CN1934176A - 填充纤维增强的热塑性复合材料 - Google Patents

填充纤维增强的热塑性复合材料 Download PDF

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CN1934176A
CN1934176A CNA2005800092835A CN200580009283A CN1934176A CN 1934176 A CN1934176 A CN 1934176A CN A2005800092835 A CNA2005800092835 A CN A2005800092835A CN 200580009283 A CN200580009283 A CN 200580009283A CN 1934176 A CN1934176 A CN 1934176A
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matrix material
glass
density
add
reinforced thermoplastic
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安德鲁·S·德·苏扎
布赖恩·C·伊斯汀
罗纳德·J·伊斯雷尔森
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3M Innovative Properties Co
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Abstract

含有中空泡的纤维增强的热塑性复合材料，意想不到地提供了低密度并保持强的物理特性。

Description

填充纤维增强的热塑性复合材料
发明领域
本发明涉及改进的纤维增强的热塑性树脂复合材料，尤其是由玻璃泡(glass bubbles)填充的纤维增强的复合材料。
背景技术
已知可将纤维混入热塑性复合材料以改进该热塑性材料的机械性能。例如，热塑性材料可以通过在其中混入纤维而得到增强，从而改进热塑性制品或膜的冲击强度，拉伸强度，拉伸和弯曲模量，和抗缩性。
还已经知道，可将中空粒子作为填料混入树脂组合物以减小热塑性制品或膜的密度，并获得与纤维相比更大的各向同性线性热膨胀系数和收缩特性。然而，通过中空粒子的混入获得的密度减小的代价是降低了复合材料希望的物理特性。
存在对改进的纤维增强的热塑性复合材料的需求。
发明简述
本发明提供了由中空玻璃微球填充的纤维增强的热塑性树脂复合材料。本发明的复合材料提供了较低的密度和强的物理机械特性的意想不到的结合，所述强的物理机械性能例如，抗冲击性，拉伸强度，拉伸和弯曲模量，减小的收缩性，和减小的吸水性。
意想不到地发现，通过由中空玻璃泡或微球进行填充，可显著降低纤维增强的热塑性树脂复合材料的密度，同时基本上不会明显降低该复合材料的拉伸强度和其他物理特性。因此可以以更轻而且具有希望强度的形式制备纤维增强的热塑性复合材料。
本发明可用于制备用于各种结构应用中的复合材料，如作为用于机动车中的部件。
简言之，本发明的复合材料包括一种或多种热塑性树脂，纤维增强填料，和中空玻璃泡或微球。在一些具体实施方式中，该复合材料可进一步包括其他添加剂，如增强所述复合材料中的树脂、纤维、泡、和其他组分的相容性的偶联剂或处理剂，阻燃剂，着色剂等。
适用于本发明的热塑性树脂的示例性例子包括：聚酰胺，热塑性聚酰亚胺(TPI)，聚酯，聚烯烃，尼龙，及其共混物和共聚物。示例性的例子包括：DuPont的ZytelTM 101L树脂，尼龙6，6树脂，和尼龙共混物(例如可购自GE的NORYL GTX，它是尼龙和聚苯醚的共混物)。
可以使用许多已知的纤维增强填料。适用于本发明的纤维增强填料的示例性例子包括：玻璃，石墨，KevlarTM纤维等。可部分地依据希望得到的复合材料具有的特性而选择所述填料。在一些情况下，可使用两种或更多种填料。
通常，本发明的复合材料将包括约7到约35重量百分比的所述纤维增强填料。可以使用更低的量，但可能倾向于不能足够调整物理性能。可以使用更高的量，但可能倾向产生过度装填的复合材料。
纤维增强填料可以进行表面处理以改进与树脂母体的相容性。例如，可使用硅偶联剂或钛酸酯偶联剂，例如氨基硅烷如氨丙基三乙氧基硅烷(“APS”)或N-2-(氨乙基)-3-氨丙基三甲氧基硅烷。市售的纤维增强的填料通常在其上具有偶联剂。
可使用许多已知的中空微球或泡，通常优选为玻璃。为改进复合材料加工过程中泡的留存(survival)以达到所希望的密度减小，通常优选使用高强度的玻璃泡。
在某些情况下，所述泡的绝大部分应表现出至少3,000PSI，优选为高于10,000PSI的均衡抗压强度，以经受热塑性混合和挤出操作。在某些具体实施方式中，当暴露于至少18,000PSI的均衡的抗压强度下，以经受造粒和注塑成型以及混合和挤出操作时，它们优选为将表现出高的可留存性。通常利用ASTM D3102-72；“Hydrostatic Collapse Strengthof Hollow Glass Microsphere”测量玻璃泡的强度。这种玻璃泡的示例性例子为3MTM ScotchliteTM S60HS Glass Bubbles，其为苏打-石灰-硼硅酸盐玻璃，并表现出18,000psi的均衡抗压强度，0.60g/cc的密度，和约30微米的平均直径。
通常，本发明的复合材料将包括约5到约20重量百分比的所述泡。若希望的话，可以使用更低的量，但将可能仅提供更有限的密度降低。可以使用更高的量，但是可能倾向导致复合材料的过度装填。
尽管需要的话，可用偶联剂对所述泡进行表面处理，以改进与树脂母体的相容性，意想不到的发现这种处理并未提供性能的明显改变，这与当将泡混入无纤维增强的树脂母体中时所观察到的情况不同。
