CN101536190A - 具有分级电压响应的电压可切换介电材料的配方及其制造方法 - Google Patents

具有分级电压响应的电压可切换介电材料的配方及其制造方法 Download PDF

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CN101536190A
CN101536190A CNA200780035343XA CN200780035343A CN101536190A CN 101536190 A CN101536190 A CN 101536190A CN A200780035343X A CNA200780035343X A CN A200780035343XA CN 200780035343 A CN200780035343 A CN 200780035343A CN 101536190 A CN101536190 A CN 101536190A
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semiconductive
voltage switchable
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particulate
switchable dielectric
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L·科索沃斯基
R·弗莱明
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Shocking Technologies Inc
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Abstract

电压可切换介电材料的配方包括均匀分散在介电基质材料内的两种或多种不同类型的半导电材料。半导电材料被选择成具有不同的带隙能量以为电压可切换介电材料提供分级电压响应。半导电材料可包括无机微粒、有机微粒、或可溶解于介电基质材料或可与介电基质材料混溶的有机材料。配方还可任选地包括导电材料。配方中的导电或半导电材料的至少一种可包括以至少3或更大的长径比为特征的粒子。

Description

具有分级电压响应的电压可切换介电材料的配方及其制造方法
发明背景
发明领域
本发明一般涉及电子器件领域，具体涉及过压保护。
相关领域
包括半导体管芯或芯片的半导体器件易受过压事件影响或毁坏。过压事件的示例包括静电放电(ESD)、线路瞬变、以及闪电冲击。静电放电一般在携带静电荷的人触摸半导体器件时发生。线路瞬变包括交流输电线上的功率波动，而且可由诸如开关闭合或马达启动之类的事件引起。
电压可切换介电材料也被称为非线性电阻材料，其正常表现为介电材料，但只要施加被称为切换电压的足够电压，其将迅速变为导电材料。电压可切换介电材料在非导电和导电状态之间切换的能力使这些材料非常适合于过压保护应用。然而，多数应用的一个要求是，在其中采用了电压可切换介电材料的器件的正常工作电压之下，电压可切换介电材料不能明显地漏电。
用于制造电压可切换介电材料的常见方法是用高水平的金属微粒填充聚合物至非常接近渗透阈值，通常体积上超过40％。不幸的是，以此方式制造的电压可切换介电材料会在正常工作电压下漏电。而且，制造这样的电压可切换介电材料会是有问题的。金属微粒必须遍及聚合物均匀地分散，较小的浓度差异会显著减弱其性质或在电性质中产生不可接受的变化。虽然通过较长的混合时间能改善均匀性，但因为包括成本的许多原因，长混合时间是不合需要的。
发明内容
