CN113782978A - Preparation method of electromagnetic metamaterial based on graphene - Google Patents

Preparation method of electromagnetic metamaterial based on graphene Download PDF

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Publication number
CN113782978A
CN113782978A CN202111111029.3A CN202111111029A CN113782978A CN 113782978 A CN113782978 A CN 113782978A CN 202111111029 A CN202111111029 A CN 202111111029A CN 113782978 A CN113782978 A CN 113782978A
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plate
graphene
stirring
fixedly connected
electromagnetic metamaterial
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CN113782978B (en
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聂文艳
王仲根
张文海
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Huainan Normal University
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Huainan Normal University
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01QANTENNAS, i.e. RADIO AERIALS
    • H01Q15/00Devices for reflection, refraction, diffraction or polarisation of waves radiated from an antenna, e.g. quasi-optical devices
    • H01Q15/0006Devices acting selectively as reflecting surface, as diffracting or as refracting device, e.g. frequency filtering or angular spatial filtering devices
    • H01Q15/0086Devices acting selectively as reflecting surface, as diffracting or as refracting device, e.g. frequency filtering or angular spatial filtering devices said selective devices having materials with a synthesized negative refractive index, e.g. metamaterials or left-handed materials
    • 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
    • C01B32/19Preparation by exfoliation
    • C01B32/192Preparation by exfoliation starting from graphitic oxides
    • 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
    • C01B32/194After-treatment

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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention is suitable for the technical field of electromagnetic metamaterials, and provides a preparation method of an electromagnetic metamaterial based on graphene, which comprises the following steps: s1, calculating return loss of the electromagnetic metamaterial with different structure sizes according to the types of the magnetic material and the adhesive in the magnetic composite material, the mass fraction ratio of the magnetic material and the type of the conductive material by using a line scan model in CST simulation software to obtain the structure size with the maximum return loss, and then casting to obtain a first matrix; and S2, placing a conductive material in the vacancy of the upper surface of the first substrate, and then bonding the conductive material to the periodic unit of the placed metamaterial by using a universal adhesive to obtain the electromagnetic metamaterial. According to the preparation method of the electromagnetic metamaterial based on the graphene, disclosed by the invention, when the electromagnetic metamaterial based on the graphene is prepared, the process is simpler, the preparation difficulty is lower, and the electromagnetic metamaterial based on the graphene is further convenient to prepare, so that the practicability of the preparation method is reflected.

Description

Preparation method of electromagnetic metamaterial based on graphene
Technical Field
The invention belongs to the technical field of electromagnetic metamaterials, and particularly relates to a preparation method of an electromagnetic metamaterial based on graphene.
Background
The graphene is sp2Carbon atoms in hybridized connection are tightly packed into a single-layer two-dimensional honeycombNew materials with lattice-like structures.
The graphene has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future.
At present, when the electromagnetic metamaterial of graphene is prepared, certain defects exist, for example, the preparation process is complicated, conditions required in the preparation process are difficult to realize, and the difficulty of the prepared electromagnetic metamaterial of graphene is further increased.
Disclosure of Invention
The invention provides a preparation method of a graphene-based electromagnetic metamaterial, and aims to solve the problem that the process is complicated when the graphene-based electromagnetic metamaterial is prepared.
