CN103965616B - 一种导热树脂组合物及其制备方法 - Google Patents
一种导热树脂组合物及其制备方法 Download PDFInfo
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Abstract
本发明属于高分子复合材料,涉及一种导热树脂组合物及其制备方法。该材料由包含以下重量份的组分制成:100重量份热塑性树脂,5~40重量份氮化硼纤维填充的树脂母料,2~50重量份碳化硼粒子,0.2~1重量份偶联剂,0.1~0.5重量份润滑剂,0.1~1重量份抗氧剂。本发明制得的树脂组合物具有高导热性和高机械强度;由所述树脂组合物,可以容易地获得具有高导热性的构件,尤其是电气和电子部件中的构件。氮化硼导热纤维在组合物中起到了“桥梁”的作用,把单独分散在基体树脂中的导热填料颗粒粘接在一起,把孤立的导热单元连接成大的导热网络,使得填料组分间更容易形成导通网络,导热性能大大增加。
Description
技术领域
本发明属于高分子复合材料,涉及一种导热树脂组合物及其制备方法。
背景技术
在电子技术领域,由于电子线路的集成度越来越高,热量的累积导致器件温度升高从而导致器件工作稳定性降低。为保证电子元器件长时间高可靠性地工作,材料的散热能力就成为影响其使用寿命的重要限制因素。
由于聚合物树脂组合物的优异机械性能和电绝缘性能,它们可用于多种应用中,如机动车部件、电子和电气部件、机器部件等。在多种情况下,由于聚合物树脂组合物允许的设计适应性、密封性能和它们的电绝缘性能,它们可被用作电子和电气装置或马达的包封剂。然而,包封聚合物组合物不仅需要电绝缘性能,它们通常还需要具有更高的导热性。
近年来在电气和电子部件领域中,需求具有高导热性的树脂材料。例如,已经提出进行一种通过高填充包含高导热材料比如广泛使用的氮化铝、氮化硼、碳黑、石墨或金属填料的球形填料而赋予树脂材料高导热性的方法(参见CN 101568599 B)。
上述专利中公开的技术不能给树脂材料提供足够高的导热性或机械强度,并且由于一些填料是高导电填料的缘故,而难于将一些树脂材料应用于电气和电子部件中的构件。
发明内容
本发明的目的在于为克服现有技术的缺陷而提供一种导热树脂组合物及其制备方法。
本发明通过在树脂组合物中同时添加导热填料与导热纤维,使其产生协同导热效果,以达到能改进导热性能。
为实现上述目的,本发明采用如下技术方案:
一种导热树脂组合物,由包含以下重量份的组分制成:
热塑性树脂 100份,
氮化硼纤维填充的树脂母料 5~40份,
碳化硼粒子 2~50份,
偶联剂 0.2~1份,
润滑剂 0.1~0.5份
抗氧剂 0.1~1份。
所述的热塑性树脂为聚酰胺树脂、丙烯腈-苯乙烯-丁二烯共聚物、聚苯乙烯、聚碳酸酯树脂或聚苯硫醚树脂。
所述的碳化硼粒子的数均粒径为10~150μm。
所述的氮化硼纤维填充的树脂母料由包含以下重量份的组分制成:
树脂基体 4~15份,
氮化硼纤维 1~25份。
所述的树脂基体选自聚酰胺树脂、丙烯腈-苯乙烯-丁二烯共聚物、聚苯乙烯、聚碳酸酯树脂或聚苯硫醚树脂。
所述的氮化硼纤维直径为1~50μm。
所述的抗氧剂为四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯、三(2,4-二叔丁基苯基)亚磷酸酯、β-(4-羟基-3,5-二叔丁基苯基)丙酸正十八碳醇酯中的一种或一种以上。
所述的偶联剂为γ-氨丙基三乙氧基硅烷、γ-缩水甘油醚氧丙基三甲氧基硅烷、γ-(甲基丙烯酰氧)丙基三甲氧基硅烷中的一种或一种以上。
所述的润滑剂为硬脂酸钙、月桂酸二乙醇酰胺、硬脂酸锌或聚乙烯蜡中的一种或一种以上。
一种上述的导热树脂组合物的制备方法,该方法包括以下步骤:
(1)制备氮化硼纤维填充的树脂母料:将4~15重量份的树脂、1~25重量份的氮化硼纤维在高速搅拌机里混合3~5min后,采用螺杆挤出的熔融捏合共混方法制成氮化硼纤维填充的树脂母料。
