CN1144503A - 具有涂碳的高能表面的保护膜 - Google Patents

具有涂碳的高能表面的保护膜 Download PDF

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CN1144503A
CN1144503A CN95192302A CN95192302A CN1144503A CN 1144503 A CN1144503 A CN 1144503A CN 95192302 A CN95192302 A CN 95192302A CN 95192302 A CN95192302 A CN 95192302A CN 1144503 A CN1144503 A CN 1144503A
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coating
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J·R·瓦格纳
E·M·芒特第三
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ExxonMobil Oil Corp
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Abstract

用等离子增强化学蒸气沉积技术制备一种涂覆碳的聚合物薄膜。将具有至少一个外露的高能表面的非晶形尼龙层粘附于聚合物基材上。然后在等离子体的存在下通过可分解的前体的汽相淀积将碳层沉积在该外露的高能表面。

Description

具有涂碳的高能表面的保护膜
本发明涉及保护膜，具体涉及具有至少一个用于接收碳层的外露的高能表面的保护膜。
众所周知碳层可提供保护特性。例如，碳层能阻止分子(如水和氧)通过。因此，通常将碳层涂敷于基材(如聚合物薄膜)，这些基材如果不涂敷碳层，则不具有这些保护特性。带有该碳层的薄膜通常称作保护膜。
碳层可以通过各种技术沉积在基材上。一种优选的技术是等离子增强化学蒸气沉积(PECVD)，运用该技术可以使碳沉积在低温基材(如聚合物薄膜)上。尤其是，运用该技术可以使碳的沉积在比其它沉积方法中所需的更低的反应室温度下进行。结果，该较低的反应室温度使碳可以沉积在低温基材上。
然而，该PECVD方法是一种相对较慢和时间较长的方法，因此在许多情况下该技术是无实用价值的。所以，在该技术领域需要有一种方法能提高PECVD保护膜的生产速度，同时保持所需的对涂碳基材的保护性能。
本发明根据现有技术的需要，提供一种用于生产具有保护特性的聚合物薄膜的方法。该方法包括在等离子体的存在下，通过可分解的前体的汽相淀积将碳层沉积在外露的非晶形尼龙层的高能表面上的步骤。
较好的是，将非晶形尼龙层粘附在聚合物基材上。随后较好的是在双频率的条件下，通过PECVD将碳沉积在外露的高能表面上。
该方法较好的是包括将约13.5MHz的主要频率施加于位于反应室的第一电极以产生等离子体以及将90kHz至450kHz的次要频率施加于位于该反应室的第二电极以促进碳层沉积在外露的高能表面的步骤。
本发明也提供了一种用于提高保护膜的生产速度的方法。该方法包括将具有至少一个外露的高能表面的非晶形尼龙层粘附于聚合物基材上的步骤。该方法还包括在等离子体的存在下通过可分解的前体的汽相淀积将碳层沉积在该外露的高能表面的步骤。
本发明还提供了一种具有保护特性的聚合物薄膜。该薄膜是用在等离子体的存在下通过可分解的前体的汽相淀积将碳层沉积在该外露的非晶形尼龙层的高能表面的方法制备的。该非晶形尼龙层较好的是粘附在聚合物基材上。
作为本发明的结果，制备涂碳聚合物薄膜所需的时间大大减少，从而提高了PECVD技术的实用价值。并且，得到的薄膜对于氧和水的透过具有更好的保护作用。
本发明提供了制备具有保护特性的聚合物薄膜的方法。该方法包括在等离子体的存在下通过可分解的前体的汽相淀积将碳层沉积在外露的聚合物层的高能表面的步骤。
在一个较好的实例中，非晶形尼龙层粘附在聚合物基材上。由该尼龙层的外露表面提供上述的高能表面。该高能表面接收沉积的碳。
非晶形尼龙层可以用现有技术中已知的各种技术粘附在该基材上。例如，可以使用粘合剂将该尼龙层层压在聚合物基材上。一个特别优选将尼龙层固定在聚合物基材上的方法是通过将聚合物材料与非晶形尼龙共挤塑而进行的，由此得到在至少一面上具有非晶形尼龙层的聚合物基材。典型的是使用粘结层将非晶形尼龙粘附在聚合物基材上。例如，可以使用如苹果酸酐改性的聚丙烯之类的材料作为粘结层。一种这样的市售产品为AtmerQF-500A。
本发明中使用的非晶形尼龙较好的是基于六亚甲基二胺和间苯二酸与对苯二酸的混合物的非晶形共聚多酰胺。一种这样的市售产品为DupontPA-3426。
非晶形尼龙层具有高能表面，该表面能促进沉积的碳在其上的粘附。尤其是非晶形尼龙的外露表面与其它聚合物相比表现出高的“湿润性”。湿润性会影响材料之间紧密接触的能力。在这方面已经得到证明，即将具有高能表面的聚合物层(例如非晶形尼龙)应用于聚合物基材，大大减少了通过PECVD沉积碳层所需的时间。因此设想其它具有相同湿润性的聚合物也能有效地提供用于接收碳层的高能表面。
本发明中设想的聚合物基材的实例包括聚丙烯、聚乙烯、双轴尼龙和聚酯。然而，在本发明中也可以使用其它基材，只要这些基材与呈现高能表面的材料是相容的。
本发明也提供了一种用于提高保护膜的生产速度的方法。该方法包括将具有至少一个外露的高能表面的聚合物层粘附在聚合物基材上，以及随后的在等离子体的存在下通过可分解的前体的汽相淀积将碳层沉积在该外露的高能表面步骤。同样，该聚合物层较好为非晶形尼龙。
如上所述，碳层是通过可分解的前体的沉积形成的。使用含有1至20个碳原子的烃类气体作为可分解的前体。乙炔是其中优选的前体气体。
