CN1568253A - 用于形成电极的银涂料 - Google Patents

用于形成电极的银涂料 Download PDF

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CN1568253A
CN1568253A CN02819857.3A CN02819857A CN1568253A CN 1568253 A CN1568253 A CN 1568253A CN 02819857 A CN02819857 A CN 02819857A CN 1568253 A CN1568253 A CN 1568253A
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conductive ink
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付波
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Vibrantz Corp
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Ferro Corp
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Abstract

本发明提供一种电极涂料组合物及其使用方法。该涂料包括银粉、载体和抑制剂。银粉优选不含有钯和金并包括具有最大粒子尺寸小于或等于大约1μm的粒子，抑制剂包括粉碎具有最大粒子尺寸小于或等于0.9μm粒子的陶瓷金属氧化组合物。

Description

用于形成电极的银涂料
技术领域
本发明涉及一种用于形成具有低温烧制多层陶瓷电容的电极的银涂料。
背景技术
多层陶瓷电容(MLC)装置在电子行业是公知的。MLC装置通常是由绝缘坯片和通常含有金属银和钯的导电涂料制备而得。特别地，导电银-钯涂料在坯片上按照需要的图案进行丝网印刷。印刷坯片层叠在一起形成一种顺序(registry)然后在压力作用下层压形成一个单片结构。该单片结构然后进行烧制(通常在大约1250℃)形成MLC装置。
近几年，陶瓷绝缘材料经过改进已经能够在大约880℃和925℃范围内烧制。由于较低的烧制温度，尝试降低用于形成电极的传导涂料中的钯组分。钯的价格要远远高于银，所以减少它的使用能够缩减大量成本。不幸地，试图以含有100％银配方制造传导涂料只有很少的成效。主要问题是低粘性，银移动，银扩散，和/或衰减的电子性能。
发明内容
本发明提供一种新型和增强的传导银涂料用于形成低温烧制MLC装置。本发明涂料显示了优异的粘性和电子性能。在优选实施方式中，该涂料包括银粉，载体和抑制剂。银粉包括具有小于或等于大约1μm最大粒子尺寸的粒子。抑制剂优选包括钛酸钡基质的含有小于或等于大约0.9μm最大粒子尺寸粒子的陶瓷组分。本发明还提供一种新型的低温烧制陶瓷电容及其形成方法。
本发明前述和其他特征将在下文中更详细地描述，尤其在权利要求书中指出，以下描述将详细阐明本发明的具体实施方式，这些是可显示的，但是，也可以按照本发明原则使用不同的方法。
具体实施方式
本发明传导涂料包括银粉、载体和抑制剂。本发明涂料不含有钯、金或除了银之外的任何金属。优选地，该涂料还包括稳定剂和/或抗氧化剂。也可以包括其他辅助剂例如分散剂和触变胶。
本发明涂料中使用的银粉可以从各种可得到的资源中获得。例如，适合的银粉可以是美国罗得岛州(Rhode Island)Engineered PowdersDivision of Technic Inc.of Woonsocket公司的商品名称SILSPHERETM514银粉。这种银粉的粒子平均直径在0.4～1.0μm以及纯度超过99.5％(重量)。银粉也可以由其他商业渠道获得，但是具有小于或等于大约1μm平均粒子尺寸银粉的使用是该涂料的一个关键因素。
本发明中使用的抑制剂优选含有陶瓷金属氧化物。优选地，这样的抑制剂含有钛酸钡基质的材料。更特别地，该抑制剂优选具有与用于形成坯片的绝缘粉相同或近似的组成。
抑制剂用于帮助促进在绝缘层和后来烧制的电极层之间一致的膨胀率。抑制剂优选具有小于或等于大约0.9μm的最大粒子尺寸。如前面提到的，抑制剂的适合来源可以是用于形成绝缘带的绝缘粉。最好需要进行粉末的粉碎，这样可以为抑制剂提供合适的粒子尺寸。
用于形成坯片也可以用作本发明涂料组成中抑制剂的适合绝缘粉的示例，是一种低温绝缘粉，其主要含有美国俄亥俄州Ferro Corporation ofCleveland公司出售的商品名称ULFX7R的钛酸钡和氧化钕混合物。这种绝缘粉可以在880℃和925℃温度范围烧制。这种绝缘粉具有大约0.84μm粒子尺寸(d50)。抑制剂还可以在银粉上以涂层的形式应用。附着于银粉的ZrO2可以从美国新泽西州Degussa Corporation of SouthPlainfield公司购买。
本发明涂料中使用的载体优选含有树脂和溶剂的混合物。优选的树脂/溶剂混合物包括在甲苯/乙醇的80/20(重量百分比)混合物中的10溶液百分重量的乙基纤维素。其他用于形成载体的适合溶剂包括，例如，乙基己醇和/或Exxon Chemical Company公司出售商标为Exxsol D70的脱芳构化脂肪族。
涂料优选包括稳定剂/抗氧化剂，例如，Ciba-Geigy’s IrganoxMD-1024。当然，可以使用通用稳定剂/抗氧化剂中的任何一种或其组合。稳定剂/抗氧化剂用于保证涂料的保质期延缓系统损坏时间。涂料还可以包括其他通用辅助剂例如触变胶和分散剂。辅助剂的这些种类是在电子涂料中通常使用的并且是本领域公知的。
