CN115505910A - Magnetic metal @ SiC wave-absorbing powder and preparation method thereof - Google Patents
Magnetic metal @ SiC wave-absorbing powder and preparation method thereof Download PDFInfo
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000007747 plating Methods 0.000 claims abstract description 67
- 239000002184 metal Substances 0.000 claims abstract description 49
- 239000000126 substance Substances 0.000 claims abstract description 47
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000000576 coating method Methods 0.000 claims abstract description 33
- 239000011248 coating agent Substances 0.000 claims abstract description 31
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims abstract description 24
- 229940044175 cobalt sulfate Drugs 0.000 claims abstract description 24
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims abstract description 24
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 12
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 12
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 12
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 44
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000007772 electroless plating Methods 0.000 claims description 19
- 229910052742 iron Inorganic materials 0.000 claims description 18
- 229910052759 nickel Inorganic materials 0.000 claims description 18
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 15
- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 claims description 15
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 15
- 239000001433 sodium tartrate Substances 0.000 claims description 15
- 229960002167 sodium tartrate Drugs 0.000 claims description 15
- 235000011004 sodium tartrates Nutrition 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 8
- 238000007788 roughening Methods 0.000 claims description 8
- 206010070834 Sensitisation Diseases 0.000 claims description 7
- 230000008313 sensitization Effects 0.000 claims description 7
- 230000003213 activating effect Effects 0.000 claims description 6
- 230000004913 activation Effects 0.000 claims description 6
- 230000001235 sensitizing effect Effects 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 24
- 239000002245 particle Substances 0.000 abstract description 15
- 239000011358 absorbing material Substances 0.000 abstract description 11
- 230000009471 action Effects 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- 239000011258 core-shell material Substances 0.000 abstract description 4
- 230000005672 electromagnetic field Effects 0.000 abstract description 3
- 230000010287 polarization Effects 0.000 abstract description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 102
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 82
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 39
- 239000010410 layer Substances 0.000 description 19
- 238000003756 stirring Methods 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
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- 239000000047 product Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006172 buffering agent Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- FQMNUIZEFUVPNU-UHFFFAOYSA-N cobalt iron Chemical compound [Fe].[Co].[Co] FQMNUIZEFUVPNU-UHFFFAOYSA-N 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
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- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/48—Coating with alloys
- C23C18/50—Coating with alloys with alloys based on iron, cobalt or nickel
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/18—Non-metallic particles coated with metal
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
- C23C18/1639—Substrates other than metallic, e.g. inorganic or organic or non-conductive
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1886—Multistep pretreatment
- C23C18/1893—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F41—WEAPONS
- F41H—ARMOUR; ARMOURED TURRETS; ARMOURED OR ARMED VEHICLES; MEANS OF ATTACK OR DEFENCE, e.g. CAMOUFLAGE, IN GENERAL
- F41H3/00—Camouflage, i.e. means or methods for concealment or disguise
-
- 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
Abstract
The invention provides magnetic metal @ SiC wave-absorbing powder and a preparation method thereof, and belongs to the technical field of wave-absorbing materials. According to the invention, the surface of the SiC particles is coated with the magnetic heterogeneous metal to form a unique core-shell structure, so that the wavelength of electromagnetic waves in an absorption medium is increased, the absorption of the electromagnetic waves is enhanced, and meanwhile, the absorption of the electromagnetic waves can also be enhanced by the interface polarization existing at the core-shell interface. In addition, the magnetic metal layer can form induced current under the action of electromagnetic waves, the current can be converted into heat energy, the loss of the electromagnetic waves is realized, the magnetic metal layer can generate magnetic loss under the action of the electromagnetic field, and the wave absorbing performance of the SiC particles is further improved. According to the invention, the content of Co/Fe element (or Co/Ni element) in the coating is changed by controlling the mass ratio of cobalt sulfate to ferrous sulfate (or the mass ratio of cobalt sulfate to nickel sulfate) in the chemical plating solution, so that the effects of changing electromagnetic parameters, optimizing impedance matching and improving wave absorption performance are achieved.
Description
Technical Field
The invention relates to the technical field of wave-absorbing materials, in particular to magnetic metal @ SiC wave-absorbing powder and a preparation method thereof.
Background
With the development of radar detection technology, the survivability of the aircraft in war is seriously threatened, and the stealth performance becomes an important index for measuring the advancement of future military aircraft. The key of realizing stealth is to reduce the radar scattering cross section (RCS) of a target, effectively reduce the RCS through the appearance stealth design and the application of radar wave-absorbing materials, and achieve the ideal radar stealth effect. Therefore, the development of a wave-absorbing material with wide frequency band, strong absorption and thin thickness is always the key point of research in various countries.
