CN111032352A - 具有含颜料涂层的抗红外光学产品 - Google Patents
具有含颜料涂层的抗红外光学产品 Download PDFInfo
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- CN111032352A CN111032352A CN201880056287.6A CN201880056287A CN111032352A CN 111032352 A CN111032352 A CN 111032352A CN 201880056287 A CN201880056287 A CN 201880056287A CN 111032352 A CN111032352 A CN 111032352A
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Abstract
公开了包括聚合物基材的光学产品,所述聚合物基材在其外表面上具有易受氧化的红外反射金属层。所述光学产品进一步具有使用化学气相沉积直接沉积在红外反射金属层上的保护涂层,其包含一种或多种金属氧化物或金属氮化物。所述光学产品进一步具有沉积在保护涂层上的复合颜料涂层,其包括至少第一层和第二层,其中至少一个层包含第一颜料,其中第一层和第二层各自包含结合基团组分,各结合基团组分一起形成互补结合基团对。
Description
技术领域
本发明广泛地涉及用于例如汽车和建筑窗户应用的光学产品,及其制造方法。更特别地,本发明涉及具有一个或多个金属层、保护层和含颜料复合涂层的抗红外膜(infrared-rejecting films)。
背景技术
为了降低红外线、可见光和紫外线辐射透过建筑物或车辆窗户的透射率,业内已经开发出可粘贴到平面或曲面窗户的各种不同产品。该产品,通常被称为阳光控制膜或片,改变窗户的太阳能透射、反射和吸收。最常见的功能是降低日照得热量,由此在建筑结构或车辆内改善舒适度和降低冷却负荷。
许多阳光控制膜使用红外反射金属如铝、铜或银作为薄膜层,对红外波长的反射水平在这些层中提高,以使它们至少有点光谱选择性。但是,这样的薄金属层在碱性或酸性条件下,尤其是在盐存在下发生快速氧化。如果这些层具有使用水性技术施加到其上的进一步层,这尤其成问题。已经使用各种方法在防止此类层氧化的同时改进它们的性能。
美国专利5,956,175描述了由带有薄的光学透明金属层的透明基材、近红外能量吸收材料的光学透明层和覆盖并保护近红外能量吸收材料和金属的保护材料的透明层构成的阳光控制窗膜。
美国专利6,929,864公开了含有被交联聚合物间隔层隔开的第一和第二金属或金属合金层的膜,它们的厚度使得该膜可延展、可见光透射和红外反射。可将该膜接合或层压到玻璃窗(glazing)(尤其是非平面车辆安全玻璃窗)中,其中金属或金属合金层受损或变形的可能性降低。
美国专利7,659,002公开了包括至少一个吸收层的低辐射叠层。该低辐射涂层以从基材向外的顺序包括第一介电层、第一Ag层、第一阻隔层、第一吸收层、第二介电层、第二Ag层、第二吸收层、第三介电层和任选的顶涂层。还公开了在基材上沉积这样的涂层的方法。
美国专利7,951,473公开了具有改进的耐久性的光学涂层,所述涂层包括耐久性增强层、成核层和红外反射层。该专利也公开了制造具有增强的耐久性的薄膜层的方法。
与本文具有共同受让人的美国专利公开2014/0242321 [Docket 85880] (其公开内容经此引用并入本文)公开了用于制备桥接膜(bridging films)的方法和材料。在一个方面中,该桥接膜是无孔的并适于保护相邻多孔膜。例如,桥接膜接触多孔膜并保护多孔膜以防止气体和/或液体转移到多孔膜的孔隙中。在另一实例中,桥接膜保护多孔膜免受磨损。
美国专利公开2015/0285956公开了制造多层光学膜的方法。在一个实施方案中,该方法包括提供多层光学膜和在多层光学膜上安置通过纳米粒子、聚合物及其组合的逐层自组装沉积的多个层。该多层光学膜通常包括低折射率层和高折射率层的多个交替聚合物层,所述层反射从紫外线到近红外线的电磁辐射的至少一个带宽。还公开了包括安置到多层光学膜上的多个层的多层光学膜制品,其中所述多个层包含逐层自组装的纳米粒子、聚合物及其组合。
美国专利申请公开2016/0168035公开了用于如窗膜和电子显示器之类的产品的光学产品,其包括聚合物基材和具有指定耐磨性和渗透性的硬涂层。该硬涂层可包含氧化硅。
美国专利5,071,206公开了用于太阳热控制的视觉透明、颜色校正的红外反射膜,其使用具有直接毗邻介电间隔层和任选边界层的三个或更多个溅射沉积金属如银的透明层的Fabry-Perot夹层式干涉滤光片。该文献承认,这种类型的某些现有技术产品可表现出强色偏。
通常使用有机染料对光学产品如阳光控制膜进行颜色校正。更特别地,由聚酯生产染色膜的现行商业实践涉及在染色法过程中在热有机溶剂如乙二醇的浴中溶胀基材的分子结构,因为溶胀的聚酯(特别是PET)膜能够吸收有机染料。这些膜和它们的制造方法具有许多缺点。
首先,基材需要暴露于有机溶剂和升高的温度,这带来机械和化学挑战,如与储存原料溶剂和处置所产生的废物有关的环境危害和成本。此外,溶胀的基材需要特殊处理以避免下游拉伸,因此降低生产产率。其次,提高的聚酯加工温度和在干燥后在基材膜中的残余溶剂限制基材的下游使用和加工,这进而限制这样的染色膜的潜在最终用途。在工艺方面,现有方法使用大体积染料浴,这使得在商业制造中快速更换颜色是困难的。最后,只有数量有限的有机染料在热溶剂溶胀介质中可溶和稳定,并且其中许多被基材在用于窗膜应用时受到的高能辐射(sub 400 nm波长)降解,因此缩短产品的有效寿命。
