CN112175220B - 耐高温的改性聚丙烯薄膜及其制备方法和应用 - Google Patents

耐高温的改性聚丙烯薄膜及其制备方法和应用 Download PDF

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CN112175220B
CN112175220B CN202010913566.9A CN202010913566A CN112175220B CN 112175220 B CN112175220 B CN 112175220B CN 202010913566 A CN202010913566 A CN 202010913566A CN 112175220 B CN112175220 B CN 112175220B
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polypropylene film
modified polypropylene
temperature
ald
precursor
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CN112175220A (zh
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谭启
宋光辉
吴旭东
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Guangdong Israel Institute Of Technology
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Guangdong Israel Institute Of Technology
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Priority to CN202010913566.9A priority Critical patent/CN112175220B/zh
Priority to US17/038,210 priority patent/US11597808B2/en
Priority to EP20199355.7A priority patent/EP3965127A1/en
Priority to JP2020170584A priority patent/JP7166317B2/ja
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Abstract

本发明属于薄膜材料领域，公开了耐高温的改性聚丙烯薄膜及其制备方法和应用。该改性聚丙烯薄膜包括聚丙烯薄膜和聚丙烯薄膜表面的氧化物层和/或氮化物层；氧化物层或氮化物层的厚度为20‑500nm。利用ALD技术在聚丙烯薄膜表面沉积适当厚度的氧化物层或氮化物层可显著提高聚丙烯薄膜的热稳定和高温耐电压性能。该改性聚丙烯薄膜具有耐高温性能，例如耐150℃的高温，在高温下形变量极小，且在高温下能承受高击穿电压，例如在140℃下改性聚丙烯薄膜可承受的电压为580kV/mm，该改性聚丙烯薄膜在对温度要求高的电子产品领域，例如电容器领域具有广泛的应用。

Description

耐高温的改性聚丙烯薄膜及其制备方法和应用
技术领域
本发明属于薄膜材料领域，特别涉及耐高温的改性聚丙烯薄膜及其制备方法和应用。
背景技术