本发明涂料通过一起混合不同的组分而制备，例如，使用三辊粉碎机。粉碎后，涂料组成进行过滤来去除大颗粒和结块。优选地，过滤器具有的最大开孔为大约1μm。为了确保涂料不含有超过1μm的银粒子，过滤是关键的步骤。
低温烧制的MLC装置可以使用本发明涂料组成来制备。这种电容器的形成是通过提供多层绝缘坯片然后在坯片层上沉降涂料而得到。涂料可以使用任何一种通用技术进行沉降，例如丝网印刷。一旦这些坯片以涂料涂覆，这些坯片叠形成重合并压制形成一个单片。然后单片在860℃～940℃温度范围内烧制来形成电容器。申请人因此结合参考美国专利No.5,296,426(尤其是第7列第26行(col.7，line26)到第8列第3行(col.7，line3))和No.4,379,319(尤其是图2)，利用它们关于MLC装置的技术教导。
以下实施例仅是用来说明本发明，并不应该解释为对权利要求的限制。
实施例1、
涂料组合物A、B、C和D的制备是通过使用三辊粉碎机混合表1中列举的重量份数的组分三小时然后在经过1μm过滤器过滤混合物而得到。
                            表1
涂料组成                                          A                  B                  C                   D银粉
Technic Silsphere514 50
PGP7000ID 50
Degussa7000C 50
Degussa11000SP 50
抑制剂
ULF X7R粉末* 4 4 4 4
树脂溶液
在80/20甲苯/乙醇中10(重量％)乙基纤维素(低分子量) 21 21 21 21
在80/20甲苯/乙醇中10(重量％)乙基纤维素(高分子量) 21.5 21.5 21.5 21.5
抗氧化剂
Irganox MD-1024 0.5 0.5 0.5 0.5
溶剂
乙基己醇 1.7766 1.7766 1.7766 1.7766
Exxsol D70-Exxon 0.2234 0.2234 0.2234 0.2234
辅助剂
触变胶(Thixatrol 1) 0.5 0.5 0.5 0.5
分散剂(Solsperse 13940) 0.5 0.5 0.5 0.5
*粉碎到最大粒子尺寸为0.5μm。
实施例2
用于制备绝缘坯片的成型涂料是通过在250ml球磨机中混合表2中列举的组分。
        表2
组分 数量
ULF X7R粉末* 140克
甲苯 30克
甲醇 20克
M1135分散剂 1.6克
M1125分散剂 1.6克
*可以从Ferro Corporation公司获得。
使用175克0.5”氧化锆介质混合物150RMP粉碎大约2小时。加入43.4克B74001粘合溶液(大约36.5％PVB树脂)到混合物中，然后混合6～8小时。然后该混合物经过5μm标准过滤器，使用通用片式成型机成型形成大约千分之六寸厚度的坯片。
实施例3
实施例1中的涂料组合物A在按照实施例2中描述的方法形成的坯片上进行丝网印刷。坯片的印刷层进行层叠形成顺序(registry)并碾压成单片进行烧制。然后加上通用终止胶(TM63-120)。然后经过常规的粘合剂烧毁周期进行加热单片并在925℃烧制经4小时浸泡形成MLC装置。相同的过程重复三次，除了分别使用实施例1中涂料组合物B，C和D而不是组合物A。每个形成的MLC装置都显示了大于140,000pF的电容以及在6μm小于大约2.5％的分散因子。
实施例4
多层陶瓷电容(MLC)装置1，2，3和4是按照实施例3中描述的同样方式使用实施例2中形成的绝缘坯片而形成的。应用于制造MLC装置1，2，3和4的传导涂料具有如实施例1中组成A相同的配方，除了传导涂料含有表3中显示的金属和抑制剂。
                        表3
MLC装置           1                         2                          3                         4传导涂料
金属 54重量份的90/10(重量％)Ag/Pd 50重量份的Ag(100％) 50重量份的Ag(100％) 50重量份的Ag*
抑制剂 没有 4重量份的ULF-X7R** 4重量份的ZrO2 ** ZrO2 *
*以2000ppmZrO2涂覆的Degussa银粉
**粉碎到最大粒子尺寸为0.5μm。
MLC装置1，2，3和4是120mils(千分之一英寸)×60mils(1206面积大小)并具有35层，每层都分别具有8.25μm、10μm、10μm和μm烧制厚度。MLC装置1是控制器(含有Pd的传导涂料)。检测MLC装置1，2，3和4的电子性能，其结果如表4所示。
                        表4
MLC装置                1                       2                      3                      4
电容 207,530pF 158,897pF 147,031pF 140,307pF
分散因子 5μm的占1.95％ 5μm的占1.85％ 5μm的占1.61％ 5μm的占1.68％
对于本领域技术人员，可以很容易明白本发明的其它优点以及改进。因此，具有较宽范围的本发明不受在此显示和描述的具体细节和具体实施例。相应地，在不离开由权利要求及其等同所定义的精神可以进行各种改进。

