CN114192073A - Cobalt ferrite composite wave-absorbing material and preparation device thereof - Google Patents
Cobalt ferrite composite wave-absorbing material and preparation device thereof Download PDFInfo
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- CN114192073A CN114192073A CN202111529723.7A CN202111529723A CN114192073A CN 114192073 A CN114192073 A CN 114192073A CN 202111529723 A CN202111529723 A CN 202111529723A CN 114192073 A CN114192073 A CN 114192073A
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- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 40
- 239000010941 cobalt Substances 0.000 title claims abstract description 40
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 40
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 239000011358 absorbing material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000007789 sealing Methods 0.000 claims abstract description 59
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 26
- 230000007246 mechanism Effects 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 18
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims description 39
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 9
- 238000013329 compounding Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 9
- 230000002093 peripheral effect Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 239000002048 multi walled nanotube Substances 0.000 description 5
- 229910002518 CoFe2O4 Inorganic materials 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 125000004434 sulfur atom Chemical group 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910003321 CoFe Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000011218 binary composite Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229940044631 ferric chloride hexahydrate Drugs 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000011206 ternary composite Substances 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
Abstract
The invention provides a cobalt ferrite composite wave-absorbing material and a preparation device thereof, belonging to the technical field of wave-absorbing material production equipment and comprising a mixing mechanism and a composite mechanism; the hydrothermal reaction kettle comprises an outer cylinder, an inner cylinder and a sealing cover, wherein the inner cylinder is arranged in the outer cylinder, and the sealing cover is detachably arranged on the outer cylinder; the sealing cover is suitable for sealing the opening of the outer cylinder body and is provided with a sealing part; the inner cylinder body comprises a first half cylinder and a second half cylinder, and the first half cylinder and the second half cylinder are spliced into a cylindrical structure; a tight-supporting mechanism suitable for tightly supporting the first half barrel and the second half barrel is arranged in the outer barrel body; through the matching of the mixing mechanism and the composite mechanism, the compounding of the cobalt ferrite and the carbon nano tube can be realized, and the wave-absorbing performance of the composite material is improved conveniently; the inner cylinder body can be thoroughly cleaned after the reaction is finished, and the residual substances on the inner cylinder body are reduced, so that the influence on the next use can be reduced.
Description
Technical Field
The invention belongs to the technical field of wave-absorbing material production equipment, and particularly relates to a cobalt ferrite composite wave-absorbing material and a preparation device thereof.
Background
An electromagnetic wave absorbing material is a material that can attenuate an incident electromagnetic wave by its own absorption, and its principle is to convert an electromagnetic wave into energy consumption in other forms such as thermal energy, electric energy, or mechanical energy by medium consumption. In the prior art, carbon nano tubes are compounded on the surfaces of other materials, and the wave-absorbing property of the whole body is improved by utilizing the wave-absorbing property of the carbon nano tubes. When compounding the carbon nano tube, putting the materials into a hydrothermal reaction kettle for reaction; because the volume of the hydrothermal reaction kettle is small, the corner position of the hydrothermal reaction kettle is not cleaned in place when the hydrothermal reaction kettle is cleaned at the later stage, and the influence on the next use can be caused.
Disclosure of Invention
The embodiment of the invention provides a cobalt ferrite composite wave-absorbing material and a preparation device thereof, aiming at solving the technical problem that a reaction kettle cannot be cleaned in place after the preparation of the hydrothermal reaction kettle in the prior art is finished.
In order to achieve the purpose, the invention adopts the technical scheme that:
providing a manufacturing apparatus comprising:
the mixing mechanism is provided with a mixing cavity suitable for mixing materials and a stirring structure suitable for stirring the materials in the mixing cavity; and
the composite mechanism comprises a hydrothermal reaction kettle suitable for containing materials and a temperature control structure suitable for heating the hydrothermal reaction kettle;
the hydrothermal reaction kettle comprises an outer cylinder, an inner cylinder and a sealing cover, wherein the inner cylinder is arranged in the outer cylinder, and the sealing cover is detachably arranged on the outer cylinder; the sealing cover is suitable for sealing the opening of the outer cylinder body, and a sealing part suitable for sealing the opening of the inner cylinder body is arranged on the sealing cover;
the inner cylinder body comprises a first half cylinder and a second half cylinder, and the first half cylinder and the second half cylinder are spliced into a cylindrical structure; a sealing structure is arranged at the splicing position of the first half barrel and the second half barrel; and a tight-supporting mechanism suitable for tightly supporting the first half barrel and the second half barrel is arranged in the outer barrel body.
