CN111863966A - 一种硅基背栅全石墨烯场效应晶体管的制备方法 - Google Patents
一种硅基背栅全石墨烯场效应晶体管的制备方法 Download PDFInfo
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Abstract
本发明属于纳机电系统应用领域，具体涉及一种硅基背栅全石墨烯场效应晶体管的制备方法；首先采用机械剥离法制备出高质量单层石墨烯，经转移到Si/SiO2衬底上后，旋涂氢‑倍半硅氧烷(HSQ)抗蚀剂作为掩模版，借助电子束曝光对其进行图案化处理，随后通过氧等离子体对其进行刻蚀处理，最终得到器件尺寸可控的硅基背栅全石墨烯场效应晶体管；本发明根据石墨烯量子限域效应，把片层半金属特性石墨烯作为电极，半导体特性石墨烯纳米带作为沟道，通过图案化处理，一次性刻蚀成全石墨烯器件，避免了多次转移带来的缺陷，回避了外接电极引入的接触电阻与寄生电容，提高了器件的电学特性。
Description
技术领域
本发明属于纳机电系统应用领域，具体涉及一种硅基背栅全石墨烯场效应晶体管的制备方法。
背景技术
石墨烯是碳原子以sp2轨道杂化组成的六角蜂窝状平面结构，拥有独特的机械和电学性能。它独特的电学性能源于其特殊的电子能带结构，本征石墨烯具有极高的载流子迁移率，室温下可达15000cm2V-1s-1。此外，石墨烯还具有非常好的光学和热力学性质，这些特性促使石墨烯在纳机电系统应用领域具有极大的研究意义。但是由于石墨烯是零带隙半导体，在逻辑器件应用中无法实现电流的关断。这极大地阻碍着石墨烯在电学领域中的应用。理论计算表明，由于量子限域效应，将石墨烯裁剪成准一维的纳米带状结构(宽度小于50nm)可打开石墨烯带隙，且带隙大小与石墨烯纳米带的宽度成反比，这为石墨烯场效应晶体管提供契机，为石墨烯在逻辑电路中的应用奠定了理论基础。
目前石墨烯场效应晶体管的制备面临的困难主要有两点：首先是石墨烯纳米带的制备；尽管目前已有报道通过化学衍生法制备石墨烯纳米带，但该方法需要通过特殊单体发生环化聚合反应，反应过程复杂，且难以找到合适的单体分子，不适合任意宽度石墨烯纳米带的制备；同时，也有文献报道采用裂解碳纳米管法法制备石墨烯纳米带，但是酸解碳纳米管的同时不可避免地引入离子掺杂，影响石墨烯纳米带的电学特性。另一个难点就是石墨烯纳米带的转移，对于亚微米级石墨烯纳米带进行电学性能表征，就必须搭建器件，这其中涉及到样品的转移。就目前来看，转移难度较大，并且在转移的过程中，不可避免地引入杂质，这也随机性的影响器件的性能。
采用有掩模氧等离子体刻蚀的方法制备全石墨烯器件，可以避免了传统器件制备中操作复杂、引入离子掺杂等缺陷，通过机械剥离的方式制备单层石墨烯膜，再直接转移到氧化硅衬底上，随后借助电子束曝光技术对石墨烯进行图案化处理，最终利用氧等离子体刻蚀加工得到全石墨烯场效应晶体管。这种先转移后刻蚀的的方式避免了后期对石墨烯纳米带的转移，为全石墨烯器件规模化制备提供了可能性。
发明内容
本发明的目的在于克服现有技术中存在的技术缺陷，提出一种硅基背栅全石墨烯场效应晶体管的制备方法，先通过电子束曝光技术进行掩模图案化处理，再借助氧等离子体刻蚀石墨烯，一次性制备背栅硅基全石墨烯场效应晶体管器件。较传统方法相比，没有引入离子掺杂，同时也避免了对石墨烯纳米带沟道及石墨烯电极得转移，简化了传统全石墨烯器件的制备，提升了器件的电学性能，使其规模化生产成为可能。
为了实现以上目的，本发明包括以下步骤：
(1)首先采用机械剥离法制备单层石墨烯薄膜，再经干法转移将其转移到Si/SiO2衬底上，得到石墨烯样品；
(2)将步骤(1)得到的石墨烯样品旋涂氢-倍半硅氧烷(HSQ)无机光刻胶，具体步骤为：先低速旋涂，持续一段时间后，转为中高速旋涂，旋涂完毕，得到的样品转移到恒温加热台，经烘干处理得到图案化掩模版；
(3)将步骤(2)中得到的图案化掩模版进行电子束曝光处理，具体步骤为：首先打开电子束光刻机(EBL)舱门，将图案化掩模版固定在载物台上，关闭舱门，设定曝光参数进行曝光处理，曝光完毕后取出图案化掩模版进行显影和定影处理，烘烤后得到待刻蚀样品；
