CN1328732C - 基于钛酸钡的介电材料组合物 - Google Patents

基于钛酸钡的介电材料组合物 Download PDF

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CN1328732C
CN1328732C CNB038108089A CN03810808A CN1328732C CN 1328732 C CN1328732 C CN 1328732C CN B038108089 A CNB038108089 A CN B038108089A CN 03810808 A CN03810808 A CN 03810808A CN 1328732 C CN1328732 C CN 1328732C
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dielectric material
composite dielectric
weight
batio
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CN1653560A (zh
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D·汉宁斯
B·施雷内马彻尔
U·马肯斯
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Koninklijke Philips NV
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Abstract

本发明涉及基于在钙钛矿结构中与Ba(Zn1/3Nb2/3)O3共存的钛酸钡的介电材料组合物，该介电材料组合物的平均粒度d50为0.2μm-0.5μm，微晶粒度d10＜0.3μm。

Description

基于钛酸钡的介电材料组合物
本发明涉及基于在钙钛矿结构中与Ba(Zn1/3Nb2/3)O3共存的钛酸钡(BaTIO3)的介电材料组合物。
基于钛酸钡的介电材料组合物，构成在电子学和通讯中使用的部件的重要原料。使用它们制造无源电子部件，例如电容器。为此目的，介电材料组合物必须在环境温度下具有≥2,000的高介电常数K，也可以获得超过5,000的介电常数值。
制造具有高封装密度的微电子基片的重要技术，也称作“低温共焙烧陶瓷”技术，以下称作LTCC技术。按照所述的技术，绝缘陶瓷箔片按惯例也包含垂直连接孔，在绝缘陶瓷箔片上印刷金属线图案，然后在温度850℃-900℃下焙烧层压箔片。然而，如果采用已知的介电材料组合物，为了确保以令人满意的方式完成烧结过程，必须显著地提高焙烧或烧结温度。
US4283753公开了具有高介电常数的介电材料组合物，旨在使这种组合物在低温下是可以烧结的。通过对理想配比和装料均衡性的具体监测，能够提供在温度约1100℃下可以烧结的基于钛酸钡的介电材料组合物。这种较低的烧结温度能够使用由包括至少30重量％银的钯-银合金组成的导体磁迹(conductor tracks)。
特别是在无线电通讯技术中对高频的应用，在按照LTCC技术生产的组件中，金属导体磁迹必须由导电好的金属组成，优选纯银。由于银的熔点低——961℃，在可能时，陶瓷物质的烧结温度不超过920℃值，此外，重要的是陶瓷物质应该具有相似的热膨胀系数τ。
本发明的目的是提供在开始段落中提到类型的介电材料组合物，该组合物能使烧结温度低到可以使用纯银作为金属导体磁迹的材料。
对于基于在钙钛矿结构中与Ba(Zn1/3Nb2/3)O3共存的钛酸钡的介电材料组合物，本发明的目的是以所述的介电材料组合物平均粒度d50为0.2μm-0.5μm，微晶粒度d10＜0.3μm实现的。优选平均粒度d50为0.3μm-0.4μm，微晶粒度d10≤0.2μm。意外地发现，所用基本材料的粒度和微晶粒度，对将烧结温度降低到920℃以下具有决定意义。
此外，为了改善介电材料组合物的膨胀系数τ，在优选的实施方案中，使用实施本发明的选择方案所需要的烧结添加剂，因为通常使用的烧结添加剂能使介电常数显著降低。所述的烧结添加剂还能进一步改善烧结温度。
