CN1418845A - 介电陶瓷组合物 - Google Patents

介电陶瓷组合物 Download PDF

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CN1418845A
CN1418845A CN02105610A CN02105610A CN1418845A CN 1418845 A CN1418845 A CN 1418845A CN 02105610 A CN02105610 A CN 02105610A CN 02105610 A CN02105610 A CN 02105610A CN 1418845 A CN1418845 A CN 1418845A
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sintering
weight
composition
glass powder
dielectric
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CN1219716C (zh
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金俊熙
许康宪
金钟翰
金佑燮
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Samsung Electro Mechanics Co Ltd
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Abstract

提供一种可以与Ag电极共烧的、具有高介电常数和低介电损耗的介电陶瓷组合物用于电器和电子器具的各种部件中。该组合物由下面的化学式表示：a重量％{xBaO－y1Nd2O3－y2Sm2O3－wBi2O3－zTiO2}+b重量％(基于ZnO－B2O3－SiO2－PbO的玻璃粉)+c重量％CuO，其中，10.0摩尔％≤x≤20.0摩尔％；7.0摩尔％≤y1+y2≤20.0摩尔％；0.5摩尔％≤w≤5.0摩尔％；60.0摩尔％≤z≤80.0摩尔％，条件是x+y1+y2+w+z＝100；80.0重量％≤a≤98.0重量％；1.0重量％≤b≤10.0重量％；1.0重量％≤c≤10.0重量％。

Description

介电陶瓷组合物
技术领域
本发明涉及广泛应用于高频电子元器件中的介电陶瓷组合物，更具体说，本发明涉及一种低温共烧的介电陶瓷组合物，其具有高介电常数和低介电损耗。
低温共烧的介电组合物(材料)是指可以在低于银(Ag)或铜(Cu)的熔点的、800-950℃的温度范围下烧成的组合物(材料)，这与在1,300℃或更高温度下烧结的常规陶瓷介电体不同。
背景技术
鉴于近来高频电子器件小型化、轻盈和模块化的趋势，需要开发可被多层化，然后可与内电极共烧的介电材料。
要实现多层化及与常规介电材料共烧，就需要使用高熔点金属，如Mo或W作为内电极结构。
但是，当使用Mo或W制成内电极结构时，由于其高成本而带来经济上的缺陷。最重要的是，由于存在射频电流集中在靠近导体表面的趋肤效应，所以需要在电极结构中使用低电阻的金属以减少介电损耗。因此，使用相对廉价、电导率高的金属如Ag或Cu是不可避免的。
因此，找到一种可在低于Ag(960℃)或Cu(1083℃)熔点的温度下烧结的介电材料是一项非常重要的研究课题。
通常，低温共烧的介电体可以通过将高温烧结材料与少量的低熔点材料如玻璃粉或诸如CuO、PbO和Bi2O3、V2O5等的一种添加剂混合来制备，或可以通过烧结含有陶瓷作为填料的玻璃陶瓷来制备。
使用后者方法时，所得的基于玻璃的介电基层的介电常数为10或10以下。
由于低介电常数在加速信号处理和改善信号传输方面具有优点，具有10或10以下的介电常数的材料广泛应用于低温共烧陶瓷(LTCC)。
同时，有时根据应用电路的性质，由具有低介电常数和中等介电常数(15-100)的介电体制成的基质通常可能在电路设计和功能方面具有优势，而且不延迟信号的处理。
另外，使用具有高介电常数的介电体使导波的波长变短，这使得电路的尺寸减小。因此，这样的介电体对强调电子器件尺寸的用途非常有用，而且还具有减少某些电路中的介入损耗或频率偏移的优点。
较大的介电常数能够把传输线的宽度和介电体的厚度的比降至更大的程度，这给予电路设计者们设计更好的叠层结构的机会。
按照韩国专利公开公报(1999-62997号)，通过添加基于B2O3-SiO2的玻璃粉，可在低烧结温度下制成具有70或70以上的介电常数的BaO-Re2O-TiO2(Re＝稀土元素)介电组合物。
