CN105940479A - 使用宽离子场穿孔二维材料 - Google Patents
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Abstract
具有期望的尺寸范围、窄的尺寸分布以及高孔密度的、其内含孔的穿孔石墨烯和其他二维材料是难以获得的。与石墨烯、石墨烯基体材料和其他二维材料连续接触的薄层有助于促进孔的形成。对二维材料进行穿孔的方法可以包括:将二维材料暴露于离子源下,其中所述二维材料连续接触于至少一层;以及将来自于离子源的大量离子与二维材料和所述至少一层相互作用。所述离子源可以为宽离子束。
Description
相关申请的交叉引用
本申请基于35U.S.C.§119要求2014年1月31日提交的美国临时专利申请号61/934,530的优先权,其全部内容通过引用纳入本文。
关于联邦资助研发下所作出发明的权利的声明
不适用。
领域
本发明公开内容普遍地涉及二维材料,以及,更具体地,涉及穿孔二维材料的方法。
背景
石墨烯代表碳的一种形式,其中,碳原子存在于六元稠环的单个原子厚的薄层或多个层状薄片(例如,约20或更小),形成延伸的平面晶格。石墨烯以其各种形态在许多用途中获得了广泛关注,主要是由于它的高电导率和热导值的有利组合、良好的面内机械强度,以及独特的光学和电学特性。在许多方面,石墨烯的性能可与碳纳米管匹敌,因为这两种纳米材料都是基于延伸的sp2-杂化的碳框架。其它具有几个或更小的纳米厚度以及延伸的平面晶格的二维材料,也在许多用途中得到关注。在一个实施例中,所述二维材料具有0.3至1.2nm的厚度。在其他实施例中,所述二维材料具有0.3至3nm的厚度。
由于它的延伸平面结构,石墨烯提供了一些不与碳纳米管共享的功能。产业界特别感兴趣的是大面积石墨烯薄膜,可用于例如,特殊的阻挡层、涂层、大面积导电元件(例如,射频辐射器(RF radiator)或天线)、集成电路、透明电极、太阳能电池、气体屏障、柔性电子器件等。此外,与碳纳米管相比,目前石墨烯膜可以更廉价地大批量生产。
一些对于石墨烯和其他二维材料的预期应用,是基于在这些纳米材料的平面结构中形成多个纳米级孔洞来预测的。在石墨烯和其他二维材料中形成孔洞的方法在本文中被称为“穿孔(perforation)”,并且在本文中将此类纳米材料称为“穿孔的(perforated)”。在石墨烯薄片中,由片层中的各六元碳原子环结构形成了填隙孔径,并且该填隙孔径少于一纳米跨度。特别地,沿其最长尺寸方向,该填隙孔径被认为是约0.3纳米(碳原子间的中心至中心距离约为0.28nm,并且孔径稍微小于该距离)。典型地,对具有二维网络结构的薄层进行穿孔,是指在网络结构中形成大于填隙孔径的孔洞。
石墨烯和其他二维材料的穿孔可以改变材料的电性能和对流过材料的流体的阻力。例如,穿孔的石墨烯的孔密度可用于调节纳米材料的导电性,并且,某些情况下,可用于调节其带隙。过滤用途是穿孔的石墨烯和其他穿孔的二维材料已经引起相当兴趣的另一领域。由于石墨烯和其他二维材料的原子级薄度,在过滤过程中实现高液体通量流量是可能的,即使存在的孔洞仅具有单纳米尺寸。
高性能、高选择性的过滤用途,取决于过滤膜中存在足够数量的期望尺寸的孔洞。尽管已知对石墨烯和其他二维材料进行穿孔的许多方法,但是生产具有期望尺寸范围的、窄的尺寸分布和高的孔密度的孔洞仍然是一个挑战。在常规的穿孔方法中,通常至少缺乏这些参数中的某个参数。
可以使用化学技术在石墨烯和其他二维材料中创建孔洞。石墨烯和其他二维材料暴露于臭氧或常压等离子体(例如,氧气/氩气或氮气/氩气等离子体)可实现穿孔,但是这些孔洞通常在密度和尺寸分布上有所不足。在许多情况下,难以分别控制孔洞成核和孔洞生长,因此,这些方法通常产生了孔洞尺寸的宽分布。此外,许多化学穿孔技术产生的孔是极端的:1)低孔密度以及小的孔洞尺寸的极端孔,和2)高孔密度以及大的孔洞尺寸的极端孔。这些极端孔对于过滤用途都是特别不理想的。第一种极端孔对于通量是不利的,第二种极端孔对于选择性地排除比孔径小的杂质是不利的。
也可使用物理技术从二维材料的平面结构中除去物质以创建孔洞。高热离子束趋向在石墨烯和其他二维材料中产生孔洞,这些孔洞的尺寸太小以至于不能发生有效过滤,这主要是因为石墨烯和其他二维材料与在高热速度的离子的反应相当差。高热能量范围被定为介于热能量范围和低能量范围之间。例如,高热能量范围包括1eV和500eV之间的能量范围。相反地,聚焦离子束往往形成数量过少的孔洞。由于它们有很高的能量通量,聚焦离子束对于许多放置二维材料的基板而言,也是极其破坏性的。由于它们的高能量需求和小光束尺寸,使用聚焦离子束来穿孔大尺寸区域也是不切实际的。
具有约0.3nm至约10nm尺寸范围、高孔密度和窄孔尺寸分布的孔洞的穿孔纳米材料,是尤其难制备的。具有这个尺寸范围内的孔洞,对于多种不同过滤应用尤其有效,其中包括,例如,反渗透、分子过滤、超滤和纳滤过程。举个例子,尺寸范围在0.3nm至0.5nm的孔洞可用于某些气体分离工艺。尺寸范围在0.7nm至1.2nm的孔洞可用于某些脱盐工艺。
鉴于以上所述,本领域很需要规模化的、用于对石墨烯和其他二维材料进行穿孔方法,以便生产具有高孔密度、窄尺寸分布和小孔尺寸的孔洞。尤其地,本领域非常需要用于产生具有适于不同过滤应用的尺寸、孔密度和尺寸分布的孔洞的规模化方法。本发明公布内容满足上述需求,并提供了相关优点。
概述
在不同实施例中,本文描述了对二维材料穿孔的方法。一方面,将含有二维材料层和另一种材料层的复合材料暴露于离子源,会在二维材料中产生多个孔洞,即使在离子的能量和/或通量相对较低时。在一个实施例中,其他材料层不是二维材料的片层或薄层。
在一些实施例中,穿孔的方法可包括:(1)将二维材料暴露于离子源,其中所述二维材料与不同于所述二维材料的至少一个材料层相接触,和(2)将来自于离子源的多个离子与所述二维材料以及与所述的至少一个材料层相互作用。在一个实施例中,所述的至少一层与所述二维材料是连续接触的,当该二维材料暴露于离子源时。在一个实施例中,该离子在二维材料中引进了大量缺陷,并且该离子与所述的至少一层的相互作用,促进了所述缺陷膨胀成为所述限定于二维材料中的大量孔。在一些实施例中,该离子源提供了以下离子能量范围:从0.75keV至10keV、从1keV至10keV、从1keV至5keV、从2keV至10keV、或从5keV至10keV。在一些实施例中,该离子源提供了以下离子剂量范围,从1x1010个离子/cm2至1x1017个离子/cm2、从1x1011个离子/cm2至1x1015个离子/cm2、或从1x1013个离子/cm2至1x1019个离子/cm2。