(2)将步骤(1)制成的氮化硼纤维填充的树脂母料,与100重量份基体树脂、2~50重量份碳化硼粒子、0.2~1重量份偶联剂、0.1~0.5重量份润滑剂、0.1~1重量份抗氧剂,混合均匀,采用螺杆挤出的熔融捏合共混方法制成导热树脂。
所述的步骤(1)中,双螺杆挤出机自喂料口至挤出模头温度分别是170~190℃,190~220℃,210~240℃,220~240℃,220~240℃,主机转速是20~40赫兹。
所述的步骤(2)中,双螺杆挤出机自喂料口至挤出模头温度分别是190~210℃,200~230℃,210~230℃,220~230℃,220~240℃,主机转速是30~50赫兹。
本发明与现有技术相比,具有以下优点和有益效果:
使用上述的树脂组合物,可以获得具有高导热性和高机械强度的成型制品。由所述树脂组合物,可以容易地获得具有高导热性的构件,尤其是电气和电子部件中的构件。氮化硼导热纤维在组合物中起到了“桥梁”的作用,把单独分散在基体树脂中的导热填料颗粒粘接在一起,把孤立的导热单元连接成大的导热网络,使得填料组分间更容易形成导通网络,导热性能大大增加。
具体实施方式
以下结合实施例对本发明作进一步的说明。
以下实施例中,相关的测试的标准和方法为:
导热系数:按ASTM E1530方法;
拉伸强度:按ASTM D638方法,测试环境温度为23℃;
弯曲强度、弯曲模量:按ASTM D790方法,测试环境温度为23℃。
实施例1
将15重量份的聚酰胺树脂、25重量份直径为50μm的氮化硼纤维在高速搅拌机里混合3min后,采用螺杆挤出的熔融捏合共混方法制成氮化硼纤维填充的聚酰胺树脂母料,其中双螺杆挤出机自喂料口至挤出模头温度分别是170℃,190℃,210℃,220℃,220℃,主机转速是20赫兹。
将40重量份制成的氮化硼纤维填充的树脂母料,与100重量份聚酰胺树脂、2重量份数均粒径为150μm碳化硼粒子、0.5重量份四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯、1重量份γ-氨丙基三乙氧基硅烷、0.5重量份硬脂酸钙,按比例混合后,采用螺杆挤出的熔融捏合共混方法制成导热树脂,其中双螺杆挤出机,自喂料口至挤出模头温度分别是190℃,200℃,210℃,220℃,220℃,主机转速是50赫兹。
本发明制得的导热树脂组合物的相关性能测试见表1。
实施例2
将4重量份的聚碳酸酯树脂、1重量份直径为1μm的氮化硼纤维在高速搅拌机里混合5min后,采用螺杆挤出的熔融捏合共混方法制成氮化硼纤维填充的聚碳酸酯树脂母料,其中双螺杆挤出机自喂料口至挤出模头温度分别是190℃,220℃,230℃,240℃,240℃,主机转速是40赫兹。
将5重量份制成的氮化硼纤维填充的树脂母料,与100重量份聚碳酸酯树脂、20重量份数均粒径为10μm碳化硼粒子、0.8重量份三(2,4-二叔丁基苯基)亚磷酸酯、0.5重量份γ-缩水甘油醚氧丙基三甲氧基硅烷、0.3重量份月桂酸二乙醇酰胺,按比例混合后,采用螺杆挤出的熔融捏合共混方法制成导热树脂,其中双螺杆挤出机,自喂料口至挤出模头温度分别是
210℃,230℃,230℃,230℃,240℃,主机转速是30赫兹。
本发明制得的导热树脂组合物的相关性能测试见表1。
实施例3
将9重量份的聚苯硫醚树脂、15重量份直径为25μm的氮化硼纤维在高速搅拌机里混合4min后,采用螺杆挤出的熔融捏合共混方法制成氮化硼纤维填充的聚苯硫醚树脂母料,其中双螺杆挤出机自喂料口至挤出模头温度分别是180℃,200℃,220℃,230℃,230℃,主机转速是30赫兹。