发明内容
本发明人对LTCC进行了广泛而全面的研究，结果发现CuO与玻璃粉一起可以发挥助烧结剂的作用而提高介电常数，并在控制频率的温度系数方面发挥作用而不引起大的Q值变化，并促成了本发明。
因此，本发明的一个目的是克服现有技术所遇到的上述问题，并提供一种具有高介电常数和低介电损耗、并可低温烧结的介电陶瓷组合物。
按照本发明的一个方面，提供一种由下面的化学式1表示的介电陶瓷组合物：
化学式1
a重量％{xBaO-y1Nd2O3-y2Sm2O3-wBi2O3-zTiO2}+b重量％(基于ZnO-B2O3-SiO2-PbO的玻璃粉)+c重量％CuO
其中，10.0摩尔％≤x≤20.0摩尔％；7.0摩尔％≤y1+y2≤20.0摩尔％；0.5摩尔％≤w≤5.0摩尔％；60.0摩尔％≤z≤80.0摩尔％，条件是x+y1+y2+w+z＝100；80.0重量％≤a≤98.0重量％；1.0重量％≤b≤10.0重量％；1.0重量％≤c≤10.0重量％。
具体实施方式
本发明的介电陶瓷组合物以BaO-Nd2O3-Sm2O3-Bi2O3-TiO2为基础，含有ZnO-B2O3-SiO2-PbO玻璃粉和CuO。仅由BaO-Nd2O3-Sm2O3-Bi2O3-TiO2组成的组合物的烧结温度为1,350℃或1,350℃以上，此温度太高而不能共烧银(Ag)电极，Ag电极在961℃熔化。在本发明中，采用玻璃粉和CuO以利液相烧结基础组合物，从而可与Ag电极共烧。
能够低温烧结具有高烧结温度的材料的、液相烧结稠化的驱动力是由施加在固相微粒之间的液相毛细管压力产生的。要实现液相烧结，需要以下条件。
首先，需要基础介电组合物含有足量的液相，以完全覆盖组合物的初级粒子，还需要该组合物具有一定程度的溶解度。另外，需要该基础介电组合物在液相中具有良好的可湿性。最重要的是，液相烧结需要形成液相。在这一点上，添加剂必须与基础介电组合物发生反应以形成液相。此外，玻璃粉必须具有合适的软化温度(Ts)。另一个必需条件是形成的液相具有低粘度以流过所有的粒子，从而均匀地润湿基础组合物。
另外，越小的初级粒子会引起越大的毛细管压力并因此表现出更大的压实驱动力。而且，初级粒子间的液相分布是影响稠化的一个重要因素。
因此按照本发明，基础介电组合物与玻璃粉和CuO混合，并在稍高于玻璃粉的Ts的温度下对所得混合物进行热处理，以形成均匀分散在整个基础介电组合物中的液相，然后烧结。结果，可以在本发明的介电组合物中获得极佳的稠化。因此，重要的是限定基础介电组合物组成化合物的摩尔比，以及能够通过与基础组合物反应形成液相的添加剂的组成和用量，即CuO的用量和玻璃粉的组成和用量。
对本发明的基础组合物有用的组合物含有10.0-20.0摩尔％的BaO、7.0-20.0摩尔％的Nd2O3和Sm2O3、0.5-5.0摩尔％的Bi2O3和60.0-80.0摩尔％的TiO2，条件是各组分的总摩尔％为100。
如果任何组分的含量超出其范围，则基础介电组合物会表现出过低的介电常数或过高的共振频率温度系数，导致无法在实践中使用。详细地说，当BaO的用量低于10.0摩尔％时，TiO2过量或形成具有低介电常数的Nd2O3-TiO2复合物，从而增大共振频率的温度系数或降低介电常数。另一方面，如果BaO的用量超过20摩尔％，则形成具有低介电常数的BaO-TiO2复合物，从而使基础组合物的介电常数降低。因此，BaO的含量范围优选为10-20摩尔％。
另外，与BaO的用量相关，Nd2O3(Sm2O3)和TiO2的用量也必须落在其各自上述的范围内，以使组合物具有高介电常数和稳定的TCF。
当Nd2O3和Sm2O3的用量之和超过20摩尔％时，具有低介电常数的Nd2O3(Sm2O3)-TiO2相过量，导致介电常数和Q值下降。
为保持高介电常数及控制TCF，特别是稳定物相，Bi2O3对组合物是必不可少的。其用量限制在5.0摩尔％以内：否则，由于组合物的Q值大幅降低而不能用作介电材料。
对本发明有用的是基于ZnO-B2O3-SiO2-PbO的玻璃粉。其用量优选为约1.0-10.0重量％。优选其含有30-70重量％的ZnO、5-30重量％的B2O3、5-40重量％的SiO2和2-40重量％的PbO。
B2O3降低玻璃的粘度并促进本发明的介电陶瓷组合物的烧结。当B2O3的用量低于5重量％时，介电陶瓷组合物很可能不能在低于900℃的温度下烧结。当其用量超过30重量％时，介电陶瓷组合物的耐湿性不好。因此，其在玻璃粉中的用量范围优选为5-30重量％。
