CN108455986B - 一种复合微波介质陶瓷材料及其制备方法 - Google Patents
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 12
- 239000002131 composite material Substances 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 6
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- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000010532 solid phase synthesis reaction Methods 0.000 claims abstract description 4
- 239000010936 titanium Substances 0.000 claims description 26
- 239000011701 zinc Substances 0.000 claims description 26
- 239000010955 niobium Substances 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
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- 239000008187 granular material Substances 0.000 claims description 2
- 238000005469 granulation Methods 0.000 claims description 2
- 230000003179 granulation Effects 0.000 claims description 2
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 2
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- 239000012071 phase Substances 0.000 abstract description 19
- 239000000919 ceramic Substances 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000003990 capacitor Substances 0.000 abstract description 2
- 229910019792 NbO4 Inorganic materials 0.000 description 12
- 150000002500 ions Chemical class 0.000 description 7
- 239000012535 impurity Substances 0.000 description 4
- 238000006467 substitution reaction Methods 0.000 description 4
- 238000012876 topography Methods 0.000 description 4
- 238000013329 compounding Methods 0.000 description 2
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- 230000007423 decrease Effects 0.000 description 2
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- 238000005457 optimization Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明属于电子陶瓷及其制造领域,具体涉及一种复合微波介质陶瓷材料及其制备方法。该材料化学式为Zn0.15+0.35xTi0.55‑0.05xNb0.3+0.7xO2+2x(x=0.2‑0.8mol),其原料组成为ZnO、TiO2、Nb2O5,通过固相法制得;具有中等介电常数(40‑84),低损耗(1.10×10‑4‑3.02×10‑4),频率温度系数近零。通过调节x数值调节两相的含量,在保证低的烧结温度的同时,起到改善微波介电性能的作用。适用于多层介质谐振器、微波天线、微波电容器、滤波器等微波器件的制造。
Description
技术领域
本发明属于电子陶瓷及其制造领域,具体涉及一种复合微波介质陶瓷材料及其制备方法。
背景技术
微波介质陶瓷是指应用于微波(300MHz到300GHz)频段电路中作为介质材料并实现一种或多种功能的陶瓷材料,是现代通信技术中的基础。微波介质陶瓷现已被广泛应用于介质谐振器、滤波器、介质基片、介质波导回路、微波电容、双工器、天线等微波元器件。
微波介质陶瓷的实际应用应当满足以下要求:(1)介电常数适中以利于器件的小型化;(2)高的品质因数Q×f值和低的损耗(其中Q~1/tanδ,f是谐振频率);(3)近零的谐振频率温度系数。
Zn0.5Ti0.5NbO4陶瓷具有良好的微波介电性能:εr=34、Q×f=42500GHz,烧结温度适中(1100℃-1200℃),但τf=-52ppm/℃,较大的谐振频率温度稳定系数限制了其应用。在大量文献报道中发现,对Zn0.5Ti0.5NbO4进行性能改善主要通过离子掺杂以及复合两种方法。
对Zn0.5Ti0.5NbO4进行离子掺杂不会大幅提高烧结温度,但离子掺杂后体系的品质因数Q×f值欠佳。如Zn位被Ca2+、Co2+离子取代,Ti位被Zr4+、Sn4+离子取代,Nb位被Ta5+取代,超过一定取代量均会导致Zn0.15Nb0.3Ti0.55O2相的出现,该相作为离子掺杂过程中引入的杂质相,因此未被引起重视。
