CN110963460B - Two-dimensional material cleavage method - Google Patents
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Abstract
一种二维材料解理方法,包括:在母体层状晶体的表面形成绝缘薄膜镀层;在绝缘薄膜镀层表面粘贴热释放胶带;揭起热释放胶带,使热释放胶带粘附绝缘薄膜镀层,且绝缘薄膜镀层表面具有由部分母体层状晶体构成的中间层状晶体;在热释放胶带表面覆盖粘附印章,且粘附印章覆盖绝缘薄膜镀层和中间层状晶体;热处理热释放胶带,使热释放胶带与粘附印章、以及热释放胶带与绝缘薄膜镀层分离;之后,将粘附印章、中间层状晶体和绝缘薄膜镀层按压在衬底上,且绝缘薄膜镀层与衬底接触;之后,揭起粘附印章,粘附印章表面带走部分中间层状晶体,使绝缘薄膜镀层表面形成二维材料。所述方法能够制备大面积高质量的二维材料,拓宽二维材料库。
A two-dimensional material cleavage method, comprising: forming an insulating film coating on the surface of a parent layered crystal; pasting a heat release tape on the surface of the insulating film coating; lifting the heat release tape to make the heat release tape adhere to the insulating film coating, and The surface of the insulating film coating has intermediate layered crystals composed of part of the parent layered crystals; the adhesive seal is covered on the surface of the heat release tape, and the adhesive seal covers the insulating film coating and the intermediate layered crystals; heat treatment of the heat release tape to release the heat The tape is separated from the adhesive stamp, and the heat release tape is separated from the insulating film coating; after that, the adhesive stamp, the interlayer crystal and the insulating film coating are pressed on the substrate, and the insulating film coating is in contact with the substrate; after that, lift up The seal is adhered, and the surface of the adhering seal takes away part of the intermediate layered crystals, so that a two-dimensional material is formed on the surface of the insulating film coating. The method can prepare large-area and high-quality two-dimensional materials and expand the library of two-dimensional materials.
Description
技术领域technical field
本发明涉及纳米材料制备技术领域,尤其涉及一种二维材料解理方法。The invention relates to the technical field of nanomaterial preparation, in particular to a two-dimensional material cleavage method.
背景技术Background technique
二维材料指的是由单原子层或几个原子层构成的晶体材料。绝大多数的二维材料可从其对应的三维母体材料获得。比如,单个原子层的碳,即石墨烯,可以由层状的石墨得来。在石墨中,原子层间的碳是由范德瓦尔斯力连接的,这种力相较于共价键或离子键要弱,因此可以较为容易地将石墨从层间分开,得到单层的石墨烯,如同将一页纸从一本书中取出。2004年,Geim课题组使用透明胶带对石墨进行了机械解理,首次得到了单层石墨烯。而这种机械解理的方式适用于很多如同石墨的层状体材料,使得二维材料领域有了前所未有的发展。Two-dimensional materials refer to crystalline materials consisting of a single atomic layer or several atomic layers. The vast majority of 2D materials can be obtained from their corresponding 3D parent materials. For example, a single atomic layer of carbon, known as graphene, can be derived from layered graphite. In graphite, the carbon between atomic layers is connected by van der Waals forces, which are weaker than covalent or ionic bonds, so graphite can be easily separated from the layers to obtain a monolayer of Graphene is like taking a page out of a book. In 2004, Geim's group used scotch tape to mechanically cleavage graphite and obtained single-layer graphene for the first time. This mechanical cleavage method is suitable for many layered materials like graphite, which has made the field of two-dimensional materials unprecedented development.
二维材料有着许多与三维母体材料不同的物理性质,并且,二维材料对外界调控更加敏感,更易被调控,使其在诸如自旋电子学、光电子学等应用方面具有其三维母体材料所不具备的优越性质。另外,二维材料堆叠后形成的新结构,即范德瓦尔斯异质结,有着更不为人知的优异性能,大大拓宽了已有的材料体系。Two-dimensional materials have many different physical properties from three-dimensional parent materials, and two-dimensional materials are more sensitive to external regulation and easier to be regulated, making them unique in applications such as spintronics and optoelectronics. possessed superior properties. In addition, the new structure formed by stacking two-dimensional materials, namely van der Waals heterojunction, has even more unknown excellent properties, which greatly broadens the existing material system.
然而,目前亟需一种能够适用于较多材料的制备大面积高质量的二维材料的方法。However, there is an urgent need for a method for preparing large-area and high-quality two-dimensional materials that can be applied to more materials.
发明内容SUMMARY OF THE INVENTION
本发明解决的问题是提供一种二维材料解理方法,以实现从较多种母体层状材料中分离出大面积且高质量的二维材料,拓宽二维材料库。The problem solved by the present invention is to provide a two-dimensional material cleavage method, so as to realize the separation of large-area and high-quality two-dimensional materials from more kinds of parent layered materials, and to expand the two-dimensional material library.
