CN108646793B - Device and method for controlling three-dimensional shape of two-dimensional material - Google Patents
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- 229910000889 permalloy Inorganic materials 0.000 claims description 3
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Abstract
本发明一种二维材料三维化形貌控制的装置及方法,属于二维材料合成领域;解决了目前二维材料三维化过程中形貌结构难以控制的技术难题;技术方案为:一种二维材料三维化形貌控制装置,包括电磁屏蔽罩、腔体、电流源、PID控制器、偏电压基底、电压源、磁场计和三对磁线圈,偏电压基底设置在腔体内,在腔体的四周设置有三对磁线圈,每对磁线圈中的两个磁线圈的中心的磁力线贯穿腔体,电磁屏蔽罩覆盖三对磁线圈,电压源与偏电压基底相连,磁场计与PID控制器相连,PID控制器与电流源相连,电流源与每对磁线圈相连;本发明适用于合成定制形貌的三维化二维材料、研究二维材料生长机理以及开发新型二维材料。
The invention relates to a device and method for controlling the three-dimensional shape of two-dimensional materials, belonging to the field of two-dimensional material synthesis; it solves the technical problem that the topography and structure are difficult to control in the current three-dimensional process of two-dimensional materials; the technical scheme is as follows: a two-dimensional material A three-dimensional topography control device for three-dimensional materials, including an electromagnetic shield, a cavity, a current source, a PID controller, a bias voltage base, a voltage source, a magnetometer and three pairs of magnetic coils. Three pairs of magnetic coils are arranged around the magnetic coil, the magnetic field lines in the center of the two magnetic coils in each pair of magnetic coils run through the cavity, the electromagnetic shield covers the three pairs of magnetic coils, the voltage source is connected to the bias voltage base, and the magnetic field meter is connected to the PID controller. The PID controller is connected with the current source, and the current source is connected with each pair of magnetic coils; the invention is suitable for synthesizing three-dimensional two-dimensional materials with customized morphology, studying the growth mechanism of two-dimensional materials and developing new two-dimensional materials.
Description
技术领域technical field
本发明一种二维材料三维化形貌控制装置及方法,属于二维材料合成领域。The invention relates to a device and a method for controlling the three-dimensional shape of a two-dimensional material, belonging to the field of two-dimensional material synthesis.
背景技术Background technique
二维材料三维化不仅保持了二维材料本征的优异性质,还获得了三维结构带来的机械特性增强、导电性增加、有效比表面积增大等优点。将二维材料合成为三维宏观结构是充分利用二维材料特性,并将其投入实际应用的最佳途径之一。二维材料的三维结构对应用效果起着至关重要的作用。对于实际应用,形貌人为精确可控对于提升材料应用效果尤为重要。目前阶段,三维化的二维材料形貌控制方法单一且控制力低。仅能通过改变合成过程中的温度、时间等常规合成条件来微调材料形貌,导致形貌可控性差。因此需要一种新装置和方法,使得二维材料三维化形貌人为可控,优化三维化二维材料形貌结构,提升三维化二维材料应用性能。The three-dimensionalization of two-dimensional materials not only maintains the inherent excellent properties of two-dimensional materials, but also obtains the advantages of enhanced mechanical properties, increased electrical conductivity, and increased effective specific surface area brought by the three-dimensional structure. Synthesizing 2D materials into 3D macrostructures is one of the best ways to fully exploit the properties of 2D materials and put them into practical applications. The three-dimensional structure of two-dimensional materials plays a crucial role in the application effect. For practical applications, the artificially precise and controllable morphology is particularly important for improving the application effect of materials. At present, the three-dimensional shape control method of two-dimensional materials is single and the control force is low. The material morphology can only be fine-tuned by changing the conventional synthesis conditions such as temperature and time during the synthesis process, resulting in poor controllability of the morphology. Therefore, a new device and method are needed to make the three-dimensional morphology of two-dimensional materials artificially controllable, optimize the morphology and structure of three-dimensional two-dimensional materials, and improve the application performance of three-dimensional two-dimensional materials.
发明内容SUMMARY OF THE INVENTION
本发明为解决目前二维材料三维化形貌难以控制的问题,提供一种二维材料三维化形貌控制装置及方法。The present invention provides a device and method for controlling the three-dimensional topography of two-dimensional materials in order to solve the problem that the three-dimensional topography of two-dimensional materials is difficult to control at present.
为了解决上述技术问题,本发明采用的技术方案为:一种二维材料三维化形貌控制装置,包括电磁屏蔽罩、腔体、电流源、PID控制器、偏电压基底、电压源、磁场计和三对磁线圈,偏电压基底设置在腔体内,在腔体的四周设置有三对磁线圈,每对磁线圈中的两个磁线圈的中心的磁力线贯穿腔体,电磁屏蔽罩覆盖三对磁线圈,电压源与偏电压基底相连,磁场计与PID控制器相连,PID控制器与电流源相连,电流源与每对磁线圈相连。In order to solve the above technical problems, the technical solution adopted in the present invention is: a three-dimensional shape control device for two-dimensional materials, including an electromagnetic shield, a cavity, a current source, a PID controller, a bias voltage base, a voltage source, and a magnetic field meter. And three pairs of magnetic coils, the bias voltage base is set in the cavity, three pairs of magnetic coils are set around the cavity, the magnetic lines of force in the centers of the two magnetic coils in each pair of magnetic coils run through the cavity, and the electromagnetic shield covers the three pairs of magnetic coils. The coil, the voltage source is connected with the bias voltage base, the magnetic field meter is connected with the PID controller, the PID controller is connected with the current source, and the current source is connected with each pair of magnetic coils.