本发明提供能对不同电平的过压提供分级响应的电压可切换介电材料的配方。本发明的示例电压可切换介电材料包括介电基质材料和布置在该基质材料内的三种半导电材料。这三种半导电材料的每一种以不同的带隙能量为特征。这些半导电材料的任一个可包括例如无机微粒、有机微粒、或可被溶剂溶解的有机材料。在某些实施例中，这些半导电材料的一种具有约2eV到3eV范围内的带隙能量。在这些实施例的某一些中，第二半导电材料具有小于2eV的带隙能量，而第三半导电材料具有大于3eV的带隙能量。在某些实施例中，电压可切换介电材料还包括布置在基质材料内的导电材料。
本发明的另一示例电压可切换介电材料包括介电基质材料和以不同带隙能量为特征的两种半导电材料。这些半导电材料的一种包括以至少3:1的长径比为特征的微粒。
本发明的又一示例电压可切换介电材料包括介电基质材料和以不同带隙能量为特征的两种半导电材料。在这些实施例中，电压可切换介电材料还包括布置在基质材料内且以至少3:1的长径比为特征的导电材料的微粒。在这些实施例的某一些中，这些半导电材料的一种还包括以至少3:1的长径比为特征的微粒。在一些实例中，电压可切换介电材料可具有小于约35％的导电微粒的体积比。
本发明还提供用于制造电压可切换介电材料的方法，以及通过这些方法制造的电压可切换介电材料。示例方法包括：向树脂中添加第一、第二、以及第三半导电材料；混合该树脂直到第一、第二、以及第三半导电材料均匀分散在树脂中；以及固化该树脂。此处，第一、第二、以及第三半导电材料的每一种以不同的带隙能量为特征。第一、第二、或第三半导电材料的至少一种可包括溶剂可溶解的有机材料。在某些实施例中，混合通过转子-定子混合器来执行和/或包括超声处理。该方法还可包括在混合期间向树脂添加溶剂。在某些实例中，固化树脂包括将树脂暴露给多个固化周期，其中每一相继固化周期处于比前一个固化周期更高的温度。
附图简述
图1示出根据本发明的示例实施例的电压可切换介电材料的截面图。
图2是电流作为向电压可切换介电材料的示例实施例施加的电压的函数的曲线图。
图3是用于制造根据本发明的示例实施例的电压可切换介电材料的方法的流程图表示。
图4是根据本发明一个示例实施例的施用到两个电极之间的间隙的示例电压可切换介电材料的截面。
图5是在根据本发明的示例实施例的电压可切换介电材料的一层上设置的两个电极的截面。
本发明详细描述
本发明提供电压可切换介电材料的配方。此配方以在介电基质材料内分布的两种或多种不同类型的半导电材料为特征。半导电材料被选择成具有不同的带隙能量以为所得的电压可切换介电材料提供对不同的过压电平的分级响应。半导电材料可采取微粒的形式，但不限于此。替换地，半导电材料可溶解在介电基质材料中或与其混溶。配方还可任选地包括导电和/或绝缘材料。在某些实施例中，导电或半导电材料的至少一种包括以至少3或更大的长径比为特征的微粒。这样的高长径比的微粒允许导电微粒的体积百分比相对于现有技术配方的总体减少。从这些配方得到的好处包括在正常工作电压下漏电流较低，以及诸如电容、介电常数、抗裂性、以及热膨胀系数之类的电子应用的性质的一般改善。
图1示意性地示出根据本发明的示例实施例的电压可切换介电材料100的配方。在图1中，基质材料110填充有导电材料的微粒120、具有不同带隙能量的三种半导电材料的微粒130、140、150、以及绝缘材料的微粒160。将理解虽然图1示出包括五种不同类型的微粒120、130、140、150、160的配方，但本发明的配方可略去导电微粒120和/或绝缘微粒150。其它各实施例仅包括具有不同带隙能量的两种半导电材料的微粒130、140，而不是所有三种微粒130、140、以及150。将理解微粒120、130、140、150、160的形状、大小、以及数量仅仅是说明性的而不意味着代表任意特定配方。
另外，虽然图1示出半导电材料的微粒130、140、150，但将可理解微粒130、140、150的一个或多个能被至少部分可溶于基质材料110中或可与其混溶的有机半导电材料替换。在某些实施例中，这样的半导电材料在基质材料110内可能不会呈现为分离的微粒，而仅仅是为了说明而被示为微粒。
