CN106683991A - 一种石墨烯/金属复合电极的碳纳米管器件的互连方法 - Google Patents
一种石墨烯/金属复合电极的碳纳米管器件的互连方法 Download PDFInfo
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Abstract
本发明公开了一种石墨烯/金属复合电极的碳纳米管器件的互连方法，包括以下步骤：在衬底上设计并制备预图形化的金属薄膜电极；在图形化的金属薄膜电极之间装配碳纳米管；使与金属薄膜电极接触的碳纳米管两端被金属原子刻蚀，形成缺陷；使碳源分子被金属原子催化分解；使石墨烯与碳纳米管两端通过共价成键实现互连。本发明实现了石墨烯与指定碳纳米管特定位置，即对应电极之间的碳纳米管两端的共价连接，这不同于之前石墨烯与碳纳米管间随机的连接。载流子能够在石墨烯与碳纳米管之间良好地输运，降低了石墨烯与碳纳米管的接触电阻，降低了器件的功耗。同时，在预图形化的金属催化基底生长石墨烯，无需转移和刻蚀。
Description
技术领域
本发明属于半导体器件的互连技术领域，特别地涉及一种无转移预图形化石墨烯/金属复合电极的碳纳米管器件的碳-碳共价互连技术。
背景技术
迄今碳纳米管已经在场效应晶体管、传感器、场发射显示器、储能等领域取得了长足的发展。互连电极技术是碳纳米管器件进行系统集成的关键技术之一。现阶段基于碳纳米管的微纳器件通常采用传统金属如金、铂、铜等薄膜电极。但是，金属薄膜电极中电子迁移率较低，同时金属电极与碳纳米管有较大的肖特基势垒，接触电阻较大。这大大地限制了碳纳米管器件在工作电压越来越低的电子系统中的集成应用。
石墨烯具有较高的电子迁移率，能带间隙为零，并且与碳纳米管具有相似的晶格结构，是碳纳米管器件的理想电极。石墨烯通过范德华力与碳纳米管直接接触，可以获得比金属薄膜电极更低的肖特基势垒，接触电阻减小。但是，石墨烯与碳纳米管之间仍属于肖特基接触，接触电阻一般仍远大于碳纳米管本身电阻，而且石墨烯与碳纳米管之间存在的原子级别的物理间隙会引起附加势垒。此外，石墨烯与碳纳米管直接接触的间隙还受到器件工作环境影响，气体吸附等因素也造成接触的不稳定。
现有的石墨烯“加”碳纳米管的复合材料或结构，依其内部的结构特点可分为两类。一类是复合材料中碳纳米管的轴向与石墨烯平面垂直的复合结构，其超大的比表面积特别适用于超级电容器，或者将碳纳米管作为石墨烯与其他材料的层间互连。另一类是复合材料中碳纳米管的轴向与石墨烯平面平行的薄膜，其中的碳纳米管一般都是随机分散地与石墨烯通过范德华力接触。虽然人们正在趋向于尝试经过特别化学处理步骤的基团修饰使碳纳米管与石墨烯之间共价成键，但是，目前已经实现共价连接方法中石墨烯和碳纳米管的连接仍然是随机的。而在碳纳米管器件应用时，其互连需要满足应用所需的特定位置互连的需要。
发明内容
针对现有技术中存在的上述问题和需求，本发明提供了一种预图形化石墨烯/金属复合电极的碳纳米管器件的碳-碳互连方法，目的在于降低碳纳米管与石墨烯电极之间的接触电阻，降低器件的功耗，同时在预图形化的金属催化基底生长石墨烯，无需转移和刻蚀，避免引入额外的杂质和缺陷。
本发明所述方法包括如下步骤：
(1)根据碳纳米管器件的布局，在衬底上设计并制备预图形化的金属薄膜电极；
(2)在碳纳米管和易挥发有机溶剂混合的分散悬浮液中，在预图形化的金属薄膜电极之间装配碳纳米管，使碳纳米管两端与金属薄膜电极连接，形成碳纳米管器件；
(3)将碳纳米管器件在氢气与氩气的混合气氛中高温退火，使与金属薄膜电极接触的碳纳米管两端的部分碳原子被金属原子刻蚀掉，形成缺陷；