为了解决这些缺点,一些膜制造商已转向在基底聚合物膜的表面上使用含颜料层以将聚合物膜着色。例如,美国公开申请2005/0019550A1描述了包括具有至少一个取向热塑性聚合物材料层的单层或多层芯材的颜色稳定的含颜料光学体,其中该取向热塑性聚合物材料具有分散在其内的颗粒颜料。这样的产品可具有许多加工和性能缺点。例如,这种类型的层通常作为薄膜施加并可使用相对较高的颜料浓度以实现所需着色水平,特别是在所需暗化(darkening)度相对较高的汽车窗膜,如在可见光区的电磁能量透过率(或Tvis)小于50%的那些中。这些高颜料浓度难以均匀分散在薄层内。更通常,含颜料层甚至在所需暗化度相对适中、低或甚至轻微的应用(例如建筑窗膜)中可具有较高的雾度和降低的清澈度。
美国专利9,453,949公开了特别可用于汽车和建筑窗膜的吸收电磁能的光学产品。该吸收电磁能的光学产品包括聚合物基材和包括第一和第二层的复合涂层,所述第一和第二层各自含有结合基团组分,它们一起形成互补结合基团对。所述层之一可具有电磁能吸收粒子,其可以是颜料。
但是在本领域中仍然需要抗红外光学产品,其满足现有商业窗膜以及汽车窗和车辆着色和/或保护膜的雾度、清澈度、表面均匀性、UV稳定性和产品寿命要求、抗氧化并允许施加能够通过可在环境温度和压力下进行的环境友好的水基着色法制造的含颜料涂层。
发明内容
在一个方面中,本发明涉及光学产品如窗膜,其包括在外表面上具有易受氧化的红外反射金属层的聚合物基材。所述光学产品进一步包括使用物理或化学气相沉积直接沉积在红外反射金属层上的保护涂层,其包含一种或多种金属氧化物或金属氮化物。所述光学产品进一步具有沉积在保护涂层上的复合颜料涂层,其包括至少第一层和第二层,其中至少一个层包含第一颜料,其中第一层和第二层各自包含结合基团组分,各结合基团组分一起形成互补结合基团对。
本发明的进一步方面如本文中公开和要求保护。
附图说明
下面参考附图更详细地描述本发明,其中在附图各处类似的附图标记是指类似的元件并且其中:
图1是本发明的光学产品的一个实施方案的示意性横截面;
图2是具有和不具有本发明的复合涂层的主题膜的透射百分比的曲线图。
详述
因此,本发明涉及光学产品如窗膜,其包括具有一个或多个易受氧化的金属或金属合金层(在下文中为方便起见有时简单描述为“一个或多个金属层”)的聚合物基材,例如PET或PVB。该光学产品进一步包括毗邻,即使用物理或化学气相沉积直接沉积在所述一个或多个金属或金属合金层上的金属氧化物或金属氮化物保护涂层。该产品进一步包括沉积在保护涂层上的包括多个逐层(LbL)双层的复合颜料涂层,其中至少一个层是或具有并入其中的颜料。为了描述相邻层(各层可能接触),如本文所述的各层可被理解为具有两个面,第一面和第二面。
现在参考图1—不按比例的示意图,在一个实施方案中,本发明大体上涉及光学产品如窗膜10。窗膜10包括聚合物基材15,例如PET或PVB,其在一面上具有至少一个易受氧化的金属或金属合金层35。该光学产品进一步包括毗邻,即使用物理或化学气相沉积直接沉积在所述一个或多个金属或金属合金层的一面上的金属氧化物或金属氮化物保护涂层40。该产品进一步包括沉积在保护涂层上的包括多个逐层(LbL)双层20、20’的复合颜料涂层50,其中至少一个层是或具有并入其中的颜料。本发明的各双层20、20’进一步由第一层25、25’和第二层30、30’构成。当用作外侧或内侧窗膜时,该基材可另外具有在其底部提供的用于将该基材粘贴到窗户的胶粘剂5。
我们发现,在复合颜料涂层和一个或多个金属层之间的氧化硅保护涂层在LbL涂层施加法过程中保护一个或多个金属层免受化学侵袭,尤其是氧化,并可提供一种或多种附加特征,如1/8波(wave)或¼波(wave)行为、IR反射、IR吸收、可见光反射或透射、或降低的可见光透射及提高的IR拒斥或反射。本发明例如可用于将提供颜色的LbL涂层施加到用原本在后续LbL涂布条件下具有快速氧化风险的金属,例如铝金属化的基材上。
常规窗膜产品可能将金属化膜的红外性能与染色PET的可见着色相结合。相反,根据本发明,我们提供易受氧化的金属化膜并使用逐层沉积施加定制颜色,而不需要染色的PET基材。在所述一个或多个金属层与LbL层之间提供保护层使得可以直接沉积而不需要对一个或多个金属层作出任何进一步的准备以防止其在LbL法过程中氧化。
本发明的光学产品因此可以是通常施加到窗户的内表面或外表面,优选内表面的膜。这些膜被理解为具有两个面,构成这些膜的各层也具有两个面。对本公开而言,还应该认识到,本文所用的IR能量通常被理解为是波长大于大约700 nm的长波长IR辐射。
当用作外侧或内侧窗膜时,基材可另外具有在其底部提供的用于将该基材粘贴到窗户上的构件(means)。该光学产品因此可具有在基材上提供的胶粘剂层。胶粘剂层可由适用于将基材结合到窗户上的任何胶粘剂构成。当结合到窗户上时,压敏胶粘剂是优选的,特别优选丙烯酸系胶粘剂。Loctite Duro-Tak 109A(可获自Henkel)是这样的胶粘剂的一个实例。胶粘剂层还可具有粘贴到其上的离型衬层。离型衬层有利地提供相对于粘性胶粘剂层的离型效应。离型衬层在所示实施方案中可包含具有硅酮离型涂层的任何聚对苯二甲酸乙二醇酯(PET)膜,所述硅酮离型涂层可从胶粘剂层上剥离以将胶粘剂层留在基材上。或者,胶粘剂层和离型层可包含透明无畸变胶粘剂和聚丙烯衬层。
本发明包括聚合物基材,优选由热塑性塑料,如聚酯,优选聚对苯二甲酸乙二醇酯(PET)形成的膜。合适的PET膜可购得,例如以Melinex 454或LJX 112为名购自DuPontTeijin Films。用于形成聚合物基材的其它合适的热塑性塑料包括例如聚乙烯醇缩丁醛、聚丙烯酸系、聚酰亚胺、聚酰胺如尼龙、和聚烯烃如聚乙烯、聚丙烯等。聚合物基材可包含共混在其中或涂布在其上的常规添加剂,如紫外线吸收剂、稳定剂、填料、润滑剂等。聚合物基材优选透明,这通常意味着透过其视觉察觉物体、标记、字词等的能力。