可通过注塑成型、挤出、和其他已知的由热塑性聚合物形成制品的方法，将本发明的复合材料制备成制品。
具有良好拉伸特性的轻质部件的一些应用例子包括：减轻使用者疲劳和/或提高性能的运动产品，为燃料节约、改进加速或更高的最高速度、和减少燃料排放的运输工具(汽车，飞机等)的部件。
实施例
  代号   分子式，结构和/或名称   购自
Nylon 66   ZYTELTM101L：275℃时熔融指数为60g/10min，Tg为50℃，Tm为260-262℃，密度为1.14g/cm3 DuPont，Wilmington，DE
GF   玻璃纤维：PPGTM 3540，密度2.65g/cm3   PPG Industries，Shelby，NC
GM   玻璃泡：SCOTCHLITETM S60HS，密度为0.6g/cm3，18,000psi(124.0MPa)10％破坏强度 3M Company，St.Paul，MN
AEAPTMS   A-1120：N-2-(氨乙基)-3-氨丙基三甲氧基硅烷   OSI Specialties，Wilton，CN
APTES   A-1100：氨丙基三乙氧基硅烷 OSI Specialties
热解法二氧化硅   Cabot Corporation，GAorJ.M.Huber.Edison，NJ
表面处理
具体地，在表面处理之前用去离子水洗涤玻璃泡并干燥。洗涤之后，将热解法二氧化硅(高达2重量％)与所述的玻璃微球混合。将硅烷处理剂(APTES或AEAPTMS)溶于水(0.2-0.5重量％)。随后将溶液(1500g)装入Ross Mixer中(购自Charles Ross&Son Company，Hauppauge，NY)。然后以中等速度开始混合并缓慢加入玻璃微球(GM)。完成GM的添加后，继续另外混合该混合物15分钟。然后将得到的湿GM浆倒入铝盘并于80℃在烘箱中进行干燥。干燥后，将所述微球通过180微米筛进行筛选。通常处理后的GM收率大于90％。
复合材料的混合和成型
将所有样品在Berstorff Ultra Glide双螺杆挤出机(TSE；螺杆直径25mm；长径比为36∶1；购自Berstorff GmbH，Hannover，Germany)上混合，该挤出机装配有用于微球和玻璃纤维进料的顶部进料器，水浴和造粒附件。螺杆转速范围为140到160rpm。设定温度的范围为从200到575(93℃到302℃)，而实际值的范围为从500到575(93℃到260℃)。TSE生产能力约为101bs/hr。
然后，利用ASTM四模穴模具将测试样品在150吨Engel InjectionMolding Machine(购自ENGEL GmbH，Schwertberg，Austria)上成型。所用的螺杆直径为30mm，注塑压力保持在低于18,000psi(124Mpa)以最小化微球的破裂。
测试方法
拉伸模量
根据ASTM测试方法D-638测定拉伸模量并以Mpa表示。
最大拉伸模量
根据ASTM测试方法D-638测定拉伸模量并以Mpa表示。
弯曲模量
根据ASTM测试方法D-790测定弯曲模量并以Mpa表示。
最大弯曲强度
根据ASTM测试方法D-790测定最大弯曲强度并以Mpa表示。
断裂伸长率
根据ASTM测试方法D-638测定断裂伸长率并以％表示。
密度
使用购自Micromeritics，Norcross，Georgia的商品名为″ACCUPYC1330 PYCNOMETER″的全自动气体置换比重瓶，根据ASTMD-2840-69，″Average True Particle Density of Hollow Microspheres″来测定注塑成型复合材料材料的密度。
物理测量步骤
使用Micromeretics Accupyc 1330 Helium Pycnometer(购自Micromeritics Instrument Corporation，Norcross，GA)测量注塑成型复合材料样品的密度。利用表1中所列的ATSTM标准测试方法测定注塑成型复合材料的机械性能和热性能。
表1
  测试   代号   ASTM#
  拉伸模量(Mpa)   TM   D-638
  最大拉伸强度(Mpa)   TS   D-638
  弯曲模量(Mpa)   FM   D-790
  最大弯曲强度(Mpa)   FS   D-790
  断裂伸长率(Mpa)   EL   D-638
  Izod无缺口冲击(J/cm)   UI   D-4812
  Izod缺口冲击(J/cm)   NI   D-256
制备具有表2中组成的各种复合材料。
表2
实施例   硅烷(％加入) GM(wt％) GF(wt％)   尼龙(wt％)   模制件密度(g/cm3)
  C-1   未添加   0   33   67   1.39
  1   未添加   5   31   64   1.34
  2   未添加   10   30   60   1.29
  3   未添加   15   28   57   1.24
  4   未添加   20   26   54   1.19
  5*   AEAPTMS(0.5)   5   31   64   1.33
  6*   AEAPTMS(0.35)   10   30   60   1.27
  7*   AEAPTMS(0.5)   15   28   57   1.22
  8*   AEAPTMS(0.5)   20   26   54   1.17
  C-2   未添加   0   20   80   1.27
  9   未添加   5   19   76   1.22
