CN109257915B - Cobalt-nickel/silicon dioxide aerogel composite wave-absorbing material and preparation method thereof - Google Patents
Cobalt-nickel/silicon dioxide aerogel composite wave-absorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a cobalt-nickel/silicon dioxide aerogel composite wave-absorbing material and a preparation method thereof, wherein the wave-absorbing material comprises silicon dioxide aerogel and cobalt, nickel and cobalt-nickel alloy magnetic metal growing on the silicon dioxide aerogel in situ, and the preparation method comprises the following steps: step 1: mixing cobalt nitrate, nickel nitrate, ethylene glycol, ethyl orthosilicate and phosphoric acid; step 2: cooling the mixed solution, adding isopropanol and deionized water, and continuing stirring; and step 3: placing the wet gel obtained in the step 2 in an isopropanol solution of nickel nitrate and cobalt nitrate for normal-temperature aging; and 4, step 4: subjecting the aged wet gel obtained in the step 3 to supercritical drying treatment; the wave-absorbing material has the wave-absorbing property of magnetic metal of metal cobalt, nickel and alloy thereof. The preparation method can prepare the light wave-absorbing material with abundant porous structures.
Description
Technical Field
The invention relates to the technical field of wave-absorbing materials, in particular to a cobalt-nickel/silicon dioxide aerogel composite wave-absorbing material and a preparation method thereof.
Background
The wave-absorbing material is a key factor of stealth technology, plays an important role in modern war and is always valued by all countries in the world. Traditional wave-absorbing materials, such as single ferrite or metal powder coatings, have been widely researched and applied due to their high magnetic saturation strength and large theoretical coercive force, but have the disadvantages of large specific gravity and single loss mechanism, which limits their use in the field of high demand for light wave-absorbing materials, so that wave-absorbing materials with "light, thin and wide" excellent properties have become hot spots developed in various countries.
The magnetic metal has high saturation magnetization, excellent magnetic conductivity and smaller magnetostriction coefficient, so that the magnetic metal is very important for obtaining a high-absorption electromagnetic wave absorption material, and the cobalt-nickel alloy, especially the nano cobalt-nickel alloy micro powder has physical, chemical and mechanical properties different from those of simple substance nickel and cobalt metal micro powder, so that the magnetic metal has wide application prospects in the industries of hard alloys, magnetic materials, catalysts, batteries and the like.
The magnetic metal micro powder wave-absorbing material mainly absorbs electromagnetic waves in modes of magnetic hysteresis loss, eddy current loss and the like, and has the advantages of high Curie temperature, good temperature stability, high magnetization intensity, larger microwave permeability and the like, so the magnetic metal micro powder wave-absorbing material is widely applied to the field of wave-absorbing materials. However, the magnetic metal micro powder has the problems of high density, poor oxidation resistance, poor acid and alkali resistance, low filling rate, low resistivity, high dielectric constant and the like.
The aerogel is a novel porous material with a nano-scale continuous network structure, has the characteristics of large specific surface area, high porosity, low density, low thermal conductivity and the like, shows special properties in various aspects such as optics, electrics, thermology and the like, and has wide application in the research fields of catalysts, drug carriers, heat insulation materials and the like. However, silica aerogel is formed by stacking nano-sized particles, and thus has low strength and is easily broken, resulting in limited use.
At present, research on aerogel composite nano materials prepared by introducing metal cobalt and nickel components into aerogel is reported, but the introduced metal cobalt and nickel components are single nickel or cobalt, the research on composite materials prepared by introducing cobalt-nickel alloy into aerogel materials by an in-situ synthesis method is rarely reported, the prepared composite materials mainly focus on the application of catalytic performance, and the research on the wave-absorbing performance of the metal aerogel composite materials is rarely reported.
