CN105073493A - 聚合物厚膜正温度系数碳组合物 - Google Patents

聚合物厚膜正温度系数碳组合物 Download PDF

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CN105073493A
CN105073493A CN201480019388.8A CN201480019388A CN105073493A CN 105073493 A CN105073493 A CN 105073493A CN 201480019388 A CN201480019388 A CN 201480019388A CN 105073493 A CN105073493 A CN 105073493A
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J·R·多尔夫曼
V·阿兰西奥
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DuPont Electronics Inc
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Abstract

本发明涉及聚合物厚膜正温度系数碳电阻器组合物，基本上由以下组成：(a)有机介质，所述有机介质由以下组成：(i)含氟聚合物树脂，所述含氟聚合物树脂由偏二氟乙烯和六氟丙烯的共聚物组成；和(ii)有机溶剂，所述有机溶剂由磷酸三乙酯组成；以及(b)导电碳粉末。可在除去所有溶剂所必需的时间和温度下加工所述组合物。本发明还涉及包含经干燥以除去溶剂的本发明的组合物的正温度系数(PTC)电路，并且涉及包含此类PTC电路的制品，例如后视镜加热器和座椅加热器，以及用于制备此类PTC电路的方法。

Description

聚合物厚膜正温度系数碳组合物
技术领域
本发明涉及用于自调节加热器电路的聚合物厚膜(PTF)正温度系数(PTC)碳电阻器组合物。这种组合物可用作PTF银导体组合物上的丝网印刷层。
背景技术
本领域所熟知的是，导电聚合物的电特性很多情况下取决于它们的温度。极小比例的导电聚合物表现出正温度系数(PTC)，即在特定温度下或在特定温度范围内电阻率迅速增加。表现出PTC行为的材料可用于许多应用中，其中流过电路的电流大小受控于形成电路的一部分的PTC元件的温度。
PTC电路通常用作自恒温电路，诸如在汽车等中发现的后视镜加热器和座椅加热器。它们用于代替外部恒温器。虽然它们已在这些类型的应用中使用多年，但PTC电路通常具有问题，诸如电阻变化稳定性、电源开/关周期易变性以及对制造中使用的粘合剂的敏感性。所有这些问题会且确实对功能化PTC电路具有负面影响。本发明的目的是帮助减轻这些问题，从而帮助生产更有效且可靠的PTC电路。
发明内容
本发明涉及聚合物厚膜正温度系数碳电阻器组合物，基本上由以下组成：
(a)50至99重量百分比的有机介质，所述有机介质由以下组成：
(i)含氟聚合物树脂，所述含氟聚合物树脂由偏二氟乙烯和六氟丙烯的共聚物组成；和
(ii)有机溶剂，所述有机溶剂由磷酸三乙酯组成，其中含氟聚合物树脂占有机介质的总重量的10至50重量百分比并且溶解于有机溶剂中；以及
(b)1至50重量百分比的导电碳粉末，其中导电碳粉末分散于有机介质中，并且其中有机介质和导电碳粉末的重量百分比是基于聚合物厚膜正温度系数碳电阻器组合物的总重量计的。
可在除去所有溶剂所必需的时间和温度下加工所述组合物。
本发明还涉及包含经干燥以除去溶剂的本发明的组合物的PTC电路，涉及用于形成此类PTF电路的方法，并且涉及包含此类PTC电路的制品，例如后视镜加热器和座椅加热器。
具体实施方式
本发明描述用于PTC加热电路的聚合物厚膜正温度系数碳电阻器组合物。其通常用于对总体电路提供加热。有时在有源PTC碳电阻器的顶部印刷一层包封材料并干燥。
本发明中使用的含氟聚合物树脂为偏二氟乙烯(VF2)和六氟丙烯(HFP)的共聚物(VF2/HFP)。与所测试的其他含氟聚合物相比，含氟聚合物树脂提供具有改善的电阻率偏移的浆料。所用溶剂为磷酸三乙酯。含氟聚合物树脂(VF2/HFP)和磷酸三乙酯溶剂的组合提供具有甚至更低的电阻率偏移的碳电阻器和具有稳定性改善的浆料。
一般来讲，厚膜组合物包含向组合物赋予适当电功能性质的功能相。功能相包含分散于有机介质中的电功能粉，所述有机介质充当功能相的载体。一般来讲，通过焙烧组合物来烧尽有机物并赋予电功能性质。然而，对于聚合物厚膜组合物，聚合物或树脂组分在干燥和去除溶剂后仍作为组合物的整体部分。
厚膜包封剂组合物的主要组分为包含聚合物树脂和溶剂的有机介质。
聚合物厚膜正温度系数碳电阻器组合物的组分在下文讨论。
有机介质
将聚合物树脂添加到溶剂中以制备具有适于印刷的稠度和流变特性的“有机介质”。有机介质必须为使固体能够以适当的稳定性程度在其中分散的物质。介质的流变性质必须使得它们赋予组合物良好的应用性质。此类性质包括：具有适当的稳定性程度的固体分散、良好的组合物施涂、适当且相对稳定的粘度、触变性、基底与固体适当的可润湿性、良好的干燥速率、以及足以抵挡粗糙处理的干燥膜强度。