(4)以包括甲烷、乙烯和乙炔在内的任一种烃类气体作为碳源气体，通过CVD工艺，使碳源气体分子被碳纳米管器件的金属薄膜电极的金属原子催化分解成含碳自由基，吸附在金属薄膜电极表面，或在金属薄膜电极中大量溶解，达到饱和浓度时在金属表面析出成核生长成石墨烯；石墨烯在碳纳米管缺陷处成核，形成碳-碳键并生长成石墨烯薄膜，石墨烯与碳纳米管两端通过共价成键实现互连。
进一步的，所述电极的厚度为200nm～1.64μm，宽度为0.5～5μm，间距为0.5～6μm。
进一步的，所述步骤(1)中的衬底材料为耐高温材料，包括Si、SiO2、SiO2/Si、GaN、GaAs、SiC或BN中的任意一种。
进一步的，所述步骤(1)中的预图形化的金属薄膜电极材料包括镍、铜、铁、钴和铂等具有催化作用的过渡金属或合金之一，优选原子数比为90:10～60:40铜/镍双层金属薄膜。
进一步的，所述步骤(2)中的易挥发有机溶剂为酒精，碳纳米管/酒精混合分散悬浮液的浓度为0.0001～0.001mg/ml。
进一步的，所述步骤(2)中装配碳纳米管的方法为介电电泳技术或具有实时力/视觉反馈的AFM纳米操作方法。
进一步的，在进行步骤(2)之前，选择性地将碳纳米管和包括浓硫酸、浓硝酸或过氧化氢在内的强氧化剂混合处理，使碳纳米管顶端碳环被强氧化剂破坏，形成开口，用于附着氧化剂基团，从而实现修饰；(同时强氧化剂所含的基团会连接在开口处碳原子上，即在开口处引入包括磺酸基、羧基、羟基基团，实现对碳纳米管的顶端端口的修饰)(碳纳米管两端有完整的碳环结构，强氧化剂将部分碳氧化掉，碳纳米管碳环完整性被破坏，并形成“开口”；有了开口，基团才能连接在开口处；而“端口”是指碳纳米管两端的边缘碳环。基团连接到端口，就是对端口的修饰)。
进一步的，通过改变强氧化剂的浓度、混合处理时间，调节碳纳米管端口上基团数量和位置，使石墨烯与碳纳米管两端通过CVD工艺共价成键互连的过程中，实现对成键数量、成键处碳原子位置和碳原子晶向的调节。
进一步的，所述步骤(3)中为700～1020℃下气体流量为200:100～275:450sccm(标准毫升/分钟)的H2气与Ar气的混合气氛退火0.5～5h，优选为200:450sccm。
进一步的，所述步骤(4)中石墨烯生长是在常压下流量为200:100:2～275:450:4sccm的H2/Ar/CH4混合氛围中700～1020℃生长10～15min。
本发明对衬底上的金属薄膜进行图形化，它作为石墨烯生长的催化基底提供了石墨烯的预图形化。预图形化的金属薄膜作为电极用于装配碳纳米管，使碳纳米管两端与金属薄膜连接。退火工艺中碳纳米管两端被连接的金属薄膜刻蚀，形成缺陷；然后通入碳源气体，碳源气体分子被金属薄膜电极催化分解，在碳纳米管两端的缺陷处成核并生长。图形化的石墨烯薄膜作为电极，与碳纳米管两端共价连接，实现了石墨烯与碳纳米管特定位置，即碳纳米管两端的共价连接，这不同于之前石墨烯与碳纳米管间随机的连接。
本发明以石墨烯与特定位置上的单根碳纳米管(或多根碳纳米管)共价成键形成碳纳米管器件的互连电极为目标，提供了一种无转移预图形化石墨烯/金属复合电极的碳纳米管器件的平面内的互连技术，碳纳米管的轴向与石墨烯平面平行。石墨烯/金属复合电极中的石墨烯与碳纳米管两端共价成键，使得载流子能够有效地从石墨烯电极输运到碳纳米管，降低了碳纳米管与石墨烯电极之间的接触电阻，与现有技术相比，本发明具有以下有益效果:
石墨烯/金属复合电极中石墨烯与碳纳米管两端之间形成碳-碳共价键，载流子能够在石墨烯与碳纳米管之间良好地输运，降低了石墨烯与碳纳米管的接触电阻，降低了器件的功耗，实现了碳纳米管器件的良好互连。同时，在预图形化的金属催化基底生长石墨烯，无需转移和刻蚀，是一种良好的碳纳米管器件互连的解决方案。
附图说明
图1是预图形化石墨烯/金属复合电极与碳纳米管的互连结构示意图。
图2是预图形化石墨烯/金属复合电极的碳纳米管器件的互连方法的示意图。