Claims (17)

1.一种形成低温烧制陶瓷电容装置的方法包括步骤：
(i)制备多层绝缘坯片；
(ii)制备含有银粉、载体和抑制剂的传导涂料组合物，所述银粉具有小于1.0μm的最大粒子尺寸，所述抑制剂包括具有最大粒子尺寸小于0.9μm的粉碎陶瓷金属氧化组合物；
(iii)在所述绝缘坯片上沉降所述传导涂料组合物，所述传导涂料组合物置放在所述绝缘坯片层上，从而经过烧制形成传导电极；
(iv)层叠所述绝缘坯片层形成一定顺序并碾压绝缘坯片层在一起而形成单片；然后
(v)在860℃～940℃温度范围内烧制所述单片。
2.权利要求1所述的方法，其中所述传导涂料组合物不含有钯和金。
3.权利要求1所述的方法，其中所述粉碎陶瓷金属氧化组合物包括钛酸钡。
4.权利要求3所述的方法，其中所述粉碎陶瓷金属氧化组合物还包括氧化钕。
5.权利要求1所述的方法，其中所述粉碎陶瓷金属氧化组合物与用于形成所述绝缘坯片的材料是相同的。
6.权利要求1所述的方法，其中所述粉碎陶瓷金属氧化组合物包括氧化锆。
7.一种不含钯的传导涂料组合物，其包括银粉、载体和抑制剂，用于形成低温烧制多层陶瓷电容装置的电极，所述银粉具有小于1.0μm的最大粒子尺寸，所述抑制剂包括具有最大粒子尺寸小于0.9μm的粉碎陶瓷金属氧化组合物。
8.权利要求7所述的传导涂料组合物，其中所述传导涂料不含有金。
9.权利要求7所述的传导涂料组合物，其中所述粉碎陶瓷金属氧化组合物包括钛酸钡。
10.权利要求7所述的传导涂料组合物，其中所述粉碎陶瓷金属氧化组合物还包括氧化钕。
11.权利要求7所述的传导涂料组合物，其中所述粉碎陶瓷金属氧化组合物包括氧化锆。
12.一种低温烧制多层陶瓷电容装置，其包括具有在多层之间形成导电电极的多层绝缘材料，所述多层陶瓷电容装置的形成包括下述步骤：
(i)制备多层绝缘坯片；
(ii)制备含有银粉、载体和抑制剂的传导涂料组合物，所述银粉具有小于1.0μm的最大粒子尺寸，所述抑制剂包括具有小于0.9μm最大粒子尺寸的粉碎陶瓷金属氧化组合物；
(iii)在所述绝缘坯片上沉降所述传导涂料组合物，所述传导涂料组合物分布在所述绝缘坯片层上，可以经过烧制形成传导电极；
(iv)层叠所述绝缘坯片层形成一定序顺并将绝缘坯片层碾压在一起形成单片；然后
(v)在860℃～940℃温度范围内烧制所述单片。
13.权利要求12所述的多层陶瓷电容装置，其中所述传导涂料组合物不含有钯和金。
14.权利要求12所述的多层陶瓷电容装置，其中所述粉碎陶瓷金属氧化组合物包括钛酸钡。
15.权利要求14所述的多层陶瓷电容装置，其中所述粉碎陶瓷金属氧化组合物还包括氧化钕。
16.权利要求12所述的多层陶瓷电容装置，其中所述粉碎陶瓷金属氧化组合物与用于形成所述绝缘坯片的材料是相同的。
17.权利要求12所述的多层陶瓷电容装置的形成方法，其中所述粉碎陶瓷金属氧化组合物包括氧化锆。
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