在图1所示实施例中，微粒120、130、140、150、160遍及基质材料110均匀分散，以使某些微粒120、130、140、150完全被基质材料110隔离，而其它微粒120、130、140、150彼此接触。因此，穿过电压可切换介电材料100的最小电阻的典型导电路径将穿过微粒120、130、140、150的每一种的一些。
适于基质材料110的一些合适的介电材料是有机聚合物。这样的合适的有机聚合物的示例包括硅树脂聚合物、酚醛树脂、环氧树脂、聚氨酯、聚(甲基)丙烯酸酯、聚酰胺、聚酯、聚碳酸酯、聚丙烯酰胺、聚酰亚胺、聚乙烯、聚丙烯、聚苯醚、聚砜、陶瓷聚合体(溶凝胶/聚合物合成物)、以及聚苯砜。能良好工作的一种特定的环氧树脂是EPON树脂828，它是通过正确的固化试剂能被固化的一种未稀释的纯净双官能双酚A/环氧氯丙烷衍生的液态环氧树脂。某些介电无机聚合物也适合于诸如硅氧烷、和聚磷嗪之类的基质材料110。
在某些实施例中，导电材料的微粒120包括金属。合适的金属包括铜、铝、镍、银、金、钛、不锈钢、铬、及其合金。用于导电微粒120的其它合适材料包括TiC、TiN、以及TiB2。导电材料的微粒120的合适微粒大小是2微米(μ)量级。虽然图1所示的导电材料的微粒120被示为稍稍细长(即具有大于1的长径比)，但将理解导电材料的微粒120不限于稍稍细长的形状。在多个实施例中，导电材料的微粒120可包括从球形到高度细长的形状，或甚至可包括形状分布。
半导电材料的微粒130、140、150是具有在约1eV到6eV的范围内的带隙能量的材料的微粒，但此范围不应被视为是严格限制性的。带隙能量是将电子激发出价带并进入导带所需的能量。合适的半导材料的示例包括Si、NiO、SiC、ZnO、BN、C(以金刚石、纳米管、或球壳状碳分子的形式)、ZnS、Bi2O3、Fe2O3、CeO2、TiO2、AlN以及二硒化铟的化合物。具体地，TiO2可以是未掺杂的或例如用WO3掺杂的，而此实施例中的掺杂指的是表面涂敷。虽然图1所示的半导电材料的微粒130、140、150被示为稍稍细长(即具有大于1的长径比)，但将再次理解半导电材料的微粒130、140、150不限于稍稍细长的形状。在多个实施例中，半导电材料的微粒130、140、150的任一种可以是从球形到高度细长的形状，或甚至可包括形状分布。
在某些实施例中，导电材料的微粒120包括高长径比的微粒，诸如单壁和多壁的导电碳纳米管、球壳状碳分子、金属纳米杆、或金属纳米线。形成纳米杆和/或纳米线的材料的示例包括氮化硼、氧化锡锑、二氧化钛、银、铜、锡、以及金。
在其它实施例中，半导电材料的微粒130、140、150中的一种或多种包括高长径比的微粒。示例包括半导电的碳纳米管、半导电的纳米杆、以及半导电的纳米线。在又一其它实施例中，导电微粒120和半导电材料的微粒130、140、150的至少一种包括高长径比的微粒。微粒120、130、140、150的任一种可具有至少3:1的长径比。在某些实施例中，微粒120、130、140、150的一种或多种具有至少10:1、100:1、或1000:1的长径比。
以不大于500nm的最小尺寸为特征的纳米尺度微粒也可被采用作为微粒120、130、140、150的任一种。在多个实施例中，微粒120、130、140、150的至少一些具有小于100nm或50nm的最小尺寸。在某些实例中，微粒120、130、140、150的至少一些以约20nm的直径为特征。
在又一实施例中，半导电材料的微粒130、140、150的任一种可包括有机材料。将有机材料纳入基质材料110内可导致电压可切换介电材料100相比于仅包括无机材料的电压可切换介电材料100具有出众的性能。这样的性质包括热膨胀系数和热传导率、介电常数、断裂韧度、压缩强度、以及粘附到金属的能力。