为解决上述问题,本发明提供一种二维材料解理方法,包括:提供母体层状晶体、热释放胶带、粘附印章和衬底;在所述母体层状晶体的表面形成绝缘薄膜镀层;在所述绝缘薄膜镀层表面粘贴热释放胶带;揭起所述热释放胶带,使热释放胶带粘附所述绝缘薄膜镀层,且所述绝缘薄膜镀层表面具有由部分母体层状晶体构成的中间层状晶体;在所述热释放胶带表面覆盖粘附印章,且所述粘附印章覆盖所述绝缘薄膜镀层和所述中间层状晶体;热处理所述热释放胶带,使所述热释放胶带与所述粘附印章、以及所述热释放胶带与所述绝缘薄膜镀层分离;热处理所述热释放胶带后,将所述粘附印章、中间层状晶体和绝缘薄膜镀层按压在所述衬底上,且所述绝缘薄膜镀层与所述衬底接触;将所述粘附印章、中间层状晶体和绝缘薄膜镀层按压在所述衬底上后,揭起所述粘附印章,所述粘附印章表面带走部分中间层状晶体,使所述绝缘薄膜镀层表面形成二维材料。In order to solve the above problems, the present invention provides a two-dimensional material cleavage method, comprising: providing a parent layered crystal, a heat release tape, an adhesive stamp and a substrate; forming an insulating film coating on the surface of the parent layered crystal; Paste heat release tape on the surface of the insulating film coating; lift up the heat release tape to make the heat release tape adhere to the insulating film coating, and the surface of the insulating film coating has an intermediate layer composed of part of the parent layered crystals The surface of the heat release tape is covered with an adhesive seal, and the adhesive seal covers the insulating film coating and the intermediate layered crystal; heat treatment of the heat release tape to make the heat release tape and the The adhesive seal, and the heat release tape are separated from the insulating film coating; after heat-treating the heat release tape, the adhesive seal, the intermediate layered crystal and the insulating film coating are pressed on the substrate, And the insulating film coating is in contact with the substrate; after pressing the adhesive seal, the intermediate layered crystal and the insulating film coating on the substrate, lift up the adhesive seal, and the adhesive seal Part of the intermediate layered crystal is taken away from the surface, so that a two-dimensional material is formed on the surface of the insulating film coating.
可选的,所述母体层状晶体具有相对的第一面和第二面;所述二维材料解理方法还包括:提供胶带;在所述母体层状晶体的表面形成绝缘薄膜镀层之前,将所述母体层状晶体粘贴在所述胶带表面,第一面与所述胶带接触;将所述母体层状晶体粘贴在所述胶带表面后,在所述母体层状晶体的第二面形成所述绝缘薄膜镀层。Optionally, the parent layered crystal has opposite first faces and second faces; the two-dimensional material cleavage method further includes: providing an adhesive tape; before forming an insulating film coating on the surface of the parent layered crystal, pasting the parent layered crystals on the surface of the tape, with the first surface in contact with the tape; after pasting the parent layered crystals on the surface of the tape, forming on the second surface of the parent layered crystals The insulating film is coated.
可选的,所述超真空胶带的材料包括聚酰亚胺薄膜材料、丙烯酸黏合剂材料或有机硅黏合剂材料。Optionally, the material of the ultra-vacuum adhesive tape includes polyimide film material, acrylic adhesive material or silicone adhesive material.
可选的,将所述母体层状晶体粘贴在所述胶带表面的步骤在惰性气体环境中进行。Optionally, the step of pasting the precursor layered crystals on the surface of the tape is performed in an inert gas environment.
可选的,所述绝缘薄膜镀层的材料包括氧化铝、氧化硅、氧化镁或二氧化钛。Optionally, the material of the insulating thin film coating includes aluminum oxide, silicon oxide, magnesium oxide or titanium dioxide.
可选的,形成所述绝缘薄膜镀层的工艺包括蒸镀工艺、溅射工艺或电镀工艺。Optionally, the process of forming the insulating thin film coating includes an evaporation process, a sputtering process or an electroplating process.
可选的,所述绝缘薄膜镀层的材料为氧化铝;形成所述绝缘薄膜镀层的工艺为蒸镀工艺,参数包括:蒸镀环境的氧气分压为1E-4毫巴~2E-4毫巴,蒸镀源为铝。Optionally, the material of the insulating film coating is aluminum oxide; the process for forming the insulating film coating is an evaporation process, and the parameters include: the partial pressure of oxygen in the evaporation environment is 1E-4 mbar to 2E-4 mbar , the evaporation source is aluminum.
