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CN118612898B - High-temperature graphene flexible heating device and preparation method thereof - Google Patents

High-temperature graphene flexible heating device and preparation method thereof Download PDF

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Publication number
CN118612898B
CN118612898B CN202411074663.8A CN202411074663A CN118612898B CN 118612898 B CN118612898 B CN 118612898B CN 202411074663 A CN202411074663 A CN 202411074663A CN 118612898 B CN118612898 B CN 118612898B
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electrode
graphene
heating device
graphene layer
reinforcing ribs
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CN118612898A (en
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崔金安
施惠庆
张郁佳
佘旭波
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Kechuan New Materials Technology Huai'an Co ltd
Suzhou Kechuan Electronic Technology Co ltd
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Kechuan New Materials Technology Huai'an Co ltd
Suzhou Kechuan Electronic Technology Co ltd
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    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/02Details
    • H05B3/03Electrodes
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/02Details
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/10Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
    • H05B3/14Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
    • H05B3/145Carbon only, e.g. carbon black, graphite

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  • Resistance Heating (AREA)

Abstract

The application discloses a high-temperature graphene flexible heating device and a preparation method thereof, and relates to the technical field of graphene heating. The preparation method comprises the following steps: depositing graphene on a substrate by using vacuum magnetron sputtering equipment to form a graphene layer; fixing the reinforcing ribs in an electrode area of the graphene layer; and thirdly, preparing an electrode in the electrode area of the graphene layer, and forming a conductive electrode unit by the electrode and the reinforcing ribs to finish manufacturing of the heating device. Therefore, the problem of the existing graphene heating device is solved, the strength of the whole conductive electrode unit structure is increased due to the combination of the reinforcing ribs and the electrodes, external stress and deformation can be resisted, smooth transmission of current between the electrodes and the graphene layer heating material is ensured, resistance and energy loss are reduced, and durability and stability of products are improved.

Description

High-temperature graphene flexible heating device and preparation method thereof
Technical Field
The application relates to the technical field of graphene heating, in particular to a high-temperature graphene flexible heating device and a preparation method thereof.
Background
High-temperature graphene flexible heating devices are a novel heating product, and have attracted wide attention in various industry fields in recent years. The glass fiber high-temperature graphene flexible heating device is a novel heating material prepared by organically combining glass fibers and graphene, then preparing electrodes on the graphene and adopting a special process. The material can maintain uniform and stable temperature distribution in the heating process, and combines the excellent mechanical property of glass fiber and the high heat-conducting property of graphene, thereby providing high-efficiency, uniform and stable heating effect. However, as the flexible glass fiber cloth has certain flexibility and deformability, the electrode is influenced by the matrix to deform after being prepared on the heating plate, and cracks or defects can appear on the electrode layer, so that uncertainty exists in the conductivity and stability of the product electrode, and the quality of the heating plate is greatly influenced.
Disclosure of Invention
In order to solve the problems, improve the conductivity and stability of the electrode and ensure the quality of the high-temperature graphene flexible heating device, the application provides the high-temperature graphene flexible heating device and a preparation method thereof.
The application provides a high-temperature graphene flexible heating device and a preparation method thereof, and adopts the following technical scheme.
The utility model provides a flexible heating device of high temperature graphite alkene, includes the base member, be provided with the graphite alkene layer on the base member, graphite alkene layer surface is provided with the electrode, be provided with the strengthening rib of being made by conductive material in the electrode.
Through adopting above-mentioned technical scheme, through the setting at graphene layer surface strengthening rib and electrode, can guarantee the conductivity and the stability of electrode, even if this heating device takes place to buckle deformation, electrode crack or defect have also been guaranteed the smooth and easy transmission of electric current between electrode and graphene layer heating material, have reduced resistance and energy loss, have improved whole conductive efficiency, can guarantee high-efficient, even and stable heating effect.
Optionally, an oxidation preventing layer covers the graphene layer and the electrode.
Through adopting above-mentioned technical scheme, through the setting of oxidation prevention layer, encapsulation accomplishes the surfacing, makes the electrode have higher durability and stability to this heating device's life has been prolonged.
Optionally, the upper surface and the lower surface of the base body are both provided with graphene layers, and two electrodes corresponding to the graphene layers are provided.
By adopting the technical scheme, the upper and lower double-layer heating structure of the substrate is realized, and the heating efficiency of the heating device is improved.
Optionally, the reinforcing ribs are in a wire shape or a grid shape.