Disclosure of Invention
The invention provides a cobalt-nickel/silicon dioxide aerogel composite wave-absorbing material and a preparation method thereof, wherein the cobalt-nickel/silicon dioxide aerogel composite wave-absorbing material has the wave-absorbing property of magnetic metal of metal cobalt, nickel and alloy thereof, overcomes the defect of high density of the traditional wave-absorbing material, and has the characteristics of high specific surface area of a nano material and the like; the preparation method can prepare the wave-absorbing material with abundant porous structures, and effectively enhances the wave-absorbing capacity of the material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a cobalt-nickel/silicon dioxide aerogel composite wave-absorbing material comprises silicon dioxide aerogel and cobalt, nickel and cobalt-nickel alloy magnetic metal growing on the silicon dioxide aerogel in situ.
Further, the composite wave-absorbing material comprises 1-25 parts of cobalt, nickel and cobalt-nickel alloy magnetic metal and 75-99 parts of silica aerogel, wherein the components are calculated by mass.
Further, cobalt, nickel, and cobalt nickel alloy magnetic metals can be grown in the form of nanowires in silica aerogel materials.
The invention also provides a preparation method of the cobalt-nickel/silicon dioxide aerogel composite wave-absorbing material, which comprises the following steps:
step 1: mixing cobalt nitrate, nickel nitrate, ethylene glycol, ethyl orthosilicate and phosphoric acid, and stirring to form a mixed solution, wherein the stirring temperature is 90 ℃;
step 2: cooling the mixed solution, adding isopropanol and deionized water, continuously stirring to form uniform mixed liquid, and standing at normal temperature to form wet gel;
and step 3: placing the wet gel obtained in the step 2 in an isopropanol solution of nickel nitrate and cobalt nitrate for normal-temperature aging, wherein the aging time is 48 hours;
and 4, step 4: and (4) carrying out supercritical drying treatment on the aged wet gel in the step (3) to obtain the composite wave-absorbing material loaded with metal cobalt, nickel and alloy thereof and silicon dioxide aerogel.
Further, the step 2 further comprises a step of adding a chemical drying control agent to the cooled mixed solution, wherein the chemical drying control agent is urea or N, N-dimethylacetamide.
Further, the step 4 comprises a step of adding isopropanol into the aged wet gel for solution replacement.
Further, the step 4 comprises a step of carrying out surface modification treatment on the gel before drying, wherein the used surface modifier is an isopropanol solution containing 8-10 vol% of trimethylchlorosilane, and the modification time is 12 h.
Further, the mol ratio of the cobalt nitrate, the nickel nitrate, the ethylene glycol, the ethyl orthosilicate and the phosphoric acid in the step 1 is 0.08-0.25:0.02-0.25:4-5:1:1x10-3Stirring for 10 hours by adopting a magnetic stirring device; in the step 2, the molar ratio of the addition amount of the isopropanol and the deionized water to the tetraethoxysilane is 4:3-4: 1.
Furthermore, the molar ratio of the added urea or N, N-dimethylacetamide to the cobalt nitrate and the nickel nitrate in the step 2 is 10:4-5: 1-5.
Compared with the prior art, the invention has the following advantages:
according to the cobalt-nickel/silicon dioxide aerogel composite wave-absorbing material, cobalt, nickel and cobalt-nickel alloy magnetic metal are grown on the silicon dioxide aerogel in situ, so that the cobalt-nickel/silicon dioxide aerogel composite wave-absorbing material has the wave-absorbing property of the magnetic metal of metal cobalt, nickel and alloy thereof, overcomes the defect of high density of the traditional wave-absorbing material, and has the characteristics of high specific surface area of a nano material and the like; according to the preparation method of the cobalt-nickel/silicon dioxide aerogel composite wave-absorbing material, the steps 1-4 are matched, so that the wave-absorbing material with rich porous structures can be prepared, and the wave-absorbing capacity of the material is effectively enhanced.
Drawings
Fig. 1 is a schematic wave-absorbing diagram of a cobalt-nickel/silica aerogel composite wave-absorbing material prepared in embodiment 3 of the present invention.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings.