对Zn0.5Ti0.5NbO4进行复合可以大幅改善体系介电常数、品质因数以及谐振频率温度稳定系数,但是体系烧结致密所需的烧结温度过高。如利用TiO2进行复合,TiO2烧结温度为1400℃,耗能较大并且对设备要求较高。
发明内容
针对上述存在问题或不足,为解决在保证Zn0.5Ti0.5NbO4陶瓷的应用前提下,其参数优化以及制备温度的问题;本发明提供了一种复合微波介质陶瓷材料及其制备方法。
该复合微波介质陶瓷材料化学式为Zn0.15+0.35xTi0.55-0.05xNb0.3+0.7xO2+2x(x=0.2-0.8mol),其原料组成为ZnO、TiO2、Nb2O5,通过固相法制得;具有中等介电常数(40-84),低损耗1.10×10-4-3.02×10-4,频率温度系数近零。
制备上述复合微波介质陶瓷材料的步骤如下:
步骤1:将氧化锌(ZnO)、二氧化钛(TiO2)、氧化铌(Nb2O5)的原始粉料按照化学式Zn0.15+0.35xTi0.55-0.05xNb0.3+0.7xO2+2x(x=0.2-0.8mol)配料。
步骤2:将步骤1制备的配料按照粉料、氧化锆球、去离子水质量比为1:4-5:2-3进行行星球磨,混合4-8小时,取出后在80℃-100℃下烘干,以40-60目筛网过筛,然后在800℃-1000℃大气氛围中预烧3-6小时。
步骤3:再将步骤2预烧后的粉料按照粉料、氧化锆球、去离子水质量比1:4-5:1-2,行星球磨混合2-6小时,取出后在80℃-100℃下烘干,烘干后添加剂量占原料总质量的2~5%的PVA溶液作为粘结剂造粒,压制成型,最后在1100℃-1150℃大气气氛中烧结4-6小时,即制得微波介质陶瓷材料。
本发明将离子掺杂中出现的杂质相直接以复合的方式引入,设计出Zn0.5Ti0.5NbO4相与Zn0.15Nb0.3Ti0.55O2相的复合体系Zn0.15+0.35xTi0.55-0.05xNb0.3+0.7xO2+2x,通过调节x数值调节两相的含量,在保证低的烧结温度的同时,起到改善微波介电性能的作用。本发明利用了Zn0.15Nb0.3Ti0.55O2相这一离子掺杂中的杂质相具有调节介电常数以及谐振频率温度稳定系数的作用,以及适中的烧结温度(1100℃-1200℃)。
综上所述,本发明提供的Zn0.15+0.35xTi0.55-0.05xNb0.3+0.7xO2+2x陶瓷,其烧结温度低,介电常数可调,损耗小,具有优异的微波性能。
附图说明
图1为实施例1-5的XRD衍射花样;
图2(A)为烧结1150℃,x=0.4时样品的表面形貌图,图2(B)为烧结1100℃,x=0.516时样品的表面形貌图。
具体实施方式
下面结合附图和实施例详述本发明。
本发明材料化学式Zn0.15+0.35xTi0.55-0.05xNb0.3+0.7xO2+2x(x=0.2-0.8mol),通过固相法制得本材料,具体步骤同上述步骤一样。
具体实施例的成分和微波介电性能如下
从上表可以看出,随着x的增多,样品的介电常数逐渐降低,品质因数逐渐升高,谐振频率温度稳定系数也从+300左右降低至-77左右,在实施例3中取得了近零的谐振频率温度稳定系数,并且样品保持优异的微波介电性能。
以实施例1、2、3、4、5(No.1-5)为例,其XRD衍射花样如图1所示。
从图中衍射花样的变化可以看出。在实施例1中,样品的衍射花样与Zn0.15Nb0.3Ti0.55O2卡片(JCPDS#79-1186)吻合,未检测到第二相。随着Zn0.5Ti0.5NbO4相含量的增加,样品出现Zn0.5Ti0.5NbO4相(JCPDS#48-0323),并且从右侧局部图的衍射峰相对强度变化可以看出Zn0.5Ti0.5NbO4的30°左右的(111)晶面成为最强衍射峰,说明此时样品的主晶相已经转变为Zn0.5Ti0.5NbO4,并且该相的相含量也逐渐增加。在实施例5中仅检测到Zn0.5Ti0.5NbO4相。
以实施例12、3(No.12、3)为例,其SEM扫描电镜图如图2所示。
图2(A)为烧结1150℃,x=0.4时样品的表面形貌图,图2(B)为烧结1100℃,x=0.516时样品的表面形貌图。从图中可以看出在这两个组分下样品致密,并且(A)图具有较大的平均晶粒尺寸,约为5.37μm。(B)图晶粒尺寸较小,约为1.65μm。
综上可见,本发明将离子掺杂中出现的杂质相直接以复合的方式引入,设计出Zn0.5Ti0.5NbO4相与Zn0.15Nb0.3Ti0.55O2相的复合体系Zn0.15+0.35xTi0.55-0.05xNb0.3+0.7xO2+2x,通过调节x数值调节两相的含量,在保证低的烧结温度的同时,起到改善微波介电性能的作用。
Claims (2)
1.一种复合微波介质陶瓷材料,其特征在于:
化学式为Zn0.15+0.35xTi0.55-0.05xNb0.3+0.7xO2+2x,x=0.2-0.8mol,其原料组成为ZnO、TiO2、Nb2O5,通过固相法制得;介电常数40-84,损耗1.10×10-4-3.02×10-4,频率温度系数近零。
2.如权利要求1所述复合微波介质陶瓷材料的制备方法,具体如下:
步骤1:将氧化锌ZnO、二氧化钛TiO2、氧化铌Nb2O5的原始粉料按照化学式Zn0.15+ 0.35xTi0.55-0.05xNb0.3+0.7xO2+2x,x=0.2-0.8mol配料;
步骤2:将步骤1制备的配料按照粉料、氧化锆球、去离子水质量比为1:4-5:2-3进行行星球磨,混合4-8小时,取出后在80℃-100℃下烘干,以40-60目筛网过筛,然后在800℃-1000℃大气氛围中预烧3-6小时;
步骤3:再将步骤2预烧后的粉料按照粉料、氧化锆球、去离子水质量比1:4-5:1-2,行星球磨混合2-6小时,取出后在80℃-100℃下烘干,烘干后添加剂量占原料总质量的2~5%的PVA溶液作为粘结剂造粒,压制成型,最后在1100℃-1150℃大气气氛中烧结4-6小时,即制得微波介质陶瓷材料。
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