在所有附图中，相同的附图标记用来表示相同的元件或结构，其中：1为衬底，21、22为金属电极，3为碳纳米管，41、42为石墨烯。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
本发明形成的预图形化石墨烯/金属复合电极的碳纳米管器件的互连结构如图1所示。其特征在于：衬底1采用耐高温材料，在衬底上形成两个金属薄膜电极21、22，两个电极的距离为0.5～6μm；单根或多根碳纳米管3架设在两个石墨烯电极41、42之间，碳纳米管长度大于0.5μm；以金属薄膜21、22作为催化剂，以CVD方法原位生长的图形化石墨烯电极41、42，在金属薄膜电极与碳纳米管3接触部分形成共价连接，构成互连结构。
如图2所示，本发明提供的预图形化石墨烯/金属复合电极与碳纳米管互连结构的制备方法即工艺步骤如下：
(1)采用物理气相沉积工艺和光刻工艺在衬底表面1制备出预图形化的金属薄膜电极，如图2(a)、(b)所示；
(2)配置碳纳米管/酒精混合分散悬浮液。选择性地，在配置前将碳纳米管和包括浓硫酸、浓硝酸或过氧化氢在内的强氧化剂混合处理，使碳纳米管顶端碳环被强氧化剂破坏，形成开口，用于附着氧化剂基团，从而实现修饰。
(3)采用介电电泳技术或利用AFM操作在预图形化金属21和22之间间装配碳纳米管3，使碳纳米管3的两端与金属薄膜电极21、22连接，如图2(c)所示；
(4)在H2气与Ar气混合气氛中进行退火处理，退火温度为700～1020℃，退火时间为0.5～5h，使与金属薄膜电极接触的碳纳米管两端被金属原子刻蚀，形成缺陷；
(5)通入碳源气体，通过CVD工艺在图形化的铜镍电极上生长石墨烯41、42，形成预图形化石墨烯/金属复合电极的碳纳米管器件的碳-碳共价互连，如图2(d)所示。
本发明提供的预图形化石墨烯/金属复合电极与碳纳米管互连结构的制备方法中利用介电电泳或AFM操作装配碳纳米管的方法都是现有技术。装配碳纳米管时用的是碳纳米管/酒精(挥发性有机溶剂)分散悬浮液，碳纳米管参数的选取取决于具体器件应用的需求。
介电电泳技术需要用到的设备包括：移液器，交流信号发生射器。AFM操作需要用到的设备包括：需要一台原子力显微镜，即AFM。
下面结合附图和实施例对本发明中的预图形化石墨烯/金属复合电极与碳纳米管互连结构的制备方法，即工艺步骤作进一步详细的说明。
实施例1
(1)以生长有氧化层的硅片作为衬底，采用磁控溅射分别淀积厚度为640nm的镍膜、1μm的铜膜，使铜与镍原子数比为60.6:39.4。
(2)采用光刻和化学刻蚀工艺，对铜/镍双层金属薄膜进行图形加工，得到相应的碳纳米管器件用的互连电极布局，电极间距为6μm，电极宽度为5μm。
(3)在图形化铜/镍电极之间加上频率为1MHz、峰峰值为16V的正弦交流电压，用移液器取0.001mg/mL的碳纳米管/酒精分散悬浮液滴在电极之间，待溶剂挥发后撤除外加电场。
(4)在700℃下气体流量为200:100sccm的H2气与Ar气混合气氛中退火5h，然后升温至1020℃，在常压下通入流量为200:100:2sccm的H2/Ar/CH4混合气体，生长15min。CVD工艺在图形化的催化基底上生长石墨烯，实现预图形化石墨烯/金属复合电极的碳纳米管器件的碳-碳共价互连。
实施例2
(1)以石英玻璃为衬底，采用光刻工艺，在衬底表面得到催化基底图形的反转图案。
(2)采用电子束蒸发工艺，在衬底上分别淀积厚度110nm的镍膜、1μm的铜膜，使铜与镍原子数比为90:10。
(3)将衬底置于丙酮中超声数分钟，去掉光刻胶上的铜/镍膜部分。依次置于乙醇、去离子水中超声清洗10min，通过剥离工艺得到图形化的铜/镍双层金属薄膜，即相应的碳纳米管器件用的互连电极布局，电极间距为3μm，电极宽度为2μm。