在一个实施例中,所述方法包括步骤:将复合多层材料暴露于离子源产生的离子,该多层材料包括含二维第一材料的第一层,和与第一层接触的第二材料的第二层;并且通过来自离子源的大量离子、来自离子源的中和离子、或其组合与所述二维第一材料和所述第二材料的相互作用,从而在二维第一材料中产生大量孔。在一个实施例中,所述离子源为宽射束或泛源。在一些实施例中,就中和离子而言,当与多层材料相互作用时,至少一部分来源于离子源的离子是被中和的。例如,离子可以在给定层表面附近或在层内碰撞过程中被中和。在一个实施例中,所述第一层具有第一侧和第二侧,其中第一侧面向离子源。所述第一层的第一侧可被称为第一层的“正面”。
在一个实施例中,第二层为置于所述第一层的第一侧上的正面层。在多层材料暴露于离子源期间,至少一部分离子和/或中和离子与正面层的材料相互作用,并且,大量离子和/或中和离子穿过正面层,随后与包含二维材料的层反应。在一个实施例中,在穿孔之后除去正面层。当第二层为置于所述第一层的第二侧上的“背面层”时,至少一部分离子和/或中和离子与第一层的二维材料相互作用,并且,大量离子和/或中和离子穿过第一层,随后与背面层反应。所述多层材料可进一步包括第三材料的第三层。在一个实施例中,第三层置于第一层的相对于第二层的对侧,因此含有二维材料的第一层与其他材料的正面层和背面层都接触。
在一个实施例中,选取第二材料,以便离子和/或中和离子与第二材料的相互作用有助于穿孔过程。在一个实施例中,第二材料与离子和/或中和离子的相互作用会形成碎片。形成的碎片类型至少部分取决于第二材料。所述碎片可以是原子、离子或分子碎片(例如,聚合物链的一部分)。
当第二材料的层为正面层时,所述层的厚度足够薄,以允许离子和/或中和离子穿透到含有二维材料的层中。在一个实施例中,第二材料的层的平均厚度为1至10nm。正面层可以是连续的或不连续的。在一些实施例中,所述的至少一层可以为,例如,沉积硅、沉积聚合物、冷凝气体或冷凝有机化合物、或其任意组合。在一些实施例中,所述聚合物包括碳元素和氢元素,和任选地,进一步包括一种或多种选自下组的元素:硅、氧、氮、氟、氯和溴。在一些实施例中,所述聚合物为聚碳酸酯、聚丙烯酸酯、聚环氧乙烷、环氧化物、硅酮、聚四氟乙烯(PTFE)或聚氯乙烯(PVC)。在一个实施例中,所述冷凝气体为惰性气体,如氙气。在实施例中,所述冷凝有机化合物是硫醇、胺或醇。在一个实施例中,所述有机化合物包括具有2至15个、2至10个或5至15个碳原子的烷基基团。
当第二材料的层为背面层时,该层可以比含有二维材料的层更厚。在一个实施例中,所述背面层为1微米至10微米厚。在另一实施例中,所述背面层为5微米至10微米厚。在一个实施例中,该层提供用于二维材料层的基板。在一个实施例中,该背面层是石墨烯或其他二维材料在其上生长的生长基板。在一个实施例中,所述生长基板为金属生长基板。在一个实施例中,所述金属生长基板为基本连续的金属层,而不是网格或网眼。与石墨烯以及基于石墨烯的材料的生长相兼容的金属生长基板,包括过渡金属及其合金。在一些实施例中,所述金属生长基板为铜基或镍基的基板。在一些实施例中,所述金属生长基板为铜或镍。在另一个实施例中,所述背面层可以是二级基板,而石墨烯或其他二维材料在生长之后已经转移到该二级基板上。
在一些实施例中,离子能量范围从0.01keV至10keV、0.5keV至10keV、0.75keV至10keV、从1keV至10keV、从1keV至5keV、从2keV至10keV、或从5keV至10keV。在一些实施例中,当所述二维材料包括石墨烯基体材料薄层并进一步包括至少一些非石墨烯的碳基材料时,超过0.75keV或1keV的离子能量是较佳的。在一些实施例中,所述离子源提供给多层材料的离子剂量范围,为从1x1010个离子/cm2至1x1017个离子/cm2、从1x1011个离子/cm2至1x1015个离子/cm2、或从1x1013个离子/cm2至1x1019个离子/cm2。在一个实施例中,离子剂量基于离子进行调整,其中对于较轻的离子(较低质量的离子)提供较高的剂量。在一些实施例中,离子通量或离子束流密度范围为从0.1nA/mm2至100nA/mm2、从0.1nA/mm2至10nA/mm2、0.1nA/mm2至1nA/mm2、从1nA/mm2至10nA/mm2、或从10nA/mm2至100nA/mm2。
在不同实施例中,二维材料包括石墨烯基体材料的薄层。在一个实施例中,第一层包括石墨烯基体材料薄层。在一个实施例中,石墨烯基体材料薄层为单层或多层石墨烯薄层,或者为含有大量互连的单层或多层石墨烯域的薄层。在一些实施例中,多层石墨烯域具有2至5层或2至10层。在一个实施例中,含有石墨烯基体材料的薄层的层,进一步包括位于石墨烯基体材料薄层表面上的非石墨烯的碳基材料。在一个实施例中,非石墨烯的碳基材料的数量少于石墨烯的数量。在一些实施例中,在石墨烯基体材料中的石墨烯的数量为从60%至95%或从75%至100%。
在一些实施例中,穿孔的特征性尺寸是从0.3至10nm,从0.3到0.5nm、从0.4至10nm、从0.5至2.5nm、从0.5至10nm、从5nm至20nm、从0.7nm至1.2nm、从10nm至50nm、从50nm至100nm、从50nm至150nm、或从100nm至200nm。在一个实施例中,平均孔尺寸在特定范围内。在一些实施例中,70%至99%、80%至99%、85%至99%或90至99%的穿孔落在特定范围内,但是其它孔落在特定范围之外。如果落在特定范围之外的孔洞比落在特定范围之内的孔洞大时,这些孔洞可被称为“非选择性的”。
在更具体的实施例中,所述方法可以包括:提供在金属生长基板上的石墨烯基体材料薄层;将该石墨烯基体材料薄层暴露于离子源,该离子源提供的离子剂量范围为从1x1010个离子/cm2至1x1017个离子/cm2、从1x1011个离子/cm2至1x1015个离子/cm2、或从1x1013个离子/cm2至1x1019个离子/cm2,并且具有以下的离子能量范围,从0.75keV至10keV、从1keV至10keV、从1keV至5keV、从2keV至10keV、或从5keV至10keV;将来自离子源的大量离子和/或中和离子与石墨烯以及与金属生长基板相互作用,其中,所述离子在石墨烯中引进了大量缺陷,并且离子和/或中和离子与金属生长基板的相互作用,使得从金属生长基板向石墨烯喷射出大量层碎片;以及用所述层碎片使石墨烯中的所述缺陷膨胀,从而在石墨烯中形成多个孔洞。所述金属生长基板置于石墨烯的相对于离子源的对面一侧,并且构成背面层。在一个实施例中,当该层为金属生长基板时,所述层碎片构成金属原子或金属离子。