Silicon carbide (SiC) has the characteristics of high temperature resistance, high strength, small density, excellent dielectric property and the like, has great potential in the field of microwave absorption, but pure SiC powder cannot meet the requirements of wide frequency band and strong absorption.
Disclosure of Invention
The invention aims to provide magnetic metal @ SiC wave-absorbing powder and a preparation method thereof, which can achieve the effects of enhancing absorption strength and widening absorption frequency band.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of magnetic metal @ SiC wave-absorbing powder, which comprises the following steps: coarsening the SiC powder to obtain coarsened SiC powder;
placing the coarsened SiC powder in SnCl 2 Sensitizing in a hydrochloric acid solution to obtain sensitized SiC powder;
placing the sensitized SiC powder in PbCl 2 Activating in hydrochloric acid solution to obtainActivating SiC powder;
placing the activated SiC powder in a chemical plating solution for chemical plating to form a magnetic metal coating on the surface of the activated SiC powder to obtain intermediate wave-absorbing powder; the chemical plating solution comprises 20-30 g/L of cobalt sulfate, 1-10 g/L of ferrous sulfate, 45-55 g/L of sodium hypophosphite, 25-35 g/L of ammonium citrate, 15-25 g/L of sodium tartrate and NH 3 ·H 2 O, or the chemical plating solution comprises 15-30 g/L of cobalt sulfate, 5-15 g/L of nickel sulfate, 20-30 g/L of sodium hypophosphite, 15-25 g/L of ammonium citrate, 5-15 g/L of sodium tartrate and NH 3 ·H 2 O; the pH value of the chemical plating solution is 9-10; the magnetic metal comprises Co and Fe, or comprises Co and Ni;
and carrying out heat treatment on the intermediate wave-absorbing powder under a vacuum condition to obtain the magnetic metal @ SiC wave-absorbing powder.
Preferably, when the magnetic metal comprises Co and Fe, the chemical plating temperature is 85-95 ℃; when the magnetic metal comprises Co and Ni, the chemical plating temperature is 45-55 ℃.
Preferably, the time of the chemical plating is 20 to 40min.
Preferably, the temperature of the heat treatment is 400-500 ℃, and the holding time is 2-4 h.
Preferably, the coarsening solution used for coarsening is a NaOH solution, and the concentration of the NaOH solution is 5-10 mol/L.
Preferably, the coarsening temperature is 40-50 ℃ and the time is 20-30 min.
Preferably, the SnCl 2 pH of hydrochloric acid solution<0.5，SnCl 2 The concentration of (b) is 10 to 15g/L.
Preferably, the sensitization time is 20-30 min.
Preferably, the PbCl is 2 pH of hydrochloric acid solution<1，PbCl 2 The concentration of (b) is 0.5g/L; the activation time is 20-30 min.
The invention provides magnetic metal @ SiC wave-absorbing powder prepared by the preparation method in the scheme, which comprises SiC powder and a magnetic metal coating coated on the surface of the SiC powder, wherein the magnetic metal coating comprises Co and Fe or Co and Ni; the magnetic metal coating is in a crystalline structure.
The invention provides a preparation method of magnetic metal @ SiC wave-absorbing powder, which comprises the following steps: coarsening the SiC powder to obtain coarsened SiC powder; placing the coarsened SiC powder in SnCl 2 Sensitizing in a hydrochloric acid solution to obtain sensitized SiC powder; placing the sensitized SiC powder in PbCl 2 Activating in a hydrochloric acid solution to obtain activated SiC powder; placing the activated SiC powder in a chemical plating solution for chemical plating to form a magnetic metal coating on the surface of the activated SiC powder to obtain intermediate wave-absorbing powder; the chemical plating solution comprises 20-30 g/L of cobalt sulfate, 1-10 g/L of ferrous sulfate, 45-55 g/L of sodium hypophosphite, 25-35 g/L of ammonium citrate, 15-25/L of sodium tartrate and NH 3 ·H 2 O, or the chemical plating solution comprises 15-30 g/L of cobalt sulfate, 5-15 g/L of nickel sulfate, 20-30 g/L of sodium hypophosphite, 15-25 g/L of ammonium citrate, 5-15 g/L of sodium tartrate and NH 3 ·H 2 O; the pH value of the chemical plating solution is 9-10; the magnetic metal comprises Co and Fe, or comprises Co and Ni; and carrying out heat treatment on the intermediate wave-absorbing powder under a vacuum condition to obtain the magnetic metal @ SiC wave-absorbing powder.
The SiC particles are used as a matrix and coated with magnetic heterogeneous metals (Co and Fe or Co and Ni) to form a unique core-shell structure, the structure can increase the wavelength of electromagnetic waves in an absorption medium, so that the absorption of the electromagnetic waves is enhanced, and meanwhile, the absorption of the electromagnetic waves is enhanced by the interface polarization existing at the interface between the core shells. In addition, the magnetic metal layer on the surface of the SiC particles can form induced current under the action of electromagnetic waves, and the current can be converted into heat energy, so that the loss of the electromagnetic waves is realized, the magnetic metal layer can generate magnetic loss under the action of the electromagnetic field, and the wave absorbing performance of the SiC particles is further improved.
