WO2016192391A1 - Preparation method of molybdenum disulfide thin film, and molybdenum disulfide thin film - Google Patents

Preparation method of molybdenum disulfide thin film, and molybdenum disulfide thin film Download PDF

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WO2016192391A1
WO2016192391A1 PCT/CN2015/099600 CN2015099600W WO2016192391A1 WO 2016192391 A1 WO2016192391 A1 WO 2016192391A1 CN 2015099600 W CN2015099600 W CN 2015099600W WO 2016192391 A1 WO2016192391 A1 WO 2016192391A1
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molybdenum disulfide
film
buffer layer
disulfide film
oxide buffer
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PCT/CN2015/099600
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French (fr)
Chinese (zh)
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刘新科
何佳铸
吕有明
韩舜
曹培江
柳文军
曾玉祥
贾芳
朱德亮
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深圳大学
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Publication of WO2016192391A1 publication Critical patent/WO2016192391A1/en

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating

Definitions

  • the invention relates to the technical field of nano material preparation, in particular to a preparation method of a molybdenum disulfide film and a molybdenum disulfide film.
  • the molybdenum sulfide film is similar in structure and properties to graphene. However, unlike graphene, the molybdenum sulfide film has a tunable band gap.
  • the band gap of MoS2 is 1.2eV, and its electronic transition mode is indirect transition. When the thickness is single layer, the band gap of MoS2 can reach 1.8eV, and its electronic transition mode is transformed into direct transition. Therefore, the unique structure and excellent physical properties of the MoS2 film and the adjustable band gap make it more potential than graphene in the field of electronic devices. It will be an important application prospect in the fields of electricity, optics and semiconductors. Two-dimensional nanomaterials.
  • MoS2 film With its nano-sized layered structure, it is possible to manufacture smaller-sized, more energy-efficient semiconductor chips, making them widely used in the field of nanoelectronic components.
  • the MoS2 film has excellent physical properties, its electrical, thermal, optical and mechanical properties and its potential for application in the field of semiconductor electronic components, it is necessary to open the door of the MoS2 application field. Looking for a better method for preparing large-area high-quality MoS2 film, and focusing on realizing rapid transfer of MoS2 film on different substrates, making up for the shortcomings of MoS2 film in the process preparation method, and realizing the revolutionary development of MoS2 material preparation, The widespread use of MoS2 film materials in the industry is just around the corner.
  • the MoS2 film with larger area can be grown in the prior art, the compactness of the product is relatively poor, and the sulfur vacancies are more, resulting in poor performance of the film.
  • the key point is that the product cannot achieve rapid film transfer and the transfer speed is slow. The process is cumbersome, requires a lot of materials, and is difficult to transfer.
  • the object of the present invention is to provide a method for preparing a molybdenum disulfide film and a molybdenum disulfide film, which are intended to improve the relatively poor compactness and sulfur vacancy of the MoS2 film material obtained by the prior art. More, resulting in poor film properties, can not achieve rapid film transfer and other issues.
  • the technical scheme of the present invention is as follows: a preparation method of a molybdenum disulfide film, comprising the following steps:
  • a molybdenum disulfide film is grown on the surface thereof by a CVD method.
  • the present invention provides a method for preparing a molybdenum disulfide film and a molybdenum disulfide film, which are prepared by the method of the present invention, using a chemical vapor deposition (CVD) method on a silicon substrate coated with an oxide buffer layer.
  • CVD chemical vapor deposition
  • MoS2 molybdenum sulfide
  • Figure 1 is a schematic diagram showing the comparison of the lattice constants of different compound films.
  • FIG. 2 is a schematic view showing the structure of a MoS2 film grown by a conventional process CVD method.
  • FIG. 3 is a schematic view showing the structure of a MoS2 film prepared by the preparation method of the present invention.
  • Example 4 is a Raman spectrometer test result of the MoS2 film prepared in Example 1 of the present invention.
  • Fig. 5 is a view showing a film observed by an optical microscope of a MoS2 film prepared in Example 1 of the present invention.
  • the present invention provides a method for preparing a molybdenum disulfide film and a molybdenum disulfide film, and the present invention will be further described in detail in order to clarify and clarify the objects, technical solutions and effects of the present invention. It is understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
  • the invention provides a method for preparing a molybdenum disulfide film, which directly grows large-area, high-quality, low-defect molybdenum sulfide (MoS2) on a silicon substrate coated with an oxide buffer layer by chemical vapor deposition (CVD). Film, and innovatively achieve rapid transfer of MoS2 film.
  • MoS2 molybdenum disulfide
  • the main method for preparing large-area high-quality molybdenum sulfide thin films is to use the chemical vapor deposition (CVD) method for the growth of MoS2 thin films, which has the advantages of large-area continuous synthesis in batches, and controllable preparation of MoS2 thin films. And can control the structure of the film, but can not achieve the rapid transfer of the film product, the transfer speed is slow, the process is cumbersome, the cost of materials is large, and the transfer is difficult, and the product compactness is relatively poor, the sulfur vacancy is relatively Many, resulting in poor electrical properties of the film.
  • the key point of the present invention is also the key innovation of the present invention.
