CN105214890A - 辊涂机 - Google Patents

辊涂机 Download PDF

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CN105214890A
CN105214890A CN201510608825.6A CN201510608825A CN105214890A CN 105214890 A CN105214890 A CN 105214890A CN 201510608825 A CN201510608825 A CN 201510608825A CN 105214890 A CN105214890 A CN 105214890A
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fluid
deposit
recirculation circuit
reprocessing
substrate
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CN105214890B (zh
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E.赖亚博瓦
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A Dewen Ni La Business Corp
ADCO Engineering Inc
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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Abstract

本文公开了具有再循环回路的辊涂机。在搅拌器单元中处理来自辊涂机的废涂布材料，所述搅拌器单元含有例如一个或多个超声波换能器以及任选过滤单元和/或温度控制单元，以产生经再处理的涂布溶液，如经再处理的溶胶-凝胶前体溶液。还公开了包括清洁单元的预防性维护模块，所述清洁单元被设计成啮合并清洁辊涂机中的施涂器和/或计量辊。

Description

辊涂机
本申请是申请号为201180016577.6、申请日为2011年4月1日、发明名称为“辊涂机”的中国发明专利申请的分案申请。
本申请依据35U.S.C.§119(e)要求2010年4月2日提交的美国临时申请系列号61/320,634的权益，该临时申请的内容被明确地并入本文。
发明领域
本发明公开了用于将纳米复合材料膜及涂层沉积在多种基板上的方法及辊涂机系统，所述基板包括但不限于玻璃、金属、塑料片或箔。
发明背景
各种组成的二元及三元金属-非金属化合物被广泛地用作用于各种用途的薄膜。例如，已经沉积了二元及三元金属-非金属化合物，包括但不限于Y2O3、ZrO2、YZO、HfO2、YHO、Al2O3、AlO2、ZnO、AZO、ITO、SiC、Si3N4、SixCyNz、SixOyNz、TiO2、CdS、ZnS、Zn2SnO4、SiO2、WO3、CeO3等等，作为用于各种用途的多层膜堆叠的薄膜涂层或层，如透明导电氧化物(TCO)电极、钝化膜、背面场层、上与下转换器、选择性发射极掩模、离子储存器、固体电解质、防湿层、抗磨层、热障、阻抗校正层、表面改性等。
已知许多方法可提供用于这些材料的沉积。这些方法可分成两类：真空技术(如PVD、CVD、ALD、MBE等)和非真空技术(如电镀、CBD、丝网印刷等)。真空技术具有高资本支出、操作成本及消耗成本。非真空技术具有高资本支出和废物处理成本，并且在多种方式上极为受限。
溶胶-凝胶的使用提供了对于上述方法的替代方案。溶胶-凝胶前体具有经历聚合以形成具有确切化学计量及掺杂的超纯连续膜的独特能力，从而提供用于微结构及界面工程的装置。目前溶胶-凝胶主要用于小规模的应用，如光学镜片或生物医学装置，如植入物和血管支架。通常通过浸涂、旋涂或喷涂将溶胶-凝胶前体溶液施加于镜片或生物医学装置。因为使用非牛顿流体形成和保持动态润湿线很困难，所以辊涂机尚未能成功地用于沉积基于大规模溶胶-凝胶的薄膜。
