CN109020537A - 一种抗还原低损耗型钛酸钡基介质材料 - Google Patents

一种抗还原低损耗型钛酸钡基介质材料 Download PDF

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CN109020537A
CN109020537A CN201811040946.5A CN201811040946A CN109020537A CN 109020537 A CN109020537 A CN 109020537A CN 201811040946 A CN201811040946 A CN 201811040946A CN 109020537 A CN109020537 A CN 109020537A
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李玲霞
王瑞杰
毕越
于仕辉
王文波
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Tianjin University
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
    • C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
    • C04B35/465—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
    • C04B35/468—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
    • C04B35/4682—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates based on BaTiO3 perovskite phase
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
    • C04B2235/3267—MnO2

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  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Capacitors (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

本发明公开了一种抗还原低损耗型钛酸钡基介质材料，化学式为Ba(MnxTi1‑x)O3，其中0＜x≤0.04。先将原料BaTiO3、MnO2化学式称量配料，经过球磨、烘干、过筛后于1000～1100℃下煅烧，再进行造粒，压制成生坯，生坯在还原气氛下于1350℃烧结，制得钛酸钡基介质材料。本发明的介电常数在2300～2800之间，介电损耗在0.9％～5.0％范围内，可用于多层片式陶瓷电容器(MLCC)的制备，大大提高了多层器件的性能。

Description

一种抗还原低损耗型钛酸钡基介质材料
技术领域
本发明属于一种以成分为特征的陶瓷组合物，特别涉及一种抗还原型低损耗介质材料及制备方法。
背景技术
MLCC(多层片式陶瓷电容器)的制作工艺要求内电极必须与介质材料进行共同烧结以形成独石结构，而常见的MLCC瓷料如BaTiO3系统瓷料的烧结温度较高，对于通常的空气气氛烧结而言，只有那些熔点高、难氧化、具有低电阻率的金属才能作为内电极材料，一般选用贵金属Pt、Pd或Pd-Ag合金作为MLCC内电极，这样在MLCC的生产成本中内电极材料成本占了较大比例，并一度造成MLCC的成本因电极材料昂贵而居高不下，极大地限制了其应用范围。此外，MLCC的大比容化要求减小介质层的厚度并增加陶瓷介质的层数，但是随着介质层数的增加，内电极层数也相应增加，导致MLCC的生产成本提高。因此，MLCC的低成本化迫切要求内电极贱金属化。当选用Ni电极作为金属电极时，就要求介质材料和电极同时在还原气氛中共烧，进而要求介质材料的抗还原性。由于MnO2是氧化性物质，其中的Mn离子容易从四价还原成为二价，因此作为添加剂提高BaTiO3的抗还原性能。
发明内容
本发明的目的，是为了适应多层片式陶瓷电容器制作工艺的需求，提供一种具有低频抗还原低损耗型介质材料及制备方法。
本发明通过如下技术方案予以实现。
一种抗还原低损耗型钛酸钡基介质材料，化学式为Ba(MnxTi1-x)O3，其中0＜x≤0.04。
上述低频抗还原低损耗型介质材料的制备方法，具有如下步骤：
(1)将原料BaTiO3、MnO2按Ba(MnxTi1-x)O3，其中0＜x≤0.04化学式称量配料；
(2)将步骤(1)配制的粉料放入球磨罐中，加入氧化锆球和去离子水，球磨4小时；将球磨后的原料置于红外干燥箱中烘干，烘干后过40目筛，获得颗粒均匀的粉料；
(3)将步骤(2)处理后的粉料于1000～1100℃下煅烧3小时，合成主晶相；
(4)在步骤(3)合成主晶相的粉料外加质量百分比为7％的粘结剂，过80目分样筛，造粒；
(5)将步骤(4)的造粒粉料压制成生坯，经排胶后，在还原气氛下，于1350℃烧结，保温2～4小时，制得抗还原低损耗型钛酸钡基介质材料。
所述步骤(2)的烘干温度为110℃。
所述步骤(2)的陶瓷粉体与氧化锆球、去离子水的质量比为1∶1∶2。
所述步骤(4)的坯体为Φ10mm×1mm的圆片。
本发明提供了一种高介电常数低损耗低频抗还原钛酸钡基介质材料及其制备方法，制得的Ba(MnxTi1-x)O3介质材料(其中0＜x≤0.04)，烧结温度为1350℃，介电常数在2300～2800之间，介电损耗在0.9％～5.0％范围内，可用于多层片式陶瓷电容器(MLCC)的制备，同时因为该介质材料具有较低的介电损耗，可大大提高多层器件的性能。
具体实施方式
下面通过具体实施例对本发明作进一步说明，实例中所用原料均为市售分析纯试剂，具体实施例如下。
实施例1
(1)将原料BaTiO3、MnO2按Ba(Mn0.01Ti0.99)O3化学式称量配料；
(2)将上述配制的粉料放入球磨罐中，加入氧化锆球和去离子水，球磨4小时，粉体与氧化锆球、去离子水的质量比为1∶1∶2；将球磨后的原料置于红外干燥箱中于100℃下烘干，烘干后过40目筛，获得颗粒均匀的粉料；
(3)将步骤(2)处理后的粉料于1000℃下煅烧3小时，合成主晶相；
(4)在步骤(3)合成主晶相的粉料外加质量百分比为7％的粘结剂，过80目分样筛，造粒；
(5)将步骤(4)的造粒粉料用用粉末压片机以6MPa的压力压成Φ10mm×1mm的坯体，坯体经排胶后，于1350℃烧结，保温3小时，制得高介电常数低损耗低频抗还原钛酸钡基介质材料。
(6)采用TH2828S测试其制品的电容量C和损耗tanδ以及100V下的绝缘电阻，并计算出制品的介电常数和绝缘电阻率，1KHz下，εr＝2409，tanδ＝0.89％，ρv＝1.80×1012Ω·cm。
具体实施例的相关工艺参数及其介电性能详见表1，各个实施例的制备过程与实施例1完全相同。
表1
本发明不局限于上述实施例，一些细节的变化是可能的，但这并不因此违背本发明的范围和精神。