Preferably, a groove is formed at the splicing position of the first half barrel and the second half barrel, and a protruding part suitable for being inserted into the groove is fixedly arranged on the second half barrel;
when the protruding part is plugged with the groove, the first half barrel and the second half barrel are in mutual contact.
Preferably, the opening of the outer cylinder body is provided with a guide ring suitable for guiding materials, the top of the guide ring is provided with a limit ring suitable for contacting with the opening end of the outer cylinder body, and the inner peripheral wall of the guide ring is provided with a first guide surface suitable for facing the inner cylinder body.
Preferably, the bottom of the guide ring is adapted to abut against the open end of the inner cylinder.
Preferably, the bottom in the outer cylinder body is provided with an elastic part, one end of the elastic part is connected with the bottom of the outer cylinder body, and the other end of the elastic part is abutted against the bottom of the inner cylinder body.
Preferably, the open end of the outer cylinder body is provided with a limiting structure, and the limiting structure is suitable for limiting the guide ring so as to fix the position of the inner cylinder body in the outer cylinder body.
Preferably, the limiting structure comprises a connecting column and a connecting disc fixed at one end of the connecting column, the diameter of the connecting disc is larger than that of the connecting column, and one end of the connecting column, which is far away from the connecting disc, is fixed at the opening end of the outer barrel body;
be equipped with on the spacing ring and be suitable for the first through-hole that the connection pad passed, and follow the second through-hole that the spacing ring circumferencial direction set up, the lateral wall of second through-hole be suitable for with the periphery wall contact of spliced pole.
Preferably, the abutting structure comprises a plurality of arc-shaped parts, and the arc-shaped parts and the outer cylinder body are coaxially arranged; the inner surface of the arc-shaped part is suitable for being in contact with the outer wall surface of the inner cylinder body.
Preferably, a second guide surface for guiding the inner cylinder is arranged at the top of the arc-shaped part.
In the embodiment of the application, when the hydrothermal reaction kettle needs to be cleaned after the reaction is finished, the inner cylinder body can be taken out of the outer cylinder body, then the first half cylinder body and the second half cylinder body are separated, the inner cylinder body can be cleaned conveniently, the inner part of the inner cylinder body is cleaned, the dead angle of the inner cylinder body is reduced, and the condition that the inner cylinder body is used once due to the influence of residual substances can be reduced. The mixing chamber of mixing mechanism can add the water mixture to the material to after the stirring through rabbling mechanism, can make the mixture of material more even. The hydrothermal reaction kettle can realize the compounding of the cobalt ferrite and the carbon nano tube, and is convenient for improving the wave-absorbing performance of the composite material. Through the seal structure between first half bucket and the second half bucket to and through the sealing on the sealed lid, can make interior barrel be in confined state in the use, and then reduce the leakage of material. Through the tight mechanism that supports on the outer barrel body can make first half bucket and the tight laminating of second half bucket be in the same place, and then guarantee the sealing performance after first half bucket and the concatenation of second half bucket.
The invention also provides a cobalt ferrite composite wave-absorbing material which is prepared from the following components in parts by mass: cobalt ferrite: carbon nanotube: copper sulfide: 35-45: 7-12: 1-6.
Compared with the prior art, the preparation device of the cobalt ferrite composite wave-absorbing material provided by the invention can be used for CoFe through the matching of the mixing mechanism and the composite mechanism2O4The surface of the MWCNTs composite wave-absorbing material is subjected to in-situ synthesis to form copper sulfide nano particles, so that the wave-absorbing performance of the composite wave-absorbing material is improved conveniently; the inner cylinder body can be thoroughly cleaned after the reaction is finished, and the residual substances on the inner cylinder body are reduced, so that the influence on the next use can be reduced.
Drawings
FIG. 1 is a schematic structural diagram of a hydrothermal reaction kettle according to an embodiment of the present invention;
FIG. 2 is a schematic sectional view of a hydrothermal reaction kettle according to an embodiment of the present invention;
FIG. 3 is a schematic view of an inner cylinder portion of a hydrothermal reaction kettle according to an embodiment of the present invention;
FIG. 4 is an enlarged view of portion A of FIG. 3;
FIG. 5 is a schematic view of a limiting ring portion of a hydrothermal reaction kettle according to an embodiment of the present invention.