在其他更具体的实施例中,所述方法包括:将其上具有正面层的石墨烯基体材料薄层暴露于离子源,所述离子源提供的离子剂量范围为从1x1010个离子/cm2至1x1017个离子/cm2、从1x1011个离子/cm2至1x1015个离子/cm2、或从1x1013个离子/cm2至1x1019个离子/cm2,并且具有以下的离子能量范围,从0.75keV至10keV、从1keV至10keV、从1keV至5keV、从2keV至10keV、或从5keV至10keV;将来自离子源的大量离子和/或中和离子与石墨烯以及与正面层相互作用,从而在石墨烯中引进大量缺陷。在一个实施例中,离子和/或中和离子与正面层的相互作用导致向石墨烯喷射出大量层碎片,以及用所述层碎片使石墨烯中这些缺陷膨胀,从而在石墨烯中形成多个孔洞。所述正面层与离子源置于石墨烯的相同侧。
在另一些更具体的更多实施例中,所述方法可包括:将位于背面层上的石墨烯基体材料暴露于离子源中,所述离子源提供的离子剂量范围为从1x1010个离子/cm2至1x1017个离子/cm2、从1x1011个离子/cm2至1x1015个离子/cm2、或从1x1013个离子/cm2至1x1019个离子/cm2,并且具有以下的离子能量范围,从0.75keV至10keV、从1keV至10keV、从1keV至5keV、从2keV至10keV、或从5keV至10keV;将来自离子源的大量离子和/或中和离子与石墨烯以及与背面层相互作用,从而在石墨烯中引进大量缺陷。所述背面层位于石墨烯一侧上,背向离子源。在一个实施例中,所述背面层将离子和/或中和离子与背面层的冲击能量分散给所述缺陷的周围的石墨烯区域,并促进所述缺陷膨胀成为孔洞,其中所述缺陷是离子和/或中和离子与石墨烯反应所形成的。
前述内容已经相当广泛地概述了本发明内容的特征,以便使得随后的详细描述可以更好地被理解。下文将描述本发明的附加技术特征以及优点。通过以下描述并结合附图,这些和其他的优点和特征会更加明显。
附图简述
为了更全面理解本发明以及其优点,现在结合附图参考以下说明来描述本发明的具体实施方案,其中:
图1和图2显示了与石墨烯或其他二维材料连续接触的正面层的示例性简图;
图3A、3B和3C显示了演示离子与正面层以及与石墨烯或其他二维材料的相互作用是如何在石墨烯或其他二维材料中界定出孔洞的示例性简图;以及
图4A、图4B和图4C显示了演示离子与背面层以及与石墨烯或其他二维材料的相互作用是如何在石墨烯或其他二维材料中界定出孔洞的示例性简图。
详细描述
本发明公开的内容部分地针对在石墨烯、石墨烯基体材料或其他二维材料中产生大量孔洞的方法。在一个实施例中,第一层包括石墨烯基体材料薄层。所述石墨烯基体材料包括但不限于:单层石墨烯、多层石墨烯或互联的单层或多层石墨烯域、及其组合。在一个实施例中,石墨烯基体材料还包括由堆积的单层或多层石墨烯薄层形成的材料。在一些实施例中,多层石墨烯包括2至20层、2至10层或2至5层。在一些实施例中,石墨烯是石墨烯基体材料中的主要材料。例如,石墨烯基体材料包括至少30%石墨烯、或至少40%石墨烯、或至少50%石墨烯、或至少60%石墨烯、或至少70%石墨烯、或至少80%石墨烯、或至少90%石墨烯、或至少95%石墨烯。在一些实施例中,石墨烯基体材料包括选自下组范围的石墨烯:从30%至95%、或从40%至80%、从50%至70%、从60%至95%、或从75%至100%。
如本文所用,“域”指的是材料区域,其中原子均匀有序地进入晶格。所述域在其边界范围内是均匀有序的,但是不同于相邻的区域。例如,单晶材料具有有序原子的单一域。在一个实施例中,至少一些石墨烯域是纳米晶体,具有从1至100nm或10-100nm的结构域尺寸。在一个实施例中,至少一些石墨烯域具有超过100nm至1微米、或从200nm至800nm、或从300nm至500nm的结构域尺寸。在每个域的边界由晶体缺陷形成的“晶界”,将相邻的晶格之间区分开。在一些实施例中,第一晶格可相对于第二晶格绕垂直于薄层平面的旋转轴旋转,以使得两种晶格在“晶格取向”上有所不同。
在一个实施例中,石墨烯基体材料薄层包括单层或多层石墨烯薄层、或其组合。在一个实施例中,石墨烯基体材料薄层为单层或多层石墨烯薄层、或其组合。在另一个实施例中,石墨烯基体材料的薄层为包含多个互联的单层或多层石墨烯域的薄层。在一个实施例中,互联的域共价结合在一起形成薄层。当薄层中的域晶格取向不同时,该薄层是多晶的。
在一些实施例中,所述石墨烯基体材料薄层的厚度为从0.34至10nm、从0.34至5nm、或从0.34至3nm。在一个实施例中,石墨烯基体材料薄层包括本征缺陷。与通过穿孔选择性地在石墨烯基体材料薄层或石墨烯薄层中引入的缺陷不同,本征缺陷是由石墨烯基体材料的制备所造成的。这些本征缺陷包括但不限于:晶格反常、孔、开口、裂纹或皱纹。晶格反常可包括但不限于:除了6元之外的碳环(例如5、7或9元环)、空位、填隙缺陷(包括晶格内掺入非碳原子),以及晶界。
在一个实施例中,包括石墨烯基体材料薄层的所述层,可进一步包括位于石墨烯基体材料薄层表面的、非石墨烯的碳基材料。在一个实施例中,非石墨烯的碳基材料不具有长程有序性,并且可被归类为是无定形的。在一些实施例中,非石墨烯的碳基材料进一步包括除碳和/或碳氢化合物之外的元素。可掺入非石墨烯的碳的非碳元素包括但不限于:氢、氧、硅、铜和铁。在一些实施例中,所述非石墨烯的碳基材料包括碳氢化合物。在一些实施例中,碳是非石墨烯的碳基材料中的主要材料。例如,非石墨烯的碳基材料包括至少30%的碳、或至少40%的碳、或至少50%的碳、或至少60%的碳、或至少70%的碳、或至少80%的碳、或至少90%的碳、或至少95%的碳。在一些实施例中,非石墨烯的碳基材料包括选自下组范围的碳:从30%至95%、或从40%至80%、或从50%至70%。
本文中,这种有意地创建孔隙的纳米材料被称为“穿孔石墨烯”、“穿孔石墨烯基体材料”或“穿孔二维材料”。本发明还部分针对含有大量范围从0.3nm至10nm尺寸大小的孔洞的穿孔石墨烯、穿孔石墨烯基体材料和其他穿孔二维材料。本发明进一步部分针对含有大量范围从约0.3nm至约10nm尺寸大小的、具有窄尺寸分布的孔洞的穿孔石墨烯、穿孔石墨烯基体材料和其他穿孔二维材料,其中包括但不限于:1-10%的尺寸偏差或1-20%的尺寸偏差。在一个实施例中,所述孔洞的特征尺寸从0.5nm至10nm。对于圆孔,特征尺寸为孔直径。在一些实施例中,相对于非圆形的孔洞,特征尺寸可认为是横跨孔的最大距离、横跨孔的最小距离、横跨孔的最大距离和最小距离的平均值、或者基于孔面内区域的等效直径。如本文所用,穿孔石墨烯基体材料包括那些非碳原子已经掺入到孔边缘的材料。