SiO2的用量超过40重量％会使玻璃粉的软化温度上升过多从而不能用作助烧结剂。当SiO2的用量低于5重量％时，不能发挥其作用。也就是说，SiO2的用量范围优选为5-40重量％。
如果PbO的用量低于2重量％，玻璃粉的软化温度(Ts)过高，致使其无助于介电陶瓷组合物的烧结。另一方面，PbO的用量超过40重量％会降低玻璃粉的Ts从而改进组合物的烧结，但存在减小Q值的问题。考虑到这些事实，PbO在玻璃粉中的含量范围限定在2-40重量％。
优选ZnO的用量为30-70重量％。过量的ZnO会导致玻璃粉的软化温度上升，致使不可能进行低温烧结。
按照本发明，在本发明的介电陶瓷组合物中使用CuO。为改进可烧结性及控制介电性能，优选CuO的添加量为1.0-10.0重量％。CuO在液相烧结中起主要作用，而玻璃粉促进烧结完成。
添加以上限定的量的玻璃粉和CuO，本发明的介电陶瓷组合物可以在低于900℃的温度下烧结，并表现出50或50以上的介电常数、高Q值和±20ppm/℃或以下的TCF。
以下将描述本发明的介电陶瓷组合物的制备。
按照所需要的组合物xBaO-y1Nd2O3-y2Sm2O3-wBi2O3-zTiO2称量各自纯度为99.0％或99.0％以上的起始物质BaO、Nb2O3、Sm2O3、Bi2O3和TiO2，并将各组分以湿法混合。关于这一点，湿法混合是通过在一台棒磨机中，借助3Φ氧化锆球在去离子水中碾磨起始物质约16小时进行的。干燥并煅烧如此得到的浆料。优选以5℃/分的加热速率，在1,1000-1,150℃下煅烧约2-3小时。当煅烧温度过低时，形成中间相而不是完整的相，使收缩率增大。另一方面，当煅烧温度过高时，粉末变得过于粗糙而无法在以后磨碎。
按照所需要的组合物称量以后，玻璃粉组分在1,200-1,400℃熔化、用水淬火并以干法磨碎。之后，将粗糙的颗粒在乙醇中精磨成大小为0.5～1.0μm的粉末，因为过大的粒子尺寸会产生非均相混合物。
将基础介电陶瓷组合物与玻璃粉组合物、适宜量的CuO在一批中混合。混合优选进行16小时。
干燥后，优选在600-700℃下热处理如此获得的粉末2-3小时。热处理温度比玻璃粉的软化温度(Ts)稍高，从而形成玻璃粉液相并均匀地覆盖在全部基础组合物粒子上，从而提高了反应性和均匀性。由此可以提高介电陶瓷组合物的可烧结性。
接下来，进一步将热处理过的粉末分解至所需的粒子尺寸，并模塑为所需要的形状如圆盘状或片状。
然后，在模塑成的圆盘或片中形成电极，并在低于900℃的温度下共烧电极，得到所需要的器件。
以上概括说明了本发明，参照某些特定的实施例可以进一步理解本发明，在本文中列出这些实施例的目的是仅用于说明，除非另有说明，无意限制本发明。
实施例1
根据下表1中的数据，按照组合物xBaO-y1Nd2O3-y2Sm2O3-wBi2O3-zTiO2称量各自纯度为99.0％或99.0％以上的BaO、Nd2O3、Sm2O3、Bi2O3和TiO2，并使用一台棒磨机，用3Φ氧化锆球将各组分在去离子水中混合16小时。
将如此获得的浆料干燥，在研钵中粗磨，以5℃/分的加热速率加热至1,150℃，在该温度下煅烧2小时。
随后，首先在研钵中研磨，之后使用行星式轧机以200转/分(rpm)的转速研磨80分钟，磨碎煅烧的粉末。与一种粘合剂结合后，通过单轴压缩机，使用14mmΦ的模具，以2.0吨/平方厘米(cm2)的压力将磨碎的粉末模塑为一个圆盘。将试样在1,350℃烧结3小时，并测定其介电常数(K)、Q值、TCF和烧结密度。结果列在下表1中。
在表1中，通过Hakki & Coleman法测定介电常数(K)和Q值，通过空腔谐振法测定共振频率的温度系数(TCF)。在20-85℃之间测量TCF。关于这一点，试样保持在20℃后测定其共振频率，然后加热到85℃并在该温度下保持30分钟后，测定共振频率。通过该测量，测得了TCF。
表1
    基础组合物编号                       组合物(摩％) K Q(在1GHz) TCF(ppm/℃)   烧结温度(℃)
x y1 y2 w z
    1     23.0   16.0     2.0     1.0     58.0     51.0     6,000   8.0   1350
    2     9.0   8.0     1.0     1.0     81.0     95.0     8,200   98.0   1350
    3     9.0   17.5     2.0     1.5     71.0     58.5     2,000   30.0   1350