The invention is realized in such a way that a preparation method of an electromagnetic metamaterial based on graphene comprises the following steps:
s1, calculating return loss of the electromagnetic metamaterial with different structure sizes according to the types of the magnetic material and the adhesive in the magnetic composite material, the mass fraction ratio of the magnetic material and the type of the conductive material by using a line scan model in CST simulation software to obtain the structure size with the maximum return loss, and then casting to obtain a first matrix;
s2, placing a conductive material in the vacancy of the upper surface of the first substrate, and then bonding the conductive material on the periodic unit of the placed metamaterial by using a universal adhesive to obtain the electromagnetic metamaterial;
s3, preparing graphene oxide: (1) slowly adding quantitative natural crystalline flake graphite into a stirring device filled with 120ml of concentrated sulfuric acid under stirring at 0 ℃ in an ice-water bath, continuously stirring for half an hour, slowly adding 18-25g of potassium permanganate, continuously stirring for 1-2 hours under stirring at 0 ℃, stirring for 1-2 hours at 10-20 ℃, and stirring for 1-2 hours at the temperature of not higher than 20-35 ℃;
(2) then adding hydrogen peroxide under the condition of keeping the room temperature until the mixture is changed from black brown to bright yellow and no bubbles are generated; removing the acid waste liquid dissolved with a small amount of graphene oxide, and adding a 5-10% hydrochloric acid solution to fully wash the mixture;
(3) adding ammonia water into the mixture graphite oxide washed by hydrochloric acid until the pH value is close to neutral, and then repeatedly washing by using deionized water until no precipitate appears after the mixture graphite oxide is detected by using a silver nitrate solution; settling and separating the washed neutral product or performing solid-liquid separation by a centrifugal machine to finally obtain viscous brown colloidal graphite oxide;
(4) putting the obtained graphite oxide into vacuum freeze drying equipment for drying treatment to obtain graphite oxide flocculent solid; dissolving dried graphite oxide flocculent powder into deionized water, fully stirring, and then carrying out ultrasonic treatment in an ultrasonic cleaner to strip graphite oxide sheets to obtain a light yellow graphite oxide suspension;
s4, mixing the raw materials: and putting the electromagnetic metamaterial obtained in the step S2 into the graphite oxide suspension, and then mixing and stirring in a stirring device to obtain the graphene electromagnetic metamaterial.
Preferably, the natural flake graphite in S3 is 5-10 g.
Preferably, the content of hydrogen peroxide in the S3 is 30-35%.
Preferably, S4 is mixing the stirring in-process, needs to use agitating unit, agitating unit includes agitator tank and base, the bottom fixedly connected with bottom plate of agitator tank, the equal fixedly connected with backup pad in both sides at bottom plate top, two sliding connection has the movable plate between the relative one side of backup pad, the both sides of movable plate all run through the backup pad and extend to one side of backup pad, the bottom of movable plate is through two connecting plate fixedly connected with cover, the bottom of cover contact in on the agitator tank.
Preferably, the other side of the supporting plate is fixedly connected with a control box, one side inside the control box is rotatably connected with a disc, a sliding piece is fixedly connected to the disc, a sliding plate is slidably connected between two sides inside the control box, a sliding groove is formed in the sliding plate, and the outer surface of the sliding piece is slidably connected inside the sliding groove.
Preferably, one side of the sliding plate penetrates through the control box and extends to the outside of the control box, one side of the sliding plate extending to the outside of the control box is fixedly connected with a threaded plate, and one side of the control box is fixedly connected with a fixed block.
Preferably, a driving motor is arranged on one side of the control box, a lead screw is fixedly connected to an output shaft of the driving motor, one end of the lead screw is rotatably connected to the fixed block, the outer surface of the lead screw is in threaded connection with the inside of the threaded plate, an extrusion plate is fixedly connected to the bottom of the sliding plate, the bottom of the extrusion plate penetrates through the control box and extends to the bottom of the control box, and one side of the extrusion plate, which extends to the bottom of the control box, is fixed to the moving plate.
Preferably, a motor is arranged on the tank cover, a stirring piece is fixedly connected to an output shaft of the motor, and the bottom of the stirring piece penetrates through the tank cover and extends to the bottom of the tank cover.
Preferably, the equal fixedly connected with locking plate in both sides of movable plate bottom, one side fixedly connected with location box of backup pad, sliding connection has the displacement plate between the inside both sides of location box, the bottom of displacement plate is provided with two compression spring, two compression spring's bottom all set up in the inside one side of location box, the bottom of locking plate is run through the location box extends to the inside of location box, the locking plate extends to the inside one side contact of location box in on the displacement plate.
Preferably, the both sides of locking plate are all seted up flutedly, the equal fixedly connected with locating part in the inside both sides of location box, sliding connection has the retaining member between the inside both sides of locating member, one side of retaining member runs through in proper order locating member and recess extend to the inside of recess, one side of retaining member is provided with the extrusion spring, the one end of extrusion spring set up in the inside one side of locating member, the equal fixedly connected with T type pole in both sides at base top, the inside sliding connection of bottom plate is in the surface of two T type poles, the surface cover of T type pole is equipped with buffer spring.
