CN107068745A - A kind of field-effect transistor and preparation method thereof - Google Patents
A kind of field-effect transistor and preparation method thereof Download PDFInfo
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Abstract
范德瓦尔斯异质结以其原子层级界面,突出的机械柔性和极高的化学稳定性等特点将功能型异质结的研究带向了一个新的纪元。它的层间耦合特性使得打破了在选择制备材料时的束缚,并消除了传统材料在制备异质结构时的巨大限制。本发明意在提供一种工艺流程简单,对衬底和不同材料间晶格匹配要求低,不需要进行材料掺杂等工艺,而是利用范德瓦耳斯力将二种不同的二维晶体组成异质结结构,再利用该异质结结构作为导电沟道材料制备场效应晶体管及其制备方法。
Van der Waals heterojunction brings the research of functional heterojunction to a new era with its atomic-level interface, outstanding mechanical flexibility and high chemical stability. Its interlayer coupling characteristics break the shackles in the selection of materials and eliminate the huge limitations of traditional materials in the preparation of heterostructures. The present invention intends to provide a simple process flow, low requirements for lattice matching between the substrate and different materials, no material doping and other processes, but using van der Waals force to combine two different two-dimensional crystals A heterojunction structure is formed, and the heterojunction structure is used as a conductive channel material to prepare a field effect transistor and a preparation method thereof.
Description
技术领域technical field
本发明涉及二维纳米材料制备及其场效应晶体管的制备方法,主要是利用范德瓦耳斯力将二种不同的二维晶体组成异质结结构,利用该异质结结构作为导电沟道材料制备场效应晶体管,该器件适用于集成电路等领域。The invention relates to the preparation of two-dimensional nanomaterials and a method for preparing field effect transistors. The main method is to use van der Waals force to form two different two-dimensional crystals into a heterojunction structure, and use the heterojunction structure as a conductive channel The material is used to prepare field effect transistors, which are suitable for the fields of integrated circuits and the like.
背景技术Background technique
IC工业中随着器件尺寸越来越小,传统的硅基半导体已经逐步接近材料本身的物理极限。硅基微电子技术愈来愈受到短沟道效应,量子隧穿效应,功率损耗等因素的挑战,急需找到能够替代硅的下一代半导体材料。In the IC industry, as the size of devices becomes smaller and smaller, traditional silicon-based semiconductors are gradually approaching the physical limit of the material itself. Silicon-based microelectronics technology is increasingly challenged by factors such as short channel effects, quantum tunneling effects, and power loss. It is urgent to find next-generation semiconductor materials that can replace silicon.
随着2004年石墨烯的发现,开始掀起一阵研究二维材料的浪潮。当过渡金属二硫化物(TMDCs)由体材料变为二维结构时,电子的能带结构会由间接带隙变为直接带隙,这会使过渡金属二硫化物的光学和电学性能发生很大的变化,被誉为半导体界的“石墨烯”。二维材料以其超薄的材料厚度,载流子迁移率和带隙宽度可调控,超高的光吸收系数、良好的导电性、非常好的机械强度、延展性、柔性、不同材料之间不需要严格的晶格匹配等优点,在半导体高效率的太阳能电池、光探测器、电子及光电子器件应用方面展现出了极大的应用潜力。With the discovery of graphene in 2004, a wave of research on two-dimensional materials began. When transition metal dichalcogenides (TMDCs) change from bulk materials to two-dimensional structures, the electronic band structure changes from an indirect bandgap to a direct bandgap, which greatly changes the optical and electrical properties of transition metal dichalcogenides. Big changes, known as the "graphene" of the semiconductor industry. Two-dimensional materials are characterized by their ultra-thin material thickness, adjustable carrier mobility and band gap width, ultra-high light absorption coefficient, good electrical conductivity, very good mechanical strength, ductility, flexibility, and compatibility between different materials. It does not require strict lattice matching and other advantages, and has shown great application potential in the application of semiconductor high-efficiency solar cells, photodetectors, electronics and optoelectronic devices.
这其中,像过渡金属二硫化物中的二硫化钼、二硫化钨和二硫化锡等具有较宽带隙有利于克服器件的短沟道效应,制备出更小尺寸的器件;材料具有层状结构,层与层之间仅靠微弱的范德瓦耳斯力结合在一起,容易通过机械剥离法制备成二维材料。Among them, molybdenum disulfide, tungsten disulfide, and tin disulfide in transition metal dichalcogenides have a wide bandgap, which is beneficial to overcome the short channel effect of the device and prepare smaller-sized devices; the material has a layered structure , the layers are only bonded together by weak van der Waals force, and it is easy to prepare two-dimensional materials by mechanical exfoliation.