如上所述,对石墨烯和其他二维材料进行穿孔以形成大量孔的常规方法,在获得的孔密度、孔尺寸和孔分布方面存在局限性。具有约10nm或更少的有效尺寸的小孔的穿孔的纳米材料,是特别难以生产的,以便其具有足够孔密度和尺寸分布以支持许多预期的应用。例如,无法产生选定尺寸和孔密度的孔洞,那么会显著妨碍过滤应用,因为选择性和通过流量会受到严重影响。此外,目前用于穿孔石墨烯和其他二维材料的技术,据信是无法规模放大到大尺寸的区域(例如,一到几十平方厘米或更大),以便支撑商业化生产应用。
穿孔石墨烯和其他二维材料的现行方法包括化学和物理方法。化学方法通常涉及孔洞成核和孔洞生长阶段。然而,孔洞成核和孔洞生长通常难以彼此分离,从而导致了孔洞尺寸的宽分布。物理过程通常涉及用强力将原子从二维材料平面结构上脱除。然而,物理方法在能量上是相当低效的,尤其是考虑到对其进行规模放大以便应用于商业生产时。此外,高能离子实际上与石墨烯和其他二维材料的相互作用非常弱,这导致了脱除过程中被溅射原子的产率低。
在一个实施例中,对石墨烯、石墨烯基体材料和其他二维材料的能量离子穿孔过程可显著增强,这是通过在其暴露于宽射束或泛源离子源期间,用至少一层第二材料连续接触于石墨烯或其他二维材料,从而进行穿孔过程。宽射束或泛源离子源可提供与聚焦离子束相比显著降低的离子通量。在一个实施例中,离子通量为从0.1nA/mm2至100nA/mm2。通过利用宽离子场并结合与石墨烯或其他二维材料连续接触的所述至少一层,可以获得在小的孔尺寸、窄的尺寸分布和高的孔密度方面显著改善的穿孔。在一个实施例中,所述孔密度由孔之间的间距所表征。在一个实施例中,其中平均孔尺寸为从0.5nm至2.5nm,孔之间的平均间距为从0.5nm至5nm。本发明的方法可容易地与聚焦离子束方法区分开来,聚焦离子束方法具有更高的离子通量和/或离子能量。就工业化生产过程的面积覆盖率来说,本发明的宽离子场方法相当具有规模扩展性。如在下文中讨论的,取决于它们的位置,连续接触石墨烯或其他二维材料的所述层可以以几种不同的方式影响穿孔方法。
在一些实施例中,本文所描述的高能离子穿孔方法利用物理穿孔方法的脱除方法,同时也像化学方法一样促进了离散孔生长阶段。然而,不同于传统的化学和物理穿孔方法,本发明的穿孔方法有利地将孔成核和孔生长阶段区分开来,同时仍然允许以高度协调的方式发生成核和生长。在一些实施例中,与石墨烯或其他二维材料的连续接触的单层或多层,允许进行高度协调的成核和生长。具体地,由于单入射离子与石墨烯或其他二维材料发生碰撞,所述单层或多层使得孔成核之后立即进行孔生长。在传统方法中,孔成核和孔生长是不协调的。因为在本发明的方法中,孔成核和孔生长是分开的但协调的阶段,因此可获得窄的孔尺寸分布。此外,本发明的方法更有利地适于产生那些约10nm尺寸或更小的孔洞,这对于许多应用是有利的,其中包括过滤。进一步地,孔尺寸和/或孔密度可调整为适应特定应用的需要。在一个实施例中,更高的能量密度(fluence)或暴露时间增加了孔的数量(直至孔开始重叠)。取决于相互作用的详情,更高的离子能量可以增加或减少孔尺寸。孔密度可通过调整石墨烯或其他二维材料暴露于离子源的暴露时间来调节。
因此,本发明的方法能够提供对穿孔石墨烯、石墨烯基体材料和其他二维材料的所有三种关键需求(小的孔尺寸、窄的尺寸分布和高的孔密度)。此外,因为它们采用宽离子场来实现穿孔,本发明方法有利地规模扩大至大维度区域,并能够支撑商业生产应用。
如上所述,在本发明方法实施例中用于影响穿孔的宽离子场提供了具有0.75keV和约10keV之间的离子能量范围的离子。在一个实施例中,离子能量范围为从1keV至10keV。在一个额外的实施例中,离子能量范围从1keV至5keV。在进一步的实施例中,离子能量范围从2keV至10keV。在一个额外的实施例中,离子能量范围从5keV至10keV。一些具有该范围能量的离子可能与石墨烯和其他二维材料的相互作用弱,以每个入射离子仅脱除1-2个原子的形式在平面结构产生点缺陷(单空位和双空位)。在一个实施例中,由本发明方法生成的孔洞产生了比此类点缺陷尺寸更大的孔。本发明的方法,尤其是连续接触于石墨烯或其他二维材料的所述层,能够产生比单独基于离子能量所能预测的更大尺寸的孔。不希望受任何观点的约束,通过将高能入射离子转换成石墨烯或其他二维材料的热碰撞,正面层或背面层与二维材料在离子辐射期间的接触,被认为有利地促进了将缺陷膨胀形成有意义的尺寸的孔。如下文进一步讨论,相对于所述离子源的而言处于不同位置中的所述层,可以通过结合能失配以多种方式协助这种效果。
尽管本文所述特定实施例中以石墨烯作为二维材料,应该认识到的是,除非另有说明,其他二维材料可同样用于替代实施例中。因此,实行本发明具有相当大的灵活性,以产生特定的具有期望性能的穿孔二维材料。
在不同实施例中,本发明所述方法可包括:将与至少一层连续接触的二维材料暴露于离子源,并且将来自离子源的多个离子和/或中和离子与二维材料以及与至少一层相互作用。在一些实施例中,所述离子和/或中和离子在二维材料中引进大量缺陷,并且离子和/或中和离子与至少一层的相互作用,促进所述缺陷膨胀形成限定在二维材料中的大量孔洞。当所述二维材料暴露于离子源时,所述至少一层与二维材料连续接触。
在不同实施例中,所述二维材料包括石墨烯、硫化钼、或氮化硼。在更具体的实施例中,所述二维材料可以为石墨烯。根据本发明实施例的石墨烯可包括:单层石墨烯、多层石墨烯、或其组合。其他具有扩展的二维分子结构的纳米材料也可以构成本发明不同实施例中的二维材料。例如,硫化钼是代表性的具有二维分子结构的硫族化物,并且其他各种不同硫族化物可构成本发明实施例中的二维材料。合适的用于特定应用的二维材料的选择可由许多因素决定,其中包括石墨烯或其他二维材料最终应用的化学和物理环境。
在本发明的不同实施例中,石墨烯或其他二维材料中产生的孔的尺寸范围可从约0.3nm至约10nm。在更具体的实施例中,所述孔的尺寸范围可从0.5nm至约2.5nm。在另外的实施例中,所述孔尺寸是0.3至0.5nm。在一个进一步的实施例中,孔尺寸是0.5至10nm。在一个额外的实施例中,孔尺寸是5nm至20nm。在一个进一步的实施例中,孔尺寸是0.7nm至1.2nm。在一个额外的实施例中,孔尺寸是10nm至50nm。在优选更大孔尺寸的实施例中,所述孔尺寸是从50nm至100nm,从50nm至150nm,或从100nm至200nm。这些尺寸范围内的孔对于过滤应用的是特别有利的。0.5nm至2.5nm的尺寸范围对反渗透过滤是特别有效的。
石墨烯或其它二维材料与离子源的接触时间,可在约0.1秒-约120秒的范围内,以产生足够生成这些孔密度的离子通量。如果需要,为了调节平面结构中获得的孔数量,可以使用更长的接触时间。
