Controllable preparation method and equipment for ferroferric oxide coating on surface of nitrogen-doped carbon fiber

Abstract

The invention relates to a controllable preparation method and equipment for a ferroferric oxide coating on the surface of nitrogen-doped carbon fiber, which can enable nanometer ferroferric oxide dispersion liquid to be sprayed in a vapor flow state, and cover the wall surface of a nitrogen-doped carbon fiber composite nanometer film in a balanced thickness and flush manner under the action of increasing pressure intensity. Moreover, gaps and side walls of the nitrogen-doped carbon fiber composite nano-film can be completely sprayed, and the equivalence of the wave-absorbing performance of the nitrogen-doped carbon fiber composite nano-film is efficiently improved, so that the wave-absorbing performance is balanced, and the synergistic wave-absorbing effect is good.

Description

Technical Field

[0001] The invention belongs to the technical field of nitrogen-doped carbon fibers, and in particular relates to a controllable preparation method and equipment for a ferroferric oxide coating on the surface of a nitrogen-doped carbon fiber. Background Art

[0002] With the advent of the information age, the harmfulness of electromagnetic radiation has attracted widespread attention. Absorbing materials refer to materials that can absorb and attenuate electromagnetic waves. Carbon fiber, as an electrically lossy absorbing material, has a certain ability to absorb electromagnetic waves. It plays an important role and has great application potential in the absorption of electromagnetic waves in civil buildings and military equipment. However, the complex dielectric constant of carbon fiber is too large, the wave impedance is very small, and the absorbing performance is not ideal.

[0003] Generally speaking, there are two ways to improve the wave absorption performance of carbon fiber. One is to modify the surface of carbon fiber with a carbon-containing coating with moderate resistivity, and the other is to use a magnetic coating compounded on the surface of carbon fiber. Both coatings are designed to improve the wave impedance of carbon fiber, thereby improving the wave absorption performance and having a good synergistic wave absorption effect. However, it is very technically difficult to construct a structurally stable carbon / magnetic heterogeneous coating on the surface of nitrogen-doped carbon fiber.

[0004] Specifically, at present, as in the nitrogen-doped carbon fiber composite nanofilm prepared with patent application number "CN202011386329.8", a carbon / magnetic heterogeneous coating is constructed by spraying a nano-iron tetroxide dispersion on the nitrogen-doped carbon fiber composite nanofilm. The previous spraying scheme of the nitrogen-doped carbon fiber composite nanofilm is to use a row of nozzles to spray the nitrogen-doped carbon fiber composite nanofilm. The nano-iron tetroxide dispersion sprayed by this method is uneven in thickness and size, and cannot ensure the equality of the absorbing performance of the nitrogen-doped carbon fiber composite nanofilm, thereby resulting in defects of uneven absorbing performance and poor synergistic absorbing effect. Summary of the invention

[0005] In order to overcome the defects in the prior art, the present invention proposes a controllable preparation method and equipment for the ferroferric oxide coating on the surface of nitrogen-doped carbon fiber, which can allow the nano-ferroferric oxide dispersion to be sprayed out in a vapor state, and under the action of increased pressure, the thickness and size are evenly and evenly covered on the wall of the nitrogen-doped carbon fiber composite nanofilm, and the gaps and side walls of the nitrogen-doped carbon fiber composite nanofilm can be sprayed completely, which effectively improves the equality of the absorbing performance of the nitrogen-doped carbon fiber composite nanofilm, so that the absorbing performance is balanced and the synergistic absorbing effect is good.

[0006] The present invention uses the following technical solutions.

[0007] A controllable preparation method of a ferroferric oxide coating on the surface of a nitrogen-doped carbon fiber, comprising: Step 1: Place the nitrogen-doped carbon fiber composite nanofilm 31 to be sprayed with nano-ferroferric oxide dispersion in a closed containing chamber 22, and place the bottom of the equipment component 21 in a heating furnace for heating treatment; Step 2: Sprinkle the nano-ferroferric oxide dispersion in a vapor state into the closed receiving chamber 22 through the dispersion outlet 41 of the nano-ferroferric oxide dispersion; Step 3: The pulling operation sheet 51 moves downward to increase the air pressure acting on the nitrogen-doped carbon fiber composite nano-film 31 in the closed containing chamber 22, so that the vapor-state nano-ferroferric oxide dispersion is evenly covered on the wall surface of the nitrogen-doped carbon fiber composite nano-film 31; Step 4: After the temperature treatment, take out the nitrogen-doped carbon fiber composite nanofilm 31 and pull the running sheet 51 to restore; Step 5: Take out the nitrogen-doped carbon fiber composite nanofilm 31, turn it over and put it back into the closed containing chamber 22, and then perform steps 2 to 4 once to achieve a controllable preparation method of the nitrogen-doped carbon fiber surface ferroferric oxide coating.