本发明使用的含氟聚合物树脂(VF2/HFP)为偏二氟乙烯(VF2)和六氟丙烯(HFP)的共聚物并且赋予PTC组合物重要的性质。具体地，与其他被测试的含氟聚合物相比，发现该树脂在溶剂中的溶解度和温度稳定性不同。偏二氟乙烯和六氟丙烯的共聚物有助于同时实现对PTF银层和下面的基底的良好粘附性并且与PTC性能相容，即PTC电路的两个关键性质，从而将不会不利地影响PTC性能。在一个实施例中，这种含氟聚合物树脂可以占有机介质总重量的10至50重量百分比(重量％)、25至45重量％、或30至40重量％。
聚合物厚膜正温度系数碳电阻器组合物中使用的溶剂为磷酸三乙酯。
包含本发明的PTFPTC组合物的PTC电路随时间推移的电阻率偏移大大减小并且该组合物的粘度随时间推移显示出较小变化。
本发明的PTFPTC组合物具有50至99重量百分比的有机介质。在一个实施例中，本发明的PTFPTC组合物具有80至95重量百分比的有机介质。
导电粉末
本发明的PTFPTC组合物中使用的导电粉末为要求达到目标电阻(1-50千欧/平方)和所需PTC效应的导电碳或炭黑。可使用其他碳粉末和/或石墨。常用导电粉末诸如银和金也可与碳粉末结合使用。
本发明的PTFPTC组合物具有1至50重量百分比的导电碳粉末。在一个实施例中，本发明的PTFPTC组合物具有5至20重量百分比的导电碳粉末。
厚膜的施涂
通常将聚合物厚膜组合物(也称为“浆料”)沉积在气体和水分不可渗透的基底上，如聚酯。基底也可为由塑性片材与沉积在其上的任选的金属或电介质层的组合组成的复合材料片材。
优选地通过丝网印刷进行PTFPTC组合物的沉积，但也可使用其他沉积技术，诸如孔版印刷、注射式滴涂或其他涂覆技术。在丝网印刷的情况下，筛网的目尺寸控制沉积的厚膜的厚度。
通过在140℃下暴露于热通常10至15分钟来干燥沉积的厚膜，即除去溶剂。
在一个实施例中，PTFPTC碳电阻器组合物用作PTF银组合物诸如DuPont5064银导电油墨(DuPontCo.,Wilmington,DE)的顶部上的丝网印刷层。
将通过给出实际实例，对本发明进行更为详细的讨论。然而，本发明的范围并不以任何方式受到该实际实例的限制。
实例1和比较实验A&B
比较实验A
PTFPTC碳电阻器组合物(浆料)的制备方法为首先按照如下方法制备有机介质：将25.0重量％的偏二氟乙烯和六氟丙烯的共聚物树脂(ADS2ArkemaInc.KingofPrussia,PA)与75.0重量％的二元酯DBETM-9(InvistaTM,Wlmington,DE)有机溶剂混合。树脂的分子量为大约20,000。将上述混合物在90℃下加热1-2小时以溶解所有树脂并形成有机介质。然后将导电炭黑120(CabotCorp.,Boston,MA)添加到有机介质中。
PTFPTC碳电阻器组合物为：
82.72％有机介质
8.18导电炭黑粉末
9.10DBETM-9溶剂
将该组合物在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，在此使其在0psi下通过一次并在150psi下通过一次。最终得到PTFPTC碳电阻器组合物。
然后如下制造电路：采用280目不锈钢筛网，用DuPont5064银导电油墨(DuPontCo.,Wilmington,DE)在聚酯基底上印刷一系列相互交错的银线。在鼓风烘箱中，将该银导体在140℃下干燥15min。接着，将用以上PTFPTC碳电阻器组合物制成的具有相互交错的线的PTC电路图案印刷在银导体的顶部上。然后在鼓风烘箱中，在140℃下干燥15min，以形成PTC电路。
测量PTC电路的电阻，然后在30天后再次测量。计算电阻的偏移百分比并且在表I中示出。测量PTFPTC碳电阻器组合物的粘度，然后在30天后再次测量。计算粘度的变化百分比并且在表I中示出。
比较实验B
基本上如以上在比较实验A中所述制得PTC电路。与比较实验A的唯一区别是使用DuPont7282碳电阻器厚膜组合物(DuPontCo.,Wilmington,DE)，而不是比较实验A的PTFPTC碳电阻器组合物。
测量PTC电路的电阻，然后在30天后再次测量。计算电阻的偏移百分比并且在表I中示出。测量PTFPTC碳电阻器组合物的粘度，然后在30天后再次测量。计算粘度的变化百分比并且在表I中示出。
实例1
基本上如以上在比较实验A中所述制得PTC电路。与比较实验A的唯一区别是使用本发明的PTFPTC碳电阻器组合物，而不是比较实验A的PTFPTC碳电阻器组合物。本发明的PTFPTC碳电阻器组合物使用92.0重量百分比的有机介质和8.0重量百分比的导电碳粉末制成。有机介质由35重量百分比的偏二氟乙烯和六氟丙烯树脂的共聚物(ADS2ArkemaInc.KingofPrussia,PA)和65重量百分比的磷酸三乙酯组成。不同的是使用磷酸三乙酯作为溶剂，而不是比较实验A的二元酯DBETM-9。
测量PTC电路的电阻，然后在30天后再次测量。计算电阻的偏移百分比并且在表I中示出。测量PTFPTC碳电阻器组合物的粘度，然后在30天后再次测量。计算粘度的变化百分比并且在表I中示出。
表I：
30天后的电阻偏移30天后的粘度变化
比较实验A 12.5％ 220％
比较实验B 40.0％ 280％
实例1 4.2％ 50％