本领域中有许多已知的辊涂机设计。然而，在很大程度上来讲，这种设计无法使用溶胶-凝胶前体进行许多关键的薄膜工业化沉积。
因此，需要有可提供前述二元、三元及其它化合物作为大尺寸扁平基板上的单层或多层膜堆叠构件的系统和方法，所述构件兼具刚性和柔性，而不有失纳米复合材料膜的纯度、化学计量、形态及厚度均匀性。
另外需要提供可在材料损失最少的情况下有效地使用溶胶-凝胶前体的辊涂机。
还需要对辊涂机部件(如与溶胶-凝胶前体溶液一起使用的施涂辊)提供预防性维护的装置。
发明概要
本公开内容涉及使用辊涂机而基本上避免与用于薄膜沉积的常规方法相关的一种或多种上述及其它问题的方法和系统，所述辊涂机被设计成利用溶胶-凝胶前体且特别是利用非牛顿溶胶-凝胶前体。
在一方面，辊涂机包括：
(1)计量辊和施涂辊，其中辊的旋转轴彼此平行，并被布置成在计量辊与施涂辊之间产生间隙；
(2)与计量辊和施涂辊之间的间隙流体连通的储槽；
(3)被布置成接收在辊涂机的操作期间产生的废流体的容器；
(4)用于运输来自所述容器的废流体的导管；和
(5)一个或多个布置成向废流体里赋予超声波能量的超声波换能器。
在一些情况下，通过换能器以及任选的过滤单元和温度控制单元将废流体转变成经再处理的涂布溶液，例如经再处理的溶胶-凝胶前体溶液，其基本上不含颗粒物，并且能够在辊涂机或其它应用中重新使用。
在又一实施方案中，辊涂机含有预防性维护单元，所述预防性维护单元包括可逆地啮合施涂辊和/或计量辊的清洁单元。清洁单元的啮合表面具有允许其啮合施涂辊或计量辊表面的形状。该表面优选与圆筒的角度部分的内部适形，所述圆筒具有等于或稍大于施涂辊或计量辊外径的内径。啮合表面具有通过导管连接于溶剂源的一个或多个冲洗口，以及连接于低压源以从施涂辊表面移除溶剂和碎屑的至少一个抽吸口。也可使用刷(如固定刷和旋转刷)以便于从辊的表面移除碎屑。
在另一方面，辊涂室是封闭或半封闭的系统，其中辊涂机环境受控，包括温度、暴露于外部污染物以及所述室之内的气体性质。当可以将基板容纳在涂布室之内时(如在卷到卷应用中)，辊涂室可以是完全封闭的。然而当使用比涂布室大的固体基板时，必须规定提供基板进出所述室的进口和出口。可以使用比基板的截面稍大的进口和出口，优选与涂布室内的正压力结合使用以使来自外部的污染最少。
再循环回路也优选为封闭系统，其中可调节和/或保持废涂布溶液的温度、压力、过滤及层流。
在优选的实施方案中，控制辊涂室及再循环回路两者的环境，以便最大限度地使用涂布溶液，并使沉积薄膜内的缺陷形成最少。
附图说明
图1是完全封闭的辊涂系统的示意图，除了其它部件之外，该系统含有具有热稳定夹套的辊涂室、具有搅拌器的再循环回路、过滤装置和温度控制区以及预防性维护装置。
图2是根据一个公开实施方案的辊涂机的示意图，其利用再循环回路和超声波换能器以处理废溶胶-凝胶液体。
图3是显示图2中的涂布室的工作部件的示意图。
图4是辊涂室的替代实施方案的移动部件的三维视图，其中为清楚起见，已经删除了涂布室的外壁。
图5描述图4中给出的实施方案的替代实施方案，其中将薄层施加于基板的底侧。
图6显示包括预防性维护模块的另外的实施方案。
图7显示如图6中给出的预防性维护单元的替代实施方案。
具体实施方式
存在可单独使用或者与其它实施方案结合使用的若干公开实施方案。第一实施方案有时被称为具有再循环回路的辊涂机。在搅拌器单元中处理来自辊涂机的废涂布材料，所述搅拌器单元含有例如一个或多个超声波换能器以及任选的过滤单元和/或温度控制单元，以产生经再处理的涂布溶液，如经再处理的溶胶-凝胶前体溶液，其基本上不含聚合核及颗粒物质，并且可以被返回到储槽中供在辊涂机中重新使用。