聚丙烯(PP)是一种具有广泛应用的廉价高分子材料。除了用于水净化、医疗卫生用品、电池隔膜以外，致密的PP膜还在食品工业、包装、高压绝缘以及储能电容器等方面具有重要的作用。目前PP已成为建立现代化世界最重要的聚合物之一。许多功能化、复合型的PP材料在获得物理和化学改性后作为工程塑料也有利于工业、商业等应用。其中薄膜电容器对PP薄膜的依赖性尤为突出。由于该类电容器具有非常高的功率密度、极大的充放电速率、超长的使用寿命、自愈能力和稳定性，在新型能源、高速铁路运输、高压输送、电动汽车、石油勘探、航空航天以及电磁武器等高端技术领域极为重要。聚丙烯薄膜在经过双向拉伸后成为双向拉伸聚丙烯薄膜(BOPP)，BOPP显示很高的耐电压性能(击穿强度)和机械强度，是电容器技术不可多得的首选薄膜材料。然而，目前改性薄膜材料受制于较低的最高工作温度(90-105℃)，尤其是在高温端出现巨大的尺寸变化和较低的耐电压能力，因此无法满足广大高温领域应用的需要，有机薄膜和电容器工业必须进一步创新，提高有机薄膜的性能，改进相关技术方案。
PP是一种柔软且易弯曲的材料，熔点在160-175℃之间，相对较低。虽然填充无机粉料或纤维制成复合材料可以增强机械强度，但同时会失去柔软性和耐电压的绝缘性能。这类复合材料也不再能做成超薄的薄膜材料去制备高性能电容器。有学者试图通过改变PP的分子链末端的官能团，提高其介电常数或电容量，但介电损耗和薄膜制备的成本和工艺难度也同时极大地增加。双向拉伸提高PP薄膜的结晶度和取向是传统公认的提高介电耐电压强度的方法，已经达到60-70％，继续提升的空间已经很有限(参见文献T.C.Chung,Prog.Polym.Sci.2002,27,39)。目前欧洲和日本的薄膜制造公司试图通过进一步地增加PP的结晶度和结晶工业控制来适当地提升其工作温度，但是至今还没有成功，没有产品投入市场。与此同时聚丙烯原料公司也试图通过添加剂和减少杂质含量改进其性能，但是尝试还处于研究阶段。
此外，在过去的10年中，国际上大力改进BOPP的生产工艺，进一步降低薄膜厚度(现已降到2微米)。这样超薄的BOPP更面临表面粗造度和缺陷以及厚度的非均匀性问题。总之，高温尺寸不稳定性，在高温下不能承受高击穿电压是聚丙烯薄膜的主要缺点。
因此，希望提供一种耐高温的改性聚丙烯薄膜及其制备方法。
发明内容
本发明旨在至少解决上述现有技术中存在的技术问题之一。为此，本发明提出耐高温的改性聚丙烯薄膜及其制备方法，本发明所述改性聚丙烯薄膜具有耐高温性能(例如150℃以上的高温)，在高温下依然形变量极小、具有良好的机械性能，且在高温下能承受高击穿电压。
因此，本发明的第一方面提供耐高温的改性聚丙烯薄膜。
具体的，耐高温的改性聚丙烯薄膜，包括聚丙烯薄膜和聚丙烯薄膜表面的氧化物层和/或氮化物层；所述氧化物层或氮化物层的厚度为20-500nm。
优选的，所述氧化物层或氮化物层的厚度为30-300nm；进一步优选的，所述氧化物层或氮化物层的厚度为40-200nm。
优选的，所述氧化物层由铝的氧化物、钛的氧化物、锌的氧化物、硅的氧化物、锆的氧化物、钽的氧化物、铌的氧化物、镁的氧化物、钙的氧化物、铁的氧化物、钛酸锶或钛酸钡中的至少一种构成。
进一步优选的，所述氧化物层由Al2O3、TiO2-x、TiO2、Ti2O3、ZnO、SiO2、ZrO2、Ta2O5、Nb2O5、MgO、Fe2O3、SrTiO3或BaTiO3中的至少一种构成，其中0<x<1。
优选的，氮化物层由铝的氮化物、钛的氮化物、硼的氮化物、硅的氮化物或钽的氮化物中的至少一种构成。
进一步优选的，所述氮化物层由AlN、TiN、BN、Si3N4或TaN中的至少一种构成。
优选的，所述聚丙烯薄膜的厚度为0.5-50μm；进一步优选的，所述聚丙烯薄膜的厚度为1-20μm。
优选的，所述聚丙烯薄膜的单面或双面含氧化物层和/或氮化物层。
本发明的第二方面提供上述耐高温的改性聚丙烯薄膜的制备方法。
具体的，上述耐高温的改性聚丙烯薄膜的制备方法，包括以下步骤：