  • a ZnO buffer layer is selected among Si, SiO2 and Al2O3, and the technical solution of the present invention is described in detail with a ZnO buffer layer. This is because the lattice constant a of the lead-zinc ZnO thin film is very close to the lattice constant a of the MoS2 thin film. It can be clearly seen from Fig.
  • the oxide buffer layer is an oxide buffer layer matched with the lattice size of MoS2, and may be a series of oxide buffer layers such as magnesium oxide (MgO) or a multi-oxide oxide, in addition to zinc oxide (ZnO). Buffer layer (such as MgZnO).
  • the existing process for preparing the MoS2 film is generally to deposit a thin layer of silicon dioxide (SiO2) on the silicon wafer (Si), and then grow the MoS2 film by CVD.
  • the structure diagram is shown in FIG. 2, thereby realizing MoS2. Film growth.
  • SiO2 is very difficult to be corroded by acid or alkali during the transfer process, it is difficult to transfer the MoS2 film.
  • the innovative use of ZnO as a growth buffer layer is proposed.
  • the structure of the structure is shown in FIG. 3, which not only greatly improves the quality of the growth of the MoS2 film, but more importantly, enables rapid film transfer, which is the most critical.
  • the steps are also different from the prior art.
  • the method for preparing the molybdenum disulfide film comprises the following steps:
  • PLD pulsed laser deposition
  • magnetron sputtering technique or the like to coat a clean silicon substrate with an oxide buffer layer matching the size of the MoS2 lattice
  • a MoS2 film is grown on the surface thereof by a CVD method
  • the transfer process is to pass the etching buffer layer, and the MoS2 film is detached from the substrate, and then transferred to other substrates.
  • the transfer process mainly includes the following steps:
  • the film is cleaned with deionized water, and the molybdenum disulfide film is separated from the silicon substrate by a polymethyl methacrylate film;
  • the chemical reaction occurs in the traditional buffer layer transfer process: SiO2+2NaOH ⁇ Na2SiO3+H2O (heating).
  • the process takes a long time, usually takes 2 to 3 hours, the conditions are harsh, and the concentration of the NaOH solution is required to be very high.
  • a MoS2 film is also provided in the present invention, and the MoS2 film is prepared by the above method.
  • Cleaning the silicon (Si) substrate, the cleaning process includes the following steps:
  • PLD pulsed laser deposition
  • magnetron sputtering technology and the like are used to plate a ZnO buffer layer on a silicon substrate with a thickness of about 130 nm:
  • PLD technology is an ultra-high vacuum film preparation technology. It bombards the target with a high-power pulsed laser beam, and the atoms, molecules and their clusters required to deposit the film are separated from the surface of the target, and gasification is converted into plasma; the plasma is directed from the target to the target.
  • the substrate is transported in a direction, and then deposited on a substrate having a certain temperature to nucleate and grow to form a thin film.
  • magnetron sputtering techniques and the like can also plate a ZnO buffer layer on a silicon substrate.
  • the CVD method refers to a process in which a vapor containing a gaseous reactant or a liquid reactant constituting a thin film element and other gases required for the reaction are introduced into a reaction chamber to chemically react on the surface of the substrate to form a thin film.
  • the experimental conditions of the process of the present invention are: using sulfur powder and MoO3 (99.9%, analytical purity) as a sulfur source and a molybdenum source, high purity argon as a carrier gas, and depositing MoS2 on a silicon wafer coated with a ZnO buffer layer. film.
  • PMMA Polymethyl methacrylate
  • an optical microscope and a laser Raman spectrometer are used.
  • Spectrometer Spectrometer
  • AFM atomic force microscopy
  • SEM scanning electron microscopy
  • EDS energy dispersive spectroscopy
  • a few layers of MoS2 in the present invention can be imaged under an optical microscope and directly observed. Characterization by laser Raman spectroscopy, as the number of atomic layers decreases, the blue shift A1g of the MoS2 Raman vibration mode E12g is red-shifted. The two vibration modes will be shifted toward each other. The number of layers of molybdenum sulfide can be directly determined by measuring the spacing between the two vibration modes.
  • the spacing between the two vibration modes of the single layer of molybdenum sulfide is 18-20.
  • Cm-1 double vibration molybdenum two vibration modes with a spacing of 20 ⁇ 22
  • the spacing between the two vibration modes of cm-1, three layers or more than three layers of molybdenum sulfide is 22 ⁇ 24cm-1. According to this, the number of layers of MoS2 can be identified.
  • Fluorescence scanning of the sample film using a laser Raman spectrometer (PL) Mapping) the shape and thickness of the film are characterized according to different luminescent properties of the crystal film of different thicknesses. Finally, the film thickness and surface morphology were accurately measured by AFM, and the surface morphology and EDS were used to analyze the main components of the film.
  • FIG. 4 is a test result of a Raman spectrometer
  • Figure 5 is a film observed by an optical microscope.
  • the product obtained by the process conditions proposed by the present invention can be seen from the Raman spectrum.
  • the two characteristics of MoS2 are Raman vibrations E12g and A1g, indicating that the product obtained by the process conditions is indeed a MoS2 film with a thickness of multiple layers. It can be seen from the picture of the optical microscope that the MoS2 film obtained by the process conditions has uniform thickness and good quality.
