5%,MnO2相对于主料的质量分数为c,0%≤c≤0.5%。本发明还公开了该钡钐钛系低损耗微波介质陶瓷的制备方法。本发明的微波介质陶瓷具有优异的微波介电性能,且制备原料无毒又价格低廉,制备工艺简单,具有广泛的应用前景。
Description
技术领域
本发明属于电子陶瓷及其制备技术领域,具体地,涉及一种钡钐钛系低损耗微波介质陶瓷及其制备方法。
背景技术
微波是指波长从lm~lmm(相应频率为300MHz~300GHz)的电磁波,它具有波长短、频率高、量子特性明显等特征微波技术是本世纪内得到迅速发展的一门技术,广泛应用于雷达、导航、多路通讯、遥感及电视等方面。
微波陶瓷介质在介质谐振器、介质滤波器、介质天线等微波通信元器件中的应用,使实现无线通信设备小型化和低成本化成为了现实。如今,微波介质陶瓷广泛应用于微波和移动通信领域,研制拥有自主知识产权的微波介质陶瓷新材料,已经成为事关国家长远发展和国家安全的战略性、前沿性和前瞻性高技术问题。近年来,随着5G移动通信、卫星通信、无线网络、全球卫星定位系统、蓝牙等技术的快速发展,微波器件正朝着小型化、高频化和轻量化方向发展,对微波介质陶瓷材料提出了更高的要求:介电常数系列化,以满足不同通信频段器件的需求;Q×f值越高越好,以减少微波元器件的损耗;频率温度系数尽可能小,以减少微波元器件性能随外界环境的变化的影响。因此高介电常数、高品质因数、频率温度系数接近零且烧结温度低是微波介质陶瓷的重点研究发展方向。对于Ba-Sm2O3-TiO2体系陶瓷烧结温度通常大于1350℃,而且损耗较大,这些阻碍了它的大规模实际应用。
发明内容
为解决上述技术问题,本发明的目的在于提供一种钡钐钛系低损耗微波介质陶瓷及其制备方法,该微波介质陶瓷具有优异的微波介电性能,制备原料无毒且价格低廉,制备工艺简单,具有广泛的应用前景。
为实现上述技术目的,达到上述技术效果,本发明通过以下技术方案实现:一种钡钐钛系低损耗微波介质陶瓷,其是由主料和辅料复合而成,主料的组成表达式为Ba7- xSm(8+2x/3)Ti30O79,其中,0.01≤x≤0.06,所述辅料为Cu-ZnO、Al2O3和MnO2,其中,Cu-ZnO相对于主料的质量分数为a,1%≤a≤5%,Al2O3相对于主料的质量分数为b,0%≤b≤5%,MnO2相对于主料的质量分数为c,0%≤c≤0.5%。
其中,辅料中的Cu-ZnO是通过CuO和ZnO按照1:1的摩尔比配制而成。
作为本发明优选的技术方案,各个辅料相对于主料的质量分数中,1%≤a≤5%,1%≤b≤5%,0.1%≤c≤0.5%。
本发明还提供了一种钡钐钛系低损耗微波介质陶瓷的制备方法,具体的,包括以下步骤:
(1)制备微波介质陶瓷的主料:按照组成表达式Ba7-xSm(8+2x/3)Ti30O79中各元素的摩尔比对BaCO3、Sm2O3、TiO2进行配料,混合充分后进行球磨,球磨后烘干、过筛,然后放入刚玉坩埚中进行焙烧,得到主料,其中,在Ba7-xSm(8+2x/3)Ti30O79中,0.01≤x≤0.06;
(2)制备Cu-ZnO辅料:将ZnO和CuO混合充分后球磨,球磨后烘干、过筛,再放入刚玉坩埚中进行焙烧,得到Cu-ZnO辅料;
(3)制备钡钐钛系低损耗微波介质陶瓷:按照质量百分比分别称取步骤(1)制备的Ba7-xSm(8+2x/3)Ti30O79、步骤(2)制备的Cu-ZnO、Al2O3和MnO2,将主料和所有辅料进行混合,然后充分球磨,再经过烘干、造粒和过筛,将过筛后的混合粉料压制成型,最后烧结得到该钡钐钛系低损耗微波介质陶瓷;其中,Cu-ZnO相对于主料的质量分数为a,1%≤a≤5%,Al2O3相对于主料的质量分数为b,0%≤b≤5%,MnO2相对于主料的质量分数为c,0%≤c≤0.5%。
作为本发明优选的技术方案,步骤(1)中的焙烧过程为在1100~1180℃下焙烧保温3~5小时。