用ALD(原子层沉积)、PVD(物理气相沉积)、PECVD(等离子体增强化学的气相沉积法)、e-beam(电子束蒸发)技术在聚丙烯薄膜薄膜表面沉积氧化物层或氮化物层，制得所述改性聚丙烯薄膜。
优选的，用ALD技术在聚丙烯薄膜薄膜表面沉积氧化物层或氮化物层，制得所述改性聚丙烯薄膜。用ALD技术制得的改性聚丙烯薄膜的耐高温性能优于用PVD、PECVD、e-beam技术制得的改性聚丙烯薄膜的耐高温性能。
优选的，用ALD技术在聚丙烯薄膜薄膜表面沉积氧化物层或氮化物层，制得所述改性聚丙烯薄膜的具体过程为：
将聚丙烯薄膜置于ALD的反应腔体中，抽真空，然后升温，通入载气，将至少两种前驱体交替通入反应腔体中进行反应，即制得所述改性聚丙烯薄膜；所述前驱体包括提供金属元素或Si的前驱体和提供氧或氮元素的前驱体。
优选的，所述金属元素选自Al、Ti、Zn、Zr、Ta、Nb、Mg、Fe、Sr或Ba中的至少一种。
优选的，所述抽真空的真空度为250mTorr以下。
优选的，所述升温的温度不超过100℃；优选的，所述升温的温度为60-100℃(该温度即可避免聚丙烯薄膜变形，又能有助于反应生成氧化物层或氮化物层)。在通入两种前驱体前，ALD的反应腔体在不超过100℃的温度下保温3-6分钟。
优选的，所述载气为惰性气体；进一步优选的，所述载气为氩气。
优选的，所述载气在整个ALD过程中流速保持恒定，为5-15sccm，优选为8-10sccm。
优选的，每一次每种前驱体的脉冲时长为21-200毫秒；每一次前驱体脉冲之后惰性气体的冲洗时长为3-6秒钟。
优选的，为保证聚丙烯薄膜在进入沉积腔之后保持平整，在沉积氧化物层或氮化物层之前，需要用离子风机对聚丙烯薄膜表面进行除静电处理。所采用的离子风机为Tronovo品牌TR7045型号，需要在室温下对每片200cm2的聚丙烯薄膜吹3-5秒钟，聚丙烯薄膜薄膜距离风口25-30cm。
具体的，ALD反应腔体中，在反应起始的时候，气态的提供金属元素或Si的前驱体分子首先被氩气流带向聚丙烯薄膜，通过吸附作用滞留于聚丙烯薄膜表面，然后氩气将剩余的提供金属元素或Si的前驱体分子清洗带走，接下来气态的提供氧或氮元素的前驱体分子被氩气流带到聚丙烯薄膜表面与已经停留在那里的提供金属元素或Si的前驱体分子发生反应，生成固态的氧化物或氮化物和气态的副产物，然后剩余的提供氧或氮元素的前驱体分子和气态副产物一并被氩气流清洗带走，ALD的第一周到此结束。接下来的ALD的第二周当中，提供金属元素或Si的前驱体分子和提供氧或氮元素的前驱体分子先后被氩气流交替带到聚丙烯薄膜表面，与先前通过反应或者吸附留在聚丙烯薄膜表面的另一种前驱体分子发生反应。在生成气态副产物的同时，使得金属或Si和氧或氮交替被逐层沉积在聚丙烯薄膜表面。两种前驱体交替通入到ALD反应腔体中，即每种前驱体以脉冲的形式通入。在进行一定时长的两种前驱体脉冲之间，均需要进行一定时长的惰性气体清扫，以带走副产物和剩余反应物。所沉积的氧化物层或氮化物层的厚度，与ALD总的周数(即总时长)总体上成正比，与ALD的温度反应动力特性关系密切，与前驱体脉冲和惰性气体冲洗的时长亦存在一定关系。
用上述ALD技术在聚丙烯薄膜薄膜表面沉积氧化物层或氮化物层，制得所述改性聚丙烯薄膜的方法也适用于制备改性热塑性薄膜。
优选的，所述改性热塑性薄膜包括改性聚氯乙烯薄膜、改性聚苯乙烯薄膜、改性聚酯薄膜、改性聚碳酸酯薄膜、改性聚奈二甲酸已二醇酯薄膜或改性聚偏氟乙烯薄膜中的任意一种。制得的改性热塑性薄膜的性能与改性聚丙烯薄膜的性能相似。
本发明的第三方面提供上述耐高温的改性聚丙烯薄膜的应用。
上述耐高温的改性聚丙烯薄膜在电子产品中的应用。
优选的，所述电子产品为电容器。
