CN1252755C - 温度稳定型的贱金属内电极多层陶瓷电容器介电材料 - Google Patents

温度稳定型的贱金属内电极多层陶瓷电容器介电材料 Download PDF

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CN1252755C
CN1252755C CNB021314314A CN02131431A CN1252755C CN 1252755 C CN1252755 C CN 1252755C CN B021314314 A CNB021314314 A CN B021314314A CN 02131431 A CN02131431 A CN 02131431A CN 1252755 C CN1252755 C CN 1252755C
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temperature
ceramic capacitor
metal inner
multilayer ceramic
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CN1404080A (zh
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王晓慧
陈仁政
桂治轮
李龙土
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Tsinghua University
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Abstract

本发明公开了属于电容器材料制备技术范围的一种温度温度型贱金属内电极多层陶瓷电容器介电材料。包括BaTiO3主料和作CaO、CaTiO3、BaO、SiO2、SrO、MnO2、MgO、Co2O3和Y2O3，以及一种或一种以上的稀土氧化物作添加物，然后加入玻璃料，按比例配制而成陶瓷材料；并用低价格金属Ni、Cu或合金作多层电容器的内电极，在还原气氛中，在1200℃到1350℃进行烧结，获得性能优良的X7R型MLCC材料，材料的室温介电常数在2000和3500之间，容温变化率≤±15%，室温介电损耗≤2%，陶瓷的晶粒在1000nm范围内，性能稳定，适用于生产大容量、超薄介电层的多层陶瓷电容器。