能适合介电材料组合物使用的烧结添加剂是氧化物混合物，其中至少包括氧化锌(ZnO)，氧化硼(B2O3)、二氧化硅(SiO2)、和一氧化铜(CuO)。相对BaTiO3-Ba(Zn1/3Nb2/3)O3混合晶体的量，一氧化铜的优选含量为0.25重量％-1.5重量％。
更优选介电材料组合物包括硼沸石(boralite)(Zn4B6O13)形式的氧化锌和氧化硼。相对于BaTiO3-Ba(Zn1/3Nb2/3)O3混合晶体的量，硼沸石的加入量可以为1重量％-5重量％。
按照同样优选的实施方案，烧结添加剂包括因而介电材料组合物也包括二氧化钛(TiO2)和碳酸锂(Li2CO3)。在所述的混合物中，碳酸锂和二氧化硅可以预先反应生成硅酸锂(Li2SiO3)。相对BaTiO3-Ba(Zn1/3Nb2/3)O3混合晶体的量，所述硅酸锂的存在量可以为0.5重量-2.5重量％。
可以使氧化锌、二氧化硅、和二氧化钛预先反应，生成ZST(ZnSiTiO5)；相对于BaTiO3-Ba(Zn1/3Nb2/3)O3混合晶体的量，ZST的存在量可以为1重量％-5重量％。
为了提高绝缘电阻IR和使用寿命，优选在混合晶体中加入少量的锰(Mn)，于是获得基本材料Ba(Ti1-x-yMny[Zn1/3Nb2/3]x)O3，其中0.03≤x≤0.1和0.001≤y≤0.01。
生产用于上述介电材料组合物的BaTiO3-Ba(Zn1/3Nb2/3)O3混合晶体的方法包括下列步骤：
-提供钡、锌、钛、和铌的原料，如果需要，还提供磨碎形式的锰；
-将适宜mol量的原料混合成含水的悬浮体；
-将悬浮体干燥并消除干混合物的结块，制成粉末；
-煅烧粉末；
-将煅烧的粉末磨碎到粒度d50为0.2μm-0.5μm。使微晶粒度d10＜0.3μm。
“以磨碎形式”在此系指将固体形式的原料磨碎到粒度＜0.5μm，或原料是可以以溶解形式或以胶体形式等使用的。
生产烧结温度和热膨胀系数与在市场上可以买到的玻璃陶瓷层相匹配的介电材料组合物的方法，包括下列步骤：
-提供BaTiO3-Ba(Zn1/3Nb2/3)O3混合晶体的粉末，如果需要，还掺杂锰，粉末的平均粒度d50为0.2μm-0.5μm，优选0.3μm-0.4μm，微晶粒度d10＜0.3μm，优选≤0.2μm。
-提供平均粒度d50＜0.5μm的烧结添加剂，烧结添加剂选自：
a)氧化锌、氧化硼、二氧化硅、和一氧化铜的混合物，
a1)硼沸石、二氧化硅、和一氧化铜的混合物，
b)氧化锌、氧化硼、二氧化硅、一氧化铜、二氧化钛、和碳酸锂的混合物，或
b1)硼沸石、ZST、硅酸锂、和一氧化铜的混合物，相对BaTiO3-Ba(Zn1/3Nb2/3)O3混合晶体的量，其用量为1.5重量％-15重量％；
-将BaTiO3-Ba(Zn1/3Nb2/3)O3混合晶体与所选择的烧结添加剂混合，确保维持平均粒度。
采用按照本发明的介电材料组合物，可以生产烧结的层压部件，其中包括至少两层玻璃陶瓷，在它们之间配置按照本发明的介电材料组合物，其中还包括银(Ag)或含银合金的一体化电极(integrated electrodes)。
根据下面所述的实施方案，本发明的这些和其它方面是显而易见的，下面参照所述的实施方案来说明本发明的这些和其它方面。
在附图中：
图1用曲线示出当应用按照本发明的介电材料组合物时，温度对圆盘形试样的电容和损耗的依赖关系；
图2示出由两个玻璃陶瓷层Hereus AHT01-004和按照本发明的介电材料组合物中央层组成的层压部件烧结后的情况。
实施例1
用下列原料生产BaTiO3-Ba(Zn1/3Nb2/3)O3混合晶体(基本材料)：
-Ba：BaCO3，超细的，d50＝0.16μm(Solvay BM040，意大利Massa生产)
-Zn：ZnCO3，磨碎的，d50＜0.5μm(Merck，Darmstadt生产)
-Ti：四丁酸Ti(TBT；Ti[OC3H7]4)，在H2O中水解成胶体的TiO(OH)2；(Dynamit-Nobel，Troisdorf生产)
-Nb：草酸铌，水溶液(H.C.Starck，Goslar生产)
以Mn(NO3)2(Merck，Darmstadt生产)的形式使用掺杂材料锰。
目的是获得组合物的基本材料Ba(Ti1-x-yMny[Zn1/3Nb2/3]xO3，其中0.03≤x≤0.1和0.001≤y≤0.01。求得x和y的最佳值是x＝0.07和y＝0.003。
