CN115611316B - Rod-shaped composite manganese oxide radar wave absorbent and preparation method and application thereof - Google Patents
Rod-shaped composite manganese oxide radar wave absorbent and preparation method and application thereof Download PDFInfo
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- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 title claims abstract description 87
- 239000002131 composite material Substances 0.000 title claims abstract description 52
- 230000002745 absorbent Effects 0.000 title claims abstract description 43
- 239000002250 absorbent Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000011572 manganese Substances 0.000 claims abstract description 57
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 49
- 239000011358 absorbing material Substances 0.000 claims abstract description 45
- 239000002073 nanorod Substances 0.000 claims abstract description 42
- 241000257465 Echinoidea Species 0.000 claims abstract description 15
- 230000000877 morphologic effect Effects 0.000 claims abstract description 12
- 239000006096 absorbing agent Substances 0.000 claims abstract description 6
- 238000013329 compounding Methods 0.000 claims abstract description 4
- 150000002696 manganese Chemical class 0.000 claims description 22
- 238000005406 washing Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 10
- 239000012266 salt solution Substances 0.000 claims description 8
- 239000004744 fabric Substances 0.000 claims description 6
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 5
- 235000006748 manganese carbonate Nutrition 0.000 claims description 5
- 239000011656 manganese carbonate Substances 0.000 claims description 5
- 229940093474 manganese carbonate Drugs 0.000 claims description 5
- 229940099596 manganese sulfate Drugs 0.000 claims description 5
- 235000007079 manganese sulphate Nutrition 0.000 claims description 5
- 239000011702 manganese sulphate Substances 0.000 claims description 5
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 5
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 5
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical group [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 5
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical group [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 5
- 239000011230 binding agent Substances 0.000 claims description 4
- 229920001721 polyimide Polymers 0.000 claims description 4
- LWXVCCOAQYNXNX-UHFFFAOYSA-N lithium hypochlorite Chemical compound [Li+].Cl[O-] LWXVCCOAQYNXNX-UHFFFAOYSA-N 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 239000011889 copper foil Substances 0.000 claims description 2
- 239000000835 fiber Substances 0.000 claims description 2
- 239000011888 foil Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- SATVIFGJTRRDQU-UHFFFAOYSA-N potassium hypochlorite Chemical compound [K+].Cl[O-] SATVIFGJTRRDQU-UHFFFAOYSA-N 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 13
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical class [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- 230000003647 oxidation Effects 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 3
- 238000005215 recombination Methods 0.000 abstract description 3
- 230000006798 recombination Effects 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 2
- 239000002114 nanocomposite Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 54
- 229910021642 ultra pure water Inorganic materials 0.000 description 18
- 239000012498 ultrapure water Substances 0.000 description 18
- 238000005303 weighing Methods 0.000 description 18
- 238000000926 separation method Methods 0.000 description 12
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 239000007788 liquid Substances 0.000 description 9
- 239000011259 mixed solution Substances 0.000 description 9
- 238000007789 sealing Methods 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 238000013461 design Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 230000010287 polarization Effects 0.000 description 4
- 230000010485 coping Effects 0.000 description 3
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- XQHAGELNRSUUGU-UHFFFAOYSA-M lithium chlorate Chemical compound [Li+].[O-]Cl(=O)=O XQHAGELNRSUUGU-UHFFFAOYSA-M 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000005770 birds nest Nutrition 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 235000005765 wild carrot Nutrition 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/32—Radiation-absorbing paints
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
- H01Q17/00—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/08—Oxygen-containing compounds
Abstract
The invention belongs to the technical field of radar wave absorption, and particularly relates to a bar-shaped composite manganese oxide radar wave absorbent, and a preparation method and application thereof. The radar wave absorbent realizes MnO through hydrothermal reaction 2 /Mn 2 O 3 Fully compounding on nano scale to form MnO 2 /Mn 2 O 3 Composite material, mnO 2 /Mn 2 O 3 The composite material has a nanorod-shaped structure, the diameter of the nanorod is 100-500nm, the nanorod-shaped structures are mutually connected and aggregated into sea urchin balls or bird nest-shaped morphological structures. The invention is characterized by reacting Mn in the process of hydrothermal reaction 2+ The undersaturation oxidation of ions realizes the full recombination of two manganese oxides on nanometer scale, the preparation process is safe and environment-friendly, the preparation cost is low, the yield of the nanocomposite is high, and the effective wave absorption frequency width ratio of MnO is single 2 The radar wave absorber is wider, is a wave absorbing material with excellent performance, and is suitable for radar wave absorption.
