CN1671770A - 液晶聚合物组合物 - Google Patents
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Abstract
公开了液晶聚合物组合物,其可以熔体模塑,其含有全氟化聚合物、颗粒状芳族聚酰胺且任选含有中空玻璃或石英球,该液晶聚合物组合物通常具有低介电常数。它们特别可用作电连接器和其它采用高频信号的电子用途的基底。
Description
技术领域
含有全氟化聚合物、颗粒状芳族聚酰胺和任选中空玻璃或石英球的液晶聚合物组合物通常具有低介电常数,这使它们可以用作电子用途如电连接器的基底(substrate),特别是当这些用途涉及高频信号的时候。
背景技术
多种材料用作制造电连接器的基底。在涉及高频信号时,这些材料的一个特殊性能-介电常数是重要的。如果基底的介电常数太高,这些信号将被衰减到电子设备不能按设计工作的程度。因此,这些基底,特别在用于此类用途时,应具有尽可能低的介电常数。然而,令情况复杂的是在所述基底中还需要和/或希望具有其它性能,如良好的强度、耐高温性能、良好的阻燃性能和良好的成形性能等。由于改善一种特定性能往往会导致另一种(所需)性能变差,制备这样的组合物是一种挑战。因此,一直在寻求这样的组合物。
美国专利5,398,990描述了含有中空玻璃球和聚四氟乙烯的LCP组合物。未提及芳族聚酰胺的存在。
欧洲专利申请512,401描述了某些具有低介电常数的层合材料。该树脂组合物含有分子级多孔气溶胶而不是中空玻璃或石英球。
日本专利申请0455437描述了预浸渍材料,其由含氟塑料、中空玻璃球和可以是芳族聚酰胺的布或纸状材料制成。该材料可以用热固性树脂如环氧树脂饱和,但未提及LCP。
发明内容
本发明涉及一种组合物,其包含约5-约25重量%的颗粒状芳族聚酰胺,约5-约40重量%的颗粒状全氟化聚合物,0-约15重量%的中空玻璃或石英球,其余为液晶聚合物(LCP),其中重量百分数基于存在的所述颗粒状芳族聚酰胺、全氟化热塑塑料、中空玻璃或石英球和液晶聚合物的总量计。
发明详述
本文使用了某些术语,其中的一些是:
“颗粒状芳族聚酰胺”指的是平均最大尺寸不超过500μm,优选200μm,更优选低于100μm的芳族聚酰胺颗粒。所述颗粒可以是任意形状,例如短纤维、原纤维、纤条体、不规则、球形、盘状等。例如纤维、原纤维或纤条体的最大尺寸通常为其长度。“颗粒状芳族聚酰胺”还不包括织造或非织造织物或芳族聚酰胺纸形式的芳族聚酰胺,即使在任何这些类型材料中的芳族聚酰胺颗粒符合上述尺寸限制。然而,当组合物熔体成型时,组合物中的颗粒化颗粒状芳族聚酰胺之间可能会形成某些不定缠结。
“全氟化”聚合物指的是重复单元中不含有任何氢原子的聚合物,但是在例如端基中可以含有痕量的氢。
“热塑塑料”指的是熔点或玻璃化转变温度高于30℃,优选高于60℃的聚合物。为使熔点符合该标准,对于非液晶聚合物,熔融热应至少为2J/g。
“液晶聚合物”指的是当采用TOT测试或其任何适当的变型测试时呈各向异性的聚合物,如美国专利4,118,372中所描述,在此将其引入作为参考。
优选全氟化聚合物以约10-约30重量%的量存在。一般将其作为颗粒状材料加入组合物的其它成分中以有助于确保各种成分的均匀分布。优选的全氟化聚合物包括四氟乙烯(TFE)的均和共聚物。特定的优选全氟化聚合物包括聚四氟乙烯(PTFE)、TFE和六氟丙烯的共聚物,和TFE和全氟(甲基乙烯基醚)的共聚物。PTFE是特别优选的全氟化聚合物。可以以细粉末的形式从PTFE水分散体的制备中获得PTFE,这样的细粉末可用于制备本发明的组合物。虽然PTFE难以针对本发明目的进行熔融加工,仍将其当作热塑塑料。优选全氟化聚合物是热塑塑料。
适合于本发明的中空玻璃和石英(微)球可以从诸如3MCo.,St.Paul,MN,USA和PQ Corp.,Valley Forge,PA,USA的公司购得。它们一般具有约20μm-约75μm的直径。优选它们在组合物中的浓度为0-约10重量%。石英是中空微球优选的材料。可以用粘合增进剂涂覆所述球,如官能硅烷粘合增进剂(通常)为改进球和LCP之间的粘合力。