  • the etching process of the buffer layer in this embodiment takes only 1 minute and 30 seconds, and the etching process for the conventional buffer layer is 2 to 3 hours, which greatly reduces the time required for transferring the MoS2 film.

Abstract

Disclosed are a preparation method of a molybdenum disulfide thin film, and molybdenum disulfide thin film. The present invention uses chemical vapor deposition (CVD) to directly grow a molybdenum sulfide (MoS2) thin film having a large area, high quality and few defects on a silicon substrate coated with an oxide buffer layer, and innovatively realizes fast transfer of the MoS2 thin film.

Description

一种二硫化钼薄膜的制备方法及二硫化钼薄膜  Preparation method of molybdenum disulfide film and molybdenum disulfide film 技术领域Technical field
本发明涉及纳米材料制备技术领域，尤其涉及一种二硫化钼薄膜的制备方法及二硫化钼薄膜。The invention relates to the technical field of nano material preparation, in particular to a preparation method of a molybdenum disulfide film and a molybdenum disulfide film.
背景技术Background technique
硫化钼薄膜在结构和性能上类似于石墨烯， 但与石墨烯不同，硫化钼薄膜存在一个可调控的带隙。块状晶体MoS2的带隙为1.2eV，其电子跃迁方式间接跃迁；当厚度为单层时，MoS2的带隙可以达到1.8eV，且其电子跃迁方式转变为直接跃迁。因此，MoS2薄膜独特的结构和优异的物理性能以及可调节的能带隙使其在电子器件领域比石墨烯更具有应用潜力，它将是一种在电学、光学、半导体领域具有十分重要应用前景的二维纳米材料。凭借其纳米尺寸的层状结构，使得制造更小规格、更高能效半导体芯片成为可能，使其在纳米电子元器件领域被广泛应用。但尽管MoS2薄膜具有优异的物理特性，在电学、热学、光学和力学等方面的特性及其在半导体电子元器件领域具有很大的应用潜力，但是要打开MoS2应用领域的这扇大门，还需要寻找更好的制备大面积高质量MoS2薄膜的方法，并重点实现MoS2薄膜在不同衬底实现快速转移，弥补一直以来MoS2薄膜在工艺制备方法上的不足，实现MoS2材料制备的革命性发展，这样MoS2薄膜材料在工业中的广泛使用将指日可待。现有工艺中虽然能生长出面积较大的MoS2薄膜，但是其产品致密性相对较差，硫空位较多，导致薄膜的性能差，重点是其产品不能实现薄膜的快速转移，转移速度慢，过程较繁琐，花费材料多，且转移难度大。The molybdenum sulfide film is similar in structure and properties to graphene. However, unlike graphene, the molybdenum sulfide film has a tunable band gap. The band gap of MoS2 is 1.2eV, and its electronic transition mode is indirect transition. When the thickness is single layer, the band gap of MoS2 can reach 1.8eV, and its electronic transition mode is transformed into direct transition. Therefore, the unique structure and excellent physical properties of the MoS2 film and the adjustable band gap make it more potential than graphene in the field of electronic devices. It will be an important application prospect in the fields of electricity, optics and semiconductors. Two-dimensional nanomaterials. With its nano-sized layered structure, it is possible to manufacture smaller-sized, more energy-efficient semiconductor chips, making them widely used in the field of nanoelectronic components. However, although the MoS2 film has excellent physical properties, its electrical, thermal, optical and mechanical properties and its potential for application in the field of semiconductor electronic components, it is necessary to open the door of the MoS2 application field. Looking for a better method for preparing large-area high-quality MoS2 film, and focusing on realizing rapid transfer of MoS2 film on different substrates, making up for the shortcomings of MoS2 film in the process preparation method, and realizing the revolutionary development of MoS2 material preparation, The widespread use of MoS2 film materials in the industry is just around the corner. Although the MoS2 film with larger area can be grown in the prior art, the compactness of the product is relatively poor, and the sulfur vacancies are more, resulting in poor performance of the film. The key point is that the product cannot achieve rapid film transfer and the transfer speed is slow. The process is cumbersome, requires a lot of materials, and is difficult to transfer.
因此，现有技术还有待改进。Therefore, the prior art has yet to be improved.
技术问题technical problem
鉴于上述现有技术的不足，本发明的目的在于提供一种二硫化钼薄膜的制备方法及二硫化钼薄膜，旨在改善采用现有工艺得到的MoS2薄膜材料存在致密性相对较差，硫空位较多，导致薄膜的性能差、不能实现薄膜快速转移等问题。In view of the above deficiencies of the prior art, the object of the present invention is to provide a method for preparing a molybdenum disulfide film and a molybdenum disulfide film, which are intended to improve the relatively poor compactness and sulfur vacancy of the MoS2 film material obtained by the prior art. More, resulting in poor film properties, can not achieve rapid film transfer and other issues.