更为重要的是,这些二维晶体可以用于制备新型的异质结构,并且不同材料之间可以靠范德瓦尔斯力结合在一起,不需要严格的晶格匹配,并从根本上给材料科学带来革命性的进展。More importantly, these two-dimensional crystals can be used to prepare new heterostructures, and different materials can be combined by van der Waals forces without strict lattice matching, and fundamentally give materials Science leads to revolutionary advances.
现阶段场效应晶体管制备工艺需要经过衬底材料热生长,掺杂等多道复杂工艺,而且对于衬底与生长材料之间的晶格匹配要求严格。本专利意在提供一种工艺流程简单,对衬底和不同材料间晶格匹配要求低,不需要进行材料掺杂等工艺,而是利用范德瓦耳斯力将二种不同的二维晶体组成异质结结构,再利用该异质结结构作为导电沟道材料制备场效应晶体管及其制备方法。At present, the fabrication process of field effect transistors needs to go through multiple complex processes such as substrate material thermal growth and doping, and has strict requirements on the lattice matching between the substrate and the growth material. This patent intends to provide a simple process flow, low requirements for lattice matching between the substrate and different materials, no need for material doping and other processes, but using van der Waals force to combine two different two-dimensional crystals A heterojunction structure is formed, and the heterojunction structure is used as a conductive channel material to prepare a field effect transistor and a preparation method thereof.
发明内容Contents of the invention
基于上述问题,本发明提供了一种场效应晶体管的制备方法:Based on the above problems, the invention provides a method for preparing a field effect transistor:
步骤一,二维晶体的制备:将PET贴膜剪成两个2×5cm的长方形状,将高纯度晶体(石墨或硫化物晶体)置于两片PET膜粘性面之间,使两片PET膜不断接触和分离达到使晶体变薄的目的。然后将PET膜粘性面与PDMS(聚二甲基硅氧烷)接触再将PET膜缓慢揭开,一部分晶体转移到PDMS上,实现单层或少层石墨烯或二维硫化物晶体样品的制备。Step 1, preparation of two-dimensional crystals: Cut the PET film into two rectangular shapes of 2×5 cm, place high-purity crystals (graphite or sulfide crystals) between the sticky surfaces of two PET films, and make the two PET films Continuous contact and separation achieve the purpose of thinning the crystal. Then put the PET film sticky side in contact with PDMS (polydimethylsiloxane) and then slowly peel off the PET film, and a part of the crystals are transferred to PDMS to realize the preparation of single-layer or few-layer graphene or two-dimensional sulfide crystal samples .
步骤二,二维石墨烯和硫化物的筛选、转移:取步骤一中带有晶体的PDMS,将其放到显微镜下观察,利用光学显微镜的对比度筛选出想要的二维晶体。然后转移二维硫化物晶体,将PDMS与硅衬底接触,再将PDMS缓慢揭开,这样二维硫化物晶体就转到了硅衬底上。Step 2, screening and transfer of two-dimensional graphene and sulfide: take the PDMS with crystals in step one, observe it under a microscope, and use the contrast of an optical microscope to screen out the desired two-dimensional crystals. Then transfer the two-dimensional sulfide crystal, contact the PDMS with the silicon substrate, and slowly uncover the PDMS, so that the two-dimensional sulfide crystal is transferred to the silicon substrate.
步骤三,借助于光学显微镜,将获得的少层石墨烯覆盖在少层二维硫化物晶体上,利用范德瓦耳斯力将少层石墨烯和少层二维硫化物晶体结合在一起组成异质结结构。Step 3, with the help of an optical microscope, cover the obtained few-layer graphene on the few-layer two-dimensional sulfide crystal, and use the van der Waals force to combine the few-layer graphene and the few-layer two-dimensional sulfide crystal to form a heterojunction structure.