可选的,所述绝缘薄膜镀层的厚度为50纳米以上。Optionally, the thickness of the insulating film coating is more than 50 nanometers.
可选的,所述绝缘薄膜镀层的厚度为50纳米~200纳米。Optionally, the thickness of the insulating film coating is 50 nanometers to 200 nanometers.
可选的,在所述母体层状晶体的表面形成绝缘薄膜镀层的步骤在高真空环境中进行。Optionally, the step of forming an insulating thin film coating on the surface of the parent layered crystal is performed in a high vacuum environment.
可选的,在所述绝缘薄膜镀层表面粘贴热释放胶带的步骤在惰性气体环境中进行;揭起所述热释放胶带的步骤在惰性气体环境中进行;在所述热释放胶带表面覆盖粘附印章的步骤在惰性气体环境中进行;热处理所述热释放胶带的步骤在惰性气体环境中进行;将所述粘附印章、中间层状晶体和绝缘薄膜镀层按压在所述衬底上的步骤在惰性气体环境中进行;揭起所述粘附印章的步骤在惰性气体环境中进行。Optionally, the step of pasting the heat release tape on the surface of the insulating film coating is performed in an inert gas environment; the step of lifting the heat release tape is performed in an inert gas environment; the surface of the heat release tape is covered and adhered The step of stamping is carried out in an inert gas environment; the step of heat-treating the heat release tape is carried out in an inert gas environment; the step of pressing the adhering stamp, the intermediate layered crystal and the insulating film coating on the substrate is carried out in an inert gas environment; the step of lifting the adhesive seal was carried out in an inert gas environment.
可选的,所述粘附印章的材料包括聚合物。Optionally, the material for adhering the stamp includes a polymer.
可选的,所述聚合物包括聚二甲基硅氧烷。Optionally, the polymer includes polydimethylsiloxane.
可选的,热处理所述热释放胶带的温度为115摄氏度~125摄氏度。Optionally, the temperature for heat-treating the heat release tape is 115 degrees Celsius to 125 degrees Celsius.
可选的,将所述粘附印章、中间层状晶体和绝缘薄膜镀层按压在所述衬底上之前,还包括:对所述衬底的表面进行清洁处理。Optionally, before pressing the adhesive stamp, the intermediate layered crystal and the insulating film coating on the substrate, the method further includes: cleaning the surface of the substrate.
可选的,所述清洁处理包括等离子体处理。Optionally, the cleaning treatment includes plasma treatment.
可选的,所述等离子体处理采用氧等离子体。Optionally, the plasma treatment uses oxygen plasma.
可选的,所述二维材料包括单层的MoS2、单层的TaS2、单层的Fe3GeTe2、单层的VSe2、单层的FeSe、单层的CrI3、单层的Cr2Ge2Te6、单层的WSe2、单层的WS2、单层的WTe2或单层的黑磷。Optionally, the two-dimensional material includes monolayer MoS 2 , monolayer TaS 2 , monolayer Fe 3 GeTe 2 , monolayer VSe 2 , monolayer FeSe, monolayer CrI 3 , monolayer Cr2Ge2Te6 , monolayer WSe2 , monolayer WS2 , monolayer WTe2 , or monolayer black phosphorus.
可选的,所述二维材料的横向长度在100微米以上。Optionally, the lateral length of the two-dimensional material is more than 100 microns.
与现有技术相比,本发明的技术方案具有以下优点:Compared with the prior art, the technical solution of the present invention has the following advantages:
本发明技术方案提供的二维材料解理方法中,所述绝缘薄膜镀层形成在母体层状晶体表面,绝缘薄膜镀层与母体层状晶体材料之间具有很大的粘附性,且绝缘薄膜镀层可与母体层状晶体具有很大的接触面积。由于绝缘薄膜镀层与母体层状晶体材料之间具有很大的粘附性,因此绝缘薄膜镀层与中间层状晶体之间具有很大的粘附性。由于绝缘薄膜镀层与中间层状晶体之间具有很大的粘附性,因此揭起所述粘附印章后,所述绝缘薄膜镀层表面能形成质量较高的二维材料,具体表现在:二维材料的均匀性较高,二维材料的缺陷较少。由于绝缘薄膜镀层具有较大的面积,因此能在绝缘薄膜镀层表面形成大面积的二维材料。将绝缘薄膜镀层粘附在衬底表面,以实现二维材料固定在衬底上,因此二维材料的形成不受衬底材料的限制,使得二维材料的种类能够拓宽。由于没有利用液相方法,因此二维材料在制备过程中不会暴露于有机溶剂中,因此本方法适于对有机溶剂敏感的二维材料的制作,制备的二维材料的种类能够拓宽。In the two-dimensional material cleavage method provided by the technical solution of the present invention, the insulating thin film coating is formed on the surface of the parent layered crystal, the insulating thin film coating and the parent layered crystal material have great adhesion, and the insulating thin film coating Can have a large contact area with the parent layered crystal. Due to the great adhesion between the insulating film coating and the parent layered crystal material, the insulating film coating and the intermediate layered crystal have great adhesion. Due to the great adhesion between the insulating film coating and the intermediate layered crystal, after the adhesive seal is lifted, the surface of the insulating film coating can form a two-dimensional material with high quality, which is embodied in: two The homogeneity of 2D materials is higher, and the defects of 2D materials are less. Since the insulating film coating has a larger area, a large-area two-dimensional material can be formed on the surface of the insulating film coating. The insulating film coating is adhered to the surface of the substrate, so that the two-dimensional material is fixed on the substrate, so the formation of the two-dimensional material is not limited by the substrate material, so that the types of the two-dimensional material can be broadened. Since the liquid phase method is not used, the two-dimensional materials will not be exposed to organic solvents during the preparation process, so this method is suitable for the fabrication of two-dimensional materials sensitive to organic solvents, and the types of prepared two-dimensional materials can be broadened.
