WO2019184747A1 - 一种双气流生长二维材料反应室设备 - Google Patents

一种双气流生长二维材料反应室设备 Download PDF

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Publication number
WO2019184747A1
WO2019184747A1 PCT/CN2019/078524 CN2019078524W WO2019184747A1 WO 2019184747 A1 WO2019184747 A1 WO 2019184747A1 CN 2019078524 W CN2019078524 W CN 2019078524W WO 2019184747 A1 WO2019184747 A1 WO 2019184747A1
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dimensional material
growth
reaction chamber
gasflow
tube
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PCT/CN2019/078524
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English (en)
French (fr)
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段曦东
段镶锋
张正伟
马惠芳
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湖南大学
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Priority to JP2020600082U priority Critical patent/JP3231327U/ja
Publication of WO2019184747A1 publication Critical patent/WO2019184747A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/08—Reaction chambers; Selection of materials therefor
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/14—Feed and outlet means for the gases; Modifying the flow of the reactive gases

Definitions

  • the invention relates to the technical field of growing two-dimensional materials, in particular to a two-flow growth two-dimensional material reaction chamber device.
  • Two-dimensional materials have developed rapidly in recent years due to their excellent performance in optics, electricity, magnetism, and catalysis.
  • synthetic methods for two-dimensional materials such as micro-mechanical stripping, liquid-phase ultrasonic stripping, liquid phase intercalation, laser and annealing layer-by-layer thinning, and vapor deposition.
  • the vapor deposition method is the most widely used, which not only overcomes the problem that the size of the micro-mechanical stripping is too small, but also overcomes the shortcomings of the liquid-layer ultrasonic stripping method, which is difficult to obtain a single-layer nanosheet, and the liquid-phase ultrasonic stripping method takes a long time to prepare. Problems, etc.
  • the object of the present invention is to provide a two-flow growth two-dimensional material reaction chamber device, so as to effectively solve the disadvantages of premature aging of the growing two-dimensional material nucleation point or unsuitable control of growth time, thereby growing large A high quality single crystal of uniform size and shape.
  • a two-flow growth two-dimensional material reaction chamber apparatus comprising a furnace and a reaction tube disposed in the furnace, the reaction tube being connected with a conveying pipe and a flange at both ends thereof, An intake pipe and an air outlet pipe are connected to the flange.
  • reaction tube is a quartz tube or a corundum tube.
  • a reaction chamber is formed in the reaction tube, and a first porcelain boat containing a reactant and a second porcelain boat containing a silicon wafer are disposed in the reaction chamber.
  • the conveying pipe has an outer diameter of 1 mm to 600 mm and a wall thickness of 0.5 mm to 100 mm.
  • an intake valve and an air outlet valve are respectively disposed on the intake pipe and the air outlet pipe.
  • the invention has the beneficial effects that the two-flow growth two-dimensional material reaction chamber device of the invention realizes the double air flow at both ends of the reaction tube by connecting the conveying pipe and the flange in the reaction tube and connecting the intake pipe and the outlet pipe through the flange.
  • Control instead of the traditional one-way airflow control, can better control the generation time and growth time of the nucleation point of the two-dimensional material, effectively solving the premature nucleation point or uncontrollable growth time when producing two-dimensional materials. Disadvantages, thereby growing high-quality single crystals of large size, regular shape, and uniform thickness distribution.
  • the invention can achieve the effect of high efficiency and labor saving, improve the experimental efficiency, ensure the size, shape and quality of the growing two-dimensional material, and is fully applicable to the tubular furnace to control the growth of the two-dimensional material. Therefore, the dual-flow growth two-dimensional material reaction chamber equipment replaces the traditional one-way airflow, which will inevitably generate more market space and has strong practicability.
  • Figure 1 is a schematic view of the structure of the present invention.
  • the present invention provides a two-flow growth two-dimensional material reaction chamber apparatus comprising a furnace 1, a reaction tube 2 and a delivery conduit 3, the reaction tube setting In the furnace, the reaction tube is a quartz tube or a corundum tube, and a reaction chamber is formed in the reaction tube.
  • the conveying tube is arranged at two ends of the reaction tube, and the outer diameter of the conveying tube is 1 mm-600 mm, and the wall thickness is 0.5 mm-100 mm.
  • each end of the conveying pipe is provided with a flange 4, and each flange is connected with an intake pipe 5 and an air outlet pipe 6, respectively, and the air inlet pipe and the air outlet pipe respectively
  • An intake valve 9 and an outlet valve 10 are provided, and intake and exhaust can be realized through the intake pipe and the outlet pipe.
  • the two-dimensional material reaction chamber device of the structure replaces the traditional one-way airflow by connecting the conveying pipe and the flange in the reaction pipe and connecting the intake pipe and the outlet pipe through the flange, thereby realizing double air flow control at both ends of the reaction pipe.
  • Control can better control the generation time and growth time of the nucleation point of the two-dimensional material, effectively solve the shortcomings of premature nucleation point or unsuitable control of growth time when producing two-dimensional materials, thereby growing large size and shape Regular, high quality single crystal with uniform thickness distribution.
  • the invention can achieve the effect of high efficiency and labor saving, improve the experimental efficiency, ensure the size, shape and quality of the growing two-dimensional material, and is fully applicable to the tubular furnace to control the growth of the two-dimensional material. Therefore, the dual-flow growth two-dimensional material reaction chamber equipment replaces the traditional one-way airflow, which will inevitably generate more market space and has strong practicability.
  • the flanges at each end are respectively provided with an intake pipe and an air outlet pipe, and are placed in the central constant temperature zone before the experiment.
  • a first porcelain boat 7 or an alumina boat containing an appropriate amount of reaction raw materials, and a second porcelain boat 8 or an alumina boat containing a suitable size silicon wafer is placed in the downstream variable temperature zone, and the reaction raw materials are Se powder, S powder, and Te powder.
  • the thickness of raw materials is 0.7-100nm
  • the types are powders, particles, gases, metal wires and other materials that can be grown
  • the raw materials of various forms are then fitted with flanges, then the appropriate carrier gas is introduced to exhaust the oxygen in the reaction chamber, and finally an appropriate amount of flow is introduced to heat the reaction chamber for reaction.
  • the final two-dimensional nanomaterials are nanosheets, nanofilms, superlattices, and nanobelts.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