Description
Technical Field
The invention belongs to the technical field of radar wave absorption, and particularly relates to a bar-shaped composite manganese oxide radar wave absorbent, and a preparation method and application thereof.
Background
With the continuous improvement of the comprehensive national force of China, the development of military target stealth technology is an effective means for solving the reconnaissance threat, in particular to an anti-radar wave reconnaissance stealth technology. The stealth technology is focused on the stealth of the aircraft, and also the stealth of important targets on the large-scale ground is considered. Ground targets are too bulky due to the multitude of targets compared to stealth on a small scale of an aircraft, resulting in a stealth cost far higher than that of an aircraft. Therefore, development of a wave-absorbing material which can be mass-produced and has low cost, stealth camouflage of a large-scale military target, evade reconnaissance from the sky, and improvement of the survivability of a ground target become an extremely critical technology. The wave-absorbing materials can be divided into two main types, namely structural type and coating type according to the bearing capacity and the forming process. Compared with the former, the coating type wave-absorbing material has the advantages of convenient operation, adjustable form and the like when the coating type wave-absorbing material is used for coping with the stealth of large-scale irregular targets, and is always a research hot spot of stealth technology. The coated absorbent has various kinds, and can be divided into four kinds according to the contained elements, and the four kinds are respectively carbon wave absorbing materials (graphite, graphene, carbon fiber and carbon nano tube); iron-based wave absorbing materials (ferrite, carbonyl iron); ceramic wave absorbing materials (silicon carbide, silicon nitride); as well as other types of wave-absorbing materials (MoFs materials, conductive polymers). Although the absorbent is various, most of the absorbent is difficult to meet the application requirement of the large-scale object stealth under the double requirements of light, thin, wide and strong performance indexes and low-cost mass preparation. Compared with other types of absorbents, transition metal oxides are easy to prepare due to their abundant resources, and have been the focus of absorbent research. Carbonyl iron powder is a very mature transition metal oxide wave-absorbing material, has excellent wave-absorbing performance, but has poor environmental adaptability, is not oxidation-resistant, has complex production process and is accompanied by certain toxicity, and the preparation requirement of large scale and low cost is considered to be still not optimal. In recent years, with the research of other oxide absorber systems, manganese oxide has great potential in coping with the stealth direction of large-scale ground targets due to its low price and excellent wave absorbing performance.
The manganese oxide wave-absorbing material has rich resources and excellent wave-absorbing performance, but has the problems that the effective wave-absorbing frequency is narrow, the preparation cost of the nano material with special micro-nano structure morphology is too high, and the requirements of anti-broadband radar reconnaissance and low-cost stealth of large-scale targets cannot be met.
In the prior art, through material compounding and micro-nano structure design, the wave absorbing performance of the manganese oxide wave absorbing material is improved, and the effective wave absorbing bandwidth is expanded. However, the treatment means still has a certain limit, and the wave absorbing performance of the prepared absorbent is obviously improved compared with that of a single-phase manganese oxide, but the preparation cost of the nano wave absorbing material is obviously increased, so that the application value of the wave absorbing material in the aspect of coping with the large-scale target anti-radar wave reconnaissance is greatly limited.
Disclosure of Invention
In order to solve the problems, the invention provides a bar-shaped composite manganese oxide radar wave absorbent, a preparation method and application thereof, and manganese salt is fully compounded on a nano scale to form MnO through double design of compounding and micro-nano structure 2 /Mn 2 O 3 The composite material has a nano rod-shaped structure, the nano rod-shaped structures are mutually connected and gathered into sea urchin balls or bird nest-shaped morphological structures, and Mn is caused by hydrothermal reaction 2+ The undersaturation oxidation of the ionic manganese element realizes the full recombination of two manganese oxides on the nanometer scale, the preparation process is safe and environment-friendly, the preparation cost is low, the yield of the nanocomposite is high, and the effective wave absorption frequency width ratio of MnO is single 2 The radar wave absorber is wider, is a wave absorbing material with excellent performance, and is suitable for radar wave absorption.
The invention solves the technical problems through the following technical proposal.
A rod-shaped composite manganese oxide radar wave absorbent is characterized in that manganese salt is fully compounded on nano scale through hydrothermal reaction to form MnO 2 /Mn 2 O 3 The composite material is provided with a nanorod-shaped structure, the nanorod-shaped structures are mutually connected and gathered into sea urchin balls or bird nest-shaped morphological structures; the diameter of the nano rod is 100-500nm.