其次,绝缘薄膜镀层为绝缘材料,绝缘薄膜镀层不会影响对二维材料进行电输运性质的测量过程。绝缘薄膜镀层无需被刻蚀去除,因此不会对二维材料有刻蚀损伤的问题,使得二维材料的质量提高。Secondly, the insulating film coating is an insulating material, and the insulating film coating will not affect the measurement process of the electrical transport properties of the two-dimensional material. The insulating film coating does not need to be removed by etching, so there is no problem of etching damage to the two-dimensional material, so that the quality of the two-dimensional material is improved.
附图说明Description of drawings
图1是本发明一实施例中二维材料解理过程的流程图;1 is a flow chart of a two-dimensional material cleavage process in an embodiment of the present invention;
图2至图13是本发明一实施例中二维材料解理过程的结构示意图。2 to 13 are schematic structural diagrams of a two-dimensional material cleavage process in an embodiment of the present invention.
具体实施方式Detailed ways
正如背景技术所述,现有技术形成的二维材料的性能较差。As mentioned in the background art, the two-dimensional materials formed by the prior art have poor performance.
制备二维材料的方法包括机械解理法、液相解理法、化学气相沉积法和分子束外延法。Methods for preparing two-dimensional materials include mechanical cleavage, liquid cleavage, chemical vapor deposition and molecular beam epitaxy.
以制备二维材料为石墨烯为例进行说明,机械解理法是利用透明胶带将石墨按压到衬底材料表面上进行剥离,最终得到单层或少层的石墨。该方法主要受到胶带与二维材料之间的范德瓦尔斯力的限制、以及二维材料与衬底之间的范德瓦尔斯力的限制,因此制备出的二维材料的种类较少、面积小,且二维材料表面容易存在残胶,影响二维材料的质量。Taking the preparation of two-dimensional material as graphene as an example, the mechanical cleavage method is to press the graphite on the surface of the substrate material with a transparent tape to peel off, and finally obtain a single-layer or few-layer graphite. This method is mainly limited by the van der Waals force between the tape and the two-dimensional material, and the van der Waals force between the two-dimensional material and the substrate, so the prepared two-dimensional materials have fewer types, The area is small, and residual glue easily exists on the surface of the two-dimensional material, which affects the quality of the two-dimensional material.
另一种方法是,利用金与二维材料之间的强粘附性来解理二维材料,但是该方法中若金最后被保留的话,金的导电性不易于对二维材料进一步的电输运性质的测量,通常最后需要将金刻蚀去除,因此得到的二维材料表面容易受到污染和损伤。Another method is to use the strong adhesion between gold and the two-dimensional material to cleavage the two-dimensional material, but in this method, if the gold is retained at the end, the conductivity of gold is not easy for the further electrical conductivity of the two-dimensional material. The measurement of transport properties usually requires the removal of gold by etching, so the surface of the obtained 2D material is susceptible to contamination and damage.
液相解理法是利用超声震动将层状母体材料从层间分离开。液相解理法制备出的二维材料也具有面积小的缺点。且二维材料在制备过程中暴露于有机溶剂,因此该方法不适于对有机溶剂敏感的二维材料,制备的二维材料的种类受到限制。Liquid phase cleavage uses ultrasonic vibration to separate layered matrix materials from the interlayers. The two-dimensional materials prepared by the liquid phase cleavage method also have the disadvantage of small area. Moreover, the two-dimensional materials are exposed to organic solvents during the preparation process, so this method is not suitable for two-dimensional materials sensitive to organic solvents, and the types of prepared two-dimensional materials are limited.