本发明实施例中,引发针对石墨烯或其他二维材料的穿孔的离子源被认为是提供宽离子场,也通常被认为是泛源离子源。在一个实施例中,所述泛源离子源不包括聚焦透镜。在一些实施例中,所述离子源在低于大气压下运转,例如10-3至10-5托或10-4至10-6托。在一个实施例中,所述环境还包括背景量(例如,大约10-5托数量级)的氧气(O2)、氮气(N2)或二氧化碳(CO2)。如上所述,在一个实施例中,所述离子源提供从1x1010个离子/cm2至1x1017个离子/cm2的离子剂量范围,具有从0.75keV至10keV的离子能量范围。在更具体的实施例中,所述离子能量范围从1keV至10keV或从5keV至10keV。在一些实施例中,所述离子剂量范围在约1x1011个离子/cm2和约1x1015个离子/cm2之间,在约1x1012个离子/cm2和约1x1014个离子/cm2之间,在约1x1013个离子/cm2和约1x1019个离子/cm2之间。在一个实施例中,所述离子剂量范围在约1x1010个离子/cm2和约1x1017个离子/cm2之间。在一个额外的实施例中,所述离子剂量范围在约1x1011个离子/cm2和约1x1015个离子/cm2之间。在进一步的实施例中,所述离子剂量范围在约1x1013个离子/cm2和约1x1019个离子/cm2之间。在一个实施例中,通量或离子束电流密度是从10nA/nm2至100nA/nm2。在一些实施例中,离子束可垂直于多层材料的层表面(入射角为0度),或者入射角可以是1至45度、0至20度、0至15度或0至10度。
所述离子源可提供各种各样的适于在石墨烯、石墨烯基体材料和其他二维材料中引发穿孔的离子。在一个实施例中,所述离子为单电荷。在另一个实施例中,所述离子为多电荷。在一个实施例中,所述离子为稀有气体离子(来自周期表第18族元素的离子)。在一个实施例中,所述离子为非氦离子。在一个实施例中,所述离子为有机离子或有机金属离子。在一个实施例中,所述有机离子或有机金属离子具有芳香成分。在一个实施例中,所述有机离子或有机金属离子的分子量为从75至200或90至200。在示例性的实施例中,可从离子源提供的以引发石墨烯或其他二维材料穿孔的离子可包括:Xe+离子、Ne+离子、Ar+离子、环庚三烯鎓正离子(C7H7 +)和二茂铁离子[(C5H5)2Fe+]。在一些实施例中,当所述离子为Xe+离子、Ne+离子、Ar+离子时,所述剂量为1x1011个离子/cm2至1x1015个离子/cm2。在一些实施例中,当所述离子包括多种元素(例如环庚三烯鎓和二茂铁),所述能量密度为1x1011个离子/cm2至1x1015个离子/cm2。在一个实施例中,提供从1x1013个离子/cm2至1x1019个离子/cm2剂量的氦离子。选取的离子和其能量,能够决定(至少部分决定)在石墨烯或其他二维材料中得到的孔的尺寸。在特定实施例中,对选取的离子或其能量进行选择,以便其能够从朝向石墨烯或其他二维材料的所述至少一层喷射出碎片。
在一个实施例中,在离子撞击期间,控制多层复合材料的温度。在一些实施例中,所述温度控制从-130℃至200℃或从-130℃至100℃。在一个实施例中,可以选取温度使得气体在二维材料的正面侧冷凝。在一个实施例中,其中存在金属背面层,所述温度可控制在从50℃至80℃。与石墨烯或其他二维材料连续接触的一层或多层,可以是正面层或背面层,或两者都存在。术语“正面侧”指的是二维材料朝向离子源的同一侧的情况。术语“背面侧”指的是背离离子源的二维材料对侧的情况。取决于其位置,至少一层可天然地或外源地存在于石墨烯或其他二维材料上,或所述至少一层是在石墨烯或其他二维材料形成后有意地沉积的。例如,本发明不同实施例中,所述金属生长基板可构成所述背面层。
一般地,所述的至少一层具有弱于石墨烯或二维材料的键能,而该石墨烯或二维材料的特征是强键。也就是说,当至少一层与离子源相互作用时,由于键能失配,优先于石墨烯或其他二维材料中,在所述的至少一层中发生键断裂。在一些实施例中,所述至少一层可以是沉积层,例如沉积硅、沉积聚合物、或其组合。如果石墨烯或其他二维材料仍然存在于其金属生长基板上,所述沉积层可构成正面层。然而,如果石墨烯或其他二维材料已经从其金属生长基板上取下,那么沉积层可构成正面层或背面层。沉积聚合物可包含任意的聚合物材料,而所述聚合物材料可适当地附着在石墨烯基体材料或其他二维材料,例如硅氧烷聚合物。在一个实施例中,离子碰撞期间,沉积聚合物不完全地从石墨烯基体材料脱层。本领域技术人员可预见其他适当的聚合物层。
在一些实施例中,所述沉积于石墨烯或其他二维材料上的正面层可具有约1nm至约10nm之间的厚度范围。如果需要的话,也可存在更厚的正面层。尽管所述正面层可在石墨烯或其他二维材料合成期间外源地沉积,其他实施例中,所述正面层也可在单独操作中进行沉积。例如,在一些实施例中,可通过溅射、喷涂、旋涂、原子层沉积、分子束外延或类似技术来沉积所述正面层。
根据它们的位置和功能,将会进一步描述不同的层。
在一些实施例中,至少一层可以为位于与离子源同侧的二维材料上的至少一个正面层。示例性的正面层可包括如上所描述的那些。当存在一个正面层时,与石墨烯或其他二维材料相互作用之前,来自离子源的离子与正面层相互作用。如下文所述,这种相互作用的类型仍然可以促进石墨烯或其他二维材料平面结构中产生孔以及膨胀孔,通过从正面层喷射出层碎片并且用石墨烯或其他二维材料碰撞所述层碎片,从而在其中产生孔。因为正面层相对薄,其具有低的制动能力,并且允许离子和/或中和离子穿透正面层,从而进一步与石墨烯相互作用。
在一个实施例中,正面层的离子碰撞产生羽状的、更多的但是更低能量的颗粒,并对石墨烯或其他二维材料进行撞击。在更具体的实施例中,本发明的方法可包括:基于随后的离子和/或中和离子的相互作用,从正面层向二维材料喷射大量的层碎片;并且在环绕缺陷的二维材料区域中,所述层碎片与二维材料进行碰撞,而所述缺陷是基于离子和/或中和离子与二维材料的相互作用产生的;以及促进所述缺陷膨胀成孔。层碎片类型可以包括原子、离子、分子或分子碎片,所述分子碎片是在高能离子与正面层相互作用时从正面层上释放出的。所述正面层可与背面层结合存在,或者,所述正面层可单独存在。以下将进一步讨论背面层的功能。