步骤四,场效应晶体管的制备:取步骤二中找到薄层的硅衬底,用丙酮溶液浸泡,然后再快速旋涂一层PMMA光刻胶,将涂好光刻胶的硅片放入热板上烘烤。将硅衬底放上掩膜版,用电子束曝光机进行电极的曝光。用质量比为1:3 的甲基异丁酮和异丙醇混合液作为显影液显影,并用IPA定影后用干燥氮气吹干。电子束蒸发在衬底和二种不同的二维晶体组成异质结结构上沉积金属薄膜电极层。Step 4, preparation of field effect transistors: Take the thin silicon substrate found in step 2, soak it with acetone solution, and then quickly spin coat a layer of PMMA photoresist, and put the silicon wafer coated with photoresist on the hot plate bake. Put the silicon substrate on the mask, and use electron beam exposure machine to expose the electrodes. Use a mixed solution of methyl isobutyl ketone and isopropanol at a mass ratio of 1:3 as a developing solution, fix with IPA and blow dry with dry nitrogen. Electron beam evaporation deposits metal thin-film electrode layers on the substrate and heterojunction structures of two different two-dimensional crystal compositions.
所述步骤一中,1)使用的原材料为高纯度的石墨或硫化物体材料;2)其中PDMS为将184有机硅弹性体套件中基底与愈合剂按照10:1的比例混合而成,使用前先用透明胶带撕去上面几层保证其表面洁净;3)其中PET 贴膜为生活中使用的PET材质手机膜,其粘性较弱容易克服高纯度的石墨或硫化物体晶体间微弱的范德瓦尔斯力;4)PET膜接触和分离的次数由以下决定,直到肉眼观察晶体厚度变薄并且均匀铺满PET膜表面,增大剥离出单层或少层的概率。所述步骤二中,所使用的光学显微镜为配备xy方向移动平台的型号。所述步骤三中,主要依靠高倍光学显微镜和PDMS的透光特性,实现石墨烯与二维硫化物异质结的精确组装;所述步骤四中,旋涂光刻胶速度为5000转每分钟,厚度为200纳米;烘烤温度为180摄氏度,时间1分钟;显影液显影时间为40秒,定影时间为30秒;电子束蒸发沉积的金属电极为钛和金。In said step one, 1) the raw material used is high-purity graphite or vulcanized object material; 2) wherein PDMS is the The base and healing agent in the 184 silicone elastomer kit are mixed at a ratio of 10:1. Before use, tear off the upper layers with scotch tape to ensure that the surface is clean; 3) The PET film is the PET material used in daily life for mobile phones film, whose viscosity is weak and easy to overcome the weak van der Waals force between the crystals of high-purity graphite or sulfide objects; 4) The number of contact and separation of the PET film is determined by the following until the crystal thickness is thinned and evenly covered with PET The surface of the film increases the probability of peeling off a single layer or a few layers. In the second step, the optical microscope used is a model equipped with a moving platform in the xy direction. In the third step, the precise assembly of graphene and two-dimensional sulfide heterojunction is realized mainly by relying on the high-power optical microscope and the light transmission characteristics of PDMS; in the fourth step, the speed of spin-coating photoresist is 5000 rpm , the thickness is 200 nanometers; the baking temperature is 180 degrees Celsius, and the time is 1 minute; the developing time of the developer is 40 seconds, and the fixing time is 30 seconds; the metal electrodes deposited by electron beam evaporation are titanium and gold.
本发明的有益效果:Beneficial effects of the present invention:
本发明先是在PDMS衬底上利用机械剥离法制备的二维石墨烯和硫化物晶体,组成二维异质结后,将其转移到硅衬底上,再利用其制备场效应晶体管。二维晶体及其异质节的制备操作简单、快速、成本低,同时不需要经过掺杂工艺,保留了材料自身固有性质。利用二维石墨烯和硫化物纳米级别的厚度特性,可以有效减小器件尺寸。In the invention, two-dimensional graphene and sulfide crystals prepared by a mechanical exfoliation method are firstly used on a PDMS substrate to form a two-dimensional heterojunction, then transferred to a silicon substrate, and then used to prepare a field effect transistor. The preparation of two-dimensional crystals and their heterojunctions is simple, fast, and low-cost. At the same time, it does not require a doping process and retains the inherent properties of the material itself. Utilizing the nanoscale thickness characteristics of two-dimensional graphene and sulfide, the device size can be effectively reduced.
本发明经过大量实验验证,总结出一种行之有效的制备方法,相比于现有晶体管的制备方法,不仅工艺简单,而且对衬底的要求更低,同时材料本身超薄的特性,可以构建垂直结构的器件,减小器件尺寸。After a large number of experimental verifications, the present invention concludes an effective preparation method. Compared with the existing transistor preparation method, not only the process is simple, but also the requirements for the substrate are lower. At the same time, the ultra-thin characteristics of the material itself can Build vertically structured devices and reduce device size.