化学气相沉积法能够合成大面积的二维材料。但是二维材料薄膜容易存在均匀性差的问题,从而导致二维材料的质量受到影响。Chemical vapor deposition enables the synthesis of large-area two-dimensional materials. However, the two-dimensional material thin film is prone to the problem of poor uniformity, which affects the quality of the two-dimensional material.
分子束外延法能够合成大面积的二维材料,但是由于该方法合成的材料往往需要与所用的衬底的晶格匹配,且其物理性质会受到衬底的影响,所述合成的二维材料的种类有限。Molecular beam epitaxy can synthesize large-area two-dimensional materials, but since the materials synthesized by this method often need to match the lattice of the substrate used, and its physical properties will be affected by the substrate, the synthesized two-dimensional materials types are limited.
目前,还没有一种能够适用于较多材料的制备大面积高质量的二维材料的方法。At present, there is no method for preparing large-area and high-quality two-dimensional materials that can be applied to more materials.
在此基础上,本发明提供一种二维材料解理方法,请参考图1,包括以下步骤:On this basis, the present invention provides a two-dimensional material cleavage method, please refer to FIG. 1, including the following steps:
S01:提供母体层状晶体、热释放胶带、粘附印章和衬底;S01: Provide parent layered crystals, thermal release tapes, adhesive stamps and substrates;
S02:在所述母体层状晶体的表面形成绝缘薄膜镀层;S02: forming an insulating thin film coating on the surface of the parent layered crystal;
S03:在所述绝缘薄膜镀层表面粘贴热释放胶带;S03: paste heat release tape on the surface of the insulating film coating;
S04:揭起所述热释放胶带,使热释放胶带粘附所述绝缘薄膜镀层,且所述绝缘薄膜镀层表面具有由部分母体层状晶体构成的中间层状晶体;S04: lift up the heat release tape, make the heat release tape adhere to the insulating film coating, and the surface of the insulating film coating has intermediate layered crystals composed of part of the parent layered crystals;
S05:在所述热释放胶带表面覆盖粘附印章,且所述粘附印章覆盖所述绝缘薄膜镀层和所述中间层状晶体;S05: Cover the surface of the heat release tape with an adhesive seal, and the adhesive seal covers the insulating film coating and the intermediate layered crystal;
S06:热处理所述热释放胶带,使所述热释放胶带与所述粘附印章、以及所述热释放胶带与所述绝缘薄膜镀层分离;S06: heat-treating the heat release tape to separate the heat release tape from the adhesive seal, and the heat release tape and the insulating film coating;
S07:热处理所述热释放胶带后,将所述粘附印章、中间层状晶体和绝缘薄膜镀层按压在所述衬底上,且所述绝缘薄膜镀层与所述衬底接触;S07: after heat-treating the heat release tape, press the adhesive seal, the intermediate layered crystal and the insulating film coating on the substrate, and the insulating film coating is in contact with the substrate;
S08:将所述粘附印章、中间层状晶体和绝缘薄膜镀层按压在所述衬底上后,揭起所述粘附印章,所述粘附印章表面带走部分中间层状晶体,使所述绝缘薄膜镀层表面形成二维材料。S08: After pressing the adhesive seal, the intermediate layered crystal and the insulating film coating on the substrate, lift up the adhesive seal, and the surface of the adhesive seal takes away part of the intermediate layered crystal, so that the A two-dimensional material is formed on the surface of the insulating film coating.
所述方法能实现从较多种母体层状材料中分离出大面积且高质量的二维材料,拓宽二维材料库。The method can realize the separation of large-area and high-quality two-dimensional materials from more kinds of parent layered materials, and broaden the library of two-dimensional materials.
为使本发明的上述目的、特征和优点能够更为明显易懂,下面结合附图对本发明的具体实施例做详细的说明。In order to make the above objects, features and advantages of the present invention more clearly understood, the specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
图2至图13是本发明一实施例中二维材料解理过程的结构示意图。2 to 13 are schematic structural diagrams of a two-dimensional material cleavage process in an embodiment of the present invention.
参考图2,提供母体层状晶体100。Referring to Figure 2, a parent layered
所述母体层状晶体100为三维结构材料。后续的二维材料从所述母体层状晶体100中剥离而得到。The parent layered
所述母体层状晶体100的材料包括MoS2、TaS2、Fe3GeTe2、VSe2、FeSe、CrI3、Cr2Ge2Te6、WSe2、WS2、WTe2或黑磷。The material of the parent layered
本实施例中,以所述母体层状晶体100的材料为Fe3GeTe2,后续形成的二维材料为单层Fe3GeTe2为示例进行说明。In this embodiment, the material of the parent layered
在其它实施例中,所述母体层状晶体的材料还可以为其它材料。In other embodiments, the material of the parent layered crystal may also be other materials.