作为本发明优选的技术方案,步骤(2)中的CuO和ZnO的配比为1:1。
作为本发明优选的技术方案,步骤(2)中的焙烧过程为在580~650℃下焙烧保温3~5小时。
作为本发明优选的技术方案,步骤(3)中的的烧结过程为在1200~1280℃下烧结4小时。
作为本发明优选的技术方案,步骤(3)中所述的造粒是将烘干后的粉体与聚乙烯醇水溶液混合,然后制成微米级的球形颗粒。
作为本发明优选的技术方案,步骤(3)中,过筛后的混合粉料被压制成直径为10mm、高度为6mm的圆柱体。
与现有技术相比,本发明具有的以下有益效果:本发明的微波介质陶瓷在制备时采用Cu-ZnO作为助烧剂,并添加适量Al2O3,以增加陶瓷烧结的致密性,从而减少缺陷;而钡钐钛系陶瓷损耗大的一个重要原因是Ti4+的还原,因此本发明添加少量MnO2作为抗还原剂来降低陶瓷损耗;本发明微波介质陶瓷的烧结温度低,Q值达到12000~25500GHz,谐振频率温度系数达到1.5~3.8ppm/℃;该钡钐钛系低损耗微波介质陶瓷具有优异的微波介电性能,所用制备原料无毒且价格低廉,制备工艺简单,具有广泛的应用前景。
具体实施方式
下面对本发明的较佳实施例进行详细阐述,以使本发明的优点和特征能更易于被本领域技术人员理解,从而对本发明的保护范围做出更为清楚明确的界定。
本发明提供了一种钡钐钛系低损耗微波介质陶瓷,其是由主料和辅料复合而成,主料的组成表达式为Ba7-xSm(8+2x/3)Ti30O79,其中,0.01≤x≤0.06,所述辅料为Cu-ZnO、Al2O3和MnO2,其中,Cu-ZnO相对于主料的质量分数为a,1%≤a≤5%,Al2O3相对于主料的质量分数为b,0%≤b≤5%,MnO2相对于主料的质量分数为c,0%≤c≤0.5%。
其中,辅料中的Cu-ZnO是通过CuO和ZnO按照1:1的摩尔比配制而成。
作为本发明优选的技术方案,各个辅料相对于主料的质量分数中,1%≤a≤5%,1%≤b≤5%,0.1%≤c≤0.5%。
本发明还提供了一种钡钐钛系低损耗微波介质陶瓷的制备方法,具体的,包括以下步骤:
(1)制备微波介质陶瓷的主料:按照组成表达式Ba7-xSm(8+2x/3)Ti30O79中各元素的摩尔比对BaCO3、Sm2O3、TiO2进行配料,混合充分后进行球磨,球磨后烘干、过筛,然后放入刚玉坩埚中进行焙烧,得到主料,其中,在Ba7-xSm(8+2x/3)Ti30O79中,0.01≤x≤0.06;
(2)制备Cu-ZnO辅料:将ZnO和CuO混合充分后球磨,球磨后烘干、过筛,再放入刚玉坩埚中进行焙烧,得到Cu-ZnO辅料;
(3)制备钡钐钛系低损耗微波介质陶瓷:按照质量百分比分别称取步骤(1)制备的Ba7-xSm(8+2x/3)Ti30O79、步骤(2)制备的Cu-ZnO、Al2O3和MnO2,将主料和所有辅料进行混合,然后充分球磨,再经过烘干、造粒和过筛,将过筛后的混合粉料压制成型,最后烧结得到该钡钐钛系低损耗微波介质陶瓷。
其中,步骤(1)中的焙烧过程为在1100~1180℃下焙烧保温3~5小时。
其中,步骤(2)中的CuO和ZnO的配比为1:1;再者,步骤(2)中的焙烧过程为在580~650℃下焙烧保温3~5小时。
其中,步骤(3)中的的烧结过程为在1200~1280℃下烧结4小时;再者,步骤(3)中所述的造粒是将烘干后的粉体与聚乙烯醇水溶液混合,然后制成微米级的球形颗粒;另外,步骤(3)中,过筛后的混合粉料被压制成直径为10mm、高度为6mm的圆柱体。
以下的实施例将对本发明作进一步的说明,但并不因此限制本发明。
首先,制备微波介质陶瓷的主料。
实施例1
在本实施例1的组成表达式Ba7-xSm(8+2x/3)Ti30O79中,x=0.01,从而,按照组成表达式Ba6.99Sm8.007Ti30O79中各元素的摩尔比对BaCO3、Sm2O3、TiO2进行配料,混合充分后进行球磨,球磨后烘干、过筛,然后放入刚玉坩埚中,在1140℃下焙烧保温4小时,得到主料。