[0008] Preferably, the particle size of the ferroferric oxide in the nano ferroferric oxide dispersion is 10 nm to 20 nm, and the weight percentage of the nano ferroferric oxide in the nano ferroferric oxide dispersion is 20% to 25%.

[0009] Preferably, the method of temperature treatment is: heating to 650-850° C. at a heating rate of 2-4° C. / min and heating for 2-5 hours.

[0010] A controllable preparation device for a ferroferric oxide coating on the surface of a nitrogen-doped carbon fiber, comprising: The device component 21 comprises a closed containing chamber 22 of aluminum alloy material for placing a nitrogen-doped carbon fiber composite nanofilm 31, wherein the nitrogen-doped carbon fiber composite nanofilm 31 is placed in the middle of the lower wall of the closed containing chamber 22; a plurality of dispersion output holes 41 for sprinkling a vapor-state nano-ferroferric oxide dispersion into the closed containing chamber 22 are arranged on the side wall of the device component 21; a running plate 51 for increasing the pressure of the closed containing chamber 22 is movably arranged on the upper part of the device component 21, and the running plate 51 runs vertically along the inner surface of the device component 21.

[0011] Preferably, the dispersion liquid output hole 41 includes a plurality of output holes 42 arranged on one side of the equipment component 21 and a plurality of output holes 43 arranged on the other side of the equipment component 21. The output holes 42 are horizontally distributed in a row and are equidistantly arranged, and the output holes 43 are also horizontally distributed in a row and are equidistantly arranged.

[0012] Preferably, the number of the output hole 1 42 and the output hole 2 43 is determined by the size of the specific device component 21 .

[0013] Preferably, the output hole 1 42 and the output hole 2 43 are respectively arranged at locations with the same vertical span from the bottom wall of the closed receiving chamber.

[0014] Preferably, the dispersion liquid output hole 41 is provided with an ultrasonic vaporizer 61, and the ultrasonic vaporizer 61 is connected to a tank containing liquid nano-ferroferric oxide dispersion liquid via a strip-shaped passage penetrating at both ends.

[0015] Preferably, a swing pressure valve 71 is installed in the dispersion liquid output hole 41 .

[0016] Preferably, a guide piece 23 is installed on the inner side wall of the equipment component 21, and the guide pieces 23 are laterally distributed in a row and arranged equidistantly, and a strip guide opening corresponding to the guide piece 23 is installed on the side wall of the running piece 51, and the guide piece 23 is movably connected to the strip guide opening.

[0017] Preferably, a traction device for pulling the running piece 51 is also installed in the equipment component 21 , and the traction device is fixedly connected to the upper part of the equipment component 21 , and the output end of the traction device is fixedly connected or movably connected to the running piece 51 .

[0018] Preferably, the traction device 81 is a reciprocating piston, the output end of the reciprocating piston is fixedly connected to the upper part of the running piece 51, and the reciprocating piston telescopes to pull the running piece 51 to run vertically; The traction device 81 can also be a traction motor, a lead screw is installed at the output end of the traction motor, a threaded opening threadedly connected to the lead screw is installed on the running piece 51, and the lead screw rotates to pull the running piece 51 to run vertically.

[0019] Preferably, a cover plate 24 is mounted on the device component 21 .