附图说明Description of drawings
图1:二维硫化物制备和转移示意图(a)制备过程(b)转移过程(二维晶体异质结制备示意图(a)二维晶体制备过程(b)二维晶体异质结组装过程);Figure 1: Schematic diagram of two-dimensional sulfide preparation and transfer (a) preparation process (b) transfer process (schematic diagram of two-dimensional crystal heterojunction preparation (a) two-dimensional crystal preparation process (b) two-dimensional crystal heterojunction assembly process) ;
图2:二硫化锡表征图(a)原子力显微镜表征图(b)晶体管光镜图;Figure 2: Characterization diagram of tin disulfide (a) Characterization diagram of atomic force microscope (b) Optical microscope diagram of transistor;
图3:二维硫化物晶体管光镜图(a)氮化硼为绝缘层的二硒化钼晶体管Figure 3: Optical mirror image of two-dimensional sulfide transistor (a) Molybdenum diselenide transistor with boron nitride as the insulating layer
(b)二硒化钼晶体管(c)三硫化二砷晶体管;(b) molybdenum diselenide transistor (c) arsenic trisulfide transistor;
图4:场效应晶体管结构示意图。Figure 4: Schematic diagram of the field effect transistor structure.
具体实施方式detailed description
以下实例进一步说明本发明,但并不作为对本发明的限定。The following examples further illustrate the present invention, but are not intended to limit the present invention.
实施实例一Implementation example one
步骤一,首先制备二维石墨烯和二硫化锡晶体:其步骤如图1(a)所示,将 PET贴膜剪成两个2×5cm的长方形状,将高纯度石墨或二硫化锡晶体置于两片 PET膜粘性面之间,使两片PET膜不断接触和分离,直到肉眼观察晶体厚度变薄并且均匀铺满PET膜表面;在使用前先用透明胶带撕去PDMS上面几层保证其表面洁净;然后将PET膜粘性面与PDMS接触再将PET膜缓慢揭开,一部分晶体转移到PDMS上,实现二维石墨烯和二硫化锡晶体样品的制备。Step 1, first prepare two-dimensional graphene and tin disulfide crystals: as shown in Figure 1(a), the PET film is cut into two rectangular shapes of 2×5 cm, and high-purity graphite or tin disulfide crystals are placed Between the sticky surfaces of two PET films, keep the two PET films in constant contact and separation until the thickness of the crystal becomes thinner and evenly covers the surface of the PET film; before use, tear off the top layers of PDMS with transparent tape to ensure its The surface is clean; then the sticky side of the PET film is contacted with PDMS, and then the PET film is slowly peeled off, and a part of the crystals are transferred to the PDMS to realize the preparation of two-dimensional graphene and tin disulfide crystal samples.
步骤二,二维石墨烯和二硫化锡晶体的筛选、转移:取步骤一中带有晶体的PDMS,将其放到500倍的显微镜下观察,利用光学显微镜的对比度筛选出想要的二维晶体;然后转移其中的二硫化锡样品,其步骤如图1(b)所示,将PDMS 与硅衬底接触,再将PDMS缓慢揭开,这样二维二硫化锡晶体就转到了硅衬底上;Step 2, screening and transfer of two-dimensional graphene and tin disulfide crystals: take the PDMS with crystals in step one, put it under a 500-fold microscope for observation, and use the contrast of the optical microscope to screen out the desired two-dimensional crystal; then transfer the tin disulfide sample in it, the steps are shown in Figure 1(b), the PDMS is in contact with the silicon substrate, and then the PDMS is slowly uncovered, so that the two-dimensional tin disulfide crystal is transferred to the silicon substrate superior;
步骤三,利用高倍显微镜和位移台,将带有石墨烯的PDMS缓慢靠近带有二维二硫化锡的硅衬底,利用高倍显微镜和PDMS的透光特性精确的将获得的特定位置的少层石墨烯覆盖在少层二维二硫化锡晶体上,利用范德瓦耳斯力将少层石墨烯和少层二维硫化物晶体结合在一起组成异质结结构。Step 3, using a high-power microscope and a shift stage, slowly bring the PDMS with graphene close to the silicon substrate with two-dimensional tin disulfide, and use the high-power microscope and the light transmission characteristics of PDMS to accurately obtain the few layers at a specific position Graphene is covered on the few-layer two-dimensional tin disulfide crystal, and the few-layer graphene and the few-layer two-dimensional sulfide crystal are combined to form a heterojunction structure by using van der Waals force.