发明人意外的发现，利用ALD技术在聚丙烯薄膜表面沉积适当厚度的氧化物层或氮化物层可显著提高聚丙烯薄膜的热稳定，更意外地发现本发明制得的改性聚丙烯薄膜具有良好的高温耐电压性能。
相对于现有技术，本发明的有益效果如下：
(1)本发明所述改性聚丙烯薄膜具有耐高温性能(例如150℃以上的高温)，在高温下依然形变量极小、具有良好的机械性能，且在高温下能承受高击穿电压(例如在140℃下改性聚丙烯薄膜可承受的电压为580kV/mm)。
(2)本发明制得的改性聚丙烯薄膜在对温度要求高的电子产品领域，例如电容器领域具有广泛的应用。
附图说明
图1为实施例1制得的改性聚丙烯薄膜的尺寸随温度变化图；
图2为实施例1制得的改性聚丙烯薄膜的储存模量随温度变化图；
图3为实施例1制得的改性聚丙烯薄膜的XRD谱图随温度变化图；
图4为实施例1制得的改性聚丙烯薄膜的直流电压击穿强度随温度变化图；
图5为实施例2制得的改性聚丙烯薄膜的收缩率随温度变化图；
图6为实施例3制得的改性聚丙烯薄膜的尺寸随温度变化图；
图7为实施例1、实施例3、实施例4和实施例5ALD沉积800周制得的改性聚丙烯薄膜在150℃下保温半小时后的收缩率情况图。
具体实施方式
为了让本领域技术人员更加清楚明白本发明所述技术方案，现列举以下实施例进行说明。需要指出的是，以下实施例对本发明要求的保护范围不构成限制作用。
以下实施例中所用的原料、试剂或装置如无特殊说明，均可从常规商业途径得到，或者可以通过现有已知方法得到。
以下采用型号为GEMSTAR TX型热ALD设备进行改性聚丙烯薄膜的制备。以下实施例所用到的国产聚丙烯薄膜CPP是在国内商业化的聚丙烯薄膜，进口聚丙烯薄膜HCPP是国外高结晶度的聚丙烯薄膜。
实施例1：耐高温的改性聚丙烯薄膜的制备
耐高温的改性聚丙烯薄膜，包括国产聚丙烯薄膜CPP和国产聚丙烯薄膜CPP表面的Al2O3层；Al2O3层的厚度为20-200nm。
上述耐高温的改性聚丙烯薄膜的制备方法，包括以下步骤：
将聚丙烯薄膜至于ALD的反应腔体中，抽真空至250mTorr，然后升温至90℃，通入氩气，氩气的流速为10sccm，将三甲基铝(TMA)和水(H2O)前驱体交替通入反应腔体中进行反应，每一周ALD过程由如下步骤组成：TMA脉冲、氩气冲洗、H2O脉冲、氩气冲洗，时间分别为21毫秒、6秒、21毫秒、6秒，即制得改性聚丙烯薄膜。
利用本实施例的制备方法分别制得ALD沉积200周(即每一周ALD过程循环200次)、400周(即每一周ALD过程循环400次)和2000周(即每一周ALD过程循环2000次)的改性聚丙烯薄膜。沉积的周数越大，Al2O3层的厚度越厚。
实施例2：耐高温的改性聚丙烯薄膜的制备
实施例2与实施例1的区别仅在于，将国产聚丙烯薄膜CPP用进口聚丙烯薄膜HCPP替代，其余制备方法与实施例1相同。
利用本实施例的制备方法分别制得ALD沉积400周、800周和2000周的改性聚丙烯薄膜。沉积的周数越大，Al2O3层的厚度越厚。
实施例3：耐高温的改性聚丙烯薄膜的制备
耐高温的改性聚丙烯薄膜，包括国产聚丙烯薄膜CPP和国产聚丙烯薄膜CPP表面的TiO2层；TiO2层的厚度为20-200nm。
上述耐高温的改性聚丙烯薄膜的制备方法，包括以下步骤：
将聚丙烯薄膜至于ALD的反应腔体中，抽真空至250mTorr，然后升温至100℃，通入氩气，氩气的流速为10sccm，将异丙醇钛(TIP)和水(H2O)前驱体交替通入反应腔体中进行反应，每一周ALD过程由如下步骤组成：TIP脉冲、氩气冲洗、H2O脉冲、氩气冲洗，时间分别为200毫秒、6秒、200毫秒、6秒，ALD沉积800周，即制得改性聚丙烯薄膜。
实施例4：耐高温的改性聚丙烯薄膜的制备
耐高温的改性聚丙烯薄膜，包括国产聚丙烯薄膜CPP和国产聚丙烯薄膜CPP表面的ZnO层；ZnO层的厚度为20-200nm。