进一步,所述电磁屏蔽罩所用的材料为坡莫合金。Further, the material used for the electromagnetic shielding cover is permalloy.
进一步,所述腔体为石英管,所述电磁屏蔽罩的两侧设置有与石英管截面同形的用于石英管穿出的圆孔。Further, the cavity is a quartz tube, and two sides of the electromagnetic shielding cover are provided with circular holes having the same shape as the section of the quartz tube for passing through the quartz tube.
进一步,所述PID控制器包括第一PID控制器、第二PID控制器和第三PID控制器,所述磁线圈包括第一磁线圈对、第二磁线圈对和第三磁线圈对,所述电流源包括第一电流源、第二电流源和第三电流源,第一磁线圈对、第二磁线圈对和第三磁线圈对中各自的两个磁线圈相对设置,分别位于所述腔体的前后、上下和左右,第一PID控制器根据磁场计的实时读数控制第一电流源调节第一磁线圈对的磁场强度,第二PID控制器根据磁场计的实时读数控制第二电流源调节第二磁线圈对的磁场强度,第三PID控制器根据磁场计的实时读数控制第三电流源调节第三磁线圈对的磁场强度。Further, the PID controller includes a first PID controller, a second PID controller and a third PID controller, and the magnetic coil includes a first magnetic coil pair, a second magnetic coil pair and a third magnetic coil pair, so The current source includes a first current source, a second current source, and a third current source, and the respective two magnetic coils in the first magnetic coil pair, the second magnetic coil pair, and the third magnetic coil pair are arranged opposite each other, and are respectively located in the The first PID controller controls the first current source to adjust the magnetic field strength of the first magnetic coil pair according to the real-time reading of the magnetic field meter, and the second PID controller controls the second current according to the real-time reading of the magnetic field meter. The source regulates the magnetic field strength of the second magnetic coil pair, and the third PID controller controls the third current source to regulate the magnetic field strength of the third magnetic coil pair according to the real-time reading of the magnetic field meter.
进一步,所述偏电压基底和所述磁场计设置在所述第一磁线圈对、所述第二磁线圈对和所述第三磁线圈对产生磁场的重合部分内。Further, the bias voltage base and the magnetometer are disposed in the overlapping portion where the first magnetic coil pair, the second magnetic coil pair and the third magnetic coil pair generate magnetic fields.
一种二维材料三维化形貌控制方法,基于上述的一种二维材料三维化形貌控制装置完成,包括以下步骤:A method for controlling the three-dimensional shape of a two-dimensional material is completed based on the above-mentioned device for controlling the three-dimensional shape of a two-dimensional material, and includes the following steps:
目标生长基底置于偏电压基底之上,对腔体抽真空,加热腔体达到预定的反应温度之后,通入电离后的反应物,开启电流源控制磁场,开启电压源控制偏电压场,开始目标生长材料的生长过程;反应结束之后,降低腔体温度至室温,通入空气,取出目标生长材料后的目标基底备用。The target growth substrate is placed on the bias voltage substrate, the chamber is evacuated, and after the heating chamber reaches the predetermined reaction temperature, the ionized reactants are introduced, the current source is turned on to control the magnetic field, the voltage source is turned on to control the bias voltage field, and the process starts. The growth process of the target growth material; after the reaction is completed, the temperature of the cavity is lowered to room temperature, air is introduced, and the target substrate after the target growth material is taken out for use.
进一步,反应温度为200-1700℃。Further, the reaction temperature is 200-1700°C.
进一步,反应过程中,至少有一对磁线圈或电压源参与工作。Further, during the reaction, at least one pair of magnetic coils or voltage sources participates in the work.
本发明与现有技术相比,具有以下优势:Compared with the prior art, the present invention has the following advantages:
1.通过对三维磁场和基底偏电压场的方向、大小、强度等参数实时调控,实现对电离后的反应物中活性粒子运动轨迹直接、精确的控制。使得活性粒子在合成二维材料过程时的反应位置、方向可以被精确操控,最终达到达到控制二维材料三维化形貌结构的目的。1. Through real-time adjustment of the direction, size, intensity and other parameters of the three-dimensional magnetic field and the substrate bias voltage field, the direct and precise control of the active particle movement trajectory in the ionized reactant is realized. The reaction position and direction of active particles in the process of synthesizing two-dimensional materials can be precisely controlled, and finally the purpose of controlling the three-dimensional morphology and structure of two-dimensional materials is achieved.
2.本发明装置和方法适用于石墨烯、二硫化钼、二硫化钨等多种二维材料三维化的生长。2. The device and method of the present invention are suitable for the three-dimensional growth of various two-dimensional materials such as graphene, molybdenum disulfide, and tungsten disulfide.