步骤四,基于二维石墨烯和二硫化锡异质节晶体管的制备:其结构示意图如图4所示,制备出的基于二维石墨烯和二硫化锡异质节晶体管在光镜下图像如图2(b)所示;用丙酮溶液浸泡带有薄层材料的硅片;快速旋涂一层PMMA 光刻胶,速度为5000转每分钟,厚度为200纳米;将涂好光刻胶的硅片放入热板上烘烤,烘烤温度为180摄氏度,时间1分钟;将硅片放上掩膜版,用电子束曝光机进行电极的曝光;用质量比为1:3的甲基异丁酮和异丙醇混合液作为显影液显影,并用IPA定影后用干燥氮气吹干,显影液显影时间为40秒,定影时间为30秒;电子束蒸发在衬底和基于二维石墨烯和二硫化锡异质节上沉积金属薄膜电极层,电子束蒸发沉积的金属电极为5纳米厚的钛和60纳米厚的金。Step 4, preparation of a heterojunction transistor based on two-dimensional graphene and tin disulfide: the schematic diagram of its structure is shown in Figure 4, and the image of the prepared two-dimensional graphene and tin disulfide heterojunction transistor under a light microscope is as follows Shown in Fig. 2 (b); Soak the silicon wafer with thin layer material with acetone solution; Spin coat one deck PMMA photoresist quickly, the speed is 5000 revolutions per minute, and thickness is 200 nanometers; The silicon wafer that will be coated with photoresist Put it on a hot plate for baking, the baking temperature is 180 degrees Celsius, and the time is 1 minute; put the silicon wafer on the mask, and use an electron beam exposure machine to expose the electrodes; use methyl isobutylene with a mass ratio of 1:3 A mixed solution of ketone and isopropanol was developed as a developer, and after fixing with IPA, it was blown dry with dry nitrogen. The developing time of the developer was 40 seconds, and the fixing time was 30 seconds; A metal thin film electrode layer is deposited on the tin sulfide heterojunction, and the metal electrodes deposited by electron beam evaporation are titanium with a thickness of 5 nanometers and gold with a thickness of 60 nanometers.
实施实例二Implementation example two
步骤一,首先制备二维石墨烯和二维二硫化钼晶体,其步骤如图1(a)所示,将PET贴膜剪成两个2×5cm的长方形状,将高纯度石墨或二硫化钼晶体置于两片PET膜粘性面之间,使两片PET膜不断接触和分离,直到肉眼观察晶体厚度变薄并且均匀铺满PET膜表面;在使用前先用透明胶带撕去PDMS上面几层保证其表面洁净;然后将PET膜粘性面与PDMS接触再将PET膜缓慢揭开,一部分晶体转移到PDMS上,实现二维石墨烯和二硫化钼晶体样品的制备。Step 1, first prepare two-dimensional graphene and two-dimensional molybdenum disulfide crystals, as shown in Figure 1(a), cut the PET film into two rectangular shapes of 2 × 5 cm, and place high-purity graphite or molybdenum disulfide The crystal is placed between the sticky surfaces of two PET films, and the two PET films are kept in contact and separated until the thickness of the crystal becomes thinner and evenly covers the surface of the PET film according to the naked eye; before use, tear off the top layers of PDMS with scotch tape Make sure the surface is clean; then contact the sticky side of the PET film with PDMS and then slowly peel off the PET film, and a part of the crystals are transferred to the PDMS to realize the preparation of two-dimensional graphene and molybdenum disulfide crystal samples.
步骤二,二维二硫化钼的筛选、转移:取步骤一中带有晶体的PDMS,将其放到500倍的显微镜下观察,利用光学显微镜的对比度筛选出想要的二维晶体,筛选的样品大概4层左右;然后转移样品,其步骤如图1(b)所示,事先将一层厚的hBN(六角氮化硼)转移到硅衬底上作为绝缘层,将PDMS与覆盖hBN的硅衬底接触,再将PDMS缓慢揭开,这样二维晶体就转到了硅衬底上。Step 2. Screening and transfer of two-dimensional molybdenum disulfide: take the PDMS with crystals in step one, put it under a microscope with a power of 500 times, and use the contrast of the optical microscope to screen out the desired two-dimensional crystals. The sample has about 4 layers; then the sample is transferred. The steps are shown in Figure 1(b). A thick layer of hBN (hexagonal boron nitride) is transferred to the silicon substrate as an insulating layer in advance, and PDMS and hBN are covered. The silicon substrate is in contact, and then the PDMS is slowly uncovered, so that the two-dimensional crystal is transferred to the silicon substrate.
