CN110358500B - Preparation method and application of porous carbon-loaded cobaltosic oxide-coated cobalt alloy wave-absorbing material - Google Patents
Preparation method and application of porous carbon-loaded cobaltosic oxide-coated cobalt alloy wave-absorbing material Download PDFInfo
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Abstract
The invention belongs to the technical field of electromagnetic wave-absorbing materials, and particularly relates to porous carbon loaded Co 3 O 4 A preparation method and application of a Co-coated elemental alloy light wave-absorbing material. Adjusting the fish scale extract to neutral, and adding CoCl 2 ·6H 2 O, freeze drying the mixture, and then carrying out high-temperature treatment to obtain the porous carbon loaded Co 3 O 4 A light electromagnetic wave-absorbing material coated with Co simple substance alloy. The preparation method has the advantages of wide raw materials, adjustable load capacity, low cost, simple process and the like, and the prepared material has better impedance matching and electromagnetic attenuation capabilities.
Description
Technical Field
The invention belongs to the technical field of electromagnetic wave-absorbing materials, and particularly relates to porous carbon loaded Co 3 O 4 A preparation method and application of a Co-coated elemental alloy light wave-absorbing material.
Background
In recent years, the rapid development of wireless electronic communication equipment brings convenience to people, and the problems of electronic interference and pollution caused by the excessive use of electronic equipment are increased, so that the wireless electronic communication equipment has serious interference problems to the daily life of people and some high-precision instruments. Therefore, the elimination of the electromagnetic interference problem has been achieved. Generally, electromagnetic wave absorbing materials are classified into two types according to loss mechanisms: dielectric loss materials and magnetic loss materials. However, each of them has certain disadvantages as an electromagnetic wave absorbing material. Therefore, the method for compounding the two loss materials into the composite material is a new idea of the novel electromagnetic wave-absorbing material. The dielectric loss and the magnetic loss of the composite material combined with the two materials are interacted, so that the composite material has good impedance matching performance, and can enable more electromagnetic waves to enter the wave-absorbing material and convert the loss of the wave-absorbing material into other energy forms. In addition, the composite material combined by the two materials has the advantages of low thickness, light weight and the like, but most of the preparation process flows are relatively complex, byproducts in the composite material can cause harm to the environment, human bodies and the like, and meanwhile, the obtained composite material has uneven distribution of loaded particles and is easy to stack to form a 'dead zone'. On the other hand, the microstructure of the material is another important index for determining the performance of the electromagnetic wave-absorbing material. The porous structure not only can provide good impedance matching, but also can enable electromagnetic waves to be reflected back and forth between the hole walls, and is more beneficial to the loss of the electromagnetic waves. Therefore, the structure of the porous structure is also an important direction for manufacturing the electromagnetic wave-absorbing material, but the preparation of the porous structure is often limited by the complicated preparation process (such as a template method and the like).
Disclosure of Invention
The invention aims to solve the technical problem of providing a porous carbon loaded Co 3 O 4 Co-coated elemental alloy light electromagnetic absorption material and preparation method and application thereof
In order to achieve the purpose, the invention is realized by adopting the following technical scheme:
porous carbon loaded Co 3 O 4 A preparation method of a Co-coated elemental alloy light wave-absorbing material comprises the steps of adjusting a fish scale extract to be neutral, and then mixing the fish scale extract with CoCl 2 ·6H 2 O, freeze drying the mixture, and then carrying out high-temperature treatment to obtain the porous carbon loaded Co 3 O 4 A light electromagnetic wave-absorbing material coated with Co simple substance alloy.
The fish scale extract is mixed with CoCl 2 ·6H 2 The volume mol ratio of O is 30-50: 0.005-0.02; the high-temperature treatment is to sinter the freeze-dried mixture for 1-3 hours at 600-900 ℃ in the presence of inert gas.
The fish scale extract is neutralized with CoCl after being regulated by acid 2 ·6H 2 O mixing; wherein the acid is selected from hydrochloric acid, sulfuric acid, nitric acid, acetic acid, etc., and is used for adjusting the extract to neutral; furthermore, hydrochloric acid with the concentration of 5-9 mol/L can be adopted.
The fish scale extract is prepared by dissolving fish scales and alkali in distilled water, performing hydrothermal reaction in a high-pressure reaction kettle, naturally cooling to room temperature after reaction, and performing suction filtration to obtain the fish scale extract (mainly comprising I, II, III type amino acids and I type collagen).
The ratio of the weight of the fish scales to the volume of the alkali to the volume of the deionized water is 1-3: 30-120. The alkali can be potassium hydroxide or sodium hydroxide; it can be used as adjuvant to extract amino acids, collagen, etc. from fish scales, and further potassium hydroxide can be used.