将24重量份制成的氮化硼纤维填充的树脂母料,与100重量份聚苯硫醚树脂、50重量份数均粒径为80μm碳化硼粒子、1重量份β-(4-羟基-3,5-二叔丁基苯基)丙酸正十八碳醇酯、0.2重量份γ-(甲基丙烯酰氧)丙基三甲氧基硅烷、0.3重量份月桂酸二乙醇酰胺,按比例混合后,采用螺杆挤出的熔融捏合共混方法制成导热树脂,其中双螺杆挤出机自喂料口至挤出模头温度分别是200℃,210℃,220℃,220℃,230℃,主机转速是40赫兹。
本发明制得的导热树脂组合物的相关性能测试见表1。
实施例4
将11重量份的聚苯乙烯树脂、8重量份直径为12μm的氮化硼纤维在高速搅拌机里混合5min后,采用螺杆挤出的熔融捏合共混方法制成氮化硼纤维填充的聚苯乙烯树脂母料,其中双螺杆挤出机自喂料口至挤出模头温度分别是190℃,220℃,230℃,240℃,240℃,主机转速是20赫兹。
将19重量份制成的氮化硼纤维填充的树脂母料,与100重量份聚苯乙烯树脂、10重量份数均粒径为50μm碳化硼粒子、0.4重量份三(2,4-二叔丁基苯基)亚磷酸酯、0.4重量份γ-缩水甘油醚氧丙基三甲氧基硅烷、0.4重量份聚乙烯蜡,按比例混合后,采用螺杆挤出的熔融捏合共混方法制成导热树脂,其中双螺杆挤出机,自喂料口至挤出模头温度分别是210℃,230℃,230℃,230℃,240℃,主机转速是50赫兹。
本发明制得的导热树脂组合物的相关性能测试见表1。
实施例5
将13重量份的丙烯腈-苯乙烯-丁二烯共聚物、21重量份直径为35μm的氮化硼纤维在高速搅拌机里混合4min后,采用螺杆挤出的熔融捏合共混方法制成氮化硼纤维填充的丙烯腈-苯乙烯-丁二烯共聚物树脂母料,其中双螺杆挤出机自喂料口至挤出模头温度分别是180℃,200℃,220℃,230℃,230℃,主机转速是40赫兹。
将34重量份制成的氮化硼纤维填充的树脂母料,与100重量份丙烯腈-苯乙烯-丁二烯共聚物树脂、30重量份数均粒径为120μm碳化硼粒子、0.1重量份四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯、0.8重量份γ-氨丙基三乙氧基硅烷、0.2重量份月桂酸二乙醇酰胺,按比例混合后,采用螺杆挤出的熔融捏合共混方法制成导热树脂,其中双螺杆挤出机,自喂料口至挤出模头温度分别是210℃,230℃,230℃,230℃,240℃,主机转速是40赫兹。
本发明制得的导热树脂组合物的相关性能测试见表1。
表1
实施例 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 |
导热系数(W/m.k) | 2.1 | 2.8 | 4.2 | 2.7 | 3.7 |
拉伸强度(MPa) | 130 | 80 | 140 | 100 | 127 |
弯曲强度(MPa) | 260 | 90 | 130 | 110 | 240 |
弯曲模量(MPa) | 9000 | 2800 | 8000 | 3200 | 8500 |
由表1可知,本发明的技术方案中,加入较多比例的碳化硼粒子,和较多氮化硼纤维的树脂,其导热系数较高,达到了4.2W/m.k。基体树脂中,加入的硼纤维含量较少,其拉伸强度与弯曲强度都较低。
上述的对实施例的描述是为便于该技术领域的普通技术人员能理解和应用本发明。熟悉本领域技术的人员显然可以容易地对这些实施例做出各种修改,并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此,本发明不限于这里的实施例,本领域技术人员根据本发明的揭示,不脱离本发明范畴所做出的改进和修改都应该在本发明的保护范围之内。
Claims (4)
1.一种导热树脂组合物,其特征在于:由以下重量份的组分制成:
所述的氮化硼纤维填充的树脂母料由以下重量份的组分制成:
树脂基体 4~15份,
氮化硼纤维 1~25份;
所述的热塑性树脂和所述树脂基体均为丙烯腈-苯乙烯-丁二烯共聚物,或者所述的热塑性树脂和所述树脂基体均为聚苯乙烯,或者所述的热塑性树脂和所述树脂基体均为聚苯硫醚,或者所述的热塑性树脂和所述树脂基体均为聚碳酸酯,或者所述的热塑性树脂和所述树脂基体均为聚酰胺;
