CN114751743A - 一种多层陶瓷电容器用改性Ni-Ti-Ta介质材料及其低温制备方法 - Google Patents
一种多层陶瓷电容器用改性Ni-Ti-Ta介质材料及其低温制备方法 Download PDFInfo
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- 239000003989 dielectric material Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title abstract description 7
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 6
- 229910010293 ceramic material Inorganic materials 0.000 claims description 6
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 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 description 3
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- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 3
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- 229910017676 MgTiO3 Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-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，具体为一种多层陶瓷电容器用改性Ni‑Ti‑Ta介质材料及其低温制备方法，是利用Cu2+离子以及(Al1/ 2Nb1/2)4+离子分别与Ni及Ti元素半径相近，的特点，在Ni0.5Ti0.5TaO4基料中引入复合离子Cu2+、Al3+以及Nb5+离子进行部分取代，显著降低烧结温度的同时提供‑220±30ppm/℃的负介电常数温度系数，并减少由于助烧剂带来的损耗恶化因素，制备出具有低损耗、低成本且具有良好工艺稳定性的应用于射频MLCC的介质材料。
Description
技术领域
本发明属于电子陶瓷及其制造领域，涉及一种多层陶瓷电容器用改性Ni-Ti-Ta介质材料及其低温制备方法。
背景技术
随着5G的快速发展，移动通讯朝向高频发展，电子元器件的集成化、小型化、高性能等要求逐渐提高。多层陶瓷电容器(Multi-layer Ceramic Capacitors，MLCC)具有体积小、比容大、使用寿命长、安全性高以及可应用于高频条件等优点，在通信领域发挥巨大的作用。
MLCC是由内电极、端电极以及陶瓷介质层三部分组成，其中内电极(如Ag/Pt电极)与陶瓷介质互相平行构成主体，端电极一般为三层结构：最内层起链接作用并引出内电极；中间则为阻挡层，主要防止Ag在焊接时被熔融的焊锡腐蚀；最外层为焊接层。陶瓷电容器的分类常以所采用介质陶瓷的介电常数温度系数τε表示。根据美国电子工业协会RS-198标准，陶瓷介质按可温度稳定性通常可分为三大类，I类、Ⅱ类与Ⅲ类陶瓷。其中Ⅰ类陶瓷电容器具有高稳定性及低损耗，在射频及微波通信的应用中最为广泛。其命名规则依据介电常数温度特性而不同，如S2G温度特性的陶瓷电容器指在温度范围内(-55℃～85℃)具有-330±30ppm/℃的温度漂移，该类介质陶瓷电容器可用于制备相控雷达T/R组件、射频功率放大器、发射机等线路中起耦合、协调以及滤波等作用。