技术解决方案Technical solution
本发明的技术方案如下：一种二硫化钼薄膜的制备方法，包括以下步骤：The technical scheme of the present invention is as follows: a preparation method of a molybdenum disulfide film, comprising the following steps:
a、在硅衬底上镀上一层与二硫化钼晶格大小相匹配的氧化物缓冲层；a plating an oxide buffer layer matching the lattice size of the molybdenum disulfide on the silicon substrate;
b、使用CVD法在其表面生长二硫化钼薄膜。b. A molybdenum disulfide film is grown on the surface thereof by a CVD method.
有益效果Beneficial effect
有益效果：本发明提供一种二硫化钼薄膜的制备方法及二硫化钼薄膜，采用本发明所提供的制备方法，使用化学气相沉积法（CVD）在镀有氧化物缓冲层的硅衬底上直接生长大面积、高质量、低缺陷的硫化钼（MoS2）薄膜，不仅可以实现MoS2薄膜的快速转移，还同时提高MoS2薄膜的质量，减少MoS2薄膜的材料缺陷，例如硫空穴。[Advantageous Effects] The present invention provides a method for preparing a molybdenum disulfide film and a molybdenum disulfide film, which are prepared by the method of the present invention, using a chemical vapor deposition (CVD) method on a silicon substrate coated with an oxide buffer layer. Direct growth of large-area, high-quality, low-defect molybdenum sulfide (MoS2) films not only enables rapid transfer of MoS2 films, but also improves the quality of MoS2 films and reduces material defects such as sulfur holes in MoS2 films.
附图说明DRAWINGS
图1是不同化合物薄膜的晶格常数大小对比示意图。Figure 1 is a schematic diagram showing the comparison of the lattice constants of different compound films.
图2是传统工艺CVD法生长MoS2薄膜的结构示意图。2 is a schematic view showing the structure of a MoS2 film grown by a conventional process CVD method.
图3是本发明制备方法制备MoS2薄膜的结构示意图。3 is a schematic view showing the structure of a MoS2 film prepared by the preparation method of the present invention.
图4是本发明实施例1中制备得到的MoS2薄膜的拉曼光谱仪测试结果。4 is a Raman spectrometer test result of the MoS2 film prepared in Example 1 of the present invention.
图5是本发明实施例1中制备得到的MoS2薄膜光学显微镜所观察到的薄膜图。Fig. 5 is a view showing a film observed by an optical microscope of a MoS2 film prepared in Example 1 of the present invention.
本发明的实施方式Embodiments of the invention
本发明提供一种二硫化钼薄膜的制备方法及二硫化钼薄膜，为使本发明的目的、技术方案及效果更加清楚、明确，以下对本发明进一步详细说明。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。The present invention provides a method for preparing a molybdenum disulfide film and a molybdenum disulfide film, and the present invention will be further described in detail in order to clarify and clarify the objects, technical solutions and effects of the present invention. It is understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
本发明所提供的一种二硫化钼薄膜的制备方法，使用化学气相沉积法（CVD）在镀有氧化物缓冲层的硅衬底上直接生长大面积、高质量、低缺陷的硫化钼（MoS2）薄膜，并创新性地实现MoS2薄膜的快速转移。The invention provides a method for preparing a molybdenum disulfide film, which directly grows large-area, high-quality, low-defect molybdenum sulfide (MoS2) on a silicon substrate coated with an oxide buffer layer by chemical vapor deposition (CVD). Film, and innovatively achieve rapid transfer of MoS2 film.
目前制备大面积高质量的硫化钼薄膜的主要方法是使用化学气相沉积法（CVD）进行MoS2薄膜的生长，它的优点是可以批量化实现大面积连续合成，实现对MoS2薄膜的可控化制备，并且可以对薄膜的结构加以一定的控制，但不能够实现薄膜产品的快速转移，转移速度慢，过程较繁琐，花费材料多，且转移难度大，且产品致密性相对较差，硫空位较多，导致薄膜的电学性能差。本发明的重点也是本发明的关键创新点在于，通过对薄膜生长理论原理的探究，探索出能够实现薄膜产品快速转移的缓冲层工艺条件，包括可以转移到一系列柔性衬底上，并且由于新缓冲层的革命性提出大大地提高了MoS2薄膜的质量，极高的改善了薄膜的电学性能。根据薄膜生长的晶格匹配原理，本方明实施方案中在Si、SiO2以及Al2O3中选择了ZnO缓冲层，以ZnO缓冲层对本发明技术方案进行详细说明。这是由于铅锌矿ZnO薄膜的晶格常数a大小跟MoS2薄膜的晶格常数a大小非常接近，从图1可以明显的看出，可以提高MoS2薄膜的质量。而且，ZnO缓冲层非常容易被酸腐蚀，从而容易实现MoS2薄膜的快速转移。所述氧化物缓冲层为与MoS2晶格大小相匹配的氧化物缓冲层，除了可以为氧化锌（ZnO）外，还可以是氧化镁（MgO）等一系列氧化物缓冲层，或多元氧化物缓冲层（如MgZnO）。At present, the main method for preparing large-area high-quality molybdenum sulfide thin films is to use the chemical vapor deposition (CVD) method for the growth of MoS2 thin films, which has the advantages of large-area continuous synthesis in batches, and controllable preparation of MoS2 thin films. And can control the structure of the film, but can not achieve the rapid transfer of the film product, the transfer speed is slow, the process is cumbersome, the cost of materials is large, and the transfer is difficult, and the product compactness is relatively poor, the sulfur vacancy is relatively Many, resulting in poor electrical properties of the film. The key point of the present invention is also the key innovation of the present invention. By exploring the theoretical principle of thin film growth, the buffer layer process conditions capable of realizing rapid transfer of thin film products, including transfer to a series of flexible substrates, and The revolutionary nature of the buffer layer has greatly improved the quality of the MoS2 film and greatly improved the electrical properties of the film. According to the lattice matching principle of film growth, in the embodiment of the present invention, a ZnO buffer layer is selected among Si, SiO2 and Al2O3, and the technical solution of the present invention is described in detail with a ZnO buffer layer. This is because the lattice constant a of the lead-zinc ZnO thin film is very close to the lattice constant a of the MoS2 thin film. It can be clearly seen from Fig. 1 that the quality of the MoS2 thin film can be improved. Moreover, the ZnO buffer layer is very susceptible to acid corrosion, thereby facilitating rapid transfer of the MoS2 film. The oxide buffer layer is an oxide buffer layer matched with the lattice size of MoS2, and may be a series of oxide buffer layers such as magnesium oxide (MgO) or a multi-oxide oxide, in addition to zinc oxide (ZnO). Buffer layer (such as MgZnO).