The invention also provides a preparation method of the rod-shaped composite manganese oxide radar wave absorbent, which comprises the following steps:
dissolving manganese salt in water to obtain manganese salt solution, dissolving inorganic salt in water to obtain inorganic salt solution, adding inorganic salt solution into manganese salt solution, stirring and mixing uniformly to obtain waterCarrying out thermal reaction, cooling to obtain a hydrothermal product, washing, centrifuging, ultrasonic treatment and drying to obtain MnO 2 /Mn 2 O 3 A nanorod wave absorbing material.
Further, the mass ratio of the manganese salt to the inorganic salt is 15-20:25-30.
Further, the manganese salt is manganese sulfate, manganese nitrate or manganese carbonate; the inorganic salt is sodium hypochlorite, potassium hypochlorite or lithium hypochlorite.
Further, the temperature of the hydrothermal reaction is 150-170 ℃ and the time is 8-10h.
In addition, the invention also provides application of the rodlike composite manganese oxide radar wave absorber in anti-radar wave reconnaissance camouflage net.
Further, the preparation method of the camouflage net comprises the following steps:
MnO is added to 2 /Mn 2 O 3 The nano rod is used as a radar wave absorbent, is fully and uniformly mixed with the binder, and is coated on the infrared heat insulation layer to form a wave absorbing layer so as to obtain the camouflage net.
Further, the MnO 2 /Mn 2 O 3 The mass ratio of the nano rod to the binder is 0.3-0.4:0.6-0.7, the infrared heat insulation layer is a polyimide film, and the thickness of the polyimide film is 0.1mm.
Furthermore, the lower surface of the infrared heat insulation layer is also compounded with metal paper, the upper surface of the wave absorbing layer is also coated with a camouflage layer, and the inner layer and the outer layer of the camouflage net are compounded with fabrics.
Further, the metal paper is aluminum foil or copper foil, and the thickness of the metal paper is 0.03mm; the fabric is chemical fiber woven cloth, and the thickness is 3mm.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention is characterized by reacting Mn in the process of hydrothermal reaction 2+ The undersaturation oxidation of ions realizes the full recombination of two manganese oxides on nanometer scale, the preparation method is a simple one-step hydrothermal method, the prepared wave-absorbing material has special rod-shaped structures, the rod-shaped structures are mutually connected, and sea urchin nodules are aggregated on a larger scaleConstructed such that MnO 2 /Mn 2 O 3 The nanorods have a high specific surface area.
(2) The invention realizes MnO on nanometer scale 2 With Mn 2 O 3 Abundant phase boundaries can appear between two manganese oxides, and when the manganese oxides act with electromagnetic waves, the existence of the phase boundaries can enhance the contribution of interface polarization loss to electromagnetic wave absorption, and further, the effective wave absorption bandwidth of the manganese oxide wave absorbing material is remarkably expanded through the staggered peak superposition of dipole orientation polarization loss.
(3) Because the manganese element has multiple valence states, abundant structural defects can obviously improve the conductivity of the wave-absorbing material, improve the carrier concentration in the material, further enhance the interface polarization loss and dipole orientation polarization loss and improve the electromagnetic wave absorption capacity.
(4) MnO based on undersaturated hydrothermal oxidation 2 /Mn 2 O 3 The nanorod wave-absorbing material realizes the dual design of structural design and material composite design, simultaneously remarkably reduces the preparation cost of the nano wave-absorbing material with a complex structure through one-step hydrothermal method, remarkably increases the application value of the manganese oxide wave-absorbing material, and makes the realization of anti-radar wave camouflage of a large-scale target object possible through the wave-absorbing material.
Drawings
FIG. 1 shows MnO prepared in example 1 of the present invention 2 /Mn 2 O 3 Scanning electron microscope pictures of the nanorod wave-absorbing materials;
FIG. 2 shows MnO prepared in example 4 of the present invention 2 /Mn 2 O 3 Scanning electron microscope pictures of the nanorod wave-absorbing materials;
FIG. 3 shows MnO prepared in example 7 of the present invention 2 /Mn 2 O 3 Scanning electron microscope pictures of the nanorod wave-absorbing materials;
FIG. 4 shows MnO obtained in example 1 of the present invention 2 /Mn 2 O 3 An X-ray diffraction pattern of the nanorod wave-absorbing material;
FIG. 5 shows MnO obtained in example 1 of the present invention 2 /Mn 2 O 3 Nanorods and MnO 2 Wave-absorbing material of two kinds of wave-absorbing materials of nanometer stickPerformance comparison graph.
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.