(4)将步骤(3)中得到的待刻蚀样品，通过氧等离子体刻蚀工艺制备石墨烯纳米带沟道和石墨烯电极，最后进行剥离工艺洗去HSQ光刻胶，得到硅基背栅全石墨烯场效应晶体管。
进一步的，步骤(2)中，所述低速旋涂转速为500rpm，持续时间4-8s；所述中高速旋涂转速为3000rpm，持续时间50-60s。
进一步的，步骤(2)中，所述恒温加热台的温度为150℃，烘干的时间为50-60s。
进一步的，步骤(2)中，所述得到图案化掩模版的旋涂光刻胶的厚度为45～50nm。
进一步的，步骤(3)中所述曝光参数设定：电子剂量为1mC/cm 2，电子束流选用400pA。
进一步的，步骤(3)中所述显影和定影处理中，显影剂为0.26mol/L的四甲基氢氧化铵(TMAH)水溶液，显影时间为30-60s。
进一步的，步骤(3)中所述烘烤的温度为30-80℃，烘烤时间50-60s。
进一步的，步骤(4)中所述氧等离子体刻蚀工艺过程中的功率为45-60W，真空度低于28Pa，处理时间为30-50s。
进一步的，步骤(4)中所述剥离工艺使用丙酮和异丙醇有机溶液，所述剥离的时间为1-2h。
本发明的有益效果是：本发明利用石墨烯的尺寸效应，把石墨烯纳米带作沟道，片层石墨烯作电极，充分利用石墨烯不同尺寸下的半导体特性和金属特性制备器件。具体通过电子束曝光技术图案化，借助等离子体刻蚀，最终得到全石墨烯场效应晶体管器件。与传统器件相比，该方法避免了多次转移，理论上提高了场效应管的电学性能。同时，在旋涂光刻胶过程中，低速旋涂时间5s，中高速旋涂时间为60s时，旋涂厚度达到50nm最佳厚度。除此之外，本征石墨烯做电极取代了传统的贵金属电极，这种电极与沟道之间的无缝连接，回避了传统器件中接触电阻、寄生电容的影响，进一步优化了栅介质界面，保证了全石墨烯器件高迁移率；随着高品质石墨烯制备的不断突破，本方法可能为全石墨烯器件的规模化制备提供了契机。
附图说明
图1是机械剥离法制备石墨烯转移示意图。
图2是单层石墨烯结构示意图。
图3是曝光显影后待刻蚀样品示意图。
图4是单层石墨烯拉曼光谱图像。
图5是氧等离子体刻蚀示意图。
图6是硅基背栅全石墨烯场效应晶体管电学测试原理图。
图7是硅基背栅全石墨烯场效应晶体管转移特性曲线。
图中标号为：1-粘有石墨烯的胶带；2-Si/SiO2衬底；3-加热台；4-单层石墨烯薄膜；5-HSQ光刻胶；6-氧等离子体；7-源极；8-石墨烯纳米带沟道；9-漏极。
具体实施方式
下面结合说明书附图和具体实施实例对本发明做进一步说明，但本发明不局限于这些实施例。
实施例1：
本发明先采用机械剥离法制备出高质量单层石墨烯，再转移到Si/SiO2衬底上，然后旋涂氢-倍半硅氧烷(HSQ)抗蚀剂作为掩模版，借助电子束曝光(EBL)对其进行图案化处理，之后进行显影烘干，通过氧等离子体对其进行刻蚀处理，最终得到器件尺寸可控的全石墨烯背栅场效应晶体管。本发明利用了石墨烯量子限域效应，把片层石墨烯作为电极，石墨烯纳米带作为沟道，通过图案化处理，一次性刻蚀成全石墨烯器件。
(1)采用机械剥离法制备单层石墨烯薄膜，首先将Si片置入无水乙醇溶液中利用低频超声波震荡的方式进行超声清洗；其中超声波频率为：20kHz～1MHz，功率密度为：0.5-1.0W/cm-2，清洗时间为：2-3min。清洗完成后通氮气将其吹干,放到样品盒内待用。然后用剥离专用胶带粘取块体石墨，同时取一条新胶带与之对贴，重复约30-50次。如图1所示，将少层的石墨烯贴在以清洗的硅衬底上，放置在加热台上轻轻按压约30s。然后将石墨烯样品置于光镜下观察，直至观察到淡蓝色接近透明薄膜，最后将准单层石墨烯样品进行拉曼表征，如图3所示，发现D、G、2D等特征峰位置分别位于1350cm-1、1580cm-1、2670cm-1附近，同时发现G峰强度不明显且2D峰强度为G峰强度两倍，可以确定样品为单层少缺陷石墨烯。