优选颗粒状芳族聚酰胺占组合物的约8-约22重量%。本文的所有优选重量百分数均基于所指成分(如权利要求1中)的总重计,任何优选的重量百分数可以与任何其它(优选)的重量百分数相结合。优选颗粒状芳族聚酰胺是“粉末”级的。该级别含有的颗粒大部分不是纤维状或原纤状的。所述芳族聚酰胺粉末通常具有2m2/g或更低的表面积,经常是0.2m2/g或更低。其可以通过研磨芳族聚酰胺来制备,参见例如美国专利5,474,82和5,811,042和Research Disclosure,May1996,第293页。优选这样的颗粒尺寸:在按照ASTM法D-1921-01测试法B进行测试时,至少90重量%,更优选95重量%的粉末能够通过No.100(150μm)筛。含有向热型LCP和粉末芳族聚酰胺的组合物具有特别良好(改进的)的物理性能,如拉伸和挠曲性能。对于粉末或任何其它颗粒状芳族聚酰胺形式而言,优选的芳族聚酰胺是聚(对苯二甲酰对苯二胺)。
可以采用典型的热塑塑料混合和加工技术来制备本文描述的组合物。例如,可以将所有成分向单或双螺杆挤出机进料(不必将各种成分同时或在挤出机的相同位置进料),采用挤出机的机械操作和/或加热器使LCP和任选的全氟化聚合物熔融并与其它成分混合。形成的组合物优选应是相当均匀的,颗粒状芳族聚酰胺、玻璃或石英球和全氟化聚合物被适当均匀地分散在LCP中。
LCP一般以连续相存在于组合物中。全氟化聚合物和/或芳族聚酰胺优选以非连续相存在于LCP连续相中。
其它成分如一般用在热塑塑料组合物中那些也可以存在,特别是少量地存在。这样的成分包括填料和增强剂、颜料、染料、抗氧化剂、润滑剂和成核剂。优选这些其它成分不会对组合物的重要性能造成不利且显著的影响。
一般,本发明的组合物可以熔体模塑,同时具有比其它典型LCP组合物更低的介电常数(特别是在如5GHz的较高频率下),且保持其它适当的物理性能例如拉伸强度和伸长率、挠曲强度和伸长率。它们经常还具有良好的阻燃性能,例如在1.59mm(1/16”)厚度下具有V-O的UL-94评级。这使它们特别可用于电气或电子部件,如电连接器,其中在高频用途中,降低的介电常数使低寄生损耗的快速通路成为可能,而且它们的强度性能对该用途而言是足够的。可以以常规技术如注塑、挤出等来实施熔体模塑。
本发明按如下测量了某些性能:
通过方法ASTM方法D3418测量了熔点和玻璃化转变温度。将熔融吸热峰处的温度作为熔点,转变的中点作为玻璃化转变温度。采用25℃/分钟的加热速率,对二次热测量了熔点和玻璃化转变温度。如果存在多于一个的熔点,则取最大的熔点作为聚合物的熔点。熔融吸热曲线下的面积作为熔融热。
通过ASTM方法D-150测量了介电常数(e’)、介电损耗(e”)和介质损耗角正切(e”/e’)。
在实施例中,采用ASTM方法D-638(采用应变仪)测量了拉伸强度和断裂伸长率,通过ASTM方法D-790测定了弯曲模量和弯曲强度,在1.82MPa载荷下通过ASTM方法D648测定了热挠曲温度(HDT)。通过ASTM方法D-257测量了电性能。
在实施例中,采用了以下的LCP(所有给出的比值均为摩尔份数):
A-氢醌50;4,4’-双酚50;对苯二甲酸70;2,6-萘二甲酸30;4-羟基苯甲酸320。
B-氢醌50;4,4’-双酚50;对苯二甲酸85;2,6-萘二甲酸15;4-羟基苯甲酸320。
C-氢醌50;4,4’-双酚50;对苯二甲酸87.5;2,6-萘二甲酸12.5;4-羟基苯甲酸320,还含有25ppm的钾离子。
通过美国专利5,110,896和5,397,502中描述的方法制备LCP,将此二专利引入作为参考。
实施例1-8
将指定为A、B或C的液晶聚合物与10重量%(实施例4中为20重量%)的Kevlar芳族聚酰胺树脂,R120型,或10重量%的1.5mm长Kevlar切断絮(实施例7和8)(二者均购自E.I.DuPont de Nemours&Co.,Wilmington,DE,USA),10重量%的中空玻璃球(3M ScotchliteGlass Bubbles,Grade 522,购自3M Co.,St.Paul,MN,USA),20重量%由DuPont以商品名MP1200粉末出售的Teflon粉末,0.25重量%的对苯二甲酸(仅实施例1),和0.20重量%的PE 190聚乙烯蜡(由Clariant Corp,Charlotte,NC出售)混合在一起。材料其余部分为液晶聚合物。将Kevlar粉末或絮和中空玻璃球以外的全部材料经由Werner&Pfleiderer(Stuttgart,Germany)制造的30mm bilobal双螺杆挤出机的进料区进料。将螺杆RPM设定在250。采用6oz.的HPM模塑机和以下的模塑条件将得到的混合产物成形为15.2cm×15.2cm×0.16cm的板(电加热模具):机筒温350℃,模具温度110℃,增压时间2秒,注射时间10秒,保压时间15秒,增压压力4.8MPa,注射压力3.5MPa,螺杆速度120RPM。