Compared with the prior art, the invention has the beneficial effects that: according to the preparation method of the electromagnetic metamaterial based on the graphene, disclosed by the invention, when the electromagnetic metamaterial based on the graphene is prepared, the process is simpler, the preparation difficulty is lower, and the electromagnetic metamaterial based on the graphene is further convenient to prepare, so that the practicability of the preparation method is reflected;
through the driving motor who sets up, can realize dismantlement and installation between cover and the agitator tank, the operating personnel of being convenient for washs the inside of agitator tank, improves abluent effect, avoids remaining raw materials to remain in the bottom of agitator tank, and then influences next use to through the fixed joint between retaining member and the recess, fix the position after the installation, avoid taking place the displacement, thereby cause revealing of raw materials in stirring process, influence normal use.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic cross-sectional view of the agitator tank of FIG. 1;
FIG. 3 is a schematic view of the inner structure of the positioning box of FIG. 2;
fig. 4 is a schematic view of the internal structure of the control box of fig. 2.
In the figure: 1-stirring tank, 2-base, 3-bottom plate, 4-supporting plate, 5-moving plate, 6-tank cover, 7-control box, 8-disc, 9-sliding piece, 10-sliding piece, 11-sliding groove, 12-thread plate, 13-fixed block, 14-driving motor, 15-lead screw, 16-extrusion plate, 17-motor, 18-stirring piece, 19-locking plate, 20-positioning box, 21-displacement plate, 22-compression spring, 23-limiting piece, 24-locking piece, 25-extrusion spring, 26-T-shaped rod, 27-buffer spring and 28-groove.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1 to 4, the present invention provides a method for preparing a graphene-based electromagnetic metamaterial, including the following steps:
s1, calculating return loss of the electromagnetic metamaterial with different structure sizes according to the types of the magnetic material and the adhesive in the magnetic composite material, the mass fraction ratio of the magnetic material and the type of the conductive material by using a line scan model in CST simulation software to obtain the structure size with the maximum return loss, and then casting to obtain a first matrix;
s2, placing a conductive material in the vacancy of the upper surface of the first substrate, and then bonding the conductive material on the periodic unit of the placed metamaterial by using a universal adhesive to obtain the electromagnetic metamaterial;
s3, preparing graphene oxide: (1) slowly adding quantitative natural crystalline flake graphite into a stirring device filled with 120ml of concentrated sulfuric acid under stirring at 0 ℃ in an ice-water bath, continuously stirring for half an hour, slowly adding 18-25g of potassium permanganate, continuously stirring for 1-2 hours under stirring at 0 ℃, stirring for 1-2 hours at 10-20 ℃, and stirring for 1-2 hours at the temperature of not higher than 20-35 ℃;
(2) then adding hydrogen peroxide under the condition of keeping the room temperature until the mixture is changed from black brown to bright yellow and no bubbles are generated; removing the acid waste liquid dissolved with a small amount of graphene oxide, and adding a 5-10% hydrochloric acid solution to fully wash the mixture;
(3) adding ammonia water into the mixture graphite oxide washed by hydrochloric acid until the pH value is close to neutral, and then repeatedly washing by using deionized water until no precipitate appears after the mixture graphite oxide is detected by using a silver nitrate solution; settling and separating the washed neutral product or performing solid-liquid separation by a centrifugal machine to finally obtain viscous brown colloidal graphite oxide;
(4) putting the obtained graphite oxide into vacuum freeze drying equipment for drying treatment to obtain graphite oxide flocculent solid; dissolving dried graphite oxide flocculent powder into deionized water, fully stirring, and then carrying out ultrasonic treatment in an ultrasonic cleaner to strip graphite oxide sheets to obtain a light yellow graphite oxide suspension;
s4, mixing the raw materials: putting the electromagnetic metamaterial obtained in the step S2 into the graphite oxide suspension liquid for mixing and stirring to obtain a graphene electromagnetic metamaterial;
in the embodiment, 5-10g of natural flake graphite in the S3;
the natural flake graphite is preferably 8g, and may be modified depending on the specific use.
In the embodiment, the hydrogen peroxide in the S3 is 30-35%;
the hydrogen peroxide is preferably 32%, and may be modified depending on the specific use.