步骤三,借助于光学显微镜,将获得的少层石墨烯覆盖在少层二维二硫化钼晶体上,利用范德瓦耳斯力将少层石墨烯和少层二维步骤三,借助于光学显微镜,将获得的少层石墨烯覆盖在少层二维二硫化钼晶体上,利用范德瓦耳斯力将少层石墨烯和少层二维二硫化钼晶体结合在一起组成异质结结构。晶体结合在一起组成异质结结构。Step 3, with the help of an optical microscope, cover the obtained few-layer graphene on the few-layer two-dimensional molybdenum disulfide crystal, and use the van der Waals force to combine the few-layer graphene and the few-layer two-dimensional Microscope, covering the obtained few-layer graphene on the few-layer two-dimensional molybdenum disulfide crystal, and using the van der Waals force to combine the few-layer graphene and the few-layer two-dimensional molybdenum disulfide crystal to form a heterojunction structure . The crystals bond together to form a heterojunction structure.
步骤四,基于二维石墨烯和二硫化钼异质节晶体管的制备:其结构示意图如图4所示,制备出的基于二维石墨烯和二硫化钼异质结在光镜下图像如图3(a) 所示;用丙酮溶液浸泡带有薄层材料的硅片;快速旋涂一层PMMA光刻胶,速度为5000转每分钟,厚度为200纳米;将涂好光刻胶的硅片放入热板上烘烤,烘烤温度为180摄氏度,时间1分钟;将硅片放上掩膜版,用电子束曝光机进行电极的曝光;用质量比为1:3的甲基异丁酮和异丙醇混合液作为显影液显影,并用IPA定影后用干燥氮气吹干,显影液显影时间为40秒,定影时间为30秒;电子束蒸发在衬底和基于二维石墨烯和步骤三,借助于光学显微镜,将获得的少层石墨烯覆盖在少层二维二硫化钼晶体上,利用范德瓦耳斯力将少层石墨烯和少层二维二硫化钼晶体结合在一起组成异质结结构。异质结上沉积金属薄膜电极层,电子束蒸发沉积的金属电极为10纳米厚的钛和60纳米厚的金。Step 4, preparation of heterojunction transistors based on two-dimensional graphene and molybdenum disulfide: the schematic diagram of its structure is shown in Figure 4, and the image of the prepared two-dimensional graphene and molybdenum disulfide heterojunction under the light microscope is shown in Figure 4. As shown in 3(a); soak the silicon wafer with a thin layer of material in acetone solution; quickly spin coat a layer of PMMA photoresist at a speed of 5000 rpm and a thickness of 200 nanometers; place the silicon wafer coated with photoresist Bake on a hot plate, the baking temperature is 180 degrees Celsius, and the time is 1 minute; put the silicon wafer on the mask plate, and use an electron beam exposure machine to expose the electrodes; use methyl isobutyl ketone with a mass ratio of 1:3 Develop with isopropanol mixed solution as developer, and dry with dry nitrogen after fixing with IPA. The developing time of developing solution is 40 seconds, and the fixing time is 30 seconds; , with the help of an optical microscope, the obtained few-layer graphene was covered on the few-layer two-dimensional molybdenum disulfide crystal, and the few-layer graphene and the few-layer two-dimensional molybdenum disulfide crystal were combined by van der Waals force. heterojunction structure. A metal thin film electrode layer is deposited on the heterojunction, and the metal electrodes deposited by electron beam evaporation are titanium with a thickness of 10 nanometers and gold with a thickness of 60 nanometers.
