CN104619475B - 制造包含分散的纳米颗粒的连续电介质膜的方法 - Google Patents

制造包含分散的纳米颗粒的连续电介质膜的方法 Download PDF

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CN104619475B
CN104619475B CN201380047341.8A CN201380047341A CN104619475B CN 104619475 B CN104619475 B CN 104619475B CN 201380047341 A CN201380047341 A CN 201380047341A CN 104619475 B CN104619475 B CN 104619475B
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nano
particle
dielectric film
secondary feeding
complex
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CN104619475A (zh
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M·A·布朗
M·S·兰
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UK Secretary of State for Defence
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    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/14—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the particular extruding conditions, e.g. in a modified atmosphere or by using vibration
    • B29C48/142—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the particular extruding conditions, e.g. in a modified atmosphere or by using vibration using force fields, e.g. gravity or electrical fields
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Abstract

本发明提供一种制作均匀地加载有分散的纳米颗粒的连续自由形式的热塑性电介质膜(25)的方法，该方法包括如下步骤：将热塑性微粒(21)馈送到挤压机(23)内；喷射包括悬浮液的二次给料(27)以形成纳米复合物，所述悬浮液在液态载体中具有纳米颗粒；以及以预设速率将所述复合物挤压到冷却的辊(26)上，由此能够控制纳米复合物膜(25)的晶体结构，其中，在所述二次给料(27)被喷射到所述挤压机(23)内的同时借助于超声发生器(29)来连续地混合所述二次给料(27)。通过基于晶体聚合物中纳米颗粒的德布罗意波长来选择纳米颗粒的尺寸，可以批量地生产电介质，以制造高电容高能量密度的存储电容器。