现有制备MoS2薄膜的工艺一般是在硅片（Si）上镀上一层二氧化硅（SiO2）薄层，然后再使用CVD法生长MoS2薄膜，其结构示意图如图2所示，从而实现MoS2薄膜的生长。但是在转移过程中由于SiO2非常难被酸或是碱腐蚀，因此难以实现MoS2薄膜的转移。而本发明中创新性的提出使用ZnO作为生长缓冲层，其结构示意图如图3所示，不仅大大提高MoS2薄膜生长的质量，更为重要的是能够实现薄膜的快速转移，这是最关键的步骤，也是与现有技术的区别。The existing process for preparing the MoS2 film is generally to deposit a thin layer of silicon dioxide (SiO2) on the silicon wafer (Si), and then grow the MoS2 film by CVD. The structure diagram is shown in FIG. 2, thereby realizing MoS2. Film growth. However, since SiO2 is very difficult to be corroded by acid or alkali during the transfer process, it is difficult to transfer the MoS2 film. In the present invention, the innovative use of ZnO as a growth buffer layer is proposed. The structure of the structure is shown in FIG. 3, which not only greatly improves the quality of the growth of the MoS2 film, but more importantly, enables rapid film transfer, which is the most critical. The steps are also different from the prior art.
具体地，所述二硫化钼薄膜的制备方法，包括以下步骤：Specifically, the method for preparing the molybdenum disulfide film comprises the following steps:
使用脉冲激光沉积技术（PLD）或者是磁控溅射技术等类似技术在洁净的硅衬底上镀上一层与MoS2晶格大小相匹配的氧化物缓冲层；Using a pulsed laser deposition technique (PLD) or a magnetron sputtering technique or the like to coat a clean silicon substrate with an oxide buffer layer matching the size of the MoS2 lattice;
使用CVD法在其表面生长MoS2薄膜；A MoS2 film is grown on the surface thereof by a CVD method;
转移MoS2薄膜至其他衬底上。Transfer the MoS2 film to other substrates.
其中，转移过程为通过腐蚀缓冲层，使MoS2薄膜脱离衬底，继而转移到其他衬底上。Wherein, the transfer process is to pass the etching buffer layer, and the MoS2 film is detached from the substrate, and then transferred to other substrates.
具体地，转移过程主要包括以下步骤：Specifically, the transfer process mainly includes the following steps:
在二硫化钼薄膜表面涂上一层聚甲基丙烯酸甲酯（PMMA），作为支撑MoS2薄膜的支架；Applying a layer of polymethyl methacrylate (PMMA) on the surface of the molybdenum disulfide film as a support for supporting the MoS2 film;
烘干，聚甲基丙烯酸甲酯成膜；Drying, forming polymethyl methacrylate film;
将带有二硫化钼薄膜的硅衬底浸泡于稀酸溶液中，直至氧化物缓冲层被腐蚀完毕，聚甲基丙烯酸甲酯薄膜浮起；Soaking a silicon substrate with a molybdenum disulfide film in a dilute acid solution until the oxide buffer layer is etched, and the polymethyl methacrylate film floats;
用去离子水清洗薄膜，此时二硫化钼薄膜带着聚甲基丙烯酸甲酯薄膜脱离了硅衬底；The film is cleaned with deionized water, and the molybdenum disulfide film is separated from the silicon substrate by a polymethyl methacrylate film;
将二硫化钼薄膜转移至其他衬底上；Transferring the molybdenum disulfide film to other substrates;
烘干；drying;
滴加聚甲基丙烯酸甲酯，软化聚甲基丙烯酸甲酯薄膜，并保持湿润，浸泡数分钟；Add polymethyl methacrylate dropwise, soften the polymethyl methacrylate film, keep it moist, soak for several minutes;
用丙酮冲洗，洗去PMMA。Rinse with acetone and wash away PMMA.