It should be noted that the technical terms used in the present invention are only for describing specific embodiments, and are not intended to limit the scope of the present invention, and various raw materials, reagents, instruments and equipment used in the following embodiments of the present invention may be purchased commercially or prepared by existing methods unless otherwise specifically described.
Example 1
A rod-shaped composite manganese oxide radar wave absorbent is characterized in that manganese salt is fully compounded on nano scale through hydrothermal reaction to form MnO 2 /Mn 2 O 3 The composite material is provided with a nanorod-shaped structure, the nanorod-shaped structures are mutually connected and gathered into sea urchin balls or bird nest-shaped morphological structures; the diameter of the nano rod is 100-500nm.
The preparation method of the rod-shaped composite manganese oxide radar wave absorbent comprises the following steps:
s1, weighing 17mmol of manganese sulfate, and dissolving in 30mL of ultrapure water to obtain a solution A;
s2, weighing 28mmol of sodium hypochlorite, and dissolving in 30mL of ultrapure water to obtain a solution B;
s3, slowly adding the solution B obtained in the S2 into the solution A obtained in the S1, stirring for 40min by a magnetic stirrer to obtain a uniformly mixed solution C, adding 60mL of the solution C into a 100mL hydrothermal reaction kettle, placing into a vacuumizing device to extract negative pressure, evacuating air in the solution, sealing, and performing hydrothermal reaction at 160 ℃ for 9h to obtain a hydrothermal product;
s4, after the hydrothermal reaction is finished, collecting S3 to obtainRepeatedly washing with deionized water for 3 times or more, ultrasonic washing for 30min for 3 times or more, performing solid-liquid separation with centrifuge at 8000-10000r/min, repeatedly separating for three times or more, and oven drying at 60deg.C under vacuum for 4 hr to obtain MnO 2 /Mn 2 O 3 A broadband wave-absorbing material of a nano rod.
Example 2
A rod-shaped composite manganese oxide radar wave absorbent is characterized in that manganese salt is fully compounded on nano scale through hydrothermal reaction to form MnO 2 /Mn 2 O 3 The composite material is provided with a nanorod-shaped structure, the nanorod-shaped structures are mutually connected and gathered into sea urchin balls or bird nest-shaped morphological structures; the diameter of the nano rod is 100-500nm.
The preparation method of the rod-shaped composite manganese oxide radar wave absorbent comprises the following steps:
s1, weighing 16mmol of manganese sulfate, and dissolving in 30mL of ultrapure water to obtain a solution A;
s2, weighing 30mmol of potassium chlorate, and dissolving in 30mL of ultrapure water to obtain a solution B;
s3, slowly adding the solution B obtained in the S2 into the solution A obtained in the S1, stirring for 40min by a magnetic stirrer to obtain a uniformly mixed solution C, adding 60mL of the solution C into a 100mL hydrothermal reaction kettle, placing into a vacuumizing device to extract negative pressure, evacuating air in the solution, sealing, and performing hydrothermal reaction at 150 ℃ for 10h to obtain a hydrothermal product;
s3, after the hydrothermal reaction is finished, collecting a hydrothermal product obtained in the step S3, repeatedly washing with deionized water for more than 3 times, washing with ultrasonic waves for more than 3 times for 30min, carrying out solid-liquid separation by using a centrifugal machine, repeatedly separating for more than three times at the rotating speed of 8000-10000r/min, and drying at the temperature of 55 ℃ for 5h in a vacuum state to obtain MnO 2 /Mn 2 O 3 A broadband wave-absorbing material of a nano rod.
Example 3
A rod-shaped composite manganese oxide radar wave absorbent is characterized in that manganese salt is fully compounded on nano scale through hydrothermal reaction to form MnO 2 /Mn 2 O 3 The composite material is provided with a nanorod-shaped structure, the nanorod-shaped structures are mutually connected and gathered into sea urchin balls or bird nest-shaped morphological structures; the diameter of the nano rod is 100-500nm.