Description

制造包含分散的纳米颗粒的连续电介质膜的方法
技术领域
本发明涉及电介质以及它们在电容器中的应用。电容器是一种存储电荷的装置，并且一般包括由电介质分开的两个导电板。在理想的系统中，导电板保持它们的电荷，直到需要放电为止，并且在这样做的方法中导电板能够以受控方式向系统供应电能。
背景技术
影响电容的因素有板的面积、它们的间隔以及它们之间的电介质存储电荷和延期所施加电压的能力。电介质可以由任何合适的绝缘材料制成。介电常数和介质击穿强度越大，能够存储的能量就越多。当电位差上升到高于介质强度并导致电介质电击穿时，最终任何电容器都将失效。
电介质经常由热塑性塑料或热固性聚合物制成。在商业上已经使用热塑性材料用于电容器电介质应用，例如，所述热塑性材料为聚对苯二甲酸乙二醇酯(PET)、聚丙烯(PP)、聚碳酸酯和聚苯乙烯，其中PET和PP最普遍。热固性聚合物也普遍使用，要么独立使用，要么与其他绝缘系统组合地使用。这些材料的相对介电常数在大约2到3.5的范围内。已知其他电容器，例如陶瓷电容。陶瓷电容往往易碎，并且经常缺乏在非良性环境中有效工作的足够健壮性。另外，它们缺乏基于聚合物的塑料电介质的柔性，塑料电介质能够紧凑地卷绕，从而提供大表面面积且在高电压/电场条件下具有对应的较高能量存储密度。
电介质材料的介电常数依赖于频率，因此当频率升高时，会从第一介电常数过渡到可能具有低得多的值的第二介电常数。这是因除了电子和离子传导机制以外偶极分子在电场中的行为方式引起的。当建立电场时，偶极分子沿着以及迎着场线排列自身，在这样做的方法中偶极分子能够增加材料的能量存储能力。该机制使得能够在电容器中存储更多能量。在AC系统中，正弦电场致使分子根据频率改变排列。
申请GB 1004393.3证明，聚合物与遍及该聚合物分散的高介电常数颗粒的混合物导致能量密度存储增强。当在一定电场强度时或低于该电场强度时颗粒尺寸接近电子的德布罗意波长时，颗粒像电子一样表现，仿佛遍及塑料被“涂抹”一样，由此显著地提高总体介电常数，同时维持电介质的柔性和高电压能力。复合物的德布罗意波长由材料中的电子迁移率和所施加的电场(即电子漂移速度)来确定。当电子迁移率是基础聚合物和材料形态二者的函数时，重要的是确保用于挤压膜的熔融聚合物的正确结晶，这需要受控的热力学环境。德布罗意波长可以通过简单地改变结晶条件而改变若干个数量级。
以这种方式混合较高介电常数的颗粒从而在材料中具有正确分布比较重要。颗粒必须遍及聚合物分散和分布。
已知必须引入高剪切率以确保颗粒在聚合物内具有合适的空间分布。US2008/0262126阐述了一种方法，该方法使用复合作为实现这种分散和分布的方法。该复合步骤作为离散批次方法执行，以获得母料，该母料被进一步处理成最终产品。然而，为了产生连续的馈送，这种原地混合是不可能的，并且在该过程中没有办法确保颗粒变成适当地混合。
发明内容
本发明的目的是生产连续的热塑性自由形式(不受基板支撑)的电介质膜，该电介质膜均匀地加载有分散的纳米颗粒(在所有尺寸上都是纳米制)。本发明还有一个目的是在单个连续处理步骤中生产这种电介质。
因而，本发明提供了一种制作均匀地加载有分散的纳米颗粒的连续自由形式的热塑性电介质膜的方法，该方法包括如下步骤：
将热塑性微粒馈送到挤压机内；
喷射包括悬浮液的二次给料以形成纳米复合物，所述悬浮液在液态载体中具有纳米颗粒；以及
以预设速率将所述复合物挤压到冷却的辊上，由此能够控制纳米复合物膜的晶体结构，
其中，在将所述二次给料喷射到所述挤压机内的同时借助于超声发生器来连续地混合所述二次给料。
这种方法使得能够以如下方式形成纳米复合物，即：控制德布罗意波长并具有适当分布和分散的颗粒。根据需要，所述颗粒可以是金属氧化物，例如二氧化钛，所述聚合物可以是PET、聚苯乙烯、聚对二甲苯、聚乙烯、聚乙烯、聚丙烯。
术语“自由形式”是指所述膜并没有被支撑在基板上。这意味着体积减小、柔性增加，并且重要的是使得电容器能够被卷绕。这是高电容、高能量密度存储、高电压电容器的基础，所述电容器具有许多工业上的好处。
所述方法利用同步旋转、相互啮合、自清洁的双螺杆挤压机，该挤压机允许以受控的温度和压力进行高剪切率的混合。所述螺杆交错，并且在这种情况下以相同速率同步旋转，使得聚合物上的剪切力和流率得到控制。对于特定应用，所述螺杆可以根据所需要的剪切力和温度反向旋转。类似地，螺杆间距可以被改变以给予不同的流变处理效应。螺杆间距将是期望的结构和所需的厚度和晶体结构的函数，而这又取决于基础聚合物的类型。诸如剪切力之类的参数取决于聚合物的热弹性特性。
由纳米颗粒构成的二次给料通过主挤压机圆筒的低压区域以给定压力馈送到聚合物基质中。必须形成可以喷射所述二次给料的低压区域，这些颗粒通过低压蠕动泵喷射。这是通过在双螺杆螺纹内设置合适的稀疏区实现的，从而使得低粘性的二次给料能够在螺杆螺纹连续旋转的同时进入，从而以给定速率混合开。所述二次给料在喷射到挤压机圆筒内之前还被超声破碎，以提高所述二次给料中纳米颗粒的分散。与螺杆之间的高剪切率一起，超声破碎确保纳米颗粒遍及聚合物分散和分布。所述螺杆及其螺纹可以以适当的间距和间隔设置，以实现期望的产出量和剪切率。超声破碎可以使用液体储存器(作为标准)来执行，或者可以通过利用超声发生器流动池来执行。流动池可以产生更高效的气穴现象，这是由于通过流动池泵送的全部材料都紧密靠近超声发生器探头。