[0020] The beneficial effect of the present invention is that, compared with the prior art, the present invention allows the nano-ferroferric oxide dispersion to be sprayed out in a vapor state, and under the action of increased pressure, the thickness and size are evenly and evenly covered on the wall surface of the nitrogen-doped carbon fiber composite nanofilm 31, and the gaps and side walls of the nitrogen-doped carbon fiber composite nanofilm 31 can be sprayed completely, which effectively improves the equality of the absorbing performance of the nitrogen-doped carbon fiber composite nanofilm 31, thereby making the absorbing performance balanced and the synergistic absorbing effect good. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 It is an overall schematic diagram of the controllable preparation method of the nitrogen-doped ferroferric oxide coating on the wall of carbon fiber described in the present invention; Figure 2 It is a side view of the controllable preparation equipment structure of the nitrogen-doped ferroferric oxide coating on the wall of the carbon fiber in the present invention. Implementation

[0022] In order to make the purpose, technical solution and advantages of the present invention clearer, the technical solution of the present invention will be clearly and completely expressed in combination with the drawings in the embodiments of the present invention. The embodiments expressed in this application are only embodiments of a part of the present invention, not all embodiments. Based on the spirit of the present invention, other embodiments obtained by ordinary technicians in this field without making creative work are all within the scope of protection of the present invention.

[0023] like Figure 1 As shown, the controllable preparation method of a ferroferric oxide coating on the surface of a nitrogen-doped carbon fiber according to the present invention comprises: Step 1: Place the nitrogen-doped carbon fiber composite nanofilm 31 to be sprayed with nano-ferroferric oxide dispersion in a closed containing chamber 22, and place the bottom of the equipment component 21 in a heating furnace for heating treatment; Step 2: Sprinkle the nano-ferroferric oxide dispersion in a vapor state into the closed receiving chamber 22 through the dispersion outlet 41 of the nano-ferroferric oxide dispersion; Step 3: The pulling operation sheet 51 moves downward to increase the air pressure acting on the nitrogen-doped carbon fiber composite nano-film 31 in the closed containing chamber 22, so that the vapor-state nano-ferroferric oxide dispersion is evenly covered on the wall surface of the nitrogen-doped carbon fiber composite nano-film 31; Step 4: After the temperature treatment, take out the nitrogen-doped carbon fiber composite nanofilm 31 and pull the running sheet 51 to restore; Step 5: Take out the nitrogen-doped carbon fiber composite nanofilm 31, turn it over and put it back into the closed containing chamber 22, and then perform steps 2 to 4 once to achieve a controllable preparation method of the nitrogen-doped carbon fiber surface ferroferric oxide coating.

[0024] In a specific embodiment, the ferrosoferric oxide coating on the surface of the nitrogen-doped carbon fiber obtained by the present method has a reflectivity of R<-10dB in several randomly set areas in the coating from 4.92 to 16 GHz, and the frequency bandwidth of the reflectivity <-12 dB is 14.24 GHz; the maximum absorption peak is at 11.6 GHz, and the reflectivity R is -24.76 dB, which illustrates the equivalence of the wave absorbing properties of the nitrogen-doped carbon fiber composite nanofilm 31 in this embodiment obtained by the present invention.

[0025] The controllable preparation method of the ferroferric oxide coating on the surface of the nitrogen-doped carbon fiber of the present invention allows the nano-ferroferric oxide dispersion to be sprayed out in a vapor state, and under the action of increased pressure, the thickness and size are evenly and evenly covered on the wall surface of the nitrogen-doped carbon fiber composite nanofilm 31, and the gaps and side walls of the nitrogen-doped carbon fiber composite nanofilm 31 can be sprayed completely, which effectively improves the equality of the absorbing performance of the nitrogen-doped carbon fiber composite nanofilm 31, thereby making the absorbing performance balanced and the synergistic absorbing effect good.

[0026] In a preferred but non-limiting embodiment of the present invention, the particle size of the ferroferric oxide in the nano-ferroferric oxide dispersion is 10 nm to 20 nm, and the weight percentage of the nano-ferroferric oxide in the nano-ferroferric oxide dispersion is 20% to 25%.

[0027] In a preferred but non-limiting embodiment of the present invention, the method of temperature treatment is: heating to 650-850° C. at a heating rate of 2-4° C. / min and heating for 2-5 hours.