The preparation method of the rod-shaped composite manganese oxide radar wave absorbent comprises the following steps:
s1, weighing 18mmol of manganese sulfate, and dissolving in 30mL of ultrapure water to obtain a solution A;
s2, weighing 25mmol of lithium hypochlorite, and dissolving in 30mL of ultrapure water to obtain a solution B;
s3, slowly adding the solution B obtained in the S2 into the solution A obtained in the S1, stirring for 40min by a magnetic stirrer to obtain a uniformly mixed solution C, adding 60mL of the solution C into a 100mL hydrothermal reaction kettle, placing into a vacuumizing device to extract negative pressure, evacuating air in the solution, sealing, and performing hydrothermal reaction at 170 ℃ for 8h to obtain a hydrothermal product;
s4, after the hydrothermal reaction is finished, collecting a hydrothermal product obtained in the step S3, repeatedly washing with deionized water for more than 3 times, washing with ultrasonic waves for more than 3 times for 30min, carrying out solid-liquid separation by using a centrifugal machine, carrying out repeated separation for more than three times at the rotating speed of 8000-10000r/min, and then drying for 6h at the temperature of 50 ℃ in a vacuum state to obtain MnO 2 /Mn 2 O 3 A broadband wave-absorbing material of a nano rod.
Example 4
A rod-shaped composite manganese oxide radar wave absorbent is characterized in that manganese salt is fully compounded on nano scale through hydrothermal reaction to form MnO 2 /Mn 2 O 3 The composite material is provided with a nanorod-shaped structure, the nanorod-shaped structures are mutually connected and gathered into sea urchin balls or bird nest-shaped morphological structures; the diameter of the nano rod is 100-500nm.
The preparation method of the rod-shaped composite manganese oxide radar wave absorbent comprises the following steps:
s1, weighing 17mmol of manganese nitrate, and dissolving in 30mL of ultrapure water to obtain a solution A;
s2, weighing 28mmol of sodium hypochlorite, and dissolving in 30mL of ultrapure water to obtain a solution B;
s3, slowly adding the solution B obtained in the S2 into the solution A obtained in the S1, stirring for 30min by a magnetic stirrer to obtain a uniformly mixed solution C, adding 65mL of the solution C into a 100mL hydrothermal reaction kettle, placing into a vacuumizing device to extract negative pressure, evacuating air in the solution, sealing, and performing hydrothermal reaction at 160 ℃ for 9h to obtain a hydrothermal product;
s4, after the hydrothermal reaction is finished, collecting a hydrothermal product obtained in the step S3, repeatedly washing with deionized water for more than 3 times, washing with ultrasonic waves for more than 3 times for 30min, carrying out solid-liquid separation by using a centrifugal machine, repeatedly separating for more than three times at the rotating speed of 8000-10000r/min, and drying at the temperature of 60 ℃ for 4 hours under a vacuum state to obtain MnO 2 /Mn 2 O 3 A broadband wave-absorbing material of a nano rod.
Example 5
A rod-shaped composite manganese oxide radar wave absorbent is characterized in that manganese salt is fully compounded on nano scale through hydrothermal reaction to form MnO 2 /Mn 2 O 3 The composite material is provided with a nanorod-shaped structure, the nanorod-shaped structures are mutually connected and gathered into sea urchin balls or bird nest-shaped morphological structures; the diameter of the nano rod is 100-500nm.
The preparation method of the rod-shaped composite manganese oxide radar wave absorbent comprises the following steps:
s1, weighing 16mmol of manganese nitrate, and dissolving in 30mL of ultrapure water to obtain a solution A;
s2, weighing 30mmol of potassium chlorate, and dissolving in 30mL of ultrapure water to obtain a solution B;
s3, slowly adding the solution B obtained in the S2 into the solution A obtained in the S1, stirring for 30min by a magnetic stirrer to obtain a uniformly mixed solution C, adding 65mL of the solution C into a 100mL hydrothermal reaction kettle, placing into a vacuumizing device to extract negative pressure, evacuating air in the solution, sealing, and performing hydrothermal reaction at 150 ℃ for 10h to obtain a hydrothermal product;
s4, after the hydrothermal reaction is finished, collecting the hydrothermal product obtained in the step 3, repeatedly washing with deionized water for more than 3 times, washing with ultrasound for 30min for more than 3 times, performing solid-liquid separation with a centrifuge,the rotational speed is 8000-10000r/min, repeatedly separating for more than three times, and drying at 55deg.C under vacuum for 5h to obtain MnO 2 /Mn 2 O 3 A broadband wave-absorbing material of a nano rod.
Example 6
A rod-shaped composite manganese oxide radar wave absorbent is characterized in that manganese salt is fully compounded on nano scale through hydrothermal reaction to form MnO 2 /Mn 2 O 3 The composite material is provided with a nanorod-shaped structure, the nanorod-shaped structures are mutually connected and gathered into sea urchin balls or bird nest-shaped morphological structures; the diameter of the nano rod is 100-500nm.