第二实施方案是具有清洁单元的辊涂机，该清洁单元被设计成清洁辊涂机中的施涂辊和/或计量辊(如果使用的话)。
I.辊涂机系统
图1是完全封闭的辊涂机系统2的示意图。该系统包括涂布室4、热稳定夹套6、搅拌装置8、过滤装置10和热交换器12。下面将解释这些装置彼此的关系，其中的一些或所有这些构成再循环回路。
此外，该系统可以包括布置在涂布室下游的模块14，其可例如用于进一步处理涂有薄膜的基板。这种处理包括热处理和/或暴露于UV和/或IR辐射以引发或进一步聚合并干燥薄膜。
该系统的另一任选部件包括预防性维护(PM)单元16。这一单元被设计成啮合涂布室4中的施涂器和/或计量器，以移除操作期间积累且如果不移除这些物质就可能导致在薄膜中形成缺陷的碎屑及其它物质。下文将更详细地对此进行讨论。
该系统的其它部件可以包括混合室18和量配室20，其中可分别地制备涂布溶液并计量给辊涂机。
整个系统由壁22以及底壁和顶壁(未示出)封闭。布置适当的通道口(未示出)以允许用于操作和维护的进入。
I.辊涂机再循环回路
一些涂布溶液，如溶胶-凝胶前体溶液，特别是非牛顿溶胶-凝胶前体溶液(例如膨胀溶液)，会由于在辊涂过程中被操作而开始聚合。因此来自辊涂机的废流体可能会含有溶胶-凝胶前体、聚合核，并且在一些情况下含有颗粒物质。这种废流体需要避免缺陷和保持化学计量的非常关键的应用中是不适用的。为避免丢弃这种废流体，所公开的辊涂机利用电磁换能器(如超声波换能器)向废流体中赋予超声波能量以逆转聚合反应。在换能器组件下游的废流体流中可任选使用过滤器以移除任何残留的颗粒材料。此外，可任选将温度控制单元布置在换能器的下游以降低流体流的温度，以便防止发生任何另外的聚合。在本质上，废流体转变成经再处理的溶胶-凝胶前体流，其可经由再循环回路按相同的过程由辊涂机重新使用。或者，经再处理的溶胶-凝胶前体可用于其它的应用。
图2是根据一个利用再循环回路和超声波换能器以处理废溶胶-凝胶液体的实施方案的辊涂机的示意图。有四个主要部件：涂布室4、储槽24、搅拌室26和任选的温度控制单元28。储槽24经由导管26和蠕动泵28流体地连接于涂布室4。涂布室4经由导管30和蠕动泵32流体地连接于搅拌室26。同样地，搅拌装置26经由导管34和蠕动泵36流体地连接于任选的温度控制装置28和储槽24。导管优选由TeflonTM或其它塑料制成或涂有TeflonTM或其它塑料，这些物质可在导管中提供平滑的内表面，以便使湍流最小化。蠕动泵也用于使湍流最小化。
搅拌装置26含有由框架40支撑的多个搅拌装置38。在优选的实施方案中，搅拌器为将电能转换成压力能的换能器。这种换能器的例子包括在约20KHz与约200MHz之间、更优选在约2兆Hz与约200兆Hz之间操作的超声波换能器。然而，也可使用低于20KHz的频率。因此，频率范围可低至1Hz、10Hz、100Hz、1KHz、10KHz或20KHz中的任何一个值，并且可高至100KHz、200KHz、500KHz、1MHz、10MHz、100MHz和200MHz中的任何一个值。可从许多供应商处获得换能器，这些供应商包括Olympus(http://www.olympus-ims.com/en/probes/)、Omega(http://www.omega.com)和UPCORP(http://www.upcorp.com)。
转换的能量透入废流体将取决于频率的选择以及由换能器所产生的功率。频率的选择及功率将取决于导管的物理尺寸，包括内径、导管壁厚度和导管中废涂布溶液的组成以及粘度和速度。为了对废溶液赋予能量，在许多情况下可能需要两个或更多个以及多达六个或八个不同的频率以穿透通过搅拌装置26的废涂布溶液的整个体积。换能器可与导管的表面直接接触，或者布置成与导管表面相距数毫米以内。
因此，在一些实施方案中，以第一频率操作两个或更多个换能器(例如超声波换能器)，并将其布置成在废流体中产生相位干扰(例如超声波相位干扰)。在其它实施方案中，使用两个或更多个附加的超声波换能器。以不同的第二频率操作附加换能器，并将其布置成在废流体中产生相位干扰(如超声波相位干扰)。