By adopting the technical scheme, the reinforcing ribs are in the shape of the wire body, and the wire-type reinforcing rib structure is added into the electrode, so that the overall rigidity and stability of the electrode can be remarkably improved; the line type reinforcing ribs can clearly define the flow path of the current, are favorable for optimizing current distribution, and reduce current concentration and obvious local overheating phenomenon. The reinforcing ribs are in a net shape, and the reinforcing rib structure shows excellent performance effect in the electrode in a unique geometric shape; the active area of the electrode can be increased by changing the shape of the surface of the electrode, so that the electrochemical reaction efficiency is improved.
Optionally, the reinforcing ribs and the electrodes form a conductive electrode unit, the filling rate of the reinforcing ribs accounts for 10 to 50 percent of the whole conductive electrode unit, the thickness of the electrode is 1 to 500um, and the width of the electrode is 2 to 12mm.
By adopting the technical scheme, the filling rate of the reinforcing ribs is 10-50%, the effect of the reinforcing ribs is not obvious when the ratio is too small, and the stability of the electrode can be affected after the electrode is sprayed by the ratio is too high.
A method for preparing the high-temperature graphene flexible heating device, comprising the following steps:
Depositing graphene on a substrate by using vacuum magnetron sputtering equipment to form a graphene layer;
Fixing the reinforcing ribs in an electrode area of the graphene layer;
And thirdly, preparing an electrode in the electrode area of the graphene layer, and forming a conductive electrode unit by the electrode and the reinforcing ribs to finish manufacturing of the heating device.
Optionally, the substrate is pretreated before the first step, including cleaning and surface activation.
By adopting the technical scheme, the substrate is subjected to cleaning and surface activation treatment so as to ensure the cleaning and activity of the surface of the substrate, thereby enhancing the combination between the graphene and the substrate.
Optionally, the specific process of fixing the reinforcing ribs on the electrode area of the graphene layer through the fixture includes the following steps:
s1, placing a substrate on which a graphene layer is formed by depositing graphene in the first step at the groove position of a lower clamp;
S2, fixing the reinforcing ribs on the fixing columns of the lower clamp;
s3, pressing and fixing the base body and the reinforcing ribs by using an upper clamp to finish the fixing of the reinforcing ribs;
The specific process for preparing the electrode in the electrode area of the graphene layer is as follows: spraying electrode materials at the hollowed-out position of the upper clamp, and covering and fixing the reinforcing ribs; and finishing the manufacturing of the heating device.
Optionally, plating an anti-oxidation layer on the heating device by using a vacuum magnetron sputtering or magnetron sputtering evaporation integrated machine.
By adopting the technical scheme, the oxidation resistance of the heating device is improved through the arrangement of the oxidation prevention layer, and particularly oxidation and decay failure in the high-temperature use process are prevented.
Optionally, the fixture comprises a lower fixture and an upper fixture which are mutually close, wherein the lower fixture is provided with a plurality of positioning columns, and the upper fixture is provided with a plurality of positioning holes matched with the positioning columns; the lower clamp is provided with a groove for placing a substrate, and the lower clamps on two opposite sides of the groove are provided with fixing columns for fixing the reinforcing ribs; and an avoidance hole is formed in the position, corresponding to the fixed column, on the upper clamp, and an electrode covering hole is formed in the connecting line position area of the fixed columns on the two sides of the corresponding substrate on the upper clamp.
Through adopting above-mentioned technical scheme, through the use of anchor clamps, can be quick carry out the clamping to strengthening rib and base member fixedly for two positions are relatively fixed, are favorable to carrying out the preparation of electrode, and this anchor clamps simple structure, the simple operation is favorable to improving production efficiency and quality.
In summary, the application at least comprises the following beneficial effects:
1. By adopting the technical scheme, the electric conductivity and the stability of the electrode can be ensured through the arrangement of the reinforcing ribs and the electrodes on the surface of the graphene layer, and even if the heating device is bent and deformed and the electrode is cracked or defective, smooth transmission of current between the electrode and the heating material of the graphene layer can be ensured, the resistance and the energy loss are reduced, the overall electric conduction efficiency is improved, and the efficient, uniform and stable heating effect can be ensured.
2. The reinforcing ribs are in a wire shape, and the wire-shaped reinforcing rib structure is added into the electrode through the wire-shaped reinforcing ribs, so that the overall rigidity and stability of the electrode can be remarkably improved; the line type reinforcing ribs can clearly define the flow path of the current, are favorable for optimizing current distribution, and reduce current concentration and obvious local overheating phenomenon.