聚合物基材在最广义上可以是本领域中已知可用作光学产品组件的任何基材。合适的聚合物基材通常是柔性热塑性聚合物膜,更特别是厚度为例如大约10µ至大约400µ、或15µ至300µ、或20µ至250µ的聚对苯二甲酸乙二醇酯(PET)膜;或厚度优选为0.01至1 mm、或0.05至0.5 mm、或0.1mm至0.45mm,厚度更优选为15至30密尔的聚乙烯醇缩丁醛(PVB)膜。由于使用染料的窗膜表现出各种缺点,聚合物基材优选是未染色的透明聚对苯二甲酸乙二醇酯膜。术语“未染色”是指原始膜没有可察觉的颜色,并且无意排除少量存在且无意影响膜外观的添加剂如紫外线阻隔剂的存在。聚合物基材也可以是柔性聚氨酯或柔性聚(氯乙烯)膜或可以是柔性多层聚合物复合膜,如例如U.S. 8,765,263(其公开内容经此引用并入本文)中描述的基于聚氨酯的多层复合膜。
聚合物基材可进一步包含本领域中已知的添加剂以提供合意的特性。实例包括紫外线(UV)吸收材料,如苯并三唑类、羟基二苯甲酮类或三嗪类。具有并入其中的UV吸收添加剂的可用的聚合物基材描述在美国专利6,221,112中,其经此引用并入本文。
在一个实施方案中,其中聚合物基材是柔性聚合物膜如PET,该光学产品可以是窗膜。如本领域中众所周知,常规窗膜以根据各种因素,例如产品最终用途市场应用等选择的电磁能量透射率或反射率水平设计和制造。在一些情况中,所需光学性质包括最大化拒斥(反射)热(红外波长),较少关注透射或反射的可见光的量。在另一些应用中,必须达到特定程度的可见光透射率以满足政府法规,例如在汽车挡风玻璃中,法规可能要求Tvis为70%或更高。
可见光透射率(VLT或Tvis)是透过窗膜/玻璃系统的总可见光的百分比。该数值越低,透射的可见光越少。其可使用CIE Standard Observer(CIE 1924 1931)和D65Daylight计算。本公开的光学产品可具有在宽范围的VLT值内的可见光透射率,取决于辐射率和所需透明度,例如小于大约1%;大约2%至大约5%;大约25%至大约50%;大约28.5%至大约47%;大约30%至大约45%;大约28.5%;大约47%;大约55%;最多大约70%;或最多大约75%或最多大约90%。
在另一些实施方案中,本发明的光学产品可具有不大于50%、或不大于45%或不大于40%的可见光透射率(Tvis或VLT)。在用于某些汽车最终用途,如侧窗(sidelights)的具有高暗化度的窗膜中通常需要如此水平的可见光透射率。
在另一实施方案中,本发明的光学产品具有80%至85%的可见光透射率或Tvis。在用于(在政府法规允许的程度上)某些汽车最终用途,如挡风玻璃的具有相对适中至低的暗化度(通常也具有红外吸收)的窗膜中通常需要如此水平的可见光透射率。在再一实施方案中,本发明的光学产品具有不小于85%、或不小于88%或不小于90%的可见光透射率或Tvis。在用于某些建筑最终用途的具有低至轻微暗化度的窗膜中通常需要如此水平的可见光透射率。
根据本发明可通过由金属层和由复合颜料涂层实现的可见光透射率降低的组合实现这些各种水平的可见光透射率。在一个方面中,随后可通过所需或实现的可见光透射率的降低在功能上描述这些层的任一种或两者。
该窗膜可任选包括窗膜领域的普通技术人员已知的除所述一个或多个金属或金属合金层、保护涂层和复合颜料涂层之外的层或涂层。涂层例如可包括如本文所述的胶粘剂层、保护性离型衬层等。此类层或涂层可以是聚合物基材的组件。此外,聚合物基材可以是层压或多层结构。
在一个实施方案中,光学产品是用于层压玻璃的夹层。在这一实施方案中,聚合物基材由本领域中已知用于这一用途的成膜材料形成,包括例如塑化聚乙烯醇缩丁醛(PVB)、聚氨酯、聚氯乙烯、聚乙烯醇缩醛、聚乙烯、乙烯乙酸乙烯酯(ethyl vinyl acetates)等。用于该夹层的优选成膜材料是塑化PVB,如来自Eastman Chemical Company的市售产品SAFLEX® PVB夹层中所用的。在这一实施方案中,可在聚合物基材的至少一个表面上形成复合涂层。
在一个实施方案中,其中聚合物基材是柔性聚合物膜如PET,该光学产品可以是用于层压玻璃的复合夹层,其包括至少一个安全膜或夹层。安全膜可由本领域中已知用于这一用途的成膜材料形成,包括例如塑化聚乙烯醇缩丁醛(PVB)、聚氨酯、聚氯乙烯、聚乙烯醇缩醛、聚乙烯、乙烯乙酸乙烯酯等。安全膜可以是可作为SAFLEX® PVB夹层购自EastmanChemical Company的塑化PVB膜或夹层。该复合夹层可包括包封聚合物基材的两个安全膜或一个安全膜和一个涂层,如PVB涂层。这种一般类型的复合夹层是本领域中已知的并描述在例如美国专利4,973,511和5,091,258中,它们的内容经此引用并入本文。
本文所述的聚合物基材因此可包含一种或多种热塑性聚合物。合适的热塑性聚合物的实例可包括但不限于聚(乙烯醇缩醛)树脂(如PVB)、聚氨酯(“PU”)、聚(乙烯-共聚-乙酸乙烯酯)(“EVA”)、聚氯乙烯(“PVC”)、聚(氯乙烯-共聚-甲基丙烯酸酯)、聚乙烯、聚烯烃、乙烯丙烯酸酯共聚物、聚(乙烯-共聚-丙烯酸丁酯)、硅酮弹性体、环氧树脂和酸共聚物,如乙烯/羧酸共聚物,及衍生自任何上列聚合物的其离聚物,及其组合。在一些实施方案中,该热塑性聚合物可选自聚(乙烯醇缩醛)树脂、聚氯乙烯和聚氨酯,或该树脂可包含一种或多种聚(乙烯醇缩醛)树脂。尽管在本文中可能就聚(乙烯醇缩醛)树脂描述一些聚合物层,但应该理解的是,可以与下文根据本发明的各种实施方案描述的聚(乙烯醇缩醛)树脂一起或代替其包含一种或多种上述聚合物树脂和/或包含该聚合物树脂的聚合物层。