(4)用移液器取0.001mg/mL的碳纳米管/酒精分散悬浮液滴在铜/镍电极之间，待溶剂挥发后用AFM探针推动碳纳米管，使碳纳米管装配在电极之间。
(5)在1020℃下气体流量为275:450sccm的H2气与Ar气混合气氛中退火0.5h，然后在常压下通入流量为275:450:4sccm的H2/Ar/CH4混合气体，生长15min。CVD工艺在图形化的催化基底上生长石墨烯，实现预图形化石墨烯/金属复合电极的碳纳米管器件的碳-碳共价互连。
实施例3
(1)以生长有氧化层的硅片作为衬底，采用磁控溅射淀积厚度200nm的镍薄膜。
(2)采用光刻和化学刻蚀工艺，对镍薄膜进行图形加工，得到相应的碳纳米管器件用的互连电极布局，电极间距为0.5μm，电极宽度为0.5μm。
(3)在图形化镍电极之间加上频率为1MHz、峰峰值为16V的正弦交流电压，用移液器取0.0002mg/mL的碳纳米管/酒精分散悬浮液滴在电极之间，待溶剂挥发后撤除外加电场。
(4)气体流量为250:450:2sccm的H2/Ar/CH4混合气体在750℃下预先加热，然后再通入CVD生长区域，在常压700℃下生长10min。CVD工艺在图形化的镍薄膜上生长石墨烯，实现预图形化石墨烯/金属复合电极的碳纳米管器件的碳-碳共价互连。
实施例4
(1)以SiC作为衬底，采用磁控溅射分别淀积200nm的镍薄膜。
(2)采用光刻和化学刻蚀工艺，对镍金属薄膜进行图形化，得到相应的碳纳米管器件用的互连电极布局，电极间距为6μm，电极宽度为5μm。
(3)将碳纳米管和浓硫酸混合处理，碳纳米管顶端的碳环被浓硫酸破坏形成开口，磺酸基对单壁碳纳米管的顶端端口进行修饰，配置成0.0001mg/mL的碳纳米管/酒精分散悬浮液，在图形化的镍电极之间加上频率为1MHz、峰峰值为16V的正弦交流电压，用移液器将碳纳米管/酒精分散悬浮液滴在电极之间，待溶剂挥发后撤除外加电场。
(4)升温至1020℃，在气体流量为250:450:2sccm的H2/Ar/CH4混合气氛中生长15min。CVD工艺在图形化的镍薄膜上生长石墨烯，实现预图形化石墨烯/金属复合电极的碳纳米管器件的碳-碳共价互连。
实施例5
(1)以SiC作为衬底，采用磁控溅射淀积200nm的镍薄膜。
(2)采用光刻和化学刻蚀工艺，对镍金属薄膜进行图形化，得到相应的碳纳米管器件用的互连电极布局，电极间距为3μm，电极宽度为2μm。
(3)将碳纳米管和浓硝酸混合处理，碳纳米管顶端的碳环被浓硝酸破坏形成开口，采用羧基对单壁碳纳米管的顶端端口进行修饰，配置成0.0001mg/mL的碳纳米管/酒精分散悬浮液，在图形化的镍电极之间加上频率为1MHz、峰峰值为16V的正弦交流电压，用移液器将碳纳米管/酒精分散悬浮液滴在电极之间，待溶剂挥发后撤除外加电场。
(4)升温至1020℃，在气体流量为250:450:2sccm的H2/Ar/CH4混合气氛中生长15min。CVD工艺在图形化的镍薄膜上生长石墨烯，实现预图形化石墨烯/金属复合电极的碳纳米管器件的碳-碳共价互连。
实施例6
(1)以SiC作为衬底，采用磁控溅射淀积200nm的镍薄膜。
(2)采用光刻和化学刻蚀工艺，对镍金属薄膜进行图形化，得到相应的碳纳米管器件用的互连电极布局，电极间距为6μm，电极宽度为5μm。
(3)将碳纳米管和过氧化氢混合处理，碳纳米管顶端的碳环被过氧化氢破坏形成开口，羟基对单壁碳纳米管的顶端端口进行修饰，配置成0.0001mg/mL的碳纳米管/酒精分散悬浮液，在图形化的镍电极之间加上频率为1MHz、峰峰值为16V的正弦交流电压，用移液器将碳纳米管/酒精分散悬浮液滴在电极之间，待溶剂挥发后撤除外加电场。