[0028] like Figure 2 As shown, the controllable preparation device of the ferroferric oxide coating on the surface of the nitrogen-doped carbon fiber according to the present invention comprises: The device component 21 comprises a closed containing chamber 22 of aluminum alloy material for placing a nitrogen-doped carbon fiber composite nanofilm 31, wherein the nitrogen-doped carbon fiber composite nanofilm 31 is placed in the middle of the lower wall of the closed containing chamber 22; a plurality of dispersion output holes 41 for sprinkling a vapor-state nano-ferroferric oxide dispersion into the closed containing chamber 22 are arranged on the side wall of the device component 21; a running plate 51 for increasing the pressure of the closed containing chamber 22 is movably arranged on the upper part of the device component 21, and the running plate 51 runs vertically along the inner surface of the device component 21.

[0029] In a preferred but non-limiting embodiment of the present invention, the dispersion liquid output hole 41 includes a plurality of output holes 42 arranged on one side of the equipment component 21 and a plurality of output holes 43 arranged on the other side of the equipment component 21, the output holes 42 are horizontally distributed in a row and are equidistantly arranged, and the output holes 43 are also horizontally distributed in a row and are equidistantly arranged.

[0030] In a preferred but non-restrictive embodiment of the present invention, the number of the output hole 1 42 and the output hole 2 43 is determined by the size of the specific equipment component 21, and sufficient output holes are installed for spraying to ensure that the sprayed vapor-state nano-iron tetroxide dispersion can be evenly dispersed in the closed containing chamber 22, thereby ensuring that the nano-iron tetroxide dispersion can be evenly covered on the wall surface of the nitrogen-doped carbon fiber composite nanofilm 31 after the pressure is increased.

[0031] In a preferred but non-limiting embodiment of the present invention, the output hole 1 42 and the output hole 2 43 are both disposed at the same location with a vertical span from the bottom wall of the closed containing chamber. The output holes for spraying on both sides are disposed at the same location with a vertical span from the bottom wall of the closed containing chamber, thereby ensuring that the sprayed vapor-state nano-iron oxide dispersion can also be disposed at the same location with a vertical span from the bottom wall of the closed containing chamber, and similarly ensuring that the nano-iron oxide dispersion on the wall surface of the nitrogen-doped carbon fiber composite nano-film 31 is evenly covered by the dispersion after deposition and spraying.

[0032] In a preferred but non-limiting embodiment of the present invention, an ultrasonic vaporizer 61 is installed at the dispersion output hole 41, and the ultrasonic vaporizer 61 is connected to a tank containing liquid nano-ferroferric oxide dispersion via a strip-shaped passage that penetrates both ends.

[0033] In a preferred but non-limiting embodiment of the present invention, a swing pressure valve 71 is installed in the dispersion output hole 41 to ensure the sealing of the equipment component 21.

[0034] In a preferred but non-restrictive embodiment of the present invention, a guide piece 23 is installed on the inner side wall of the equipment component 21, and the guide pieces 23 are horizontally distributed in a row and equidistantly arranged. A strip guide opening corresponding to the guide piece 23 is installed on the side wall of the running piece 51, and the guide piece 23 and the strip guide opening are movably connected. The guide piece 23 can achieve a guiding function for the vertical operation of the running piece 51, and can also improve the smoothness of the running piece 51 during operation.

[0035] In a preferred but non-limiting embodiment of the present invention, a traction device for pulling the running piece 51 is also installed in the equipment component 21, and the traction device is fixedly connected to the upper part of the equipment component 21, and the output end of the traction device is fixedly connected or movably connected to the running piece 51.

[0036] In a preferred but non-limiting embodiment of the present invention, the traction device 81 is a reciprocating piston, the output end of the reciprocating piston is fixedly connected to the upper part of the running piece 51, and the reciprocating piston telescopically pulls the running piece 51 to run vertically; The traction device 81 can also be a traction motor, a lead screw is installed at the output end of the traction motor, a threaded opening threadedly connected to the lead screw is installed on the running piece 51, and the lead screw rotates to pull the running piece 51 to run vertically.

[0037] In a preferred but non-limiting embodiment of the present invention, a cover plate 24 is installed on the equipment component 21, and the nitrogen-doped carbon fiber composite nano film 31 to be sprayed or already sprayed can be placed in or taken out through the cover plate 24.