上述耐高温的改性聚丙烯薄膜的制备方法，包括以下步骤：
将聚丙烯薄膜至于ALD的反应腔体中，抽真空至250mTorr，然后升温至90℃，通入氩气，氩气的流速为10sccm，将二乙基锌(DEZ)和水(H2O)前驱体交替通入反应腔体中进行反应，每一周ALD过程由如下步骤组成：DEZ脉冲、氩气冲洗、H2O脉冲、氩气冲洗，时间分别为200毫秒、6秒、200毫秒、6秒，ALD沉积800周，即制得改性聚丙烯薄膜。
实施例5：耐高温的改性聚丙烯薄膜的制备
耐高温的改性聚丙烯薄膜，包括国产聚丙烯薄膜CPP和国产聚丙烯薄膜CPP表面的AlN层；AlN层的厚度为20-200nm。
上述耐高温的改性聚丙烯薄膜的制备方法，包括以下步骤：
将聚丙烯薄膜至于ALD的反应腔体中，抽真空至250mTorr，然后升温至100℃，通入氩气，氩气的流速为10sccm，将三甲基铝(TMA)、DEZ和水(H2O)前驱体交替通入反应腔体中进行反应，每一周ALD过程由如下步骤组成：TMA脉冲、氩气冲洗、H2O脉冲、氩气冲洗，时间分别为200毫秒、6秒、200毫秒、6秒，ALD沉积800周，即制得改性聚丙烯薄膜。
产品效果测试
1.实施例1制得的改性聚丙烯薄膜性能测试
1.1.尺寸随温度的变化测试
取实施例1制得的ALD沉积200周、400周和2000周的改性聚丙烯薄膜(初始长度为16mm)和未改性的CPP(初始长度为16mm)，测试其沿拉伸方向的尺寸随温度的变化图，结果如图1所示，图1为实施例1制得的改性聚丙烯薄膜的尺寸随温度变化图，图1中的a)表示在测试过程中，待测样品在125℃保温半小时，图1中的b)表示在测试过程中，待测样品在150℃保温半小时，图1中的CPP曲线表示没有改性的聚丙烯薄膜其尺寸变化与温度的关系，CPP+ALD沉积200周、CPP+ALD沉积400周、CPP+ALD沉积2000周表示实施例1制得的改性聚丙烯薄膜其尺寸变化与温度的关系。从CPP表示的曲线可以看出，没有改性的CPP在100℃时已发生收缩，150℃时的收缩率达到3％。改性聚丙烯薄膜150℃时的收缩率远小于3％。
1.2.储存模量随温度变化测试
取实施例1制得的ALD沉积2000周的改性聚丙烯薄膜和未改性的CPP，测试其储存模量和损耗模量随温度的情况，结果如图2所示。图2为实施例1制得的改性聚丙烯薄膜的储存模量随温度变化图。图2中的a)表示未改性的CPP其储存模量和损耗模量随温度变化关系，图2中的b)表示实施例1制得的ALD2000周的改性聚丙烯薄膜其储存模量和损耗模量随温度变化关系。从图2中可以看出，未改性的CPP随着温度的升高，其储存模量迅速降低，实施例1制得的ALD沉积2000周的改性聚丙烯薄膜其储存模量在150℃的高温下依然有200MPa。
1.3.XRD谱图(X-射线衍射谱图)随温度变化测试
取实施例1制得的ALD沉积2000周的改性聚丙烯薄膜和未改性的CPP，测试其XRD谱图(X-射线衍射谱图)随温度变化的情况，结果如图3所示。图3为实施例1制得的改性聚丙烯薄膜的XRD谱图随温度变化图；图3中的a)表示未改性的CPP的XRD谱图随温度变化图，图3中的b)表示实施例1制得的ALD沉积2000周的改性聚丙烯薄膜随温度变化图，从图3中可以看出，未改性的CPP在高温下失去结晶取向，实施例1制得的ALD沉积2000周的改性聚丙烯薄膜在高温下基本不会失去结晶取向。
1.4.直流电压击穿强度随温度变化测试
取实施例1制得的ALD沉积2000周的改性聚丙烯薄膜和未改性的CPP，测试其直流电压击穿强度随温度变化的情况，结果如图4所示；图4中的a)表示未改性的CPP的直流电压(DC)击穿强度随温度变化图，图4中的b)表示实施例1制得的ALD沉积2000周的改性聚丙烯薄膜的直流电压(DC)击穿强度随温度变化。从图4中可以看出，未改性的CPP在高温下的直流电压(DC)击穿强度明显降低，实施例1制得的ALD沉积2000周的改性聚丙烯薄膜在高温(140℃)下的直流电压(DC)击穿强度降低并不明显。