Description

温度稳定型的贱金属内电极多层陶瓷电容器介电材料
技术领域
本发明属于电容器材料技术领域，特别涉及一种温度稳定型贱金属内电极多层陶瓷电容器介电材料。
背景技术
随着多种类型的电子设备诸如数码相机、移动电话、笔记本电脑、掌上电脑等移动电子设备的高速发展，小型化和轻型化是必然的趋势，构成这些电子设备的元器件也必须减小体积和重量，以适应电子元件的安装技术转变为表面贴装技术(SMD)的需要，表面贴装技术要求的元器件为片式元器件。多层陶瓷电容器是片式元件中应用最广泛的一类。多层陶瓷电容器(Multilayer CeramicCapacitors)简称MLCC。它是将电极材料与陶瓷坯体以多层交替并联叠合起来，并同时烧成一个整体。根据国际电子工业协会EIA(Electronic IndustriesAssociation)标准，温度稳定(X7R)型MLCC是指以25℃的电容值为基准，在温度从-55到+125℃的范围之内，容温变化率＜±15％，介电损耗(DF)≤2.5％。X7R型MLCC按组成分两大类：一类由含铅的铁电体组成，另一类以BaTiO3基非铅系的铁电体组成。而后者由于对环境无污染，并且机械强度及可靠性优于前者，因此非铅系BaTiO3基X7R型MLCC具有广阔的应用前景。
当以钛酸钡为基的多层陶瓷电容器在空气中烧结时，需要使用贵金属(Pt、Au、Pd金属及其合金等)作为内电极。贵金属内电极的成本为多层陶瓷电容器生产成本的30％～70％。因此使用贵金属作为内电极成为降低MLCC成本的障碍。基于降低成本的考虑，使用诸如Ni、Fe、Co等贱金属作为MLCC的内电极，但是当这些贱金属内电极在介电陶瓷材料的常规空气中烧结条件下会发生氧化，因此失去作为内电极的作用。为了防止贱金属内电极在烧结过程中的氧化，必须使用中性或者还原性气氛。同时要保证钛酸钡基介电陶瓷在中性或还原气氛下烧结后不成为半导体，而且有足够的绝缘电阻和优良的介电性能。一般将介电层与内电极相互叠加形成生坯，接着在由N2、H2和水蒸气产生的还原气氛下，在1200℃～1400℃的温度范围内进行烧结，然后在1000℃～1100℃的温度下，在具有10-6atm以上氧分压的气氛中进行退火，以提高陶瓷的抗击穿能力，之后加上端电极。目前，在日本专利JP-A-63-103861，陶瓷材料的基本组成为BaTiO3-MnO-MgO-稀土氧化物。这个组成的绝缘电阻和介电温度系数受钛酸钡主料的晶粒大小影响，因此很难通过控制材料组成来获得温度稳定的介电性能。在美国专利US-005403797A，陶瓷材料的基本组成是BaTiO3-Y2O3-MgO-V2O5。该组成基本满足X7R性能要求，室温介电常数为2500以上，但是烧结温度过高，大于1350℃；介电温度系数较大，在-55℃接近-15％；损耗较大，基本都高于2.0％。因此不适合用于大规模生产。
发明内容
本发明的目的是提供一种制备工艺简便，配方简单可调，烧结工艺易控，具有较高介电常数的温度稳定型贱金属内电极多层陶瓷电容器介电材料，主要由占材料总量94～99mol％的钛酸钡主料和占材料总量的1～6mol％的添加物组成，并且在配制过程中再加入占材料总量的1.5～2.5wt％的玻璃料，其特征在于：所述添加物包括CaTiO3、CaO、BaO、SiO2、SrO、MnO2、MgO、Co2O3、和Y2O3、以及一种或一种以上的稀土氧化物Re2O3；其各材料配比为：CaTiO3；0.5～0.7mol％；CaO：0.3～0.4mol％；SiO2：0.7～0.8mol％；SrO：0.3mol％；MnO2：0.2～0.4mol％；MgO：0.2～0.4mol％；Co2O3：0.2mol％；Y2O3：0.5～0.8mol％和Re2O3：1～1.1mol％。
所述稀土氧化物Re2O3中Re代表：镧系元素镧La、铈Ce、镨Pr、钕Nd、钐Sm、铕Eu、钆Gd、铽Tb、镝Dy、钬Ho、铒Er、铥Tm、镱Yb、镥Lu。
所述玻璃料的形式为(BaACa(1-A)O)x·(SiBTi(1-B)O2)，其中0≤A，B≤1和0.9≤x≤1.1，是将SiO2、BaO、CaO、和CaTiO3或相应的前驱体，按照A、B、x的配比进行混合，然后在1000～1200℃下煅烧得到的。
制造MLCC的具体工艺步骤如下：
①将主料钛酸钡与添加物及玻璃料进行混合，以水为介质，球磨24小时；
②烘干：在70～120℃温度下烘10小时；
③流延成介电层：介电层厚度为10μm或10μm以下；
④与贱金属内电极层相互叠加，制造出生坯；
⑤排胶：在300℃，空气中，保温20个小时；若高于300℃排胶温度的话，可以使用氮气保护；
⑥在还原气氛下烧结：烧结过程中通入N2/H2，同时加湿，将氧分压控制在10-8～10-12atm的范围内；例如：以200℃/小时的速度升温到1250℃，保温时间为2小时；
⑦在弱氧化条件下退火：炉温在800℃～1100℃，保温4小时，氧分压控制在10-3～10-4atm的范围内；
⑧冷却至室温；
⑨端电极工艺：端电极为Cu或Ag，炉温在600℃～800℃，保温1小时，氮气保护，自然冷却后，即得到X7R型内电极为贱金属的多层陶瓷电容介电材料。
本发明的有益效果为按本发明的材料配方，可以在1200℃～1350℃的温度下烧结出性能优异的X7R型MLCC材料。其室温介电常数可以控制在2000～3500之间，满足X7R性能要求，容温在-55℃～+125℃范围内的变化率＜±15％，变化率小，介电损耗小，材料均匀性好。适用于生产大容量、超薄介电层(介电层厚度小于10μm)的多层陶瓷电容器。并且具有高绝缘电阻率，性能稳定。
附图说明
图1为实施例1样品的介电常数随温度变化的特性曲线；
图2为实施例1样品的电容变化率随温度变化的曲线；
图3为实施例2样品的介电常数随温度变化的特性曲线；
图4为实施例2样品的电容变化率随温度变化的曲线。
图5为实施例3样品的介电常数随温度变化的特性曲线；
图6为实施例3样品的电容变化率随温度变化的曲线。
具体实施方式
本发明是一种制备工艺简便，配方简单可调，烧结工艺易控，具有较高介电常数的温度温度型贱金属内电极多层陶瓷电容器介电材料，它由粒度小于1000nm的钛酸钡BaTiO3主料本发明的目的是提供一种制备工艺简便，配方简单可调，烧结工艺易控，具有较高介电常数的温度稳定型贱金属内电极多层陶瓷电容器介电材料，主要由占材料总量94～99mol％的钛酸钡主料和占材料总量的1～6mol％的添加物组成，并且在配制过程中再加入占材料总量的1.5～2.5wt％的玻璃料，在温度稳定型贱金属内电极多层陶瓷电容器介电材料中：
其添加物包括CaTiO3、CaO、BaO、SiO2、SrO、MnO2、MgO、Co2O3、和Y2O3、以及一种或一种以上的稀土氧化物Re2O3；其添加物的材料配比为：CaTiO3；0.5～0.7mol％；CaO：0.3～0.4mol％；SiO2：0.7～0.8mol％；SrO：0.3mol％；MnO2：0.2～0.4mol％；MgO：0.2～0.4mol％；Co2O3：0.2mol％；Y2O3：0.5～0.8mol％和Re2O3：1～1.1mol％。
上述稀土氧化物Re2O3中Re代表：镧系元素镧La、铈Ce、镨Pr、钕Nd、钐Sm、铕Eu、钆Gd、铽Tb、镝Dy、钬Ho、铒Er、铥Tm、镱Yb、镥Lu。