Example 1
A cobalt-nickel/silicon dioxide aerogel composite wave-absorbing material comprises silicon dioxide aerogel and cobalt, nickel and cobalt-nickel alloy magnetic metal growing on the silicon dioxide aerogel in situ.
The composite wave-absorbing material comprises 1-25 parts of cobalt, nickel and cobalt-nickel alloy magnetic metal and 75-99 parts of silica aerogel, wherein the components are calculated by mass.
Cobalt, nickel and cobalt nickel alloy magnetic metals can be grown in the form of nanowires in silica aerogel materials.
The invention also provides a preparation method of the cobalt-nickel/silicon dioxide aerogel composite wave-absorbing material, which comprises the following steps:
step 1: mixing cobalt nitrate, nickel nitrate, ethylene glycol, ethyl orthosilicate and phosphoric acid, and stirring to form a mixed solution, wherein the stirring temperature is 90 ℃;
step 2: cooling the mixed solution, adding isopropanol and deionized water, continuously stirring to form uniform mixed liquid, and standing at normal temperature to form wet gel;
and step 3: placing the wet gel obtained in the step 2 in an isopropanol solution of nickel nitrate and cobalt nitrate for normal-temperature aging, wherein the aging time is 48 hours;
and 4, step 4: and (4) carrying out supercritical drying treatment on the aged wet gel in the step (3) to obtain the composite wave-absorbing material loaded with metal cobalt, nickel and alloy thereof and silicon dioxide aerogel.
The step 2 also comprises a step of adding a chemical drying control agent into the cooled mixed solution, wherein the chemical drying control agent is urea.
The step 4 also comprises the step of adding isopropanol into the aged wet gel before drying for solution replacement.
The step 4 also comprises a step of carrying out surface modification treatment on the gel before drying, wherein the used surface modifier is an isopropanol solution containing 10 vol% of trimethylchlorosilane, and the modification time is 12 h.
In the step 1, the molar ratio of the cobalt nitrate to the nickel nitrate to the ethylene glycol to the ethyl orthosilicate to the phosphoric acid is 0.1:0.1:5:1:1x10-3Stirring for 10 hours by adopting a magnetic stirring device; in the step 2, the molar ratio of the addition amount of the isopropanol and the deionized water to the tetraethoxysilane is 4:4: 1.
The stirring temperature in step 1 was 90 ℃.
In the step 2, the molar ratio of the added urea to the cobalt nitrate and the nickel nitrate is 2:1: 1.
The stirring time in step 2 was 8 hours.
Through the steps, the prepared wave-absorbing material has the metal content of 12 percent and the specific surface area of 448.3m2And g, when the thickness of the composite material is 2mm, the peak value of the reflectivity can reach-27 dB in the range of 2-18 GH.
Example 2
In this example, cobalt nitrate, nickel nitrate, ethylene glycol in step 1The molar ratio of the ethyl orthosilicate to the phosphoric acid is 0.08:0.02:4:1:1x10-3Stirring for 10 hours by adopting a magnetic stirring device; in the step 2, the molar ratio of the addition amount of the isopropanol and the deionized water to the tetraethoxysilane is 3:4: 1; in the step 2, the molar ratio of the addition amount of the N, N-dimethylacetamide to the cobalt nitrate and the nickel nitrate is 10:4: 1. Otherwise, the same as in example 1 was applied.
Through the steps, the prepared wave-absorbing material has the metal content of 5 percent and the specific surface area of 676.5m2And g, when the thickness of the composite material is 2mm, the reflectivity peak value in the range of 2-18GH can reach-20 dB.
Example 3
As shown in attached figure 1, in the embodiment, the molar ratio of the cobalt nitrate to the nickel nitrate to the ethylene glycol to the ethyl orthosilicate in the step 1 is 0.25:0.25:5:1:1x10-3Stirring for 10 hours by adopting a magnetic stirring device; in the step 2, the molar ratio of the addition amount of the isopropanol and the deionized water to the tetraethoxysilane is 3:4: 1; in the step 2, the molar ratio of the addition amount of the N, N-dimethylacetamide to the cobalt nitrate and the nickel nitrate is 2:1: 1. Otherwise, the same as in example 1 was applied.
