CN110340376B - Flower-shaped nickel wire wave-absorbing material and preparation method thereof - Google Patents
Flower-shaped nickel wire wave-absorbing material and preparation method thereof Download PDFInfo
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- CN110340376B CN110340376B CN201910641275.6A CN201910641275A CN110340376B CN 110340376 B CN110340376 B CN 110340376B CN 201910641275 A CN201910641275 A CN 201910641275A CN 110340376 B CN110340376 B CN 110340376B
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- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
Abstract
The invention discloses a flower-shaped nickel wire wave-absorbing material, which is a linear nickel wire formed by connecting and stacking flower-shaped nickel balls, wherein the flower-shaped nickel balls are formed by stacking sheet nickel, the thickness of the sheet nickel is 10-20 nm, the particle size of the flower-shaped nickel balls is 500-1000 nm, the flower-shaped nickel balls contain holes, and the pore size distribution is 100-400 nm. The preparation method comprises the following steps: dissolving nickel nitrate in glycol solution, and adding a mixed solution of hydrazine hydrate, sodium hydroxide and sodium borohydride at room temperature. Black nickel powder is generated through reaction, the obtained nickel powder is subjected to heat treatment, the heat treatment temperature range is 300-400 ℃, and the flower-shaped nickel wire wave-absorbing material can be obtained. The wave-absorbing material has the characteristics of thin matching thickness and wide wave-absorbing frequency band, can be used for wave-absorbing coatings, and has wide application in the fields of electromagnetic shielding and stealth.
Description
Technical Field
The invention relates to a wave-absorbing material and a preparation method thereof, in particular to a flower-shaped nickel wire wave-absorbing material and a preparation method thereof.
Background
With the use of electronic devices and the development of communication technologies in life, they have become one of the high and new technologies indispensable in our life. However, it also has negative effects, which bring electromagnetic pollution to us, and the radiation of electromagnetic wave can cause abnormal operation of the instrument, and electromagnetic shielding and wave-absorbing materials are needed to reduce the pollution. The wave-absorbing material needs to be developed in the direction of large attenuation coefficient, small reflection loss, wide absorption frequency band, small density and thin matching thickness.
The attenuation coefficient, reflection loss, absorption frequency band and matching thickness of the wave-absorbing material are all determined by the electromagnetic parameters. Therefore, the good wave-absorbing material can be obtained by adjusting the electromagnetic parameters of the wave-absorbing material theoretically. The main mechanisms of the existing wave-absorbing material are magnetic loss and dielectric loss, namely, the loss is improved by improving the imaginary parts of dielectric constant and magnetic conductivity, but the simple improvement of the loss is not feasible, and the impedance matching is required to be achieved. The nickel material has excellent magnetic performance and magnetic loss, but the resistivity is low, the skin effect of a metal conductor can occur, electromagnetic waves are easy to reflect, cannot enter the material, and impedance matching cannot be achieved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the flower-shaped nickel wire wave-absorbing material and the preparation method thereof.
The flower-shaped nickel wire wave-absorbing material is a wire formed by stacking flower-shaped nickel balls, wherein the flower-shaped nickel balls are formed by stacking sheet nickel, the thickness of the sheet nickel is 10-20 nm, the particle size of the flower-shaped nickel balls is 500-1000 nm, the flower-shaped nickel balls contain holes, and the pore size distribution is 100-400 nm.
The preparation method of the flower-shaped nickel wire wave-absorbing material comprises the following steps:
1) dissolving soluble nickel salt in an ethylene glycol solution, wherein the concentration of nickel ions is 0.1-0.5 mol/L;
2) placing the solution obtained in the step 1) in a magnetic field;
3) preparing a sodium hydroxide solution of hydrazine hydrate and sodium borohydride, wherein the molar ratio of nickel ions to sodium borohydride in the step 1) is as follows: 1: 5-1: 25, in a molar ratio to hydrazine hydrate of 1: 13-1: 70;
4) adding the solution obtained in the step 3) into the solution obtained in the step 2), reacting for 3-5 min, and collecting precipitates;
5) drying the sample obtained in the step 4), and then carrying out heat treatment to obtain the flower-shaped nickel wire wave-absorbing material.
In the technical scheme, further, the magnetic field intensity of the magnetic field is 100-200 mT.
Further, the hydrazine hydrate and sodium borohydride sodium hydroxide solution is prepared by adding hydrazine hydrate and sodium borohydride into a sodium hydroxide aqueous solution, wherein the concentration of the sodium hydroxide aqueous solution is 1-4 mol/L.
Further, the preparation method is carried out at room temperature and normal pressure.
Further, the heat treatment conditions in step 5) are as follows: treating at 300-400 ℃ for 1-2 h.