3. The reinforcing ribs are in a grid shape, and the reinforcing rib structure shows excellent performance effect in the electrode by the unique geometric shape of the reinforcing ribs through the mesh shape of the reinforcing ribs; the active area of the electrode can be increased by changing the shape of the surface of the electrode, so that the electrochemical reaction efficiency is improved.
4. According to the application, through the arrangement of the oxidation prevention layer, the surface of the packaged electrode is smooth, so that the electrode has higher durability and stability, particularly oxidation and decay failure in the high-temperature use process are prevented, and the service life is prolonged.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the following description will briefly explain the drawings used in the embodiments or the description of the prior art, and it is obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings can be obtained according to these drawings without inventive effort to a person skilled in the art.
Fig. 1 is a schematic cross-sectional structure diagram of a high-temperature graphene flexible heating device in a first embodiment.
Fig. 2 is a schematic structural diagram of a high-temperature graphene flexible heating device (excluding an oxidation preventing layer) in the first embodiment.
Fig. 3 is a schematic diagram of an end face structure of a high-temperature graphene flexible heating device (excluding an oxidation preventing layer) in the first embodiment.
Fig. 4 is a schematic view of the sectional structure of fig. 3 taken along the section line A-A.
Fig. 5 is a schematic structural diagram of a high-temperature graphene flexible heating device (excluding an oxidation preventing layer) in the second embodiment.
Fig. 6 is a schematic diagram of an end face structure of a high-temperature graphene flexible heating device (excluding an oxidation preventing layer) in the second embodiment.
Fig. 7 is a schematic view of the sectional structure of fig. 6 taken along the section line B-B.
Fig. 8 is a schematic structural diagram of a high-temperature graphene flexible heating device (excluding an oxidation preventing layer) in the third embodiment.
Fig. 9 is a schematic diagram of an end face structure of a high-temperature graphene flexible heating device (excluding an oxidation preventing layer) in the third embodiment.
Fig. 10 is a schematic view of the sectional structure of fig. 9 taken along the section line C-C.
Fig. 11 is a schematic structural diagram of a high-temperature graphene flexible heating device (excluding an oxidation preventing layer) in the fourth embodiment.
Fig. 12 is a schematic diagram of an end face structure of a high-temperature graphene flexible heating device (excluding an oxidation preventing layer) in a fourth embodiment.
Fig. 13 is a schematic view of the sectional structure of fig. 12 taken along the section line D-D.
Fig. 14 is a process flow diagram of a preparation method of a high-temperature graphene flexible heating device in the first embodiment, the second embodiment, the third embodiment and the fourth embodiment.
Fig. 15 is a schematic view of a structure of a jig in the fifth embodiment.
Fig. 16 is a schematic view of the structure of the lower clamp in the fifth embodiment.
Fig. 17 is a schematic diagram of the structure of the upper jig in the fifth embodiment.
Fig. 18 is a schematic view showing a structure in which a base and a reinforcing rib are fixed to a lower jig in the fifth embodiment.
Fig. 19 is a schematic structural diagram of the fifth embodiment after clamping the clamp.
Reference numerals illustrate: 1. a base; 2. a graphene layer; 3. reinforcing ribs; 4. an electrode; 5. an oxidation preventing layer; 6. a lower clamp; 7. a clamp is arranged; 8. positioning columns; 9. positioning holes; 10. a groove; 11. fixing the column; 12. avoidance holes; 13. the electrode covers the aperture.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The application is described in further detail below with reference to fig. 1 to 19.
The embodiment of the application discloses a high-temperature graphene flexible heating device and a preparation method thereof.
Embodiment one: referring to fig. 1, 2, 3, 4, 14, a high temperature graphene flexible heating device includes:
The matrix 1, the matrix 1 comprises glass fiber cloth materials, and the glass fiber cloth has certain flexibility and deformability, so that the heating device has locally excellent mechanical properties, can resist external stress and deformation, improves the durability and stability of the heating device, and can also use other fiber cloth materials.
Be provided with graphene layer 2 on the base member 1, the upper surface and the lower surface of base member 1 all are provided with graphene layer 2, have realized the upper and lower bilayer heating structure of base member 1, have improved heating device's heating efficiency.