(2)将表征后的石墨烯样品置入匀胶机中，旋涂光刻胶，在旋涂HSQ过程中，先采用500rpm低速旋涂，持续时间为5s，后采用3000rpm中高速旋涂，持续时间60s，双速旋涂保证受胶均匀且不易损坏样品，最终光刻胶的厚度约为50nm。
(3)接下来将旋涂好的样品进行电子束曝光处理，曝光过程中，选用剂量为1mC/cm2，之后，将图案化后的样品置入0.26mol/L的四甲基氢氧化铵(TMAH)水溶液进行显影，显影时间30-60s，接下来放入30-80℃的环境中烘烤60s，最终的到如图4所示的待刻蚀样品，其中，沟道尺寸为2μm×50nm，电极尺寸为2μm×2μm。
(4)将得到待刻蚀样品放入等离子处理仪中刻蚀处理，如图5是氧等离子体刻蚀示意图；所示，采用的刻蚀功率为45-60W，真空度低于28Pa，处理时间为30-50s。经过去离子水清理并氮气干燥，随后300℃氩气环境退火2h，最终得到的硅基背栅全石墨烯场效应晶体管器件，结构如图6所示。
最后，对本发明制备的硅基背栅全石墨烯场效应晶体管电学性能测试，电学测试曲线如图7所示，结果显示器件的载流子迁移率达到371.6cm2V-1s-1，电流开关比达到103。
说明：以上实施例仅用以说明本发明而并非限制本发明所描述的技术方案；因此，尽管本说明书参照上述的各个实施例对本发明已进行了详细的说明，但是本领域的普通技术人员应当理解，仍然可以对本发明进行修改或等同替换；而一切不脱离本发明的精神和范围的技术方案及其改进，其均应涵盖在本发明的权利要求范围内。
Claims (9)
1.一种硅基背栅全石墨烯场效应晶体管的制备方法，其特征在于，具体步骤如下：
(1)首先采用机械剥离法制备单层石墨烯薄膜，再经干法转移将其转移到Si/SiO2衬底上，得到石墨烯样品；
(2)将步骤(1)得到的石墨烯样品旋涂氢-倍半硅氧烷无机光刻胶，具体步骤为：先低速旋涂，持续一段时间后，转为中高速旋涂，旋涂完毕，得到的样品转移到恒温加热台，经烘干处理得到图案化掩模版；
(3)将步骤(2)中得到的图案化掩模版进行电子束曝光处理；具体步骤为：首先打开电子束光刻机舱门，将图案化掩模版固定在载物台上，关闭舱门，设定曝光参数进行曝光处理，曝光完毕后取出图案化掩模版进行显影和定影处理，烘烤后得到待刻蚀样品；
(4)将步骤(3)中得到的待刻蚀样品，通过氧等离子体刻蚀工艺制备石墨烯纳米带沟道和石墨烯电极，最后进行剥离工艺洗去氢-倍半硅氧烷光刻胶，得到硅基背栅全石墨烯场效应晶体管。
2.根据权利要求1所述的一种硅基背栅全石墨烯场效应晶体管的制备方法，其特征在于，步骤(2)中，所述低速旋涂转速为500rpm，持续时间4-8s；所述中高速旋涂转速为3000rpm，持续时间50-60s。
3.根据权利要求1所述的一种硅基背栅全石墨烯场效应晶体管的制备方法，其特征在于，步骤(2)中，所述恒温加热台的温度为150℃，烘干的时间为50-60s。
4.根据权利要求1所述的一种硅基背栅全石墨烯场效应晶体管的制备方法，其特征在于，步骤(2)中，所述得到图案化掩模版的旋涂光刻胶的厚度为45～50nm。
5.根据权利要求1所述的一种硅基背栅全石墨烯场效应晶体管的制备方法，其特征在于，步骤(3)中所述曝光参数设定：电子剂量为1mC/cm2，电子束流选用400pA。
6.根据权利要求1所述的一种硅基背栅全石墨烯场效应晶体管的制备方法，其特征在于，步骤(3)中所述显影和定影处理中，显影剂为0.26mol/L的四甲基氢氧化铵水溶液，显影时间为30-60s。
7.根据权利要求1所述的一种硅基背栅全石墨烯场效应晶体管的制备方法，其特征在于，步骤(3)中所述烘烤的温度为30-80℃，烘烤时间50-60s。
8.根据权利要求1所述的一种硅基背栅全石墨烯场效应晶体管的制备方法，其特征在于，步骤(4)中所述氧等离子体刻蚀工艺过程中的功率为45-60W，真空度低于28Pa，处理时间为30-50s。
9.根据权利要求1所述的一种硅基背栅全石墨烯场效应晶体管的制备方法，其特征在于，步骤(4)中所述剥离工艺使用丙酮或异丙醇有机溶液，所述剥离的时间为1-2h。
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