[0038] The beneficial effect of the present invention is that, compared with the prior art, the present invention allows the nano-ferroferric oxide dispersion to be sprayed out in a vapor state, and under the action of increased pressure, the thickness and size are evenly and evenly covered on the wall surface of the nitrogen-doped carbon fiber composite nanofilm 31, and the gaps and side walls of the nitrogen-doped carbon fiber composite nanofilm 31 can be sprayed completely, which effectively improves the equality of the absorbing performance of the nitrogen-doped carbon fiber composite nanofilm 31, thereby making the absorbing performance balanced and the synergistic absorbing effect good.

[0039] The present disclosure can be a system, method and / or computer program product. The computer program product can include a computer-readable medium carrying computer-readable program instructions for causing a processor to achieve each aspect of the present disclosure.

[0040] The computer readable storage medium can be a tangible storage medium capable of holding and storing instructions for use by the instruction execution circuit. The computer readable storage medium can be, but is not limited to, an electrical storage medium, a magnetic storage medium, an optical storage medium, an electromagnetic storage medium, a semiconductor storage medium, or any suitable combination thereof. Further examples (not an exhaustive list) of computer readable storage mediums include: a portable computer disk, a hard disk, a random access memory (RAM), a read-only memory (RyM), an erasable programmable read-only memory (EPRyM or flash memory), a static random access memory (SRAM), a portable compact disk read-only memory (HD-RyM), a digital versatile disk (DXD), a memory stick, a floppy disk, a mechanically encoded storage medium, such as a punch card or a raised structure in a groove with instructions stored thereon, and any suitable combination thereof. The computer readable medium used herein is not to be construed as transient information per se, such as radio waves or other freely propagating electromagnetic waves, electromagnetic waves propagating through waveguides or other transmission media (e.g., light pulses through power line cables), or electrical information transmitted through wires.

[0041] The computer readable program instructions expressed herein can be downloaded from the computer readable attached medium to each computing / processing grid line, or downloaded to an external computer or external attached grid line through a wireless network, such as the Internet, a local area network, a wide area network and / or a wireless network. The wireless network can include copper transmission cables, power line transmission, wireless transmission, routers, firewalls, switches, WIFI device computers and / or edge servers. The wireless network adapter card or wireless network port in each computing / processing grid line receives the computer readable program instructions from the wireless network and forwards the computer readable program instructions to be stored in the computer readable attached medium in each computing / processing grid line.

[0042] The computer program instructions for performing the operations of the present disclosure can be assembler instructions, instruction set architecture (ISA) instructions, machine instructions, machine-specific instructions, microcode, firmware instructions, conditional definition values, or source code or object code written in any combination of one or more programming languages, including object-oriented programming languages ​​such as SdallqalA, H++, etc., and conventional procedural programming languages ​​such as "H' language or similar programming languages. The computer readable program instructions can be executed entirely on the client computer, partially on the client computer, as a single software package, partially on the client computer and partially on a remote computer. The computer may be executed on the client computer, or entirely on a remote computer or server. In the case of a remote computer, the remote computer may be connected to the client computer via any wireless network, including a local area network (LAb) or a wide area network (UAb), or may be connected to an external computer (such as using an Internet service provider to connect via the Internet). In some embodiments, the electronic circuit may be customized by using the operating values ​​of computer-readable program instructions, such as a programmable logic circuit, a field programmable gate array (processing platform) or a programmable logic array (PLA), and the electronic circuit may execute computer-readable program instructions to achieve each aspect of the fee disclosure.

[0043] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the above embodiments, ordinary technicians in the relevant field should understand that the specific implementation methods of the present invention can still be modified or updated equivalently, and any modifications or equivalent updates that do not deviate from the spirit and range of the present invention should be covered within the protection range of the claims of the present invention.

Claims

1. A controllable preparation method of a ferroferric oxide coating on the surface of a nitrogen-doped carbon fiber, characterized in that: include: Step 1: Place the nitrogen-doped carbon fiber composite nanofilm to be sprayed with nano-ferroferric oxide dispersion in a closed containing chamber, and place the bottom of the equipment component in a heating furnace for heating treatment; Step 2: Sprinkle the nano-ferroferric oxide dispersion in a vapor state into the closed containing chamber through the dispersion outlet of the nano-ferroferric oxide dispersion; Step 3: The pulling operation sheet moves downward to increase the air pressure acting on the nitrogen-doped carbon fiber composite nanofilm in the closed containing chamber, so that the vapor-state nano-iron tetroxide dispersion is evenly covered on the wall surface of the nitrogen-doped carbon fiber composite nanofilm; Step 4: After the temperature treatment, take out the nitrogen-doped carbon fiber composite nanofilm and pull the running sheet to restore; Step 5: Take out the nitrogen-doped carbon fiber composite nanofilm, turn it over and put it back into the closed holding chamber, and then perform steps 2 to 4 once to complete the controllable preparation method of the nitrogen-doped carbon fiber surface ferroferric oxide coating.