所述的氮化硼纤维直径为1~50μm;
所述的碳化硼粒子的数均粒径为10~150μm;
所述的偶联剂为γ-氨丙基三乙氧基硅烷或γ-(甲基丙烯酰氧)丙基三甲氧基硅烷中的一种以上;
所述导热树脂组合物的制备方法包括以下步骤:
(1)制备氮化硼纤维填充的树脂母料:
将4~15重量份的树脂基体、1~25重量份的氮化硼纤维在高速搅拌机里混合3~5min后,采用螺杆挤出的熔融捏合共混方法制得氮化硼纤维填充的树脂母料;
(2)将5~40份由步骤(1)制成的氮化硼纤维填充的树脂母料,与100重量份基体树脂、2~50重量份碳化硼粒子、0.2~1重量份偶联剂、0.1~0.5重量份润滑剂、0.1~1重量份抗氧剂,混合均匀,采用螺杆挤出的熔融捏合共混方法制成导热树脂;
所述的步骤(1)中,双螺杆挤出机自喂料口至挤出模头温度分别是170~190℃,190~220℃,210~240℃,220~240℃,220~240℃,主机转速是20~40赫兹;
所述的步骤(2)中,双螺杆挤出机自喂料口至挤出模头温度分别是190~210℃,200~230℃,210~230℃,220~230℃,220~240℃,主机转速是30~50赫兹。
2.根据权利要求1所述的导热树脂组合物,其特征在于:所述的润滑剂为硬脂酸钙、月桂酸二乙醇酰胺、硬脂酸锌或聚乙烯蜡中的一种以上。
3.根据权利要求1所述的导热树脂组合物,其特征在于:所述的抗氧剂为四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯、三(2,4-二叔丁基苯基)亚磷酸酯或β-(4-羟基-3,5-二叔丁基苯基)丙酸正十八碳醇酯中的一种以上。
4.一种上述权利要求1-3任一项所述的导热树脂组合物的制备方法,其特征在于:该方法包括以下步骤:
(1)制备氮化硼纤维填充的树脂母料:
将4~15重量份的树脂、1~25重量份的氮化硼纤维在高速搅拌机里混合3~5min后,采用螺杆挤出的熔融捏合共混方法制得氮化硼纤维填充的树脂母料;
(2)将5~40份由步骤(1)制成的氮化硼纤维填充的树脂母料,与100重量份基体树脂、2~50重量份碳化硼粒子、0.2~1重量份偶联剂、0.1~0.5重量份润滑剂、0.1~1重量份抗氧剂,混合均匀,采用螺杆挤出的熔融捏合共混方法制成导热树脂;
所述的步骤(1)中,双螺杆挤出机自喂料口至挤出模头温度分别是170~190℃,190~220℃,210~240℃,220~240℃,220~240℃,主机转速是20~40赫兹;
所述的步骤(2)中,双螺杆挤出机自喂料口至挤出模头温度分别是190~210℃,200~230℃,210~230℃,220~230℃,220~240℃,主机转速是30~50赫兹。
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Denomination of invention: Heat-conducting resin composition and preparation method thereof Effective date of registration: 20191202 Granted publication date: 20180803 Pledgee: Chuzhou economic and Technological Development Corporation Pledgor: Shanghai Jieshijie New Materials (Group) Co., Ltd. Registration number: Y2019980000815 |
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