CN104538295A - 一种基于pmma的碳质电极制备方法 - Google Patents
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Abstract
本发明涉及一种基于PMMA的碳质电极制备方法,包括以下制备步骤:(1)通过匀胶工艺将PMMA溶液均匀覆盖在待做电极的基板表面,并烘干固化形成覆盖于基板表面的PMMA薄膜;(2)在基板所需要制备电极的位置并根据电极的形状,利用电子束曝光设备对覆盖有PMMA薄膜的基板进行电子束辐照,辐照剂量需要足以使得PMMA变性,即由正胶特性转变为负胶特性;优选电子束能量大于5keV;(3)将经过上述(2)处理的整个基板在真空或者惰性气体的保护下进行高温退火处理,优选退火温度大于400℃。本发明具有良好的兼容性;极大地简化了电极制备工序、减少了设备投入、节约了制备成本;对基板破坏更小,制备的电极导电性能更优异;与传统的金属材质一起,丰富了电极材料的可选择性。
Description
技术领域
本发明涉及一种非金属电极的制备方法,属于微纳电子器件制备和研究领域。
背景技术
目前各种具有优异性能的新材料不断被发现,特别是以石墨烯为代表的二维材料发展迅速,而这些材料的应用和研究大部分都需要被做成电子器件,从而来研究其电学性能或者通过电学性能的变化来研究其它比如光学、力学、磁学等方面的性能,而制作这些微纳器件的关键就在于电极的制备。传统的电极基本都是采用金属材料,比如铬(Cr),钛(Ti),钯(Pd),金(Au)等等。制备工艺主要包括金属蒸镀和离子束/电子束诱导沉积这两类方式。金属蒸镀首先需要利用电子束曝光或者光学曝光结合光刻胶显影、定影技术来制作确定电极形状的掩膜版(包括光刻胶掩膜版),然后利用电子束蒸发、热蒸发、磁控溅射、离子溅射等方式蒸镀金属薄膜,最后通过剥离工艺得到所需形状的金属电极。这种工艺虽然比较成熟,但是工艺流程复杂繁琐,对贵重金属的消耗也很大,而且所用到的光刻胶仅仅是作为牺牲层,造成原材料的极大浪费。而离子束诱导沉积的方式会对样品产生严重的损伤和破坏,电子束诱导沉积制备的电极导电性非常差,并且诱导沉积所需的气体源都非常昂贵。另一方面,金属与半导体材料的接触容易形成肖特基势垒或者较大的接触电阻,严重影响电子器件的性能。因此,一种简单易行的非金属电极制备方式对于微纳电子器件的发展和研究将具有重要的意义。
发明内容
本发明的目的在于提出一种基于PMMA的碳质电极制备方法,以克服现有工艺中流程复杂,成本昂贵,制备周期长等方面的不足,同时也为电极材料提供更广泛的选择。
为实现上述发明目的,本发明采用了如下技术方案:
一种基于PMMA的碳质电极制备方法,包括以下制备步骤:
(1). 通过匀胶工艺将PMMA溶液均匀覆盖在待做电极的基板表面,并烘干固化形成覆盖于基板表面的PMMA薄膜;
(2). 在基板所需要制备电极的位置并根据电极的形状,利用电子束曝光设备对覆盖有PMMA薄膜的基板进行电子束辐照,辐照剂量需要足以使得PMMA变性,即由正胶特性转变为负胶特性。优选电子束能量大于5 keV;
(3). 将经过上述(2)处理的整个基板在真空或者惰性气体的保护下进行高温退火处理,优选退火温度大于400 ℃。高温退火处理能提高负性PMMA的导电性能,同时使得没有受到电子束辐照或者受到辐照但还没有变性的PMMA分解为可挥发性气体。从而只保留具有电极形状的负性PMMA,电极制备过程完毕。
上述技术方案中,为了使得没有受到电子束辐照或者受到辐照但还没有变性的PMMA去除更加干净,可在步骤 (2) 之后,步骤 (3) 之前,增加步骤(4)即用丙酮等能溶解PMMA的有机溶剂清洗基板。特别声明,此步骤(4)仅做改进之用,并非本发明所涉及的碳质电极制备方法的必要步骤,属于本发明保护的范围但不是对本发明的限制。
上述技术方案中,所述的待做电极的基板根据不同的电子器件采用不同的材质,如Si,SiO2,石英,树脂,环氧树脂玻纤固化板等。
与现有技术相比,本发明的有益效果在于: 作为本发明实施过程中最主要的加工手段和原材料——电子束曝光和PMMA,都是现有微纳加工技术中最为普遍的,因此本发明具有与现有技术良好的兼容性;与传统的电子束曝光或者光学曝光与金属蒸镀工艺相结合的电极制备工艺相比,本发明涉及的电极制备方法不需要对光刻胶进行显影、定影等工艺步骤,也不需要任何形式的金属蒸镀,而是直接以电子束抗蚀剂PMMA作为电极的原材料,由电子束直写而成,极大地简化了电极制备工序、减少了设备投入、节约了制备成本;与聚焦离子束/电子诱导沉积制备电极的方式相比,本发明涉及的电极制备方法对基板破坏更小,制备的电极导电性能更优异;本发明制备的电极是碳质材料,进一步说是石墨的纳米颗粒或纳米碎片,与传统的金属材质一起,丰富了电极材料的可选择性。
附图说明
图1为本发明的工艺流程示意图,其中虚线表示步骤(4)可以加上也可以省略;