实施实例三Implementation example three
步骤一,首先制备二维石墨烯和二硒化钼晶体,其步骤如图1(a)所示,将 PET贴膜剪成两个2×5cm的长方形状,将二高纯度石墨或二硒化钼晶体置于两片PET膜粘性面之间,使两片PET膜不断接触和分离,直到肉眼观察晶体厚度变薄并且均匀铺满PET膜表面;在使用前先用透明胶带撕去PDMS上面几层保证其表面洁净;然后将PET膜粘性面与PDMS接触再将PET膜缓慢揭开,一部分晶体转移到PDMS上,实现二维石墨烯和二硒化钼晶体样品的制备。Step 1, first prepare two-dimensional graphene and molybdenum diselenide crystals, the steps are shown in Figure 1(a), cut the PET film into two rectangular shapes of 2 × 5cm, and two high-purity graphite or molybdenum diselenide Molybdenum crystals are placed between the sticky surfaces of two PET films, so that the two PET films are in constant contact and separation until the thickness of the crystals becomes thinner and evenly covers the surface of the PET film; layer to ensure its surface is clean; then the sticky side of the PET film is in contact with PDMS and then the PET film is slowly peeled off, and a part of the crystals are transferred to the PDMS to realize the preparation of two-dimensional graphene and molybdenum diselenide crystal samples.
步骤二,二维二硒化钼晶体的筛选、转移:取步骤一中带有晶体的PDMS,将其放到500倍的显微镜下观察,利用光学显微镜的对比度筛选出想要的二维二硒化钼晶体,筛选的样品大概3层左右;然后转移样品,其步骤如图1(b)所示,将PDMS与硅衬底接触,再将PDMS缓慢揭开,这样二维晶体就转到了硅衬底上。Step 2, screening and transfer of two-dimensional molybdenum diselenide crystals: Take the PDMS with crystals in step one, put it under a microscope at 500 times to observe, and use the contrast of the optical microscope to screen out the desired two-dimensional molybdenum diselenide Molybdenum oxide crystals, the screened sample has about 3 layers; then transfer the sample, the steps are shown in Figure 1(b), the PDMS is in contact with the silicon substrate, and then the PDMS is slowly uncovered, so that the two-dimensional crystal is transferred to the silicon substrate. on the substrate.
步骤三,借助于光学显微镜,将获得的少层石墨烯覆盖在少层二维二硒化钼晶体上,利用范德瓦耳斯力将少层石墨烯和少层二维二硒化钼晶体结合在一起组成异质结结构。Step 3, with the help of an optical microscope, cover the obtained few-layer graphene on the few-layer two-dimensional molybdenum diselenide crystal, and use the van der Waals force to combine the few-layer graphene and the few-layer two-dimensional molybdenum diselenide crystal combined to form a heterojunction structure.
步骤四,基于二维石墨烯和二硒化钼异质节晶体管的制备:其结构示意图如图4所示,制备出的基于二维石墨烯和二硫化钼异质结在光镜下图像如图3(b) 所示;用丙酮溶液浸泡带有薄层材料的硅片;快速旋涂一层PMMA光刻胶,速度为5000转每分钟,厚度为200纳米;将涂好光刻胶的硅片放入热板上烘烤,烘烤温度为180摄氏度,时间1分钟;将硅片放上掩膜版,用电子束曝光机进行电极的曝光;用质量比为1:3的甲基异丁酮和异丙醇混合液作为显影液显影,并用IPA定影后用干燥氮气吹干,显影液显影时间为40秒,定影时间为30秒;电子束蒸发在衬底和二维硫化物上沉积金属薄膜电极层,电子束蒸发沉积的金属电极为10纳米厚的钛和60纳米厚的金。Step 4, preparation of a heterojunction transistor based on two-dimensional graphene and molybdenum diselenide: the schematic diagram of its structure is shown in Figure 4, and the image of the prepared two-dimensional graphene and molybdenum disulphide heterojunction under the light microscope is as Shown in Fig. 3 (b); Soak the silicon wafer with thin layer material with acetone solution; Spin coat one deck PMMA photoresist quickly, the speed is 5000 revolutions per minute, and the thickness is 200 nanometers; The silicon wafer that will be coated with photoresist Put it on a hot plate for baking, the baking temperature is 180 degrees Celsius, and the time is 1 minute; put the silicon wafer on the mask, and use an electron beam exposure machine to expose the electrodes; use methyl isobutylene with a mass ratio of 1:3 A mixture of ketone and isopropanol was developed as a developer, fixed with IPA and blown dry with dry nitrogen. The developing time of the developer was 40 seconds, and the fixing time was 30 seconds; electron beam evaporation deposited metal on the substrate and two-dimensional sulfide Thin-film electrode layer, metal electrode deposited by electron beam evaporation is 10 nanometers thick titanium and 60 nanometers thick gold.