该可分解的前体一导入等离子体，该前体气体即分解并随后沉积在外露的高能表面成为非晶形碳层。该碳层的厚度可为10至5000A。非晶形碳层的厚度主要取决于沉积的时间。
本发明中的等离子体是通过将主要射频施加于第一电极而产生的。该射频激发流经该室的气体混合物，从而形成等离子体。该气体混合物较好的是上述前体气体(如乙炔)和惰性气体(如氩)的混合物。
适用于PECVD的装置是可以购得的。这类装置通常包括一个用于接收基材的腔体。该装置还包括一个用于将该腔体抽空的真空泵，用于在控制的条件下将气体混合物导入该腔体的装置，以及用于在腔体内产生等离子体的装置。
在一个特别好的实例中，该等离子体产生装置包括放置在两端的第一和第二电极，它们可一起用于将独立的双能源导入反应室中。13.56MHz的主要射频施加于第一电极，90kHz至450kHz的次要射频施加于第二电极。较好的是，该腔体用作两种射频的接地端。
主要射频产生等离子体(通过激发气体混合物)，而次要频率能通过激发沉积的碳分子而促进碳在高能表面的沉积。该理论得到以下事实的支持，即施加该第二种射频时观察到等离子体中的明显变化。
也可以设想其它的产生等离子体的装置。例如可在电极间施加2.45GHz的主要射频。另外，也可用激光或磁场激发该气体混合物。
该腔体也包括基材支撑片用于支撑欲涂覆的聚合物基材。该基材支撑片较好的是与第二电极结合成一体。另外，基材支撑片可以包括平的或弧形的支撑表面。预计使用弧形支撑表面将促进本发明的工业生产。
下面的实施例说明了本发明。实施例1
制备两种对照薄膜。将长为11″、宽为15.5″、厚为1密耳的取向聚丙烯薄膜置于与第二电极连接的长为10″、宽为15.5″的基材支撑片上。该基材支撑片包括曲率半径为40″的弧形表面。将该薄膜沿其长度伸出基材支撑片之外以使该薄膜固定在该支撑片上。
将腔体中的压力降至1mTorr。然后以100sccm的流速将乙炔/氩气体混合物导入该腔体，混合物中70％为乙炔。使用位于真空泵入口处的闸阀将腔体内的压力升至100mTorr的反应压力。将100瓦特功率的13.5MHz主要频率施加于第一电极，将25瓦特功率的95kHz次要频率施加于第二电极。
对基材涂覆300秒钟左右。然后停止加入气体混合物，腔体的压力再次降至1mTorr。然后通过放入干燥的氮气，解除腔体内的真空，取出已涂覆的基材。
然后对两种对照薄膜进行测定。第一种对照薄膜的氧透过率(TO2)在23℃及0％相对湿度下为0.4cc O2/100in2/atm/24hr，水蒸气透过率(WVTR)在100°F及90％相对湿度下为0.02gH2O/100in2/atm/24hr。第二种对照薄膜的氧透过率在23℃及0％相对湿度下为0.6ccO2/100in2/atm/24hr，水蒸气透过率在100°F及90％相对湿度下为O.09gH2O/100in2/atm/24hr。
因此，对照薄膜的平均氧透过率在23℃及0％相对湿度下为0.5ccO2/100in2/atm/24hr，平均水蒸气透过率在100°F及90％相对湿度下为0.055gH2O/100in2/atm/24hr。实施例2
根据本发明通过非晶形尼龙与聚丙烯共挤塑得到一种基片然后使其双轴取向而制备保护膜。使用Dupont nylon PA-3426的树脂颗粒以及AtmerQF-500A粘结层。取向的薄膜的厚度约为1mil，非晶形尼龙层为薄膜总厚度的约6％或0.06mil。
将长为约11″、宽为15.5″、厚为1密耳的聚合物样品置于实施例1中所述的与第二电极连接的基材支撑片上。
将腔体中的压力降至1mTorr。然后以60sccm的流速将乙炔/氩气体混合物导入该腔体，混合物中约83％为乙炔。使用位于真空泵入口处的闸阀将腔体内的压力升至100mTorr的反应压力。将100瓦特功率的13.5MHz主要频率施加于第一电极，将25瓦特功率的95kHz次要频率施加于第二电极。
对基材涂覆60秒钟左右。然后停止加入气体混合物，腔体的压力再次降至1mTorr。然后通过放入干燥的氮气，解除腔体内的真空，取出已涂覆的基材。
然后对该聚合物样品进行测定。该样品薄膜的氧透过率在23℃及0％相对湿度下为0.42ccO2/100in2/atm/24hr，水蒸气透过率在100°F及90％相对湿度下为0.024gH2O/100in2/atm/24hr。
改变试验条件制备其它的聚合物样品。所有聚合物样品(即样品1-8)的测定结果列于下表中：
 样品   TO2   WVTR     压力(mTorr)     流C2H2   量Ar  主要功率(瓦特)  次要功率(瓦特)   时间(sec.)
对照1对照2样品1样品2样品3样品4样品5样品6样品7样品8   0.40.60.420.180.110.100.180.260.070.09   0.020.090.0240.0050.0150.0240.0200.0620.0360.051     100100100100100100100100150100     70705050505050505050   30301010101010101010     10010010050757575757550     25252525252525252525    3003006060604530153030
TO2：23℃及0％R.H.下cc/100in2/atm/24hr
WVTR：100°F及90％R.H.下g/100in2/atm/24hr
流量：标准立方厘米(sccm)
从上面所列的测定数据中可以明显看出，保护膜可以通过将碳沉积在非晶形尼龙层的外露的高能表面而制备。特别重要的是该保护膜的生产速度可以提高10倍，即涂覆时间从300秒左右减少至约15至60秒。同样重要的是得到的薄膜的氧透过率明显减小，同时改善了或至少保持水蒸气透过率的水平。