The temperature of the hydrothermal reaction is 80-180 ℃, and the time of the hydrothermal reaction is 12-24 h.
Porous carbon loaded Co prepared by the method 3 O 4 Coating with Co 3 O 4 The Co-coated simple substance alloy light electromagnetic wave-absorbing material is prepared by the method, has uniform porous and pore distribution, and is prepared by uniformly distributing granular simple substance cobalt in the pores of the porous carbon, so that the porous carbon loaded with Co is obtained 3 O 4 Coated Co 3 O 4 The light electromagnetic wave-absorbing material coated with Co simple substance alloy.
Porous carbon loaded Co 3 O 4 Coated Co 3 O 4 Application of Co-coated elemental alloy light electromagnetic wave-absorbing material, and porous carbon loaded Co 3 O 4 Coating with Co 3 O 4 The application of the Co-coated elemental alloy light electromagnetic wave-absorbing material in the treatment of the problem of electromagnetic pollution in daily life. Furthermore, the problem of electromagnetic pollution in the daily life of material processing can be the harm of electromagnetic radiation of mobile phones, computers and the like to human bodies and the problem of electromagnetic interference in civil communication.
The invention has the advantages that:
compared with the existing reported wave-absorbing material, the porous carbon loaded Co prepared by the method disclosed by the invention 3 O 4 The Co-coated simple substance alloy light electromagnetic wave-absorbing material combines magnetic loss and dielectric loss to attenuate electromagnetic waves, wherein Co 3 O 4 The interface of the Co elemental alloy and the porous carbon material is coated, and the interface polarization loss at the interface of the porous carbon material and the air plays a main role. The appropriate volume of the holes provides good impedance matching and provides an important prerequisite for more electromagnetic waves to enter the absorber. On the other hand, the porous structure can further cause the return reflection loss of the electromagnetic wave; in addition, the preparation method has the advantages of wide raw materials, adjustable load capacity, low cost, simple process, environmental friendliness and the like, and the prepared material has good electromagnetic attenuation capability.
Drawings
FIGS. 1(a), (b), (c) are the present inventionPorous carbon loaded with Co prepared in inventive examples 1,2,3 3 O 4 A scanning electron microscope image of the Co-coated elemental alloy light electromagnetic wave-absorbing material;
FIGS. 2(a), (b), (c) are porous carbon Co-loaded carbon materials prepared in examples 1,2,3 of the present invention 3 O 4 A transmission electron microscope picture of the Co-coated elemental alloy light electromagnetic wave-absorbing material;
FIG. 3 shows the porous carbon Co-supported catalyst prepared in example 1 of the present invention 3 O 4 An X-ray diffraction pattern of the Co-coated elemental alloy light electromagnetic wave-absorbing material;
FIG. 4 shows the porous carbon Co-supported catalyst prepared in example 2 of the present invention 3 O 4 An X-ray diffraction pattern of the Co-coated elemental alloy light electromagnetic wave-absorbing material;
FIG. 5 shows the porous carbon loaded with Co prepared in example 3 of the present invention 3 O 4 An X-ray diffraction pattern of the Co-coated elemental alloy light electromagnetic wave-absorbing material;
FIG. 6 shows the porous carbon Co-supported catalyst prepared in example 1 of the present invention 3 O 4 A Raman spectrogram of the Co-coated elemental alloy light electromagnetic wave-absorbing material;
FIG. 7 shows the porous carbon Co-supported catalyst prepared in example 2 of the present invention 3 O 4 A Raman spectrogram of the Co-coated elemental alloy light electromagnetic wave-absorbing material;
FIG. 8 shows the porous carbon Co-supported catalyst prepared in example 3 of the present invention 3 O 4 A Raman spectrogram of the Co-coated elemental alloy light electromagnetic wave-absorbing material;
FIG. 9 is a porous carbon Co-loaded sample prepared in example 1 of the present invention 3 O 4 A reflection loss spectrogram of the Co-coated elemental alloy light electromagnetic wave-absorbing material;
FIG. 10 shows the porous carbon Co-supported catalyst prepared in example 2 of the present invention 3 O 4 A reflection loss spectrogram of the Co-coated elemental alloy light electromagnetic wave-absorbing material;
FIG. 11 is a porous carbon Co-loaded sample prepared in example 3 of the present invention 3 O 4 And (3) a reflection loss spectrogram of the Co-coated elemental alloy light electromagnetic wave-absorbing material.
Detailed Description
In order to make the purpose and technical solution of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings.
