CN115505910B - Magnetic metal @ SiC wave-absorbing powder and preparation method thereof - Google Patents

Magnetic metal @ SiC wave-absorbing powder and preparation method thereof Download PDF

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CN115505910B
CN115505910B CN202211308169.4A CN202211308169A CN115505910B CN 115505910 B CN115505910 B CN 115505910B CN 202211308169 A CN202211308169 A CN 202211308169A CN 115505910 B CN115505910 B CN 115505910B
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magnetic metal
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absorbing
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CN115505910A (en
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裴延玲
胡晓甫
刘巧沐
李树索
陈小雨
宫声凯
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Beihang University
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    • 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

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  • Engineering & Computer Science (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemically Coating (AREA)

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 particle 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 is also 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, and the magnetic metal layer can generate magnetic loss under the action of the electromagnetic field, so that the wave absorbing performance of SiC particles is further improved. The invention changes the content of Co/Fe element (or Co/Ni element) in the plating layer by controlling the mass ratio of cobalt sulfate and ferrous sulfate (or the mass ratio of cobalt sulfate and nickel sulfate) in the chemical plating solution, thereby achieving the effects of changing electromagnetic parameters, optimizing impedance matching and improving the wave absorbing performance.

Description

Magnetic metal @ SiC wave-absorbing powder and preparation method thereof
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 a serious threat, and stealth performance becomes an important index for measuring the advancement of future military aircraft. The key to realizing stealth is to reduce radar cross-sectional area (RCS) of the 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, development of a broadband, strong-absorption, and thin-thickness wave-absorbing material has been the focus of research in various countries.
Silicon carbide (SiC) has the characteristics of high temperature resistance, high strength, low density, excellent dielectric properties and the like, has great potential in the field of microwave absorption, but pure SiC powder is difficult to 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 bands.
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 Sensitization is carried out in the hydrochloric acid solution of (2) to obtain sensitized SiC powder;
placing the sensitized SiC powder in PbCl 2 Activating in hydrochloric acid solution to obtain activated SiC powder;
the activated SiC powderPlacing the powder into chemical plating solution for chemical plating, and forming a plating layer of magnetic metal 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 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 electroless plating temperature is 85-95 ℃; when the magnetic metal comprises Co and Ni, the electroless plating temperature is 45-55 ℃.
Preferably, the electroless plating time is 20-40 min.
Preferably, the temperature of the heat treatment is 400-500 ℃, and the heat preservation time is 2-4 hours.
Preferably, the roughening solution adopted in the roughening is NaOH solution, and the concentration of the NaOH solution is 5-10 mol/L.
Preferably, the roughening temperature is 40-50 ℃ and the roughening time is 20-30 min.
Preferably, the SnCl 2 pH value of hydrochloric acid solution of (2)<0.5，SnCl 2 The concentration of (C) is 10-15 g/L.
Preferably, the sensitization time is 20-30 min.
Preferably, the PbCl 2 pH value of hydrochloric acid solution of (2)<1，PbCl 2 Is 0.5g/L; the activation time is 20-30 min.
The invention provides the magnetic metal@SiC wave-absorbing powder prepared by the preparation method, 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 Sensitization is carried out in the hydrochloric acid solution of (2) to obtain sensitized SiC powder; placing the sensitized SiC powder in PbCl 2 Activating in hydrochloric acid solution to obtain activated SiC powder; placing the activated SiC powder into chemical plating solution for chemical plating, and forming a magnetic metal plating layer 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 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 invention takes SiC particles as a matrix, coats magnetic heterogeneous metals (Co and Fe or Co and Ni) and can form a unique core-shell structure, the structure can increase the wavelength of electromagnetic waves in an absorption medium, thereby enhancing the absorption of the electromagnetic waves, and simultaneously, the interface polarization existing at the interface between the core-shells can enhance the absorption of the electromagnetic waves. 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, and the magnetic metal layer can generate magnetic loss under the action of the electromagnetic field, so that the wave absorbing performance of the SiC particles is further improved.
The invention adopts binary alloy plating, and the mass ratio of cobalt sulfate and ferrous sulfate (or the mass ratio of cobalt sulfate and nickel sulfate) in the chemical plating solution is controlled, so that the content of Co/Fe element (or Co/Ni element) in the plating layer is changed, thereby achieving the effects of changing electromagnetic parameters, optimizing impedance matching and improving the wave absorbing performance.