所述母体层状晶体100具有相对的第一面101和第二面102。The parent layered
所述第一面101和第二面102平行于母体层状晶体100中各层原子分布的平面。The
参考图3,提供胶带110。Referring to Figure 3,
所述胶带110的材料包括聚酰亚胺薄膜材料、丙烯酸黏合剂材料或有机硅黏合剂材料。所述胶带110的材料还可以为其它材料。The material of the
本实施例中,所述胶带110的材料包括聚酰亚胺薄膜材料、丙烯酸黏合剂材料或有机硅黏合剂材料,好处在于:所述胶带110可适用于在超高真空环境中使用,所述胶带110在超高真空环境中使用时,所述胶带110不会释放气泡,避免污染超高真空环境。In this embodiment, the material of the
参考图4,将所述母体层状晶体100粘贴在所述胶带110表面,第一面101与所述胶带110接触。Referring to FIG. 4 , the parent layered
本实施例中,将所述母体层状晶体100粘贴在胶带110表面的步骤在惰性气体环境中进行,这样的好处在于:避免母体层状晶体100受到污染;即使母体层状晶体100的化学性质非常不稳定,也可以保证母体层状晶体100不受到工艺环境的污染。In this embodiment, the step of pasting the parent layered
所述惰性气体包括氩气。The inert gas includes argon.
参考图5,将所述母体层状晶体100粘贴在所述胶带110表面后,在所述母体层状晶体100的表面形成绝缘薄膜镀层130。Referring to FIG. 5 , after the parent layered
具体的,在所述母体层状晶体100的第二面102形成绝缘薄膜镀层130。Specifically, an insulating thin
所述绝缘薄膜镀层130的材料包括氧化铝、氧化硅、氧化镁或二氧化钛。所述绝缘薄膜镀层130的材料还可以为其它绝缘材料。The material of the insulating thin
本实施例中,所述绝缘薄膜镀层130的材料为氧化铝时,所述绝缘薄膜镀层130与母体层状晶体100之间的粘附性更大。In this embodiment, when the material of the insulating thin
形成所述绝缘薄膜镀层130的工艺包括蒸镀工艺、溅射工艺或电镀工艺。The process of forming the insulating thin
在所述母体层状晶体100的表面形成绝缘薄膜镀层130的步骤在高真空环境中进行,所述高真空环境包括粗真空环境或超高真空环境。The step of forming the insulating thin
本实施例中,所述绝缘薄膜镀层130的材料为氧化铝;形成所述绝缘薄膜镀层130的工艺为蒸镀工艺,参数包括:蒸镀环境的氧气分压为1E-4毫巴~2E-4毫巴,蒸镀源为铝。形成所述绝缘薄膜镀层130采用的设备为热蒸发镀膜机。In this embodiment, the material of the insulating thin
本实施例中,蒸镀环境的氧气分压为1E-4毫巴~2E-4毫巴,使得蒸镀源的材料能够被完全氧化。In this embodiment, the partial pressure of oxygen in the evaporation environment is 1E-4 mbar to 2E-4 mbar, so that the material of the evaporation source can be completely oxidized.
本实施例中,所述绝缘薄膜镀层130的厚度为50纳米以上,所述绝缘薄膜镀层130的厚度此范围的意义在于:若所述绝缘薄膜镀层130的厚度小于50纳米,则在后续揭起热释放胶带的过程中绝缘薄膜镀层130容易碎裂,减小最终形成的二维材料的面积。In this embodiment, the thickness of the insulating thin
在一个具体的实施例中,所述绝缘薄膜镀层130的厚度为50纳米~200纳米。所述绝缘薄膜镀层130的厚度在200纳米以下,这样使得绝缘薄膜镀层130的成本降低,且满足使用需要。In a specific embodiment, the thickness of the insulating thin
所述绝缘薄膜镀层130形成在母体层状晶体100表面,绝缘薄膜镀层130与母体层状晶体100材料之间具有很大的粘附性,且绝缘薄膜镀层130与母体层状晶体100具有很大的接触面积。The insulating
本实施例中,形成绝缘薄膜镀层130后,后续的步骤均在惰性气体环境中进行,这样能够避免绝缘薄膜镀层130表面吸附氢,避免降低绝缘薄膜镀层130与母体层状晶体100材料的粘附性。In the present embodiment, after the insulating
参考图6,提供热释放胶带140;在所述绝缘薄膜镀层130表面粘贴热释放胶带140。Referring to FIG. 6 , a
所述热释放胶带140的粘性在热处理的条件下能够消失。The adhesiveness of the