    4     15.0   14.3     9.0     1.5     60.2     52.4     4,200   7.0   1350
    5     14.0   9.0     6.5     6.0     64.5     88.0     1,200   15.0   1350
    6     17.0   10.0     6.0     0.5     66.5     86.0     9,500   16.0   1350
    7     11.5   9.0     7.0     3.0     69.5     89.0     9,000   15.0   1350
    8     10.0   11.0     2.0     1.5     75.5     93.0     7,000   12.5   1350
    9     12.0   15.0     1.0     0.5     71.5     86.5     5,500   17.0   1350
    10     15.0   9.5     6.0     1.9     67.6     93.0     7,000   16.0   1350
如表1所示，除表现出高Q值和适宜的TCF外，本发明的基础陶瓷组合物(6-10号)具有60以上的介电常数。
大部分适用于本发明的低温烧结的玻璃粉具低至10的介电常数，并因此当与基础介电组合物结合时，使介电常数和Q值下降。另外，期望当在低至900℃的温度下进行烧结时，由于基础组合物的煅烧相不能变为高温烧结相而使介电常数下降。因此，为确保最终的介电陶瓷组合物具有50或50以上的介电常数，基础组合物的介电常数必须大于60。此外，基础组合物的TCF必须为0ppm/℃或0ppm/℃以上，这是因为当其与玻璃粉和CuO结合时，其TCF倾向于向负方向移动。
因此，从表1的数据明显看出6-10号组合物适合开发具有50或50以上的介电常数的低温共烧介电体。
实施例2
将表1的7号和8号组合物分别在研钵里粗磨以后，向每30g组合物中加入4.0-12.0重量％的玻璃粉，然后加入0-12.0重量％的CuO，如下表3所示。
玻璃粉的制备方法是：按照表2的组合物称量其组分，使各组分在1,200-1,400℃熔化，在水中淬火，干法研磨成粗颗粒，及在乙醇中将其研磨至尺寸为0.5-1.0μm。
接下来，将混合物干燥，并在600-700℃下煅烧2小时。
随后，先在研钵中研磨煅烧的粉末，后在行星式轧机中以200rpm的转速研磨30分钟。
与一种粘合剂结合后，通过单轴压缩机，使用14mmΦ的模具，以2.0吨/平方厘米的压力将磨碎的粉末模塑为一个圆盘。将试样在900或1,150℃烧结3小时，并测定其介电常数(K)、Q值、TCF和烧结密度。结果列在下表3中。
在表3中，通过在1,050℃下烧结比较组合物2制备比较组合物3。另外，还分析了试样的烧结状态，结果列于表3中。
以与实施例1相同的方式测定介电性能，包括介电常数(K)、Q值和TCF。
                      表2
    玻璃粉编号     B2O3     SiO2     ZnO     PbO
    实施例G1     25     12     60     3
    实施例G2     17     10     57     15
    比较例G3     3     27     60     10
    比较例G4     35     20     40     5
    比较例G5     20     3     55     22
    比较例G6     15     45     35     5
    比较例G7     20     30     49     1
    比较例G8     10     15     32     43
    比较例G9     12     10     75     3
                                                        表3
介电体编号   基础组合物           玻璃粉 CuO(重量％) 介电常数(K) Q(在1GHz) TCFppm/℃ 烧结温度(℃) 备注
种类     量(重量％) 种类   量(重量％)
  比较例1     7     96.0     G1   4.0   0   -     -     -   900  2N.S.