Description of reference numerals: 1. a hydrothermal reaction kettle; 11. an outer cylinder; 12. an inner cylinder; 121. a first half-tub; 1211. a groove; 122. a second half-tub; 1221. a projection; 13. a sealing cover; 131. a sealing part; 2. a guide ring; 21. a first guide surface; 3. a limiting ring; 31. a first through hole; 32. a second through hole; 4. an elastic member; 5. connecting columns; 6. a connecting disc; 7. an arc-shaped portion; 71. a second guide surface.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in 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 5, a device for preparing a cobalt ferrite composite wave-absorbing material according to the present invention will now be described. The preparation device comprises a mixing mechanism and a composite mechanism; the mixing mechanism is provided with a mixing cavity suitable for mixing materials and a stirring structure suitable for stirring the materials in the mixing cavity; the composite mechanism comprises a hydrothermal reaction kettle 1 suitable for containing materials and a temperature control structure suitable for heating the hydrothermal reaction kettle 1; the hydrothermal reaction kettle 1 comprises an outer cylinder body 11, an inner cylinder body 12 and a sealing cover 13, wherein the inner cylinder body 12 is arranged in the outer cylinder body 11, and the sealing cover 13 is detachably arranged on the outer cylinder body 11; the sealing cover 13 is suitable for sealing the opening of the outer cylinder body 11, and the sealing cover 13 is provided with a sealing part 131 suitable for sealing the opening of the inner cylinder body 12; the inner cylinder 12 comprises a first half-cylinder 121 and a second half-cylinder 122, and the first half-cylinder 121 and the second half-cylinder 122 are spliced into a cylindrical structure; a sealing structure is arranged at the splicing position of the first half barrel 121 and the second half barrel 122; the inner of the outer cylinder 11 is provided with a pressing mechanism adapted to press against the first half-barrel 121 and the second half-barrel 122.
In the embodiment of the present application, when the hydrothermal reaction kettle 1 needs to be cleaned after the reaction is completed, the inner cylinder 12 can be taken out from the outer cylinder, and then the first half-barrel 121 and the second half-barrel 122 are separated, so that the inner cylinder 12 can be cleaned, the inside of the inner cylinder 12 is cleaned conveniently, the dead angle of the inner cylinder 12 is reduced, and the situation of one-time use due to the influence of residual substances can be reduced. The mixing chamber of mixing mechanism can add the water mixture to the material to after the stirring through rabbling mechanism, can make the mixture of material more even. The hydrothermal reaction kettle 1 can realize the compounding of the cobalt ferrite and the carbon nano tube, and is convenient for improving the wave-absorbing performance of the composite material. Through the sealing structure between the first half-barrel 121 and the second half-barrel 122 and the sealing part 131 on the sealing cover 13, the inner barrel 12 can be in a closed state in the using process, and further the leakage of materials is reduced. The tight mechanism that supports through on the outer barrel 11 can make first half bucket 121 and second half bucket 122 closely paste together, and then guarantee the sealing performance after first half bucket 121 and the concatenation of second half bucket 122.
Compared with the prior art, the preparation device provided by the invention can realize the compounding of the cobalt ferrite and the carbon nano tube by the matching of the mixing mechanism and the compounding mechanism, and is convenient for improving the wave-absorbing performance of the composite material; after the reaction is completed, the inner cylinder 12 can be thoroughly cleaned, and the residual substances on the inner cylinder 12 can be reduced, so that the influence on the next use can be reduced.