The invention adopts binary alloy plating, and further changes the content of Co/Fe element (or Co/Ni element) in the plating layer by controlling the mass ratio of cobalt sulfate to ferrous sulfate (or the mass ratio of cobalt sulfate to nickel sulfate) in the chemical plating solution, thereby achieving the effects of changing electromagnetic parameters, optimizing impedance matching and improving wave absorption performance.
The method adopts chemical plating to carry out heterogeneous coating on SiC, and has the advantages of environmental protection, low cost, high efficiency, large-scale mass production, uniform thickness of the plating layer formed by chemical plating, uniform components and the like.
When the magnetic metal is Co and Fe, the Curie temperature of the Co and the Fe is higher than 1000K, so that the obtained wave-absorbing material has an application prospect in the field of high-temperature stealth.
Drawings
FIG. 1 is a scanning electron micrograph of pure SiC powder;
FIG. 2 is a scanning electron microscope image of (Co, fe) @ SiC microwave absorbing powder prepared in examples 1-3;
FIG. 3 is the scanning electron microscope image of (Co, ni) @ SiC microwave-absorbing powder prepared in examples 4-6;
FIG. 4 is a scan of the element surface of (Co, fe) @ SiC microwave absorbing powder prepared in examples 1-3;
FIG. 5 is a scan of the element surface of (Co, ni) @ SiC microwave absorbing powder prepared in examples 4-6;
FIG. 6 shows Co and Fe elements in the coating layers of (Co, fe) @ SiC samples of examples 1 to 3, in accordance with the electroless Co plating solution 2+ /Fe 2+ A graph of the change in concentration ratio;
FIG. 7 shows Co and Ni elements in the (Co, ni) @ SiC wave-absorbing powder coatings prepared in examples 4-6, along with the chemical plating solution Co 2+ /Ni 2+ A graph of the change in concentration ratio;
FIG. 8 is a graph of the Reflection Loss (RL) for the (Co, fe) @ SiC samples at different frequencies and thicknesses in examples 1-3;
FIG. 9 is a graph of reflection loss at different frequencies and thicknesses for the (Co, ni) @ SiC samples of examples 4-6;
fig. 10 is a graph of the reflection loss of pure SiC powder at different frequencies and thicknesses.
Detailed Description
The invention provides a preparation method of magnetic metal @ SiC wave-absorbing powder, which comprises the following steps: coarsening the SiC powder to obtain coarsened SiC powder;
placing the coarsened SiC powder in SnCl 2 Sensitizing in hydrochloric acid solution to obtain sensitized SiC powder;
placing the sensitized SiC powder in PbCl 2 Activating in a hydrochloric acid solution to obtain activated SiC powder;
placing the activated SiC powder in a chemical plating solution for chemical plating to form a magnetic metal coating on the surface of the activated SiC powder to obtain intermediate wave-absorbing powder; the chemical plating solution comprises 20-30 g/L of cobalt sulfate, 1-10 g/L of ferrous sulfate, 45-55 g/L of sodium hypophosphite, 25-35 g/L of ammonium citrate, 15-25/L of sodium tartrate and NH 3 ·H 2 O, or the chemical plating solution comprises 15-30 g/L of cobalt sulfate, 5-15 g/L of nickel sulfate, 20-30 g/L of sodium hypophosphite, 15-25 g/L of ammonium citrate, 5-15 g/L of sodium tartrate and NH 3 ·H 2 O; the pH value of the chemical plating solution is 9-10; the magnetic metal comprises Co and Fe, or comprises Co and Ni;
and carrying out heat treatment on the intermediate wave-absorbing powder under a vacuum condition to obtain the magnetic metal @ SiC wave-absorbing powder.
In the present invention, the starting materials used are all commercially available products well known in the art, unless otherwise specified.
The invention coarsens SiC powder to obtain coarsened SiC powder.
In the present invention, the particle size of the SiC powder is preferably in the micrometer range, and in the examples of the present invention, the median particle size of the SiC powder is specifically 10 μm. In the present invention, the roughening solution used for roughening is preferably a NaOH solution, and the concentration of the NaOH solution is preferably 5 to 10mol/L, more preferably 6 to 9mol/L, and still more preferably 7 to 8mol/L. In the invention, the temperature of the coarsening is preferably 40-50 ℃, and more preferably 43-46 ℃; the coarsening time is preferably 20-30 min. In the present invention, the coarsening is preferably performed under ultrasonic and stirring conditions. In general, HF solution is mostly adopted for coarsening, but HF has strong corrosivity and can cause irreversible damage to a human body when not operated properly. The surface of the SiC particles can be formed by coarseningForming rugged micro-surfaces which facilitate subsequent sensitization of Sn 2+ Adsorption of (3). After the roughening is completed, the invention preferably washes the SiC powder with deionized water for 2-3 times until the SiC powder is neutral, so as to obtain the roughened SiC powder.