当本文所述的聚合物基材包含聚(乙烯醇缩醛)树脂时,该聚(乙烯醇缩醛)树脂可根据任何合适的方法形成。聚(乙烯醇缩醛)树脂可通过在酸催化剂存在下用一种或多种醛将聚乙烯醇缩醛化形成。所得树脂可随后根据已知方法,例如美国专利2,282,057和2,282,026以及Wade, B. 2016, Vinyl Acetal Polymer, Encyclopedia of Polymer Scienceand Technology, 1-22(在线,版权2016 John Wiley & Sons, Inc.)中描述的方法分离、稳定化和干燥。除非另行指明,所得聚(乙烯醇缩醛)树脂可具有根据ASTM D1396测得的至少大约50、至少大约60、至少大约70、至少大约75、至少大约80、至少大约85重量%的总缩醛化百分比。聚(乙烯醇缩醛)树脂中的醛残基的总量可统称为缩醛组分,该聚(乙烯醇缩醛)树脂的余量是残留羟基和残留乙酸酯基团,它们将在下文中更详细论述。
根据本发明的各种实施方案的聚合物基材可进一步包含至少一种增塑剂。根据聚合物层中的一种或多种树脂的具体组成,增塑剂可以每百份树脂至少大约5、至少大约15、至少大约25、或至少大约35或至少大约50份(phr)和/或不大于大约120、不大于大约100、不大于大约90、不大于大约75、不大于大约70、或不大于大约55、不大于大约50、不大于大约45或不大于大约40 phr、或在大约5至大约120、大约10至大约110、大约20至大约90、或大约25至大约75 phr的范围内的量存在。
本文所用的术语“每百份树脂的份数”或“phr”是指在重量基础上与一百份树脂相比存在的增塑剂的量。此外,当在本文中提供聚合物层的增塑剂含量时,其参照用于制造该聚合物层的混合物或熔体中的增塑剂的量提供。
根据本发明,聚合物基材具有沉积在其上的一个或多个易受氧化的透明金属或金属合金层,例如铝、铜、银或金、或其中任何金属的合金,包括银/金合金,在本文中有时简单描述为“一个或多个金属层”。本发明的透明金属层是由一种或多种易受氧化的金属,如铝构成的均匀连贯金属层,其厚度能够实现基本透明,通常同时降低在其上沉积这些层的膜的可见光透射量。所述一个或多个金属或金属合金层可进一步包含铜、镍、铂、钯、钨、钛或其中任何金属的合金的一种或多种。本发明的金属层可以是单层,或可包含多于一个金属层。如果在聚合物基材上存在一个或多个金属层,这些金属层可在各金属层之间具有非金属层或金属氧化物层,例如,如美国专利5,071,206中所公开,其相关部分经此引用并入本文。根据本发明,无论如何,所述一个或多个金属层的至少一个存在于聚合物基材的外表面上,即在其上提供保护层的表面上,不需要例如厚的硬涂层或其它保护金属层免受氧化的特别方法。我们已经发现,本发明的保护涂层足以在施加后续LbL层的同时防止氧化。我们无意从所述一个或多个金属层的定义中排除部分氧化物或氮化物,只要这些层主要由金属或金属合金构成并因此易受氧化作用,本发明意图减轻这些氧化作用。
所述一个或多个易受氧化的金属层可使用本领域中已知的沉积方法沉积在聚合物基材上。例如,可通过溅射,也称为溅射沉积(一种通过使用磁控溅射器铺设材料层的方法)将一个或多个金属层施加到基材上。如下文进一步详述,同样可使用任何其它合适的沉积施加,包括例如蒸发或化学或物理沉积。因此可通过物理或化学气相沉积法,如电子束沉积等沉积金属层。磁控溅射是尤其合适的沉积方法。
一个或多个金属层可由在IR范围内具有高反射性的任何易受氧化的一个或多个透明金属层构成。可以控制IR反射层中的金属和金属合金的类型和量以实现所需辐射率和VLT。例如,钨和钛比银和金更高度吸光,因此最可用于具有较低VLT的实施方案。根据本发明的一个或多个金属层可包含金属单层或金属多层叠层。
各透明金属层的厚度可以例如为大约3至大约50纳米(nm),或4至40nm、或5至35nm,金属的总厚度通常为大约10至大约100 nm、或大约15至大约75 nm。或者,可就该膜在施加透明金属层后表现出的可见光透射率描述透明金属层。例如,可实现至少2%、或至少5%或至少10%、最多大约50%、或最多60%、或最多75%或最多大约90%的可见光透射率。这也可表示为由透明金属层实现的可见光透射率的降低,例如降低至少大约1%、或至少2%、或至少5%、或至少10%、或至少15%或更多。
在一个方面中,所述一个或多个金属层在它们之间具有一个或多个非金属层或金属氧化物层。例如,如上所述,美国专利5,071,206公开了视觉透明、颜色校正的红外反射膜,其使用Fabry-Perot夹层式干涉滤光片,所述滤光片的特征在于具有直接毗邻介电间隔层和任选边界层的三个或更多个溅射沉积金属如银的透明层。本发明的所述一个或多个金属层因此可包括这样的干涉滤光片,其除金属层外还包括在它们之间的非金属层。
类似地,本发明的一个或多个金属层可包括其它滤光片产品,例如如美国专利4,337,990中描述的由金属-电介质夹层结构构成的被称为“诱导透射滤光片”的那些,所述专利的相关部分经此引用并入本文。这样的滤光片可包括透明基材,其上覆盖相位匹配层、单金属银层和减反射外层,这三个覆盖层构成透明热反射体(heat reflector)。再次,不需要采取特别措施保护聚合物基材的外表面上的金属层。根据本发明,至少一个金属层存在于聚合物基材的外表面上,而不需要例如厚的硬涂层或其它保护金属层免受氧化的特别方法。我们已经发现,本发明的保护涂层足以在施加后续复合颜料涂层的同时防止氧化。
此外,所述一个或多个金属层可包含用交替的高/低折射率电介质的叠层实现的波长选择性滤光片或与其组合。只要在聚合物基材的外表面上提供至少一个金属层,就可获得本发明的优点。
根据本发明沉积在聚合物基材上的所述一个或多个金属或金属合金层(其中至少一个在基材的外表面上提供)在其上进一步具有使用本领域中已知的化学或物理气相沉积法直接沉积在该一个或多个金属层上的保护涂层。根据本发明,该保护涂层包含一种或多种金属氧化物或金属氮化物,并因此包含金属氮氧化物。本发明的所述一种或多种金属氧化物或金属氮化物可包括例如硅、铟、锡、钛、铬、铋、锌等的氧化物或氮化物。这种保护层与刚刚描述的所述一个或多个金属层之一毗邻。本文所用的“毗邻”是指与相邻层实际接触。