The invention adopts chemical plating to carry out heterogeneous coating on SiC, and has the advantages of environmental protection, low cost, high efficiency, mass production, uniform thickness of plating formed by chemical plating, uniform components and the like.
When the magnetic metal is Co and Fe, the Curie temperature of the Co and Fe is higher than 1000K, so that the obtained wave-absorbing material has application prospect in the field of high Wen Yinshen.
Drawings
FIG. 1 is a scanning electron microscope image of a pure SiC powder;
FIG. 2 is a scanning electron microscope image of the (Co, fe) @ SiC absorbing powder prepared in examples 1 to 3;
FIG. 3 is a scanning electron microscope image of the (Co, ni) @ SiC absorbing powder prepared in examples 4 to 6;
FIG. 4 is a scanning view of the elemental surface of the (Co, fe) @ SiC wave-absorbing powder prepared in examples 1 to 3;
FIG. 5 is a scanning view of the elemental surface of the (Co, ni) @ SiC wave-absorbing powders prepared in examples 4 to 6;
FIG. 6 shows the chemical plating solution Co of the (Co, fe) @ SiC sample plating layers of examples 1 to 3 2+ /Fe 2+ A graph of the concentration ratio;
FIG. 7 shows the chemical plating solution Co of Co, ni element in the (Co, ni) @ SiC wave-absorbing powder coating prepared in examples 4 to 6 2+ /Ni 2+ A graph of the concentration ratio;
FIG. 8 is a graph of Reflection Loss (RL) for (Co, fe) @ SiC samples of examples 1-3 at different frequencies and thicknesses;
FIG. 9 is a graph of reflection loss for (Co, ni) @ SiC samples of examples 4-6 at different frequencies and thicknesses;
fig. 10 is a graph of 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 Sensitization is carried out in the hydrochloric acid solution of (2) to obtain sensitized SiC powder;
placing the sensitized SiC powder in PbCl 2 Activating in hydrochloric acid solution to obtain activated SiC powder;
placing the activated SiC powder into chemical plating solution for chemical plating, and forming a magnetic metal plating layer 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 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 raw materials used are commercially available products well known in the art, unless specifically described otherwise.
The coarsening method coarsens the SiC powder to obtain coarsened SiC powder.
In the present invention, the particle diameter of the SiC powder is preferably in the order of micrometers, and in the embodiment of the present invention, the median particle diameter of the SiC powder is specifically 10 μm. In the present invention, the roughening liquid used for the roughening is preferably an NaOH solution, and the concentration of the NaOH solution is preferably 5 to 10mol/L, more preferably 6 to 9mol/L, and even more preferably 7 to 8mol/L. In the present invention, the roughening temperature is preferably 40 to 50 ℃, more preferably 43 to 46 ℃; the roughening time is preferably 20 to 30 minutes. In the present invention, the roughening is preferably performed under ultrasonic and agitation conditions. Generally, HF solution is adopted for coarsening, but HF has strong corrosiveness, and improper operation can generate irreversible harm to human bodies. The roughened micro-surface can be formed on the surface of SiC particles, which is beneficial to the subsequent sensitization of Sn 2+ Adsorption of (3). After the coarsening is completed, the method preferably uses deionized water to rinse the SiC powder for 2 to 3 times until the SiC powder is neutral, so as to obtain coarsened SiC powder.
After coarsened SiC powder is obtained, the coarsened SiC powder is placed in SnCl 2 Sensitization is carried out in the hydrochloric acid solution of (2) to obtain sensitized SiC powder.
In the present invention, the SnCl 2 Preferably from SnCl 2 Is dissolved in hydrochloric acid. In the present invention, the SnCl 2 The pH of the hydrochloric acid solution of (2) is preferably<0.5，SnCl 2 The concentration of (C) is preferably 10 to 15g/L, more preferably 12 to 13g/L. In the present invention, the sensitization time is preferably 20 to 30 minutes. In the present invention, the sensitization is preferably performed under room temperature, ultrasonic and stirring conditions. The invention adsorbs Sn on the surface of SiC particles by sensitization 2+ ，Sn 2+ Having reducibility, pb can be reduced 2+ The Pb simple substance is reduced to be adsorbed on the surface of SiC particles. After the sensitization is finished, the sensitized SiC powder is washed by deionized water and dried, so that the sensitized SiC powder is obtained.