In this embodiment, in the mixing and stirring process of S4, a stirring device is required, the stirring device includes a stirring tank 1 and a base 2, a bottom plate 3 is fixedly connected to the bottom of the stirring tank 1, support plates 4 are fixedly connected to both sides of the top of the bottom plate 3, a moving plate 5 is slidably connected between two opposite sides of the support plates 4, both sides of the moving plate 5 penetrate through the support plates 4 and extend to one side of the support plates 4, a tank cover 6 is fixedly connected to the bottom of the moving plate 5 through two connecting plates, and the bottom of the tank cover 6 contacts the stirring tank 1;
sealing gaskets are arranged on two sides of the bottom of the tank cover 6 and used for sealing the space between the tank cover 6 and the stirring tank 1;
the base 2 is placed in contact parallel to the ground.
In the present embodiment, a control box 7 is fixedly connected to the other side of the support plate 4, a disc 8 is rotatably connected to one side inside the control box 7, a sliding member 9 is fixedly connected to the disc 8, a sliding plate 10 is slidably connected between two sides inside the control box 7, a sliding groove 11 is formed in the sliding plate 10, and an outer surface of the sliding member 9 is slidably connected to the inside of the sliding groove 11;
the sliding piece 9 is matched with the sliding groove 11;
the sliding part 9 and the sliding groove 11 are arranged and used for limiting the thread plate 12 on the screw rod 15.
In this embodiment, one side of the sliding plate 10 penetrates through the control box 7 and extends to the outside of the control box 7, a threaded plate 12 is fixedly connected to one side of the sliding plate 10 extending to the outside of the control box 7, and a fixed block 13 is fixedly connected to one side of the control box 7.
In the present embodiment, a driving motor 14 is disposed at one side of the control box 7, a lead screw 15 is fixedly connected to an output shaft of the driving motor 14, one end of the lead screw 15 is rotatably connected to the fixed block 13, an outer surface of the lead screw 15 is screwed inside the screw plate 12, a pressing plate 16 is fixedly connected to the bottom of the sliding plate 10, the bottom of the pressing plate 16 penetrates through the control box 7 and extends to the bottom of the control box 7, and one side of the pressing plate 16 extending to the bottom of the control box 7 is fixed to the moving plate 5;
the driving motor 14 is connected with an external power supply and a control switch;
the driving motor 14 is a positive and negative rotation driving motor 14, so that the tank cover 6 and the stirring tank 1 can be mounted and dismounted without the trouble of manual dismounting.
In the present embodiment, the tank cover 6 is provided with a motor 17, an output shaft of the motor 17 is fixedly connected with a stirring piece 18, and the bottom of the stirring piece 18 penetrates through the tank cover 6 and extends to the bottom of the tank cover 6;
the motor 17 is connected with an external power supply and a control switch;
the stirring member 18 is made by the prior art, and only needs to stir the raw materials in the stirring tank 1.
In this embodiment, both sides of the bottom of the moving plate 5 are fixedly connected with locking plates 19, one side of the supporting plate 4 is fixedly connected with a positioning box 20, a displacement plate 21 is slidably connected between both sides of the inside of the positioning box 20, the bottom of the displacement plate 21 is provided with two compression springs 22, the bottom ends of the two compression springs 22 are both arranged at one side of the inside of the positioning box 20, the bottom of the locking plate 19 penetrates through the positioning box 20 and extends to the inside of the positioning box 20, and one side of the locking plate 19 extending to the inside of the positioning box 20 is in contact with the displacement plate 21;
through the arranged compression spring 22, when the locking plate 19 is inserted into the positioning box 20, the locking plate 19 is buffered, and then the locking plate 19 is extruded in the rebound process of the compression spring 22, so that the locking plate 19 extrudes the locking piece 24, and the stability of clamping the locking piece 24 and the groove 28 is improved;
in addition, the clamping firmness between the locking piece 24 and the groove 28 is not influenced during the rebound process of the compression spring 22;
two sides of the bottom of the locking member 24 are provided with cambered surfaces which are convenient for extruding the locking member 24, so that the locking member 24 slides on the locking plate 19 and enters the groove 28 for fixed clamping;
the equal fixedly connected with stopper in both sides inside location box 20, when displacement plate 21 contacts with the stopper, contact between cover 6 and agitator tank 1 this moment, accomplish the installation.