本发明的所述一种或多种金属氧化物或金属氮化物在化学计量方面不受限制,并意在包括该化合物能够获得的任何金属与氧或氮原子之比。因此,尽管硅石(silica)通常被理解和描述为二氧化硅,但不要求在氧和硅原子的量之间存在2:1的比率。术语“硅石”和“二氧化硅”因此意在包括该化合物在硅和氧反应时能够保持的任何硅氧比。
保护层因此可由氮化硅、氧化硅(即硅石)或氮氧化硅层或其组合构成。因此可包含例如氧化硅的保护层可具有大约1 nm至大约200nm、或大约5nm至大约150 nm、或10至75nm、或15nm至60nm的厚度。在一个方面中,该层可简单地为溅射到一个或多个金属层的表面上的二氧化硅薄层。使用气相沉积(其可以是化学气相沉积或物理气相沉积、或化学和物理气相沉积的组合)在金属层上形成本发明的保护层。
物理气相沉积的特征在于,材料从凝相变成气相然后回到薄膜凝相而在该材料中没有明显化学变化的过程。物理气相沉积的两个常见实例是溅射和蒸发气相沉积。例如,可通过溅射氧化硅、氮化硅或其混合物而将保护涂层施加到基材上,这也被称为溅射沉积,一种使用磁控溅射器铺设材料层的方法。同样可使用任何其它合适的物理气相沉积施加,例如电子束沉积等。磁控溅射是尤其合适的物理气相沉积方法。
或者,可使用化学气相沉积(一种化学方法,其中使基材暴露于一种或多种在基材表面上反应和/或分解以产生所需沉积物的挥发性前体)在金属层上形成保护层。例如,任选在等离子体存在下,可由气体前体在一个或多个金属层上形成保护层。等离子体发生和等离子体涂布材料、条件和参数是本领域中已知的并且它们的选择可根据所需结果而变。通常,使用液体或蒸气输送系统将前体引入等离子体,从而以例如20至250 sccm的速率生成前体气体。可以使用选自O2、Ar、N2、He、H2、H2O、N2O或其组合的常规等离子体来源和气体生成等离子体。可以使用例如1:1至50:1的气体/前体体积比形成典型的涂层。
在化学气相沉积中,气体前体供应例如硅组分,且气体前体的选择因此主要取决于保护层的所需组成,以及许多其它加工因素。合适的气体前体包括金属-有机前体,如六甲基二硅氧烷(HMDSO)、1,1,3,3-四甲基二硅氧烷(TMDSO)、原硅酸四乙酯(TEOS)、四氢化硅或硅烷(SiH4)、四乙氧基硅烷、十甲基四硅氧烷、1,3-二乙氧基-1,1,3,3-四甲基二硅氧烷、三(三甲基甲硅烷基)硅烷、六甲基环三硅氧烷、1,3,5,7-四乙烯基四甲基环四硅氧烷、十甲基环五硅氧烷、八甲基环四硅氧烷,和这些的胺、乙酸酯和β二酮化物。在保护层中的基于硅的材料是例如氧化硅或硅石的一个实施方案中,该气体前体优选选自HMDSO(六甲基二硅氧烷)、TMDSO(四甲基二硅氧烷)、TEOS(原硅酸四乙酯)和SiH4(四氢化硅或硅烷)。
尽管化学气相沉积法中的气体前体在施加步骤的过程中为气体(或蒸气)形式,要理解的是,其可能最初是液体或流体形式,使得本发明的方法可任选包括在施加步骤之前或与施加步骤同时地将流体前体转变成气体或蒸气形式,例如通过加热。更具体地,转变步骤可包括加热液体前体以使足量的液体前体汽化以建立通常大约至少10 Torr的蒸气压。该方法可包括例如在鼓泡器布置中组合气体前体与载体气体以形成前体/载体气体混合物,优选进一步包括用合适的方法和设备,如用质量流量控制器测量和调节前体/载体气体混合物的流量。
本发明的光学产品意在进一步包括复合颜料涂层。我们注意到,通常可将逐层(LbL)涂层直接施加到裸聚合物基材上,或在涂布前最多电晕处理PET。但是,LbL法使表面暴露于碱性pH(在一些情况下大约9.5或更高)和高电导率溶液(50 mM NaCl或更高)。金属层如溅射铝膜在这些条件下发生快速氧化并快速变成氧化铝,其在阳光控制应用中几乎没有价值。氧化的一个指示是例如如红外辐射阻挡的降低所示,作为阳光控制膜的效力降低。
我们已经发现,根据本发明,在铝膜表面上溅射二氧化硅薄层足够长时间地保护其免受氧化以撑过(survive)LbL沉积。大约60 nm的二氧化硅已经显示防止氧化,但我们期望甚至更少就足够。我们已经发现,如下方一个或多个金属层持续阻挡红外辐射的能力所证实,100 nm或60 nm二氧化硅涂层是令人满意的。我们因此相信,根据本发明可施加大多数常规LbL膜而不用担心下方金属层降解,并可调节这样的常规窗膜产品的性能以包括任何所需颜色。
因此,在各种方面中,保护涂层,例如二氧化硅可为至少5 nm厚、或至少10nm厚、或至少15 nm厚、最多大约60 nm、或最多大约75 nm、或最多100 nm、或最多150nm。尽管基于硅的保护涂层的厚度在理论上没有上限,但本领域技术人员会理解,只需要使用足以在施加后续复合颜料涂层的同时保护一个或多个金属层的涂层。
本发明因此涉及包括聚合物基材的光学产品,所述聚合物基材在其上具有易受腐蚀的金属层(在所述金属层上提供如刚刚描述的保护层),并进一步具有复合颜料涂层。该复合颜料涂层包括至少第一层和第二层以形成双层,其中至少一个层包含或含有颜料。优选地,第一层紧邻保护层且第二层紧邻施加到或沉积在基于硅的保护涂层上的第一层。第一和第二层因此一起形成双层。可以使用一个或多个附加的第一和第二层以形成多个双层。这些双层各自或多个双层一起在本文中也可被描述为双层系统,或LbL涂层。各双层可以相同或不同。
根据本发明,复合颜料涂层包括含有一种或多种颜料的逐层涂层。给定双层的各层可包含聚离子粘合剂、不溶性颜料粒子或两者。一个或多个双层的各层包含结合基团组分,其中第一层的结合基团组分和第二层的结合基团组分构成互补结合基团对。本文所用的短语“互补结合基团对”是指在该复合涂层的第一层的结合基团组分和第二层的结合基团组分之间存在结合相互作用,如静电结合、氢键、范德华相互作用、疏水相互作用和/或化学诱发的共价键。“结合基团组分”是与互补的结合基团组分共同建立一种或多种上述结合相互作用的化学官能团。组分在通过它们各自的电荷建立结合相互作用的意义上是互补的。