  比较例2     7     92.0     G1   8.0   0   -     -     -   900  2N.S.
  比较例3     7     92.0     G1   8.0   0   80.2     6500     9.0   1150   烧结
  比较例4     7     97.0     -   -   3.0   -     -     -   900  1P.S.
  比较例5     7     93.0     -   -   7.0   -     -     -   900  1P.S.
  实施例1     7     95.0     G1   4.0   1.0   55.0     2800     6.0   900   烧结
  实施例2     7     93.0     G1   4.0   3.0   60.0     3500     3.2   900   烧结
  实施例3     7     91.0     G1   4.0   5.0   65.0     4000     -3.6   900   烧结
  实施例4     7     89.0     G1   4.0   7.0   70.5     3800     -4.0   900   烧结
  比较例6     7     86.0     G1   4.0   12.0   49.2     500     -12.0   900   烧结
  实施例5     7     89.0     G1   6.0   5.0   62.0     3500     -4.5   900   烧结
  实施例6     7     87.0     G1   8.0   5.0   59.0     3000     -5.0   900   烧结
  比较例7     7     83.0     G1   12.0   5.0   47.9     700     -7.0   900   烧结
  比较例8     7     96.0     G2   4.0   0   -      -     -   900  2N.S.
  比较例9     7     92.0     G2   8.0   0   -      -     -   900  2N.S.
  实施例7     7     95.0     G2   4.0   1.0   55.3     2600     -3.0   900   烧结
  实施例8     7     93.0     G2   4.0   3.0   61.2     3300     -3.2   900   烧结
  实施例9     7     91.0     G2   4.0   5.0   62.7     3900     -3.6   900   烧结
  实施例10     7     89.0     G2   4.0   7.0   61.5     3700     -4.0   900   烧结
  比较例10     7     84.0     G2   4.0   12.0   48.5     800     -14.2   900   烧结
  实施例11     7     89.0     G2   6.0   5.0   56.6     3200     -4.6   900   烧结
  实施例12     7     87.0     G2   8.0   5.0   53.5     1900     -5.2   900   烧结
  比较例11     7     84.0     G2   11.0   5.0   45.0     700     -7.3   900   烧结
  实施例13     8     91.0     G1   4.0   5.0   66.5     3400     -4.6   -   烧结
  实施例14     8     87.0     G2   8.0   5.0   54.5     2400     -5.6   900   烧结
  实施例15     8     91.0     G2   4.0   5.0   63.7     3400     -3.2   900   烧结
比较例12 7 92.0     比较例G3 6.0 2.0 - - - 900 1P.S.