After sensitized SiC powder is obtained, the sensitized SiC powder is placed in PbCl 2 Activated in the hydrochloric acid solution of (2) to obtain activated SiC powder.
In the present invention, the PbCl 2 Preferably from PbCl 2 Is dissolved in hydrochloric acid. In the present invention, the PbCl 2 The pH of the hydrochloric acid solution of (2) is preferably<1，PbCl 2 Preferably 0.5g/L; the activation time is preferably 20 to 30 minutes. In the present invention, the activation is preferably performed under ultrasonic and agitation conditions. According to the invention, pb simple substance can be formed 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 activated SiC powder is obtained, the activated SiC powder is placed in chemical plating solution for chemical plating, a plating layer of magnetic metal is formed on the surface of the activated SiC powder, and intermediate wave-absorbing powder is obtained.
In the invention, the chemical plating solution comprises 20 to 30g/L of cobalt sulfate, 1 to 10g/L of ferrous sulfate, 45 to 55g/L of sodium hypophosphite, 25 to 35g/L of ammonium citrate, 15 to 25g/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。
As a further preferable scheme, the chemical plating solution preferably 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 to 25g/L of cobalt sulfate, 8 to 12g/L of nickel sulfate, 23 to 27g/L of sodium hypophosphite, 18 to 22g/L of ammonium citrate, 8 to 12g/L of sodium tartrate and NH 3 ·H 2 O。
The preparation process of the electroless plating solution is not particularly required, and the preparation process well known in the art is adopted.
In the invention, cobalt sulfate and ferrous sulfate (or cobalt sulfate and nickel sulfate) are used as main salts, and the main function is to provide metal cations required for forming a coating, sodium hypophosphite is a reducing agent, sodium citrate and sodium tartrate are complexing agents, and the complexing agents can be used with Co in electroless plating solution 2+ 、Fe 2+ 、Ni 2+ A complex is formed, thereby improving the stability at high pH and avoiding the formation of hydroxide precipitate. Ammonia water is used as a pH regulator, and simultaneously has the functions of a complexing agent and a buffer.
In the invention, the pH value of the electroless plating solution is 9-10.
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 even more 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 even more preferably 50 ℃.
In the 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.
The invention changes the content of Co/Fe element (or Co/Ni element) in the plating layer by controlling the mass ratio of cobalt sulfate and ferrous sulfate (or the mass ratio of cobalt sulfate and nickel sulfate) in the chemical plating solution, thereby achieving the effects of changing electromagnetic parameters, optimizing impedance matching and improving the wave absorbing performance.
In the invention, when the electroless plating solution is based on cobalt sulfate and ferrous sulfate, coSO is contained in the electroless plating solution 4 ·7H 2 The concentration of O was 27.5g/L, feSO 4 ·7H 2 When the concentration of O is 2.5g/L, the wave absorbing performance of the obtained magnetic metal@SiC wave absorbing powder is optimal, and at the moment, the content of Co in the magnetic metal coating is 88.45wt% and the content of Fe 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 obtained magnetic metal@SiC 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 is 44.89wt%.
In the invention, after the chemical plating is completed, 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, has poor magnetism and is unfavorable for the magnetic loss of the coating to the incident electromagnetic wave.
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 furnace. The invention uses heat treatment to crystallize magnetic metal, to strengthen magnetic property, to improve the propertySo as to enhance the loss of the incident electromagnetic wave and further improve the wave absorbing performance of the electromagnetic wave.
The invention provides the magnetic metal@SiC wave-absorbing powder prepared by the preparation method, 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 Co content is 88.45wt% and the Fe content is 5.1wt%.
When the magnetic metal coating comprises Co and Ni, the content of Co in the magnetic metal coating 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 invention takes SiC particles as a matrix, coats magnetic heterogeneous metals (Co and Fe or Co and Ni) and can form a unique core-shell structure, the structure can increase the wavelength of electromagnetic waves in an absorption medium, thereby enhancing the absorption of the electromagnetic waves, and simultaneously, the interface polarization existing at the interface between the core-shells can enhance the absorption of the electromagnetic waves. 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, and the magnetic metal layer can generate magnetic loss under the action of the electromagnetic field, so that the wave absorbing performance of the SiC particles is further improved.