根据本发明,可以例如通过聚离子粘合剂或颜料提供结合基团组分。也就是说,如果所选颜料例如带电荷,以使其可充当双层系统的给定层的结合基团组分,则该颜料可独自用于形成该双层的一个层。如果颜料不包含结合基团组分,则颜料可与具有结合基团组分的分子,例如聚离子粘合剂组合以形成双层。我们注意到,并非双层系统的每个双层都需要包含颜料,而是根据本发明,包含颜料的那些双层可具有带电荷的颜料或不带电荷的颜料或两者。
根据本发明,复合颜料涂层的第一层因此可包含聚离子粘合剂,其被定义为沿该聚合物含有多个带正电荷或带负电荷的部分的大分子。具有正电荷的聚离子粘合剂被称为聚阳离子粘合剂,而具有负电荷的那些被称为聚阴离子粘合剂。普通技术人员也会理解,一些聚离子粘合剂可充当聚阳离子粘合剂或聚阴离子粘合剂,取决于如pH之类的因素,并且被称为两性的。聚离子粘合剂的带电荷部分构成给定层的“结合基团组分”。
合适的聚阳离子粘合剂的实例包括聚(烯丙胺盐酸盐)、线性或支化聚(乙烯亚胺)、聚(二烯丙基二甲基氯化铵)、被称为聚季铵盐或polyquats的大分子和它们的各种共聚物。本发明也设想了聚阳离子粘合剂的共混物。
合适的聚阴离子粘合剂的实例包括含羧酸的化合物,如聚(丙烯酸)和聚(甲基丙烯酸),以及含磺酸盐的化合物,如聚(苯乙烯磺酸盐)和它们的各种共聚物。本发明也设想了聚阴离子粘合剂的共混物。聚阳离子和聚阴离子类型的聚离子粘合剂都是本领域普通技术人员公知的并且描述在例如Krogman等人的美国公开专利申请US20140079884中,其经此引用并入本文。合适的聚阴离子粘合剂的实例包括聚丙烯酸(PAA)、聚(苯乙烯磺酸盐)(PSS)、聚(乙烯醇)或聚(乙酸乙烯酯)(PVA、PVAc)、聚(乙烯基磺酸)、羧甲基纤维素(CMC)、聚硅酸、聚(3,4-亚乙基二氧噻吩)(PEDOT)及其与其它聚合物的组合(例如PEDOT:PSS)、多糖和上文提到的这些的共聚物。合适的聚阴离子粘合剂的其它实例包括三甲氧基硅烷官能化的PAA或PAH或生物分子如DNA、RNA或蛋白质。合适的聚阳离子粘合剂的实例包括聚(二烯丙基二甲基氯化铵)(PDAC)、壳聚糖、聚(烯丙胺盐酸盐)(PAH)、多糖、蛋白质、线性聚(乙烯亚胺)(LPEI)、支化聚(乙烯亚胺)(BPEI)和上文提到的这些的共聚物等。可充当聚阴离子粘合剂或聚阳离子粘合剂的聚离子粘合剂的实例包括两性聚合物,如蛋白质,和上文提到的聚阳离子和聚阴离子粘合剂的共聚物。
聚离子粘合剂在第一层中的浓度可部分基于其带电荷的重复单元的分子量选择,但通常为0.1 mM – 100 mM,更优选为0.5 mM至50mM,最优选为1至20 mM,基于带电荷的重复单元的分子量。
根据本发明,如果给定层的结合基团组分包括带负电荷的颜料,则互补层的聚离子粘合剂通常是聚阳离子粘合剂,如聚烯丙胺盐酸盐。聚离子粘合剂通常可溶于水并且用于形成该层的组合物是聚离子粘合剂的水溶液。在聚离子粘合剂是聚阳离子粘合剂且第一层由水溶液形成的一个实施方案中,可以选择该水溶液的pH以将5至95%,优选25至75%,更优选大约一半的可电离基团质子化。第一层中的其它任选成分包括杀生物剂或保质期稳定剂(shelf-life stabilizers)。
要理解的是,当双层的第一层包含聚阳离子粘合剂时,第二层可包含聚阴离子粘合剂或带负电荷的不溶性颜料粒子或两者。当然,在复合颜料涂层中可为本发明的光学产品提供附加功能。例如,一个或多个层可具有吸收电磁能的不溶性粒子,其本身可以是带电粒子。短语“吸收电磁能”是指由于其在一个或多个特定光谱波长或一个或多个波长范围的优先吸收而有意选择该粒子作为光学产品的组分。术语“不溶性”意在反映该粒子基本不溶解在用于形成给定层的组合物中并作为粒子存在于光学产品结构中。当然,术语吸收电磁能的不溶性粒子包括颜料;但是,不一定表现出颜色的不溶性粒子,如UV吸收剂或IR吸收剂或在电磁谱的各种部分中的吸收剂也在该术语范围内并可根据本发明提供。
适合根据本发明使用的颜料优选是具有大约5至大约300纳米、或10至50纳米的平均粒径的颗粒颜料,在本领域中通常被称为纳米粒子颜料,尽管在更大粒度在根据本发明可用的LbL法中可表现良好的那些情况下,不一定存在粒度的上限。在一个方面中,颜料表面包含给定层的结合基团组分。合适的颜料可作为胶体稳定的水分散体购自制造商如Cabot、Clariant、DuPont、Dainippon和DeGussa。特别合适的颜料包括可以Cab-O-Jet®为名购自Cabot Corporation的那些,例如250C(青色)、265M(品红色)、270Y(黄色)或352K(黑色)。为了作为胶体分散体在水中稳定,通常处理颜料粒子表面以赋予其可电离特性并由此在其表面上为颜料提供所需结合基团组分。要理解的是,市售颜料以各种形式出售,如悬浮液、分散体等,并且应该小心评估颜料的商业形式并视需要将其改性以确保其与光学产品组分的相容性和性能,特别是在该颜料表面也充当第二层的结合基团组分的实施方案中。
可以使用多种颜料以实现最终产品中的特定色调或色度或颜色;但是,仍要理解的是,如果使用多种颜料,应该小心地选择它们以确保它们与彼此和与光学产品组分的相容性和性能。这在颜料表面也充当该层的结合基团组分的实施方案中特别重要,因为例如颗粒颜料可由于会影响相容性的不同的化学改性而表现出不同的表面电荷密度。