本实施例中,在所述绝缘薄膜镀层130表面粘贴热释放胶带140的步骤在惰性气体环境中进行。In this embodiment, the step of pasting the
参考图7,在所述绝缘薄膜镀层130表面粘贴热释放胶带140之后,揭起所述热释放胶带140,使热释放胶带140粘附所述绝缘薄膜镀层130,且所述绝缘薄膜镀层130表面具有由部分母体层状晶体100构成的中间层状晶体150。Referring to FIG. 7 , after the
本实施例中,揭起所述热释放胶带140的步骤在惰性气体环境中进行。In this embodiment, the step of peeling off the heat release
由于绝缘薄膜镀层130与母体层状晶体100之间具有较强的粘附性,因此在揭起所述热释放胶带140的过程中,绝缘薄膜镀层130会将母体层状晶体100的材料带走,使得绝缘薄膜镀层130表面具有由部分母体层状晶体100构成的中间层状晶体150。Due to the strong adhesion between the insulating
所述中间层状晶体150在各处的厚度均匀性具有差异,例如,在某些区区域有较多原子层的材料,在某些区域有单个原子层的材料。且中间层状晶体150后续还会经历热处理热释放胶带140的热过程,中间层状晶体150表面的原子会变质,因此中间层状晶体150不能作为最终具有高质量的二维材料。The thickness uniformity of the intermediate
由于绝缘薄膜镀层130与母体层状晶体100材料之间具有很大的粘附性,因此绝缘薄膜镀层130与中间层状晶体150之间具有很大的粘附性。Since the insulating
参考图8,提供粘附印章160;揭起所述热释放胶带140之后,在所述热释放胶带140表面覆盖粘附印章160,且所述粘附印章160覆盖所述绝缘薄膜镀层130和所述中间层状晶体150。Referring to FIG. 8, an
所述粘附印章160的材料包括聚合物。所述聚合物包括聚二甲基硅氧烷。The material of the
本实施例中,在所述热释放胶带140表面覆盖粘附印章160的步骤在惰性气体环境中进行。In this embodiment, the step of covering the
参考图9,热处理所述热释放胶带140,使所述热释放胶带140与所述粘附印章160、以及所述热释放胶带140与所述绝缘薄膜镀层130分离。Referring to FIG. 9 , the
热处理所述热释放胶带140,使所述热释放胶带140的粘性解除,因此使所述热释放胶带140与所述粘附印章160、以及所述热释放胶带140与所述绝缘薄膜镀层130分离。The
本实施例中,热处理所述热释放胶带140的步骤在惰性气体环境中进行。In this embodiment, the step of heat-treating the
在一个具体的实施例中,热处理所述热释放胶带140的温度为115摄氏度~125摄氏度,如120摄氏度。这样的好处在于:所述热处理的温度在125摄氏度以下,这样使得粘附印章160能够承受所述热处理的温度,避免粘附印章160的性能受到影响;所述热处理的温度在115摄氏度以上,利于解除热释放胶带140的粘性。In a specific embodiment, the temperature of heat-treating the heat release
参考图10,提供衬底170。Referring to Figure 10, a
本实施例中,所述衬底170的材料为二氧化硅。In this embodiment, the material of the
在其它实施例中,衬底的材料可以为氧化铝或硅片。In other embodiments, the material of the substrate may be aluminum oxide or silicon wafer.
参考图11,对所述衬底170的表面进行清洁处理。Referring to FIG. 11 , the surface of the
所述清洁处理包括等离子体处理。The cleaning treatment includes plasma treatment.
对所述衬底170的表面进行清洁处理,去除衬底170表面的杂质,使衬底170表面的清洁度提高,这样能够提高后续绝缘薄膜镀层130和衬底170之间的粘附性。The surface of the
本实施例中,所述等离子体处理采用氧等离子体。In this embodiment, oxygen plasma is used for the plasma treatment.
本实施例中,采用氧等离子体而不是其它等离子体清洁衬底170的表面,好处在于:氧等离子体可以清洁衬底170表面并使衬底170表面活化,使其粘性增强。In this embodiment, oxygen plasma is used instead of other plasmas to clean the surface of the
在其它实施例中,可不对衬底的表面进行清洁处理。In other embodiments, the surface of the substrate may not be cleaned.