Two electrodes 4 are arranged at two edges of the outer surface of the graphene layer 2, and the cross section of each electrode 4 is rectangular. The electrode 4 is internally provided with the reinforcing ribs 3 made of conductive materials, the reinforcing ribs 3 and the electrode 4 form a conductive electrode unit, the reinforcing ribs 3 are in a wire shape and comprise a plurality of reinforcing ribs, and the electrode is added with a linear reinforcing rib structure, so that the overall rigidity and stability of the electrode can be remarkably improved; the line type reinforcing rib can clearly define a current flow path, is favorable for optimizing current distribution, reduces current concentration and is obvious in local overheating phenomenon, the reinforcing rib 3 and the electrode 4 materials comprise tungsten, molybdenum, copper, zirconium, titanium, rhenium, iron chromium aluminum and other materials or two alloy materials, the filling rate of the reinforcing rib 3 is 10-50% of that of the whole conductive electrode unit, the effect of the reinforcing rib is not obvious when the filling rate is too small, the stability is influenced after the electrode is sprayed with the electrode with too high proportion, and the thickness of the electrode is 1-500 um and the width of the electrode is 2-12 mm.
The anti-oxidation layer 5 covers the graphene layer 2 and the electrode 4, and the surface of the packaging is smooth through the arrangement of the anti-oxidation layer 5, so that the electrode has higher durability and stability, and the service life of the heating device is prolonged.
Referring to fig. 1, 2, 3, 4, 14, a method for preparing a high-temperature graphene flexible heating device includes the following steps:
firstly, depositing graphene on a substrate 1 by using vacuum magnetron sputtering equipment to form a graphene layer 2;
The substrate 1 is first pre-treated, including cleaning, surface activation, to ensure the cleaning and activity of the surface of the substrate 1, thereby enhancing the bonding between the graphene and the substrate 1. And then, the pretreated substrate 1 is subjected to reel-to-reel deposition of graphene on the substrate 1 by using a vacuum magnetron sputtering device to form a graphene layer 2, the uniform and tight coverage of the graphene layer 2 on the surface of a base layer is ensured by precisely controlling sputtering parameters, the vacuum degree is controlled within 1.0x10 -2 pa to 4.0x10 -4 pa, and the sputtering power supply power is controlled within 10 KW to 20KW (the deposition thickness can be adjusted according to requirements).
Fixing the reinforcing ribs 3 in the electrode area of the graphene layer 2;
and a special fixing clamp is used for fixing and flattening the material of the wire-shaped reinforcing ribs 3 in the electrode area of the base layer, and the wire size can be set according to the over-current, power and temperature requirements of the product.
The fixing of the reinforcing ribs 3 specifically includes the following steps:
S1, placing a substrate 1 on which graphene is deposited in the first step to form a graphene layer 2 at the position of a groove 10 of a lower clamp 6;
S2, fixing two ends of the reinforcing rib 3 on the fixing columns 11 of the lower clamp 6;
and S3, pressing and fixing the base body 1 and the reinforcing ribs 3 by using the upper clamp 7, and finishing the fixing of the reinforcing ribs 3.
Step three, preparing an electrode 4 in an electrode area of the graphene layer 2;
Spraying electrode materials at the hollowed-out position of the upper clamp 7, and covering and fixing the reinforcing ribs 3; and finishing the manufacturing of the heating device.
The electrode material is prepared on the electrode area of the base layer by spraying or brazing, the electrode 4 is formed, the electrode is formed by fully combining and fixing the spraying/brazing process and the graphene, and the specification of the electrode can be set according to the over-current, power and temperature requirements of the product.
And fourthly, plating an anti-oxidation layer 5 on the heating device manufactured in the third step by using a vacuum magnetron sputtering or magnetron sputtering evaporation integrated machine, and completing manufacturing of the heating device. The vacuum degree is controlled within 1.0x10 -2 pa to 4.0x10 -4 pa, the power of a sputtering power supply is controlled within 10 KW to 20KW (the deposition thickness can be adjusted according to the requirement), the oxidation prevention layer 5 is made of aluminum oxide, hexagonal boron nitride and aluminum silicate, and the aluminum oxide, hexagonal boron nitride and aluminum silicate have the advantages of good high temperature resistance, high heat conduction, insulation, high mechanical strength and the like, and can protect the graphene layer 2 from oxidation and decay failure in the high-temperature use process; the thickness of the oxidation preventing layer 5 is 28nm to 1000nm.
After the device is manufactured, the device needs to be tested, and the heating device is tested:
(1) Conductivity test:
direct current resistance: test data of 100 to 500mΩ using direct current resistance instrument test
Square resistance: test data < 20mΩ using an instrument such as ST 2253-type four-probe Fang Zuyi
(2) Oxidation resistance test: the environment device can keep the effective service time more than 5000H under the condition of high temperature of 1000 ℃.