LbL复合颜料涂层的一个或多个层可进一步包含掩蔽剂,其通过提高离子强度和降低粒子间静电排斥而经由颜料或聚离子粘合剂在该层内的改进的分散促进该层的均匀和可再现的沉积。掩蔽剂是本领域普通技术人员已知的并且例如描述在Krogman等人的美国公开专利申请US20140079884中。合适的掩蔽剂的实例包括低分子量盐,如卤化物盐、硫酸盐、硝酸盐、磷酸盐、氟磷酸盐等。卤化物盐的实例包括氯化物盐,如LiCl、NaCl、KCl、CaCl2、MgCl2、NH4Cl等,溴化物盐,如LiBr、NaBr、KBr、CaBr2、MgBr2等,碘化物盐,如LiI、NaI、KI、CaI2、MgI2等,和氟化物盐,如NaF、KF等。硫酸盐的实例包括Li2SO4、Na2SO4、K2SO4、(NH4)2SO4、MgSO4、CoSO4、CuSO4、ZnSO4、SrSO4、Al2(SO4)3和Fe2(SO4)3。有机盐,如(CH3)3CCl、(C2H5)3CCl等也是合适的掩蔽剂。基于成分成本,氯化钠通常是优选的掩蔽剂。掩蔽剂的存在和浓度水平可允许颜料或粘合剂的更高载量,如在具有不大于50%的Tvis的光学产品中需要的那些,也可实现可定制和可小心控制的载量以实现可定制和可小心控制的光学产品Tvis水平。
合适的掩蔽剂浓度可随盐的特征(identity)而变并且也描述在例如Krogman等人的美国公开专利申请US20140079884中,其全文经此引用并入本文。在一些实施方案中,掩蔽剂浓度可为1 mM至1000 mM或10 mM至100 mM或30 mM至80 mM。在一些实施方案中,掩蔽剂浓度大于1 mM、10 mM、100 mM或500 mM。
复合颜料涂层的层还可含有其它成分,如杀生物剂或保质期稳定剂。
如所述,本发明的复合颜料涂层可包括可能相同或不同的多个双层。例如,本发明的光学产品可包括第一和第二双层,其各自具有第一层和第二层。对于具有多个双层的实施方案,要认识到,可以独立地选择双层的各层的粘合剂或颜料并且含颜料的层例如联合为光学产品提供相加效应。可以部分通过经由掩蔽剂的存在分散的所用各层中的颜料粒子的浓度定制并小心地控制这种相加效应。例如,含颜料的层联合提供对光学膜产品的视觉感知颜色的近似相加效应。在提供多个包含颜料的双层的实施方案中,各层的颜料可具有相同或类似的组成和/或颜色以使该相加效应是提高光学产品的视觉感知颜色的强度或深度或暗度,或换言之,降低在可见波长范围内的电磁透射率(或Tvis)。
在一个实施方案中,使用炭黑作为至少一个层的颜料,并使用例如上文所列的那些颜料作为一个或多个其它层的颜料,以使该相加效应是视觉感知的变暗颜色,以降低在可见波长范围内的电磁透射率(或Tvis)。如上文论述,本发明可用于需要相对较高暗化度的产品。因此,在一个实施方案中,本发明的光学产品具有不大于50%或不大于70%的Tvis。在再一实施方案中,各层的颜料可具有互补组成和/或颜色以使该相加效应是不同于独立颜料并由独立颜色的组合形成的视觉感知颜色,例如通过一层使用蓝色颜料和另一层使用黄色颜料实现的相加的感知“绿色”。
普通技术人员会认识到,术语“着色”是指例如赋予不透明制品颜色、多种颜色或基于颜色的美学设计或图案。
在另一个方面中,本发明涉及形成光学产品的方法。在一个实施方案中,本发明的方法包括:(a) 将一个或多个金属层施加到聚合物基材上;(b) 在所述一个或多个金属层上施加保护层;和(c) 在所述保护层上施加复合颜料涂层。可通过将第一层施加到保护层上和此后施加第二层以形成双层来将复合颜料涂层施加到保护层上。该双层的第一层可包含聚离子粘合剂和/或颜料,第二层可同样包含粘合剂和/或颜料,第一层和第二层各自包含结合基团组分,它们一起形成互补结合基团对。至少一个层,尤其是包含带电荷的颜料粒子的那些层,可包含如上文定义的掩蔽剂。
在一个优选实施方案中,第一和第二层的至少一个作为水性分散体或水溶液施加,最优选第一和第二层都是水性分散体或水溶液。在这一实施方案中,施加步骤(a)和(b)都在环境温度和压力下进行。
本发明的光学产品优选使用例如Langmuir, 2007, 23, 3137-3141或美国专利8,234,998和8,689,726和美国公开申请US 20140079884(由本申请的共同发明人Krogman共同发明)(它们的公开内容经此引用并入本文)中描述的已知的“逐层”(LbL)法制造。
下列实施例在用于具体和详细举例说明本发明的许多方面和优点的同时,不应被解释为以任何方式限制其范围。本领域普通技术人员容易认识到不背离本发明的精神的变动、修改和调整。
实施例
通过每升去离子水溶解1.87克聚(烯丙胺盐酸盐)和使用氢氧化钠滴定所得溶液的pH至9.5,制备聚合物粘合剂溶液。通过用蒸馏水将33.33克Cab-o-Jet 352K炭黑(可购自Cabot Corp.的胶体稳定的炭黑颜料)稀释到1升并加入2.92克氯化钠以离子掩蔽胶体粒子和使它们准备好用于沉积,形成0.5重量%固含量颜料溶液。使用这些溶液根据下列描述制备和测试实验膜样品。
在厚度3密尔的PET膜上溅射涂布铝层至大约72%的可见光透射率。然后使用等离子体增强化学气相沉积在铝层上沉积二氧化硅层至60nm或100nm的层厚度。此后通过使二氧化硅保护的金属化PET暴露于上述聚合物粘合剂溶液和颜料溶液的交替喷雾,在二氧化硅保护的层上沉积复合膜。各交替喷雾持续大约10秒,接着用去离子水冲洗大约6秒。在这种情况下施加20个双层,这意味着该表面用高电导率碱性溶液润湿总共20遍。当未保护的金属化PET暴露于第一碱性溶液时,我们立即观察到该膜变透明,意味着铝金属溶解或氧化。此时停止LbL法并且没有获得VLT值。
如图2中所示的结果表明,在对本发明的实施例施加LbL涂层后的红外性能证实,铝层没有被氧化成氧化铝,而是受到厚度60nm的薄二氧化硅层保护。通过使用LbL涂层,该金属化膜因此从72%可见光透射率变暗到7.5%可见光透射率。在图2中,HB3是聚对苯二甲酸乙二醇酯膜,HB3 + Al/SiO2是指已施加铝层和二氧化硅层,而HB3 + Al/SiOx + LbL是指还已施加复合含颜料涂层。