传统缓冲层转移过程发生的化学反应：SiO2+2NaOH→Na2SiO3+H2O（加热），该过程时间长，通常需要2到3小时，条件较为苛刻，且要求NaOH溶液浓度非常高。The chemical reaction occurs in the traditional buffer layer transfer process: SiO2+2NaOH→Na2SiO3+H2O (heating). The process takes a long time, usually takes 2 to 3 hours, the conditions are harsh, and the concentration of the NaOH solution is required to be very high.
而本发明转移过程发生的化学反应：ZnO+2HCl→ZnCl2+H2O，该过程时间非常短，仅仅需要1到2分钟，且腐蚀液浓度很低，普通的稀酸（稀盐酸、稀硫酸或是稀氢氟酸等）都可以迅速腐蚀缓冲层。However, the chemical reaction occurring in the transfer process of the present invention: ZnO+2HCl→ZnCl2+H2O, the process time is very short, only takes 1 to 2 minutes, and the concentration of the etching solution is very low, ordinary dilute acid (diluted hydrochloric acid, dilute sulfuric acid or Dilute hydrofluoric acid, etc.) can quickly etch the buffer layer.
本发明中还提供一种MoS2薄膜，所述MoS2薄膜是采用上述方法制备而成的。A MoS2 film is also provided in the present invention, and the MoS2 film is prepared by the above method.
以下通过具体的实施例对本发明做进一步说明。The invention is further illustrated by the following specific examples.
实施例1Example 1
一、对硅（Si）衬底进行清洗，清洗过程包括以下步骤：1. Cleaning the silicon (Si) substrate, the cleaning process includes the following steps:
1、三氯乙烯超声清；1. Trichloroethylene ultrasonic cleaning;
2、丙酮超声清洗；2. Acetone ultrasonic cleaning;
3、乙醇超声清洗；3. Ultrasonic cleaning of ethanol;
4、去离子水烧杯中冲洗；4. Rinse in a deionized water beaker;
5、硫酸：硝酸=1：1在80℃煮数分钟，去离子水冲洗；5, sulfuric acid: nitric acid = 1:1 at 80 ° C for a few minutes, rinse with deionized water;
6、盐酸：双氧水：水=3：1：1，轻摇数分钟，去离子水冲净；6, hydrochloric acid: hydrogen peroxide: water = 3: 1:1, lightly shake for a few minutes, rinsed with deionized water;
7、氢氟酸：水=1：20，轻摇数分钟，去离子水冲净；7. Hydrofluoric acid: water = 1:20, shake for a few minutes, rinse with deionized water;
8、去离子水烧杯中冲洗数遍，流水冲洗。8. Rinse several times in a deionized water beaker and rinse with running water.
二、采用脉冲激光沉积法（PLD）或者是磁控溅射技术等类似技术在硅衬底上镀ZnO缓冲层，厚度约为130nm：Second, pulsed laser deposition (PLD) or magnetron sputtering technology and the like are used to plate a ZnO buffer layer on a silicon substrate with a thickness of about 130 nm:
PLD技术是一种超高真空薄膜制备技术。它是用一束高功率的脉冲激光束轰击靶材，将欲沉积薄膜所需的原子、分子与它们的团簇从靶材表面剥离出来，气化转变为等离子体；等离子体从靶材向衬底方向传输，然后沉积在具有一定温度的衬底上成核、长大形成薄膜。同样，磁控溅射技术等类似技术也能在硅衬底镀上ZnO缓冲层。PLD technology is an ultra-high vacuum film preparation technology. It bombards the target with a high-power pulsed laser beam, and the atoms, molecules and their clusters required to deposit the film are separated from the surface of the target, and gasification is converted into plasma; the plasma is directed from the target to the target. The substrate is transported in a direction, and then deposited on a substrate having a certain temperature to nucleate and grow to form a thin film. Similarly, magnetron sputtering techniques and the like can also plate a ZnO buffer layer on a silicon substrate.
三、采用化学气相沉淀法（CVD）法在ZnO缓冲层上生长MoS2薄膜：3. Growth of MoS2 film on ZnO buffer layer by chemical vapor deposition (CVD) method:
CVD法指把含有构成薄膜元素的气态反应剂或液态反应剂的蒸气及反应所需其它气体引入反应室，在衬底表面发生化学反应生成薄膜的过程。本发明此工艺的实验条件是：以硫粉和MoO3(99.9%,分析纯）为硫源和钼源，高纯氩气为载流气体，在镀有ZnO缓冲层的硅片上沉积制备MoS2薄膜。The CVD method refers to a process in which a vapor containing a gaseous reactant or a liquid reactant constituting a thin film element and other gases required for the reaction are introduced into a reaction chamber to chemically react on the surface of the substrate to form a thin film. The experimental conditions of the process of the present invention are: using sulfur powder and MoO3 (99.9%, analytical purity) as a sulfur source and a molybdenum source, high purity argon as a carrier gas, and depositing MoS2 on a silicon wafer coated with a ZnO buffer layer. film.