Claims (4)

1.一种抗还原低损耗型钛酸钡基介质材料，化学式为Ba(MnxTi1-x)O3，其中0＜x≤0.04。
上述低频抗还原低损耗型介质材料的制备方法，具有如下步骤：
(1)将原料BaTiO3、MnO2按Ba(MnxTi1-x)O3，其中0＜x≤0.04化学式称量配料；
(2)将步骤(1)配制的粉料放入球磨罐中，加入氧化锆球和去离子水，球磨4小时；将球磨后的原料置于红外干燥箱中烘干，烘干后过40目筛，获得颗粒均匀的粉料；
(3)将步骤(2)处理后的粉料于1000～1100℃下煅烧3小时，合成主晶相；
(4)在步骤(3)合成主晶相的粉料外加质量百分比为7％的粘结剂，过80目分样筛，造粒；
(5)将步骤(4)的造粒粉料压制成生坯，经排胶后，在还原气氛下，于1350℃烧结，保温2～4小时，制得抗还原低损耗型钛酸钡基介质材料。
2.根据权利要求1所述的一种低频抗还原低损耗型介质材料，其特征在于，所述步骤(2)的烘干温度为110℃。
3.根据权利要求1所述的一种低频抗还原低损耗型介质材料，其特征在于，所述步骤(2)的陶瓷粉体与氧化锆球、去离子水的质量比为1∶1∶2。
4.根据权利要求1所述的一种低频抗还原低损耗型介质材料，其特征在于，所述步骤(4)的坯体为Φ10mm×1mm的圆片。
CN201811040946.5A 2018-09-05 2018-09-05 一种抗还原低损耗型钛酸钡基介质材料 Pending CN109020537A (zh)

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CN110256067A (zh) * 2019-06-19 2019-09-20 天津大学 一种铌锰掺杂抗还原型电介质材料的制备方法

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110183224A (zh) * 2019-06-19 2019-08-30 天津大学 一种施受主共掺高介电常数低损耗电介质材料的制备方法
CN110256067A (zh) * 2019-06-19 2019-09-20 天津大学 一种铌锰掺杂抗还原型电介质材料的制备方法

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Application publication date: 20181218