(3) High temperature resistance test: and testing by using a high-temperature-resistant tester, wherein the temperature resistance is within 1000 ℃.
(4) Insulation test: the insulation data is 3 KV to 3.6KV by using an insulation voltage withstanding tester.
After the preparation is finished, the qualified products after the test are subjected to necessary post-treatment, such as vacuum packaging, so that the products are ensured to be transported and stored.
According to the high-temperature graphene flexible heating device manufactured by the technical scheme, the electrode 4 comprises a wire-shaped reinforcing rib 3 material, so that the problem that the electrode 4 is influenced by a base material to deform after being manufactured on a heating plate, and the electrode layer is cracked or defective is solved; the pre-buried wire-shaped reinforcing ribs 3 form good conductive connection with the electrode 4, and the connection ensures smooth transmission of current between the electrode 4 and the heating material, reduces resistance and energy loss and improves the overall conductive efficiency; the built-in reinforcing ribs 3 and the electrodes 4 form a built-in conductive material and electrode combination, so that the strength of the whole conductive electrode unit structure is increased, the reinforced structure can resist external stress and deformation, the efficient, uniform and stable heating effect can be ensured, and the durability and stability of the product are improved.
Embodiment two: referring to fig. 5, 6, 7, 14, a high temperature graphene flexible heating apparatus includes:
The matrix 1, the matrix 1 comprises glass fiber cloth materials, and the glass fiber cloth has certain flexibility and deformability, so that the heating device has locally excellent mechanical properties, can resist external stress and deformation, improves the durability and stability of the heating device, and can also use other fiber cloth materials.
Be provided with graphene layer 2 on the base member 1, the upper surface and the lower surface of base member 1 all are provided with graphene layer 2, have realized the upper and lower bilayer heating structure of base member 1, have improved heating device's heating efficiency.
Two electrodes 4 are arranged at two edges of the outer surface of the graphene layer 2, and the cross section of each electrode 4 is rectangular. The electrode 4 is internally provided with a reinforcing rib 3 made of conductive materials, and the reinforcing rib 3 and the electrode 4 form a conductive electrode unit. The reinforcing ribs 3 are in a grid shape and are round hole type grid electrode plates, round hole type reinforcing rib structures are added in the electrodes, the round hole type reinforcing rib structures are in unique geometric shapes, the active area of the round hole type reinforcing rib structures can be increased by changing the shape of the surfaces of the electrodes, so that the electrochemical reaction efficiency is improved, excellent performance effects are shown in the electrodes, the round holes can effectively disperse current, more uniform current distribution is realized, the current density is reduced, and hot spots and local damage caused by current concentration are reduced. The materials of the reinforcing ribs 3 and the electrodes 4 comprise tungsten, molybdenum, copper, zirconium, titanium, rhenium, iron-chromium-aluminum and other materials or two alloy materials, the filling rate of the reinforcing ribs 3 is 10-50% of that of the whole conductive electrode material, the effect of the reinforcing ribs is not obvious when the filling rate is too small, the stability is affected after the electrode is sprayed with the reinforcing ribs too high, the thickness of the electrode is 1-500 um, and the width is 2-12 mm.
The anti-oxidation layer 5 covers the graphene layer 2 and the electrode 4, and the surface of the packaging is smooth through the arrangement of the anti-oxidation layer 5, so that the electrode has higher durability and stability, and the service life of the heating device is prolonged.
Referring to fig. 5, 6, 7, 14, a method for preparing a high-temperature graphene flexible heating device includes the following steps:
firstly, depositing graphene on a substrate 1 by using vacuum magnetron sputtering equipment to form a graphene layer 2;
The substrate 1 is first pre-treated, including cleaning, surface activation, to ensure the cleaning and activity of the surface of the substrate 1, thereby enhancing the bonding between the graphene and the substrate 1. And then, the pretreated substrate 1 is subjected to reel-to-reel deposition of graphene on the substrate 1 by using a vacuum magnetron sputtering device to form a graphene layer 2, the uniform and tight coverage of the graphene layer 2 on the surface of a base layer is ensured by precisely controlling sputtering parameters, the vacuum degree is controlled within 1.0x10 -2 pa to 4.0x10 -4 pa, and the sputtering power supply power is controlled within 10 KW to 20KW (the deposition thickness can be adjusted according to requirements).
Fixing the reinforcing ribs 3 in the electrode area of the graphene layer 2;
and the electrode area of the base layer is fixed with the grid-shaped reinforcing ribs 3 by using a special fixing clamp, and the wire body size can be set according to the over-current, power and temperature requirements of the product.