The magnetic metal @ SiC wave-absorbing powder and the method of preparing the same according to the present invention will be described in detail 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=10μm), placing in 10mol/L NaOH solution, maintaining the temperature at 50 ℃, coarsening for 30min under the conditions of ultrasonic treatment and continuous stirring, and flushing the SiC powder with deionized water until the SiC powder is neutral to obtain coarsened SiC powder;
coarsening the raw materialPlacing SiC powder in 10g/L SnCl 2 Is a hydrochloric acid solution of 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;
placing the sensitized SiC powder in 0.5g/L PbCl 2 Is a hydrochloric acid solution of pH value<1, activating the solution for 30min at room temperature under ultrasonic and stirring conditions, washing and drying to obtain activated SiC powder;
placing the activated SiC powder into an electroless plating solution for plating cobalt iron, wherein the electroless plating solution (500 mL of plating solution) comprises the following components: coSO 4 ·7H 2 O 27.5g/L、FeSO 4 ·7H 2 Adjusting the pH to 9 by using 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 denoted as (Co, fe) @SiC wave-absorbing powder; the Co content in the coating was 88.45wt% and the Fe content was 5.1wt%.
Example 2
The only difference from example 1 is the CoSO in the electroless plating solution formulation 4 ·7H 2 O is 25g/L, feSO 4 ·7H 2 O is 5g/L. The final (Co, fe) @ SiC wave-absorbing powder coating had a Co content of 81.47wt% and a Fe content of 9.11wt%.
Example 3
The only difference from example 1 is the CoSO in the electroless plating solution formulation 4 ·7H 2 O is 22.5g/L, feSO 4 ·7H 2 O is 7.5g/L. The final (Co, fe) @ SiC wave-absorbing powder coating had a Co content of 82.5wt% and a Fe content of 13.21wt%.
Example 4
The only difference from example 1 is that the electroless plating solution formulation is: coSO 4 ·7H 2 O 25g/L、NiSO 4 ·6H 2 Regulating pH to 10 with O5 g/L, sodium hypophosphite 30g/L, ammonium citrate 20g/L, sodium tartrate 10g/L, and ammonia water at 50deg.C for 10min, and obtaining (Co, ni) @ SiC wave-absorbing powderThe Co content in the coating was 58.26wt% and the Ni content was 39.23wt%.
Example 5
The only difference from example 4 is the CoSO in the electroless plating solution formulation 4 ·7H 2 O is 20g/L, niSO 4 ·6H 2 O is 10g/L. The Co content in the plating layer was 48.4wt% and the Ni content was 44.89wt%.
Example 6
The only difference from example 4 is the CoSO in the electroless plating solution formulation 4 ·7H 2 O is 15g/L, niSO 4 ·6H 2 O is 15g/L. The Co content in the coating was 36.48wt% and the Ni content was 57.63wt%.
Structure and performance characterization:
1. as a result of scanning electron microscope observation of SiC powder, as shown in fig. 1, the surface was smooth as can be seen from fig. 1. Scanning electron microscope observation was performed on the (Co, fe) @ SiC powder prepared in examples 1 to 3 and the (Co, ni) @ SiC powder prepared in examples 4 to 6, respectively, and as a result, as shown in FIGS. 2 and 3, in FIG. 2, (a) is example 1, (b) is example 2, and (c) is example 3, and all of the picture scales in FIG. 2 are 2. Mu.m. 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 through electroless plating.
2. The elemental plane scanning was performed on the (Co, fe) @ SiC absorbing powders prepared in examples 1 to 3, respectively, and the results are shown in fig. 4, wherein (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 elements, and the Co elements are distributed uniformly, while the Fe element content is small and irregularly distributed because of Fe 2+ Electrode potential ratio Co 2+ More negative, indicating that the alloy is more difficult to be reduced in the same electroless plating solution, and Fe in the solution 2+ Concentration is lower than Co 2+ So the Fe element content in the coating is far lower than the Co element.