本发明公开了一种双气流生长二维材料反应室设备，包括火炉以及设在火炉内的反应管，所述反应管两端均连接有输送管道和法兰，所述法兰上连接有进气管和出气管。该结构的二维材料反应室设备，通过两端双气流控制代替单向气流控制，能够更好的控制二维材料成核点的产生时间以及生长时间，有效的解决了生产二维材料时成核点产生过早或者生长时间不宜控制的缺点，从而生长出大尺寸，形状规则，厚度分布均匀的高质量单晶。总之，本发明能够起到高效，节约人工成本的效果，同时提高了实验效率，保证了生长二维材料的尺寸、形状和质量，完全适用于管式炉控制生长二维材料。

Description

一种双气流生长二维材料反应室设备 技术领域
本发明涉及生长二维材料技术领域，具体涉及一种双气流生长二维材料反应室设备。
 背景技术
长久以来，人们一直认为二维晶体不可能单独稳定存在。然而，2004 年英国曼彻斯特大学物理学家 Andre Geim 和 Konstantin Novoselov 用实验证实，以石墨这种层状材料为原料，通过简单的物理剥离方法便能得到碳的单原子薄片—石墨烯，从而开启了材料科学革命的新篇章。自此，以石墨烯为代表的二维层状材料的相关研究获得了迅猛的发展。比如，MoS 2，MoSe 2，WS 2，WSe 2。
由于在光学，电学，磁学，催化等方面的优异性能，二维材料近年来得到迅猛的发展。目前，二维材料的合成方法也很多，主要有微机械剥离法、液相超声剥离法、液相插层法、激光法和退火逐层变薄法、气相沉积法。其中气相沉积法应用最为广泛，它不仅克服了微机械剥离的尺寸太小的问题，也克服了液相超声剥离法不易得到单层纳米片的缺点，还有液相超声剥离法制备时间较长的问题等。但是利用气相沉积可控合成高质量的大尺寸的单晶二维纳米材料还一直是一个挑战。其中CVD和PVD的合成方法被广泛使用，在该方法中，气流是影响二维材料的生长的重要原因之一，这对用于控制气流来提高二维材料的质量提出了更为严格的挑战。
目前绝大多数企业采用的是单向气流来生长二维材料。在单向气流中，很难精确控制生产二维材料时成核点产生的时间或者生长时间不宜控制，从而严重影响材料的形状、尺寸和质量。
 技术问题
有鉴于此，本发明的目的是提供一种双气流生长二维材料反应室设备，以便有效的解决现有生长二维材料成核点产生过早或者生长时间不宜控制的缺点，从而生长出大尺寸，形状规则，分布均匀的高质量单晶。
 技术解决方案
本发明通过以下技术手段解决上述问题：一种双气流生长二维材料反应室设备，包括火炉以及设在火炉内的反应管，所述反应管两端均连接有输送管道和法兰，所述法兰上连接有进气管和出气管。
进一步，所述反应管为石英管或刚玉管。
进一步，所述反应管内形成反应腔，所述反应腔内设置有盛有反应物的第一瓷舟以及盛有硅片的第二瓷舟。
进一步，所述输送管道的外径为1mm-600mm，壁厚为0.5mm-100mm。
进一步，所述进气管和出气管上分别设置有进气阀门和出气阀门。
 有益效果