After obtaining the coarsened SiC powder, the invention places the coarsened SiC powder in SnCl 2 Sensitizing in hydrochloric acid solution to obtain sensitized SiC powder.
In the present invention, the SnCl 2 The hydrochloric acid solution is preferably composed of SnCl 2 Dissolving in hydrochloric acid to obtain the final product. In the present invention, the SnCl 2 The pH of the hydrochloric acid solution is preferably<0.5，SnCl 2 The concentration of (B) is preferably 10 to 15g/L, more preferably 12 to 13g/L. In the present invention, the time for sensitization is preferably 20 to 30min. In the present invention, the sensitization is preferably performed under room temperature, ultrasonic and stirring conditions. The invention utilizes sensitization to adsorb Sn on the surface of SiC particles 2+ ，Sn 2+ Has reducibility, can convert Pb 2+ Reducing the Pb into a simple substance to be adsorbed on the surface of the SiC particles. After the sensitization is finished, the sensitized SiC powder is washed by deionized water and dried to obtain the sensitized SiC powder.
After obtaining the sensitized SiC powder, the invention puts the sensitized SiC powder in PbCl 2 And activating in a hydrochloric acid solution to obtain activated SiC powder.
In the present invention, the PbCl is 2 The hydrochloric acid solution is preferably composed of PbCl 2 Dissolving in hydrochloric acid to obtain the final product. In the present invention, the PbCl is 2 The pH of the hydrochloric acid solution is preferably<1，PbCl 2 The concentration of (B) is preferably 0.5g/L; the activation time is preferably 20 to 30min. In the present invention, the activation is preferably performed under ultrasonic and stirring conditions. The invention can form Pb simple substance on the surface of SiC particles through activation, and Pb has stronger catalytic activity and can promote the reduction of metal cations. After the activation is completed, the activated SiC powder is washed by deionized water to obtain the activated SiC powder.
After the activated SiC powder is obtained, the activated SiC powder is placed in chemical plating solution for chemical plating, and a magnetic metal coating is formed on the surface of the activated SiC powder to obtain intermediate wave-absorbing powder.
In the invention, the chemical plating solution comprises 20-30 g/L of cobalt sulfate, 1-10 g/L of ferrous sulfate, 45-55 g/L of sodium hypophosphite, 25-35 g/L of ammonium citrate, 15-25 g/L of sodium tartrate and NH 3 ·H 2 O, or the chemical plating solution comprises 15-30 g/L of cobalt sulfate, 5-15 g/L of nickel sulfate, 20-30 g/L of sodium hypophosphite, 15-25 g/L of ammonium citrate, 5-15 g/L of sodium tartrate and NH 3 ·H 2 O。
Preferably, the chemical plating solution comprises 23-27 g/L of cobalt sulfate, 4-8 g/L of ferrous sulfate, 48-52 g/L of sodium hypophosphite, 28-32 g/L of ammonium citrate, 18-22 g/L of sodium tartrate and NH 3 ·H 2 O, or the chemical plating solution comprises 20-25 g/L of cobalt sulfate, 8-12 g/L of nickel sulfate, 23-27 g/L of sodium hypophosphite, 18-22 g/L of ammonium citrate, 8-12 g/L of sodium tartrate and NH 3 ·H 2 O。
The preparation process of the chemical plating solution has no special requirement, and the preparation process known in the field can be adopted.
In the invention, cobalt sulfate and ferrous sulfate (or cobalt sulfate and nickel sulfate) are used as main salts and mainly used for providing metal cations required for forming a plating layer, sodium hypophosphite is used as a reducing agent, sodium citrate and sodium tartrate are used as complexing agents, and the complexing agents can be mixed with Co in chemical plating solution 2+ 、Fe 2+ 、Ni 2+ A complex is formed, thereby improving the stability at high pH and avoiding the formation of hydroxide precipitates. The ammonia water is used as a pH regulator and has the functions of a complexing agent and a buffering agent.
In the present invention, the pH of the electroless plating solution is 9 to 10.
In the present invention, when the magnetic metal includes Co and Fe, the electroless plating temperature is preferably 85 to 95 ℃, more preferably 88 to 92 ℃, and further preferably 90 ℃; when the magnetic metal includes Co and Ni, the electroless plating temperature is preferably 45 to 55 ℃, more preferably 48 to 52 ℃, and further preferably 50 ℃.