The fixing of the reinforcing ribs 3 specifically includes the following steps:
S1, placing a substrate 1 on which graphene is deposited in the first step to form a graphene layer 2 at the position of a groove 10 of a lower clamp 6;
S2, fixing two ends of the reinforcing rib 3 on the fixing columns 11 of the lower clamp 6;
And S3, pressing and fixing the base body and the reinforcing ribs 3 by using the upper clamp 7, and finishing the fixing of the reinforcing ribs 3.
Step three, preparing an electrode 4 in an electrode area of the graphene layer 2;
Spraying electrode materials at the hollowed-out position of the upper clamp 7, and covering and fixing the reinforcing ribs 3; and finishing the manufacturing of the heating device.
The electrode material is prepared on the electrode area of the base layer by spraying or brazing, the electrode 4 is formed, the electrode is formed by fully combining and fixing the spraying/brazing process and the graphene, and the specification of the electrode can be set according to the over-current, power and temperature requirements of the product.
And fourthly, plating an anti-oxidation layer 5 on the heating device manufactured in the third step by using a vacuum magnetron sputtering or magnetron sputtering evaporation integrated machine, and completing manufacturing of the heating device. The vacuum degree is controlled within 1.0x10 -2 pa to 4.0x10 -4 pa, the power of a sputtering power supply is controlled within 10 KW to 20KW (the deposition thickness can be adjusted according to the requirement), the oxidation prevention layer 5 is made of aluminum oxide, hexagonal boron nitride and aluminum silicate, and the aluminum oxide, hexagonal boron nitride and aluminum silicate have the advantages of good high temperature resistance, high heat conduction, insulation, high mechanical strength and the like, and can protect the graphene layer 2 from oxidation and decay failure in the high-temperature use process; the thickness of the oxidation preventing layer 5 is 28nm to 1000nm.
After the device is manufactured, the device needs to be tested, and the heating device is tested:
(1) Conductivity test:
direct current resistance: test data of 100 to 500mΩ using direct current resistance instrument test
Square resistance: test data < 20mΩ using an instrument such as ST 2253-type four-probe Fang Zuyi
(2) Oxidation resistance test: the environment product with the high temperature of 1000 ℃ can be kept for more than 5000H.
(3) High temperature resistance test: and testing by using a high-temperature-resistant tester, wherein the temperature resistance of the product is less than 1000 ℃.
(4) Insulation test: and (3) testing by using an insulation voltage withstanding tester, wherein the insulation data of the product is 3-3.6 KV.
After the preparation is finished, the qualified products after the test are subjected to necessary post-treatment, such as vacuum packaging, so that the products are ensured to be transported and stored.
According to the high-temperature graphene flexible heating device manufactured by the technical scheme, the electrode 4 comprises a wire-shaped reinforcing rib 3 material, so that the problem that the electrode 4 is influenced by a base material to deform after being manufactured on a heating plate, and the electrode layer is cracked or defective is solved; the pre-buried wire-shaped reinforcing ribs 3 form good conductive connection with the electrode 4, and the connection ensures smooth transmission of current between the electrode 4 and the heating material, reduces resistance and energy loss and improves the overall conductive efficiency; the built-in reinforcing ribs 3 and the electrodes 4 form a built-in conductive material and electrode combination, so that the strength of the whole conductive electrode unit structure is increased, the reinforced structure can resist external stress and deformation, the efficient, uniform and stable heating effect can be ensured, and the durability and stability of the product are improved.
Embodiment III: referring to the second embodiment, referring to fig. 8, 9, 10 and 14, the reinforcing ribs 3 are in a grid shape, are grid-shaped electrode plates with hexagonal holes, and the hexagonal hole-shaped reinforcing rib structure shows excellent performance effects in the electrode by virtue of the unique geometric shape; the hexagonal holes can effectively disperse current, realize more uniform current distribution, reduce current density and reduce hot spots and local damage caused by current concentration.
Embodiment four: referring to fig. 11, 12, 13 and 14, the reinforcing ribs 3 are in a grid shape, are square hole grid electrode plates, are added with square hole type reinforcing rib structures, and can increase the active area by changing the shape of the electrode surface, so that the electrochemical reaction efficiency is improved; square hole type reinforcing ribs are also beneficial to optimizing the flow path of current, so that the current distribution is more uniform, and the local damage caused by overlarge current density is reduced.