In this embodiment, two sides of the locking plate 19 are both provided with a groove 28, two sides of the inside of the positioning box 20 are both fixedly connected with a limiting member 23, a locking member 24 is slidably connected between two sides of the inside of the limiting member 23, one side of the locking member 24 sequentially penetrates through the limiting member 23 and the groove 28 and extends to the inside of the groove 28, one side of the locking member 24 is provided with an extrusion spring 25, one end of the extrusion spring 25 is arranged at one side of the inside of the limiting member 23, two sides of the top of the base 2 are both fixedly connected with T-shaped rods 26, the inside of the bottom plate 3 is slidably connected to the outer surfaces of the two T-shaped rods 26, and the outer surface of the T-shaped rod 26 is sleeved with a buffer spring 27;
the groove 28 is matched with the locking plate 19;
through the arranged extrusion spring 25, in the rebound process, the locking piece 24 and the groove 28 are fixedly clamped, and further the position of the moving plate 5 is locked, so that the tank cover 6 and the stirring tank 1 are hermetically fixed;
through the buffer spring 27, the generated shaking in the stirring process is buffered, and the damage of parts in the stirring tank 1 caused by long-time shaking is avoided;
the top of the T-bar 26 is slidably attached to the support plate 4.
The working principle of the invention is as follows: s1, calculating return loss of the electromagnetic metamaterial with different structure sizes according to the types of the magnetic material and the adhesive in the magnetic composite material, the mass fraction ratio of the magnetic material and the type of the conductive material by using a line scan model in CST simulation software to obtain the structure size with the maximum return loss, and then casting to obtain a first matrix;
s2, placing a conductive material in the vacancy of the upper surface of the first substrate, and then bonding the conductive material on the periodic unit of the placed metamaterial by using a universal adhesive to obtain the electromagnetic metamaterial;
s3, preparing graphene oxide: (1) slowly adding quantitative natural crystalline flake graphite into a stirring device filled with 120ml of concentrated sulfuric acid under stirring at 0 ℃ in an ice-water bath, continuously stirring for half an hour, slowly adding 18-25g of potassium permanganate, continuously stirring for 1-2 hours under stirring at 0 ℃, stirring for 1-2 hours at 10-20 ℃, and stirring for 1-2 hours at the temperature of not higher than 20-35 ℃;
(2) then adding hydrogen peroxide under the condition of keeping the room temperature until the mixture is changed from black brown to bright yellow and no bubbles are generated; removing the acid waste liquid dissolved with a small amount of graphene oxide, and adding a 5-10% hydrochloric acid solution to fully wash the mixture;
(3) adding ammonia water into the mixture graphite oxide washed by hydrochloric acid until the pH value is close to neutral, and then repeatedly washing by using deionized water until no precipitate appears after the mixture graphite oxide is detected by using a silver nitrate solution; settling and separating the washed neutral product or performing solid-liquid separation by a centrifugal machine to finally obtain viscous brown colloidal graphite oxide;
(4) putting the obtained graphite oxide into vacuum freeze drying equipment for drying treatment to obtain graphite oxide flocculent solid; dissolving dried graphite oxide flocculent powder into deionized water, fully stirring, and then carrying out ultrasonic treatment in an ultrasonic cleaner to strip graphite oxide sheets to obtain a light yellow graphite oxide suspension;
s4, mixing the raw materials: putting the electromagnetic metamaterial obtained in the step S2 into the graphite oxide suspension, and then mixing and stirring in a stirring device to obtain the graphene electromagnetic metamaterial;
when in use, the first step is as follows: quantitative raw materials are required to be put into the stirring tank 1 for stirring, then the driving motor 14 is started, the screw rod 15 on the output shaft of the driving motor 14 is rotated to drive the threaded plate 12 to slide on the screw rod 15, the sliding plate 10 on the threaded plate 12 slides in the control box 7 and drives the sliding groove 11 to extrude the sliding piece 9, then the extruding plate 16 on the sliding plate 10 pushes the moving plate 5 to slide downwards on the supporting plate 4, the locking plate 19 at the bottom of the moving plate 5 is driven to be inserted into the positioning box 20, the locking plate 19 extrudes the locking piece 24, the extruding spring 25 is compressed, then, the bottom of the locking plate 19 is in contact extrusion with the displacement plate 21, the compression spring 22 is in compression deformation, when the displacement plate 21 is in contact with the limiting block, the groove 28 on the locking plate 19 just slides into the locking piece 24, the locking piece 24 and the groove 28 are clamped and fixed, so that the tank cover 6 is installed and fixed;