该方法允许形成特别长的、潜在地连续的柔性电介质条带，该条带能够通过与铝箔或任何其他合适的金属或非金属电极交织而卷绕成电容器。这种条带的优点是不需要用基板进行支撑。由于该方法是没有分批的单个过程，因此聚合物不可能经受成批产品聚合物(其中塑料经受若干次加热/冷却循环)的热降解。单个过程远非能量密集型过程，不可能在过程中引入杂质或薄弱点。
本发明相比于现有的纳米复合物膜处理技术提供了显著的益处，这是因为所有其他技术都使用成批处理方法，而本发明可以在单个连续处理布置中制造大规模纳米复合物电介质膜。在工业中被广泛接受的是，连续处理方法由于若干原因而固有地更节约成本，例如：敏感材料的驻留时间更短，获得最终产品的总处理时间最短，误差引入减少，对处理的控制最大。
可能的是，可以将不同的纳米颗粒喷射到挤压机圆筒的多于一个的部分处。例如，在某些情况下，产生耗损电介质可能是有利的。在不期望电荷经久不消的应用中(换言之，例如在机械工人需要确定电荷已分散的汽车应用中)，电介质可以被设计成以不减小其能量存储能力的方式在预定时期上释放电荷。这可以通过在系统中引入电子来实现。电介质中的一些损耗通过纳米颗粒的偶极松弛来进行。附加电子可以引入更大的阻抗分量。这通常是不期望的，但是在仅对一定时期来说期望能量存储而安全要求需要将电放掉的一些情况下，这将具有效用。
这样一种富含电子的材料将为银。可以在分开的超声破碎给料中在喷射阶段将小的纳米尺寸的银球与较高介电常数颗粒混合，因而提供在从板消除电位时快速将其电压泄放的较高介电常数的电介质。
另选地，可以将第二较高介电常数的纳米颗粒类型喷射到挤压机内。
可能必要的是在喷射之前对纳米颗粒进行预处理。颗粒的预处理能够有助于在二次给料中的分散，在圆筒内的熔融聚合物以及随后的膜内的分布以及最终产品内的稳定性。在一定条件下，如果不进行预处理，TiO2可能导致一些聚合物在正常UV光下催化降解。在现有技术中还已知小直径金属氧化物是吸湿的。这会引入可能以电子的形式降低最终产品的质量的水分。为了防止这一点所进行预处理包括但不限于使用表面活性剂以及诸如将硅烷耦合至涂覆纳米颗粒的聚合物之类的表面处理。本领域技术人员将理解预处理要求以及如何基于纳米颗粒的具体选择而采用适合于最终期望电介质特性的方法。
尽管已经针对用于电介质的纳米复合物进行该描述，但是将认识到，可以生产任何合适的纳米复合物，例如为了向聚合物内结合UV保护或者为了具有辐射硬化光敏条，其中对于加载膜的好处是在聚合物基质中包含了分散和分布的颗粒。
实际上，本发明允许有单个过程，该单个过程制造由聚合物基质内的任何纳米颗粒构成的连续自由形式的柔性纳米复合物产品。
附图说明
现在将通过参照如下附图描述本发明的具体实施方式：
图1示出了在材料中分布和分散的颗粒。
图2示出了方法的示意图。
具体实施方式
图1解释了术语“分布”和“分散”。颗粒1包含在基质2中。在图1a中，颗粒1在一个区域中成团块。这些颗粒既没有被分散，也没有被分布。在图1b中，有若干个随机的颗粒1的团块。这些颗粒被分布但是尚未被分散。在图1c中，颗粒既被分散又被分布。
转到图2，图2示出了方法。聚苯乙烯的一般挤压在现有技术中是已知的。聚苯乙烯微粒通过漏斗21添加到机器20内，并由位于圆筒23内的重叠的同步旋转螺杆22带走，螺杆22通过摩擦和剪切力使聚苯乙烯熔化。测量并控制沿着螺杆22的温度，以确保温度和压力恒定。在机器20的末端，熔融聚苯乙烯被挤压通过模具24以确定出现的条带25的形状。条带25然后在冷却抛光辊26上通过以将条带25固化。
在这种情况下，机器20是由荣朵技术公司(Rondol Technologies)制造的具有二次给料的双螺杆挤压生产线。
诸如甲苯或乙酸乙酯之类的挥发性液态载体中悬浮的纳米颗粒通过二次给料储存器27经由低压蠕动泵28馈送到流动池29中，该流动池29在纳米颗粒喷射到圆筒23的低压区域内之前将纳米颗粒超声破碎。含有纳米颗粒的挥发性液态载体在由低压蠕动泵28产生的压力作用下连续地喷射到圆筒23(在圆筒23处，液态载体在螺杆22中被夹带走)内。这允许纳米颗粒在其熔化并通过圆筒23输送时分散在聚苯乙烯中，这在所输送的熔融聚苯乙烯中产生了纳米颗粒的良好分布混合。为了在喷射之前通过防止颗粒聚集而进一步确保纳米颗粒的完全分散，含有纳米颗粒的挥发性液体在进入流动池29之前也经受连续的超声破碎。在通过模具24挤出之前，挥发性液态载体被蒸发(30)并循环利用，所得到的聚苯乙烯和纳米颗粒混合物被挤出到冷却抛光辊26。辊26是成对的，并且被冷却，以产生给予期望晶体尺寸的冷却率。这被控制成能够产生最合适的晶体尺寸，而不会形成球粒。辊26被抛光以给予没有缺陷的表面，这是因为在微米厚度的条带中，小缺陷也会对产品的质量带来显著影响。所得到的冷却条带31被卷绕在卷轴32上。
本领域技术人员将认识到，在聚合物晶体的晶体尺寸和残余内部机械应力之间有一个折衷，不过这可以通过再次加热以减少该应力中的一些应力而消除。类似地，根据期望的厚度和应用，可以使用诸如压延而不是铸造之类的其他挤压机/冷却机机构。
可以设置另一个二次给料，不过这是可选的。例如，可以将纳米范围内的银颗粒的另一个二次给料引入，从而提供将确保在不需要电压时电容器取消电压的电子；或者，如果期望的电介质特性需要不同的更高介电常数的纳米颗粒，则可以引入所述不同的更高介电常数的纳米颗粒。