Compared with a nickel wire formed by connecting nickel ball particles only prepared by adopting hydrazine hydrate as a reducing agent, the reaction can be more violent and quicker by adding sodium borohydride, the nickel wire is formed by flaky aggregation on the surface and a magnetic field, and a large-hole-level hole is formed in the flower-shaped nickel wire.
The invention has the beneficial effects that:
the nickel wire constructed by flower-shaped nickel balls is prepared by adopting a liquid phase reduction method, so that the nickel wire has good magnetic loss and dielectric loss, and the nickel wire is subjected to impedance matching by heat treatment, so that the prepared material can obtain very low matching thickness (which can be as low as 0.7mm) and extremely wide absorption frequency band (which can be as high as 13.5+ GHz), and can realize complete absorption in the R frequency band. Compared with other methods for preparing nickel, the method has the advantages that the flower-shaped nickel wire is prepared by using the hydrazine hydrate serving as the double reducing agent and the sodium borohydride, particularly, the sodium borohydride has a porous structure due to the addition of the double reducing agent, the wave absorbing performance of the sodium borohydride is greatly improved, the method can be well applied to the field of wave absorption, the preparation method is simple, the nickel source is rich, the price is low, the reaction can be carried out at room temperature and normal pressure, the reaction time is short, the energy is saved, and the method can be used for industrial production.
Drawings
FIG. 1 is a variation curve of the wave-absorbing performance of the flower-shaped nickel wire wave-absorbing material obtained in example 1 with thickness and frequency in a frequency band of 26.5 GHz-40 GHz;
FIG. 2 is a variation curve of the wave-absorbing performance frequency of the flower-shaped nickel wire wave-absorbing material obtained in example 1 in the matching thickness within the frequency band of 26.5 GHz-40 GHz;
FIG. 3 is a variation curve of the wave-absorbing property of the flower-shaped nickel wire wave-absorbing material obtained in example 2 with thickness and frequency in the frequency band of 26.5 GHz-40 GHz;
FIG. 4 is a variation curve of the wave-absorbing performance frequency of the flower-shaped nickel wire wave-absorbing material obtained in example 2 in the matching thickness within the frequency band of 26.5 GHz-40 GHz;
FIG. 5 is a variation curve of the wave-absorbing property of the flower-shaped nickel wire wave-absorbing material obtained in example 3 with thickness and frequency in the frequency band of 26.5 GHz-40 GHz;
FIG. 6 is a variation curve of the wave-absorbing performance frequency of the flower-shaped nickel wire wave-absorbing material obtained in example 3 in the matching thickness within the frequency band of 26.5 GHz-40 GHz;
FIG. 7 is a variation curve of the wave-absorbing property of the flower-shaped nickel wire wave-absorbing material obtained in example 4 with thickness and frequency in the frequency band of 26.5 GHz-40 GHz;
FIG. 8 is a variation curve of the wave-absorbing performance frequency of the flower-shaped nickel wire wave-absorbing material obtained in example 4 in the matching thickness within the frequency band of 26.5 GHz-40 GHz;
FIG. 9 is a curve showing the wave-absorbing property of the flower-shaped nickel wire wave-absorbing material obtained in example 5 varying with thickness and frequency in the frequency band of 26.5 GHz-40 GHz;
FIG. 10 is an electron microscope image of the flower-like nickel wire wave-absorbing material prepared in example 3;
FIG. 11 is a high power electron microscope image of the flower-like nickel wire wave-absorbing material prepared in example 3;
FIG. 12 is a high power electron microscope image of the flower-like nickel wire wave-absorbing material prepared in example 5;
FIG. 13 is an X-ray diffraction pattern of a flower-like nickel wire without heat treatment.
Detailed Description
The present invention will be described with reference to examples.
Example 1:
1) dissolving soluble nickel salt into 100mL of glycol solution in a beaker, and controlling the concentration of the soluble nickel salt to be 0.1 mol/L;
2) adding two magnets on two sides of the beaker in the step 1) to enable the magnetic field intensity to be 200 mT;
3) preparing a sodium hydroxide solution of hydrazine hydrate and sodium borohydride, wherein the sodium hydroxide solution comprises 0.8g of sodium hydroxide, 5mL of deionized water, 13mL of hydrazine hydrate aqueous solution with the mass fraction of 85%, and 0.001moL of sodium borohydride;
4) adding the solution obtained in the step 3) into the glycol solution obtained in the step 2), fully reacting the solution, and collecting the obtained sample;
5) drying the sample obtained in the step 4), and then carrying out heat treatment at 300 ℃ for 1h to obtain black powder;
6) mixing the obtained black powder with solid paraffin according to a mass ratio of 8: 2, uniformly mixing, controlling the thickness of the mixture to be 1.2mm, and testing the wave absorbing performance of the mixture by using an Agilent vector network analyzer E8363C.