有机半导体的示例包括诸如半导电的碳纳米管和球壳状碳分子(例如C60和C70)之类的碳形态。在某些实施例中，球壳状碳分子和纳米管可被改性为职能化成包括共价键合的化学基团或部分。有机半导体的其它示例包括聚3-己基噻吩、聚噻吩、聚乙炔、聚(3，4-二氧乙基噻吩)、聚(苯乙烯磺酸)、并五苯、8-羟基喹啉铝(III)、以及N，N′-二-[(萘基)-N，N′二苯基]-1，1′-联苯基-4，4′-二胺[NPD]。此外，有机半导体能从单体、低聚物、以及噻吩、苯胺(analine)、苯撑、乙烯撑、芴、萘、吡咯、乙炔、咔唑、吡咯烷酮、氰基材料、蒽、并五苯、红荧烯、苝、及二唑的聚合物衍生。这些有机材料的一些被认为是光敏有机材料，诸如聚噻吩。
概言之，本发明提供包括上述导电的、半导电的以及绝缘材料的大范围的配方。例如，基质材料110的体积百分比可从约5％到约99％之间变化，且可包括体积占0到约70％的导电材料、以及体积占约0.01到约95％的半导电材料。在这些宽范围内，导电的和半导电的材料的任一种或全部可包括长径比为至少3的微粒。而且在这些宽范围内，半导电材料的任一种或全部可包括有机材料。
在某些实施例中，基质材料110构成约20％到约80％的体积，导电材料构成约10％到约50％的体积，以及半导电材料构成约0％到约70％的体积。这些实施例可包括体积百分比在0.01％到约40％范围内的长径比至少为3的导电和/或半导电微粒。这些实施例可进一步包括体积百分比在约0.01％到约40％范围内的半导电有机材料。
如上所述，半导电材料的微粒130、140、150以不同的带隙能量为特征，以提供具有对过压的分级响应的电压可切换介电材料100。图2示出具有半导电材料的两种粒子130、140的配方的分级响应。在图2中，绘出了施加在电压可切换介电材料100上的电压相对于电压可切换介电材料100将传导的电流的曲线。将理解电压可替换图2中的电流而绘出可切换介电材料100的电导并且可得到相同的例图。
在所示示例中，具有超过第一阈值(V1)的峰值电压的过压事件足以使具有最低带隙的半导电材料的微粒130传导，但将不足以使具有较高带隙的半导电材料的微粒140传导，除非峰值电压还超过第二阈值(V2)。该概念很容易被延伸至具有三种或更多种类型的半导电材料的粒子130、140、150的配方，各种材料以不同的带隙能量为特征。各种半导电材料的带隙能量的差异将确定从一个阈值到下一个阈值的电压差异。在包括三种半导电材料的某些实施例中，具有最低带隙能量的材料具有小于2eV的带隙能量，具有最高带隙能量的材料具有大于3eV的带隙能量，而剩下的材料具有在约2eV到3eV的范围内的带隙能量。
本发明还提供用于制造电压可切换介电材料的方法。图3是用于制造电压可切换介电材料的示例方法300的流程图表示。在步骤310中用硅烷耦合剂将多种材料添加到诸如EPON树脂828之类的树脂。多种材料可包括上述导电的、半导电的、以及绝缘材料。半导电材料可包括无机微粒、有机微粒、或在溶剂中溶解的有机材料。例如，聚3-己基噻吩可在甲苯中溶解。导电的和半导电的材料可任选地包括高长径比的微粒。
在步骤310中，多种材料可顺序地，全部一起地、或者以各种组合的形式来被添加。在某些实施例中，高长径比的微粒首先被添加，随后继之以余下材料。步骤310还可包括向树脂中添加诸如NMP(N-甲基-2毗咯烷酮)之类的溶剂。步骤310还可包括向树脂中添加固化和/或催化剂试剂。合适的固化试剂是溶解在NMP中的重量15％的Dyhard T03的溶液。
在步骤310中添加到树脂的导电和/或半导电微粒的量将至少部分地取决于它们的长径比。长径比越大，必需的量越少。例如，具有超过1000的长径比的碳纳米管可按将导致碳纳米管在最终合成物中的重量百分比介于约0.01％和约10％之间的量被添加。在某些实例中，被添加到树脂的碳纳米管的量使碳纳米管在最终合成物中的重量百分比为约1％。具有较小长径比的微粒可按照将导致在最终合成物中的重量百分比大于10％的量被添加。例如，具有约10的长径比的微粒可按照足以向最终配方提供约25％或更高的重量百分比的这样微粒的量被添加。