Claims (9)

1.一种制作均匀地加载有分散的纳米颗粒的连续自由形式的在高电压时使用的热塑性电介质膜(31)的方法，该方法包括如下步骤：
将热塑性微粒馈送到挤压机(20)内；
喷射包括悬浮液的二次给料以形成纳米复合物，所述悬浮液在液态载体中具有纳米颗粒；
在将所述二次给料喷射到所述挤压机(20)内的同时借助于超声发生器来连续地混合所述二次给料；以及
以预设速率将所述纳米复合物挤压到冷却的辊(26)上，由此能够控制所述电介质膜(31)的晶体结构，
其中，控制所述纳米颗粒的几何形状，以使每个所述纳米颗粒的所有直径都低于所述热塑性微粒中的电子的德布罗意波长。
2.根据权利要求1所述的方法，其中，借助于流动池(29)来进一步超声破碎所述二次给料。
3.根据权利要求1或2所述的方法，其中，所述纳米颗粒包括二氧化钛。
4.根据权利要求1或2所述的方法，其中，所述液态载体为甲苯。
5.根据权利要求1或2所述的方法，其中，所述液态载体为乙酸乙酯。
6.根据权利要求1或2所述的方法，所述方法还包括喷射纳米颗粒的附加给料的步骤，该纳米颗粒被选择以提供额外电子。
7.根据权利要求6所述的方法，其中，所述附加给料中的所述纳米颗粒包括银。
8.一种根据前述权利要求中任一项所述的方法制作的连续自由形式的电介质膜(31)。
9.一种根据权利要求1至3中任一项所述的方法制作的连续自由形式的电介质膜(31)，其中，所述膜包含聚苯乙烯，以给予增强的耐辐射性。
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