  10   未添加   10   18   72   1.18
  11   未添加   15   17   68   1.14
  12   未添加   20   16   64   1.10
  13*   APTES(0.5)   5   19   76   1.23
  14   APTES(0.35)   10   18   72   1.17
  15   AEAPTMS(0.5)   15   17   68   1.14
  16   AEAPTMS(0.5)   20   16   64   1.08
  C-3   未添加   0   10   90   1.20
  17   未添加   5   10   85   1.16
  18   未添加   10   9   81   1.11
  19   未添加   15   8   77   1.07
  20   未添加   20   8   72   1.03
  21   AEAPTMS(0.5)   5   10   85   1.15
  22   AEAPTMS(0.5)   10   9   81   1.11
  23   AEAPTMS(0.5)   15   8   77   1.07
  24   AEAPTMS(0.5)   20   8   72   1.03
*如前述洗涤GMs。
根据上面说明的步骤评价该复合材料并得到表3所列的结果。
表3
  例   TS(Mpa)   TM(Mpa)   EL(％)   FS(Mpa)   FM(Mpa)   UI(J/cm)   NI(J/cm)
  C-1   187   2567   8.9   280   9266   6.3   1.1
  1   178   3135   8.7   260   9607   7.0   1.4
  2   179   3240   9.4   239   9000   7.4   0.9
  3   149   3156   7.7   226   9786   6.8   1.1
  4   145   3230   7.6   203   9545   5.8   1.1
  5*   192   2672   9.2   272   9223   7.2   1.2
  6*   183   3256   9.4   254   8875   7.5   0.9
  7*   178   2834   8.8   246   8955   6.3   0.8
  8*   166   3141   8.9   235   8971   5.9   1.1
  C-2   117   3175   7.0   196   6060   3.9   0.8
  9   98   2401   6.3   189   6393   4.3   0.9
  10   131   2993   8.8   184   6244   4.0   0.5
  11   117   2617   7.1   174   6868   4.2   0.9
  12   111   2553   6.9   160   6965   4.5   0.8
  13*   126   2393   7.3   214   6693   4.3   1.1
  14   136   2715   8.3   207   6261   3.7   0.5
  15   127   3532   7.4   196   6371   3.5   0.9
  16   129   2528   7.8   199   6864   3.9   0.7
  C-3   78   1727   6.2   147   4495   2.8   0.6
  17   84   1861   6.5   140   4428   2.5   0.7
  18   83   1998   6.3   136   4706   2.5   0.6
  19   76   2035   5.8   128   4800   2.3   0.6
  20   79   2163   6.0   116   4997   2.4   0.4
  21   76   1885   5.9   139   4323   2.6   0.6
  22   82   1933   6.2   153   4652   2.7   0.6
  23   85   2049   6.1   156   4955   2.8   0.6
  24   96   2101   7.0   158   5047   2.5   0.6
*如前述洗涤GMs。

Claims (6)

1.一种复合材料，包括一种或多种热塑性树脂，一种或多种纤维增强填料，和中空微球。
2.权利要求1的复合材料，其中所述的树脂选自：聚酰胺、热塑性聚酰亚胺(TPI)、聚酯、聚烯烃、尼龙、及其共混物和共聚物。
3.权利要求1的复合材料，其中所述的纤维增强填料选自玻璃、石墨、和KevlarTM纤维。
4.权利要求1的复合材料，其中所述的复合材料包括从7到35重量百分比的所述纤维增强填料。
5.权利要求1的复合材料，其中所述的微球是玻璃泡。
6.权利要求1的复合材料，其中所述的复合材料包括从5到20重量百分比的所述泡。
CNA2005800092835A 2004-03-22 2005-03-22 填充纤维增强的热塑性复合材料 Pending CN1934176A (zh)

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