The preparation method of the rod-shaped composite manganese oxide radar wave absorbent comprises the following steps:
s1, weighing 18mmol of manganese nitrate, and dissolving in 30mL of ultrapure water to obtain a solution A;
s2, weighing 25mmol of lithium chlorate, and dissolving in 30mL of ultrapure water to obtain a solution B;
s3, slowly adding the solution B obtained in the S2 into the solution A obtained in the S1, stirring for 30min by a magnetic stirrer to obtain a uniformly mixed solution C, adding 65mL of the solution C into a 100mL hydrothermal reaction kettle, placing into a vacuumizing device to extract negative pressure, evacuating air in the solution, sealing, and performing hydrothermal reaction at 170 ℃ for 8h to obtain a hydrothermal product;
s4, after the hydrothermal reaction is finished, collecting a hydrothermal product obtained in the step S3, repeatedly washing with deionized water for more than 3 times, washing with ultrasonic waves for more than 3 times for 30min, carrying out solid-liquid separation by using a centrifugal machine, carrying out repeated separation for more than three times at the rotating speed of 8000-10000r/min, and then drying for 6h at the temperature of 50 ℃ in a vacuum state to obtain MnO 2 /Mn 2 O 3 A broadband wave-absorbing material of a nano rod.
Example 7
A rod-shaped composite manganese oxide radar wave absorbent is characterized in that manganese salt is fully compounded on nano scale through hydrothermal reaction to form MnO 2 /Mn 2 O 3 A composite material having nanorod-like structures, the nanorod-like structures being interconnected with each other and aggregated intoSea urchin ball or bird nest shaped morphology; the diameter of the nano rod is 100-500nm.
The preparation method of the rod-shaped composite manganese oxide radar wave absorbent comprises the following steps:
s1, weighing 17mmol of manganese carbonate, and dissolving in 30mL of ultrapure water to obtain a solution A;
s2, weighing 28mmol of sodium hypochlorite, and dissolving in 30mL of ultrapure water to obtain a solution B;
s3, slowly adding the solution B obtained in the S2 into the solution A obtained in the S2, stirring for 50min by a magnetic stirrer to obtain a uniformly mixed solution C, adding 65mL of the solution C into a 100mL hydrothermal reaction kettle, placing into a vacuumizing device to extract negative pressure, evacuating air in the solution, sealing, and performing hydrothermal reaction at 160 ℃ for 9h to obtain a hydrothermal product;
s4, after the hydrothermal reaction is finished, collecting a hydrothermal product obtained in the step S3, repeatedly washing with deionized water for more than 3 times, washing with ultrasonic waves for more than 3 times for 30min, carrying out solid-liquid separation by using a centrifugal machine, repeatedly separating for more than three times at the rotating speed of 8000-10000r/min, and drying at the temperature of 60 ℃ for 4 hours under a vacuum state to obtain MnO 2 /Mn 2 O 3 A broadband wave-absorbing material of a nano rod.
Example 8
A rod-shaped composite manganese oxide radar wave absorbent is characterized in that manganese salt is fully compounded on nano scale through hydrothermal reaction to form MnO 2 /Mn 2 O 3 The composite material is provided with a nanorod-shaped structure, the nanorod-shaped structures are mutually connected and gathered into sea urchin balls or bird nest-shaped morphological structures; the diameter of the nano rod is 100-500nm.
The preparation method of the rod-shaped composite manganese oxide radar wave absorbent comprises the following steps:
s1, weighing 16mmol of manganese carbonate, and dissolving in 30mL of ultrapure water to obtain a solution A;
s2, weighing 30mmol of potassium chlorate, and dissolving in 30mL of ultrapure water to obtain a solution B;
s3, slowly adding the solution B obtained in the S2 into the solution A obtained in the S1, stirring for 50min by a magnetic stirrer to obtain a uniformly mixed solution C, adding 65mL of the solution C into a 100mL hydrothermal reaction kettle, placing into a vacuumizing device to extract negative pressure, evacuating air in the solution, sealing, and performing hydrothermal reaction at 150 ℃ for 10h to obtain a hydrothermal product;
s4, after the hydrothermal reaction is finished, collecting a hydrothermal product obtained in the step S3, repeatedly washing with deionized water for more than 3 times, washing with ultrasonic waves for more than 3 times for 30min, carrying out solid-liquid separation by using a centrifugal machine, repeatedly separating for more than three times at the rotating speed of 8000-10000r/min, and drying at the temperature of 55 ℃ for 5h in a vacuum state to obtain MnO 2 /Mn 2 O 3 A broadband wave-absorbing material of a nano rod.