对所述板进行高频电性能测试,这些性能和每个实施例中所用的聚合物种类列于表1中。
在电性能以外,测试了挤出成拉伸样条后的实施例8的聚合物物理性能。这些物理性能总结如下:
拉伸强度/断裂伸长率=66.9MPa/2.42%
弯曲模量/弯曲强度4.70GPa/86.9MPa
针对0.16cm厚样条的UL-94燃烧时间(时间/评级)/HDT=(18.3秒/V-O)/250℃。
对比例A-D
将液晶聚合物A与如下成分混配(百分数是重量百分数):
对比例A和B-30%的玻璃纤维,0.20重量%的PE190和5%的TiO2:
对比例C和D-除了用30%的滑石粉代替30%的玻璃纤维之外与A和B相同。
将这些组合物成形为板状并测试高频电性能。所述性能列于表1中。
表1
实施例 | LCP | 样品厚度cm | 频率GHz | 介电常数DK | 介电损耗系数e″ | 介质损耗角正切e″/e′,DF |
1 | C | 0.15 | 5.2270 | 2.9130 | 0.0107 | 0.0037 |
2 | C | 0.16 | 5.2130 | 2.9900 | 0.0106 | 0.0035 |
3 | A | 0.17 | 5.1980 | 2.9550 | 0.0110 | 0.0037 |
4 | C | 0.16 | 5.2150 | 2.9670 | 0.0130 | 0.0044 |
5 | B | 0.16 | 5.2120 | 2.9690 | 0.0104 | 0.0035 |
6 | A | 0.17 | 5.206 | 2.974 | 0.0111 | 0.0038 |
7 | A | 0.16 | 5.176 | 3.372 | 0.0102 | 0.003 |
8 | A | 0.16 | 5.177 | 3.394 | 0.0104 | 0.0031 |
A | A | 0.16 | 5.082 | 4.147 | 0.0202 | 0.0049 |
B | A | 0.17 | 5.071 | 4.151 | 0.0197 | 0.0047 |
C | A | 0.16 | 5.146 | 3.701 | 0.0067 | 0.0018 |
D | A | 0.15 | 5.148 | 3.724 | 0.007 | 0.0019 |
实施例6-两块板的平均值。
Claims (15)
1、一种组合物,其包含约5-约25重量%的颗粒状芳族聚酰胺,约5-约40重量%的颗粒状全氟化聚合物,0-约15重量%的中空玻璃或石英球,其余为液晶聚合物,其中重量百分数基于存在的所述颗粒状芳族聚酰胺、全氟化热塑塑料、中空玻璃或石英球和液晶聚合物的总量。
2、权利要求1的组合物,其中所述颗粒状芳族聚酰胺是芳族聚酰胺粉末。
3、权利要求1的组合物,其中存在约10-约30重量%的所述全氟化聚合物。
4、权利要求1的组合物,其中所述全氟化聚合物是四氟乙烯的均或共聚物。
5、权利要求1的组合物,其中存在0-约10重量%的所述中空玻璃或石英球。
6、权利要求1的组合物,其中存在约8-约22重量%的所述颗粒状芳族聚酰胺。
7、权利要求2的组合物,其中所述颗粒状芳族聚酰胺是聚(对苯二甲酰对苯二胺)。
8、权利要求1的组合物,其中存在约10-约30重量%的所述全氟化聚合物,其中存在0-约10重量%的所述中空玻璃或石英球,且存在约8-约22重量%的所述颗粒状芳族聚酰胺。
9、权利要求2的组合物,其中所述颗粒状芳族聚酰胺是聚(对苯二甲酰对苯二胺)。
10、包含权利要求1组合物的电气或电子部件。
11、包含权利要求1组合物的电连接器。
12、包含权利要求8组合物的电气或电子部件。
13、包含权利要求8组合物的电连接器。
14、包含权利要求2组合物的电气或电子部件。
15、包含权利要求9组合物的电气或电子部件。
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US7744802B2 (en) * | 2004-06-25 | 2010-06-29 | Intel Corporation | Dielectric film with low coefficient of thermal expansion (CTE) using liquid crystalline resin |