The main component of the flower-shaped nickel wire wave-absorbing material prepared by the embodiment is nickel, the flower-shaped nickel wire wave-absorbing material contains little nickel oxide after heat treatment, and fig. 1 and fig. 2 are respectively a change curve of the wave-absorbing performance of the wave-absorbing material obtained in the embodiment 1 along with frequency and thickness in a frequency band of 26.5 GHz-40 GHz and a change curve of the wave-absorbing material along with frequency under the matching thickness, so that the wave-absorbing material has the wave-absorbing performance at the frequency of 32.8-40 + GHz when the matching thickness is 0.71 mm.
Example 2:
1) dissolving soluble nickel salt into 100mL of glycol solution in a beaker, and controlling the concentration of the soluble nickel salt to be 0.2 mol/L;
2) adding two magnets on two sides of the beaker in which the glycol solution is in the step 1), wherein the magnetic field intensity is 340 mT;
3) preparing a sodium hydroxide solution of hydrazine hydrate and sodium borohydride, wherein the sodium hydroxide solution is 0.4g, the deionized water is 5mL, the hydrazine hydrate aqueous solution with the mass fraction of 85% is 26mL, and the sodium borohydride is 0.002 moL;
4) adding the solution obtained in the step 3) into the glycol solution obtained in the step 2), fully reacting the solution, and collecting the obtained sample;
5) drying the sample obtained in the step 4), and then carrying out heat treatment at 300 ℃ for 1h to obtain black powder;
6) mixing the obtained black powder with solid paraffin according to a mass ratio of 8: 2, uniformly mixing, controlling the thickness of the mixture to be 1.2mm, and testing the wave absorbing performance of the mixture by using an Agilent vector network analyzer E8363C.
The main component of the flower-shaped nickel wire wave-absorbing material prepared by the embodiment is nickel, the flower-shaped nickel wire wave-absorbing material contains little nickel oxide after heat treatment, and fig. 3 and 4 are respectively a change curve of the wave-absorbing performance of the wave-absorbing material obtained in the embodiment 2 along with frequency and thickness in a frequency band of 26.5 GHz-40 GHz and a change curve of the wave-absorbing material along with frequency under the matching thickness, so that the wave-absorbing performance of the wave-absorbing material is shown in 26.7-40 + GHz when the matching thickness is 0.97mm, and a strong absorption peak is shown in the vicinity of 34.7GHz, and the wave-absorbing performance reaches-65 dB.
Example 3:
1) dissolving soluble nickel salt into 100mL of glycol solution in a beaker, and controlling the concentration of the soluble nickel salt to be 0.3 mol/L;
2) adding two magnets on two sides of the beaker in which the glycol solution is positioned in the step 1), wherein the magnetic field intensity is 170 mT;
3) preparing a sodium hydroxide solution of hydrazine hydrate and sodium borohydride, wherein the sodium hydroxide solution comprises 0.8g of sodium hydroxide, 5mL of deionized water, 26mL of hydrazine hydrate aqueous solution with the mass fraction of 85%, and the sodium borohydride is 0.003 moL;
4) adding the solution obtained in the step 3) into the glycol solution obtained in the step 2), fully reacting the solution, and collecting the obtained sample;
5) drying the sample obtained in the step 4), and then carrying out heat treatment at 300 ℃ for 1h to obtain black powder;
6) mixing the obtained black powder with solid paraffin according to a mass ratio of 8: 2, uniformly mixing, controlling the thickness of the mixture to be 1.2mm, and testing the wave absorbing performance of the mixture by using an Agilent vector network analyzer E8363C.
The main component of the flower-shaped nickel wire wave-absorbing material prepared by the embodiment is nickel, the flower-shaped nickel wire wave-absorbing material contains little nickel oxide after heat treatment, and fig. 5 and 6 are respectively a change curve of the wave-absorbing performance of the wave-absorbing material obtained in the embodiment 3 along with frequency and thickness within a frequency band of 26.5 GHz-40 GHz and a change curve of the wave-absorbing material along with frequency under matching thickness, so that the wave-absorbing material has the wave-absorbing performance at the frequency of 26.5-40 + GHz when the matching thickness is 1.1mm, and has a strong absorption peak near 27.4GHz, and the wave-absorbing performance reaches-59 dB.