Fifth embodiment: 15-19, the special fixture described above includes:
the lower clamp 6 and the upper clamp 7 which are mutually close to each other, the lower clamp 6 and the upper clamp 7 are rectangular plates, a plurality of positioning columns 8 are arranged on the lower clamp 6, the four positioning columns 8 are distributed at the positions, close to four corners, of the lower clamp 6, and a plurality of positioning holes 9 matched with the positioning columns 8 are formed in the upper clamp 7.
The lower clamp 6 is provided with a groove 10, the groove 10 is used for placing the base body 1, the lower clamp 6 on two opposite sides of the groove 10 is provided with fixing columns 11, the fixing columns 11 are used for fixing the reinforcing ribs 3 in a binding mode and the like, the fixing columns 11 on two opposite sides of the groove 10 are respectively used for fixing two ends of the reinforcing ribs 3, and fixing of the reinforcing ribs 3 on the base body 1 is completed.
The upper clamp 7 is provided with avoidance holes 12 corresponding to the positions of the fixed columns 11, the connecting line position areas of the fixed columns 11 on the two sides of the substrate 1 corresponding to the upper clamp 7 are provided with electrode covering holes 13, a hollowed-out design of the upper clamp 7 is formed, namely, the reinforcing rib areas corresponding to the substrate 1 are formed, the substrate 1 is provided with electrode areas, the electrode areas convenient for preparing the electrode 4 are provided with electrode materials, namely, the hollowed-out positions of the upper clamp 7 are sprayed with electrode materials.
Through the use of anchor clamps, can be quick carry out the clamping to strengthening rib 3 and base member 1 fixedly for two positions are relatively fixed, are favorable to carrying out the preparation of electrode 4, and this anchor clamps simple structure, the simple operation is favorable to improving production efficiency and quality.
In the description of the present invention, it should be understood that the directions or positional relationships indicated by the terms "upper", "lower", "outer", "both sides", "both ends", etc. are based on the directions or positional relationships shown in the drawings, are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention. In the description of the present invention, unless otherwise specified and defined, it should be noted that the term "connected" should be interpreted broadly, and for example, it may be a mechanical connection or an electrical connection, or may be a connection between two elements, or may be a direct connection or may be an indirect connection through an intermediary, and it will be understood to those skilled in the art that the specific meaning of the term may be interpreted according to the specific circumstances.
The foregoing description of the preferred embodiment of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.

Claims (7)

1.一种高温石墨烯柔性加热装置的制备方法,其特征在于,所述高温石墨烯柔性加热装置包括基体(1),所述基体(1)上设置有石墨烯层(2),所述石墨烯层(2)表面设置有电极(4),所述电极(4)内设置有由导电材料制成的加强筋(3);1. A method for preparing a high-temperature graphene flexible heating device, characterized in that the high-temperature graphene flexible heating device comprises a substrate (1), a graphene layer (2) is arranged on the substrate (1), an electrode (4) is arranged on the surface of the graphene layer (2), and a reinforcing rib (3) made of a conductive material is arranged inside the electrode (4); 所述制备方法包括以下步骤:The preparation method comprises the following steps: 步骤一、使用真空磁控溅射设备在基体(1)上沉积石墨烯形成石墨烯层(2);Step 1: using a vacuum magnetron sputtering device to deposit graphene on a substrate (1) to form a graphene layer (2); 步骤二、将加强筋(3)固定在石墨烯层(2)的电极区域;Step 2: fix the reinforcing rib (3) to the electrode region of the graphene layer (2); 步骤三、在石墨烯层(2)的电极区域制备电极(4),与加强筋(3)组成导电电极单元,完成加热装置制作;Step 3: preparing an electrode (4) in the electrode region of the graphene layer (2) and forming a conductive electrode unit with the reinforcing rib (3), thereby completing the production of the heating device; 所述步骤二、将加强筋(3)通过夹具固定在石墨烯层(2)的电极区域的具体过程包括以下步骤:The specific process of