2.实施例2制得的改性聚丙烯薄膜性能测试
取实施例2制得的ALD沉积400周、800周和2000周的改性聚丙烯薄膜和未改性的HCPP(即ALD沉积0周)，测试其沿拉伸方向的收缩率随温度的变化图，结果如图5所示，图5为实施例2制得的改性聚丙烯薄膜的收缩率随温度变化图(125℃半小时是指待测样品在125℃保温半小时，150℃半小时是指待测样品在150℃保温半小时)；从图5中可以看出，未改性的HCPP在125℃时收缩率已经达到3％以上，而实施例2制得的改性聚丙烯薄膜在150℃保温半小时后收缩率小于3％。
3.实施例3制得的改性聚丙烯薄膜性能测试
取实施例3制得的ALD沉积800周的改性聚丙烯薄膜和未改性的CPP，测试其沿拉伸方向的尺寸随温度的变化图，结果如图6所示，图6为实施例3制得的改性聚丙烯薄膜的尺寸随温度变化图，图6中的CPP 125℃表示未改性的CPP在125℃下保温半小时，其沿拉伸方向的尺寸随温度的变化情况，CPP 150℃表示未改性的CPP在150℃下保温半小时，其沿拉伸方向的尺寸随温度的变化情况；CPP 125℃ALD沉积800周表示实施例3制得的ALD沉积800周的改性聚丙烯薄膜在125℃下保温半小时，其沿拉伸方向的尺寸随温度的变化情况，CPP 150℃ALD沉积800周表示实施例3制得的ALD沉积800周的改性聚丙烯薄膜在150℃下保温半小时，其沿拉伸方向的尺寸随温度的变化情况。从图6可以看出，实施例3制得的ALD沉积800周的改性聚丙烯薄膜的尺寸变化比未改性的CPP的尺寸变化要小，实施例3制得的ALD沉积800周的改性聚丙烯薄膜的收缩率不到2％。
4.实施例1、实施例3、实施例4和实施例5ALD沉积800周的制得改性聚丙烯薄膜性能测试
取实施例1、实施例3、实施例4和实施例5ALD沉积800周的制得改性聚丙烯薄膜和未改性的CPP在150℃下保温半小时后，测试其沿拉伸方向的收缩率的情况，结果如图7所示，图7为实施例1、实施例3、实施例4和实施例5ALD沉积800周制得的改性聚丙烯薄膜在150℃下保温半小时后的收缩率情况图。图7中的CPP表示未改性的CPP，CPP+TiO2表示实施例3制得的改性聚丙烯薄膜，CPP+Al2O3表示实施例1制得的改性聚丙烯薄膜，CPP+ZnO表示实施例4制得的改性聚丙烯薄膜，CPP+AlN表示实施例5制得的改性聚丙烯薄膜，从图7中可以看出，实施例1、实施例3、实施例4和实施例5ALD沉积800周的制得改性聚丙烯薄膜的收缩率明显低于未改性的CPP的收缩率。

Claims (1)

1.改性聚丙烯薄膜的制备方法，其特征在于，包括以下步骤：
用ALD技术在聚丙烯薄膜薄膜表面沉积氮化物层，制得所述改性聚丙烯薄膜；
用所述ALD技术在聚丙烯薄膜薄膜表面沉积氮化物层，制得所述改性聚丙烯薄膜的具体过程为：将聚丙烯薄膜置于ALD的反应腔体中，抽真空，然后升温，通入载气，将至少两种前驱体交替通入反应腔体中进行反应，即制得所述改性聚丙烯薄膜；所述前驱体包括提供金属元素或Si、硼的前驱体和提供氮元素的前驱体；
所述金属元素选自Al、Ti、Ta中的至少一种；所述抽真空的真空度为250mTorr以下；所述前驱体的反应的温度不超过100℃；
每一次每种前驱体的脉冲时长为21-200毫秒；每一次前驱体脉冲之后惰性气体的冲洗时长为3-6秒钟；
所述氮化物层的厚度为20-500nm;
所述改性聚丙烯薄膜在140℃下可承受的电压为580KV/mm。
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