本发明的有益效果：本发明的双气流生长二维材料反应室设备，通过在反应管连通连接输送管道和法兰，并通过法兰连接进气管和出气管，从而实现反应管两端双气流控制，取代了传统的单向气流控制，能够更好的控制二维材料成核点的产生时间以及生长时间，有效的解决了生产二维材料时成核点产生过早或者生长时间不宜控制的缺点，从而生长出大尺寸，形状规则，厚度分布均匀的高质量单晶。总之，本发明能够起到高效，节约人工成本的效果，同时提高了实验效率，保证了生长二维材料的尺寸、形状和质量，完全适用于管式炉控制生长二维材料。因此，此种双气流生长二维材料反应室设备取代了传统的单向气流，必将会产生更大的市场空间，具有很强的实用性。
 附图说明
下面结合附图和实施例对本发明作进一步描述。
图1为本发明的结构示意图。
 本发明的实施方式
以下将结合附图对本发明进行详细说明，如图1所示：本发明提供了一种双气流生长二维材料反应室设备，包括火炉1、反应管2和输送管道3，所述反应管设置在火炉内，反应管为石英管或刚玉管，反应管内形成反应腔，所述输送管道布置在反应管的两端，述输送管道的外径为1mm-600mm，壁厚为0.5mm-100mm，以及其它可能应用的外径和壁厚，每根输送管道的端部均设置有法兰4，每个法兰上均连接有进气管5和出气管6，所述进气管和出气管上分别设置有进气阀门9和出气阀门10，通过进气管和出气管可实现进气和出气。该结构的二维材料反应室设备，通过在反应管连通连接输送管道和法兰，并通过法兰连接进气管和出气管，从而实现反应管两端双气流控制，取代了传统的单向气流控制，能够更好的控制二维材料成核点的产生时间以及生长时间，有效的解决了生产二维材料时成核点产生过早或者生长时间不宜控制的缺点，从而生长出大尺寸，形状规则，厚度分布均匀的高质量单晶。总之，本发明能够起到高效，节约人工成本的效果，同时提高了实验效率，保证了生长二维材料的尺寸、形状和质量，完全适用于管式炉控制生长二维材料。因此，此种双气流生长二维材料反应室设备取代了传统的单向气流，必将会产生更大的市场空间，具有很强的实用性。为使上述技术方案更加清楚，下面详细介绍采用该设备生长二维材料的具体步骤：在生长二维材料时，每端的法兰各装有进气管和出气管，实验前在中心恒温区放入盛有适量反应原材料的第一瓷舟7或氧化铝舟，在下游变温区放入盛有大小合适硅片的第二瓷舟8或氧化铝舟，反应原材料为Se粉、S粉、Te粉，氯化钒，WS 2，WSe 2，MoS 2，MoSe 2等过渡金属和化合物和可能应用的其他材料，原材料厚度为0.7-100nm，种类有粉末、颗粒、气体、金属线以及其他可以生长材料的各种形态的原材料，接着装上法兰，然后通入合适的载气排尽反应室的氧气，最后通入适量的流量，加热反应室进行反应。最终生长的二维纳米材料种类为纳米片、纳米薄膜、超晶格、纳米带。
最后说明的是，以上实施例仅用以说明本发明的技术方案而非限制，尽管参照较佳实施例对本发明进行了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的宗旨和范围，其均应涵盖在本发明的权利要求范围当中。