四、将MoS2薄膜快速转移到其他衬底上：4. Transfer the MoS2 film to other substrates quickly:
1、将聚甲基丙烯酸甲酯（PMMA）旋涂在生长好的样品片子上，作为支撑MoS2薄膜的支架；1. Polymethyl methacrylate (PMMA) is spin-coated on the grown sample sheet as a support for supporting the MoS2 film;
3、在样品片子周围用刀子刮几下，防止前后面的PMMA粘合上；3. Scrap a few times around the sample piece with a knife to prevent the PMMA from bonding to the front and back;
4、烘干；4, drying;
5、将上述烘干的片子浸泡在0.5mol/L的盐酸（HCl）溶液中，迅速腐蚀ZnO缓冲层，直至PMMA薄膜漂浮起来，这也是本发明的关键点；5. Soaking the dried sheet in a 0.5 mol/L hydrochloric acid (HCl) solution, rapidly etching the ZnO buffer layer until the PMMA film floats, which is also a key point of the present invention;
6、多次浸泡在DI水（去离子水），目的是洗干净薄膜；6, immersed in DI water (deionized water) multiple times, the purpose is to clean the film;
7、转移，带有MoS2薄膜的PMMA薄膜，直接将其贴合在新转移的片子上；7. Transfer, PMMA film with MoS2 film, directly attached to the newly transferred film;
8、烘干；8, drying;
9、滴加PMMA在已硬化的PMMA薄膜中间使其软化，并保持湿润，浸泡数分钟；9. Add PMMA in the middle of the hardened PMMA film to soften it, keep it moist, soak for several minutes;
10、丙酮冲洗，洗去PMMA。10. Rinse with acetone and wash away PMMA.
本实施例中采用光学显微镜（optical microscope）、激光拉曼光谱仪（laser Raman spectrometer）、原子力显微镜（AFM）、扫描电子显微镜（SEM）以及能谱仪（EDS）来表征产品。本发明中少数层的MoS2可以在光学显微镜下成像，并被直接观察到。使用激光拉曼光谱仪进行表征，随着原子层数的减少，MoS2拉曼振动模式E12g发生蓝移A1g发生红移。两个振动模式将朝着相互靠近的方向偏移，可以通过测量这两个振动模式的间距来直接地判断硫化钼的层数，单层硫化钼两个振动模式的间距为18~20 cm-1，双层硫化钼两个振动模式的间距为20~22 cm-1，三层或大于三层硫化钼两个振动模式的间距为22~24cm-1。据此可以鉴别MoS2的层数。同时也使用激光拉曼光谱仪对样品薄膜进行荧光扫描（PL mapping），根据不同厚度的晶体薄膜发光性质不同表征薄膜形状以及厚度。最后通过AFM准确测量薄膜厚度以及表面形貌，通过SEM描绘表面形态以及EDS分析薄膜主要成分。In this embodiment, an optical microscope and a laser Raman spectrometer (laser Raman) are used. Spectrometer), atomic force microscopy (AFM), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS) to characterize the product. A few layers of MoS2 in the present invention can be imaged under an optical microscope and directly observed. Characterization by laser Raman spectroscopy, as the number of atomic layers decreases, the blue shift A1g of the MoS2 Raman vibration mode E12g is red-shifted. The two vibration modes will be shifted toward each other. The number of layers of molybdenum sulfide can be directly determined by measuring the spacing between the two vibration modes. The spacing between the two vibration modes of the single layer of molybdenum sulfide is 18-20. Cm-1, double vibration molybdenum two vibration modes with a spacing of 20~22 The spacing between the two vibration modes of cm-1, three layers or more than three layers of molybdenum sulfide is 22~24cm-1. According to this, the number of layers of MoS2 can be identified. Fluorescence scanning of the sample film using a laser Raman spectrometer (PL) Mapping), the shape and thickness of the film are characterized according to different luminescent properties of the crystal film of different thicknesses. Finally, the film thickness and surface morphology were accurately measured by AFM, and the surface morphology and EDS were used to analyze the main components of the film.
检测结果如图4和图5所示，图4是拉曼光谱仪的测试结果，图5是光学显微镜所观察到的薄膜。本发明提出的工艺条件得到的产品，由拉曼光谱图可以看出， MoS2的两个特征拉曼振动E12g与A1g，说明本工艺条件所得到的产品确实为MoS2薄膜，厚度为多层。从光学显微镜的图片中可以看出，本工艺条件所得到的MoS2薄膜厚度均匀且质量好。The test results are shown in Figures 4 and 5, Figure 4 is a test result of a Raman spectrometer, and Figure 5 is a film observed by an optical microscope. The product obtained by the process conditions proposed by the present invention can be seen from the Raman spectrum. The two characteristics of MoS2 are Raman vibrations E12g and A1g, indicating that the product obtained by the process conditions is indeed a MoS2 film with a thickness of multiple layers. It can be seen from the picture of the optical microscope that the MoS2 film obtained by the process conditions has uniform thickness and good quality.
另外，本实施例中缓冲层的腐蚀过程只用了1分30秒，相对于传统的缓冲层腐蚀过程为2到3小时，大幅度减少了转移MoS2薄膜所需的时间。In addition, the etching process of the buffer layer in this embodiment takes only 1 minute and 30 seconds, and the etching process for the conventional buffer layer is 2 to 3 hours, which greatly reduces the time required for transferring the MoS2 film.