接着，在步骤320，树脂被混合数分钟到数小时(例如8小时)量级的时间以产生均匀的混合物，其中长径比至少为3的微粒均匀分散在树脂内。混合可包括例如超声处理和转子-定子混合。在混合期间还可添加另外的溶剂。
混合之后，在步骤330，混合物被施用至期望位置，且树脂被固化。混合物可例如通过丝网印刷或通过钢丝缠绕刮棒式涂敷(wire wound rodcoating)被施用。对于钢丝缠绕刮棒式涂敷工艺适合的钢丝是#50钢丝。示例固化工艺将混合物暴露给多个固化周期，其中每一相继固化周期处于比前一固化周期更高的温度。一个这样的合适固化过程依次连续采用75℃下10分钟的固化周期、125℃下10分钟的固化周期、175℃下45分钟的固化周期、以及187℃下30分钟的固化周期。
在步骤330中，期望位置可以例如在印刷电路板、半导体封装、半导体器件、射频识别(RFID)标签、发光二极管(LED)、显示器背板、分立电涌抑制器件、或在这些当中任一个的制造期间产生的中间组件上或其内部。
图4示出其中电压可切换介电材料400被设置在接地的电极420与相对于地偏置的电极430之间的间隙410中。这样的安排可用来保护几乎任意的电路或器件抵抗过压事件。通过在间隙410内施用和固化如上关于图2和3所述的均匀混合物，可在间隙410中形成电压可切换介电材料400。
另一安排在图5中示出，其中电极500、510被设置在衬底530上的电压可切换介电材料的层520上。此处，如上关于图3所描述地，通过在衬底530上涂敷和固化均匀的混合物，可以在衬底530上形成电压可切换介电材料的层520。然后通过常规手段可在层520上制造电极500、510。例如，籽层可被沉积在层520上，在籽层上图案化掩模、以及电极500、510通过电镀形成。替换地，籽层可从现有方法中略去。在掩模已被图案化之后，通过施加合适的电压可使电压可切换介电材料的层520导电。一旦导电，则电极500、510可直接被电镀到层520上。用于直接向电压可切换介电材料上电镀的方法在题为“利用电压可切换介电材料的电流携带结构(Current Carrying Structure using Voltage Switchable Dielectric Material)”的美国专利No.6,797,145中已具体描述。
在上述说明书中，参考其特定实施例描述了本发明，但本领域普通技术人员将认识到本发明不限于此。上述发明的各种特征和方面可被单独使用或共同使用。此外，本发明可在超过本文中所描述的任意数量的环境和应用中被采用，而不背离本说明书的更宽的精神和范围。因此，说明书和附图应被认为是说明性的而不是限制性的。将认识到本文中所使用的术语“包括”、“包括”、以及“具有”具体旨在被当作无限度的技术术语。

Claims (25)

1.一种电压可切换介电材料，包括：
介电基质材料；
以第一带隙能量为特征且布置在所述基质材料内的第一半导电材料；
布置在所述介电基质材料内且以不同于所述第一带隙能量的第二带隙能量为特征的第二半导电材料；以及
布置在所述介电基质材料内且以不同于所述第一和第二带隙能量的第三带隙能量为特征的第三半导电材料。
2.如权利要求1所述的电压可切换介电材料，其特征在于，布置在所述介电基质材料内的所述第一半导电材料包括微粒。
3.如权利要求1所述的电压可切换介电材料，其特征在于，还包括布置在所述基质材料内的导电材料。
4.如权利要求1所述的电压可切换介电材料，其特征在于，所述介电基质材料从包括硅树脂聚合物、酚醛树脂、环氧树脂、聚氨酯、聚(甲基)丙烯酸酯、聚酰胺、聚酯、聚碳酸酯、聚丙烯酰胺、聚酰亚胺、聚乙烯、聚丙烯、聚苯醚、聚砜、陶瓷聚合体、聚苯砜、硅氧烷、以及聚磷嗪的组中选出。