将适宜mol量的原始成分在球磨机中强烈混合成水悬浮体。悬浮体然后在辐射加热器下干燥，在球磨机中消除结块，获得松散的粉末。然后所述的粉末在空气中在约1000℃下煅烧12h。X-射线衍射记录显示出正六面体的钙钛矿相以及少量碳酸盐(BaCO3)第二相。在球磨机中将煅烧的基本材料尺寸磨碎到粒度d50≈0.3-0.4μm。磨碎粉末的比表面积为约5-6m2/g，相应于微晶粒度d10≤0.2μm。
实施例2
为了生产烧结添加剂，使用在市场上购买形式的原料，例如B2O3、ZnO、CuO、Li2CO3(Merck，Darmstadt)、TiO2(TM-3，日本富士钛公司(Fuji Titanium)生产)、SiO2(Erosil Ox-50，Degusa Hanau生产)。
如果烧结添加剂也包括预反应的中间产物，即硼沸石(boralith)、ZST、和硅酸锂，则在球磨机中混合适宜的原料，制备这些预反应的中间产物，然后在空气中将它们煅烧2h。对于boralith，煅烧温度约940℃，对于ZST约900℃，对于硅酸锂约800℃。
制备在下面表1中列出的混合物：
表1
原料  相对基本材料的百分率(重量％)   最佳值(重量％)
混合物A  Zn4B6O13     1...5     2
 SiO2     0.25...2.5     0.5
 CuO     0.25...1.5     0.5
混合物B  Zn4B6O13     1...5     2
 ZnSiTiO5     1...5     2.7
 CuO     0.25...1.5     0.5
 Li2SiO3     0.5...2.5     1
将烧结添加剂磨碎到平均粒度d50＜0.5μm。
在球磨机中将基本材料与称作混合物A和混合物B的适宜烧结添加剂混合，制备可烧结的介电材料组合物。对于这些组合物，在温度20℃-900℃，膨胀系数τ值为τ＝10...11ppm/K。在市场上购买的玻璃陶瓷的膨胀系数τ＝9...11ppm/K。膨胀系数意外地匹配得很好，所以烧结不会产生应力裂缝。
在厚度600μm直径6mm的圆盘电容器中，检测按照本发明的介电材料组合物的介电和陶瓷性质。为此目的，在10KN的压力下，将粉末状的介电材料组合物压制成圆盘形的坯体，然后在加热和冷却速率300K/h下，在900℃、920℃、和940℃在空气中等温烧结2h。电极使用气相沉积的CrN1/Au层。在-50℃-+150℃，在1V交流电压和1kHz频率下介电性质的测量结果表明，在室温下介电常数的范围最宽，K为2400-3400，视试样的烧结温度而异，图1示出在烧结温度900℃的结果，
所有试样的性质列于表2：
表2
烧结添加剂混合物A  烧结温度900℃   烧结温度920℃   烧结温度940℃
密度g/cm3 5.72 5.76 5.81
介电常数K  2510   2830   3380
Tanδ(介质损耗角正切) 0.006 0.005 0.005
烧结添加剂混合物B
密度g/cm3 5.64 5.66 5.7
介电常数K  2850   3230   4820
Tanδ  0.006   0.006   0.007
δ＝损耗角
使用的混合晶体组合物是Ba(Ti0.927Mn0.03[Zn1/3Nb2/3]0.07)O3。
实施例3
使用磨细的基本材料以及所选择的烧结添加剂，制备基于聚乙烯醇的含水粘合剂乳液。将粘合剂乳液倒出，使用“刮片”方法制成厚度40μm的陶瓷坯箔片。在厚度100μm的玻璃陶瓷材料坯箔片(Heraeus AHT01-004型)之间叠加这些坯箔片，在85℃下施加300bar的低压进行层压。以60K/h的速率将层压的坯体加热到温度450℃，在450℃下在空气中灼烧2h，将粘合剂烧掉、然后以120K/h的加热速率，将如此制备的LTCC层压坯体加热到最高温度900℃-940℃，在空气中烧结半小时。
图2是无断裂(fracture-free)的单片层压部件的显微截面图，其中这些层彼此粘合得很好，几乎显示不出互相反应的痕迹。
按照本发明的方法能在适宜的温度900℃-920℃下以无断裂的方式将层压部件与纯银电极烧结。如果该过程需要更高的温度，例如940℃，则可以以无断裂方式生产Ag/Pd-98/2电极。
因此本发明能将无源电路部件例如滤波器、高通和低通滤波器、和配有阻抗的电路填加到层压结构中，集成的无源电子部件不仅能包括电容器，而且也能包括线圈和其它部件。

