CN108646793B - Device and method for controlling three-dimensional shape of two-dimensional material - Google Patents

Device and method for controlling three-dimensional shape of two-dimensional material Download PDF

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CN108646793B
CN108646793B CN201810295285.4A CN201810295285A CN108646793B CN 108646793 B CN108646793 B CN 108646793B CN 201810295285 A CN201810295285 A CN 201810295285A CN 108646793 B CN108646793 B CN 108646793B
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dimensional
current source
cavity
pid controller
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CN108646793A (en
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马一飞
元晋鹏
王梅
陈旭远
汪丽蓉
肖连团
贾锁堂
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Shanxi University
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    • GPHYSICS
    • G05CONTROLLING; REGULATING
    • G05DSYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
    • G05D5/00Control of dimensions of material
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/184Preparation
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00Compounds of molybdenum
    • C01G39/06Sulfides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G41/00Compounds of tungsten
    • GPHYSICS
    • G05CONTROLLING; REGULATING
    • G05BCONTROL OR REGULATING SYSTEMS IN GENERAL; FUNCTIONAL ELEMENTS OF SUCH SYSTEMS; MONITORING OR TESTING ARRANGEMENTS FOR SUCH SYSTEMS OR ELEMENTS
    • G05B11/00Automatic controllers
    • G05B11/01Automatic controllers electric
    • G05B11/36Automatic controllers electric with provision for obtaining particular characteristics, e.g. proportional, integral, differential
    • G05B11/42Automatic controllers electric with provision for obtaining particular characteristics, e.g. proportional, integral, differential for obtaining a characteristic which is both proportional and time-dependent, e.g. P.I., P.I.D.

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Abstract

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; the technical problem that the appearance structure is difficult to control in the three-dimensional process of the two-dimensional material at present is solved; the technical scheme is as follows: a two-dimensional material three-dimensional shape control device comprises an electromagnetic shielding cover, a cavity, a current source, a PID controller, a bias voltage substrate, a voltage source, a magnetic field meter and three pairs of magnetic coils, wherein the bias voltage substrate is arranged in the cavity; the invention is suitable for synthesizing three-dimensional two-dimensional materials with customized appearances, researching the growth mechanism of the two-dimensional materials and developing novel two-dimensional materials.

