CN102812082A - 聚合物厚膜包封剂和稳定性增强的ptc碳体系 - Google Patents

聚合物厚膜包封剂和稳定性增强的ptc碳体系 Download PDF

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CN102812082A
CN102812082A CN2011800147049A CN201180014704A CN102812082A CN 102812082 A CN102812082 A CN 102812082A CN 2011800147049 A CN2011800147049 A CN 2011800147049A CN 201180014704 A CN201180014704 A CN 201180014704A CN 102812082 A CN102812082 A CN 102812082A
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V·阿兰西奥
J·R·多尔夫曼
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Abstract

本发明涉及聚合物厚膜包封剂组合物，所述组合物包含溶解于有机溶剂中的热塑性含氟聚合物树脂和丙烯酸类树脂。在足以除去所有溶剂并形成包封剂的时间和能量下，加工所述沉积的包封剂组合物。本发明还涉及使用所述包封剂组合物以在PTC加热器电路中形成包封剂，并且具体地在镜加热器和座椅加热器应用中。

Description

聚合物厚膜包封剂和稳定性增强的PTC碳体系
发明领域
本发明涉及聚合物厚膜包封剂组合物。由该组合物制成的包封剂能够在各种电子应用中用于保护电气元件，尤其是用于包封自调节加热器电路中适用的正温度系数碳电阻器。
发明背景
包封剂已被用于保护电气元件。例如，在汽车镜加热器和座椅加热器中，正温度系数(PTC)电路通常被用作自恒温电路。它们用于代替外部恒温器。虽然它们已被用于此类应用多年，但由于电阻转变稳定性、电源开/关循环不一致性以及对环境的灵敏性，PTC电路的性能通常具有性能问题。所有这些问题会对功能化PTC电路具有负面影响。本发明的目的之一是减轻这些问题并生产具有更强稳定性的更高效并且可靠的PTC电路。
发明概述
本发明涉及聚合物厚膜包封剂组合物，所述包封剂组合物包含：
(a)第一有机介质，所述第一有机介质包含30-60重量%的溶解于第一有机溶剂中的热塑性含氟聚合物树脂，其中重量百分比是基于第一有机介质的总重量计的；和
(b)第二有机介质，所述第二有机介质包含10-50重量%的溶解于第二有机溶剂中的丙烯酸类树脂，其中重量百分比是基于第二有机介质的总重量计的。
在一些实施方案中，热塑性含氟聚合物树脂为聚偏二氟乙烯均聚物或基于聚偏二氟乙烯的共聚物。在一个此类实施方案中，热塑性含氟聚合物树脂为聚偏二氟乙烯-六氟丙烯-四氟乙烯共聚物。一些实施方案的丙烯酸类树脂为异丁烯酸甲酯共聚物。
本发明还涉及使用该包封剂形成PTC加热器电路中的包封剂，具体地，镜加热器和座椅加热器应用中的PTC电路中的包封剂。本发明提供了包含此类包封剂的加热器。已发现该包封剂改善PTC电路的稳定性。
发明详述
本发明涉及聚合物厚膜包封剂组合物，该组合物用于形成电路中的包封剂，具体地，PTC加热电路中的包封剂。将包封剂层印刷到活性PTC碳电阻器上并干燥以包封并保护PTC电阻器。
聚合物厚膜(PTF)包封剂组合物由两种有机介质构成，每一种均包含聚合物树脂和溶剂。另外，可添加粉末和印刷助剂以改善组合物。
有机介质
第一有机介质由溶解于第一有机溶剂中的热塑性含氟聚合物树脂构成。含氟聚合物树脂必须对电气元件（例如PTC碳层和下面的基底）均达到良好的粘附性。它必须与电气元件兼容，并且不对电气元件的性能产生不利影响。在一个实施方案中，热塑性含氟聚合物树脂为第一介质总重量的30-60重量%。在另一个实施方案中，热塑性含氟聚合物树脂为第一介质总重量的35-55重量%，并且在另一个实施方案中，热塑性含氟聚合物树脂为第一介质总重量的47-53重量%。在一些实施方案中，热塑性含氟聚合物树脂为聚偏二氟乙烯均聚物或基于聚偏二氟乙烯的共聚物。一种此类基于聚偏二氟乙烯的共聚物为聚偏二氟乙烯-六氟丙烯-四氟乙烯共聚物。
第二有机介质由溶解于第二有机溶剂中的丙烯酸类树脂构成。在一个实施方案中，丙烯酸类树脂为第二介质总重量的10-50重量%。在另一个实施方案中，丙烯酸类树脂为第二介质总重量的20-40重量%，并且在另一个实施方案，丙烯酸类树脂为第二介质总重量的25-35重量%。在一个实施方案中，丙烯酸类树脂为异丁烯酸甲酯共聚物。
通常通过机械混合向有机溶剂中加入聚合物树脂以形成介质。适用于聚合物厚膜组合物的溶剂是本领域技术人员已知的，包括乙酸酯和萜烯，如卡必醇乙酸酯和α-或β-萜品醇，或它们与其它溶剂的混合物，其它溶剂如煤油、邻苯二甲酸二丁酯、丁基卡必醇、丁基卡必醇乙酸酯、己二醇和高沸点醇以及醇酯。此外，可包含挥发性液体以促进在涂覆到基底上之后快速硬化。在本发明的多个实施方案中，溶剂可使用例如乙二醇醚、酮、酯和拥有相似沸点（在180℃至250℃的范围内）的其它溶剂、以及它们的混合物。对这些溶剂和其它溶剂的各种组合进行配制以达到所需的粘度和挥发性要求。所用溶剂必须使树脂溶解。第一溶剂和第二溶剂可不同或可相同。