3. The elemental plane scanning was performed on the (Co, ni) @ SiC absorbing powders prepared in examples 4 to 6, respectively, and the results are shown in fig. 5, wherein (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 the Co and Ni elements is very uniform.
4. FIG. 6 shows the chemical plating solution Co of the (Co, fe) @ SiC sample plating layers of examples 1 to 3 2+ /Fe 2+ In FIG. 6, sample1 is example 1, sample2 is example 2, and sample3 is example 3. As can be seen from fig. 6: with electroless plating solution Co 2+ /Fe 2+ The concentration ratio is smaller and smaller, and 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 plating solution 2+ /Fe 2+ The concentration of (2) affects the Co/Fe element content of the coating.
5. FIG. 7 shows the chemical plating solution Co of Co, ni element in the (Co, ni) @ SiC wave-absorbing powder coating prepared in examples 4 to 6 2+ /Ni 2+ A graph of the concentration ratio, wherein sample1 is example 4, sample2 is example 5, and sample3 is example 6. As can be seen from FIG. 7, with electroless plating solution Co 2+ /Ni 2+ The concentration ratio is smaller and smaller, and the content ratio of Co/Ni element in the plating layer is also smaller and smaller, which indicates Co in the plating solution 2+ /Ni 2+ The concentration of (2) affects the Co/Ni element content of the coating.
6. The electromagnetic parameters are measured by adopting a coaxial method, and the test frequency is 2-18 GHz. Measuring a pair of complex scattering parameters S of the coaxial sample by using an E5071C type vector network analyzer 11 And S is 21 The complex dielectric constant and complex magnetic permeability of the material are obtained through the size of the sample and the transmission coefficient of electromagnetic waves in the sample. The test sample was a coaxial ring specimen having an outer diameter of 7.00mm and an inner diameter of 3.04mm, which was cast after 20wt% paraffin wax and 80wt% (Co, fe) @ SiC powder were uniformly mixed.
The microwave absorption properties of the materials were evaluated using reflection loss RL (Reflection Loss). According to the principle of a microwave transmission line, the condition analysis of a single-layer uniform absorber on a metal substrate is adopted, and the reflection loss RL can be obtained by the following formula:
wherein Zin is the normalized input impedance of electromagnetic waves incident from free space to the material interface; mu (mu) r 、ε r The complex permeability and the complex permittivity 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 shows the relationship between the reflection loss and the absorption percentage of the incident wave, and as shown in table 1, the smaller the reflection loss, the larger the absorption ratio of the surface wave absorbing material to the electromagnetic wave of the society, the better the wave absorbing performance.
TABLE 1 reflection loss versus percent absorption of incident waves
Reflection Loss (RL) Percentage of absorption of incident wave (%)
1 ＜-5dB ＞70％
2 ＜-10dB ＞90％
3 ＜-15dB ＞96.8％
4 ＜-20dB ＞99％
5 ＜-40dB ＞99.9％
Fig. 8 is a graph of Reflection Loss (RL) for (Co, fe) @ SiC samples of examples 1-3 at different frequencies and thicknesses, where (a) is example 1, (b) is example 2, and (c) is example 3. As can be seen from fig. 8: the wave-absorbing properties of the (Co, fe) @ SiC powder were progressively worse as the Co/Fe element in the coating increased, and the sample prepared with the electroless plating solution of example 1 had the best wave-absorbing properties than the pure SiC powder (FIG. 10 is a graph of reflection loss of pure SiC powder at different frequencies and thicknesses), thus it was concluded that Co in the electroless plating solution could be changed 2+ /Fe 2+ The concentration ratio is used for controlling the content ratio of Co/Fe elements in the sample coating, so that the electromagnetic parameters of the wave-absorbing material are regulated and controlled, and the wave-absorbing performance of the wave-absorbing material is further improved.
FIG. 9 is a graph showing the reflection loss of (Co, ni) @ SiC samples at different frequencies and thicknesses in examples 4 to 6, and it is understood from FIG. 9 that the wave-absorbing properties of the (Co, ni) @ SiC powder vary with the variation of the Co/Ni element content ratio in the plating layer, and that the wave-absorbing properties of the sample prepared by the electroless plating solution in example 5 are optimal and higher than those of the pure SiC powder, so that it was concluded that the Co in the electroless plating solution can be changed 2+ /Ni 2+ The concentration ratio is used for controlling the content ratio of Co/Ni elements in the sample plating layer, so that the electromagnetic parameters of the wave-absorbing material are regulated and controlled, and the wave-absorbing performance of the wave-absorbing material is further improved. The wave-absorbing properties of the examples and the pure SiC powders are summarized in table 2.