图2为按本发明方法制备的电极的特性表征:(a) X射线能量散射谱(EDS);(b) 拉曼(Raman)谱;(c) 高分辨率透射电子显微照片(HRTEM)。其中,(a)通过EDS分析表明,该方法制备的电极材料元素主要为碳元素;(b)通过拉曼散射,表明该材料具有与石墨相类似的结构;(c)通过高分辨透射电子显微镜看到,该材料含有结晶颗粒,且结晶形状符合石墨的层状叠加结构,层间距为0.33-0.34 nm,与石墨的层间距完全一致,表明该材料确实是由石墨纳米颗粒或者纳米碎片组成。
图3为实施例中应用本发明制备的具有碳质电极的石墨烯场效应晶体管的SEM照片;
图4为图3中石墨烯场效应晶体管的性能测试:(a)I-V特性曲线,(b)背栅场效应曲线。表明用该方法制备的碳质电极石墨烯场效应晶体管具有与金属电极石墨烯场效应晶体管相媲美的电学特性。
具体实施方式
本发明中,术语“PMMA”是指聚甲基丙烯酸甲酯,英文名称Poly(methyl methacrylate)。“PMMA溶液”是指含有PMMA分子的任何溶液,与何种溶剂无关,与何种分子量的PMMA无关,与溶液中PMMA的固体含量无关,与溶液浓度无关,与溶液中是否含有其它添加物无关。
术语“匀胶工艺”包括但不限于旋涂、滚涂、浸涂、喷涂等等方式。
术语“电子束曝光设备”是指能实现对样品进行电子束辐照的设备装置,包括但不限于电子束曝光机、聚焦电子束/离子束系统、扫描电子显微镜和透射电子显微镜等。
术语“高温退火”是指将样品以适当的速度加热到一定温度,并保持一定时间,然后又以适当的速度冷却,以改变或者改善样品的性能。加热方式包括但不限于红外线加热、电磁加热、微波加热、电阻炉加热、感应加热、辐射加热、激光加热等等。冷却方式可以是自然冷却也可以用其它方式辅助冷却。
下面将结合附图及具体应用实施例,对基于PMMA的碳质电极制备方法作进一步的详细说明。
实施例:
制备具有碳质电极的石墨烯场效应晶体管,包括以下制备步骤:
(1). 通过旋涂的方式(旋涂速率1000 rpm)将分子量为950K,固体含量4%的PMMA乳酸乙酯 (ethyl lactate) 溶液均匀覆盖在转移有石墨烯条带的衬底基板上,并在热板上用温度180 ℃烘烤2分钟,使PMMA固化。此处的衬底基板为表面有300 nm厚SiO2的掺杂硅,硅衬底基板同时将作为石墨烯场效应晶体管的栅极。
(2). 在上述固化有PMMA的基板上有石墨烯条带的位置处根据设计的电极形状 (如图3) ,利用聚焦离子束/电子束 (双束) 系统对样品进行电子束辐照,辐照剂量为2750 C/m2。电子束能量为10 keV,束流为22 nA。
(3). 将上述经(2)处理的基板从双束系统中取出,于丙酮溶液中静置1分钟,以溶解未受电子束辐照的PMMA。
(4). 将上述整个样品在Ar气 (5%H2+95%Ar) 的保护下进行高温退火处理,退火温度为800 ℃,退火时间2小时,得到具有碳质电极的石墨烯场效应晶体管。
附图3所示为制备的具有碳质电极的石墨烯场效应晶体管的SEM照片,可以看到,制备的电极非常规则,与衬底粘附性很好。
附图4所示为上述具有碳质电极的石墨烯场效应晶体管的电学性能测试,其中(a)为I-V曲线,(b)为背栅的场效应曲线,可以看到,I-V曲线为直线,表明碳质电极与石墨烯具有良好的欧姆接触,同时场效应曲线也表现出明显的双极性,具有石墨烯的典型特征。
上述石墨烯场效应晶体管仅为本发明的一个具体应用实例,并不能以此限制本发明的保护范围。
Claims (4)
1.一种基于PMMA的碳质电极制备方法,其特征在于,包括以下制备步骤:
(1)通过匀胶工艺将PMMA溶液均匀覆盖在待做电极的基板表面,并烘干固化形成覆盖于基板表面的PMMA薄膜;
(2)在基板所需要制备电极的位置并根据电极的形状,利用电子束曝光设备对覆盖有PMMA薄膜的基板进行电子束辐照,辐照剂量需要足以使得PMMA变性,即由正胶特性转变为负胶特性;优选电子束能量大于5 keV;
(3)将经过上述(2)处理的整个基板在真空或者惰性气体的保护下进行高温退火处理,优选退火温度大于400 ℃。
2. 根据权利要求1所述的基于PMMA的碳质电极制备方法,其特征在于,为了使得没有受到电子束辐照或者受到辐照但还没有变性的PMMA去除更加干净,可在步骤 (2) 之后,步骤 (3) 之前,增加步骤(4)即用丙酮等能溶解PMMA的有机溶剂清洗基板。
3.根据权利要求1所述的基于PMMA的碳质电极制备方法,其特征在于,所述的待做电极的基板根据不同的电子器件采用不同的材质。
4.根据权利要求3所述的基于PMMA的碳质电极制备方法,其特征在于,基板材质采用如Si、SiO2、石英、树脂或环氧树脂玻纤固化板。
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