Example 9
A rod-shaped composite manganese oxide radar wave absorbent is characterized in that manganese salt is fully compounded on nano scale through hydrothermal reaction to form MnO 2 /Mn 2 O 3 The composite material is provided with a nanorod-shaped structure, the nanorod-shaped structures are mutually connected and gathered into sea urchin balls or bird nest-shaped morphological structures; the diameter of the nano rod is 100-500nm.
The preparation method of the rod-shaped composite manganese oxide radar wave absorbent comprises the following steps:
s1, weighing 18mmol of manganese carbonate, and dissolving in 30mL of ultrapure water to obtain a solution A;
s2, weighing 25mmol of lithium chlorate, and dissolving in 30mL of ultrapure water to obtain a solution B;
s3, slowly adding the solution B obtained in the S2 into the solution A obtained in the S1, stirring for 50min by a magnetic stirrer to obtain a uniformly mixed solution C, adding 65mL of the solution C into a 100mL hydrothermal reaction kettle, placing into a vacuumizing device to extract negative pressure, evacuating air in the solution, sealing, and performing hydrothermal reaction at 170 ℃ for 8h to obtain a hydrothermal product;
s4, after the hydrothermal reaction is finished, collecting a hydrothermal product obtained in the step S3, repeatedly washing with deionized water for more than 3 times, washing with ultrasonic waves for more than 3 times for 30min, carrying out solid-liquid separation by using a centrifugal machine, carrying out repeated separation for more than three times at the rotating speed of 8000-10000r/min, and then drying for 6h at the temperature of 50 ℃ in a vacuum state to obtain MnO 2 /Mn 2 O 3 A broadband wave-absorbing material of a nano rod.
MnO prepared in examples 1, 4 and 7 is prepared by referring to the accompanying drawings 2 /Mn 2 O 3 The properties associated with nanorod wave-absorbing materials are described.
FIG. 1 shows MnO prepared in example 1 of the present invention 2 /Mn 2 O 3 Scanning Electron Microscope (SEM) images of nanorod absorbing materials, wherein fig. 1 (a) is at 1.00k magnification, (b) is at 3.00k magnification, (c) is at 10.0k magnification, and (d) is at 30.0k magnification. As can be seen from FIG. 1, mnO 2 /Mn 2 O 3 The rod-shaped structure is formed, the diameter is 100-200nm, and the length is several to tens of micrometers. MnO (MnO) 2 /Mn 2 O 3 The nanorods are interconnected with each other, and exhibit sea urchin ball morphology on a larger scale.
FIG. 2 shows MnO prepared in example 4 of the present invention 2 /Mn 2 O 3 Scanning Electron Microscope (SEM) images of nanorod absorbing materials, wherein fig. 2 (a) and (b) are at a magnification of 10.0k, (c) is at a magnification of 20.0k, and (d) is at a magnification of 50.0k. As can be seen from FIG. 2, mnO 2 /Mn 2 O 3 The rod-shaped structure is formed, the diameter is 100-300nm, and the length is several to tens of micrometers.
FIG. 3 shows MnO prepared in example 7 of the present invention 2 /Mn 2 O 3 Scanning Electron Microscopy (SEM) images of nanorod absorbing materials, wherein fig. 3 (a) is at 1.00k magnification, (b) is at 2.00k magnification, (c) is at 5.00k magnification, and (d) is at 10.0k magnification. As can be seen from the figure, mnO 2 /Mn 2 O 3 The rod-shaped structure is formed, the diameter is 200-500nm, and the length is several to tens of micrometers. MnO (MnO) 2 /Mn 2 O 3 The nanorods are interconnected with each other and exhibit a bird nest-like morphology on a larger scale.
FIG. 4 shows MnO obtained in example 1 of the present invention 2 /Mn 2 O 3 X-ray diffraction pattern of the nanorod wave-absorbing material. Diffraction angle (2-Theta) with an abscissa of 2 times, unit degree; the ordinate is the relative X-ray Intensity (Intensity) in a.u.. As can be seen from FIG. 4, mnO prepared in example 1 2 /Mn 2 O 3 Diffraction peaks of the sample are respectively pointed at MnO 2 Phases (PDF card number 30-0802) and Mn 2 O 3 Phase (PDF card number 41-1442) and two phases coexist, and the sample prepared by the undersaturation oxidization hydrothermal process in the embodiment is proved to be MnO 2 And Mn of 3 O 4 Is a complex phase of (a) and (b).