应当理解的是，本发明的应用不限于上述的举例，对本领域普通技术人员来说，可以根据上述说明加以改进或变换，所有这些改进和变换都应属于本发明所附权利要求的保护范围。 It is to be understood that the application of the present invention is not limited to the above-described examples, and those skilled in the art can make modifications and changes in accordance with the above description, all of which are within the scope of the appended claims.

Claims (9)

  1. 一种二硫化钼薄膜的制备方法，其特征在于，包括以下步骤： A method for preparing a molybdenum disulfide film, comprising the steps of:
    a、在硅衬底上镀上一层与二硫化钼晶格大小相匹配的氧化物缓冲层；a plating an oxide buffer layer matching the lattice size of the molybdenum disulfide on the silicon substrate;
    b、使用CVD法在其表面生长二硫化钼薄膜。b. A molybdenum disulfide film is grown on the surface thereof by a CVD method.
  2. 根据权利要求1所述的二硫化钼薄膜的制备方法，其特征在于，步骤a中采用脉冲激光沉积技术或是磁控溅射技术在硅衬底上镀上氧化物缓冲层。The method for preparing a molybdenum disulfide film according to claim 1, wherein in step a, an oxide buffer layer is coated on the silicon substrate by pulsed laser deposition or magnetron sputtering.
  3. 根据权利要求2所述的二硫化钼薄膜的制备方法，其特征在于，还包括以下步骤：The method according to claim 2, further comprising the steps of:
    c、将二硫化钼薄膜转移至其他衬底上。c. Transfer the molybdenum disulfide film to other substrates.
  4. 根据权利要求3所述的二硫化钼薄膜的制备方法，其特征在于，步骤c中转移的过程为通过稀酸腐蚀缓冲层，使二硫化钼薄膜脱离硅衬底，继而转移到其他衬底上。The method for preparing a molybdenum disulfide film according to claim 3, wherein the transferring in the step c is to pass the dilute acid etching buffer layer to remove the molybdenum disulfide film from the silicon substrate, and then transfer to other substrates. .
  5. 根据权利要求4所述的二硫化钼薄膜的制备方法，其特征在于，步骤c具体包括以下步骤：The method for preparing a molybdenum disulfide film according to claim 4, wherein the step c specifically comprises the following steps:
    在二硫化钼薄膜表面涂上一层聚甲基丙烯酸甲酯；Applying a layer of polymethyl methacrylate on the surface of the molybdenum disulfide film;
    烘干，聚甲基丙烯酸甲酯成膜；Drying, forming polymethyl methacrylate film;
    将带有二硫化钼薄膜的硅衬底浸泡于稀酸溶液中，直至氧化物缓冲层被腐蚀完毕，聚甲基丙烯酸甲酯薄膜浮起；Soaking a silicon substrate with a molybdenum disulfide film in a dilute acid solution until the oxide buffer layer is etched, and the polymethyl methacrylate film floats;
    用去离子水清洗薄膜，此时二硫化钼薄膜带着聚甲基丙烯酸甲酯薄膜脱离了硅衬底；The film is cleaned with deionized water, and the molybdenum disulfide film is separated from the silicon substrate by a polymethyl methacrylate film;
    将二硫化钼薄膜转移至其他衬底上；Transferring the molybdenum disulfide film to other substrates;
    烘干；drying;
    滴加聚甲基丙烯酸甲酯，软化聚甲基丙烯酸甲酯薄膜，并保持湿润，浸泡数分钟；Add polymethyl methacrylate dropwise, soften the polymethyl methacrylate film, keep it moist, soak for several minutes;
    用丙酮冲洗，洗去聚甲基丙烯酸甲酯。Rinse with acetone and wash away polymethyl methacrylate.
  6. 根据权利要求5所述的二硫化钼薄膜的制备方法，其特征在于，所述稀酸为稀盐酸、稀硫酸或是稀氢氟酸。The method for preparing a molybdenum disulfide film according to claim 5, wherein the dilute acid is dilute hydrochloric acid, dilute sulfuric acid or dilute hydrofluoric acid.
  7. 根据权利要求1~6任一所述的二硫化钼薄膜的制备方法，其特征在于，所述氧化物缓冲层为氧化锌缓冲层、氧化镁缓冲层或多元氧化物缓冲层。The method for preparing a molybdenum disulfide film according to any one of claims 1 to 6, wherein the oxide buffer layer is a zinc oxide buffer layer, a magnesium oxide buffer layer or a multi-oxide buffer layer.
  8. 根据权利要求1~6任一所述的二硫化钼薄膜的制备方法，其特征在于，所述氧化物缓冲层为氧化锌缓冲层。The method for producing a molybdenum disulfide film according to any one of claims 1 to 6, wherein the oxide buffer layer is a zinc oxide buffer layer.
  9. 一种二硫化钼薄膜，其特征在于，采用如权利要求1~8任一所述的二硫化钼薄膜的制备方法制备得到。A molybdenum disulfide film obtained by the method for producing a molybdenum disulfide film according to any one of claims 1 to 8.
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