the second step is that: then starting the motor 17 to rotate the stirring piece 18 on the output shaft of the motor 17, so as to stir the raw materials inside;
the third step: after the stirring is finished, the stirring tank 1 needs to be cleaned, and the tank cover 6 needs to be disassembled when the stirring is finished, by starting the driving motor 14, the screw rod 15 on the output shaft of the driving motor 14 is rotated to drive the sliding plate 10 on the thread plate 12 to slide upwards, so that the sliding part 9 extrudes the sliding slot 11, the moving plate 5 on the extrusion plate 16 is driven to slide upwards on the supporting plate 4, thereby pulling the can lid 6, so that the groove 28 of the locking plate 19 presses the locking piece 24, causing the pressing spring 25 to compress, so that the locker 24 slides out of the recess and over the locking plate 19, while the resilience of the compression spring 22 pushes the locking plate 19 to move upwards, so that the tank cover 6 is separated from the stirring tank 1, and the inside of the stirring tank 1 is convenient to clean.
Through the driving motor 14 who sets up, can realize dismantlement and installation between cover 6 and agitator tank 1, the operating personnel of being convenient for washs the inside of agitator tank 1, improve abluent effect, avoid remaining raw materials to remain in the bottom of agitator tank 1, and then influence next use, and through the fixed joint between retaining member 24 and the recess 28, fix the position after the installation, avoid taking place the displacement, thereby cause the raw materials in the revealing of stirring in-process, influence normal use.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (10)

1. A preparation method of an electromagnetic metamaterial based on graphene is characterized by comprising the following steps: the method comprises the following steps:
s1, calculating return loss of the electromagnetic metamaterial with different structure sizes according to the types of the magnetic material and the adhesive in the magnetic composite material, the mass fraction ratio of the magnetic material and the type of the conductive material by using a line scan model in CST simulation software to obtain the structure size with the maximum return loss, and then casting to obtain a first matrix;
s2, placing a conductive material in the vacancy of the upper surface of the first substrate, and then bonding the conductive material on the periodic unit of the placed metamaterial by using a universal adhesive to obtain the electromagnetic metamaterial;
s3, preparing graphene oxide: (1) slowly adding quantitative natural crystalline flake graphite into a stirring device filled with 120ml of concentrated sulfuric acid under stirring at 0 ℃ in an ice-water bath, continuously stirring for half an hour, slowly adding 18-25g of potassium permanganate, continuously stirring for 1-2 hours under stirring at 0 ℃, stirring for 1-2 hours at 10-20 ℃, and stirring for 1-2 hours at the temperature of not higher than 20-35 ℃;
(2) then adding hydrogen peroxide under the condition of keeping the room temperature until the mixture is changed from black brown to bright yellow and no bubbles are generated; removing the acid waste liquid dissolved with a small amount of graphene oxide, and adding a 5-10% hydrochloric acid solution to fully wash the mixture;
(3) adding ammonia water into the mixture graphite oxide washed by hydrochloric acid until the pH value is close to neutral, and then repeatedly washing by using deionized water until no precipitate appears after the mixture graphite oxide is detected by using a silver nitrate solution; settling and separating the washed neutral product or performing solid-liquid separation by a centrifugal machine to finally obtain viscous brown colloidal graphite oxide;
(4) putting the obtained graphite oxide into vacuum freeze drying equipment for drying treatment to obtain graphite oxide flocculent solid; dissolving dried graphite oxide flocculent powder into deionized water, fully stirring, and then carrying out ultrasonic treatment in an ultrasonic cleaner to strip graphite oxide sheets to obtain a light yellow graphite oxide suspension;
s4, mixing the raw materials: and putting the electromagnetic metamaterial obtained in the step S2 into the graphite oxide suspension, and then mixing and stirring in a stirring device to obtain the graphene electromagnetic metamaterial.
2. The method for preparing the electromagnetic metamaterial based on graphene as claimed in claim 1, wherein: and 5-10g of natural flake graphite in the S3.