实施实例四Implementation example four
步骤一,首先制备二维石墨烯和二维三硫化二砷晶体,其步骤如图1(a)所示,将PET贴膜剪成两个2×5cm的长方形状,将二高纯度石墨或三硫化二砷晶体置于两片PET膜粘性面之间,使两片PET膜不断接触和分离,直到肉眼观察晶体厚度变薄并且均匀铺满PET膜表面;在使用前先用透明胶带撕去PDMS上面几层保证其表面洁净;然后将PET膜粘性面与PDMS接触再将PET膜缓慢揭开,一部分晶体转移到PDMS上,实现二维石墨烯和三硫化二砷晶体样品的制备。Step 1, first prepare two-dimensional graphene and two-dimensional arsenic trisulfide crystals, as shown in Figure 1(a), cut the PET film into two rectangular shapes of 2 × 5 cm, and put two high-purity graphite or three The arsenic sulfide crystal is placed between the sticky surfaces of two PET films, and the two PET films are kept in contact and separated until the thickness of the crystal becomes thinner and evenly covers the surface of the PET film; before use, tear off the PDMS with scotch tape The upper layers ensure that the surface is clean; then the sticky side of the PET film is in contact with PDMS, and then the PET film is slowly peeled off, and a part of the crystals are transferred to the PDMS to realize the preparation of two-dimensional graphene and arsenic trisulfide crystal samples.
步骤二,二维三硫化二砷晶体的筛选、转移:取步骤一中带有晶体的PDMS,将其放到500倍的显微镜下观察,利用光学显微镜的对比度筛选出想要的二维晶体,筛选的样品薄层区域大概4层左右;然后转移样品,其步骤如图1(b)所示,将PDMS与硅衬底接触,再将PDMS缓慢揭开,这样二维三硫化二砷晶体就转到了硅衬底上。Step 2. Screening and transfer of two-dimensional arsenic trisulfide crystals: take the PDMS with crystals in step one, put it under a microscope with a power of 500 times, and use the contrast of the optical microscope to screen out the desired two-dimensional crystals. The thin layer area of the sample screened is about 4 layers; then the sample is transferred, as shown in Figure 1(b), the PDMS is in contact with the silicon substrate, and then the PDMS is slowly uncovered, so that the two-dimensional arsenic trisulfide crystal is onto a silicon substrate.
步骤三,三硫化二砷晶体管的制备:其结构示意图如图4所示,制备出的三硫化二砷晶体管在光镜下图像如图3(c)所示;用丙酮溶液浸泡带有薄层材料的硅片;快速旋涂一层PMMA光刻胶,速度为5000转每分钟,厚度为200纳米;将涂好光刻胶的硅片放入热板上烘烤,烘烤温度为180摄氏度,时间1分钟;将硅片放上掩膜版,用电子束曝光机进行电极的曝光;用质量比为1:3的甲基异丁酮和异丙醇混合液作为显影液显影,并用IPA定影后用干燥氮气吹干,显影液显影时间为40秒,定影时间为30秒;电子束蒸发在衬底和二维三硫化二砷上沉积金属薄膜电极层,电子束蒸发沉积的金属电极为5纳米厚的钛和60 纳米厚的金。Step 3, the preparation of the arsenic trisulfide transistor: the schematic diagram of its structure is shown in Figure 4, and the image of the prepared arsenic trisulfide transistor under the light microscope is shown in Figure 3(c); The silicon wafer of the material; quickly spin-coat a layer of PMMA photoresist at a speed of 5000 rpm and a thickness of 200 nanometers; put the silicon wafer coated with photoresist on a hot plate for baking at 180 degrees Celsius for a time 1 minute; put the silicon wafer on the mask plate, and use an electron beam exposure machine to expose the electrodes; use a mixture of methyl isobutyl ketone and isopropanol with a mass ratio of 1:3 as a developing solution, and fix it with IPA Blow dry with dry nitrogen, the developing time of the developer is 40 seconds, and the fixing time is 30 seconds; electron beam evaporation deposits a metal thin film electrode layer on the substrate and two-dimensional arsenic trisulfide, and the metal electrode deposited by electron beam evaporation is 5 nanometers thick titanium and 60nm thick gold.
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CN116206981A (en) * | 2023-05-04 | 2023-06-02 | 北京大学 | A method for large-scale preparation of comprehensive two-dimensional short-channel field-effect transistors |
CN116206981B (en) * | 2023-05-04 | 2023-06-30 | 北京大学 | A method for large-scale preparation of comprehensive two-dimensional short-channel field-effect transistors |
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