Claims (9)

1.一种具有保护特性的聚合物薄膜，该薄膜含有非晶形尼龙层，在该非晶形尼龙层的外露的高能表面上沉积碳层，该碳层的沉积较好的是在等离子体的存在下，通过可分解的前体的汽相淀积而进行的。
2.如权利要求1所述的聚合物薄膜，其特征在于该尼龙层是粘附于聚合物基材或是与聚合物基材共挤塑的。
3.一种制备具有保护特性的聚合物薄膜的方法，该方法包括在等离子体的存在下通过可分解的前体的汽相淀积将碳层沉积在非晶形尼龙层的外露的高能表面。
4.如权利要求3所述的方法，其特征在于该沉积是在双频率的条件下完成的。
5.如权利要求3或4所述的方法，其特征在于该沉积步骤包括将主要的射电频率施加于位于反应室的第一电极以产生等离子体以及将90kHz至450kHz的次要频率施加于位于该反应室的第二电极以促进碳层沉积在外露的高能表面。
6.如权利要求3、4或5所述的方法，其特征在于该第二电极包括基材支撑片，将非晶形尼龙层置于该基材支撑片上以接收碳层沉积在外露的高能表面上。
7.如前面的权利要求中任何一项所述的方法，其特征在于可分解的前体包括含有1至20个碳原子的烃类。
8.如权利要求7所述的方法，其特征在于该烃类包括乙炔。
9.使用非晶形尼龙层，在该层龙层的外露的高能沉积碳涂覆层，以提高制备具有保护特性且包括较好地在等离子体的存在下，通过可分解的前体的汽相淀积而沉积的碳层的聚合物薄膜的生产速度。
CN95192302A 1994-04-01 1995-02-22 具有涂碳的高能表面的保护膜 Pending CN1144503A (zh)

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CA2183664A1 (en) 1995-10-12
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