It should be noted that the using steps of the device are as follows: 1. adding a certain mass of carbon nano tubes into a certain amount of glycol, and taking out for later use after ultrasonic dispersion; 2. weighing a certain amount of ferric chloride hexahydrate and cobalt chloride hexahydrate by using an electronic balance, adding the solution into the solution, mechanically stirring the solution until no obvious large particles exist, and pouring the solution into a mixing cavity; 3. stirring the materials in the mixing cavity by a magnetic stirrer to uniformly mix the materials in the mixing cavity; 4. pouring the uniformly mixed materials into a hydrothermal reactionPlacing the hydrothermal reaction kettle 11 in a constant-temperature heating box for testing in the kettle 11; 5. after the reaction is finished, taking out the hydrothermal reaction kettle 1 and cooling to room temperature; 6. pouring the solution after reaction into a centrifuge for centrifugation; 7. taking out the centrifuged substance, and continuously adding ultrapure water and absolute ethyl alcohol by using an ultrasonic cleaning instrument to perform repeated ultrasonic cleaning; 8. finally, drying the cleaned substances through a vacuum drying oven or a blast drying oven, and then obtaining powder for later use; 9. dissolving a certain amount of the powder into a mixed solution of thiourea and copper acetate, mechanically stirring until no obvious large particles exist, and pouring into a mixing cavity; 10. repeating the steps 3-8 to obtain the final CoFe2O4the/MWCNTs/CuS composite wave-absorbing material. Through the steps, the compounding of the cobalt ferrite and the carbon nano tube can be realized, and the wave-absorbing performance of the composite material is improved conveniently.
In some embodiments, as shown in fig. 1 to 5, a groove 1211 is formed at the joint of the first half-barrel 121 and the second half-barrel 122, and a protrusion 1221 adapted to be inserted into the groove 1211 is fixedly disposed on the second half-barrel 122; wherein, when the protrusion 1221 is inserted into the groove 1211, the first half-barrel 121 and the second half-barrel 122 are contacted with each other; the groove 1211 of the first half-tub 121 has a U-shaped configuration, and the protrusion 1221 has a U-shaped configuration; the second half barrel 122 is spliced with the groove 1211 of the first half barrel 121 through the protruding part 1221, the first half barrel 121 and the second half barrel 122 can be spliced into the inner barrel body 12, a sealing ring is arranged at the splicing position of the first half barrel 121 and the second half barrel 122, and the sealing performance of the splicing position of the first half barrel 121 and the second half barrel 122 can be enhanced.
It should be noted that the sealing ring may be disposed in the groove 1211, and after the sealing ring is disposed in the groove 1211, the sealing ring can be abutted against the groove 1211 by inserting the protrusion 1221 into the groove 1211, and the sealing ring is deformed in the groove 1211 under a stress, so that the sealing ring can be in contact with the bottom and the side wall of the groove 1211, and further the sealing performance of the joint of the first half-barrel 121 and the second half-barrel 122 is improved, and the leakage of the material from the joint of the first half-barrel 121 and the second half-barrel 122 is reduced, thereby reducing the waste of the material and improving the utilization rate of the material.
In addition, set up the clamp on the periphery wall of first half bucket 121 and second half bucket 122, after first half bucket 121 and second half bucket 122 splice together, can fix first half bucket 121 and second half bucket 122 through the clamp, be convenient for get first half bucket 121 and second half bucket 122 and put.
In some embodiments, as shown in fig. 1 to 5, a guide ring 2 adapted to guide the material is disposed at the opening of the outer cylinder 11, a stop ring 3 adapted to contact the open end of the outer cylinder 11 is disposed at the top of the guide ring 2, and a first guide surface 21 adapted to face the inner cylinder 12 is disposed on the inner circumferential wall of the guide ring 2; the spacing ring 3 is fixed on the outer wall surface of the guide ring 2, and the spacing ring 3 is positioned at the top of the guide ring 2. The guide ring 2 is arranged on the outer cylinder body 11 to guide the solution, and when the solution is poured into the inner cylinder body 12, the solution can be reduced to be poured into a gap between the inner cylinder body 12 and the outer cylinder body 11, so that the waste of materials can be reduced, and the materials attached to the inner wall of the outer cylinder body 11 can also be reduced.
In some embodiments, as shown in fig. 1 to 5, the bottom of the guide ring 2 is adapted to abut against the opening end of the inner cylinder 12, so that the guide ring 2 and the outer cylinder 11 are matched to limit the inner cylinder 12 in the axial direction, thereby reducing the shaking of the inner cylinder 12 in the using process.
In some embodiments, as shown in fig. 1 to 5, the bottom inside the outer cylinder 11 is provided with an elastic member 4, one end of the elastic member 4 is connected with the bottom of the outer cylinder 11, and the other end of the elastic member 4 abuts against the bottom of the inner cylinder; the elastic member 4 comprises a spring, one end of the spring is fixed at the bottom of the outer cylinder 11, and the other end of the spring abuts against the outer wall surface of the bottom of the inner cylinder 12. By providing the spring in the outer cylinder 11, the open end of the inner cylinder 12 can be ejected out of the outer cylinder 11 when the seal cap 13 is opened, thereby facilitating the removal of the inner cylinder 12 from the outer cylinder 11.