上述玻璃料的形式为(BaACa(1-A)O)x·(SiBTi(1-B)O2)，其中0≤A，B≤1和0.9≤x≤1.1，是将SiO2、BaO、CaO、和CaTiO3或相应的前驱体，按照A、B、x的配比进行混合，然后在1000～1200℃下煅烧得到的。
制造MLCC的具体工艺步骤如下：
①将主料钛酸钡与添加物及玻璃料进行混合，以水为介质，然后球磨24小时；
②在70～120℃下，烘10小时；
③在流延机上流延成介电层厚度为10μm或10μm以下；
④与贱金属内电极层相互叠加，制造出生坯；
⑤排胶(300℃，空气中，保温20个小时；更高排胶温度的话，可以使用氮气保护)；
⑥在还原气氛下烧结(烧结过程中通入N2/H2，同时加湿，将氧分压控制在10-8～10-12atm的范围内)例如：以200℃/小时的速度升温到1250℃；保温时间为2小时；
⑦在弱氧化条件下退火(炉温在800℃～1100℃，保温4小时，氧分压控制在10-5～10-1atm的范围内)；
⑧冷却至室温；
⑨端电极工艺(端电极为Cu或Ag，炉温在600℃～800℃，保温1小时，氮气保护)。
下面再举实施例进一步说明如下：
实施例1，先按照BaTiO3：96mol％；(晶粒大小为400nm)CaTiO3 0.5mol％；CaO：0.3mol％；SiO2 0.8mol％；SrO：0.3mol％；MnO2：0.2mol％；MgO：0.2mol％；Co2O3：0.2mol％；Y2O3：0.5mol％；Sm2O3：1.0mol％配比称量。然后再加入玻璃料(BaACa(1-A)O)x·(SiBTi(1-B)O2)，其中A＝0.4，B＝0.9，x＝1.1，占上述混料的2wt％。将上述材料进行混合，球磨，然后干燥。该瓷料流延成膜片，与Ni电极叠加，制成MLCC生坯，排胶后，在还原气氛下烧结(烧结过程中通入N2/H2，同时加湿，将氧分压控制在10-10atm，以200℃/小时的速度升温到1250℃，保温时间为2小时)，然后在弱氧化条件下退火(炉温在1100℃，保温4小时，氧分压控制为105atm)。之后加上Cu端电极(炉温在700℃，保温1小时，氮气保护)。对多层陶瓷电容其进行性能测试，介电性能参数见表一。图1的曲线给出的是本实施例样品的介电常数随温度变化的特性曲线，图2给出样品的电容变化率随温度变化的曲线。
                                  表1
样品 烧结条件   介点常数   TCC(％)   介点常数(25℃)   介点常数   TCC(％)   TGδ(25℃)(％)
          -55℃           125℃
  1   1250℃   2509   -11.9   2850   3100   8.7   0.89
实施例2，先按照BaTiO3：95.2mol％；(晶粒大小为200nm)CaTiO3：0.7mol％；CaO：0.4mol％；SiO2：0.8mol％；SrO：0.3mol％；MnO2：0.3mol％；MgO：0.3mol％；Co2O3：0.2mol％；Y2O3：0.8mol％；Lu2O3：1.0mol％配比称量。然后再加入玻璃料(BaACa(1-A)O)x·(SiBTi(1-B)O2)，其中A＝0.5，B＝0.8，x＝1，占上述混料的1.5wt％。将上述材料进行混合，球磨，然后干燥。该瓷料流延成膜片，与Ni电极叠加，制成MLCC生坯，排胶后，在还原气氛下烧结(烧结过程中通入N2/H2，同时加湿，将氧分压控制在10-9atm，以200℃/小时的速度升温到1200℃，保温时间为2小时)，然后在弱氧化条件下退火(炉温在1100℃，保温4小时，氧分压控制为10-5atm)。之后加上Cu端电极(炉温在700℃，保温1小时，氮气保护)。对多层陶瓷电容其进行性能测试，介电性能参数见表二。图3的曲线给出的是本实施例样品的介电常数随温度变化的特性曲线，图4给出样品的电容变化率随温度变化的曲线。
                                  表2
样品 烧结条件   介点常数   TCC(％)   介点常数(25℃)   介点常数   TCC(％)   TGδ(25℃)(％)
           -55℃            125℃
  2   1200℃   1895   -9.6   2097   2088   -0.4   0.92
实施例3，先按照BaTiO3：95mol％；(晶粒大小为500nm)CaTiO3：0.7mol％；CaO：0.4mol％；SiO2：0.7mol％；SrO：0.3mol％；MnO2：0.5mol％；MgO：0.4mol％；Co2O3：0.2mol％；Y2O3：0.7mol％；Gd2O3：1.1mol％配比称量。然后再加入玻璃料(BaACa(1-A)O)x·(SiBTi(1-B)O2)，其中A＝0.5，B＝0.9，x＝1.1，占上述混料的2.5wt％。将上述材料进行混合，球磨，然后干燥。该瓷料流延成膜片，与Ni电极叠加，制成MLCC生坯，排胶后，在还原气氛下烧结(烧结过程中通入N2/H2，同时加湿，将氧分压控制在10-9atm，以200℃/小时的速度升温到1280℃，保温时间为2小时)，然后在弱氧化条件下退火(炉温在1100℃，保温4小时，氧分压控制为10-5atm)。之后加上Cu端电极(炉温在700℃，保温1小时，氮气保护)。对多层陶瓷电容其进行性能测试，介电性能参数见表三。图5的曲线给出的是本实施例样品的介电常数随温度变化的特性曲线，图6给出样品的电容变化率随温度变化的曲线。
                                    表3
样品 烧结条件   介点常数   TCC(％)   介点常数(25℃)   介点常数   TCC(％)   TGδ(25℃)(％)
         -55℃         125℃
  3   1280℃   2771   -10.6   3100   3503   13   0.71
另外，陶瓷材料的绝缘电阻和击穿电压测试结果见表4。
                          表4
  样品编号   烧结条件   绝缘电阻率(1012×Ω·cm)   击穿场强(KV/mm)
  1   1250℃-2h   10.0   6.13
  2   1200℃-2h   15.5   8.21
  3   1280℃-2h   14.9   7.78
在1200～1350℃的温度范围内，制备了满足X7R性能指标要求的钛酸钡基贱金属内电极MLCC瓷料。MLCC的室温介电常数可以控制在2000到3500之间，容温变化率小于±15％，介电损耗小于2.5％。绝缘电阻率约为1013Ω.cm，击穿电压大于5KV/mm。利用本发明的配方和工艺，可获得烧结温度低，性能可调，烧结温度范围宽，稳定性和再现性良好的钛酸钡基X7R型MLCC材料。而且材料的晶粒均匀，晶粒大小可以控制在100nm～1000nm的范围内。可以应用于大容量，超薄层(介电层厚度小于10μm)多层陶瓷电容器，是一种具有广泛应用前景的MLCC材料。
上述图1～图6为对应于实施例1～3的各样品介电常数的温度特性曲线和电容随温度变化率的温度曲线。测试温度为-60℃～130℃。
表1～表3中各参数代表的意义如下：
TCC(-55℃)：-55℃时容温变化率；
TCC(125℃)：125℃时容温变化率；
tgδ(25℃)：室温时介电损耗；
TCC(T)％＝100×(ε(T)-ε(25℃))/ε(25℃)：容温变化率。