比较例13 7 92.0     比较例G4 6.0 2.0 60.1 2100 5.0 900  3P.M.S.
比较例14 7 97.0     比较例G5 6.0 2.0 - - - 900 1P.S.
比较例15 7 92.0     比较例G6 6.0 2.0 - - - 900 1P.S.
比较例16 7 92.0     比较例G7 6.0 2.0 - - - 900 1P.S.
比较例17 7 92.0     比较例G8 6.0 2.0 65.0 800 6.2 900   Q不好
比较例18 7 92.0     比较例G9 6.0 2.0 - - - 900 1P.S.
1烧结不好
2没有烧结
3耐湿性不好
如表3所示，除可在低至900℃的温度下烧结以外，本发明的介电陶瓷组合物1-15具有53.5或53.5以上的介电常数、1,900或1,900以上的Q值及±6.0ppm/℃的TCF。
相反，比较组合物1-14在900℃烧结不好，或即使烧结了，性能也不好。
当不加入CuO而只加入玻璃粉时，不管玻璃粉的组成如何，组合物根本不能烧结。另一方面，当加入CuO而不加入玻璃粉时，只获得不充分的烧结效果。因此，可以看出在玻璃粉和CuO的共同存在下，保证烧结完全。
举例来说，含有4重量％的玻璃粉、不含CuO的介电陶瓷组合物不能烧结。但是，除4重量％玻璃粉外，当仅加入1重量％的CuO时，组合物的烧结被充分改善，而表现出50或50以上的介电常数。
另外，从表3可以看出，增加CuO的含量使介电陶瓷组合物的烧结得到改善，从而即使烧结温度低也能获得稳定的介电性能。但是，CuO的用量优选约最多至10.0重量％。如果其用量超过10.0重量％，会导致Q值减小，使电阻率下降。
另外，表3的数据说明如果玻璃粉的组成(G1和G2)在本发明所设定的范围内，则组合物的介电性能并不主要依赖该组成。
如上所述，向可在1,300℃或1,300℃以上的温度下烧结的基础组合物中加入玻璃粉和CuO使本发明的介电陶瓷组合物与Ag电极在低至900℃的温度下共烧成为可能。因此，本发明的介电陶瓷组合物具有50或50以上的介电常数、1,000或1,000以上的Q值(在1GHz)及±20ppm/℃的TCF，因此这些组合物适用于多层化的LC滤波器。
以举例的方式描述了本发明，但应当理解所用的术语意在用于说明而非用于限制。按照上述教导，有可能对本发明进行多种改变和变化。因此，应当理解在附带的权利要求书的范围内，本发明可以在除特定描述的内容以外进行实践。

Claims (2)

1.一种介电陶瓷组合物，其由下面的化学式1表示：
化学式1
a重量％{xBaO-y1Nd2O3-y2Sm2O3-wBi2O3-zTiO2}+b重量％(基于ZnO-B2O3-SiO2-PbO的玻璃粉)+c重量％CuO
其中，10.0摩尔％≤x≤20.0摩尔％；7.0摩尔％≤y1+y2≤20.0摩尔％；0.5摩尔％≤w≤5.0摩尔％；60.0摩尔％≤z≤80.0摩尔％，条件是x+y1+y2+w+z＝100；80.0重量％≤a≤98.0重量％；1.0重量％≤b≤10.0重量％；1.0重量％≤c≤10.0重量％。
2.权利要求1所要求的介电陶瓷组合物，其中所述的玻璃粉含有30-70重量％的ZnO、5-30重量％的B2O3、5-40重量％的SiO2和2-40重量％的PbO。
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