实施例2
在本实施例2的组成表达式Ba7-xSm(8+2x/3)Ti30O79中,x=0.02,从而,按照组成表达式Ba6.98Sm8.013Ti30O79中各元素的摩尔比对BaCO3、Sm2O3、TiO2进行配料,混合充分后进行球磨,球磨后烘干、过筛,然后放入刚玉坩埚中,在1140℃下焙烧保温4小时,得到主料。
实施例3
在本实施例3的组成表达式Ba7-xSm(8+2x/3)Ti30O79中,x=0.03,从而,按照组成表达式Ba6.97Sm8.02Ti30O79中各元素的摩尔比对BaCO3、Sm2O3、TiO2进行配料,混合充分后进行球磨,球磨后烘干、过筛,然后放入刚玉坩埚中,在1140℃下焙烧保温4小时,得到主料。
实施例4
在本实施例4的组成表达式Ba7-xSm(8+2x/3)Ti30O79中,x=0.04,即组成表达式为Ba6.96Sm8.027Ti30O79,该主料的制备方法同实施例1。
实施例5
在本实施例5的组成表达式Ba7-xSm(8+2x/3)Ti30O79中,x=0.05,即组成表达式为Ba6.95Sm8.033Ti30O79,该主料的制备方法同实施例1。
实施例6
在本实施例6的组成表达式Ba7-xSm(8+2x/3)Ti30O79中,x=0.06,即组成表达式为Ba6.94Sm8.04Ti30O79,该主料的制备方法同实施例1。
对比例
在对比例的组成表达式Ba7-xSm(8+2x/3)Ti30O79中,x=0,从而,按照组成表达式Ba7Sm8Ti30O79中各元素的摩尔比对BaCO3、Sm2O3、TiO2进行配料,混合充分后进行球磨,球磨后烘干、过筛,然后放入刚玉坩埚中,在1140℃下焙烧保温4小时,得到主料。
对实施例1至6和对比例制备的主料进行性能测试,具体测试结果见表1。
表1实施例1至6和对比例制备的主料的性能测试结果
根据性能测试结构,选取最优的技术方案实施例2,即主料的组成表达式为Ba6.98Sm8.013Ti30O79。
然后,按1:1的配比称取ZnO和CuO,混合充分后球磨,球磨后烘干、过筛,再放入刚玉坩埚中,在600℃下焙烧保温4小时,得到Cu-ZnO辅料。
下面制备本发明的钡钐钛系低损耗微波介质陶瓷。
实施例7
按照质量百分比分别称取主料Ba6.98Sm8.013Ti30O79、辅料Al2O3、辅料MnO2以及制备的辅料Cu-ZnO,其中,Cu-ZnO相对于主料Ba6.98Sm8.013Ti30O79的质量分数a为1%,Al2O3相对于主料Ba6.98Sm8.013Ti30O79的质量分数b为0%,MnO2相对于主料Ba6.98Sm8.013Ti30O79的质量分数c为0%,将主料和所有辅料进行混合,然后充分球磨,再经过烘干、造粒和过筛,将过筛后的混合粉料压制成直径为10mm、高度为6mm的圆柱体,最后在1260℃下烧结保温4个小时,得到该钡钐钛系低损耗微波介质陶瓷。
本发明还提供了实施例8至20,实施例8至20的制备方法与实施例7类似,不同的是各个质量分数a、b、c的取值,具体的各个实施例中a、b、c的取值见表2。
对实施例7至20所制备的钡钐钛系低损耗微波介质陶瓷进行性能测试,其性能测试结果见表2。
表2实施例7至20所制备的微波介质陶瓷的性能测试结果
由表2中实施例7-20的结果比较可知,优选实施例18,即最终制备的钡钐钛系低损耗微波介质陶瓷的组成表达式为Ba6.98Sm8.013Ti30O79-4%(Cu-ZnO)-3%Al2O3-0.3%MnO2。该微波介质陶瓷的介电常数为61.7,品质因数Q为25500GHZ,谐振频率温度系数为2.333ppm/℃;该微波介质陶瓷的烧结温度低,Q值达到25500GHz,谐振频率温度系数达到2.333ppm/℃,具有优异的微波介电性能,且所用制备原料无毒又价格低廉,制备工艺简单,具有广泛的应用前景。