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KR101148384B1 (ko) * | 2009-11-26 | 2012-05-21 | 삼성전기주식회사 | 기판 형성용 조성물, 및 이를 이용한 프리프레그 및 기판 |
TWI464245B (zh) * | 2012-06-27 | 2014-12-11 | Ticona Llc | 超低黏度之液晶聚合物組合物 |
JP2021109891A (ja) * | 2020-01-07 | 2021-08-02 | パナソニックIpマネジメント株式会社 | 液晶性樹脂組成物及び成形品 |
JP2021147476A (ja) * | 2020-03-18 | 2021-09-27 | Eneos株式会社 | 樹脂組成物および該樹脂組成物からなる樹脂成形品 |
CN113930084B (zh) * | 2021-09-18 | 2024-05-07 | 珠海万通特种工程塑料有限公司 | 一种液晶聚合物组合物及其应用 |
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JPH0455437A (ja) * | 1990-06-26 | 1992-02-24 | Matsushita Electric Works Ltd | 低誘電率積層板用プリプレグ |
US5466744A (en) * | 1990-11-05 | 1995-11-14 | General Electric Company | Polymerization of macrocyclic poly(alkylene dicarboxylate) oligomers |
US5110896A (en) * | 1990-12-10 | 1992-05-05 | E. I. Du Pont De Nemours And Company | Thermotropic liquid crystalline polyester compositions |
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US5474842A (en) * | 1991-08-20 | 1995-12-12 | Hoiness; David E. | Aramid particles as wear additives |
US5348990A (en) * | 1993-03-02 | 1994-09-20 | Hoechst Celanese Corp. | Low dielectric materials |
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US5397502A (en) * | 1993-06-10 | 1995-03-14 | E. I. Du Pont De Nemours And Company | Heat resistant liquid crsytalline polymers |
AU1524897A (en) * | 1996-01-05 | 1997-08-01 | E.I. Du Pont De Nemours And Company | Liquid crystalline polymer composition |
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US6388202B1 (en) * | 1997-10-06 | 2002-05-14 | Motorola, Inc. | Multi layer printed circuit board |
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CA2393259A1 (en) * | 2000-01-13 | 2001-07-19 | E.I. Du Pont De Nemours And Company | Liquid crystalline polymer compositions containing small particle size fillers |
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