(4)升温至1020℃，在气体流量为250:450:2sccm的H2/Ar/CH4混合气氛中生长15min。CVD工艺在图形化的镍薄膜上生长石墨烯，实现预图形化石墨烯/金属复合电极的碳纳米管器件的碳-碳共价互连。
本发明提出来的预图形化石墨烯/金属复合电极的碳纳米管器件的碳-碳共价互连方法，可以降低碳纳米管器件与电极之间的接触电阻，实现碳纳米管器件的良好互连。同时，在预图形化的金属催化薄膜上生长石墨烯可以避免石墨烯的转移、刻蚀，不会额外导致石墨烯缺陷。
本领域的技术人员容易理解，以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。
Claims (10)
1.一种石墨烯/金属复合电极的碳纳米管器件的互连方法，其特征在于，包括如下步骤：
(1)根据碳纳米管器件的布局，在衬底上设计并制备预图形化的金属薄膜电极；
(2)在碳纳米管和易挥发有机溶剂混合的分散悬浮液中，在预图形化的金属薄膜电极之间装配碳纳米管，使碳纳米管两端与金属薄膜电极连接，形成碳纳米管器件；
(3)将碳纳米管器件在氢气与氩气的混合气氛中高温退火，使与金属薄膜电极接触的碳纳米管两端的部分碳原子被金属原子刻蚀掉，形成缺陷；
(4)以包括甲烷、乙烯和乙炔在内的任一种烃类气体作为碳源气体，通过CVD工艺，使碳源气体分子被碳纳米管器件的金属薄膜电极的金属原子催化分解成含碳自由基，吸附在金属薄膜电极表面，或在金属薄膜电极中大量溶解，达到饱和浓度时在金属表面析出成核生长成石墨烯；石墨烯在碳纳米管缺陷处成核，形成碳-碳键并生长成石墨烯薄膜，石墨烯与碳纳米管两端通过共价成键实现互连。
2.根据权利要求1所述的方法，其特征在于，所述电极的厚度为200nm～1.64μm，宽度为0.5～5μm，间距为0.5～6μm。
3.根据权利要求1或2所述的方法，其特征在于，所述步骤(1)中的衬底材料为耐高温材料，包括Si、SiO2、SiO2/Si、GaN、GaAs、SiC或BN中的任意一种。
4.根据权利要求1或2所述的方法，其特征在于，所述步骤(1)中的预图形化的金属薄膜电极材料包括镍、铜、铁、钴和铂等具有催化作用的过渡金属或合金之一，优选原子数比为90:10～60:40铜/镍双层金属薄膜。
碳纳米管/酒精混合分散悬浮液的浓度为0.0001～0.001mg/ml。
5.根据权利要求1或2所述的方法，其特征在于，所述步骤(2)中的易挥发有机溶剂为酒精，碳纳米管/酒精混合分散悬浮液的浓度为0.0001～0.001mg/ml。
6.根据权利要求1或2所述的方法，其特征在于，所述步骤(2)中装配碳纳米管的方法为介电电泳技术或具有实时力/视觉反馈的AFM纳米操作方法。
7.根据权利要求1或2所述的方法，其特征在于，在进行步骤(2)之前，选择性地将碳纳米管和包括浓硫酸、浓硝酸或过氧化氢在内的强氧化剂混合处理，使碳纳米管顶端碳环被强氧化剂破坏，形成开口，用于附着氧化剂基团，从而实现修饰。
8.根据权利要求7所述的方法，其特征在于，通过改变强氧化剂的浓度、混合处理时间，调节碳纳米管端口上基团数量和位置，使石墨烯与碳纳米管两端通过CVD工艺共价成键互连的过程中，实现对成键数量、成键处碳原子位置和碳原子晶向的调节。
9.根据权利要求1所述的方法，其特征在于，所述步骤(3)中为700～1020℃下气体流量为200:100～275:450sccm(标准毫升/分钟)的H2气与Ar气的混合气氛退火0.5～5h，优选为200:450sccm。
10.根据权利要求1所述的方法，其特征在于，所述步骤(4)中石墨烯生长是在常压下流量为200:100:2～275:450:4sccm的H2/Ar/CH4混合氛围中700～1020℃生长10～15min。
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