It should be noted that an external thread is provided on the outer circumferential surface of the opening end of the outer cylinder 11, an internal thread is provided on the sealing cover 13, and the sealing cover 13 is in threaded fit with the outer cylinder 11; the sealing portion 131 is fixed inside the sealing cap 13, and after the sealing cap 13 is screwed to the outer cylinder 11, the sealing portion 131 of the sealing cap 13 is positioned in the opening of the inner cylinder 12, so that the sealing portion 131 can seal the opening of the inner cylinder 12.
In addition, a connecting part is fixedly arranged on one side of the sealing cover 13, which is far away from the outer cylinder body 11, and a through hole is formed in the peripheral wall of the connecting part along the diameter direction; the through hole is internally provided with an extension bar, and the two ends of the extension bar penetrate out of the through hole of the connecting part. The length of the extension rod is larger than the diameter of the sealing cover 13, so that the torque of the sealing cover 13 can be increased when the extension rod is rotated, and the rotation of the sealing cover 13 is controlled conveniently by rotating the extension rod; the connection of the sealing cover 13 and the outer cylinder 11 can be made more tight.
The bottom of the outer cylinder 11 has a through hole (not shown) having a diameter smaller than that of the inner cylinder 12, so that the inner cylinder 12 does not slip out of the bottom of the outer cylinder 11 after the inner cylinder 12 is put into the outer cylinder 11. Through the arrangement, after the inner cylinder 12 is placed in the constant-temperature heating box, heat can be contacted with the outer wall surface of the inner cylinder 12 from the through hole at the bottom of the outer cylinder 11, and therefore the wave-absorbing material is convenient to prepare.
In some embodiments, as shown in fig. 1 to 5, the open end of the outer cylinder 11 is provided with a limiting structure, which is adapted to limit the guide ring 2 to fix the position of the inner cylinder 12 in the outer cylinder 11; the limiting structure comprises a connecting column 5 and a connecting disc 6 fixed at one end of the connecting column 5, the diameter of the connecting disc 6 is larger than that of the connecting column 5, and one end of the connecting column 5, which is far away from the connecting disc 6, is fixed at the opening end of the outer barrel body 11; the limiting ring 3 is provided with a first through hole 31 suitable for the connecting disc 6 to pass through and a second through hole 32 arranged along the circumferential direction of the limiting ring 3, and the side wall of the second through hole 32 is suitable for being in contact with the outer circumferential wall of the connecting column 5; after the inner cylinder 12 is placed in the outer cylinder 11, the guide ring 2 is installed at the open end of the outer cylinder 11, and the bottom of the guide ring 2 is in contact with the open end of the inner cylinder 12; then, the guide ring 2 is pressed along the axial direction, so that the limiting ring 3 is contacted with the opening of the outer cylinder body 11, and the connecting disc 6 penetrates through the first through hole 31 of the limiting ring 3; then, the guide ring 2 is rotated to position the connecting post 5 in the second through hole 32, and the bottom of the connecting plate 6 contacts with the top of the limiting ring 3, so that the guide ring 2 can be fixed on the outer cylinder 11. Through the arrangement, the inner cylinder body 12 cannot be ejected out of the outer cylinder body 11 under the elastic force of the spring in the process of opening the sealing cover 13; through reverse guide ring 2, when connection pad 6 is located first through-hole 31, can take out guide ring 2 from outer barrel 11, at this moment, interior barrel 12 can slide out outer barrel 11 under the effect of spring, is convenient for take out interior barrel 12, and can reduce the condition of barrel 11 outside barrel 12 slips out suddenly of interior barrel 12.
