CN111302826A - Ferrite/carbon composite inorganic foam wave-absorbing material and preparation method thereof - Google Patents
Ferrite/carbon composite inorganic foam wave-absorbing material and preparation method thereof Download PDFInfo
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/265—Compositions containing one or more ferrites of the group comprising manganese or zinc and one or more ferrites of the group comprising nickel, copper or cobalt
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/524—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from polymer precursors, e.g. glass-like carbon material
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/0615—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances the burned-out substance being a monolitic element having approximately the same dimensions as the final article, e.g. a porous polyurethane sheet or a prepreg obtained by bonding together resin particles
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Abstract
The invention discloses a ferrite/carbon composite inorganic foam wave-absorbing material and a preparation method thereof, wherein the ferrite/carbon composite inorganic foam wave-absorbing material comprises the following steps: firstly, preparing nickel-zinc ferrite wave-absorbing powder meeting the requirements by a ceramic synthesis process, secondly, preparing the powder into resin slurry, soaking a proper polyurethane foam material into the slurry, taking out the polyurethane foam material to remove the redundant slurry, and curing and drying the polyurethane foam material. And finally, putting the material into an atmosphere protection pyrolysis furnace for pyrolysis to form the ferrite/carbon composite inorganic foam wave-absorbing material. The composite inorganic foam wave-absorbing material has low surface density, high efficient absorption characteristic in a wave band from P to Ku, and high power bearing performance, can be independently applied to broadband high-power occasions, and meets the RCS reduction requirement.
Description
Technical Field
The invention relates to the technical field of wave-absorbing material preparation, in particular to a ferrite/carbon composite inorganic foam wave-absorbing material and a preparation method thereof.
Background
With the development of radar detection technology and the common application of 5G related technology in life, the demand of weaponry and civil communication fields on electric wave absorption materials is increased, and higher requirements on the surface density, application bandwidth, absorption effect, power capacity, service performance and the like of the electric wave absorption materials are provided.
In the aspect of solving the problems of large bandwidth and high absorption, in recent years, domestic research institutions generally obtain better performance by changing the structural form of materials, such as a multilayer structure, a cone structure and the like, and in addition, the design form of metamaterials is also adopted. By combining the research data at home and abroad, the reflection and absorption of more than-10 dB can be realized at 8-18GHz, the thickness is generally ensured to be within 10mm, and the absorption capacity is rapidly reduced if the frequency band extends to the P wave band. Generally speaking, no scheme is available at present, which can well realize efficient absorption from the P waveband to the Ku waveband and ensure that the areal density is low.
The invention aims to invent a material which has better absorption characteristics from a P waveband to a Ku waveband, can be used as a design base material of an all-dielectric metamaterial and obtains higher performance.
Disclosure of Invention
The invention provides a ferrite/carbon composite inorganic foam wave-absorbing material and a preparation method thereof in order to solve the various problems, and the material has broadband characteristics and power resistance characteristics which are not possessed by other materials at present. The preparation method of the material is simple and convenient in process and suitable for large-scale production.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a ferrite/carbon composite inorganic foam wave-absorbing material and a preparation method thereof are disclosed, wherein the preparation method comprises the following steps:
the method comprises the following steps: the formula design of the ferrite powder is designed according to the composition molecular formula Ni2-x-yZnxCuyFe2O4, wherein x is more than or equal to 0 and less than or equal to 0.5, and y is more than or equal to 0 and less than or equal to 0.2;
step two: weighing, namely weighing NiO, ZnO, CuO and Fe2O3 as raw materials according to the formula design result in the first step;
step three: mixing the components in the step two through a wet ball milling process;
step four: pre-sintering, namely drying the slurry in the step three, and then keeping the temperature for 2-10 hours at the maximum temperature of 1000-;
step five: performing secondary wet ball milling, namely performing wet ball milling on the pre-sintered material obtained in the step four to obtain powder with certain fineness for later use;
step six: mixing ferrite powder, phenolic resin and alcohol in the fifth step according to a certain proportion by a ball milling mode to form uniform slurry;
step seven: dipping, dipping the polyurethane foam material into the slurry in the step six, and taking out to remove the redundant slurry;
step eight: and (3) pyrolyzing the dried and cured polyurethane foam material at a high temperature under the protection of nitrogen to obtain the ferrite/carbon inorganic composite wave-absorbing material.
Preferably, the raw materials in step two are all analytically pure.