Adding fish scales and potassium hydroxide into distilled water for dissolving, then placing the mixture into a high-pressure reaction kettle for hydrothermal reaction, naturally cooling the mixture to room temperature after the reaction is completed, and carrying out suction filtration to obtain a fish scale extract; adjusting the fish scale extract to neutral, adding CoCl 2 ·6H 2 And O, freeze-drying, then carrying out high-temperature treatment on the freeze-dried product in a tubular furnace, and then cleaning and drying the product after high-temperature treatment to obtain the wave-absorbing material. The invention takes the fish scales as the precursor, and has the advantages of simple preparation process, no pollution of byproducts and the like. Meanwhile, the natural porous structure of the fish scale extract provides advantages for the preparation of the porous carbon material, and the porous carbon is used as a carrier to further effectively prevent the accumulation of load particles. The preparation method has the advantages of wide raw materials, adjustable load capacity, low cost and the like, and the prepared material has better impedance matching and electromagnetic attenuation capacity.
Example 1：
Porous carbon loaded Co 3 O 4 The preparation method of the Co-coated elemental alloy light electromagnetic absorption material comprises the following steps:
step 3, after the reaction in the step 2 is finished, carrying out vacuum filtration to obtain a light yellow solution, and adjusting the solution to be neutral by using 8mol/L hydrochloric acid;
and 6, after the tube furnace is cooled to room temperature, taking out the tube furnace, washing the tube furnace by using deionized water, and drying the tube furnace at 60 ℃ to obtain the required product (see the figure 1(a), 2(a), 3 and 6).
Examples2：
Porous carbon loaded Co 3 O 4 The preparation method of the Co-coated elemental alloy light electromagnetic absorption material comprises the following steps:
step 3, after the reaction in the step 2 is finished, carrying out vacuum filtration to obtain a light yellow solution, and adjusting the solution to be neutral by using 8mol/L hydrochloric acid;
and 6, after the tube furnace is cooled to room temperature, taking out the tube furnace, washing the tube furnace by using deionized water, and drying the tube furnace at 60 ℃ to obtain the required product (see the figures 1(b), 2(b), 4 and 7).
Examples3：
Porous carbon loaded Co 3 O 4 The preparation method of the Co-coated elemental alloy light electromagnetic absorption material comprises the following steps:
step 3, after the reaction in the step 2 is finished, carrying out vacuum filtration to obtain a light yellow solution, and adjusting the solution to be neutral by using 8mol/L hydrochloric acid;
and 6, after the tube furnace is cooled to room temperature, taking out the tube furnace, washing the tube furnace by using deionized water, and drying the tube furnace at 60 ℃ to obtain the required product (see the figures 1(c), 2(c), 5 and 8).
FIGS. 1(a), (b), and (c) are respectively the porous carbon supported Co of example 1, case 2, and case 3 3 O 4 In an SEM image of the light electromagnetic absorption material coated with the Co elemental alloy, it can be seen from FIG. 1 that the carbon material has a porous structure and the holes are distributed relatively uniformly. Further, alloy particles are supported on the porous carbon material; with CoCl 2 ·6H 2 The increasing of the O quantity, the porous carbon material becomes transparent, which shows that the thickness of the carbon wall is reduced, the cobalt simple substance particles on the porous carbon material are obviously increased, and the distribution is uniform (figure 1 b); CoCl 2 ·6H 2 Further increase in O, the particles of elemental cobalt attached to the carbon also increased significantly.
FIGS. 2(a), (b), and (c) are respectively the porous carbon supported Co of example 1, case 2, case 3 3 O 4 TEM image of Co-coated elemental alloy light electromagnetic absorption material, it can be seen from their respective lower left corner small images that the alloy presents typical core-shell structure, and Co 3 O 4 As the "shell", the elemental cobalt acts as its "core".
FIGS. 3 to 5 are X-ray diffraction patterns of examples 1 to 3, respectively, and it can be seen from the XRD patterns that diffraction peaks appear at 44.1 DEG, 51.4 DEG, and 75.6 DEG, respectively, corresponding to (111), (200), and (220) crystal planes of Co simple substance, and the peak positions are not significantly shifted.
FIGS. 6 to 8 are Raman spectra of examples 1 to 3, respectively. All samples were 1350 and 1590cm -1 Peaks appear, corresponding to the D and G peaks, respectively, for carbon. And at 750cm -1 Corresponds to the vibration peak of the cobalt simple substance, 460 and 510cm -1 The left and right peaks correspond to Co 3 O 4 And the peak intensity is continuously increased along with the increase of the cobalt elemental loading.
The materials obtained in the embodiments 1-3 are respectively and uniformly mixed with paraffin wax samples according to the mass ratio of 3:1, the mixture is pressed into circular rings with the inner diameter of 3.04mm, the outer diameter of 7.00mm and the thickness of 2.00mm by a mould, the electromagnetic parameters of the circular rings are respectively measured by a vector grid analyzer, and then the reflection loss spectrograms of the materials obtained in the embodiments are respectively simulated and calculated (see figures 9-11).