以上所述仅为本发明的实施例,并非因此限制本发明的专利范围,凡是利用本发明说明书内容所作的等效结构或等效流程变换,或直接或间接运用在其他相关的技术领域,均同理包括在本发明的专利保护范围内。
Claims (10)
1.一种钡钐钛系低损耗微波介质陶瓷,其特征在于:该微波介质陶瓷是由主料和辅料复合而成,主料的组成表达式为Ba7-xSm(8+2x/3)Ti30O79,其中,0.01≤x≤0.06,所述辅料为Cu-ZnO、Al2O3和MnO2,其中,Cu-ZnO相对于主料的质量分数为a,1%≤a≤5%,Al2O3相对于主料的质量分数为b,0%≤b≤5%,MnO2相对于主料的质量分数为c,0%≤c≤0.5%。
2.根据权利要求1所述的钡钐钛系低损耗微波介质陶瓷,其特征在于:辅料中的Cu-ZnO是通过CuO和ZnO按照1:1的摩尔比配制而成。
3.根据权利要求1所述的钡钐钛系低损耗微波介质陶瓷,其特征在于:各个辅料相对于主料的质量分数中,1%≤a≤5%,1%≤b≤5%,0.1%≤c≤0.5%。
4.一种钡钐钛系低损耗微波介质陶瓷的制备方法,其特征在于,包括以下步骤:
(1)制备微波介质陶瓷的主料:按照组成表达式Ba7-xSm(8+2x/3)Ti30O79中各元素的摩尔比对BaCO3、Sm2O3、TiO2进行配料,混合充分后进行球磨,球磨后烘干、过筛,然后放入刚玉坩埚中进行焙烧,得到主料,其中,在Ba7-xSm(8+2x/3)Ti30O79中,0.01≤x≤0.06;
(2)制备Cu-ZnO辅料:将ZnO和CuO混合充分后球磨,球磨后烘干、过筛,再放入刚玉坩埚中进行焙烧,得到Cu-ZnO辅料;
(3)制备钡钐钛系低损耗微波介质陶瓷:按照质量百分比分别称取步骤(1)制备的Ba7- xSm(8+2x/3)Ti30O79、步骤(2)制备的Cu-ZnO、Al2O3和MnO2,将主料和所有辅料进行混合,然后充分球磨,再经过烘干、造粒和过筛,将过筛后的混合粉料压制成型,最后烧结得到该钡钐钛系低损耗微波介质陶瓷;其中,Cu-ZnO相对于主料的质量分数为a,1%≤a≤5%,Al2O3相对于主料的质量分数为b,0%≤b≤5%,MnO2相对于主料的质量分数为c,0%≤c≤0.5%。
5.根据权利要求4所述的钡钐钛系低损耗微波介质陶瓷的制备方法,其特征在于,步骤(1)中的焙烧过程为在1100~1180℃下焙烧保温3~5小时。
6.根据权利要求4所述的钡钐钛系低损耗微波介质陶瓷的制备方法,其特征在于,步骤(2)中的CuO和ZnO的配比为1:1。
7.根据权利要求4所述的钡钐钛系低损耗微波介质陶瓷的制备方法,其特征在于,步骤(2)中的焙烧过程为在580~650℃下焙烧保温3~5小时。
8.根据权利要求4所述的钡钐钛系低损耗微波介质陶瓷的制备方法,其特征在于,步骤(3)中的的烧结过程为在1200~1280℃下烧结4小时。
9.根据权利要求4所述的钡钐钛系低损耗微波介质陶瓷的制备方法,其特征在于,步骤(3)中所述的造粒是将烘干后的粉体与聚乙烯醇水溶液混合,然后制成微米级的球形颗粒。
10.根据权利要求4所述的钡钐钛系低损耗微波介质陶瓷的制备方法,其特征在于,步骤(3)中,过筛后的混合粉料被压制成直径为10mm、高度为6mm的圆柱体。
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Inventor after: Ji An Inventor after: Wang Dan Inventor before: Ji An Inventor before: Wang Dan Inventor before: Wang Xiaohui |
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CB03 | Change of inventor or designer information |