Preferably, the dispersant in the third step is purified water or alcohol, and the ratio of the dispersant in the third step to the dispersant in the fourth step is as follows: ball: the mass ratio of the dispersing agent is 1: (1.5-3.5): (0.8-1.5), adopting steel balls or zirconia ceramic balls as grinding balls, and carrying out ball milling for 1-24 hours;
preferably, the dispersant in the fifth step is purified water or alcohol, and the ratio of the dispersant to the alcohol is as follows: ball: the mass ratio of the dispersing agent is 1: (1.5-3.5): (0.8-1), adopting steel balls or zirconia ceramic balls as grinding balls, and carrying out ball milling for 1-24 hours;
preferably, the material in the step six: ball: phenolic resin: the mass ratio of the alcohol is 1: (1.5-3.5): (0.3-0.5): (0.5-1), adopting steel balls or zirconia ceramic balls as grinding balls, and carrying out ball milling for 1-24 hours; the solid content of the phenolic resin is 30-50%;
preferably, the aperture of the polyurethane foam adopted in the seventh step is 1-6mm, and the diameter of the foam rib is 0.5-1.5 mm;
preferably, the curing temperature used in step eight is 80-100 ℃ for 1-5 hours. The pyrolysis temperature is 800 ℃ and 1000 ℃, and the temperature is kept for 3-6 hours.
Compared with the prior art, the invention has the advantages that: (1) the composite inorganic material has through air holes, so that the matching with the space is further optimized, and the mismatching between the inorganic material and the space caused by high dielectric constant is solved.
(2) The broadband high-reflectivity optical fiber has excellent broadband characteristics, and tests show that the thickness is 10mm, the reflectivity of a P wave band is better than-5 dB, and the reflectivity of an L-Ku wave band is better than-10 dB.
(3) Compound medicineThe inorganic wave-absorbing material has good power-resistant characteristic and power capacity superior to 5kW/m2。
(4) For a 10mm thick material, the areal density is about 7kg/m2And has great advantages in inorganic materials.
Drawings
FIG. 1 is a wave-absorbing characteristic curve of embodiment 1 of a ferrite/carbon composite inorganic foam wave-absorbing material and a preparation method thereof.
FIG. 2 is a wave-absorbing characteristic curve of embodiment 2 of a ferrite/carbon composite inorganic foam wave-absorbing material and a preparation method thereof.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1:
the chemical composition molecular formula of the adopted ferrite powder is Ni2-x-yZnxCuyFe2O4, wherein x is 0.3, y is 0.2, and the detailed preparation process of the ferrite/carbon composite inorganic foam wave-absorbing material comprises the following steps:
the method comprises the following steps: the formula is designed, and the composition molecular formula is Ni2-x-yZnxCuyFe2O4, wherein x is 0.3, and y is 0.2;
step two: weighing, namely weighing NiO, ZnO, CuO and Fe2O3 as raw materials according to the formula design result in the first step, wherein the raw materials are analytically pure and have the total mass of 1 kg;
step three: and (2) wet mixing, namely mixing the components in the step (II) by a wet ball milling process, wherein the dispersant adopts alcohol: ball: the mass ratio of the alcohol is 1: 2: 0.8, adopting steel balls as grinding balls, and carrying out ball milling for 4 hours;
step four: pre-burning, drying the slurry in the third step, and keeping the temperature for 2 hours at the maximum pre-burning temperature of 1000 ℃;
step five: and (2) secondary wet ball milling, namely obtaining powder with certain fineness from the pre-sintered material in the step four in a wet ball milling mode for later use, wherein the dispersing agent adopts alcohol and comprises the following materials: ball: the mass ratio of the alcohol is 1: 2: 0.6, adopting steel balls as grinding balls, and carrying out ball milling for 6 hours;
step six: mixing ferrite powder, phenolic resin and alcohol in the step five into uniform slurry in a ball milling mode according to a certain proportion, wherein the material comprises the following components in parts by weight: ball: phenolic resin: the mass ratio of the alcohol is 1: 2: 0.5: 0.8, adopting steel balls as grinding balls, and carrying out ball milling for 2 hours; the solid content of the phenolic resin is 40 percent;
step seven: dipping, dipping the polyurethane foam material into the slurry obtained in the step six by adopting the polyurethane foam material with the aperture of 5mm and the diameter of the foam rib of 0.5mm, and taking out and removing the redundant slurry;
step eight: and (4) performing high-temperature pyrolysis, namely drying and curing the complex at 80 ℃, and performing pyrolysis on the complex under the nitrogen protection condition to obtain the ferrite/carbon inorganic composite wave-absorbing material, wherein the pyrolysis temperature is 800 ℃, and the heat preservation time is 3 hours.
The obtained sample is subjected to performance test after certain processing, and the reflection performance curve of the sample is shown in figure 1.