在操作中，将涂布溶液(如溶胶-凝胶前体溶液)放在储槽24中。然后蠕动泵28将涂布溶液转移到涂布室4，后者的功能将在下文中更详细地描述。经由导管30和蠕动泵32移除涂布室4中所产生的废溶液并转移到搅拌装置26。搅拌器装置8中的超声波换能器38对从导管30所携带的废流体赋予超声波能量。这一能量逆转在涂布过程期间所诱导的聚合。然后在一个实施方案中将经如此处理的流体转移到任选的温度控制单元28，并经由蠕动泵36和导管34转移到储槽24。
任选但优选存在温度控制单元28以控制来自搅拌装置26的流出物的温度，而当暴露于超声波或其它电动机械能量时，所述搅拌装置会使流出物的温度升高。温度控制单元28优选降低温度，从而使返回储槽24的流出物处于与储槽中存在的涂布溶液相同的温度或接近该温度。
也可以使用过滤器装置(未示出)移除颗粒物质。可以将过滤器布置在搅拌装置26与温度控制单元28之间、温度控制装置28与储槽24之间，或布置在这两处。
可以相同或不同的频率操作换能器38。例如，换能器38A的操作频率可以在1Hz-100KHz之间，更优选在10Hz与100KHz之间，最优选在100Hz与100KHz之间。另一方面，可以不同的频率操作超声波换能器24B，如在1与500Hz之间，更优选为10-500Hz，最优选在100与500Hz之间。虽然在图2中显示的是两种不同的频率，但应意识到的是，在此实施方案中可以使用多种不同的频率。
在替代的实施方案中，可以将来自搅拌装置28和任选的温度控制单元28及颗粒过滤装置的流出物从连接涂布室4和储槽24的再循环回路中移开，并收集在不同于储槽24的容器中。当单独分离时，这种经再处理的涂布溶液可用于相同或不同的应用。
图3是显示图1和图2中的涂布室4的工作部件的示意图。工作部件由驱动辊50、施涂辊52、计量辊54、涂布室4的外壁56、导管26和基板58(当存在时)构成。在实践中，驱动辊50如所示般按逆时针方向旋转以往左推动基板58。施涂辊52和计量辊54也按逆时针方向旋转，从而作为逆向辊涂机操作。涂布流体(未示出)从储槽24经由蠕动泵28流经导管26。涂布流体沉积在施涂辊52与计量辊54之间。施涂辊52与计量辊54之间的间隙G(未示出)的宽度连同切变张量(τi,j)、旋转速度(V)和毛管数(Ca)一起决定沉积在施涂辊上的大致膜厚(H)，其正比于沉积在基板58上的层的厚度。H大致等于τi,j×G×Ca×V。施涂辊上的膜厚度(H)决定沉积在基板58上的膜厚度。
虽然在图3中显示的是作为逆向辊涂机的操作，但可以逆转施涂辊52或计量辊54的旋转方向以构成前向辊涂机进行应用。
图4是辊涂室内的移动部件的三维视图。在图4中，为清楚起见，已经删除了涂布室的外壁。驱动辊50布置在基板58之下，并且其作用是按所示的方向移动基板58。还显示了施涂辊52和计量辊54。施涂辊绕纵轴60旋转。计量辊绕纵轴62旋转。
图5描述图4中给出的实施方案的替代实施方案，其中将薄层涂布材料施加于基板58的底侧。如所指出，驱动辊70布置在基板58之上，并啮合基板58以按所示的方向将其移动。施涂辊72和计量辊74布置在基板38之下，并且施涂辊72被布置成啮合基板58的下表面，以便施加涂布材料薄膜。如同图4一样，在施涂辊72与计量辊74之间存在间隙。歧管76具有中空的内部，其与储槽24流体连通。此歧管在计量辊74上方弯曲并终止于孔78，后者提供在施涂辊72与计量辊74之间的界面处的涂布溶液装载。
当把涂布溶液放在图4和图5中的施涂辊与计量辊之间时，其填补辊之间的间隙(未示出)，并且在操作期间，施涂辊将涂层薄膜施加于基板58的表面。然而，涂布溶液也流到辊的边缘，并然后经由重力作用进入作为再循环回路的一部分的废物容器。
III.具有预防性维护模块的辊涂机