Claims (3)

1.一种温度稳定型贱金属内电极多层陶瓷电容器介电材料，主要由占材料总量94～99mol％的钛酸钡主料和占材料总量的1～6mol％的添加物组成，并且在配制过程中再加入占材料总量的1.5～2.5wt％的玻璃料，其特征在于：所述添加物包括CaTiO3、CaO、BaO、SiO2、SrO、MnO2、MgO、Co2O3、和Y2O3、以及一种或一种以上的稀土氧化物Re2O3；其添加物各材料配比为：CaTiO3：0.5～0.7mol％；CaO：0.3～0.4mol％；SiO2：0.7～0.8mol％；SrO：0.3mol％；MnO2：0.2～0.4mol％；MgO：0.2～0.4mol％；Co2O3：0.2mol％；Y2O3：0.5～0.8mol％和Re2O3：1～1.1mol％。
2.根据权利要求1所述温度稳定型贱金属内电极多层陶瓷电容器介电材料，其特征在于：所述稀土氧化物Re2O3中Re代表：镧系元素镧La、铈Ce、镨Pr、钕Nd、钐Sm、铕Eu、钆Gd、铽Tb、镝Dy、钬Ho、铒Er、铥Tm、镱Yb或镥Lu。
3.根据权利要求1所述温度稳定型贱金属内电极多层陶瓷电容器介电材料，其特征在于：所述玻璃料的形式为(BaACa(1-A)O)·(Si3Ti(1-B)O2)，其中0≤A，B≤1和0.9≤x≤1.1，是将SiO2、BaO、CaO、和CaTiO3或相应的前驱体，按照A、B、x的配比进行混合，然后在1000～1200℃下煅烧得到的。
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