Example 2:
the chemical composition molecular formula of the adopted ferrite powder is Ni2-x-yZnxCuyFe2O4, wherein x is 0.3, y is 0.1, and the detailed preparation process of the ferrite/carbon composite inorganic foam wave-absorbing material comprises the following steps:
the method comprises the following steps: the formula is designed, and the composition molecular formula is Ni2-x-yZnxCuyFe2O4, wherein x is 0.3, and y is 0.1;
step two: weighing, namely weighing NiO, ZnO, CuO and Fe2O3 as raw materials according to the formula design result in the first step, wherein the raw materials are analytically pure and have the total mass of 1 kg;
step three: and (2) wet mixing, namely mixing the components in the step (II) by a wet ball milling process, wherein the dispersant adopts alcohol: ball: the mass ratio of the alcohol is 1: 2: 0.8, adopting steel balls as grinding balls, and carrying out ball milling for 4 hours;
step four: pre-burning, drying the slurry in the third step, and keeping the temperature for 2 hours at the maximum pre-burning temperature of 1000 ℃;
step five: and (2) secondary wet ball milling, namely obtaining powder with certain fineness from the pre-sintered material in the step four in a wet ball milling mode for later use, wherein the dispersing agent adopts alcohol and comprises the following materials: ball: the mass ratio of the alcohol is 1: 2: 0.6, adopting steel balls as grinding balls, and carrying out ball milling for 6 hours;
step six: mixing ferrite powder, phenolic resin and alcohol in the step five into uniform slurry in a ball milling mode according to a certain proportion, wherein the material comprises the following components in parts by weight: ball: phenolic resin: the mass ratio of the alcohol is 1: 2: 0.5: 0.8, adopting steel balls as grinding balls, and carrying out ball milling for 2 hours; the solid content of the phenolic resin is 40 percent;
step seven: dipping, namely dipping the polyurethane foam material into the slurry obtained in the step six by adopting the polyurethane foam material with the aperture of 6mm and the diameter of the foam rib of 1mm, and taking out and removing the redundant slurry;
step eight: and (4) performing high-temperature pyrolysis, namely drying and curing the complex at 80 ℃, and performing pyrolysis on the complex under the nitrogen protection condition to obtain the ferrite/carbon inorganic composite wave-absorbing material, wherein the pyrolysis temperature is 800 ℃, and the heat preservation time is 3 hours.
The obtained sample was subjected to a performance test after a certain processing, and the reflection performance curve thereof is shown in fig. 2.
Finally, it should be noted that the above mentioned embodiments are only preferred embodiments of the present invention, and not intended to limit the present invention, and it is obvious to those skilled in the art that modifications and partial technical equivalents may be made in the technical solutions of the above mentioned embodiments, and all technical solutions formed by equivalent substitutions or equivalent changes may fall within the protection scope of the present invention.
Claims (4)
1. A ferrite/carbon composite inorganic foam wave-absorbing material and a preparation method thereof are characterized in that the preparation method comprises the following steps:
the method comprises the following steps: preparing nickel-zinc ferrite powder by using an initial oxide raw material according to a powder synthesis process;
step two: obtaining resin slurry containing nickel-zinc ferrite powder by a ball milling method;
step three: coating a layer of resin slurry on the foam ribs of the polyurethane foam material by an impregnation method;
step four: curing the polyurethane foam wrapped with the resin slurry by a drying method;
step five: the dried and cured polyurethane foam is subjected to a high-temperature pyrolysis method to obtain the ferrite/carbon composite inorganic foam wave-absorbing material.
2. The ferrite/carbon composite inorganic foam wave-absorbing material and the preparation method thereof according to claim 1, wherein the ferrite/carbon composite inorganic foam wave-absorbing material comprises the following components: the initial oxide raw materials comprise zinc oxide, copper oxide, nickel protoxide and iron oxide; the powder synthesis process is to obtain powder meeting the requirements through processes of mixing, presintering and crushing oxides; the aperture of the polyurethane foam is 1-6mm, and the diameter of the foam rib is 0.5-1.5 mm; the resin slurry solvent component comprises phenolic resin and absolute ethyl alcohol; the pyrolysis temperature of the foam is 800-.
3. The ferrite/carbon composite inorganic foam wave-absorbing material and the preparation method thereof according to claim 2, wherein the ferrite/carbon composite inorganic foam wave-absorbing material comprises the following components: the proportion of the initial oxide raw material is Ni2-x-yZnxCuyFe2O4The molecular formula is that x is more than or equal to 0 and less than or equal to 0.5, and y is more than or equal to 0 and less than or equal to 0.2; in the powder synthesis process, the dispersion agent used for mixing the oxides is distilled water or absolute ethyl alcohol, the mixing time is 10-20 hours, the highest presintering temperature is 1000-1200 ℃, the heat preservation time is 2-10 hours, the grinding process adopts a ball milling mode, the dispersion agent is distilled water or absolute ethyl alcohol, and the ball milling time is 10-20 hours; and nitrogen is adopted for protection in the pyrolysis process.
4. The ferrite/carbon composite inorganic foam wave-absorbing material and the preparation method thereof according to claim 3, wherein the ferrite/carbon composite inorganic foam wave-absorbing material comprises the following components in parts by weight: the initial oxide raw materials are analytically pure; the particle size of the mixed oxides is normally distributed, the median diameter D50 is 2-4 μm, the particle size of the mixed oxides after presintering, crushing and ball milling is normally distributed, and the median diameter D50 is 0.5-1 μm; the solid content of the phenolic resin is 30-50%.
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Application publication date: 20200619 |