Claims (5)

  1. 一种双气流生长二维材料反应室设备，包括火炉以及设在火炉内的反应管，其特征在于：所述反应管两端均连接有输送管道和法兰，所述法兰上连接有进气管和出气管。
  2. 根据权利要求1所述的双气流生长二维材料反应室设备，其特征在于：所述反应管为石英管或刚玉管。
  3. 根据权利要求2所述的双气流生长二维材料反应室设备，其特征在于：所述反应管内形成反应腔，所述反应腔内设置有盛有反应物的第一瓷舟以及盛有硅片的第二瓷舟。
  4. 根据权利要求1所述的双气流生长二维材料反应室设备，其特征在于：所述输送管道的外径为1mm-600mm，壁厚为0.5mm-100mm。
  5. 根据权利要求1所述的双气流生长二维材料反应室设备，其特征在于：所述进气管和出气管上分别设置有进气阀门和出气阀门。
PCT/CN2019/078524 2018-03-26 2019-03-18 一种双气流生长二维材料反应室设备 WO2019184747A1 (zh)

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Publication number Priority date Publication date Assignee Title
CN208038590U (zh) * 2018-03-26 2018-11-02 湖南大学 一种双气流生长二维材料反应室设备
CN109809372B (zh) * 2019-03-26 2022-05-03 湘潭大学 一种基于空间限域策略制备单层二硒化钨纳米带的方法

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US4193835A (en) * 1976-10-13 1980-03-18 Matsushita Electric Industrial Co., Ltd. Method for growing semiconductor crystal
CN206385275U (zh) * 2017-01-09 2017-08-08 中国科学院物理研究所 二维材料范德瓦尔斯外延生长与修饰系统
CN107039285A (zh) * 2017-04-06 2017-08-11 湖南大学 一种二维材料横向异质结、制备及其应用
CN107287653A (zh) * 2017-03-14 2017-10-24 湖南大学 一种碘化镉二维材料及其制备方法
CN208038590U (zh) * 2018-03-26 2018-11-02 湖南大学 一种双气流生长二维材料反应室设备

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US4193835A (en) * 1976-10-13 1980-03-18 Matsushita Electric Industrial Co., Ltd. Method for growing semiconductor crystal
CN206385275U (zh) * 2017-01-09 2017-08-08 中国科学院物理研究所 二维材料范德瓦尔斯外延生长与修饰系统
CN107287653A (zh) * 2017-03-14 2017-10-24 湖南大学 一种碘化镉二维材料及其制备方法
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CN208038590U (zh) * 2018-03-26 2018-11-02 湖南大学 一种双气流生长二维材料反应室设备

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