2. The controllable preparation method of the ferroferric oxide coating on the surface of the nitrogen-doped carbon fiber according to claim 1 is characterized in that: The particle size of the ferroferric oxide in the nano-ferroferric oxide dispersion is 10 nm to 20 nm, and the weight percentage of the nano-ferroferric oxide in the nano-ferroferric oxide dispersion is 20% to 25%.

3. The controllable preparation method of the ferroferric oxide coating on the surface of the nitrogen-doped carbon fiber according to claim 1, characterized in that: The method of heating treatment is: heating to 650-850°C at a heating rate of 2-4°C / min and heating for 2-5h.

4. A controllable preparation device for a ferroferric oxide coating on the surface of a nitrogen-doped carbon fiber, characterized in that: include: The device component comprises a closed containing chamber for placing an aluminum alloy material of a nitrogen-doped carbon fiber composite nanofilm, wherein the nitrogen-doped carbon fiber composite nanofilm is placed in the middle of the lower wall in the closed containing chamber; a plurality of dispersion liquid output holes for sprinkling a vapor-state nano-ferroferric oxide dispersion into the closed containing chamber are arranged on the side wall of the device component; an operating plate for increasing the pressure of the closed containing chamber is movably arranged on the upper part of the device component, and the operating plate runs vertically along the inner surface of the device component.

5. The controllable preparation device for the ferroferric oxide coating on the surface of nitrogen-doped carbon fiber according to claim 4, characterized in that: The dispersion liquid output holes include a plurality of output holes 1 arranged on one side of the device component and a plurality of output holes 2 arranged on the other side of the device component. The output holes 1 are horizontally distributed in a row and are equidistantly arranged, and the output holes 2 are also horizontally distributed in a row and are equidistantly arranged.

6. The controllable preparation device for the ferroferric oxide coating on the surface of nitrogen-doped carbon fiber according to claim 5, characterized in that: The number of the output hole 1 and the output hole 2 is determined by the size of the specific device component.

7. The controllable preparation device for the ferroferric oxide coating on the surface of nitrogen-doped carbon fiber according to claim 5, characterized in that: The output hole 1 and the output hole 2 are respectively arranged at locations with the same vertical span from the bottom wall of the closed receiving chamber; The dispersion liquid output hole is provided with an ultrasonic vaporizer, and the ultrasonic vaporizer is connected to a tank body containing liquid nano-ferroferric oxide dispersion liquid via a strip-shaped passage penetrating at both ends.

8. The controllable preparation device for the ferroferric oxide coating on the surface of nitrogen-doped carbon fiber according to claim 5, characterized in that: A swing pressure valve is installed in the dispersion liquid output hole; The inner side wall of the equipment component is provided with guide plates, which are laterally distributed in a row and equidistantly arranged. The side wall of the running plate is provided with strip guide openings corresponding to the guide plates, and the guide plates are movably connected with the strip guide openings.

9. The controllable preparation device for the ferroferric oxide coating on the surface of nitrogen-doped carbon fiber according to claim 5, characterized in that: The equipment component is also provided with a traction device for traction of the running piece, the traction device is fixedly connected to the upper part of the equipment component, and the output end of the traction device is fixedly connected or movably connected to the running piece.

10. The controllable preparation device for the ferroferric oxide coating on the surface of nitrogen-doped carbon fiber according to claim 9, characterized in that: The traction device is a reciprocating piston, the output end of the reciprocating piston is fixedly connected to the upper part of the running piece, and the reciprocating piston is telescopically pulled to pull the running piece to run vertically; The traction device can also be a traction motor, a lead screw is installed at the output end of the traction motor, a threaded opening connected to the lead screw is installed on the running piece, and the lead screw rotates to pull the running piece to run vertically; A cover plate is arranged on the equipment component.

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