FIGS. 9 to 11 are reflection loss spectra of the paraffin loading of 75% calculated by the reflection loss equation in examples 1 to 3, respectively. As can be seen from the graph, the maximum reflection loss at 4.8mm of the sample obtained in example 1 is-42.8 dB; the maximum reflection loss of the sample obtained in the embodiment 2 at 1.8mm is-26.8 dB; example 3 the maximum reflection loss at 2.09mm was-45.2 dB. The main reason for the difference between the three embodiments is that the loading amount of the cobalt element is changed, the loading amount is increased, the dielectric loss and the magnetic loss of the material are improved to a certain extent, and then the thickness corresponding to the maximum reflection loss is reduced (embodiment 1 is compared with embodiment 2), the loading amount is further increased, and the maximum reflection loss of the material is also increased (embodiment 2 is compared with embodiment 3).
In conclusion, amino acid protein in the fish scale extract is used as a reducing agent to reduce a cobalt simple substance, and the cobalt simple substance is oxidized by oxygen-containing groups in the material to obtain porous carbon loaded with Co 3 O 4 The Co elemental alloy coated electromagnetic wave-absorbing material can obviously regulate and control the electromagnetic wave-absorbing performance of the material along with the control of the loading capacity.
It should be understood that the above examples are only for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And such obvious variations or modifications which fall within the spirit of the invention are intended to be covered by the scope of the present invention.
Claims (7)
1. A preparation method of a porous carbon-loaded cobaltosic oxide-coated cobalt alloy wave-absorbing material is characterized in that a fish scale extract is adjusted to be neutral and then mixed with CoCl 2 •6H 2 Mixing with O, freeze drying, and concentratingPerforming temperature treatment to obtain a porous carbon loaded cobaltosic oxide coated cobalt alloy wave-absorbing material;
the porous carbon-loaded cobaltosic oxide-coated cobalt alloy wave-absorbing material is of a core-shell structure, and Co 3 O 4 As the "shell", the cobalt simple substance is used as the "core";
adding fish scales and alkali into distilled water for dissolving, performing hydrothermal reaction in a high-pressure reaction kettle, naturally cooling to room temperature after reaction, and performing suction filtration to obtain a fish scale extract;
the fish scale extract is type I, type II, type III amino acid and type I collagen;
the high-temperature treatment is to sinter the freeze-dried mixture for 1-3 hours at 600-900 ℃ in the presence of inert gas.
2. The preparation method of the porous carbon-loaded cobaltosic oxide-coated cobalt alloy wave-absorbing material according to claim 1, wherein the fish scale extract and CoCl are used 2 •6H 2 The volume mol ratio of O is 30-50: 0.005-0.02.
3. The preparation method of the porous carbon-loaded cobaltosic oxide-coated cobalt alloy wave-absorbing material according to claim 1, wherein the fish scale extract is neutralized with CoCl after being adjusted to be neutral by acid 2 •6H 2 And (4) mixing the materials.
4. The preparation method of the porous carbon-loaded cobaltosic oxide-coated cobalt alloy wave-absorbing material according to claim 1, wherein the ratio of fish scale (mass), alkali (mass) and deionized water (volume) is 1-3: 30-120.
5. The preparation method of the porous carbon-loaded cobaltosic oxide-coated cobalt alloy wave-absorbing material according to claim 1, wherein the hydrothermal reaction temperature is 80-180 ℃, and the hydrothermal reaction time is 12-24 h.
6. Porous carbon-supported tetraoxide prepared by the method of claim 1The cobaltosic oxide-coated cobalt alloy wave-absorbing material is characterized in that the porous carbon-loaded cobaltosic oxide-coated cobalt alloy wave-absorbing material prepared by the method in claim 1 is of a core-shell structure, and Co is in a Co-coated cobalt alloy wave-absorbing material 3 O 4 As a shell, the cobalt simple substance is used as a core, wherein the pores of the porous carbon are uniformly distributed, and the granular simple substance cobalt is uniformly distributed in the pores of the porous carbon.
7. The application of the porous carbon-loaded cobaltosic oxide-coated cobalt alloy wave-absorbing material in claim 6 is characterized in that the porous carbon-loaded cobaltosic oxide-coated cobalt alloy wave-absorbing material is applied to treatment of electromagnetic pollution in daily life.
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| CN109181640A (en) * | 2018-09-18 | 2019-01-11 | 北京科技大学 | The preparation method for the porous carbon absorbing material that cobalt and oxide are inlayed |
| CN109354004A (en) * | 2018-10-17 | 2019-02-19 | 西安理工大学 | A method of classifying porous carbon material is prepared using fish scale |
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| CN102107863A (en) * | 2009-12-25 | 2011-06-29 | 北京化工大学 | Porous carbon material and preparation method thereof |
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