常见的I类陶瓷电容器用介质材料以MgO-TiO2以及BaO-TiO2为代表，如MgTiO3以及BaTi4O9，但过高的烧结温度过高(≥1350℃)增加了能耗以及成本，限制了其实际应用。Ni0.5Ti0.5TaO4是一种新型的中介Trirutile结构的材料，其烧结温度为1350℃，介电性能优异：εr～39.8，Q×f～25051GHz。但较高的烧结温度影响其介电性能，从而限制了其具体应用。
发明内容
本发明的目的在于：针对现有Ni0.5Ti0.5TaO4基材料存在的技术问题，提供一种多层陶瓷电容器用改性Ni-Ti-Ta介质材料及其低温制备方法，以克服Ni0.5Ti0.5TaO4基不能兼顾低烧结温度以及优异介电性能的技术问题。
为实现上述目的，本发明采用如下技术方案：
一种多层陶瓷电容器用改性Ni-Ti-Ta介质材料，其化学通式为：
[Cu0.1Ni0.9]0.5[Ti0.92(Al1/2Nb1/2)0.08]0.5TaO4，烧结温度介于1050℃～1150℃。陶瓷材料的晶体结构属于Ni0.5Ti0.5TaO4相固溶体结构，介电常数为34～40，介质损耗为2.8×10-4～3.3×10-4，品质因数Q×f值为22000～25000GHz，介电常数温度系数稳定且满足S2G温度特性(-55℃：-334ppm/℃；85℃：-338ppm/℃)。
作为优选，当烧结温度1150℃时，材料的介电常数为39.8，介质损耗低至2.8×10-4，品质因数Q×f值高达24308GHz，介电常数温度系数稳定且满足R2G温度特性(-55℃：-196ppm/℃；85℃：-202ppm/℃)。
上述多层陶瓷电容器用改性Ni-Ti-Ta介质材料的制备方法，包括以下步骤：
步骤1：将CuO、NiO、TiO2、Al2O3、Nb2O5以及Ta2O5的原始粉料按照化学通式[Cu0.1Ni0.9]0.5[Ti0.92(Al1/2Nb1/2)0.08]0.5TaO4进行配料；
步骤2：将步骤1配好的粉体装入球磨罐并按照粉料：锆球：去离子水的质量比为1:4～6:5～7进行4～6小时的行星球磨，待球磨结束后将混合浆料置于烘箱中烘干，随后以40～200目的筛网过筛；将过筛后的粉体于900～1100℃的大气气氛中预烧3～5小时；
步骤3：将步骤2经预烧后的粉体再次按照粉体：锆球：去离子水质量比为1:4～6:3～5进行4～6小时的行星球磨，待球磨物料烘干后，向其中添加聚乙烯醇溶液进行粘结剂造粒；
步骤4：将步骤3制得的陶瓷生料压制成型，随后以2～5℃/min的升温速率在600～650℃温度下排胶3～5小时，紧接着再以相同速率升温至1050℃～1150℃中保温4～6小时，即可制得改性[Cu0.1Ni0.9]0.5[Ti0.92(Al1/2Nb1/2)0.08]0.5TaO4介质陶瓷材料。
Ni-Ti-Ta陶瓷体系属于Tri-rutile结构，其中Ni与Ta1占据阳离子格位，Ti与Ta2占据另一阳离子格位，由于Cu2+离子以及(Al1/2Nb1/2)4+离子分别与Ni及Ti元素半径相近，因此可以发生取代反应并形成固溶体。由于复合离子掺杂的共同作用，并且得益于CuO降低的烧结温度，Ni-Ti-Ta陶瓷可以在较低的烧结温度下展示优异的微波介电性能。故本发明提供的一种多层陶瓷电容器用改性Ni-Ti-Ta介质材料及其制备方法，采取复合离子掺杂改性工艺，在Ni0.5Ti0.5TaO4基料中引入复合离子Cu2+、Al3+以及Nb5+离子进行部分取代，在显著降低烧结温度的同时提供-220±30ppm/℃的负介电常数温度系数，并减少由于助烧剂带来的损耗恶化因素，制备出具有低损耗、低成本且具有良好工艺稳定性的应用于射频MLCC的介质材料。
附图说明
图1对应实施例3的XRD图谱；
图2对应实施例3的SEM形貌图。
具体实施方式
下面结合附图和实施例对本发明做进一步的详细说明。
步骤1：将CuO、NiO、TiO2、Al2O3、Nb2O5以及Ta2O5的原始粉料按照化学通式[Cu0.1Ni0.9]0.5[Ti0.92(Al1/2Nb1/2)0.08]0.5TaO4进行配料；
步骤2：将步骤1配好的粉体装入球磨罐并按照粉料：锆球：去离子水的质量比为1:6:5进行6小时的行星球磨，待球磨结束后将混合浆料置于烘箱中烘干，随后以200目的筛网过筛。将过筛后的粉体于1000℃的大气气氛中预烧5小时；