In the present invention, when the electroless plating solution uses cobalt sulfate and ferrous sulfate as main salts, the magnetic metals formed on the surface of the activated SiC powder are Co and Fe; when the electroless plating solution uses cobalt sulfate and nickel sulfate as main salts, the magnetic metals formed on the surface of the activated SiC powder are Co and Ni.
According to the invention, the content of Co/Fe element (or Co/Ni element) in the coating is changed by controlling the mass ratio of cobalt sulfate to ferrous sulfate (or the mass ratio of cobalt sulfate to nickel sulfate) in the chemical plating solution, so that the effects of changing electromagnetic parameters, optimizing impedance matching and improving wave absorption performance are achieved.
In the present invention, when the electroless plating solution uses cobalt sulfate and ferrous sulfate as main salts, coSO is contained in the electroless plating solution 4 ·7H 2 The concentration of O is 27.5g/L, feSO 4 ·7H 2 When the concentration of O is 2.5g/L, the obtained magnetic metal @ SiC wave-absorbing powder has the best wave-absorbing performance, and at the moment, the content of Co in the magnetic metal coating is 88.45wt%, and the content of Fe in the magnetic metal coating is 5.1wt%. When the chemical plating solution takes cobalt sulfate and nickel sulfate as main salts, coSO is contained in the chemical plating solution 4 ·7H 2 The concentration of O is 20g/L, niSO 4 ·6H 2 When the concentration of O is 10g/L, the wave absorbing performance of the magnetic metal @ SiC wave absorbing powder of the obtained wave absorbing powder is optimal, and at the moment, the content of Co in the magnetic metal coating is 48.4wt%, and the content of Ni in the magnetic metal coating is 44.89wt%.
In the invention, after the chemical plating is finished, the obtained powder is washed and dried to obtain the intermediate wave-absorbing powder. In the invention, the magnetic metal in the intermediate wave-absorbing powder is mainly in an amorphous state, and has poor magnetism, so that the magnetic loss of a coating to incident electromagnetic waves is not facilitated.
After the intermediate wave-absorbing powder is obtained, the intermediate wave-absorbing powder is subjected to heat treatment under a vacuum condition to obtain the magnetic metal @ SiC wave-absorbing powder.
In the present invention, the temperature of the heat treatment is preferably 400 to 500 ℃, more preferably 420 to 480 ℃; the holding time is preferably 2 to 4 hours, more preferably 2.5 to 3.5 hours. In the present invention, the degree of vacuum of the heat treatment is preferably 10 -1 ～10 - 5 Pa. In the present invention, the heat treatment is preferably performed in a vacuum heat treatment furnaceIs carried out in (1). The invention utilizes heat treatment to crystallize the magnetic metal, enhances the magnetism, and can enhance the loss of incident electromagnetic waves, thereby improving the wave absorbing performance of the electromagnetic wave absorbing material.
The invention provides magnetic metal @ SiC wave-absorbing powder prepared by the preparation method in the scheme, which comprises SiC powder and a magnetic metal coating coated on the surface of the SiC powder, wherein the magnetic metal coating comprises Co and Fe or Co and Ni; the magnetic metal coating is in a crystalline structure.
In the present invention, when the magnetic metal plating layer includes Co and Fe, the content of Co in the magnetic metal plating layer is preferably 81.47 to 88.45wt%, and the content of Fe is preferably 5.1 to 13.21wt%; most preferably, the content of Co is 88.45wt% and the content of Fe is 5.1wt%.
When the magnetic metal plating layer comprises Co and Ni, the content of Co in the magnetic metal plating layer is 36.48-58.26 wt%, and the content of Ni is 39.23-57.63 wt%; most preferably, the Co content is 48.4wt% and the Ni content is 44.89wt%.
The SiC particles are used as a matrix and coated with magnetic heterogeneous metals (Co and Fe or Co and Ni) to form a unique core-shell structure, the structure can increase the wavelength of electromagnetic waves in an absorption medium, so that the absorption of the electromagnetic waves is enhanced, and meanwhile, the absorption of the electromagnetic waves can also be enhanced by the interface polarization existing at the interface between the core shells. In addition, the magnetic metal layer on the surface of the SiC particles can form induced current under the action of electromagnetic waves, the current can be converted into heat energy, and therefore the loss of the electromagnetic waves is achieved, the magnetic metal layer can generate magnetic loss under the action of the electromagnetic fields, and the wave absorbing performance of the SiC particles is further improved.