FIG. 5 shows MnO obtained in example 1 of the present invention 2 /Mn 2 O 3 Nanorods and MnO 2 The comparison of the wave-absorbing properties of two materials of the nanorod is shown in FIG. 5 (a), which shows MnO 2 (b) is MnO 2 /Mn 2 O 3 . As can be seen from the results of FIG. 5 (a), mnO 2 Is a nano wave-absorbing material with excellent performance, and when the thickness of a coating is 1.66mm, the absorption is below-10 dB, and the effective wave-absorbing frequency width is 5.4GHz. At a coating thickness of 1.95mm, the strongest absorption was-54.84 dB. When the phase is differentiated by undersaturation enhanced hydrothermal reaction, the prepared MnO 2 /Mn 2 O 3 The effective wave-absorbing frequency of the nanorod is obviously expanded as shown in fig. 5 (b), and the effective wave-absorbing frequency is 6.68GHz when the thickness of the coating is 1.96mm and is below-10 dB. In particular, at lower frequency bands, better absorption performance and wider wave absorption frequency width are exhibited.
It should be noted that, when numerical ranges are referred to in the present invention, it should be understood that two endpoints of each numerical range and any numerical value between the two endpoints are optional, and because the adopted step method is the same as the embodiment, in order to prevent redundancy, the present invention describes a preferred embodiment. While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (9)
1. The application of the rod-shaped composite manganese oxide radar wave absorbent in the anti-radar wave reconnaissance camouflage net is characterized in that the radar wave absorbent is formed by fully compounding manganese salt on the nano scale through hydrothermal reaction to form MnO 2 /Mn 2 O 3 The composite material is provided with a nanorod-shaped structure, the nanorod-shaped structures are mutually connected and gathered into sea urchin balls or bird nest-shaped morphological structures; the diameter of the nano rod is 100-500nm.
2. The application of the rod-shaped composite manganese oxide radar wave absorbent in anti-radar wave reconnaissance camouflage net according to claim 1, wherein the preparation method of the radar wave absorbent comprises the following steps:
dissolving manganese salt in water to obtain manganese salt solution, dissolving inorganic salt in water to obtain inorganic salt solution, adding inorganic salt solution into manganese salt solution, stirring and mixing uniformly to make hydrothermal reaction, cooling to obtain hydrothermal product, washing, centrifuging, ultrasonic treatment and drying so as to obtain MnO 2 /Mn 2 O 3 A nanorod wave absorbing material.
3. The use of a rod-shaped composite manganese oxide radar wave absorber according to claim 2 in an anti-radar wave reconnaissance camouflage net, wherein the mass ratio of manganese salt to inorganic salt is 15-20:25-30.
4. The application of the rod-shaped composite manganese oxide radar wave absorbent in an anti-radar wave reconnaissance camouflage net according to claim 2, wherein the manganese salt is manganese sulfate, manganese nitrate or manganese carbonate; the inorganic salt is sodium hypochlorite, potassium hypochlorite or lithium hypochlorite.
5. The application of the rod-shaped composite manganese oxide radar wave absorbent in the anti-radar wave reconnaissance camouflage net according to claim 2, wherein the temperature of the hydrothermal reaction is 150-170 ℃ and the time is 8-10h.
6. The application of the rod-shaped composite manganese oxide radar wave absorbent in the anti-radar wave reconnaissance camouflage net according to claim 1, wherein the preparation method of the camouflage net comprises the following steps:
MnO is added to 2 /Mn 2 O 3 The composite material is used as radar wave absorbent, fully and uniformly mixed with binder, and coated on the infrared heat-insulating layer to form a wave-absorbing layer so as to obtain the camouflage net.
7. The use of a rod-shaped composite manganese oxide radar wave absorber according to claim 6, wherein the MnO is a radar wave-proof camouflage net 2 /Mn 2 O 3 The mass ratio of the composite material to the binder is 0.3-0.4:0.6-0.7, the infrared heat insulation layer is a polyimide film, and the thickness of the polyimide film is 0.1mm.
8. The application of the bar-shaped composite manganese oxide radar wave absorbent in the anti-radar wave reconnaissance camouflage net according to claim 6, wherein the lower surface of the infrared heat insulation layer is further compounded with metal paper, the upper surface of the wave absorbing layer is further coated with a camouflage layer, and the inner layer and the outer layer of the camouflage net are compounded with fabrics.
9. The application of the bar-shaped composite manganese oxide radar wave absorbent in the anti-radar wave reconnaissance camouflage net according to claim 8, wherein the metal paper is aluminum foil or copper foil, and the thickness is 0.03mm; the fabric is chemical fiber woven cloth, and the thickness is 3mm.
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