Example 4:
1) dissolving soluble nickel salt into 100mL of glycol solution in a beaker, and controlling the concentration of the soluble nickel salt to be 0.1 mol/L;
2) two magnets are added on two sides of the beaker in the step 1), and the magnetic field intensity is 170 mT;
3) preparing a sodium hydroxide solution of hydrazine hydrate and sodium borohydride, wherein the sodium hydroxide solution comprises 0.8g of sodium hydroxide, 5mL of deionized water, 13mL of hydrazine hydrate aqueous solution with the mass fraction of 85%, and 0.001moL of sodium borohydride;
4) adding the solution obtained in the step 3) into the glycol solution obtained in the step 2), fully reacting the solution, and collecting the obtained sample;
5) mixing the obtained black powder with solid paraffin according to a mass ratio of 8: 2, uniformly mixing, controlling the thickness of the mixture to be 1.2mm, and testing the wave absorbing performance of the mixture by using an Agilent vector network analyzer E8363C.
The flower-shaped nickel wire prepared in the embodiment is not subjected to heat treatment, and fig. 7 and 8 are respectively a change curve of the wave-absorbing performance of the wave-absorbing material obtained in the embodiment 4 along with frequency and thickness in a frequency band of 26.5 GHz-40 GHz and a change curve of the wave-absorbing performance along with frequency under matched thickness, so that the wave-absorbing performance of the sample prepared in the embodiment is poor, and the wave-absorbing range is only 3 GHz.
Example 5:
1) dissolving soluble nickel salt into 100mL of glycol solution in a beaker, and controlling the concentration of the soluble nickel salt to be 0.1 mol/L;
2) two magnets are added on two sides of the beaker in the step 1), and the magnetic field intensity is 200 mT;
3) preparing hydrazine hydrate sodium hydroxide solution, wherein the mass fraction of sodium hydroxide is 0.8g, the mass fraction of deionized water is 5mL, and the mass fraction of hydrazine hydrate aqueous solution is 85% 13 mL;
4) adding the solution obtained in the step 3) into the glycol solution obtained in the step 2), fully reacting the solution, and collecting the obtained sample;
5) drying the sample obtained in the step 4), and then carrying out heat treatment at 300 ℃ for 1h to obtain black powder;
6) mixing the obtained black powder with solid paraffin according to a mass ratio of 8: 2, uniformly mixing, controlling the thickness of the mixture to be 1.2mm, and testing the wave absorbing performance of the mixture by using an Agilent vector network analyzer E8363C.
In this example, hydrazine hydrate is used as a reducing agent only, fig. 12 is an electron microscope image of the sample obtained in this example, it can be seen that the obtained nickel wire is a common nickel wire, and the flower-shaped nickel wire of the present invention is not obtained (as shown in fig. 10 and 11); FIG. 9 is a curve showing the wave-absorbing property of the wave-absorbing material obtained in example 5 along with the change of frequency and thickness in the frequency band of 26.5 GHz-40 GHz, and it can be seen that the sample prepared in this example has no wave-absorbing property.
Claims (4)
1. The preparation method of the flower-shaped nickel wire wave-absorbing material is characterized in that the material is prepared by adopting the following method, and the preparation method is carried out at room temperature and normal pressure:
1) dissolving soluble nickel salt in an ethylene glycol solution, wherein the concentration of nickel ions is 0.1-0.5 mol/L;
2) placing the solution obtained in the step 1) in a magnetic field;
3) preparing a sodium hydroxide solution of hydrazine hydrate and sodium borohydride, wherein the molar ratio of nickel ions to sodium borohydride in the step 1) is as follows: 1: 5-1: 25, the molar ratio of hydrazine hydrate to hydrazine hydrate is: 1: 13-1: 70;
4) adding the solution obtained in the step 3) into the solution obtained in the step 2), reacting for 3-5 min, and collecting precipitates;
5) drying the sample obtained in the step 4), and then carrying out heat treatment to obtain a flower-shaped nickel wire wave-absorbing material; the material is in a linear shape formed by stacking flower-shaped nickel balls, wherein the flower-shaped nickel balls are formed by stacking sheet nickel, the thickness of the sheet nickel is 10-20 nm, the particle size of the flower-shaped nickel balls is 500-1000 nm, the flower-shaped nickel balls contain holes, and the pore size distribution is 100-400 nm.
2. The preparation method of the flower-shaped nickel wire wave-absorbing material according to claim 1, wherein the magnetic field strength of the magnetic field is 100-200 mT.
3. The preparation method of the flower-shaped nickel wire wave-absorbing material according to claim 1, wherein the sodium hydroxide solution of hydrazine hydrate and sodium borohydride is prepared by adding hydrazine hydrate and sodium borohydride into a sodium hydroxide solution, wherein the concentration of the sodium hydroxide solution is 1-4 mol/L.
4. The method for preparing the flower-shaped nickel wire wave-absorbing material according to claim 1, wherein the heat treatment conditions in the step 5) are as follows: treating at 300-400 ℃ for 1-2 h.
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