The magnetic metal @ SiC wave-absorbing powder and the preparation method thereof provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Weighing 10g of SiC powder (with median diameter D50=10 μm), placing the powder in 10mol/L NaOH solution, keeping the temperature at 50 ℃, roughening the powder for 30min under the conditions of ultrasonic and continuous stirring, and washing the SiC powder with deionized water until the SiC powder is neutral to obtain roughened SiC powder;
placing the coarsened SiC powder in 10g/L SnCl 2 Hydrochloric acid solution, pH value<0.5, sensitizing for 20min at room temperature under ultrasonic and stirring conditions, washing with deionized water after finishing, and drying to obtain sensitized SiC powder;
the sensitized SiC powder was placed in 0.5g/L PbCl 2 Hydrochloric acid solution, pH value<1, activating the solution for 30min at room temperature under ultrasonic and stirring conditions, and washing and drying to obtain activated SiC powder;
putting the activated SiC powder into an electroless plating solution for cobalt iron plating, wherein the electroless plating solution (500 mL plating solution) comprises the following formula: coSO 4 ·7H 2 O 27.5g/L、FeSO 4 ·7H 2 Adjusting the pH value to 9 by O2.5 g/L, sodium hypophosphite 50g/L, ammonium citrate 30g/L, sodium tartrate 20g/L and ammonia water, and obtaining intermediate wave-absorbing powder at the temperature of 85 ℃ for 30 min;
carrying out heat treatment on the intermediate wave-absorbing powder under a vacuum condition, wherein the heat treatment temperature is 400 ℃, and the time is 2 hours, so as to obtain magnetic metal @ SiC wave-absorbing powder which is marked as (Co, fe) @ SiC wave-absorbing powder; the content of Co in the plating layer is 88.45wt%, and the content of Fe is 5.1wt%.
Example 2
The only difference from example 1 is CoSO in the electroless plating bath formulation 4 ·7H 2 O is 25g/L and FeSO 4 ·7H 2 O is 5g/L. And finally, the content of Co in the (Co, fe) @ SiC wave-absorbing powder coating is 81.47wt%, and the content of Fe is 9.11wt%.
Example 3
The only difference from example 1 is CoSO in the electroless plating bath formulation 4 ·7H 2 O is 22.5g/L and FeSO 4 ·7H 2 O is 7.5g/L. And finally, the content of Co in the (Co, fe) @ SiC wave-absorbing powder coating is 82.5wt%, and the content of Fe is 13.21wt%.
Example 4
The difference from the example 1 is only that the chemical plating solution formula is as follows: coSO 4 ·7H 2 O 25g/L、NiSO 4 ·6H 2 O5 g/L, sodium hypophosphite 30g/L, ammonium citrate 20g/L, sodium tartrate 10g/L, ammonia waterThe pH value is adjusted to 10, the temperature is 50 ℃, the time is 10min, the product is marked as (Co, ni) @ SiC wave-absorbing powder, the Co content in the plating layer is 58.26wt%, and the Ni content is 39.23wt%.
Example 5
The only difference from example 4 is CoSO in the electroless plating bath formulation 4 ·7H 2 O is 20g/L and NiSO 4 ·6H 2 O is 10g/L. The content of Co in the plating layer is 48.4wt%, and the content of Ni is 44.89wt%.
Example 6
The only difference from example 4 is CoSO in the electroless plating bath formulation 4 ·7H 2 O is 15g/L and NiSO 4 ·6H 2 O is 15g/L. The content of Co in the plating layer is 36.48wt%, and the content of Ni is 57.63wt%.
And (3) structural and performance characterization:
1. as a result of observation of the SiC powder by a scanning electron microscope, the surface was smooth as shown in fig. 1, as is clear from fig. 1. Scanning electron microscope observation was performed on the (Co, fe) @ SiC wave-absorbing powder prepared in examples 1 to 3 and the (Co, ni) @ SiC wave-absorbing powder prepared in examples 4 to 6, respectively, and the results are shown in fig. 2 and 3, in fig. 2, (a) is example 1, (b) is example 2, and (c) is example 3, and all scales of the pictures in fig. 2 were 2 μm. In FIG. 3, (a) is example 4, (b) is example 5, and (c) is example 6. As can be seen from fig. 2 and 3, a uniform and complete coating layer is successfully coated on the surface of the SiC particles by electroless plating.
2. The results of element surface scanning of the (Co, fe) @ SiC absorbing powder prepared in examples 1 to 3 are shown in fig. 4, in which (a) is example 1, (b) is example 2, and (c) is example 3. As can be seen from FIG. 4, the coating layer is mainly composed of Co and Fe, the distribution of Co is very uniform, and the Fe content is small and is distributed irregularly, because Fe 2+ Electrode potential ratio Co of 2+ More negative, indicating that it is more difficult to reduce in the same electroless solution, and Fe in solution 2+ At a concentration lower than Co 2+ Therefore, the content of Fe element in the plating layer is far lower than that of Co element.
3. The elemental surface scans of the (Co, ni) @ SiC absorbing powders prepared in examples 4-6 were respectively performed, and the results are shown in fig. 5, in which (a) is example 4, (b) is example 5, and (c) is example 6. As can be seen from fig. 5, the plating layer is mainly composed of Co and Ni elements, and the distribution of Co and Ni elements is very uniform.