Through the steps, the prepared wave-absorbing material has the metal content of 22 percent and the specific surface area of 390.6m2And g, when the thickness of the composite material is 2mm, the peak value of the reflectivity can reach-32 dB in the range of 2-18 GH.
The present invention is not limited to the above-described embodiments, which are described in the specification and illustrated only for illustrating the principle of the present invention, but various changes and modifications may be made within the scope of the present invention as claimed without departing from the spirit and scope of the present invention. The scope of the invention is defined by the appended claims.
Claims (6)
1. A preparation method of a cobalt-nickel/silicon dioxide aerogel composite wave-absorbing material is characterized by comprising the following steps:
step 1: mixing cobalt nitrate, nickel nitrate, ethylene glycol, ethyl orthosilicate and phosphoric acid, and stirring to form a mixed solution, wherein the stirring temperature is 90 ℃;
step 2: cooling the mixed solution, adding isopropanol and deionized water, continuously stirring to form uniform mixed liquid, and standing at normal temperature to form wet gel;
and step 3: placing the wet gel obtained in the step 2 in an isopropanol solution of nickel nitrate and cobalt nitrate for normal-temperature aging, wherein the aging time is 48 hours;
and 4, step 4: and (4) carrying out supercritical drying treatment on the aged wet gel in the step (3) to obtain the composite wave-absorbing material loaded with metal cobalt, nickel and alloy thereof and silicon dioxide aerogel.
2. The preparation method of the cobalt nickel/silica aerogel composite wave-absorbing material according to claim 1, characterized in that the step 2 further comprises a step of adding a chemical drying control agent to the cooled mixed solution, wherein the chemical drying control agent is urea or N, N-dimethylacetamide.
3. The preparation method of the cobalt nickel/silica aerogel composite wave-absorbing material according to claim 1, characterized in that the step 4 further comprises a step of adding isopropanol into the aged wet gel for solution replacement.
4. The preparation method of the cobalt nickel/silica aerogel composite wave-absorbing material according to claim 1, characterized in that the step 4 further comprises a step of performing surface modification treatment on the gel before drying, wherein the used surface modifier is an isopropanol solution containing 8-10 vol% of trimethylchlorosilane, and the modification time is 12 hours.
5. The preparation method of the cobalt nickel/silicon dioxide aerogel composite wave-absorbing material according to claim 1, wherein the molar ratio of cobalt nitrate, nickel nitrate, ethylene glycol, ethyl orthosilicate and phosphoric acid in the step 1 is 0.08-0.25:0.02-0.25:4-5:1:1x10-3Stirring for 10 hours by adopting a magnetic stirring device; in the step 2, the molar ratio of the addition amount of the isopropanol and the deionized water to the tetraethoxysilane is 4:3-4: 1.
6. The preparation method of the cobalt nickel/silica aerogel composite wave-absorbing material according to claim 1, wherein the molar ratio of the added amount of urea or N, N-dimethylacetamide to cobalt nitrate and nickel nitrate in the step 2 is 10:4-5: 1-5.
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| CN111282522B (en) * | 2020-02-10 | 2022-02-08 | 四川大学 | Metal organic framework composite aerogel material and preparation method and application thereof |
| CN111683512A (en) * | 2020-06-12 | 2020-09-18 | 安徽理工大学 | Microwave synthesis coal-based carbon/ferromagnetic metal composite electromagnetic absorption material and method |
| CN114836095A (en) * | 2022-05-17 | 2022-08-02 | 西北工业大学太仓长三角研究院 | Stealth composite material and preparation method thereof |
| CN116589756B (en) * | 2023-04-26 | 2024-03-29 | 合肥工业大学 | Preparation method of band magnetic control adjustable inverse opal-based wave-absorbing material |
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