Description

Device and method for controlling three-dimensional shape of two-dimensional material
Technical Field
The invention discloses a device and a method for controlling the three-dimensional shape of a two-dimensional material, and belongs to the field of two-dimensional material synthesis.
Background
The three-dimension of the two-dimensional material not only maintains the intrinsic excellent properties of the two-dimensional material, but also has the advantages of enhanced mechanical properties, increased conductivity, increased effective specific surface area and the like brought by a three-dimensional structure. The synthesis of two-dimensional materials into three-dimensional macrostructures is one of the best ways to make full use of the characteristics of two-dimensional materials and put the two-dimensional materials into practical application. The three-dimensional structure of a two-dimensional material plays a crucial role for the application effect. For practical application, the artificial accurate controllable morphology is particularly important for improving the application effect of materials. At the present stage, the shape control method of the three-dimensional two-dimensional material is single and low in control force. The morphology of the material can only be finely adjusted by changing the conventional synthesis conditions such as temperature, time and the like in the synthesis process, resulting in poor controllability of the morphology. Therefore, a new device and a new method are needed, so that the three-dimensional shape of the two-dimensional material is artificially controllable, the shape structure of the three-dimensional two-dimensional material is optimized, and the application performance of the three-dimensional two-dimensional material is improved.
Disclosure of Invention
The invention provides a device and a method for controlling the three-dimensional shape of a two-dimensional material, which aim to solve the problem that the three-dimensional shape of the two-dimensional material is difficult to control at present.
In order to solve the technical problems, the invention adopts the technical scheme that: a two-dimensional material three-dimensional shape control device comprises an electromagnetic shielding cover, a cavity, a current source, a PID controller, a bias voltage substrate, a voltage source, a magnetic field meter and three pairs of magnetic coils, wherein the bias voltage substrate is arranged in the cavity, the three pairs of magnetic coils are arranged around the cavity, the magnetic force lines at the centers of the two magnetic coils in each pair of magnetic coils penetrate through the cavity, the electromagnetic shielding cover covers the three pairs of magnetic coils, the voltage source is connected with the bias voltage substrate, 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.
Further, the material used for the electromagnetic shielding case is permalloy.
Furthermore, the cavity is a quartz tube, and round holes which are in the same shape as the cross section of the quartz tube and are used for penetrating out of the quartz tube are arranged on two sides of the electromagnetic shielding cover.
Further, the PID controller comprises a first PID controller, a second PID controller and a third PID controller, the magnetic coils comprise a first magnetic coil pair, a second magnetic coil pair and a third magnetic coil pair, the current source comprises a first current source, a second current source and a third current source, the two magnetic coils in the first magnetic coil pair, the second magnetic coil pair and the third magnetic coil pair are oppositely arranged and are respectively positioned in the front, back, up, down and left and right of the cavity, 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, the second PID controller controls the second current source to adjust the magnetic field strength of the second magnetic coil pair according to the real-time reading of the magnetic field meter, and the third PID controller controls the third current source to adjust the magnetic field strength of the third magnetic coil pair according to the real-time reading of the magnetic field meter.
Further, the bias voltage substrate and the magnetic field meter are disposed within a coincidence of the first magnetic coil pair, the second magnetic coil pair, and the third magnetic coil pair that generate the magnetic field.
A control method for the three-dimensional shape of a two-dimensional material is completed based on the control device for the three-dimensional shape of the two-dimensional material, and comprises the following steps:
placing a target growth substrate on a bias voltage substrate, vacuumizing the cavity, heating the cavity to reach a preset reaction temperature, introducing ionized reactants, starting a current source control magnetic field, starting a voltage source control bias voltage field, and starting a growth process of a target growth material; and after the reaction is finished, reducing the temperature of the cavity to room temperature, introducing air, and taking out the target substrate of the target growth material for later use.
Further, the reaction temperature was 200-1700 ℃.
Further, at least one pair of magnetic coils or voltage sources is involved in the reaction.
Compared with the prior art, the invention has the following advantages:
1. the motion trail of active particles in the ionized reactant is directly and accurately controlled by regulating and controlling the parameters of the three-dimensional magnetic field and the substrate bias voltage field such as the direction, the size, the strength and the like in real time. The reaction position and direction of the active particles can be accurately controlled in the process of synthesizing the two-dimensional material, and finally the purpose of controlling the three-dimensional shape structure of the two-dimensional material is achieved.
2. The device and the method are suitable for three-dimensional growth of multiple two-dimensional materials such as graphene, molybdenum disulfide, tungsten disulfide and the like.
Drawings
Fig. 1 is an external structural diagram of an embodiment of the present invention.
Fig. 2 is a schematic diagram of an internal structure according to an embodiment of the present invention.
Fig. 3 is a schematic structural diagram of the interior of the cavity in the embodiment of the present invention.
Fig. 4 is a schematic diagram of a three-dimensional embodiment of two-dimensional graphene in the method of the present invention.
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 controller, 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.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
Examples
As shown in fig. 1 to 3, a two-dimensional material three-dimensional topography control device comprises an electromagnetic shield 1, a cavity 2, a bias voltage substrate 12, a voltage source 13, a magnetic field meter, a first PID controller 4, a second PID controller 5, a third PID controller 7, a first magnetic coil pair 9, a second magnetic coil pair 10, a third magnetic coil pair 11, a first current source 3, a second current source 6 and a third current source 8. The electromagnetic shield 1 covers three pairs of magnetic coils, a voltage source 13 is connected to a bias voltage substrate 12, and a magnetometer is connected to all PID controllers. The material used for the electromagnetic shielding case 1 is permalloy. The cavity 2 is a quartz tube, and round holes which are in the same shape as the cross section of the quartz tube and are used for the quartz tube to penetrate out are arranged on two sides of the electromagnetic shielding cover 1. A bias substrate 12 is disposed in the chamber 2, and the bias substrate 12 and the magnetic field meter are disposed in the overlapped portions of the magnetic fields generated by the first magnetic coil pair 9, the second magnetic coil pair 10, and the third magnetic coil pair 11.
The first magnetic coil pair 9, the second magnetic coil pair 10 and the third magnetic coil pair 11 are oppositely arranged and are respectively positioned at the front, back, up, down and left and right of the cavity 2, the first PID controller 4 controls the first current source 3 to adjust the magnetic field intensity of the first magnetic coil pair 9 according to the real-time reading of the magnetometer, the second PID controller 5 controls the second current source 6 to adjust the magnetic field intensity of the second magnetic coil pair 10 according to the real-time reading of the magnetometer, and the third PID controller 7 controls the third current source 8 to adjust the magnetic field intensity of the third magnetic coil pair 11 according to the real-time reading of the magnetometer.
The working process of the invention is as follows: feeding a material growth target substrate into the cavity 2, placing the material growth target substrate on a bias voltage substrate 12, starting equipment for heating, and introducing ionized reactants; when the experimental conditions reach the growth temperature, then according to the experimental design, the magnetic field and the electric field near the substrate are used for controlling the active particles in the ionized reactant through the magnetic field and the electric field, and finally the material with the target morphology is obtained.
In specific implementation, the experimental parameters in table 1 are used to synthesize the two-dimensional graphene into a special vertical three-dimensional structure, which includes the following steps:
a. quartz is taken as a target substrate, and the quartz is arranged on a bias voltage substrate 12 after being cleaned;
b. the temperature of the cavity is heated to 850 ℃;
b. introducing ionized acetylene and hydrogen;
e. the current of the horizontal magnetic field was set to 15 mA, the current of the vertical magnetic field was set to 20 mA, the substrate bias voltage was set to 10V, and then the material was synthesized for 30 min.
f. The horizontal magnetic field, the vertical magnetic field and the substrate bias voltage are used for controlling the motion behavior of active particles in the ionized reactant, so that the two-dimensional graphene is three-dimensionally arranged, as shown in fig. 4.
TABLE 1 Experimental parameters
Figure 2148DEST_PATH_IMAGE002
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it will be understood by those of ordinary skill in the art that various changes in form and details may be made therein without departing from the spirit and scope of the present invention as defined by the following claims.