通常，第一介质为PTF包封剂组合物的总重量的70-97重量%，第二介质为PTF包封剂组合物的总重量的3-30重量%。在一个实施方案中，第一介质为PTF包封剂组合物的总重量的80-96重量%，第二介质为PTF包封剂组合物的总重量的4-20重量%。
粉末
可向PTF包封剂组合物中加入各种粉末以改善粘附性、修改流变学并提高低剪切粘度，从而改善印刷适性。一种此类粉末为热解法二氧化硅。
PTF包封剂组合物的施用
通常将PTF包封剂组合物（也称为“浆料”）沉积到对气体和水分不可渗透的基底上，如聚酯。基底也能是由塑料片与沉积在其上面的任选的金属或介电层的组合组成的复合材料片。
通常通过丝网印刷完成PTF包封剂组合物的沉积，但能够使用其它沉积技术，如孔版印刷、注射式滴涂或涂覆技术。在使用丝网印刷的情况下，筛网的目尺寸控制沉积的厚膜的厚度。
一般来讲，厚膜组合物包含赋予组合物适当电功能性质的功能相。功能相包含分散在有机介质中的电功能粉，所述有机介质充当用于功能相的载体。一般来讲，焙烧组合物以烧尽有机介质的聚合物和溶剂，并赋予电功能性质。然而，就聚合物厚膜而言，有机介质的聚合物部分在干燥后保留为组合物的整体部分。焙烧之前，加工要求可包括任选的热处理，如干燥、固化、回流以及厚膜技术领域的技术人员已知的其它处理。
在除去所有溶剂所需的温度下将PTF包封剂组合物加工一段时间。例如，通过在140℃的热量中暴露通常10-15分钟来干燥沉积的厚膜。
PTC加热电路
PTF包封剂组合物的一个用途是PTC加热电路中的PTC电阻器的包封剂。在一个实施方案中，这种PTC电阻器由PTC炭黑构成。一种此类炭黑电阻器公开于Dorfman的US 5,714,096中。这种PTC炭黑电阻器通过丝网印刷正温度系数组合物形成，所述组合物包含：
(i)15-30重量%的炭黑，其具有约125cc/100g炭黑或更小的DBP吸收值；
(ii)10-40重量%的氯化马来酸酐接枝聚丙烯树脂；和
(iii)能够使树脂溶解的有机介质，其中加热组合物以除去有机介质，从而形成正温度系数碳电阻器。
然后将PTF包封剂组合物丝网印刷到PTC碳电阻器上以使其包封正温度系数碳电阻器，并且干燥以形成包封剂。如Dorfman的US 5,714,096中指出，优选低结构炭黑。用于定量低结构的常用测试为邻苯二甲酸二丁酯(DBP)油吸收值，以每100克炭黑吸收的油的cc数量度。
实施例1
按照以下方式制备PTF包封剂组合物。通过将50.0重量%
Figure BDA00002159097100041
9301（得自Arkema Inc.(Phila.,Pa.)）聚偏二氟乙烯-六氟丙烯-四氟乙烯共聚物树脂与50.0重量%卡必醇乙酸酯（得自Eastman Chemical,(Kingsport,Tenn.)）有机溶剂混合，制备第一有机介质（介质A）。树脂的分子量为大约20,000。将该混合物在90℃下加热1-2小时以溶解所有树脂。通过将30.0%
Figure BDA00002159097100042
2008丙烯酸类树脂（得自ICI Acrylics,Inc.，现在为LuciteInternational,Inc.），一种异丁烯酸甲酯树脂，添加到卡必醇乙酸酯和β-萜品醇有机溶剂的50/50混合物中来制备第二有机介质（介质B）。将该混合物在90℃下加热并搅拌1-2小时以溶解所有树脂。将两种介质按下面所示重量%比率混合。同样按所示重量%添加热解法二氧化硅（得自Cabot Corp.(Boston,Mass.)）、硅氧烷印刷助剂和附加的卡必醇乙酸酯溶剂。
基于组合物的总重量计，所述组合物为：
Figure BDA00002159097100051
将该组合物放入行星式搅拌器中混合30分钟。然后将该组合物转移到三辊磨，在此使其经过一个150psi的通道以产生PTF包封剂组合物。
然后按如下方法制造PTC电路。使用280目不锈钢筛网，采用DuPont银浆5064(E.I.DuPont(Wilmington,Del.))印刷一系列互相交叉的银线的图案。在加压气流箱式炉中，将图案化的线在140℃下干燥15分钟。然后，采用DuPont产品7282PTC碳(DuPont(Wilmington,Del.))叠印标准PTC电路图案以形成较宽的几何形状电阻器，该电阻器具有互相交叉的5064银端。这是使用280目不锈钢筛网印刷的。在加压气流箱式炉中，将PTC碳在140℃下干燥15分钟。最后，使用如上所述相同筛网将包封剂组合物丝网印刷到PTC图案上，并在140℃下干燥15分钟。将电路保持在90℃下24小时后，测量PTC电路的电阻转变并将结果示于表1中。还测得了电力循环转变。通过施加12伏特15分钟，然后移除电源45分钟，来实现电力循环。每小时重复一次该循环，并在电源开启周期测量平衡温度。结果示于表1中。
比较实施例1
完全按实施例1所述制备PTC电路。唯一的区别在于未使用包封剂组合物。该PTC电路的特性总结于表I中。
表I
Figure BDA00002159097100052
从表I中所示的结果来看，由包封剂带来的性能改善是显而易见的。无包封剂所观察到的电阻转变为有包封剂的电阻转变的4倍以上。随着电力循环，无包封剂时的平衡温度随每个周期持续升高，但包封的加热器电路显示出良好的温度稳定性。此外，与比较实施例1的PTC电路相比，在实施例1的PTC电路中，由70℃下的电阻与室温下的电阻之比量度的PTC效应的量级高出大约20%，这进一步支持了使用包封剂时所看到的改善。