4. FIG. 6 shows Co and Fe elements in the coating layers of (Co, fe) @ SiC samples of examples 1 to 3, in accordance with the electroless Co plating solution 2+ /Fe 2+ FIG. 6 shows graphs of concentration ratios, where sample1 is example 1, sample2 is example 2, and sample3 is example 3. As can be seen from fig. 6: with electroless Co plating 2+ /Fe 2+ The concentration ratio is smaller and smaller, the content ratio of Co/Fe element in the coating is smaller and smaller, but the content of Fe element is far lower than that of Co element. Indicating Co in the bath 2+ /Fe 2+ The concentration of (2) affects the Co/Fe element content of the coating.
5. FIG. 7 shows Co and Ni elements in the (Co, ni) @ SiC wave-absorbing powder coatings prepared in examples 4-6, along with the chemical plating solution Co 2+ /Ni 2+ The concentration ratio is shown in the graph, wherein sample1 is example 4, sample2 is example 5, and sample3 is example 6. As can be seen from FIG. 7, co was added to the electroless plating solution 2+ /Ni 2+ The concentration ratio is smaller and smaller, and the content ratio of Co/Ni element in the plating layer is smaller and smaller, which shows that Co in the plating solution 2+ /Ni 2+ The concentration of (2) affects the Co/Ni element content of the plating layer.
6. The electromagnetic parameters are measured by a coaxial method, and the measuring frequency is 2-18 GHz. Measuring a pair of complex scattering parameters S of a coaxial sample by adopting an E5071C type vector network analyzer 11 And S 21 And obtaining the complex dielectric constant and the complex permeability of the material according to the size of the sample and the transmission coefficient of the electromagnetic wave in the sample. The test sample is a coaxial ring sample with the outer diameter of 7.00mm and the inner diameter of 3.04mm, which is cast after 20wt% of paraffin and 80wt% of (Co, fe) @ SiC powder are evenly mixed.
Reflection Loss RL (Reflection Loss) is used to evaluate the microwave absorption performance of the material. According to the principle of microwave transmission line, by analyzing the condition of a single-layer uniform absorber on a metal substrate, the reflection loss RL can be obtained by the following formula:
zin is normalized input impedance of electromagnetic wave from free space to material interface; mu.s r 、ε r The complex permeability and the complex dielectric constant of the material are respectively, c is the propagation speed of light in vacuum, f is the frequency of electromagnetic waves, and d is the thickness of the wave-absorbing coating. Table 1 is a relation table between reflection loss and incident wave absorption percentage, and as shown in table 1, the smaller the reflection loss is, the larger the absorption ratio of the surface wave-absorbing material to the electromagnetic waves entering society is, and the better the wave-absorbing performance is.
TABLE 1 relationship of reflection loss to percent absorption of incident wave
| Reflection Loss (RL) | Percentage of incident wave absorption (%) | |
| 1 | ＜-5dB | ＞70％ |
| 2 | ＜-10dB | ＞90％ |
| 3 | ＜-15dB | ＞96.8％ |
| 4 | ＜-20dB | ＞99％ |
| 5 | ＜-40dB | ＞99.9％ |
FIG. 8 is a graph showing Reflection Loss (RL) at different frequencies and thicknesses for the (Co, fe) @ SiC samples of examples 1-3, in which (a) is example 1, (b) is example 2, and (c) is example 3. As can be seen from fig. 8: the wave absorbing performance of (Co, fe) @ SiC powder gradually worsens along with the increase of Co/Fe elements in the coating, and the wave absorbing performance of a sample prepared by the chemical plating solution in example 1 is the best and is higher than that of pure SiC powder (figure 10 is a reflection loss figure of the pure SiC powder under different frequencies and thicknesses), so the conclusion can be drawn that the Co in the chemical plating solution can be changed 2+ /Fe 2+ The concentration ratio controls the content ratio of Co/Fe element in the sample coating, thereby regulating and controlling the electromagnetic parameters of the wave-absorbing material and further improving the wave-absorbing performance of the wave-absorbing material.
FIG. 9 is a graph of reflection loss of the (Co, ni) @ SiC samples of examples 4-6 at different frequencies and thicknesses, and it can be seen from FIG. 9 that the wave-absorbing properties of the (Co, ni) @ SiC powder vary with the content ratio of Co/Ni elements in the coating, and the sample prepared by the electroless plating solution of example 5 has the best wave-absorbing properties, higher than that of pure SiC powder, so it can be concluded that the Co in the electroless plating solution can be changed 2+ /Ni 2+ The concentration ratio controls the Co/Ni element content ratio in the sample coating, thereby regulating and controlling the electromagnetic parameters of the wave-absorbing material and further improving the wave-absorbing performance of the wave-absorbing material. The wave absorbing properties of the examples and the pure SiC powder are summarized in table 2.