参考图12,将所述粘附印章160、中间层状晶体150和绝缘薄膜镀层130按压在所述衬底170上,且所述绝缘薄膜镀层130与所述衬底170接触。Referring to FIG. 12 , the
本实施例中,热处理所述热释放胶带140后,且对所述衬底170的表面进行清洁处理之后,将所述粘附印章160、中间层状晶体150和绝缘薄膜镀层130按压在所述衬底170上,且所述粘附印章160和所述绝缘薄膜镀层130分别与所述衬底170接触。In this embodiment, after the
本实施例中,将所述粘附印章160、中间层状晶体150和绝缘薄膜镀层130按压在所述衬底170上的步骤在惰性气体环境中进行。In this embodiment, the step of pressing the
参考图13,将所述粘附印章160、中间层状晶体150和绝缘薄膜镀层130按压在所述衬底170上后,揭起所述粘附印章160,所述粘附印章160表面带走部分中间层状晶体150,使所述绝缘薄膜镀层130表面形成二维材料180。Referring to FIG. 13 , after pressing the
本实施例中,揭起所述粘附印章160的速度较快,这样的好处在于:增加粘附印章160与中间层状晶体150之间的粘性,增大形成二维材料180的可能性。In this embodiment, the speed of lifting the
本实施例中,揭起所述粘附印章160的步骤在惰性气体环境中进行。In this embodiment, the step of lifting the
所述二维材料180包括单层的MoS2、单层的TaS2、单层的Fe3GeTe2、单层的VSe2、单层的FeSe、单层的CrI3、单层的Cr2Ge2Te6、单层的WSe2、单层的WS2、单层的WTe2或单层的黑磷。The two-
本实施例中,以所述二维材料180为单层的Fe3GeTe2进行示例。In this embodiment, the two-
现有的机械解离方法仅较容易地解离部分二维材料,如石墨烯、氮化硼和MoS2,且得到的二维材料的面积很小。现有的机械解离方法难以解离如Fe3GeTe2、TaS2、VSe2、FeSe、CrI3、Cr2Ge2Te6、WSe2、WS2、WTe2或黑磷材料的二维材料。Existing mechanical dissociation methods only dissociate part of two-dimensional materials relatively easily, such as graphene, boron nitride and MoS 2 , and the area of the obtained two-dimensional materials is small. Existing mechanical dissociation methods are difficult to dissociate 2D materials such as Fe 3 GeTe 2 , TaS 2 , VSe 2 , FeSe, CrI 3 , Cr 2 Ge 2 Te 6 , WSe 2 , WS 2 , WTe 2 or black phosphorus materials .
本实施例的方法不仅能够解离得到如MoS2材料的二维材料,还能够解离得到Fe3GeTe2、TaS2、VSe2、FeSe、CrI3、Cr2Ge2Te6、WSe2、WS2、WTe2或黑磷材料的二维材料,且能较为容易的获取这些二维材料。The method of this embodiment can not only dissociate to obtain two-dimensional materials such as MoS 2 materials, but also dissociate to obtain Fe 3 GeTe 2 , TaS 2 , VSe 2 , FeSe, CrI 3 , Cr 2 Ge 2 Te 6 , WSe 2 , Two-dimensional materials of WS 2 , WTe 2 or black phosphorus materials, and these two-dimensional materials can be easily obtained.
本实施例中,所述二维材料180的横向长度在100微米以上。所述横向长度指的是:所述二维材料180在二维材料180的原子分布的平面内的长度。In this embodiment, the lateral length of the two-
由于绝缘薄膜镀层130与中间层状晶体150之间具有很大的粘附性,因此揭起所述粘附印章160后,所述绝缘薄膜镀层130表面能形成质量较高的二维材料180,具体表现在:二维材料180的均匀性较高,二维材料180的缺陷较少。Since the insulating
由于绝缘薄膜镀层130具有较大的面积,因此能在绝缘薄膜镀层130表面形成大面积的二维材料180。Since the insulating thin
本实施例中,将绝缘薄膜镀层130粘附在衬底170表面,以实现二维材料180固定在衬底170上,因此二维材料180的形成不受衬底170材料的限制,使得二维材料180的种类能够拓宽。In this embodiment, the insulating thin
本实施例中,没有利用液相方法,因此二维材料180在制备过程中不会暴露于有机溶剂,因此本实施例的方法适于对有机溶剂敏感的二维材料180的制作,制备的二维材料180的种类能够拓宽,且二维材料180的质量不会受到液相溶剂的影响。In this embodiment, the liquid phase method is not used, so the two-
本实施例中,绝缘薄膜镀层130为绝缘材料,绝缘薄膜镀层130不会影响对二维材料180进行电输运性质的测量过程。In this embodiment, the insulating
本实施例中,绝缘薄膜镀层130无需被刻蚀去除,因此不会对二维材料180有刻蚀损伤的问题,使得二维材料180的质量提高。In this embodiment, the insulating
虽然本发明披露如上,但本发明并非限定于此。任何本领域技术人员,在不脱离本发明的精神和范围内,均可作各种更动与修改,因此本发明的保护范围应当以权利要求所限定的范围为准。Although the present invention is disclosed above, the present invention is not limited thereto. Any person skilled in the art can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, the protection scope of the present invention should be based on the scope defined by the claims.
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