Claims (9)

1.一种聚合物厚膜正温度系数碳电阻器组合物，其基本上由以下组成：
(a)50至99重量百分比的有机介质，所述有机介质由以下组成：
(i)含氟聚合物树脂，所述含氟聚合物树脂由偏二氟乙烯和六氟丙烯的共聚物组成；和
(ii)有机溶剂，所述有机溶剂由磷酸三乙酯组成，其中所述含氟聚合物树脂占所述有机介质的总重量的10至50重量百分比且溶解于所述有机溶剂中；以及
(b)1至50重量百分比的导电碳粉末，其中所述导电碳粉末分散于所述有机介质中，并且其中所述有机介质和所述导电碳粉末的重量百分比是基于所述聚合物厚膜正温度系数碳电阻器组合物的总重量计的。
2.根据权利要求1所述的聚合物厚膜正温度系数碳电阻器组合物，其中所述导电碳粉末是导电炭黑粉末。
3.根据权利要求1所述的聚合物厚膜正温度系数碳电阻器组合物，其中所述有机介质占所述总的聚合物厚膜正温度系数碳电阻器组合物的80至95重量百分比，并且其中所述含氟聚合物树脂占所述总的有机介质的30至40重量百分比。
4.一种正温度系数电路，其包含根据权利要求1-3中任一项所述的聚合物厚膜正温度系数碳电阻器组合物，其中所述聚合物厚膜正温度系数碳电阻器组合物经干燥以除去所述溶剂。
5.一种包括根据权利要求4所述的正温度电路的制品。
6.根据权利要求5所述的制品，所述制品为后视镜加热器的形式。
7.根据权利要求5所述的制品，所述制品为座椅加热器的形式。
8.一种用于形成正温度系数电路的方法，所述方法包括提供基底以及将根据权利要求1-3中任一项所述的聚合物厚膜正温度系数碳电阻器组合物沉积到所述基底上，其中所述聚合物厚膜正温度系数碳电阻器组合物经干燥以除去所述溶剂。
9.根据权利要求8所述的方法，其中所述基底包含干燥的PTF银组合物。
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