不受理论或机理的约束,据信,在正面层存在时,孔的界定或产生可基于一些协同效应发生。首先,在最初由高能离子和/或中和离子产生的初始缺陷附近,石墨烯或其他二维材料具有更高的化学反应性。其次,来自于正面层的层碎片可将正面层的单一撞击事件转化成石墨烯或其他二维材料上的多个撞击事件。第三,所述层碎片具有比入射高能量离子更低的能量,从而增强了成功地与石墨烯或其他二维材料相互作用的可能性,以界定所述孔。最终,因为正面层和石墨烯或其他二维材料彼此连续接触,在层碎片被转运给石墨烯或其他二维材料的过程中,层碎片的几何扩散是最小的,由此限定了孔的尺寸。因此,缺陷附近中的增强的化学反应性以及层碎片与石墨烯或其他二维材料间的更高效的相互作用的结合,可导致产生了孔。
图1和图2显示了正面层2连续接触于石墨烯4或其他二维材料的示例性简图。在图1中,只存在正面层2,而在图2中,正面层2和背面层6都存在。配置离子源8提供一定剂量的离子10,用于对石墨烯4进行穿孔。
图3A、3B和3C显示了离子与正面层和石墨烯或其他二维材料的相互作用,是如何在石墨烯或其他二维材料中界定出孔洞的示例性简图。为了清晰描述和叙述,正面层2和石墨烯4显示在部件分解图中,在图3A和3B中以分开的方式进行显示,而不是以它们真正的彼此连续接触的方式来显示。图3A显示了在离子10已经撞击和通过正面层之后的正面层2和石墨烯4。层碎片12从正面层2上喷射出,并且以热速度/能量和/或高热速度/能量向石墨烯4散射。在一个实施例中,这种喷射可能是指弹道式散射。在正面层中产生缺陷13。当离子10通过石墨烯4的平面结构时,缺陷14(没有显示在图3A中)可被引入石墨烯4中。此外,强调的是,正面层2和石墨烯4实际上彼此连续接触,因此减少了层碎片12从正面层2向石墨烯4移动发生的弹道散射的角度。在一个实施例中,层碎片12撞击石墨烯4,非常接近于缺陷14,在此处化学反应性被增强。在一个实施例中,层碎片12接着导致了缺陷14膨胀形成孔16,如图3B所示。图3C显示了正面层12和石墨烯4在孔16生成后的真正的连续接触布局。如图3A-3C所示,孔成核的阶段(即,石墨烯中通过离子的直接相互作用形成缺陷)以及孔生长(即,层碎片12对石墨烯4的撞击)是分开的,然而仍是高度协调的过程。因此,可以获得限定尺寸的孔16并具有窄的尺寸分布。
如图3B所示,在孔形成之后,正面层2可至少部分地覆盖孔16。在一些实施例中,可在孔16界定之后除去正面层2,以增强石墨烯4的实际渗透率。示例性的正面层去除技术可以包括,例如,氧化、溶剂清洗、加热,或其组合。氧化技术包括但不限于,使用活性氧进行紫外线臭氧(UVO)处理。根据正面层2的构成,本领域技术人员将能够选择适当的除去过程。
在一些实施例中,至少与石墨烯或其他二维材料连续接触的一层是位于石墨烯或其他二维材料一侧上的、位于离子源对面的背面层。在一个实施例中,所述背面层是石墨烯或其他二维材料在其上生长的金属生长基板,或者,所述背面层可以是石墨烯或其他二维材料生长之后所转移到的第二基板。在一个实施例中,所述第二基板是聚合物的,包括多孔高分子膜。在另一情况中,所述背面层可具有显著大于石墨烯或其他二维材料的厚度。因此,所述背面层比石墨烯或其他二维材料对能量离子和/或中和离子可具有更高的制动能力。一旦停止能量离子,当离子与二维材料相互作用形成缺陷时,所述背面层可将背面层的离子和/或中和离子的撞击能量分散进入产生的缺陷附近的石墨烯或其他二维材料的区域,从而促进缺陷膨胀成孔。在更具体的实施例中,所述背面层以某种程度类似于上文描述的正面层的方式促进二维材料中的缺陷膨胀成孔,其中碎片是朝向二维材料的。所述背面层还可以促进二维材料中缺陷的形成。例如,即使当离子或中和离子在穿过二维材料时不产生孔的情况下,离子和/或中和离子对背面层的撞击可能引起背面层小范围快速升温并膨胀,从而在石墨烯或其他二维材料中开孔。
图4A、4B和4C显示了演示离子与背面层和石墨烯或其他二维材料的相互作用,是如何在石墨烯或其他二维材料中界定出孔洞的示例性简图。此外,为了清晰描述和叙述,背面层6和石墨烯4显示在部件分解图中,在图4A和4B中以分开的方式进行显示,而不是以它们真正的彼此连续接触的方式来显示。图4A显示了紧接在离子已经通过石墨烯4并且撞击了背面层6之后的石墨烯4或其他二维材料和背面层6。当离子通过时,石墨烯4中产生缺陷14。至于背面层6,离子嵌入撞击区域20,因此从中产生了层碎片12’的喷射。在图4A中,撞击区域20显示为坑状。层碎片12’可包括如上关于正面层2所述的那些种类。例如,当背面层6为其上生长石墨烯4或其他二维材料的金属生长基板时,当动能从离子向背面层6转移时,层碎片12’可以为从金属生长基板喷溅出的金属原子或金属离子。以热能速度向石墨烯4喷射层碎片12’,并且再一次在很接近地撞击缺陷14以使得其膨胀成孔16,如图4B所描述。在图4A和4B的布局中,层碎片12’从下面撞击石墨烯4,而不是如图3A和3B所描述从其顶面。此外,需要强调的是,背面层6和石墨烯4实际上是彼此连续基础的,因此当层碎片12’从背面层6转移至石墨烯4时,减小了发生的散射角度。如图所示,层碎片12’接近地撞击缺陷14附近,而此处化学反应性是增强的。图4C显示了在孔16产生后,背面层6和石墨烯4的真正连续接触结构。如图4A-4C所示,孔成核阶段(即缺陷14的形成)和孔生长(即层碎片12’对石墨烯4的撞击)再一次分离,然而还是高度协调的过程。因为当层碎片12’在背面层6和石墨烯4之间转移时,存在最小限度的几何散射,因此可以获得具有限定尺寸和窄尺寸分布的孔16。
示例性的用于供石墨烯、石墨烯基体材料和其他二维材料生长并且在本发明实施例中可作为背面层的金属生长基板,包括含过渡金属的各种金属表面。对于石墨烯,例如,铜或镍可以特别有效地促进外延石墨烯生长。在一些实施例中,所述金属生长基板可以基本上完全由金属形成,例如金属箔或金属板。在其他实施例中,所述金属生长基板可包括在一种位于不同的表面下材料上的金属表面。例如,在本发明实施例中,一种具有金属表面的陶瓷基板可被用作金属生长基板和背面层。
因此,在一些实施例中,本发明的方法可包括:一旦发生离子和/或中和离子与二维材料的相互作用,从背面层向二维材料(例如石墨烯)喷射多个层碎片,以及用所述层碎片在环绕着缺陷的二维材料区域碰撞二维材料,从而促进所述缺陷膨胀成为孔。也就是说,所述背面层可促进能量以具有热速度的层碎片的形式转移至石墨烯或其他二维材料,从而促进石墨烯或其他二维材料中孔洞的形成。
在一些实施例中,所述正面层和背面层都可与石墨烯或其他二维材料连续接触,当所述石墨烯或其他二维材料与来自离子源的离子和/或中和离子相互作用时。从正面层和背面层产生的层碎片可彼此协调作用,以将石墨烯或其他二维材料中产生的缺陷膨胀成为大量孔洞。例如,在一些实施例中,产生于适当的正面层的层碎片与产生于背面金属生长基板的金属原子及金属离子,可从其平面结构的两侧撞击石墨烯,以促进其中孔洞的产生。这对于穿孔的多层二维材料(例如多层石墨烯)尤其有效,例如通过将粒子保持在局部区域。