Claims (17)

1.基于与钙钛矿结构中的Ba(Zn1/3Nb2/3)O3共存的钛酸钡BaTiO3的介电材料组合物，其特征在于，所述的介电材料组合物平均粒度d50为0.2-0.5μm，微晶粒度d10＜0.3um。
2.权利要求1的介电材料组合物，其特征在于，所述的介电材料组合物平均粒度d50为0.3μm-0.4μm，微晶粒度d10≤0.2μm。
3.权利要求1或2的介电材料组合物，其特征在于，所述的介电材料组合物包括氧化锌、氧化硼、二氧化硅、和一氧化铜。
4.权利要求3的介电材料组合物，其特征在于，相对BaTiO3-Ba-(Zn1/3Nb2/3)O3混合晶体的量，其中包括的一氧化铜含量为0.25重量％-1.5重量％。
5.权利要求3的介电材料组合物，其特征在于，其中它以硼沸石Zn4B6O13形式包括氧化锌和氧化硼。
6.权利要求5的介电材料组合物，其特征在于，相对BaTiO3-Ba-(Zn1/3Nb2/3)O3混合晶体的量，其中包括的硼沸石量为1重量-5重量％。
7.权利要求3的介电材料组合物，其特征在于，其中包括二氧化钛和碳酸锂。
8.权利要求6的介电材料组合物，其特征在于，碳酸锂和二氧化硅预先反应生成硅酸锂。
9.权利要求8的介电材料组合物，其特征在于，相对BaTiO3-Ba-(Zn1/3Nb2/3)O3混合晶体的量，其中包括的硅酸锂量为0.5重量-2.5重量％。
10.权利要求6的介电材料组合物，其特征在于，氧化锌、二氧化硅、和二氧化钛预先反应生成ZnSiTiO5。
11.权利要求10的介电材料组合物，其特征在于，相对BaTiO3-Ba-(Zn1/3Nb2/3)O3混合晶体的量，其中包括的ZnSiTiO5量为1重量-5重量％。
12.权利要求1或2的介电材料组合物，其特征在于，在所述的介电材料组合物中加入锰，生成Ba(Ti1-x-yMny[Zn1/3Nb2/3]x)O3，其中0.03≤x≤0.1和0.001≤y≤0.01。
13.生产用于权利要求1-12任一项的介电材料组合物的BaTiO3-Ba(Zn1/3Nb2/3)O3混合晶体的方法，其中包括下列步骤：
-提供钡、锌、钛、和铌的原料，如果需要，还提供粉碎形式的锰；
-将适宜mol量的原料混合成含水的悬浮体；
-干燥悬浮体并消除干混合物中的结块，制成粉末；
-煅烧粉末；
-将煅烧的粉末磨碎到粒度d50为0.2μm-0.5μm，使微晶粒度d10＜0.3μm。
14.生产介电材料组合物的方法，其中包括下列步骤：
-提供BaTiO3-Ba(Zn1/3Nb2/3)O3混合晶体的粉末，如果需要，还掺杂锰，粉末的平均粒度d50为0.2μm-0.5μm，微晶粒度d10＜0.3μm；
-提供平均粒度d50＜0.5μm的烧结添加剂，所述烧结添加剂选自：
a)氧化锌、氧化硼、二氧化硅、和一氧化铜的混合物，
a1)硼沸石、二氧化硅、和一氧化铜的混合物，
b)氧化锌、氧化硼、二氧化硅、一氧化铜、二氧化钛、和碳酸锂的混合物，或
b1)硼沸石、ZnSiTiO5、硅酸锂、和一氧化铜的混合物，相对于BaTiO3-Ba(Zn1/3Nb2/3)O3混合晶体的量，该混合物的量为1.5重量％-15重量％：
-将BaTiO3-Ba(Zn1/3Nb2/3)O3混合晶体与所选择的烧结添加剂混合，确保维持平均粒度。
15.权利要求14的方法，其中所述粉末的平均粒度d50为0.3μm-0.4μm。
16.权利要求14的方法，其中所述粉末的微晶粒度d10≤0.2μm。
17.烧结的层压部件，其中包括至少两层玻璃陶瓷，在它们之间配置权利要求1-12任一项的介电材料组合物，其中还包括银或含银合金的一体化电极。
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ATE320655T1 (de) 2006-04-15
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