In some embodiments, as shown in fig. 1 to 5, the abutting structure includes a plurality of arc portions 7, the arc portions 7 are coaxially disposed with the outer cylinder 11, and the plurality of arc portions 7 are uniformly arranged along the circumferential direction of the outer cylinder 11; the inner surface of the arc-shaped part 7 is suitable for contacting with the outer wall surface of the inner cylinder 12; the top of the arc part 7 is provided with a second guide surface 71 for guiding the inner cylinder 12; when placing interior barrel 12, the second guide surface 71 on the arc portion 7 can guide interior barrel 12 for the outer wall of interior barrel 12 contacts with the internal surface of a plurality of arc portions 7, and then is convenient for carry on spacingly radially to interior barrel 12, avoids appearing the condition that first half bucket 121 and second half bucket 122 separated.
It should be noted that, the abutting structure may be an abutting ring (not shown in the figure), the outer circumferential wall of the abutting ring is fixed on the inner circumferential wall of the outer cylinder 11, and the inner circumferential wall of the abutting ring is suitable for contacting with the outer circumferential wall of the inner cylinder 12, so that the first half-barrel 121 and the second half-barrel 122 can be circumferentially limited, so that the first half-barrel 121 and the second half-barrel 122 are tightly matched together, the leakage of the material from the joint of the first half-barrel 121 and the second half-barrel 122 is reduced, and the preparation of the wave-absorbing material is facilitated.
In addition, the upper surface of the abutting ring is a second guide surface, the second guide surface can be connected with the top of the outer peripheral wall of the abutting ring and the top of the inner peripheral wall of the abutting ring, and the top of the outer peripheral wall of the abutting ring can be smoothly transited to the top of the inner peripheral wall of the abutting ring; when placing outer barrel 11 with interior barrel 12 in, the bottom of interior barrel 12 contacts with the second guide face that supports tight ring earlier, and the second guide face can lead interior barrel 12 just for interior barrel 12 with support tight ring and peg graft, and then make and support tight ring and carry out circumference spacing to interior barrel 12, consequently can make first half bucket 121 and the connection of second half bucket 122 more stable.
The invention also provides a cobalt ferrite composite wave-absorbing material which is prepared from the following components in parts by mass: cobalt ferrite: carbon nanotube: copper sulfide: 35-45: 7-12: 1-6. More specifically, cobalt ferrite: carbon nanotube: the ratio of the copper sulfide in parts by weight is as follows: 39: 9: 2. when the cobalt ferrite/carbon nano tube reacts with copper sulfide, the structure of the cobalt ferrite is changed, the structure of the cobalt ferrite is more compact from loose pellets, and the particle size of the cobalt ferrite pellets in the composite product is reduced. The particle size of the cobalt ferrite in the wave-absorbing material is 100-150 mm. Copper sulfide nanoparticles are attached to the surface of the cobalt ferrite in the wave-absorbing material (the reason that copper sulfide is attached to the surface of the cobalt ferrite is that a new covalent bond is formed between a sulfur atom and an oxygen atom in the solvothermal reaction process).
When electromagnetic waves are incident, the cobalt ferrite mainly exerts the magnetic loss capacity, the carbon nano tubes are connected with the cobalt ferrite beads to form a net structure, so that the electron flow is increased, the conductivity inside the material is improved, and the conductive loss capacity and the dielectric loss capacity of the material are improved. The copper sulfide nanoparticles play the advantages of the P-type semiconductor, on one hand, the function of improving dielectric energy is achieved, on the other hand, copper sulfide is attached to the surface of the material, and certain influence is generated on the morphology structure of the material, so that the magnetic conductivity of the material is improved, and the impedance matching characteristic of the composite wave-absorbing material is further improved. The electrical properties of the components of the cobalt ferrite and the carbon nano tube have larger difference, a plurality of interfaces can be generated among the cobalt ferrite, the carbon nano tube and the copper sulfide, the interface polarization capability of the material is enhanced, and the interface polarization loss capability is further improved.
In the preparation process, the cobalt ferrite and the carbon nano tube both show excellent chemical stability, the phase of the cobalt ferrite is not changed, and the structure of the cobalt ferrite bead is changed from loose to compact. The sulfur atoms in the copper sulfide nanoparticles form chemical bonds with the oxygen atoms in the cobalt ferrite, resulting in a tight bond between the two. Copper sulfide in CoFe2O4the/MWCNTs/CuS composite wave-absorbing material has the function of adjusting electromagnetic parameters, and CoFe2O4After copper sulfide is attached to the surface of the/MWCNTs binary composite wave-absorbing material, the electric loss and energy consumption at the high frequency position of the materialThe force is weakened, but the magnetic loss capacity is enhanced, and the impedance matching characteristic of the material is improved, so that the wave absorbing performance of the material is improved. After optimization, 40% of wave absorber addition amount of CoFe2O4the/MWCNTs/CuS ternary composite wave-absorbing material has excellent wave-absorbing performance, and the maximum wave-absorbing bandwidth is 4GHz (14-18GHz) at the position where the material matching thickness is 1.33 mm; when the matching thickness is 1.35mm, there is a minimum reflection loss of-66.37 dB at a frequency of 15.6 GHz. Therefore, the wave-absorbing material is a wave-absorbing material with excellent performance.