本领域技术人员会认识到,本文所述的测量是可通过各种不同的具体试验方法获得的基于公开可得标准和指南的测量。所述测试方法仅代表用于获得各所需测量的一种可得方法。
已经为举例说明和描述给出本发明的各种实施方案的上述描述。其无意穷举或将本发明限于所公开的确切实施方案。在上述教导的电磁能中可能有许多修改或变动。选择并描述所论述的实施方案以提供本发明的原理及其实际应用的最佳说明,由此使本领域普通技术人员能够在各种实施方案中并借助适合所考虑的特定用途的各种修改利用本发明。在根据它们合理、合法和公正地享有的幅度解释时,所有这样的修改和变动在由所附权利要求书确定的本发明的范围内。
Claims (19)
1.一种光学产品,其包括:
a) 聚合物基材,在其外表面上具有易受氧化的红外反射金属层;
b) 使用化学或物理气相沉积直接沉积在所述红外反射金属层上的保护涂层,其包含一种或多种金属氧化物或金属氮化物;和
c) 沉积在所述保护涂层上的复合颜料涂层,其包括至少第一层和第二层,其中至少一个层包含第一颜料,其中所述第一层和所述第二层各自包含结合基团组分,所述结合基团组分一起形成互补结合基团对。
2.权利要求1的光学产品,其中所述聚合物基材包含聚对苯二甲酸乙二醇酯膜。
3.权利要求1的光学产品,其中所述红外反射金属层包含铝。
4.权利要求1的光学产品,其中所述红外反射金属层具有大约5至大约120纳米的厚度。
5.权利要求1的光学产品,其中所述具有红外反射金属层的聚合物基材在所述红外反射金属层上沉积所述保护涂层之前表现出至少70%的可见光透射率。
6.权利要求1的光学产品,其中所述一种或多种金属氧化物或金属氮化物包括硅、铟、锡、钛、铬、铋或锌的氧化物或氮化物。
7.权利要求1的光学产品,其中所述一种或多种金属氧化物或金属氮化物包括二氧化硅。
8.权利要求1的光学产品,其中所述保护涂层具有5 nm至150 nm的厚度。
9.权利要求1的光学产品,其中所述复合颜料涂层具有5 nm至300 nm的总厚度。
10.权利要求1的光学产品,其中所述第一颜料在其表面上具有结合基团组分。
11.权利要求1的光学产品,其中所述第一颜料包括炭黑。
12.权利要求1的光学产品,其中所述复合颜料涂层包含第二颜料,其与所述第一颜料联合提供对所述光学产品的感知颜色的相加效应。
13.权利要求1的光学产品,其为施加到交通工具上的窗膜形式。
14.权利要求12的光学产品,其中所述交通工具是汽车、飞机或船舶。
15.权利要求2的光学产品,其中所述光学产品是用于层压玻璃的复合夹层。
16.权利要求1的光学产品,其中所述复合颜料涂层的第一层和第二层的至少一个由水溶液形成。
17.一种着色窗膜,其包括:
a) 聚对苯二甲酸乙二醇酯膜,在其外表面上具有易受氧化的金属层;
b) 使用化学气相沉积直接沉积在所述金属层上的二氧化硅;和
c) 沉积在所述二氧化硅上的复合颜料涂层,其包括至少第一层和第二层,其中至少一个层包含第一颜料,其中所述第一层和所述第二层各自包含结合基团组分,所述结合基团组分一起形成互补结合基团对。
18.权利要求16的光学产品,其中所述光学产品具有不小于70%的可见光透射率。
19.权利要求16的光学产品,其中所述光学产品具有不小于80%的可见光透射率。
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US15/689,493 US10338287B2 (en) | 2017-08-29 | 2017-08-29 | Infrared-rejecting optical products having pigmented coatings |
US15/689493 | 2017-08-29 | ||
PCT/US2018/045933 WO2019045983A1 (en) | 2017-08-29 | 2018-08-09 | OPTICAL PRODUCTS REJECTING INFRARED PIGMENTS |
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KR20200047616A (ko) | 2020-05-07 |
US10338287B2 (en) | 2019-07-02 |
JP7280868B2 (ja) | 2023-05-24 |
RU2770577C2 (ru) | 2022-04-18 |
RU2020112265A (ru) | 2021-09-30 |
AU2018324421B2 (en) | 2022-12-08 |
CA3071689A1 (en) | 2019-03-07 |
JP2020532761A (ja) | 2020-11-12 |
IL272275A (en) | 2020-03-31 |
IL272275B1 (en) | 2023-03-01 |
IL272275B2 (en) | 2023-07-01 |
CA3071689C (en) | 2022-10-04 |
SG11202001821VA (en) | 2020-03-30 |
MY196128A (en) | 2023-03-15 |
RU2020112265A3 (zh) | 2021-11-11 |
KR102531448B1 (ko) | 2023-05-11 |
EP3676094A1 (en) | 2020-07-08 |
AU2018324421A1 (en) | 2020-02-13 |
WO2019045983A1 (en) | 2019-03-07 |
US20190064407A1 (en) | 2019-02-28 |
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