5.如权利要求1所述的电压可切换介电材料，其特征在于，所述第二带隙能量在约2eV到3eV的范围内。
6.如权利要求5所述的电压可切换介电材料，其特征在于，所述第一带隙能量小于2eV而所述第三带隙能量大于3eV。
7.一种电压可切换介电材料，包括：
介电基质材料；
以第一带隙能量为特征且布置在所述基质材料内的第一半导电材料的微粒，所述第一半导电材料的微粒还以至少3:1的长径比为特征；以及
布置在所述介电基质材料内且以不同于所述第一带隙能量的第二带隙能量为特征的第二半导电材料。
8.如权利要求7所述的电压可切换介电材料，其特征在于，还包括布置在所述基质材料内的导电材料。
9.如权利要求7所述的电压可切换介电材料，其特征在于，所述第一半导电材料的微粒包括从包括单壁纳米管、多壁纳米管、球壳状碳分子、半导电纳米杆、以及半导电纳米线的组中选出的材料的微粒。
10.如权利要求7所述的电压可切换介电材料，其特征在于，所述第二半导电材料包括从包括硅、碳化硅、氮化硼、氮化铝、氧化镍、硫化锌、氧化铋、氧化铁、氧化钨、以及二氧化钛的组中选出的材料的微粒。
11.如权利要求7所述的电压可切换介电材料，其特征在于，所述第一半导电材料的微粒的长径比至少是1000:1。
12.一种电压可切换介电材料，包括：
介电基质材料；
布置在所述基质材料内且以至少3:1的长径比为特征的导电材料的微粒；
以第一带隙能量为特征且布置在所述基质材料内的第一半导电材料；以及
布置在所述介电基质材料内且以不同于所述第一带隙能量的第二带隙能量为特征的第二半导电材料。
13.如权利要求12所述的电压可切换介电材料，其特征在于，所述导电材料的微粒从包括导电纳米杆、纳米线、单壁纳米管、多壁纳米管、以及球壳状碳分子的组中选出。
14.如权利要求12所述的电压可切换介电材料，其特征在于，所述第一半导电材料包括从包括硅、碳化硅、氮化硼、氮化铝、氧化镍、硫化锌、氧化铋、氧化铁、以及二氧化钛的组中选出的材料的微粒。
15.如权利要求12所述的电压可切换介电材料，其特征在于，所述第一半导电材料包括还以至少3:1的长径比为特征的微粒。
16.如权利要求12所述的电压可切换介电材料，其特征在于，所述导电微粒的体积百分比小于约35％。
17.一种用于制造电压可切换介电材料的方法，所述方法包括：
将第一、第二、以及第三半导电材料添加到树脂，所述第一、第二、以及第三半导电材料的每一个以不同的带隙能量为特征；
混合所述树脂直到所述第一、第二、以及第三半导电材料均匀地分散在所述树脂中；以及
固化所述树脂。
18.如权利要求17所述的方法，其特征在于，所述混合包括超声处理。
19.如权利要求17所述的方法，其特征在于，所述混合通过转子-定子混合器执行。
20.如权利要求17所述的方法，其特征在于，固化所述树脂包括将所述树脂暴露给多个固化周期，其中每一相继固化周期处于比前一固化周期更高的温度。
21.如权利要求17所述的方法，其特征在于，还包括在混合期间向所述树脂添加溶剂。
22.如权利要求21所述的方法，其特征在于，所述溶剂包括N-甲基-2毗咯烷酮。
23.如权利要求17所述的方法，其特征在于，还包括在混合所述树脂之前将导电材料添加到所述树脂。
24.如权利要求17所述的方法，其特征在于，所述第一、第二、或第三半导电材料的至少一种包括溶剂可溶解的有机材料。
25.通过以下工艺制造的一种电压可切换介电材料，所述工艺包括：
将第一、第二、以及第三半导电材料添加到树脂，所述第一、第二、以及第三半导电材料的每一个以不同的带隙能量为特征；
混合所述树脂直到所述第一、第二、以及第三半导电材料均匀地分散在所述树脂中；以及
固化所述树脂。
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