因此,在正面层和背面层都存在的实施例中,本发明的方法可包括:基于离子和/或中和离子与其的相互作用,从正面层向石墨烯或其他二维材料喷射多个层碎片,以及基于离子和/或中和离子与其的相互作用,从背面层向石墨烯或其他二维材料喷射多个层碎片,并且所述来自两层的层碎片在环绕着缺陷的区域碰撞石墨烯或其他二维材料,并促进所述缺陷膨胀成为孔,而所述缺陷是由离子和/或中和离子与石墨烯或其他二维材料相互作用而产生的。
在特定的实施例中,本发明的方法可包括:提供金属生长基板上的石墨烯;将石墨烯暴露于离子源;将来自离子源的大量离子与石墨烯和金属生长基板相互作用,从而在石墨烯中引进大量缺陷;以及,离子和/或中和离子与金属生长基板的相互作用导致向石墨烯喷射多个来自于金属生长基板的含有金属离子或金属原子的层碎片;以及,用所述层碎片膨胀石墨烯中的所述缺陷,从而界定出在石墨烯中的大量孔洞。在一个实施例中,所述离子源向石墨烯提供的离子剂量范围在约1x1011个离子/cm2和约1x1017个离子/cm2之间,并具有在约0.75keV和约10keV之间的离子能量范围。所述金属生长基板位于石墨烯的背向离子源的一侧,并构成背面层。
在一些实施例中,所述石墨烯表面包覆有在金属生长基板对面的正面层,所述正面层同离子源一样位于石墨烯同侧(例如,参见图2)。所述正面层可用不同材料形成,并且可具有例如约1nm和约10nm之间范围的厚度。在一些实施例中,所述方法可进一步包括:在石墨烯中形成大量孔之后,除去正面层。
在其他特定的实施例中,本发明的方法可包括:将石墨烯暴露于离子源,所述石墨烯其上具有同离子源一样位于石墨烯同侧的正面层;将来自于离子源的大量离子和/或中和离子与石墨烯以及正面层相互作用,从而在石墨烯中引入大量缺陷;以及,离子和/或中和离子与正面层的相互作用导致向石墨烯喷射大量层碎片;以及用所述层碎片在石墨烯中膨胀这些缺陷,从而在石墨烯中界定出大量孔。在一个实施例中,所述离子源向石墨烯提供范围在约1x1011个离子/cm2和约1x1017个离子/cm2之间的离子剂量,并且具有约0.75keV和约10keV之间的离子能量范围。
在另一特定的实施例中,本发明的方法可包括:将石墨烯暴露于离子源,所述石墨烯中存在位于石墨烯一侧并背向离子源的背面层;将来自于离子源的大量离子和/或中和离子与石墨烯和所述背面层相互作用,从而在石墨烯中引入大量缺陷;以及,离子和/或中和离子与背面层的相互作用,导致将背面层上的离子和/或中和离子的冲击能分散进入环绕着缺陷的石墨烯区域中,而所述缺陷是由离子与石墨烯的相互作用而产生的;以及促进这些缺陷膨胀成孔。在一个实施例中,所述离子源向石墨烯提供范围在约1x1010个离子/cm2和约1x1017个离子/cm2之间的离子剂量,并且具有约0.75keV和约10keV之间的离子能量范围。
在更特定的实施例中,本发明的方法可包括:将石墨烯暴露于离子源,所述石墨烯中存在位于石墨烯一侧并背向离子源的背面层;将来自于离子源的大量离子和/或中和离子与石墨烯和所述背面层相互作用,从而在石墨烯中引入大量缺陷;以及,离子和/或中和离子与背面层的相互作用导致向石墨烯喷射大量层碎片;以及用所述层碎片在石墨烯中膨胀这些缺陷,从而在石墨烯中界定出大量孔。在一个实施例中,所述离子源向石墨烯提供范围在约1x1010个离子/cm2和约1x1017个离子/cm2之间的离子剂量,并且具有约0.75keV和约10keV之间的离子能量范围。
本文所述的穿孔石墨烯、石墨烯基体材料和其他二维材料可用于许多应用中,包括过滤、电子工业、阻挡层和薄膜、气体屏障,等等。可使用穿孔石墨烯、石墨烯基体材料和其他穿孔二维材料的示例性过滤应用包括:例如,反渗透、分子过滤、超滤和纳滤过程。当在不同的过滤过程中使用时,穿孔石墨烯或其他穿孔二维材料可以被穿孔,然后转移至多孔的第二基板,其中穿孔石墨烯或其他穿孔二维过滤被用作活性过滤膜。
尽管本发明已经参照所公开的实施例进行描述,本领域技术人员将容易地理解这些仅仅是本发明的示例。应当理解的是,可以在不脱离本发明实质的前提下进行各种修改。可以修改本发明以吸收任意数量的前述未提到的变化、替代、替换或等效安排,但需与本发明的实质和范围相称。此外,虽然已经描述了本发明不同的实施例,应当理解的是,本发明的方面可仅包含一些描述的实施例。因此,本发明不应视为受前述描述的限制。
除非另有说明,可使用所描述或示例的每个构思或部件的组合来实施本发明。化合物的具体名称旨在是示例性的,因为众所周知本领域技术人员可以另外地命名这些同样的化合物。当某种如本文所描述的化合物,例如,在化学式中或在化学名称中,并未指定化合物的特定异构体或对映体时,该描述旨在包括所述化合物的单独的或任意组合的每个异构体和每个对映体。本领域技术人员将会理解的是,无需采取过度实验,除了那些特别指定的之外的方法、设备组件、起始材料和合成方法都可用于本发明实施中。任何此类方法、设备组件、起始材料和合成方法的所有已知的功能等价物都意图被包含在本发明中。每当说明书中给出一个范围,例如,温度范围、时间范围、或组成范围,所有的中间区域和子范围,还有包含在所给范围内的所有个别数值都意图包含在本发明中。如果本文采用马库斯基团或其他基团,该基团所有的个体组成和所有可能的组合以及亚组合,都被包含在本发明中。
如本文所用,“包含”与“包括”、“含有”或“特征是”同义,并且,为兼容的或开放式的,不排除额外的、未列举的部件或方法步骤。如本文所用,“构成”排除了任何没有在权利要求中指定的部件、步骤或要素。如本文所用,“基本由…构成”并不排除那些实质上不影响权利要求的基本的和新颖的特性的材料或步骤。任何本文列举的术语“包含”,尤其是在复合物成分的描述或设备部件的描述中,被理解为包含基本上由那些所述组分或要素构成,以及由所述组分或要素构成的复合物和方法。示例性地进行描述的本发明,可以在缺少任一要素或多个要素,或缺少某一限制或多个限制要素的情况下合适地实施,这在本文中没有具体披露。
所用的术语和解释是描述性的术语,而非限制性的,并且不意图在这些术语和解释的使用中,排除任何所示及所描述的特征的等同物、或其部分,但是应当认识到在本发明要求的范围内做出的各种修改是可能的。因此,应当理解的是,尽管本发明已经通过优选的例子是任选的特征进行具体公开,本领域技术人员可对本文所披露的概念进行修改和变动,并且此类修改和变动被认为是在所附权利要求限定的本发明的范围内。
通常地,本发明所用的术语和短语具有本领域公知的意义,可以通过参考本领域技术人员已知的标准教科书、期刊文献和上下文来确定含义。提供了前述的定义,以便明确它们在本发明上下文中的具体应用。