图6显示包括预防性维护模块的另外的实施方案。在许多实施方案中都需要预防性维护模块，这是因为事实上各种涂布溶液有时会沉淀和/或聚合成颗粒，这些颗粒可能会污染施涂辊82和/或计量辊84的表面。在这些辊的表面上产生的缺陷可对沉积在基板上的实际薄层具有极大的影响。因此，有必要进行周期性的维护以处理主施涂辊82的表面，从而便于在基板38上沉积均匀且基本上不含缺陷的薄膜。为此目的，涂布室4的外壁86具有室盖88，其可逆地打开和关闭，以使施涂辊82的一部分暴露于清洁单元90。清洁单元90在图6中以截面示出，并且能够平移(向下和向上，如此实施方案中所示)，以便在此情况下啮合及脱离施涂辊82的顶部。清洁单元90具有啮合表面，其尺寸匹配于施涂辊82的表面。清洁单元90含有位于啮合表面上的多个冲洗孔92和多个抽吸孔94。冲洗孔和抽吸孔优选是交替的，如图6中所示。在一些实施方案中，多个固定刷96布置在清洁单元90的啮合表面上，并且布置在冲洗孔92与抽吸孔94之间。这种刷由塑料(优选聚四氟乙烯(PTFE))制成。
在实践中，当施涂辊82需要预防性维护时，将室盖88打开，并平移清洁单元90以使之与施涂辊82接触。在进行此啮合之前，将虚设基板100插在驱动辊80与施涂辊82之间。在辊的旋转啮合之前或辊的旋转啮合开始时，使溶剂强制通过冲洗孔92，同时进行驱动辊、施涂辊和计量辊的旋转以及虚设基板的平移。可连续或间歇地对抽吸孔94施加负压以移除通过冲洗孔施加的溶剂及离开施涂辊82或计量辊84表面的任何材料。在优选的实施方案中，用于实施预防性维护的优选溶剂与用于在制造薄膜层期间所使用的涂布溶液的溶剂相同。
在维护后，移除清洁单元90，关闭室盖88并移除虚设基板90。
在大多数实施方案中，存在多个冲洗口和抽吸口，其优选在啮合表面上交替。当观察清洁单元本体的截面时，这种口的截面可以是圆形的，或者是具有矩形或其它细长截面的细长形。在清洁单元的表面处，要对冲洗口和抽吸口的表面进行修饰，以便具有适当的形状来啮合施涂辊的曲面。当与施涂辊表面啮合时，细长口可在啮合表面的整个长度上延伸，即平行于施涂辊的旋转轴。当啮合时，用来自单个细长口的溶剂冲洗施涂辊的一部分的整个表面。在施涂辊绕其轴旋转时，另外部分的表面经溶剂冲洗。在旋转期间，刷96有助于使颗粒物质脱离。
图7显示图6的预防性维护模块的替代实施方案。在此实施方案中，清洁单元的啮合表面优选含有多个旋转刷98，其布置在冲洗口与抽吸口之间，直接啮合施涂辊的表面。这些刷优选为电动机械刷。这种电动机械刷可以是具有旋转轴的细长刷，其旋转轴平行于施涂辊的旋转轴。在清洁单元的啮合期间，刷可以按与施涂辊的旋转相同或相反的方向旋转。当按相同的方向旋转时，刷和施涂辊的操作方式类似于逆向辊涂机，从而在施涂辊表面处产生磨擦环境。当按相反的方向旋转时，优选刷以能在施涂辊表面处产生磨擦环境的速度旋转，即旋转施涂器和刷辊的线速度是不同的。这种刷优选由PTFE制成。在一些实施方案中，刷是可移动的，这使得能够调节由刷施加在辊表面上的压力。
在一些实施方案中，可以对刷施加静电荷以吸引相反电荷的碎屑。在这种实施方案中，优选使用一个以上的刷，其中正或负电荷被施加于一个刷，而相反的电荷被施加于另外的刷。在此实施方案中，刷优选由导电复合PTFE制成。
虽然以上描述涉及被设计成清洁施涂辊的预防性维护模块，但可以很容易地修改这种模块以啮合其它的辊，如计量辊和驱动辊。
在一些实施方案中，优选同时清洁计量辊和施涂辊，以防止在清洁一个辊时，该辊被另一辊的碎屑污染。

Claims (20)

1.一种利用辊涂机在基板上形成膜的方法，所述方法包括：
在由施涂辊和计量辊形成的间隙中供应涂布流体，
其中所述涂布流体位于储槽中，且包括溶胶-凝胶前体或从溶胶-凝胶前体衍生出的再处理的涂布流体中的至少一种；
在所述施涂辊上形成一层所述涂布流体；
将所述一层涂布流体的的至少一部分从所述施涂辊施转移到所述基板上，从而在所述基板上形成所述膜；
将在所述辊涂机的操作期间产生的过剩流体接收到容器中；