Claims (8)

1.聚合物厚膜包封剂组合物，包含：
(a)第一有机介质，所述第一有机介质包含30-60重量%的溶解于第一有机溶剂中的热塑性含氟聚合物树脂，其中所述重量百分比是基于所述第一有机介质的总重量计的；和
(b)第二有机介质，所述第二有机介质包含10-50重量%的溶解于第二有机溶剂中的丙烯酸类树脂，其中所述重量百分比是基于所述第二有机介质的总重量计的。
2.权利要求1的聚合物厚膜包封剂组合物，其中所述热塑性含氟聚合物树脂为聚偏二氟乙烯均聚物或基于聚偏二氟乙烯的共聚物，并且所述丙烯酸类树脂为异丁烯酸甲酯共聚物。
3.权利要求2的聚合物厚膜包封剂组合物，其中所述热塑性含氟聚合物树脂为聚偏二氟乙烯-六氟丙烯-四氟乙烯共聚物。
4.权利要求1的聚合物厚膜包封剂组合物，还包含热解法二氧化硅。
5.正温度系数加热电路，包含由如权利要求1-4的任一项中所述的包封剂组合物形成的包封剂。
6.具有正温度系数加热电路的加热器，所述正温度系数加热电路包含由如权利要求1-4的任一项中所述的包封剂组合物形成的包封剂。
7.权利要求6的加热器，其呈镜加热器或座椅加热器的形式。
8.权利要求7的加热器，所述正温度系数加热电路包含正温度系数组合物，所述正温度系数组合物包含：
(i)15-30重量%的炭黑，所述炭黑具有约125cc/100g炭黑或更小的DBP吸收值；
(ii)10-40重量%的氯化马来酸酐接枝聚丙烯树脂；和
(iii)能够溶解所述树脂的有机介质，其中所述组合物已被加热以除去所述有机介质，从而形成正温度系数碳电阻器，并且其中所述包封剂包封所述正温度系数碳电阻器。
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