在整个申请中,所有参考文献,例如专利文件(包括公布的或授权的专利或其等同专利),专利申请公开;以及非专利文献或其它来源材料,以整体引用的方式纳入本文参考,好像单独引用纳入一样,达到每篇参考文献至少部分与本申请公开的内容不一致(例如,部分不一致的参考文献中除了部分不一致的内容,都纳入本文参考)。
本说明书中提到的所有专利和出版物都表明本发明相关的领域技术人员的水平。本文引用的参考文献以整体引用的方式纳入本文,表明在某些情况下截止申请日的现有技术的状态,并且,如果需要的话,此类信息可以在本文使用,并且如果需要,可用于排除(例如,放弃)现有技术的特定实施方式。例如,当要求一种化合物权利时,应当理解的是,现有技术中已知的化合物,包括参考文献中披露的特定化合物(尤其是在引用的专利文件中的),不意图包含在权利要求中。
Claims (23)
1.一种方法,包括:
将多层材料暴露于离子源提供的离子下,所述多层材料包括含二维第一材料的第一层,以及与所述第一层接触的第二材料的第二层,所述提供的离子具有从1.0keV至10keV范围的离子能量以及从0.1nA/mm2至100nA/mm2的通量;以及
通过将由离子源提供的大量离子、中和离子或其组合与所述二维第一材料以及与第二材料的相互作用,在所述二维第一材料中产生多个孔。
2.如权利要求1所述的方法,其特征在于,所述离子能量为从1.0keV至5keV。
3.如权利要求1所述的方法,其特征在于,所述离子源为宽射束源。
4.如权利要求1所述的方法,其特征在于,所述多层材料暴露于从1x1011个离子/cm2至1x1015个离子/cm2范围的离子剂量下,并且所述离子源提供选自下组的离子:Xe+离子、Ne+离子或Ar+离子。
5.如权利要求1所述的方法,其特征在于,所述多层材料暴露于从1x1011个离子/cm2至1x1015个离子/cm2范围的离子剂量下,并且所述离子源提供具有从90至200的分子量的有机离子或有机金属离子。
6.如权利要求5所述的方法,其特征在于,所述离子选自下组:环庚三烯鎓离子和二茂铁离子。
7.如权利要求1所述的方法,其特征在于,所述二维第一材料包括石墨烯。
8.如权利要求7所述的方法,其特征在于,所述第一层包括石墨烯基体材料薄层。
9.如权利要求1所述的方法,其特征在于,所述孔的特征尺寸为从0.5nm至2.5nm。
10.如权利要求1所述的方法,其特征在于,所述孔的特征尺寸为从1nm至10nm。
11.如权利要求1-10任一项所述的方法,其特征在于,所述第一层具有第一侧和第二侧,其中第一侧面向离子源,并且,所述第二层位于所述第一层的第二侧上并且具有大于第一层的厚度。
12.如权利要求11所述的方法,其特征在于,所述第二材料包括金属。
13.如权利要求12所述的方法,其特征在于,所述第二层包括用于二维第一材料的金属生长基板,并且所述碎片包括喷射自所述金属生长基板的金属原子或金属离子。
14.如权利要求11所述的方法,其特征在于,至少一部分离子、中和离子、或其组合与第一材料的相互作用,在第一材料中引入了多个缺陷;多个离子、中和离子或其组合穿过含有第一材料的第一层,并与第二材料相互作用,并且,所述离子、中和离子、或其组合与第二层的第二材料的相互作用,促进了所述缺陷膨胀成孔。
15.如权利要求14所述的方法,其特征在于,所述第二材料与所述离子、中和离子或其组合相互作用,从而产生第二材料的碎片,其中至少一些来自第二材料的碎片被朝向所述二维材料。
16.如权利要求11所述的方法,其特征在于,所述多层材料进一步包括位于第一层的第一侧上的第三材料的第三层,所述第三层具有从1nm至10nm范围的平均厚度。
17.如权利要求16所述的方法,其特征在于,所述第三层包括沉积硅、沉积聚合物、冷凝气、冷凝有机化合物、或其组合。
18.如权利要求16所述的方法,其特征在于,多个离子、中和离子、或其组合穿过所述第三材料的第三层,与第一材料相互作用;所述离子、中和离子、或其组合与第一材料(2D)的相互作用在第一材料中引入多个缺陷,多个离子、中和离子或其组合穿过含有第一材料的第一层并与第二材料相互作用,并且,至少一部分离子、中和离子、或其组合与所述第二材料和第三材料的相互作用促进了所述缺陷膨胀成孔。
19.如权利要求18所述的方法,其特征在于,所述第三材料与离子、中和离子、或其组合相互作用,从而产生第三材料的碎片,至少一些来自第三材料的碎片被朝向所述二维材料。
20.如权利要求1-10任一项所述的方法,其特征在于,所述第一层具有第一侧和第二侧,其中第一侧面向离子源,并且,所述第二层位于所述第一层的第一侧上并且具有从1nm至10nm的平均厚度。
21.如权利要求20所述的方法,其特征在于,所述第二层包括沉积硅、沉积聚合物、冷凝气、冷凝有机化合物、或其组合。
22.如权利要求20所述的方法,其特征在于,多个离子、中和离子、或其组合穿过所述第二材料的第二层,与二维材料相互作用;所述离子、中和离子、或其组合与第一材料的相互作用在第一材料中引入多个缺陷;以及至少部分的离子、中和离子或其组合与第二材料的相互作用,促进所述缺陷膨胀成孔。
23.如权利要求22所述的方法,其特征在于,所述第二材料与离子、中和离子、或其组合相互作用,从而产生第二材料的碎片,至少一些来自第二材料的碎片被朝向第一材料。
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TWI708278B (zh) * | 2017-08-01 | 2020-10-21 | 倍疆科技股份有限公司 | 在二維層狀半導體以及功能層之間形成高潔淨接面的方法及系統 |
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US20150221474A1 (en) | 2015-08-06 |
JP2017510461A (ja) | 2017-04-13 |
KR20160142820A (ko) | 2016-12-13 |
EP3100297A4 (en) | 2017-12-13 |
EP3100297A1 (en) | 2016-12-07 |
IL247005A0 (en) | 2016-09-29 |
CA2938273A1 (en) | 2015-08-06 |
AU2015210785A1 (en) | 2016-09-08 |
US9870895B2 (en) | 2018-01-16 |
WO2015116946A1 (en) | 2015-08-06 |
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