步骤3：将步骤2经预烧后的粉体再次按照粉体：锆球：去离子水质量比为1:6:3进行6小时的行星球磨，待球磨物料烘干后，向其中的粉体添加质量百分比为8％的聚乙烯醇溶液作为粘结剂造粒；
步骤4：将步骤3制得的陶瓷生料压制成型，随后以5℃/min的升温速率在650℃温度下排胶4小时，紧接着再以相同速率升温至1050℃～1150℃中保温6小时，即可制得改性[Cu0.1Ni0.9]0.5[Ti0.92(Al1/2Nb1/2)0.08]0.5TaO4介质陶瓷材料。
为更好的阐述本发明的效果，按照上述步骤制作了3份实施例样品。图1为实施例3的XRD衍射图谱，经过检索陶瓷的物相组成与Ni0.5Ti0.5TaO4的标准卡片JCPDS card No.32-0702对应，此时体系中并未发现第二相衍射峰的存在，则说明在该掺杂量下，离子取代并不会引起晶体结构的改变，该类型陶瓷属于Ni0.5Ti0.5TaO4结构。
图2为实施例3的SEM形貌图，在该烧结温度下晶粒生长充分，晶粒尺寸较小，且微观形貌上气孔较少。
各实施例样的成分和微波介电性能如下：
表1为各实施例样品组的成分
表2为各实施例样品的介电性能
从表1、表2展示的数据可以看出在实施例3中，当烧结温度为1150℃时，改性后的[Cu0.1Ni0.9]0.5[Ti0.92(Al1/2Nb1/2)0.08]0.5TaO4陶瓷材料的介电常数与Q×f值取得最佳值：εr＝39.8，tanδ＝2.8×10-4，Q×f＝24308GHz，τε介于-202～-196ppm/℃，与现有文献报道相比烧结温度得到大幅度降低的同时保持了较低的介质损耗，同时介电常数温度系数在-55℃～85℃范围内较稳定，适宜工业应用。
Claims (3)
1.一种多层陶瓷电容器用改性Ni-Ti-Ta介质材料，其特征在于：该改性Ni-Ti-Ta介质材料化学通式为：
[Cu0.1Ni0.9]0.5[Ti0.92(Al1/2Nb1/2)0.08]0.5TaO4，烧结温度介于1050℃～1150℃。陶瓷材料的晶体结构属于Ni0.5Ti0.5TaO4相固溶体结构，介电常数为34～40，介质损耗为2.8×10-4～3.3×10-4，品质因数Q×f值为22000～25000GHz，介电常数温度系数稳定且满足S2G温度特性。
2.根据权利要求1所述的一种多层陶瓷电容器用改性Ni-Ti-Ta介质材料，其特征在于：，当烧结温度1150℃时，材料的介电常数为39.8，介质损耗低至2.8×10-4，品质因数Q×f值高达24308GHz，介电常数温度系数稳定且满足R2G温度特性。
3.根据权利要求1所述的一种多层陶瓷电容器用改性Ni-Ti-Ta介质材料的制备方法，其特征在于：包括以下步骤：
步骤1：将CuO、NiO、TiO2、Al2O3、Nb2O5以及Ta2O5的原始粉料按照化学通式[Cu0.1Ni0.9]0.5[Ti0.92(Al1/2Nb1/2)0.08]0.5TaO4进行配料；
步骤2：将步骤1配好的粉体装入球磨罐并按照粉料：锆球：去离子水的质量比为1:4～6:5～7进行4～6小时的行星球磨，待球磨结束后将混合浆料置于烘箱中烘干，随后以40～200目的筛网过筛；将过筛后的粉体于900～1100℃的大气气氛中预烧3～5小时；
步骤3：将步骤2经预烧后的粉体再次按照粉体：锆球：去离子水质量比为1:4～6:3～5进行4～6小时的行星球磨，待球磨物料烘干后，向其中添加聚乙烯醇溶液进行粘结剂造粒；
步骤4：将步骤3制得的陶瓷生料压制成型，随后以2～5℃/min的升温速率在600～650℃温度下排胶3～5小时，紧接着再以相同速率升温至1050℃～1150℃中保温4～6小时，即可制得改性[Cu0.1Ni0.9]0.5[Ti0.92(Al1/2Nb1/2)0.08]0.5TaO4介质陶瓷材料。
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