其中所述过剩流体包括在下述步骤之一中，所述涂布流体的聚合所产生的聚合核：
供应所述涂布流体，
沉积所述涂布流体的层，和
转移所述涂布流体的一部分；
将所述过剩流体从所述容器转移到再循环回路，且在所述再循环回路中处理过剩流体，以形成所述再处理的涂布流体；
其中所述再循环回路包括搅拌系统；
其中所述搅拌系统包括至少两个超声波换能器；
其中处理所述过剩流体包括：利用基于通过所述再循环回路的所述过剩流体的粘度和速度而选择的至少两个不同的频率，而操作所述至少两个超声波换能器；且
其中操作所述至少两个超声波换能器在所述过剩流体中产生一个或多个相位干扰，逆转所述过剩流体的聚合，使得所述流体中没有聚合核，且减小所述过剩流体的粘度，从而形成所述再处理的涂布流体；以及
使所述再处理的涂布流体从所述再循环回路中流出，并进入所述储槽中。
2.根据权利要求1所述的方法，
其中所述再循环回路进一步包括温度控制系统；
其中，在所述再处理的涂布流体离开所述搅拌系统之后，使其流经所述温度控制系统，且利用所述温度控制系统降低所述再循环回路中的所述再处理的涂布流体的温度；且
其中降低所述再处理的涂布流体的温度防止当所述所述再处理的涂布流体在所述再循环回路中时发生额外聚合。
3.根据权利要求2所述的方法，其中降低所述再循环回路中的所述再处理的涂布流体的温度包括将所述再循环回路中的所述再处理的涂布流体的温度降低至所述储槽中的所述涂布流体的温度。
4.根据权利要求2所述的方法，
其中在所述再循环回路中处理所述过剩流体进一步包括：通过使经处理的过剩流体流过至少一个过滤单元而过滤所述经处理的过剩流体；
其中所述至少一个过滤单元中的每一过滤单元包括至少一个颗粒过滤装置；且
其中所述至少一个颗粒过滤装置位于下列位置之一：所述搅拌系统与所述温度控制系统之间；所述温度控制系统与所述储槽之间；或同时位于所述搅拌系统与所述温度控制系统之间以及所述温度控制系统与所述储槽之间。
5.根据权利要求1所述的方法，其中在所述再循环回路中处理所述过剩流体进一步包括过滤所述经处理的过剩流体。
6.根据权利要求5所述的方法，其中过滤所述经处理的过剩流体包括使经处理的过剩流体流过至少一个过滤单元。
7.根据权利要求6所述的方法，其中所述至少一个过滤单元中的每一过滤单元包括至少一个颗粒过滤装置。
8.根据权利要求1所述的方法，进一步包括在所述基板上固化所述膜。
9.根据权利要求8所述的方法，其中固化所述膜包括热处理、紫外线(UV)辐射暴露、或红外线(IR)辐射暴露。
10.根据权利要求1所述的方法，其中所述溶胶-凝胶前体包括非牛顿溶胶-凝胶前体。
11.根据权利要求1所述的方法，其中将所述一层所述涂布流体的至少一部分从所述施涂辊施转移到所述基板上包括：利用驱动辊馈送所述基板，使得所述基板穿过所述驱动辊与所述施涂辊之间。
12.根据权利要求11所述的方法，其中所述驱动辊与所述施涂辊以相反的方向旋转。
13.根据权利要求1所述的方法，其中在所述再循环回路中处理所述过剩流体进一步包括移除所述颗粒物质。
14.根据权利要求1所述的方法，其中所述膜包括二元或三元化合物。
15.根据权利要求1所述的方法，其中所述施涂辊的旋转轴和所述计量辊的旋转轴彼此平行，并被布置成产生所述间隙。
16.根据权利要求1所述的方法，其中位于所述储槽中的所述涂布流体由至少一个导管供应至所述间隙。
17.根据权利要求16所述的方法，其中所述至少一个导管由聚四氟乙烯(PTFE))制成，或者涂覆有聚四氟乙烯(PTFE))，或者包括聚四氟乙烯(PTFE))。
18.根据权利要求1所述的方法，其中所述膜是具有确切化学计量及掺杂的连续膜。
19.根据权利要求1所述的方法，其中所述基板包括玻璃、金属、塑料片或箔中的至少一种。
20.根据权利要求1所述的方法，其中所述基板是柔性的，而不有失所述膜的纯度、化学计量、形态及厚度均匀性。
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