3. The method for preparing the electromagnetic metamaterial based on graphene as claimed in claim 1, wherein: the hydrogen peroxide in the S3 accounts for 30-35%.
4. The method for preparing the electromagnetic metamaterial based on graphene as claimed in claim 1, wherein: s4 is mixing the stirring in-process, needs to use agitating unit, agitating unit includes agitator tank (1) and base (2), the bottom fixedly connected with bottom plate (3) of agitator tank (1), the equal fixedly connected with backup pad (4) in both sides at bottom plate (3) top, two sliding connection has movable plate (5) between the relative one side of backup pad (4), the both sides of movable plate (5) all run through backup pad (4) and extend to one side of backup pad (4), two connecting plate fixedly connected with cover (6) are passed through to the bottom of movable plate (5), the bottom of cover (6) contact in on agitator tank (1).
5. The method for preparing the electromagnetic metamaterial based on graphene as claimed in claim 4, wherein: the improved multifunctional support plate is characterized in that a control box (7) is fixedly connected to the other side of the support plate (4), a disc (8) is rotatably connected to one side of the interior of the control box (7), a sliding piece (9) is fixedly connected to the disc (8), a sliding plate (10) is slidably connected between two sides of the interior of the control box (7), a sliding groove (11) is formed in the sliding plate (10), and the outer surface of the sliding piece (9) is slidably connected to the interior of the sliding groove (11).
6. The method for preparing the electromagnetic metamaterial based on graphene as claimed in claim 5, wherein: one side of the sliding plate (10) penetrates through the control box (7) and extends to the outside of the control box (7), one side of the sliding plate (10) extending to the outside of the control box (7) is fixedly connected with a threaded plate (12), and one side of the control box (7) is fixedly connected with a fixed block (13).
7. The method for preparing the electromagnetic metamaterial based on graphene as claimed in claim 6, wherein: one side of the control box (7) is provided with a driving motor (14), a screw rod (15) is fixedly connected to an output shaft of the driving motor (14), one end of the screw rod (15) is rotatably connected to the fixed block (13), the outer surface of the screw rod (15) is in threaded connection with the inside of the threaded plate (12), a squeezing plate (16) is fixedly connected to the bottom of the sliding plate (10), the bottom of the squeezing plate (16) penetrates through the control box (7) and extends to the bottom of the control box (7), and one side of the bottom of the control box (7) extending to the squeezing plate (16) is fixed to the moving plate (5).
8. The method for preparing the electromagnetic metamaterial based on graphene as claimed in claim 4, wherein: the tank cover (6) is provided with a motor (17), an output shaft of the motor (17) is fixedly connected with a stirring piece (18), and the bottom of the stirring piece (18) penetrates through the tank cover (6) and extends to the bottom of the tank cover (6).
9. The method for preparing the electromagnetic metamaterial based on graphene as claimed in claim 4, wherein: the equal fixedly connected with locking plate (19) in both sides of movable plate (5) bottom, one side fixedly connected with location box (20) of backup pad (4), sliding connection has displacement board (21) between the inside both sides of location box (20), the bottom of displacement board (21) is provided with two compression spring (22), two the bottom of compression spring (22) all set up in one side of location box (20) inside, the bottom of locking plate (19) is run through location box (20) and extend to the inside of location box (20), locking plate (19) extend to the inside one side of location box (20) contact in on displacement board (21).
10. The method for preparing the electromagnetic metamaterial based on graphene as claimed in claim 9, wherein: recess (28) are all seted up to the both sides of locking plate (19), the equal fixedly connected with locating part (23) in both sides of location box (20) inside, sliding connection has retaining member (24) between the both sides of retaining member (23) inside, one side of retaining member (24) runs through in proper order locating member (23) and recess (28) extend to the inside of recess (28), one side of retaining member (24) is provided with extrusion spring (25), the one end of extrusion spring (25) set up in the inside one side of retaining member (23), the equal fixedly connected with T type pole (26) in both sides at base (2) top, the inside sliding connection of bottom plate (3) is in the surface of two T type poles (26), the surface cover of T type pole (26) is equipped with buffer spring (27).
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CN108103485A (en) * 2017-12-18 2018-06-01 西安理工大学 A kind of preparation method in graphene surface clad copper or nickel
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