Table 2 wave absorbing properties of examples and pure SiC powder
RL min Bandwidth (RL)<-5dB) Bandwidth (RL)<-10dB)
Example 1 -23.68dB@10.43GHz 7.34GHz(10.43～17.77) 3.71GHz(14.15～17.86)
Example 2 -17.28dB@10.44GHz 7.08GHz(10.24～17.32) 3.19GHz(14.01～17.20)
Example 3 -13.91dB@17.66GHz 6.62GHz(10.77～17.39) 2.08GHz(11.62～13.70)
Example 4 -9.06dB@16.64GHz 6.93GHz(10.56～17.49) 0
Example 5 -28.44dB@14.47GHz 6.73GHz(10.63～17.36) 3.53GHz(14.47～18.00)
Example 6 -2.61dB@17.49GHz 0 0
Pure SiC powder -13.56dB@15.75GHz 5.76GHz(11.90～17.66) 2.36GHz(15.30～17.66)
Note that: in Table 2, RL min Representing the minimum reflection loss over the entire frequency range, representing the strongest absorption capacity of the absorption sample at a certain frequency, such as: -23.68db@10.43GHz means that the sample has the strongest absorption capacity at 10.43GHz, up to-23.68 dB; 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) shows that the reflection loss of the sample at (10.43-17.77 GHz) is less than-5 dB, and the frequency bandwidth reaches 7.34GH; bandwidth (RL)<-10 dB) indicates a band corresponding to a sample reflection loss less than-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 frequency band.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (9)

1. The preparation method of the magnetic metal@SiC wave-absorbing powder is characterized by comprising the following steps of: coarsening the SiC powder to obtain coarsened SiC powder;
placing the coarsened SiC powder in SnCl 2 Sensitization is carried out in the hydrochloric acid solution of (2) to obtain sensitized SiC powder;
placing the sensitized SiC powder in PbCl 2 Is activated in hydrochloric acid solution to obtainTo activated SiC powder;
placing the activated SiC powder into chemical plating solution for chemical plating, and forming a magnetic metal plating layer on the surface of the activated SiC powder to obtain intermediate wave-absorbing powder; the electroless plating solution comprises CoSO 4 ·7H 2 O 27.5g/L、FeSO 4 ·7H 2 O2.5 g/L, sodium hypophosphite 50g/L, ammonium citrate 30g/L, sodium tartrate 20g/L and NH 3 ·H 2 O, or the electroless plating solution comprises CoSO 4 ·7H 2 O 20g/L、NiSO 4 ·6H 2 O10 g/L, sodium hypophosphite 30g/L, ammonium citrate 20g/L, sodium tartrate 10g/L 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 Co and Ni;
carrying out heat treatment on the intermediate wave-absorbing powder under a vacuum condition to obtain magnetic metal@SiC wave-absorbing powder; the temperature of the heat treatment is 400-500 ℃, and the heat preservation time is 2-4 hours.
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 temperature of the electroless plating is 45-55 ℃.
3. The method according to claim 1 or 2, wherein the electroless plating time is 20 to 40 minutes.
4. The preparation method of claim 1, wherein the roughening solution used for roughening is a NaOH solution, and the concentration of the NaOH solution is 5-10 mol/L.
5. The method according to claim 1 or 4, wherein the roughening temperature is 40-50 ℃ and the time is 20-30 min.
6. The preparation method according to claim 1, wherein the SnCl 2 pH value of hydrochloric acid solution of (2)<0.5，SnCl 2 The concentration of (C) is 10-15 g/L.
7. The method according to claim 6, wherein the sensitization time is 20 to 30min.
8. The method of claim 1, wherein the pbci 2 pH value of hydrochloric acid solution of (2)<1，PbCl 2 Is 0.5g/L; the activation time is 20-30 min.
9. The magnetic metal@SiC wave-absorbing powder prepared by the preparation method of any one of claims 1-8 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.
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