附图说明Description of drawings
图1为本发明实施例的外部结构示意图。FIG. 1 is a schematic diagram of an external structure of an embodiment of the present invention.
图2为本发明实施例的内部结构示意图。FIG. 2 is a schematic diagram of an internal structure of an embodiment of the present invention.
图3为本发明实施例中腔体内部的结构示意图。FIG. 3 is a schematic structural diagram of the interior of the cavity in the embodiment of the present invention.
图4为本发明方法中二维石墨烯三维化实施例示意图。4 is a schematic diagram of an embodiment of three-dimensionalization of two-dimensional graphene in the method of the present invention.
图中,1-电磁屏蔽罩,2-腔体,3-第一电流源,4-第一PID控制器,5-第二PID控制器,6-第二电流源,7-第三PID控制器,8-第三电流源,9-第一磁线圈对,10-第二磁线圈对,11-第三磁线圈对,12-偏电压基底,13-电压源。In the figure, 1-electromagnetic shield, 2-cavity, 3-first current source, 4-first PID controller, 5-second PID controller, 6-second current source, 7-third PID control device, 8-third current source, 9-first magnetic coil pair, 10-second magnetic coil pair, 11-third magnetic coil pair, 12-bias voltage base, 13-voltage source.
具体实施方式Detailed ways
下面结合附图对本发明做进一步的说明。The present invention will be further described below in conjunction with the accompanying drawings.
实施例Example
如图1至图3所示,一种二维材料三维化形貌控制装置,包括电磁屏蔽罩1、腔体2、偏电压基底12、电压源13、磁场计、第一PID控制器4、第二PID控制器5、第三PID控制器7、第一磁线圈对9、第二磁线圈对10、第三磁线圈对11、第一电流源3、第二电流源6和第三电流源8。电磁屏蔽罩1覆盖三对磁线圈,电压源13与偏电压基底12相连,磁场计与所有PID控制器相连。电磁屏蔽罩1所用的材料为坡莫合金。腔体2为石英管,电磁屏蔽罩1的两侧设置有与石英管截面同形的用于石英管穿出的圆孔。偏电压基底12设置在腔体2内,偏电压基底12和磁场计设置在第一磁线圈对9、第二磁线圈对10和第三磁线圈对11产生磁场的重合部分内。As shown in FIG. 1 to FIG. 3 , a three-dimensional topography control device for two-dimensional materials includes an
第一磁线圈对9、第二磁线圈对10和第三磁线圈对11中各自的两个磁线圈相对设置,分别位于腔体2的前后、上下和左右,第一PID控制器4根据磁场计的实时读数控制第一电流源3调节第一磁线圈对9的磁场强度,第二PID控制器5根据磁场计的实时读数控制第二电流源6调节第二磁线圈对10的磁场强度,第三PID控制器7根据磁场计的实时读数控制第三电流源8调节第三磁线圈对11的磁场强度。The respective two magnetic coils in the first
本发明的工作过程为:将材料生长目标基底送进腔体2,并置于偏电压基底12之上,开启设备加热,通入电离后的反应物;当实验条件达到生长温度的时候,然后根据实验设计,对基底附近的磁场,电场,通过磁场、电场来控制电离后反应物中的活性粒子,最终获得目标形貌的材料。The working process of the present invention is as follows: the material growth target substrate is sent into the
具体实施中,使用表1的实验参数,将二维石墨烯合成特殊竖直的三维结构,分为以下几个步骤:In the specific implementation, using the experimental parameters in Table 1, two-dimensional graphene is synthesized into a special vertical three-dimensional structure, which is divided into the following steps:
a.以石英为目标基底,清理后置于偏电压基底12之上;a. Take quartz as the target substrate, and place it on the
b.腔体温度加热至850 ℃;b. The cavity temperature is heated to 850 ℃;
b.通入电离后的乙炔、氢气;b. Introduce ionized acetylene and hydrogen;
e.将水平磁场的电流设为15 mA,垂直磁场电流 20 mA,基底偏电压设为10V,然后合成材料30 min。e. Set the current of the horizontal magnetic field to 15 mA, the current of the vertical magnetic field to 20 mA, and the substrate bias voltage to 10 V, and then synthesize the material for 30 min.
f.利用水平磁场、垂直磁场和基底偏电压控制电离后反应物中的活性粒子运动行为,从而将二维石墨烯三维化,如图4所示。f. Using the horizontal magnetic field, the vertical magnetic field and the substrate bias voltage to control the motion behavior of active particles in the reactants after ionization, so that the two-dimensional graphene can be three-dimensionalized, as shown in Figure 4.
表1 实验参数Table 1 Experimental parameters
尽管已经参照其示例性实施例具体显示和描述了本发明,但是本领域的技术人员应该理解,在不脱离权利要求所限定的本发明的精神和范围的情况下,可以对其进行形式和细节上的各种改变。Although the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it will be understood by those skilled in the art that form and detail may be made therein without departing from the spirit and scope of the invention as defined in the claims various changes on.
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