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. The cobalt ferrite composite wave-absorbing material is characterized by comprising the following components in parts by mass: cobalt ferrite: carbon nanotube: copper sulfide: 35-45: 7-12: 1-6.
2. A device for preparing the cobalt ferrite composite wave-absorbing material of claim 1, which comprises:
the mixing mechanism is provided with a mixing cavity suitable for mixing materials and a stirring structure suitable for stirring the materials in the mixing cavity; and
the composite mechanism comprises a hydrothermal reaction kettle suitable for containing materials and a temperature control structure suitable for heating the hydrothermal reaction kettle;
the hydrothermal reaction kettle comprises an outer cylinder, an inner cylinder and a sealing cover, wherein the inner cylinder is arranged in the outer cylinder, and the sealing cover is detachably arranged on the outer cylinder; the sealing cover is suitable for sealing the opening of the outer cylinder body, and a sealing part suitable for sealing the opening of the inner cylinder body is arranged on the sealing cover;
the inner cylinder body comprises a first half cylinder and a second half cylinder, and the first half cylinder and the second half cylinder are spliced into a cylindrical structure; a sealing structure is arranged at the splicing position of the first half barrel and the second half barrel; and a tight-supporting mechanism suitable for tightly supporting the first half barrel and the second half barrel is arranged in the outer barrel body.
3. The apparatus for preparing cobalt ferrite composite wave-absorbing material according to claim 2, wherein a groove is provided at the joint of the first half barrel and the second half barrel, and a protrusion adapted to be inserted into the groove is fixedly provided on the second half barrel;
when the protruding part is plugged with the groove, the first half barrel and the second half barrel are in mutual contact.
4. The apparatus according to claim 2, wherein a guide ring adapted to guide the material is disposed at the opening of the outer cylinder, a stop ring adapted to contact with the opening end of the outer cylinder is disposed at the top of the guide ring, and a first guide surface adapted to face the inner cylinder is disposed on the inner circumferential wall of the guide ring.
5. The apparatus for preparing cobalt ferrite composite wave-absorbing material according to claim 4, wherein the bottom of the guiding ring is adapted to abut against the open end of the inner cylinder.
6. The apparatus according to claim 5, wherein an elastic member is disposed at the bottom of the outer cylinder, one end of the elastic member is connected to the bottom of the outer cylinder, and the other end of the elastic member abuts against the bottom of the inner cylinder.
7. The apparatus according to claim 6, wherein a limiting structure is provided at the open end of the outer cylinder, and the limiting structure is adapted to limit the guiding ring to fix the position of the inner cylinder in the outer cylinder.
8. The device for preparing the cobalt ferrite composite wave-absorbing material as claimed in claim 7, wherein the limiting structure comprises a connecting column and a connecting disc fixed at one end of the connecting column, the diameter of the connecting disc is larger than that of the connecting column, and one end of the connecting column, which is far away from the connecting disc, is fixed at the opening end of the outer cylinder;
be equipped with on the spacing ring and be suitable for the first through-hole that the connection pad passed, and follow the second through-hole that the spacing ring circumferencial direction set up, the lateral wall of second through-hole be suitable for with the periphery wall contact of spliced pole.
9. The apparatus for preparing cobalt ferrite composite wave-absorbing material according to claim 2, wherein the abutting structure comprises a plurality of arc-shaped parts, and the arc-shaped parts are coaxially arranged with the outer cylinder; the inner surface of the arc-shaped part is suitable for being in contact with the outer wall surface of the inner cylinder body.
10. The apparatus for preparing cobalt ferrite composite wave-absorbing material according to claim 9, wherein the top of the arc-shaped portion is provided with a second guiding surface for guiding the inner cylinder.
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