Claims (7)

1. A two-dimensional material three-dimensional appearance controlling means which characterized in that: the electromagnetic shielding device comprises an electromagnetic shielding cover (1), a cavity (2), a current source, a PID controller, a bias voltage substrate (12), a voltage source (13), a magnetic field meter and three pairs of magnetic coils, wherein the bias voltage substrate (12) is arranged in the cavity (2), the three pairs of magnetic coils are arranged around the cavity (2), magnetic lines of force of centers of two magnetic coils in each pair of magnetic coils penetrate through the cavity (2), the electromagnetic shielding cover (1) covers the three pairs of magnetic coils, the voltage source (13) is connected with the bias voltage substrate (12), 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;
the PID controller comprises a first PID controller (4), a second PID controller (5) and a third PID controller (7), the magnetic coils comprise a first magnetic coil pair (9), a second magnetic coil pair (10) and a third magnetic coil pair (11), the current sources comprise a first current source (3), a second current source (6) and a third current source (8), two respective magnetic coils in the first magnetic coil pair (9), the second magnetic coil pair (10) and the third magnetic coil pair (11) are oppositely arranged and are respectively positioned at the front, back, upper, lower and left and right of the cavity (2), the first PID controller (4) controls the first current source (3) to adjust the magnetic field intensity of the first magnetic coil pair (9) according to the real-time reading of the magnetometer, and the second PID controller (5) controls the second current source (6) to adjust the magnetic field intensity of the second magnetic coil pair (10) according to the real-time reading of the magnetometer, the third PID controller (7) controls the third current source (8) to adjust the magnetic field strength of the third magnetic coil pair (11) according to the real-time reading of the magnetic field meter.
2. The three-dimensional shape control device for the two-dimensional material as recited in claim 1, wherein the electromagnetic shielding case (1) is made of permalloy.
3. The device for controlling the three-dimensional shape of the two-dimensional material according to claim 1, wherein the cavity (2) is a quartz tube, and round holes which are in the same shape as the cross section of the quartz tube and are used for the quartz tube to penetrate through are arranged on two sides of the electromagnetic shielding cover (1).
4. The apparatus for controlling the three-dimensional profile of a two-dimensional material according to claim 1, wherein said bias substrate (12) and said magnetometer are disposed in the overlapping portion of the magnetic fields generated by said first pair of magnetic coils (9), said second pair of magnetic coils (10), and said third pair of magnetic coils (11).
5. A method for controlling the three-dimensional shape of a two-dimensional material is characterized by comprising the following steps: the device for controlling the three-dimensional shape of the two-dimensional material is completed based on any one of claims 1 to 4 and comprises the following steps:
placing a target growth substrate on a bias voltage substrate (12), vacuumizing the cavity (2), heating the cavity (2) to reach a preset reaction temperature, introducing ionized reactants, starting a current source to control a magnetic field, starting a voltage source to control a bias voltage field, and starting a growth process of a target growth material; and after the reaction is finished, reducing the temperature of the cavity to room temperature, introducing air, and taking out the target substrate of the target growth material for later use.
6. The method for controlling the three-dimensional shape of the two-dimensional material according to claim 5, wherein: the reaction temperature is 200-1700 ℃.
7. The method for controlling the three-dimensional shape of the two-dimensional material according to claim 5, wherein: during the reaction, at least one pair of magnetic coils or voltage sources is involved.
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