the step 2, fixing the reinforcing rib (3) to the electrode region of the graphene layer (2) by means of a clamp, comprises the following steps: S1、将经过步骤一沉积石墨烯形成石墨烯层(2)的基体(1)放置在下夹具(6)的凹槽(10)位置;S1, placing the substrate (1) on which the graphene layer (2) is formed by depositing graphene in step 1, in the groove (10) of the lower fixture (6); S2、将加强筋固定在下夹具(6)的固定柱(11)上;S2, fixing the reinforcing rib on the fixing column (11) of the lower clamp (6); S3、使用上夹具(7)将基体以及加强筋压合固定,完成加强筋固定;S3, using the upper clamp (7) to press and fix the base and the reinforcing ribs to complete the fixing of the reinforcing ribs; 所述步骤三、在石墨烯层(2)的电极区域制备电极(4)的具体过程如下:在上夹具(7)镂空位置喷涂电极材料,将加强筋覆盖固定;完成加热装置制作;The specific process of step 3, preparing the electrode (4) in the electrode region of the graphene layer (2) is as follows: spraying the electrode material on the hollowed-out position of the upper fixture (7) to cover and fix the reinforcing ribs; and completing the production of the heating device; 所述夹具包括相互贴近的下夹具(6)、上夹具(7),在下夹具(6)上开设有若干定位柱(8),在上夹具(7)上开设有若干与定位柱(8)配合的定位孔(9);在下夹具(6)上开设有凹槽(10),凹槽(10)用于放置基体(1),在凹槽(10)相对两侧的下夹具(6)上设置有固定柱(11),固定柱(11)用于固定加强筋(3);在上夹具(7)上对应固定柱(11)的位置开设有避让孔(12),在上夹具(7)上对应的基体(1)上的两侧固定柱(11)连线位置区域开设有电极覆盖孔(13)。The clamp comprises a lower clamp (6) and an upper clamp (7) which are close to each other, a plurality of positioning columns (8) are provided on the lower clamp (6), and a plurality of positioning holes (9) which cooperate with the positioning columns (8) are provided on the upper clamp (7); a groove (10) is provided on the lower clamp (6), and the groove (10) is used to place the substrate (1); fixing columns (11) are provided on the lower clamp (6) on opposite sides of the groove (10), and the fixing columns (11) are used to fix the reinforcing ribs (3); avoidance holes (12) are provided on the upper clamp (7) at positions corresponding to the fixing columns (11), and electrode covering holes (13) are provided in the upper clamp (7) at the position area corresponding to the connection position of the fixing columns (11) on both sides of the substrate (1). 2.根据权利要求1所述的一种高温石墨烯柔性加热装置的制备方法,其特征在于,防氧化层(5)覆盖在石墨烯层(2)以及电极(4)上。2. A method for preparing a high-temperature graphene flexible heating device according to claim 1, characterized in that the anti-oxidation layer (5) covers the graphene layer (2) and the electrode (4). 3.根据权利要求1所述的一种高温石墨烯柔性加热装置的制备方法,其特征在于,所述基体(1)的上表面和下表面均设置有石墨烯层(2),所述石墨烯层(2)对应的电极(4)有两个。3. The method for preparing a high-temperature graphene flexible heating device according to claim 1, characterized in that a graphene layer (2) is provided on both the upper surface and the lower surface of the substrate (1), and there are two electrodes (4) corresponding to the graphene layer (2). 4.根据权利要求1所述的一种高温石墨烯柔性加热装置的制备方法,其特征在于,所述加强筋(3)呈线体状或网格状。4. The method for preparing a high-temperature graphene flexible heating device according to claim 1, characterized in that the reinforcing ribs (3) are in a linear or grid shape. 5.根据权利要求1所述的一种高温石墨烯柔性加热装置的制备方法,其特征在于,加强筋(3)和电极(4)组成导电电极单元,加强筋(3)的填充率占整个导电电极单元的10%至50%,电极厚度1至500um、宽度2mm至12mm。5. The method for preparing a high-temperature graphene flexible heating device according to claim 1, characterized in that the reinforcing rib (3) and the electrode (4) constitute a conductive electrode unit, the filling rate of the reinforcing rib (3) accounts for 10% to 50% of the entire conductive electrode unit, the electrode thickness is 1 to 500 um, and the width is 2 mm to 12 mm. 6.根据权利要求1所述的一种高温石墨烯柔性加热装置的制备方法,其特征在于,在步骤一之前先对基体(1)进行预处理,包括清洗、表面活化。6. The method for preparing a high-temperature graphene flexible heating device according to claim 1, characterized in that the substrate (1) is pretreated before step 1, including cleaning and surface activation. 7.根据权利要求1所述的一种高温石墨烯柔性加热装置的制备方法,其特征在于,步骤四、使用真空磁控溅镀或磁控溅镀蒸镀一体机在加热装置上镀防氧化层(5)。7. The method for preparing a high-temperature graphene flexible heating device according to claim 1, characterized in that, in step 4, an anti-oxidation layer (5) is plated on the heating device using a vacuum magnetron sputtering or a magnetron sputtering and evaporation integrated machine.
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