Table 2 examples and wave-absorbing properties of pure SiC powder
| RL min | Bandwidth (RL)<-5dB) | Bandwidth (RL)<-10dB) | |
| Example 1 | [email protected] | 7.34GHz(10.43～17.77) | 3.71GHz(14.15～17.86) |
| Example 2 | [email protected] | 7.08GHz(10.24～17.32) | 3.19GHz(14.01～17.20) |
| Example 3 | [email protected] | 6.62GHz(10.77～17.39) | 2.08GHz(11.62～13.70) |
| Example 4 | [email protected] | 6.93GHz(10.56～17.49) | 0 |
| Example 5 | [email protected] | 6.73GHz(10.63～17.36) | 3.53GHz(14.47～18.00) |
| Example 6 | -2.61 |
0 | 0 |
| Pure SiC powder | [email protected] | 5.76GHz(11.90～17.66) | 2.36GHz(15.30～17.66) |
Note: in Table 2, RL min Represents the minimum reflection loss in the whole frequency range and represents the strongest wave-absorbing capacity of a wave-absorbing sample at a certain frequency, such as: 23.68dB @10.43GHz represents that the wave absorbing capacity of the sample is strongest at 10.43GHz and reaches 23.68dB; bandwidth (RL)<-5 dB) indicates that the sample reflection loss is less than the band corresponding to-5 dB, for example: 7.34GHz (10.43-17.77) indicates that the reflection loss of the sample at (10.43 GHz-17.77 GHz) is less than-5 dB, and the frequency bandwidth reaches 7.34GH; bandwidth (RL)<-10 dB) indicates that the sample reflection loss is less than the band corresponding to-10 dB.
As can be seen from Table 2, the wave-absorbing powder provided by the invention can achieve the effects of enhancing the absorption strength and widening the absorption band.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of magnetic metal @ SiC wave-absorbing powder is characterized by comprising the following steps: coarsening the SiC powder to obtain coarsened SiC powder;
placing the coarsened SiC powder in SnCl 2 Sensitizing in hydrochloric acid solution to obtain sensitized SiC powder;
placing the sensitized SiC powder in PbCl 2 Activating in a hydrochloric acid solution to obtain activated SiC powder;
placing the activated SiC powder in a chemical plating solution for chemical plating to form a magnetic metal coating on the surface of the activated SiC powder to obtain intermediate wave-absorbing powder; the chemical plating solution comprises 20-30 g/L of cobalt sulfate, 1-10 g/L of ferrous sulfate, 45-55 g/L of sodium hypophosphite, 25-35 g/L of ammonium citrate, 15-25 g/L of sodium tartrate and NH 3 ·H 2 O, or the chemical plating solution comprises 15-30 g/L of cobalt sulfate, 5-15 g/L of nickel sulfate, 20-30 g/L of sodium hypophosphite, 15-25 g/L of ammonium citrate, 5-15 g/L of sodium tartrate and NH 3 ·H 2 O; the pH value of the chemical plating solution is 9-10; the magnetic metal comprises Co and Fe, or comprises Co and Ni;
and carrying out heat treatment on the intermediate wave-absorbing powder under a vacuum condition to obtain the magnetic metal @ SiC wave-absorbing powder.
2. The method according to claim 1, wherein when the magnetic metal includes Co and Fe, the electroless plating temperature is 85 to 95 ℃; when the magnetic metal comprises Co and Ni, the chemical plating temperature is 45-55 ℃.
3. The production method according to claim 1 or 2, wherein the electroless plating time is 20 to 40min.
4. The method according to claim 1, wherein the heat treatment temperature is 400-500 ℃ and the holding time is 2-4 h.
5. The preparation method according to claim 1, wherein the roughening solution used in the roughening process is a NaOH solution, and the concentration of the NaOH solution is 5 to 10mol/L.
6. The method according to claim 1 or 5, wherein the roughening temperature is 40-50 ℃ and the roughening time is 20-30 min.
7. Preparation method according to claim 1, characterized in that the SnCl is 2 pH of hydrochloric acid solution<0.5，SnCl 2 The concentration of (b) is 10 to 15g/L.
8. The method according to claim 7, wherein the sensitization time is 20 to 30min.
9. The method according to claim 1, wherein the PbCl is present in the composition 2 pH of hydrochloric acid solution<1，PbCl 2 The concentration of (b) is 0.5g/L; the activation time is 20-30 min.
10. The magnetic metal @ SiC wave-absorbing powder prepared by the preparation method of any one of claims 1-9 comprises SiC powder and a magnetic metal coating coated on the surface of the SiC powder, wherein the magnetic metal coating comprises Co and Fe or comprises Co and Ni; the magnetic metal coating is in a crystalline structure.
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